Final Report Summary - HELM (High-frequency ELectro-Magnetic technologies for advanced processing of ceramic matrix composites and graphite expansion)
Executive Summary:
Summary description of project context and objectives
Lightweight ceramics and fibre reinforced ceramic composites, such as non-oxide Ceramic Matrix Composites (CMCs) and Expanded Graphite (EG), represent very promising solutions for high temperature applications in strategic industrial sectors, such as transport and energy. Huge market opportunities are expected for CMC and EG provided to overcome the three major identified gaps: high cost, difficulty of processing and materials reliability. New and more efficient manufacturing technologies can pave the way to improve material quality, reduce processing time, converge towards near-net shape fabrication, trim energy spent and abate production costs.
HELM addressed these challenges by proposing innovative high-frequency electromagnetic, microwaves (MW) and radiofrequencies (RF), heating technologies for integrating and, in the long term, replacing standard thermal processing routes, i.e.: Chemical Vapour Infiltration (CVI), Liquid Silicon Infiltration (LSI), Polymer Impregnation and Pyrolysis (PIP), and Graphite Exfoliation (GE).
Description of work performed and main results
The activities were organized in three main pillars: pillar I, devoted to MW-CVI technique; Pillar II, devoted to MW assisted LSI and GE; Pillar III, dedicated to Polymer Impregnation and Pyrolysis (PIP). Transversal activities (TA) such as monitoring systems, modelling, LCA and TA, risk assessment, exploitation/dissemination and management were also considered.
The results of Pillar I activities brought to an improved knowledge of MW-CVI process thanks to the design, simulation and assembly of a pilot MW-CVI plant. The new plant was tested and infiltrations performed on three different materials. The investigations performed showed a reduction at one third of the infiltration duration. Some research is still needed for optimizing the properties of CMCs produced by MW-CVI.
The results of Pillar II activities resulted in an improved knowledge in the MW assisted LSI thanks to the building of one lab-scale prototype and the testing activities developed for optimizing both processing conditions and final properties of obtained CMCs. Two industrial pilot plants (one plant for antiballistic plates and brake system and one for SiC foams) were built and tested to obtain prototypes. In antiballistic applications and SiC foams the project reached the highest TRL, with processes and products close to market requirements. In the field of brake and GE expansion the results resulted quite promising, although some more research is needed to achieve materials properties close to the ones on the market.
The results of Pillar III consisted in the improved knowledge of the consortium about the MW/RF assisted pyrolysis and the design and assembly of a new MW/RF pyrolysis pilot plant. Thus, an up-scaled furnace was designed, constructed and validated, but there is still room for significant improvements. Some research is still needed for optimizing the properties of CMCs produced by MW/RF-pyrolysis.
Expected final results and potential impacts
The HELM projects produced results in terms of design, assembly and testing of new plants: innovations were introduced in this field because of the necessity of coupling MW or RF with conventional production processes, thus using alternative materials or modifying the design in order to achieve homogeneous fields and temperature. The produced materials resulted, in general, similar but not identical to the ones produced by conventional techniques. This point requires further research aimed at developing the opportunities evidenced in the HELM project.
Project Context and Objectives:
HELM project aims at designing and testing on a pilot scale advanced processing technologies based on high-frequency electromagnetic (EM) fields - microwaves (MW) and radiofrequencies (RF) – for thermal processing/treatment of CMCs (C/C, C/SiC and SiC/SiC composites for instance) and expanded graphite, such as: Polymer Impregnation and Pyrolysis (PIP), Liquid Silicon Infiltration (LSI), Chemical Vapour Infiltration (CVI), and Graphite Exfoliation (GE).
This project was organized in three main pillars: pillar I, devoted to MW-CVI technique; Pillar II, devoted to MW assisted LSI and GE; Pillar III, dedicated to Polymer Impregnation and Pyrolysis (PIP). Transversal activities (TA) such as monitoring systems, modelling, LCA and TA, risk assessment, exploitation/dissemination and management were also considered. In the following the objectives of the different Work Packages are reported.
Objectives of Work Packages (related to RTD and demonstration activities):
Objectives of WP1- MW assisted CVI (leader INSTM) (Pillar I)
The aim of this WP is the study and development of a hybrid thermal/MW assisted Chemical Vapour Infiltration (CVI) technology to achieve a reduction of about one order of magnitude in manufacturing time (20-30 hrs against 200-300 hrs) of CMCs, compared to conventional Isothermal CVI, by developing a cost-effective process route to build up the SiC matrix in 2D or 3D fibre performs.
Advanced MW heating (frequency combination) will be used to ensure the maximum EM field homogeneity inside the CVI-reactor, in order to achieve a homogeneous heating of samples of CMCs of realistic size based on carbon and silicon carbide fibers in carbon and silicon carbide matrices. A homogeneous heating will also help to reduce the processing time and permit energy saving in the CVI process.
Preforms of complex geometry will be selected for infiltration at operating temperatures between 900 and 1200°C.
Objectives of WP 2 - MW assisted LSI and GE (leader SUPSI) (Pillar II)
The specific objective of WP2 is to develop, assemble, and test a “modular” MW furnace capable for liquid silicon infiltration (LSI) and graphite expansion (GE) manufacturing. In particular the WP2 is devoted to:
• Develop a lab MW furnace for LSI;
• Develop a lab MW furnace for GE expansion;
• Optimize the MW assisted LSI process and product;
• Optimize MW assisted GE process and product.
Objectives of WP 3 - MW/RF assisted Pyrolysis (leader TECNALIA) (Pillar III)
The main objective of the WP3 is the reducing of time-cycle of the pyrolysis process for the manufacture of carbon fibre reinforced SiC and C ceramic composites (C/C and C/SiC), which are affected by high costs because of their long processing times and expensive raw materials. Therefore, it is a promising approach to develop a new process technology for the rapid pyrolysis of carbon fibre reinforced plastics (CFRP). Because of homogeneous heating, a rapid pyrolysis step can be achieved successfully using MW/RF assisted thermal treatment (conventional MW, mixed frequencies MW or RF). The porous C/C preforms can either be later infiltrated with a polymer, or subjected to additional infiltration/pyrolysis cycles until the required porosity is achieved, or siliconized to produce C/SiC composites in WP2. SiC pre-ceramic slurry systems, or SiC precursor polymers will be also considered for the infiltration step. Therefore specific aims of this WP are:
• Investigation of MW/RF assisted thermal treatment with respect to the conventional pyrolysis and PIP process.
• Investigation and evaluation of material properties.
• Proof-of-concept of MW/RF assisted thermal treatment with respect to the pyrolysis and PIP process.
Specific objectives for this task are a 10% improvement in the fracture toughness in comparison to conventional produced C/C and C/SiC. The process time will be reduced to less than 1/10 of the current process time, without shrinkage cracks, geometrical instabilities or other forms of damage due to the heat treatment. Related to the power consumption for MW assisted pyrolysis the objective is to achieve an energy saving of 25 % compared to conventional heating. In terms of cost efficiency, the final aim is to achieve a 25% reduction in production costs.
Objectives of WP4 - Development of new methodologies for high temperature MW/RF processing and process monitoring (leader CNR) (TA)
The goal of WP4 is to develop new methodologies for the homogeneous microwave and radio frequency heating of components of ceramic matrix composites, based on carbon and silicon carbide fibers in carbon and silicon carbide matrices, and for the monitoring of the growth process. In the framework of the WP, the acquisition of the information necessary to achieve this goal, mainly that related to the dielectric and thermal properties of the materials in the interval of temperatures of interest, will be carried out. The use of advanced multiphysics simulations, where the electromagnetic problem and the thermal problem are simultaneously solved, will allow a detailed modelling of the MW/RF and hybrid reactors in the working conditions.
The main objectives of the WP4 are:
• Characterization of the dielectric and thermal properties of the materials at the temperatures of the growth processes;
• Modelling and design of the MW/RF reactors and of the experiments;
• Development of a real-time measurement system of the dielectric properties of the ceramic composite part during the growth process;
• Development of a source system for a uniform MW/RF heating.
Objectives of WP 5 – Modeling and Simulation of Materials Processing (leader SUPSI) (TA)
This WP aims at implementing different modelling strategies in order to address specific aspects of the main processing methods (CVI, CVD, LSI, PIP) developed within the project. In particular, we will focus our attention on those microscale phenomena which can hardly be investigated using experimental tools, but that nonetheless yield a large influence on the final properties of the materials resulting from these processing techniques. Specifically, we intend to perform Density Functional Theory (DFT) and kinetic MonteCarlo (MC) simulations in order to study decomposition/reaction mechanisms in CVI/CVD processes, while we will employ recently developed Molecular Dynamics (MD) empirical potentials to investigate the reactive wetting phenomena taking place during LSI. In both cases, information obtained from these simulations will prove useful for a better understanding of phenomena occurring at the atomic scale during processing, and at the same time they will also serve as input data for further modelling at the mesoscopic scale. Mesoscopic modelling will be carried out by allowing for conjugate heat transfer and multicomponent gas transport in reactive porous media for CVI/CVD, whereas for LSI it will be based on the Lattice Boltzmann method. In this way, we aim at realizing a multiscale framework which can provide important insights about the underlying mechanisms controlling these processes and at the same time produce useful data for an effective calibration of process parameters. As far as PIP is concerned, due to the complexity of the decomposition reactions and to the scarcity of literature dealing with the modelling of this process, we will start from the current state of the art on this subject and intensively exploit DOE techniques of process optimization along with exploring the possibility of modelling such process using available commercial software.
Objectives of WP6 - MW-CVI process scale-up for refractory materials and aerospace (leader SKT) (Pillar I)
It was decided to design, develop and assemble a Hybrid Radiant/MW-CVI technology on a technical industrial level in order to demonstrate improvements in cost efficiency of CVI process of about 25% and reductions in energy consumption of about 25%. It is expected a cycle-time reduction to 1/10 compared to the conventional CVI process and a reduction of investment.
This task will also investigate possible improvements of homogeneity for CVI-produced CMCs like C/C , C/SiC and SiC/SiC and associated improvements in other properties like mechanical, physical or chemical behaviour. This WP will also provide information to WP12 and WP13 for the complete thermoeconomic analysis and process risk-analysis of the Hybrid Radiant/MW-CVI technology.
Objectives of WP7 - MW-LSI process scale-up for braking systems and antiballistic plate production (Leader BSCCB) (Pillar II)
WP7 aims to:
• Develop a pilot scale oven with MW or RF assisted heating for the LSI of SiCp/C and Cf reinforced carbon preform
• Optimize LSI scale process and products
• Technical assessment of CCM brake discs and SiC antiballistic plates produced by MW or EM-assisted
processing
Objectives of WP8 - MW-LSI process scale up for SiC foams production (leader ERBICOL) (PillarII)
WP8 objectives are:
- Reduce current processing time and costs. Because of higher heating rates and smaller heated mass, MW-LSI should allow a faster process and a smaller amount of energy consumption, resulting in time and energy savings.
- Improve material properties. MW-LSI allows processing at higher temperatures, up to 2000 °C, with a more uniform temperature distribution inside samples. This will led to new microstructures and enhanced material properties that will enlarge the application range of the product, actually limited to 1400°C.
- Production of volumetric pieces. Actual production technique, through convective heat transfer, limits the production of pieces with low volume. Through MW-LSI with a uniform heat distribution, the capillary diffusion of silicon is improved and the production of volumetric pieces should no more be a problem.
Objectives of WP 9 - MW assisted GE process scale-up (leader IMERYS) (Pillar II)
The aim of this WP is the up-scaling of the continuous MW assisted Graphite Expansion process. For this purpose, first a deep technical and economical evaluation of the process will be performed (T9.1) based on the results and experience acquired during WP2 and WP4. Following this evaluation a stop or go decision will be taken (MS9.1) on whether to build a demonstrator plant. The decision will also take into account the input from WP12 on life-cycle-analysis as well as from WP13 on process risk-analysis.
In the case the MW-GE process meets the requirement in term of economical efficiency and, especially, material improvement, a demonstrator plant will be designed, developed and installed (T9.2) based on the technical knowledge acquired during WP2 and WP4. All the information acquired will be then transferred to the WP12 and WP13 for completing the life-cycle-analysis as well as the process risk-analysis.
Objectives of WP 10 - MW/RF Pyrolysis process scale-up (leader AGI) (Pillar III)
The aim of this WP is to investigate the feasibility of the MW/RF-PIP technology upscale to fabricate large CMC structures for aerospace applications and of MW pyrolysis to produce preforms for LSI infiltration. To this purpose, first an in-depth technical and economical assessment of the MW/RF-PIP and MW pyrolysis will be performed, based on results of WP3 and a “Stop or Go” decision will be taken on whether to build an up-scaled MW/RF-PIP and/or MW pyrolysis equipment aiming to demonstrate the possibility of a further scale-up at industrial level of these processes. The decision will also take into consideration the input from WP12 on life-cycle-analysis and thermo-economic analysis and from WP13 on process risk-analysis.
In the case of the MW/RF-PIP technology, the implementation of this new technology will be considered successful if improvements in cost efficiency of PIP process of about 25% and reductions in energy consumption of about 25% will be achieved at up-scaled level. It is expected a cycle-time reduction to 1/10 compared to the conventional pyrolysis process. This task will also investigate possible improvements in other properties like mechanical, physical or chemical behaviour. An improvement of about 10% in fracture toughness, tensile strength and banding strength will be considered as a breakthrough in PIP technology. For MW pyrolysis technology, a pilot plant will be designed and built up to be able to process a preform of a brake disc. The implementation of the MW assisted pyrolysis for the manufacture of the brake disk is estimated to allow a reduction in thermal cycle from 48 to 12 h (with 75% time saving).
This WP will also provide information to WP12 and WP13 for the complete thermo-economic analysis and process risk-analysis of the MW/RF-PIP and/or MW pyrolysis technologies.
Objectives of WP11 - Pilot plant start-up and process validation (Demonstration) (leader INSTM) (all Pillars)
This WP collects the demonstration activities related to the WPs 6-7-8-9-10.
This WP will provide information to WP12 and WP13 for the complete LCA, LCC and TA analysis and process risk-analysis of the developed technology, to achieve a complete feasibility study, an overall comparison with the standard state-of-the art process technique and finally full assessment of the developed technologies and processes.
Objectives of WP12 - LCA and TA (Leader CIRCE) (TA)
WP12 aims to accomplish:
• The Assessment of the environmental (LCA), energy and exergy impacts, and associated costs to the new developed production processes compared to the conventional ones. Therefore the success and impact of the project can be measured and valorised.
• The provision of a diagnosis and advisory feedback over lab and demo scale developments. Therefore, potential improvements can be identified and implemented, enhancing the impact of the project.
Objectives of WP13 - Risk Assessment (leader R-TECH) (TA)
The WP addresses the following main open issues related to risks pertinent to HELM project:
• risks of "open innovation", i.e. risks of obtaining the desired result in terms of processing of ceramic matrix composites and graphite expansion under selected/given starting conditions,
• risks related to uncertainties in material characteristics (cf. ISO/IEC 17025, both the characteristics in the moment of obtaining the material and along its life cycle) and
• risks related to long-term impacts, including the both the HSE and socio-economical impacts as required by the new EU directives.
Project Results:
The scientific and technical results are discussed in this section by considering the different Work Packages, linked to the objectives of the project. The figures and tables referred in the text are reported in the annexed .pdf.
Work Package 1- MW assisted CVI (leader INSTM)
This Work package was dedicated to the design and assembly of a laboratory scale MW-CVI plant. The design activity involved INSTM, ATL, CNR, SKT, CVT and SAIREM. During the first 12 months of the project, the MW/ CVI plant has been designed and, for this purpose, some simulation tests were carried out.
The obtained results showed that, in order to obtain the necessary field uniformity, the size of the chamber of CVI should be larger than that of a laboratory scale furnace. For this reason, it was decided to go directly to the work stage of a pilot plant, expected in WP6, and this has resulted in an up-grade of the design work. The consortium decided of building the chamber in graphite, to avoid any contamination of the material produced and to use similar condition to conventional CVI equipment. Hence, on the basis of the design work described on deliverable D1.3 the assembly of the thermal/MW assisted CVI pilot plant was carried out. The preliminary testing of the plant was conducted in order to verify its functioning. The assembly work and the testing of the MW-CVI plant, built in ATL facilities (UK) was carried out on April 2014 and described in D1.4. The plant was then transferred to Pisa, where a laboratory was organized in the meantime considering all the requirements necessary for security and good working of the plant.
In the meantime ATL, SKT and CVT, on the basis of the knowledge of the state of the art about preparation of suitable preforms for CMCs, prepared and sent preforms based on Silicon Carbide (SiC) or Carbon (C ) to INSTM for allowing the scheduling of the successive infiltration trials. The different preforms shapes and properties were described in D1.5.
Hence the WP1 activity were propedeutic for the successive testing of the pilot plant and production of demonstration samples (WP6 and WP11-T11.1).
Work Package 2 - MW assisted LSI and GE (leader SUPSI)
After an extensive bibliographic research on the state of the art on MW processing, both on liquid silicon infiltration (LSI) and graphite expansion (GE), two documents (D2.1 and D2.2) were issued to give to the furnace manufacturer (FM) the requirements of the two furnaces. Furnaces were designed, manufactured and installed in collaboration with the industrial partners involved in WP2.
The LSI-MW furnace (D2.3) (Fig. 3) consists of a stainless steel vessel with a working zone of 250 mm in diameter and 150 mm in height. The double walls vessel (designed for vacuum levels up to 10-7 mbar) is water-cooled. The steel chamber is connected to four circular waveguides carrying a TM01 mode at 2.45 GHz. Each waveguide is supplied by an independent microwave generator delivering a power of 2 kV. As shown in Fig. 3, the system accounts on several sensors which are sending signals to the control rack. To improve in-plane temperature uniformity, a vertical rotation system is also installed. Angular velocities from 1 to 30 RPM can be selected. Samples’ temperature was measured from the top of the furnace (Fig. 4) with an optical pyrometer (PYROSPOT DSR 10N, DIAS Infrared, Dresden, Germany) equipped with a digital camera.
The infiltration process was carried out placing inside the furnace an original set-up represented in Fig. 5. It consisted in thin (1-2 mm) alumina cylindrical crucible (mostly transparent to MW) hosting the preform, the silicon grains and the susceptor powder bed. Rigid porous carbon felts were used to support the preform and to guide the molten silicon upon its melting. SiC/BN powder bed was uniformly distributed around the preform and the silicon to fill the empty space into the crucible. A boron nitride tube was placed as shown in Figure 3, enabling temperature measurement directly on the preform surface, otherwise covered with the SiC powder. The crucible was closed with a refractory lid of thin alumina with a central hole for the boron nitride tube.
Several pyrolysed micro porous preforms were produced and characterized to be Si-infiltrated by means of MW approach (D2.8).
The materials and the related HELM partners suppliers are here listed:
• C-SiC foams (Erbicol)
• C-SiC plates (Petroceramics)
• C-C preforms (BSCCB)
In a first step screening experiments allowed to asses MW-LSI feasibility. Later on process set-up was refined to increase products quality trough different series of experiments (Fig. 5). MW-LSI was applied successfully to ceramic foams by obtaining infiltrated parts of comparable to conventional products.
Microwave LSI of preforms embedded in powder field modifiers proved to be an effective method with respect to process time and energy consumption. The use of SiC/BN powder beds is an efficient way to convert MW power into heat while keeping temperature fairly uniform and without dispersing molten silicon upon its melting. Si-SiC (Petroceramics), composite (BSCCB) and foams (Erbicol) were successfully infiltrated in minutes (Fig. 6). The achieved product quality was assessed by each industrial partner to be almost the same as their standard industrial products.
A parallel Si-infiltration campaign by means of standard approach was carried by the University of Alicante (UA), in order to make a detailed comparison between the two techniques of infiltration.
UA studied the effect of vacuum, temperature and Si alloying in the synthesis of SiC by reactive infiltration, and compared the results with the standard products.
The design and characteristics of the MW GE (D2.4) furnace was fixed in D2.2. A schematic of the furnace is depicted in Fig. . The main components of the MW furnace are: 4x6 KW MW generators, an inclination system, a rotation system, a water cooling system, a feeder and a container for collecting the product. The MW furnace, as received from F&M, was modified by Imerys to better feed and collect the EG material.
Numerous tests were completed after some technical problems related to continuous processing were solved. More than 50 tests were performed varying the generators power, the feeder dosage, the gas flow, the inclination and the rotation. The time was kept constant for all the experiments at 1 min. After each GE reaction, the material was collected and weighed and the BET surface area and Scott apparent density were measured as control parameters of the process. A design of experiments (DOE) was used to analyse the data and to help to plan new experiments. In all cases it is observed a significant influence of the rotation and inclination parameters.
Results lead to the following conclusions:
• The maximum BET surface area values that were obtained after optimization of the parameters were in all cases ca. 45 m2/g, as compared to ca. 1 m2/g of the raw material.
• The highest BET values are obtained when either low values of inclination and rotation are used at low feeding rates, or a combination of low values of inclination and high values of rotation at higher feeding rates.
• The plots’ shape of the DOE results for the resulting BET when the generators’ power is lower than 90% is similar to the plots presented before with for instance an apparent maximum BET value of 35-40 m2/g when 50% power is used (see D2.7 for details).
• The use in practice of low values of inclination and rotation typically leads to complication in the transportation of the expanded graphite to the product container and lower productivity
The properties of the materials obtained with the MW furnace were comparable to the ones obtained with the current industrial process but still the productivity of the machine is considered as a lab-scale machine or small pilot-plant.
Some modifications to the current equipment were needed, such as a better or alternative gas transportation system, a better/alternative powder collection system and a further optimization of the process parameters, to increase the productivity and the efficiency of the process. Finally further decrease the reflected MW power is needed once the impedance matching (fine tuning of the MW generators) will be optimised.
Work Package 3 - MW/RF assisted Pyrolysis (leader TECNALIA)
The work carried out under WP3 in HELM project mainly consisted of the development of an MW/RF assisted Pyrolysis process suitable for intermediate products of the different industrial sectors of the project. In fact the intermediate samples were provided by BSCCB and PETROCERAMICS. Also final PIP products were prepared for AIRBUS GI and SCHUNK.
A programmatic approach was followed in correlation with WP10, having an up-to-date state-of-the-art and results from early stage of the project, through the workload at the refurbished lab furnace. Materials from four end users above indicated have been procured and processed: PETROCERAMICS (antiballistic protection), AIRBUS GI/SCHUNK (CMCs plates for the aerospace and energy sector) and BSCCBs (automotive brake disk).
The chosen approach for the MW/RF based pyrolysis and the design behind the up-scaled furnace is based on a full MW heating. The advantage is a maximization of the energy consumption and simplification of design, while the disadvantages are the associated high risk on design & development.
WP3, together with WP10 has been part of the Pillar 3 of HELM project. WP10 has been envisaged for the construction and validation of a pilot furnace, where WP3 has covered the research of the processes, the procurement of materials , the development of a lab scale furnace and the design of a pilot plant, which included two version: with quartz chamber and graphite chamber. Further details are given in the frame of WP10 description.
Main resources from Tecnalia in this WP3 package have been allocated on research and design activities to construct a lab furnace and complete the design of the up-scaled MW furnace. Procurement of new material batch has been carried out from BSCCB and AGI. A new material batch was delivered by SCHUNK to be processed by Tecnalia, as well as the new graphite chamber.
Moreover, further crosslink with WP1 (CVI), WP4 (MW processing and monitoring), WP5 (simulation), WP10 (pyrolysis process scale-up), WP12 (LCA-LCC) and WP13 (TRL calculation and risk analysis has been performed).
Work Package 4 - Development of new methodologies for high temperature MW/RF processing and process monitoring
The objectives and results of WP4 can be described according to the tasks composing the WP.
Task 4.1 - High-temperature dielectric characterization
Main objective: determination of the dielectric permittivity of the materials as a function of T.
Main obtained results:
- Construction of a setup capable of measurements up to 1200 °C and measurement times of about 300 ms, with high temperature uniformity over the sample;
- Development of a measurements and analysis methodology capable to extract with high accuracy the dielectric quantities from the cavity parameters, in a wide range of conditions;
- Determination of the dielectric properties of samples of interest for all the pillars (Ps) composing the project, in particular SiC fibers infiltrated by SiC for P1, α-SiC powders, Si powders, and β-SiC powders for P2, green body C/SiC and pyrolyzed C/SiC for P3.
The main task activity was conducted by CNR. FM contributed to the evaluation of the initial state-of-the-art. ATL provided samples for P1; Petroceramics, SUPSI, and BSCCB provided samples for P2; Tecnalia and AGI provided samples for P3.
Task 4.2 - High-temperature thermal properties
Main objective: determination of the thermal properties of the materials as a function of T.
Main obtained results:
- Definition of suited measurement setups and procedures;
- Determination of thermal conductivity, heat capacity, and linear expansion coefficient of samples of interest for all the pillars composing the project, in particular SiC/SiC and C/SiC for P1, C/SiC and Si-SiC for P2, and C/SiC for P3.
The main task activity was conducted by Petroceramics. ATL provided samples for P1, Petroceramic and BSCCB provided samples for P2, and AGI provided samples for P3.
Task 4.3 - Multiphysics simulation and design of experiments
Main objective: numerical simulation of the interrelated electromagnetic and thermal distributions in microwave reactors in operational conditions.
Main obtained results:
- Setup of suited simulation strategies for the investigation of reactor loaded by static and rotating samples, heated by means of a single port or multiport microwave excitation;
- Determination of the electromagnetic field and temperature distributions in the reactor and sample as a function of time;
- Analysis of the temperature uniformity in the sample volume. Optimization of the temperature uniformity by means of a combination of sample rotation and multiport microwave excitation.
The main task activity was conducted by CNR. Data from T4.1 T4.2 and T4.4 were employed.
Task 4.4 - Development of a source system for a uniform MW heating
Main objective: design of the microwave parts of the pilot-scale hybrid radiant/MW CVI reactor
Main obtained results:
- Definition of the most suited design approach, based on a closed oversized resonant structure;
- Design of the microwave reactor chamber, including a sample holder, a movable plate for the frequency tuning, and rotating waveguides for a continuous control over the MW polarization;
- Analysis of the most suited MW polarization as a function of the sample dielectric properties.
The main task activity was conducted by CNR. Sairem contributed to the design of the microwave excitation channels. INSTM contributed to the conceptual development.
Task 4.5 - Development of a Real-Time Monitoring System
Main objective: design and construction of a system for the real-time and in situ monitoring of the sample processing
Main obtained results:
- Construction and implementation of the system in the pilot-scale hybrid radiant/MW CVI reactor;
- Test and setup of the real-time monitoring system.
The main task activity was conducted by CNR. INSTM contributed to the conceptual development and to the test and setup of the system.
Work Package 5 – Modeling and Simulation of Materials Processing (SUPSI)
Task 5.1.1 – CVI/CVD Modeling – Atomistic Simulations. Objective: simulating decomposition and reaction mechanisms in CVI, in order to improve synthesis protocols. Results: (i) a reactive force field for describing the chemistry of MTS decomposition under hydrogen; (ii) the kinetic parameters of reaction mechanisms and successive reaction of the thus produced radical species with a growing SiC surface; (iii) an integrated computational protocol to simulate SiC CVI growth under steady-state conditions, in which DFT- and MD-based atomistic mechanisms are combined with statistical (kinetic Monte Carlo, kMC) sampling; (iv) a simulation of the long time scales relevant to experimental growth and prediction of growth rates as a function of environmental variables (temperature and reactant pressures)
Task 5.1.2 – CVI/CVD Modeling – Mesoscopic Modeling. Objective: finding process conditions which combine material performance with minimal infiltration time using simulation. Results: (i) a numerical algorithm and software package for 2D simulations allowing study of MW assisted CVI processes, allowing analysis of the flow pattern, thermal field and distributions of species concentrations in the gas region of the reactor and in the porous preform and evaluation of degree of densification; (ii) a parametric study of different modifications of CVI processes (including Isothermal, Thermal Gradient and Forced Flow CVI processes); (iii) a study of the temperature distribution in a MW CVI reactor and particularly in the bulk of the preform for different values of heating power of both MW and conventional heaters; all major mechanisms of heat transfer were considered: conductive, convective and radiative; (iv) a numerical study of flow pattern, thermal field and distributions of species concentrations in the gas region of the reactor and in the porous perform and evolution in time of the structure of the preform porous medium in the long-term MW assisted CVI process; (v) a numerical study of the long-term MW assisted CVI process for the final design of the plant with porous sample holder and a parametric study of effect of process parameters
Task 5.2.1 – LSI Modeling – Atomistic Simulations. Objective: evaluating different MD potentials with respect to their ability of describing reactive wetting phenomena in LSI. Results: (i) a study of the performance of different forcefields (ReaxFF, Tersoff, S-W) for the simulation of silicon melting using the Z-method; (ii) a MD protocol for the simulation of silicon droplets on different substrates (graphite, amorphous carbon, silicon carbide) and using different software (LAMMPS, MDCASK) and forcefields (Tersoff, ReaxFF)
Task 5.2.2 – LSI Modeling – Mesoscale Modeling. Objective: provide information on fundamental parameters controlling reactive infiltration by developing a LB code. Results: (i) a LB code for 2D simulations of capillary infiltration of structured channels and packing structures, including surface growth phenomena; (ii) a GPU implementation of the code, allowing a statistically accurate description of reaction wetting phenomena during silicon infiltration of carbon preforms; (iii) a parametric study of the influence of different factors in the infiltration process of channels (pore size and shape, liquid silicon velocity, growth rate); (iv) a direct comparison to experimental results obtained in the infiltration of mm-sized channels; (v) a parametric study of reactive wetting and infiltration of different packing structures (variable particle size and shape distributions) during LSI, allowing for the identification of factors and phenomena which determine the quality of the infiltration and the resulting material (e.g. porosity)
Task 5.3.1 – PIP Simulations – State of the Art of PIP Simulation. Objective: conducting a review on the state of the art methods for atomistic and mesoscopic simulation of PIP. Results: (i) a state of the art of available modeling and simulation methods for the study of the PIP process.
Task 5.3.2 – PIP Simulations – DOE for PIP Simulations. Objective: finding process conditions which combine material performance with minimal infiltration time. Results: (i) a screening of factors affecting the PIP process; (ii) the identification of the optimal process conditions (heating ramp duration, intermediate temperature) for MOR and weight loss; (iii) a factorial design for the analysis of the current experimental furnace obtaining a reduction of the time-cycle and the best mechanical performances of the material.
Work Package 6 - MW-CVI process scale-up for refractory materials and aerospace (leader SKT)
It was decided to design, develop and assemble a Hybrid Radiant/MW-CVI technology on a technical industrial level within WP 6. The main objective within this task was the set-up and test of a pilot Hybrid Radiant/MW-CVI plant at INSTM in Pisa (Subtask 6.2). This objective could completely be fulfilled. The set up of the plant was particularly complex for logistic reasons (installation of the necessary safety equipment) and technical reasons. The MW-CVI pilot plant was equipped with safety devices to take into account the different risks, such as explosion risks.
During test operations at high temperature the breakage of quartz windows occurred. The damages were caused by the decomposition of o-rings at high temperature and successive overheating. Hence many modifications to the plant were made in order to avoid this issue, introducing a cooling system, a Magic T system, reducing the wall thickness of graphite waveguide, adding graphite foil rings at end of graphite waveguide, using larger windows, changing the O-ring material, inserting a double quartz window and introducing a flow meter.
Conditions for SiC deposition were thus selected and the obtained deposited material was characterized. The deposited material is SiC, probably containing carbon. This testing and optimization activities related to the MW-CVI plant were described in D6.2.
After the set up of conditions it was possible to make a program of infiltrations aimed at assessing the working of the plant and its efficiency in different systems. A SiC preform, a C preinfiltrated preform and a preform consisting in knitted SiC Nicalon fabrics were the systems investigated. Several successive infiltrations were made on each system by varying processing parameters, such as pressure and gases flows. A systematic approach allowed the storage of all the information related to trials: (1) mass and parameters information; (2) Temperature profile along the trial; (3) pH profile in the scrubber; (4) Chamber temperature profile. The data of infiltration rate and also the data of efficiency were investigated in order to correlate with processing parameters. The shape and chemical composition of the preform influenced the infiltration rate. The characterization of materials allowed evidencing that the main compounds present in the composites matrix is SiC. However also some presence of minor components such as silica or nitrides was evidenced.
Some important limits must be overcome: the inhomogeneity of the infiltration (due to the inhomogeneity in heating), that can be overcome by proper rotation, and the deposition of powders in the graphite chambers or also in the furnace chamber resulting in quartz window periodical darkening to microwaves.
The MW-CVI plant can be used by INSTM for future activities and further parameter optimizations. Some problems could be already solved during installation like optimization of wave guides, cooling of flanges and improved optical ports. A preliminary technical and economical assessment of the Hybrid Radiant MW-CVI technology was thus possible. There exists still some open problems in order to enable a complete densification via MW/CVI technique. One open problem is the formation of dust. This dust formation results in a limitation of the maximum infiltration time of approximately 3 h in total. Further improvements of the quartz glass windows are necessary. The windows have to be modified by using a purge gas to avoid dust deposition on the windows. Furthermore, the sample holder has to be equipped with a rotation system in order to improve the homogeneity of the MW assisted CVI process.
The WP 6 enabled SKT to develop an isothermal CVI-SiC densification technique for high performance composites. In past SKT applied the CVI process only for mixed matrix systems or with a lower degree of densification for thermal insulation parts. The progress made in WP6 have shown further potentials for CVI optimizations at SKT, which will be used in future. Furthermore, CVT has improved their own rapid CVI-SiC densification method by optimization steps within WP 6. These two techniques were used for producing samples for comparative analysis. The processing data as well as their characteristics were described in D6.1.
Therefore, the objective of the optimization of the MW-CVI pilot plant is in a good progress, but not yet completed. This subtask (6.3) is an ongoing work, which will be continued by INSTM after the project. One open issue is the observed formation of impurities in the MW-CVI based SiC-matrix. The CVI matrix contained Silica as well as Silicon Nitrides. The reason for these impurities are not yet fully known and will be investigated after the project.
A second issue was the limitation in CVI densification due to the above mentioned dust formation. This incomplete densification as well as these impurities of the matrix did not allow to compare the mechanical, physical and microstructural properties of the MW-CVI based materials with conventional isothermal CVI densified samples.
Nevertheless, it could be demonstrated within WP 6 as well as WP 11 that the targets of energy efficiency of 25 % and expected cycle time reduction to 20% in comparison to isothermal CVI densifications seem to be feasible.
Work Package 7- MW-LSI process scale-up for braking systems and antiballistic plate production (Leader BSCCB)
In the frame of WP7, the task 7.1 was devoted to the technical evaluation of MW-LSI process to obtain braking systems (BSCCB) and antiballistic plates (Petroceramics).
The tested materials (Si-SiC samples for antiballistic and carbon ceramic samples for braking rotors purposes) have been made on small scale in WP2.
Petroceramics Si-SiC analysis
The lab scaled SiC plates Si-infiltrated by means of MW showed diffused small pores and local defects for every experimental setup and processing conditions. Anyway large areas of the samples were well infiltrated. The material well infiltrated has comparable values of flexural strength than the standard one, and the values of Young modulus are in line with the target for both well infiltrated and porous material.
BSCCB carbon ceramic analysis
Only small samples of carbon ceramic composite were made in the frame of WP2, not big enough to obtain specimens suitable to perform mechanical tests. As a consequence the material has been evaluated only in terms of the chemical-physical properties. The best thermal ramps and setups of LSI driven by means of MW entailed a carbon ceramic materials in line with the targets in terms of density, silicon uptake and microstructure.
Outcomes
LSI by means of MW approach seems a suitable way both for Si-SiC antiballistic plates and carbon ceramic brake rotors; on the basis of these evidences the scaled-up furnace building has been pursued.
In Task 7.2 Petroceramics designed and built a MW oven with a cavity able to Si-Infiltrate full scaled antiballistic plates and carbon ceramic rotors. The assembly was successfully completed and the functionality test of the components concluded. Operating at atmospheric pressure no plasma was observed at P=100%. On the basis of these evidences the experimental activity was perfomed and drove to the results reported in WP11 task 11.2.
Work Package 8 - MW-LSI process scale up for SiC foams production (leader ERBICOL)
During work package 8 a technical and economical assessment of the MW-LSI process for SiC foams was performed (task 8.1) and a pilot scale MW-furnace was designed and constructed. The work package was following WP2 where the concepts were performed at a laboratory scale and provided the input for the assessment.
The technical and economic evaluation of the MW-LSI process for SiC foams was performed in order to compare the conventional induction based process with the newly developed MW-LSI and understand if a pilot scale furnace was valuable both technically and economically. Following conclusions were drawn from the analysis:
- The process is much faster than conventional LSI, expected to be 50% faster at a pilot scale;
- The faster processing cycle increases equipment throughput, which means for a comparable investment the payback period is faster.
- Lower mass heated is the main performance advantage compare to induction heating;
- At full capacity, an overall cost saving of 20% can be expected;
- Product properties are lower than state of the art, but acceptable for non-structural applications.
Following the techno-economical evaluation of task 8.1 and the outcomes of lab-scale work package 2 for the liquid silicon infiltration of SiC foams, a pilot-scale MW-furnace of 30 L volume has been designed and built. Compared to the lab-scale furnace, the upscaling was done with more standard materials and power sources to keep costs competitive to conventional heating, and particular attention has been dedicated to the magnetron positioning to achieve an homogeneous field distribution inside the chamber. As a summary, following has been achieved:
- Modular design of the pilot-scale furnace (semi-continuous)
- Design of the cavity with asymmetric magnetron distribution to avoid high field heterogeneity
- Construction and assembly of the pilot scale MW-furnace for LSI of SiC foams
- Successful test runs up to a temperature of 1600°C in inert atmosphere
The assembled and tested furnace represents the successful end of work package 8 and the starting point for the test cycles and performance analysis of work package 11.
Work Package 9 - MW assisted GE process scale-up (leader IMERYS)
The aim of this WP was the up-scaling of the continuous MW assisted Graphite Expansion (GE) process. First a technical and economical evaluation of the process was performed based on the results and experience acquired during WP2 to decide whether to build a demonstrator plant or not.
Various parts of the initial set-up needed to be modified in order to make it run continuously and without leakages. In this context, the reactor tube rotation system was optimized and new O-rings were used at the inlet and the outlet for improving gas tightness. Different reaction parameters such as generators’ power, feeding, inclination, rotation and gas flow were modified to find optimum parameters to increase the surface area of the final product and decreasing the apparent density without blocking the reactor tube. During these tasks interactions with mainly SUPSI and F&M were essential to achieve the goals.
After all these optimizations, an economical evaluation of the process was performed taking into account a reaction using optimized parameters. The GE process by MW would need at this point of the project ca. 3 times more energy and it would cost ca. 5 times more than the industrial process. The properties of the materials obtained with the MW furnace are comparable to the ones obtained with the current industrial process but still the productivity of the machine is considered as a lab-scale machine or small pilot-plant.
It was decided not to construct a new industrial-scale pilot oven, but to modify/optimize the existing lab-scale machine to build a small lab-pilot furnace. In this context, the outlet of the equipment was modified in order to improve the material and gas transportation and product collection. A new filter-cyclone apparatus was installed using a plastic bag of container to collect the expanded graphite product. Moreover, two gas entrances were installed at the outlet to control the gas supply together with a suction valve to facilitate the transportation of the expanded graphite from the MW furnace to the filter/cyclone.
The previous design of the MW furnace for GE has been modified to make a lab/pilot scale MW equipment with increased EG productivity. The performance of the optimized lab-pilot MW furnace is a compromise between the properties and the productivity desired. The MW expanded graphite shows comparable electrical properties in a composite material as the industrially produced one with only slight differences depending on the treatment applied. A productivity of ca. 8kg/h with optimal material properties has been achieved at this point of the project. The process was be validated with focus on energy and cost reduction in order to be competitive with the industrial process (WP11).
Work Package 10 - MW/RF Pyrolysis process scale-up (leader AGI)
The objective of WP 10 was to investigate the feasibility of the MW/RF-PIP technology upscale to fabricate large CMC structures for aerospace applications and of MW pyrolysis to produce preforms for LSI infiltration. For this purpose, first an in-depth technical and economical assessment of the MW/RF-PIP and MW pyrolysis, based on results of WP3, was performed (Subtask 10.1). After a Go decision, up-scaled MW/RF-PIP and/or MW pyrolysis equipment aiming to demonstrate the possibility of a further scale-up at industrial level of these processes had to be build-up (Subtask 10.2 and 10.3).
The new technologies are considered successful if improvements in cost efficiency of about 25% and reductions in energy consumption of about 25% are achieved at up-scaled level. A cycle-time reduction to 1/10 compared to the conventional pyrolysis process was expected. The chosen approach for the MW/RF based pyrolysis was based on a full MW heating. The advantage is a maximization of the energy consumption and simplification of design, while the disadvantages are the associated high risk on design & development. A programmatic approach was followed, having results from early stage of the project, through the workload at the refurbished lab furnace. Materials from 4 end-users were processed: for Petroceramics materials excellent results were achieved at the lab furnace with quartz chamber (1 tile for each test). The set-up of the graphite chamber enables to process at least 4 tiles. It was possible to reach 600ºC within 2h without any oxidation signal. These tests enabled to validate the design of the graphite chamber. For AGI and SKT materials no arching was detected, as the MW field was designed to be perpendicular to fiber architectures. It was able to process large samples of about 300 x 300 mm2. However, the high ceramization temperature of e.g. 1600°C for PIP could not be reached due to some unsolved open problems (max. reached temperature was 600°C only). Hence, a complete ceramization process via MW/RF-PIP technology could not be performed within the project by Tecnalia, therefore there is still need of better MW adaptation in the near future.
BSCCB materials have been processed in a step-wise approach: at lab with no chamber, at lab with quartz chamber, up-scaled with quartz chamber and up-scaled with graphite chamber which was manufactured and delivered by SKT for the up-scaled MW/RF-PIP pilot plant according the design of Tecnalia. Two tests of pyrolysis with the up-scaled MW furnace have been performed on full scaled brake rotors. Due to issues related to the new equipment (too high temperature recorded on some equipment components), the tests were stopped at temperatures lower to the target one (that is over 600°C). The best trial entailed a weight loss of 16,7%, too low than expected (20wt%) but good enough to liquid silicon infiltrate the so pyrolyzed rotor by means of standard way. At present the reliability at full scale level was not completely tested but the good results fulfilled working at small scale seem to show that the MW approach seems promising also to pyrolyze a full rotor. Due to the lack of full rotors pyrolyzed by means of MW, not still available, at present it is not possible to make a reliable estimation of the costs and the energy consumption of the MW assisted pyrolysis. It can be highlighted that an up-scaled furnace was designed, constructed and validated, but there is still room for significant improvements, such as the optimization of the efficiency on BSCCB full rotors (max. pyrolysis temperature), better temperature homogeneity and integration of the second frequency 5.8 GHz to reach ceramization temperatures for the PIP technology.
Therefore it can be concluded, that the objective of the optimization of the pilot plant is in a good progress, but not yet completed. This subtask is an ongoing work, which will be continued by Tecnalia after the project. Main open issue is to reach the high ceramization temperature for the PIP technology which was not yet achieved. Consequently, it was not possible to compare the mechanical, physical and microstructural properties of the MW-PIP based materials with conventional PIP material samples. This target of WP 10 as well as WP 11 (subtask 11.5) could not be fulfilled within the project time. Tecnalia will work on this after the official project time. Nevertheless, it could be demonstrated within WP 10 as well as WP 11 that the target of expected cycle time reduction down to 1/10 in comparison to conventional processing seems to be feasible. A complete technical and economical evaluation of the MW/RF-Pyrolysis and PIP technology with conventional ones is only feasible, if all open issues are solved. All material data of the conventional processed material samples are available for comparison. Finally, it can be stated, that in WP10 there was an excellent collaboration and interaction among the involved partners.
Work Package 11 - Pilot plant start-up and process validation (Demonstration) (leader INSTM)
This WP collects the demonstration activities related to the WPs 6-7-8-9-10. The results are here summarized by considering the five different tasks of this WP.
Task 11.1 Hybrid radiant MW-CVI (task leader SKT)
Task 11.1 was aimed to compare the hybrid Radiant MW-CVI technology developed in the project with the more traditional CVI technologies. Because only a reduced number of experiments with a duration lower than three hours was possible by the new MW-CVI plant, a work of modelling was carried out to make a prediction about the potential reduction of processing time achievable by this new technique. All the predictions showed a remarkable reduction of processing time. Moreover, four infiltration trials were conducted in the same condition of CVT partner and on the same preforms provided by CVT on C based preforms preinfiltrated with SiC. The time of processing necessary for obtaining an increase in density from 0,71 to 0,91 g/cm3 was 15 hours by Rapid CVI and only 5,2 hours by MW-CVI. Hence, a reduction of time at one third of its value was achieved. Considering that the plant working was still not optimized (as described in D 6.3) and the system examined was the most difficult to process, because C-preforms do not heat easily through MWs, this result seems quite promising. Further optimization of the plant is necessary for a more definite assessment of the new technique.
Task 11.2 MW-LSI for braking system and anti-ballistic plates- pilot plant start-up and process validation (task leader BSCCB)
In this task the MW-LSI pilot scale furnace was set up for industrial production of anti-abllistic plates and 5 different setup configurations were tested to optimize materials heating. In the case of antibalistic plates prototypes production for demonstration 10 total runs of production for three different products were carried out. Mechanical properties of torso plate of some samples resulted comparable to those of well densified samples by standard heating process. In single shot test on some samples of torso plates the bullet was retained with a reduced trauma of baking layer. The analysis of the morphology showed that the properties of the MW-LSI plate was similar to the ones observed for conventional LSI, but some residual porosity could be noticed in the former. The total energy saving was 13% and time saving is also achieved.
For the production of demonstration prototypes of brake disks seven total MW_LSI runs for 1one disk size were carried out. The mechanical properties of four disks resulted close to the target but the porosity is higher than standard product and the thermal conductivity is far from the specification (<30-40%). For the production of brakes some optimization are still necessary to reduce the properties gap between the conventional and MW-LSI disks.
Task 11.3 MW-LSI for SiC foam- Pilot plant start-up and process validation (task leader ERBICOL)
The pilot MW-LSI furnace has been operated to validate process and equipment and compare it to the currently used induction furnace. Several demo samples has been produced and the furnace operations didn’t produce any serious problems or failures. Through the operation of the furnace, it was possible to demonstrate the compatibility of MW-LSI with SiSiC foam manufacturing, and collect process data to rank the MW-LSI furnace against the conventional one.
Total process energy savings of 38% have been achieved with MW-LSI, and an equipment productivity increase of 50% has been measured. Provided the MW-LSI equipment is 30% more expensive, a total 20% cost saving can be expected.
Hence, during the demo WP11.3 the furnace was successfully operated without major failures. The infiltration of SiC/C preforms was possible in a faster timeframe and delivering satisfying product properties. Summarizing, following conclusions can be drawn:
- The MW-LSI process is suitable for SiSiC foam processing and is faster than conventional LSI;
- The infiltration quality dependence on samples geometry has been overcome;
- Fully loaded MW-LSI furnaces have been processed delivering repeatable results and consistent product quality;
- The product properties of MW-LSI processed products are not as good as standard processed products, but the economic advantages of MW-LSI make the process a viable solution for a faster and cheaper liquid silicon infiltrations
Task 11.4 MW plant for GE production – pilot plant start-up and process validation (task leader IMERYS)
Several demonstration samples have been produced after modifying the equipment to be able to work at increased capacity. However, it was observed that the properties of the materials decrease when working at higher capacity. Therefore, as explained in D11.8 there are two possible scenarios that can be considered depending on the production capacity/energy/cost balance and the material properties.
The scale of the current plant is in fact too much small for achieving a good exploitation of the process developed in the HELM project for GE expansion based on MW. A scale-up machine based on the design used in HELM would probably help in optimizing the process/material properties and increase the production capacity. This possibility will be evaluated in the future.
The GE by the MW furnace build in the HELM project has shown, on a technical point of view, its potential to expand graphite in a way comparable to the industrial process. After optimization of the reaction parameters and accepting a compromise in the materials properties, a potential reduction in energy saving and production costs would be achievable. Final compatibility tests of the EG as filler in polymers and acceptance by clients would determine the potential of the process. Further increase of energy and cost saving could be realized with the scale-up of the process.
Task 11.5 MW-RF-PIP Pilot plant start-up and process validation (task leader SKT)
Several activities, trials and characterization performed at the pyrolysis and PIP up-scale equipment including a graphite chamber towards the development of a MW based PIP process. The technology has not been fully demonstrated at the up-scaled furnace. Nevertheless with the support of SUPSI (project partner) the technology has been demonstrated (in two separate steps) and a partial comparison of the technology has been feasible.
As a main conclusion, the MW/RF-PIP technology is quite promising for ~90% process time savings of std process (heating phase, excl. cooling down phase).
Work Package 12 - LCA and TA (Leader CIRCE)
A Life Cycle Analysis (LCA) can give very valuable information to assess the goodness of a solution with respect to different environmental categories. The reference impact categories chosen to refer the life cycle impact are carbon footprint in kg CO2-eq/kg and €/kg for the LCC. The main recommendations given for future improvements in the furnaces and processes using those furnaces, from an environmental and thermo-economic point of view, are summarized here below:
MW Furnaces.
1. The environmental impact of the furnace in the total process environmental impact is relatively small. The impact of the new equipment is usually higher as most of the components are made up of metallic parts with low batch manufacturing techniques. Furthermore, these furnaces are not fully optimized since the main purpose in the project is to prove feasibility.
2. For the final version of the MW industrial demonstrators, the absolute carbon footprint impact for the manufacturing of 1 unit of furnace, the relative allocation of this impact to each kg of material treated by the equipment (no energy included) and the LCC per kg (energy included) is represented in the table 1.
Processes
The results of Carbon footprint at every stage of the project for every pillar starting from the conventional process, then the lab scale testing, then the scale up testing, and finalizing with the improvement scenarios, are shown in the table 2.
With the exception of GE and CVI, all process show an improvement in carbon footprint when run with the new MW scale up furnaces in comparison with the conventional processes. The difference in GE is not very significant and in CVI, it could be cancelled out with a lower consumption of the MTS gas. These improvements could be part of further research. In all cases except GE, the efficiency in energy usage is much higher with the MW processes.
Besides the life cycle studies, exergy balances and thermoeconomic analyses were performed in order to assess the efficiency of the new technology from this novel approach. Although it is known that relevant energy savings are achieved with the new heating method (because the processing time is reduced), it is important to quantify this reduction and detect in which parts the processes have potentials of improvement.
Results showed that most of these conventional processes have low energy and exergy efficiency. A big amount of exergy is destroyed into the furnace systems and besides, there are large exergy losses in the by-products streams that could be recovered.
The new MW-systems were able to improve the conventional results for all processes from a thermoeconomic viewpoint (table below). Using the new heating mode, exergy yield has increased for all processes, especially in the most energy demanding processes, CVI and LSI. On the other hand, both the unit exergy consumption and the unit exergy cost have also improved for the five processes, and therefore, one of the main goals of the project has been successfully achieved. It must be taken into account that these MW-results were obtained from processes that they are not still completely optimized, and therefore, it is expected they will keep improving as the new systems are optimized.
Work Package 13 - Risk Assessment (leader R-TECH)
The work carried out by R-Tech represents an approach for appraisal of R&D technological and non-technological risks from an “open innovation” perspective. The approach developed is described as the ORnAMENT framework.
The ORnAMENT framework addresses the technological risks which are derived from the material and process characterization activities, OSHA and HSE identified risks. ORnAMENT framework is integrates a TRL calculator and tackle different issues identified and discussed in D13.1 by systematic method for risk comparison on the basis of quantitative scores. The framework represents an effective means to support r decisions concerned with investments in certain R&D efforts to reduce uncertainties in technological performance, avoid deviations from the project schedule or budget, and encourage technology exploitation.
The ORnAMENT methodology/tool developed afterwards was applied to the six HELM R&D efforts: 1) Chemical Vapour Infiltration; 2) Liquid Silicon Infiltration; 3) Graphite Exfoliation; 4) Pyrolysis for LSI; 5) Pyrolysis for ceramization of SiC/SiC; 6) Pyrolysis for ceramization of Cf/SiC. The risk of failure of each of them was calculated as function of the risk of failure to reach the required level of technological readiness and the sum of technology-specific risks potentially emerging from each R&D effort. These technological risks were integrated with non-technological (e.g. partnership, market, legal and regulatory) risks related to project management, external factors and the market into the HELM overall risk of failure. Preliminary results on the application of the ORnAMENT tool to the pillars of the project are detailed in the D13.6.
In order to collect information on the maturity of the HELM technologies and the probability and consequence of their risks, a survey was distributed to a group of 15 experts selected from the HELM Consortium, including the Coordinator, the Project Manager, Leaders of the technology pillars, the main contributing partners and the potential end-users of the developed technologies. The responses to this survey were complemented with information obtained by R-Tech from an analysis of the project deliverables and were used as inputs to the ORnAMENT methodology/tool, which was applied to assess the HELM R&D&I risks in months 24 (See D13.3 D13.4) and 47 (See D13.5 D13.6) of the project.
ORnAMENT proved to be a robust risk analysis tool, able to transparently provide adequate information for risk management decision making. Nevertheless, there is room for improving it. In order to achieve a more comprehensive appraisal of R&D project risks we recommend that the future version of the tool includes criteria and models to directly assess whether the project meets its schedule, cost, and performance success criteria, something that is only indirectly addressed by the current version of the tool.
GENERAL REMARKS ABOUT SCIENTIFIC AND TECHNICAL RESULTS OF THE HELM PROJECT
HELM project allowed demonstrating the feasibility of several processes for producing CMCs.
The Three pillars of the project (I-CVI, II-LSI and GE, III-PIP) corresponded to the most important industrial techniques actually used in industry to prepare CMCs and they were innovated thanks to the introduction of MW or RF.
The figure 11 shows the three different technical pillars related with the final applications considered in the project
First macro-result: a network of new innovative plants for CMCs production in Europe
The main objective of the HELM project was developing alternative techniques to produce CMCs by using microwaves and radio frequencies in order to reduce time and costs related to the processing of these materials. In this field, as described in the state of the art of the HELM proposal, new research was necessary as not many progresses were achieved in the last decades, despite of the enormous interests for these materials because their advanced performances and durability.
As reported in table 4, the project allowed in the first part the building of a totally new laboratory plant for MW-LSI, whereas laboratory scale tests were performed in refurbished existing plant for GE and PIP. Thanks to the design related to simulation and modelling it was possible to avoid the building of a laboratory scale plant for MW-CVI plant, skipping to the pilot phase. In the first phase of the project, carried out at a laboratory scale, three plants were thus used.
The further step was the building of pilot scale plants and this phase allowed the building of 4 new plants: one for MW-CVI infiltration of C and SiC preforms, one for Liquid silicon infiltration of brake and antiballistic plates, one for production of SiC foams and one for polymer infiltration and pyrolysis.
The building of the plants resulted a complex work because of technical difficulties, mainly due to plasma formation in the extreme conditions of the treatments, not easily predictable in some cases by the thorough work of simulation and modelling performed during the project (WP5).
Two of the new pilot plants were built in Italy, one in Spain and one in Switzerland, involving UK, Spain and Germany equipment producers involved in the project. This aspect evidences the European dimension of the developed network.
Many innovations were introduced in the plants and they were necessary for coupling the MW or RF techniques by the conventional techniques. Thanks to the collaboration among the consortium partners, ideas about design and used materials were shared in the consortium, thus boosting an easy application. The interdisciplinary feature of the consortium, involving experts of physics, chemistry, engineering and material science, and the use of the transversal activities, such as monitoring (WP4), modelling (WP5), LCA/LCC analysis (WP12) and risk analysis (WP13), resulted essential for reaching so many objectives in the project.
Second macro-result: new CMCs products based on the new MW-LSI technologies
The applications in the field of antiballistic plates and SiSiC foams were those in which a higher TRL, of at least 5, was achieved.
In particular mechanical properties of torso plate of some samples resulted comparable to those of well densified samples by standard heating process. In single shot test on some samples of torso plates the bullet was retained with a reduced trauma of back layer. The analysis of the morphology showed that the properties of the MW-LSI plate was similar to the ones observed for conventional LSI, but some residual porosity could be noticed in the former. The total energy saving was 13% and time saving is also achieved.
Moreover, it was possible to demonstrate the compatibility of MW-LSI with SiSiC foam manufacturing. In particular, the following conclusions can be drawn:
- The MW-LSI process is suitable for SiSiC foam processing and is faster than conventional LSI;
- The infiltration quality dependence on samples geometry has been overcome;
- Fully loaded MW-LSI furnaces have been processed delivering repeatable results and consistent product quality;
- The product properties of MW-LSI processed products are not as good as standard processed products, but the economic advantages of MW-LSI make the process a viable solution for a faster and cheaper liquid silicon infiltrations.
Demonstration prototypes of brake disks were also produced. The mechanical properties of four disks resulted close to the target but the porosity is higher than standard product and the thermal conductivity is far from the specification (<30-40%). For the production of brakes some optimization are still necessary to reduce the properties gap between the conventional and MW-LSI disks.
Third macro-result: new industry oriented knowledge in the production of CMCs
In all the pillars important knowledge results were achieved. The assistance of the monitoring techniques (WP4) applied to the different plants was fundamental for developing a knowledge about the processes.
In the MW-CVI process the use of a graphite furnace was demonstrated to be successful. The occurring of arching and plasma was demonstrated to be an issue during infiltration. Hence the conditions for infiltration must be found in pressure ranges where plasma formaton is suppressed and a peculiar configuration for sample holder is necessary for avoiding arching.
The resistance of materials employed in plants building to the high temperature generated by MW was found to be important and the necessity of cooling the coupling system (flanges) connecting the MW waveguides with the furnace was fundamental.
In the MW-LSI process the use of SiC powder susceptor for enhancing MW heating was found to be important and this result was the object of a publication. The results achieved at a laboratory scale were promising and the following scaling up into the two pilot plants of Pillar II allowed including peculiar design of magnetrons distribution keeping into account the preliminary results achieved in the laboratory plant.
In the MW/RF based pyrolysis Pillar the design behind the up-scaled furnace is based on a full MW heating keeping into account the results achieved in laboratory trials and with the aim of increasing the homogeneity of the magnetic field thanks to the peculiar waveguides distribution. The advantage is a maximization of the energy consumption and simplification of design, while the disadvantages are the associated high risk on design & development.
Dissemination activities (in particular related to scientific papers) indicate the achievement of excellent results during the project activities period. As the interdisciplinary approach typical of HELM project, being a pioneering one, is usually slow in giving a fast scientific production in terms of publications number, it can be reasonably predicted that the scientific advance of this project will be spread much also in the next years’ scientific publications about CMCs production and it will give further knowledge in the advanced ceramic materials sector. This knowledge is both of high scientific relevance and easily upheld by the market, as directly involving researchers of academy and companies.
Open issues and opportunities
Some still open issues were evidenced in the HELM project.
The objective of the optimization of the MW-CVI pilot plant is in a good progress, but not yet completed. This work will be continued by INSTM after the project. One open issue is the observed formation of impurities in the MW-CVI based SiC-matrix. The CVI matrix contained Silica as well as Silicon Nitrides. The reason for these impurities are not yet fully understood. A second issue was the limitation in CVI densification due to the dust formation on quartz windows, making impossible the realization of an infiltration longer than 3 hours up to now. This incomplete densification as well as these impurities of the matrix did not allow up to now to compare the mechanical, physical and microstructural properties of the MW-CVI based materials with conventional isothermal CVI densified samples.
The interests of HELM partners and stakeholders present at the final workshop can be addressed to a further optimization work in collaboration with INSTM and CNR, hosting the MW-CVI plant in Pisa.
In the case of MW-PIP it can be highlighted that an up-scaled furnace was designed, constructed and validated, but there is still room for significant improvements, such as the optimization of maximum pyrolysis temperature, better temperature homogeneity and integration of a second frequency to reach ceramization temperatures for the PIP technology. Therefore, the objective of the optimization of the pilot MW-PIP plant is in a good progress, but not yet completed. This subtask is an ongoing work, which will be continued by TECNALIA after the project. Main open issue is to reach the high ceramization temperature for the PIP technology which was not yet achieved. Consequently, it was not possible to compare the mechanical, physical and microstructural properties of the MW-PIP based materials with conventional PIP material samples.
Potential Impact:
POTENTIAL IMPACT
Ceramic Matrix Composites (CMCs) occupy a fundamental position in the transport sector (e.g. for elements of combustion engines of aircrafts, valve-trains, turbine blades, exhaust systems, cars braking systems) and energy sector (e.g. refractory materials for silicon foundry furnaces, energy reactors, gas burners and high pressure heat exchangers).
Regarding the technical impacts of the project, as explained in the “General remarks about Scientific and technical results of the HELM project”, interesting results were achieved in two products, both developed by the MW-LSI technique. In all the cases materials with lower properties than the conventional counterpart were obtained and this can be attributed also to the not complete optimization of the new techniques. However, in the production of antiballistic plates and SiSiC foams the MW-LSI technique was demonstrated to result in CMCs with properties similar to conventional counterparts, thus allowing predicting a fast impact on the market of these new technologies. The production of CMCs by the other techniques is also promising, but some more research is required for achieving the complete fulfilments of mechanical requirements of the developed materials.
Regarding the impacts on industrial manufacturing the building of the new plants suggested new industrial strategies for obtaining CMCs reducing processing time and energy consumption, in agreement with the objectives of the project. Companies involved in several applications of CMCs were directly impacted by the project activities.
Aerospace materials
In the HELM project the aerospace materials involve HERAKLES and AIRBUS (AGI).
HERAKLES is one of the world’s leaders in the design and production of solid rocket motors for missiles and space launchers. For more than 30 years, HERAKLES has been using thermostructural composites, designed to withstand very high loads in extreme environments and has focused his industrial efforts on CVI technology for producing CMCs for aerospace applications.
The HELM project impacted HERAKLES industrial activities thanks to the knowledge and deeper understanding of phenomena associated with MW assisted CVI. The project provided also some preliminary results about the feasibility to build MW-CVI furnaces. The reduction of processing time achieved in the project is quite promising.
AIRBUS Group is interested in all the 3 main standard process routes for the fabrication of non-oxide CMC: Polymer Infiltration Pyrolysis (PIP), Liquid Silicon Infiltration and Chemical Vapour Infiltration (CVI). However, the main commitment of AGI in HELM is to investigate the hybrid or MW/RF assisted PIP to demonstrate its feasibility (proof-of-concept) as a cost-effective process route to manufacture SiC matrix CMC materials with C and/or SiC fibre 2D/3D performs. PIP process manufactured C/SiC is currently used in AGI for Thermal Protection Systems (TPS) and Hot
Structures (HS), for instance for re-entry vehicles as well as for propulsion parts because of excellent material characteristics. HELM project contributed to demonstrating the suitability of MW/RF techniques to manufacture components, although an optimization of the pilot scale plant is still necessary.
Refractory materials
SKT is one of the leading enterprises in the field of CVI and CVD processes for graphites and composites worldwide. These manufacturing methods are all based on PIP, silicon modifications (e. g. LSI), CVI and CVD techniques as well as heat treatments for pyrolysis and graphitization treatments. The SKT main business is the manufacture of CMC-structural components for industrial plants for polysilicon production: heaters; thermal insulations; heat shields; crucibles; tools. All these applications require highest purity (low carbon contamination), toughness, thermal resistance up to 2000 °C, cost efficient, low methanisation rate, oxidation/corrosion resistance against SiO2. To this, CVI technique is the most suitable one.
The HELM project enabled SKT to develop an isothermal CVI-SiC densification technique for high performance composites. In past SKT applied the CVI process only for mixed matrix systems or with a lower degree of densification for thermal insulation parts. The progress made in WP6 have shown further potentials for CVI optimizations at SKT, which will be used in future.
Rapid CVI processing
CVT has more than 25 years experience in CVD and CVI and holds the patented process of rapid-CVI (r-CVI), well defined and high reproducible CVI procedure in house. The r-CVI is a fast and reliable techniques for manufacturing carbon-carbon (C/C) and carbon-silicon carbide (C/SiC) materials which allows densification of carbon fiber preforms within days (less than 30% wrt traditional method). For this specific competence, CVT is technology partner of SKT and AGI for r-CVI manufacturing of high purity materials with also high density, extremely uniform densification and adjustable matrix regarding texture of infiltrated carbon. CVT has improved their own rapid CVI-SiC densification method by optimization steps within WP 6.
Carbon-ceramic brake disks
BSCCB, a joint venture between Brembo SpA and SGL Brakes GmbH, is a world leader in the sector of carboceramic rotors manufacturing for high performance brake systems. Automotive brake disks are representing the first large scale application of CMC materials.
The role of BSCCB in HELM was to exploit newly developed MW-LSI and MW/RF assisted pyrolysis for the production of ceramic carbon-ceramic brake disks.
Demonstration prototypes of brake disks were produced and the mechanical properties of four disks resulted close to the target but the porosity is higher than standard product and the thermal conductivity is far from the specification (<30-40%). For the production of brakes some optimization are still necessary to reduce the properties gap between the conventional and MW-LSI disks.
Preliminary promising results were achieved also by RW-PIP technologies. Also in this case further optimizations, mainly in processing, are needed.
Antiballistic materials
PETROCERAMICS has experience in the production of antiballistic ceramics made of carbides, nitrides and carbon pre-forms densified via liquid silicon infiltration (LSI) process. Thanks to HELM project a MW-LSI pilot plant was built and tested. Mechanical properties of torso plates produced in HEM project by MW-LSI pilot plant resulted comparable to those of well densified samples by standard heating process. In single shot test on some samples of torso plates the bullet was retained with a reduced trauma of back layer. The analysis of the morphology showed that the properties of the MW-LSI plate was similar to the ones observed for conventional LSI, but some residual porosity could be noticed in the former. The total energy saving was 13% and time saving is also achieved.
SiC foams
ERBICOL is active since in the production of porous ceramics made of silicon infiltrated silicon carbide for components working in high temperature, harsh environments, where are needed materials with high thermal conductivity, high thermal shock resistance and high corrosion resistance. Such products are gas burners, radiation plates, fuel cell reformers, catalyst support and many more.
Thanks to the HELM project activities it was possible to build a MW-LSI pilot plant for foams and demonstrate the compatibility of MW-LSI with SiC foam manufacturing. In particular, the following conclusions can be drawn:
- The MW-LSI process is suitable for SiSiC foam processing and is faster than conventional LSI;
- The infiltration quality dependence on samples geometry has been overcome;
- Fully loaded MW-LSI furnaces have been processed delivering repeatable results and consistent product quality;
- The product properties of MW-LSI processed products are not as good as standard processed products, but the economic advantages of MW-LSI make the process a viable solution for a faster and cheaper liquid silicon infiltrations.
Expanded graphite
IMERYS produces high quality expanded graphite for energy applications, electrochemical storage devices, fuel cells and solar ovens, with about 2,500 t/year production and 11 Mio€ revenues annually for this segment
worldwide. The GE by the MW furnace built in the HELM project has shown, on a technical point of view, its potential to expand graphite in a way comparable to the industrial process. After optimization of the reaction parameters and accepting a compromise in the materials properties, a potential reduction in energy saving and production costs would be achievable. Final compatibility tests of the EG as filler in polymers and acceptance by clients would determine the potential of the process. Further increase of energy and cost saving could be realized with the scale-up of the process.
Impact on SMEs innovation and technology
The HELM project provided the three SMEs (ATL, FM, SAIREM) with a new technology portfolio for MW/RF processing of CMCs and GE. The expected outcome will bring development of new knowledge, new technologies and economic revenues for these SME participants.
ATL developed a hybrid/MW assisted CVI plant that will be included in his catalogue, while SAIREM and FM have the know-how on advanced MW and RF heating and can thus enrich their catalogue of products: FM
developed ovens for MW assisted LSI and GE, SAIREM developed MW componente for MW-CVI plant and RF furnace for Pyrolysis.
Environmental impact
The full LCA, LCC and TA performed in the HELM project definitively showed the benefits of proposed technologies in terms of using optimal amounts of raw materials, energy consumption and other energy saving
features.
Moreover, the spreading of CMCs in more sectors can allow the use of more durable materials, thus immediately decreasing generation of waste.
Another indirect good environmental impact consists of the development of materials for more efficient engines, allowing a reduction of fuel consumption and thus reducing not renewable resources consumption and related pollution/greenhouse effects.
Socio-economic impact
HELM project allowed the development of innovative technologies in manufacturing advanced materials to improve EU economy. By boosting the use of new processes it promoted the introduction of advanced materials on the market thus directly promoting new job opportunities in Europe. Moreover, these job opportunities are opened in the field of advanced manufacturing, considered strategic in research and innovation action strategies for SMART specializations by the Tuscany region (Italy). Smart Specialisation Strategy means the national or regional innovation strategies which set priorities in order to build competitive advantage by developing and matching research and innovation own strengths to business needs in order to address emerging opportunities and market developments in a coherent manner, while avoiding duplication and fragmentation of efforts” (Regulation 1301/2013 of the European Parliament and of the Council of 17 December 2013 ). Hence these new job places contribute to the convertion to SMART economy promoted by EC.
DISSEMINATION STRATEGY
The objective of the dissemination strategy applied was to identify and organise the activities to be performed in order to maximise the influence of the project and to promote commercial and other exploitation of the project results.
In more detail, the objectives of the dissemination were:
I. To raise public awareness about the project, its expected results and progress within defined target groups using effective communication means and tools;
II. To disseminate the fundamental knowledge, the methodologies and technologies developed during the project;
III. To pave the way for a successful commercial and non-commercial exploitation of the project outcomes.
In accordance with the Grant Agreement indications, every possible opportunity was embraced by individual partners or on collective basis through joint appearance to make HELM known among professionals and general public as well.
Ensuring effective internal communication and dissemination among the Consortium partners represented an important key success element for the Project. Periodic Meetings and TELCOs and the set-up of a Project Collaborative space were used as means to ensure a constant and effective of internal dissemination.
External dissemination targeted Academic and research community, Industrial sector, Industrial Associations, Government bodies and policy makers as well as Media and public community, at national, European and International level.
Dissemination activities in HELM project were deeply linked with the intellectual property (IP) rights protection. All issues regarding Intellectual property use and dissemination were specifically regulated by the EC-GA Articles II.26-II.34. Practical application of IP rights protection, and dissemination procedures agreed among HELM project partners were regulated also by the Consortium Agreement.
DISSEMINATION ACTIVITIES
A common graphic identity was defined at the beginning of the Project to allow for better visibility and recognition as well as branding of the HELM project, paying specific attention to the EC funding acknowledgement. Indeed all publications based on work funded by EC within the activities of the HELM Project acknowledged their affiliation to HELM and bear recognition of the EC funding.
To ensure maximum visibility to the HELM objectives and results a project website was set up registering in the “eu” domain and with intuitive URL to increase hit rates: http://www.helm-project.eu/
The design of the website built upon the following criteria, taking into account suggestions given in the EU Project Websites – Best Practice Guidelines (EC, 2010):
i. visual communication: use of colours and/or photos, web pages are easy to browse, information is kept short and links are included to websites, publications, and so on.
ii. verbal communication: the website uses simple phrasing, no jargon is used in order to attract the widest possible audience, e-devices are user friendly.
iii. visibility: maximum use of free or affordable methods to increase page ranking on search engines, Webmaster Tools provided by search engines to check indexing status, good cross-linking between the different pages of your site and other sites, add keywords to the web page metadata; use frequently used keyword search phrases both in the metadata and in the contents pages.
iv. regular update of contents: the website was maintained and the update regularly done by the Webmaster upon inputs from the partners; social media were also used.
v. Monitoring and feedback tools: the website includes a counter of visitors to measure the number of visits; a visitors’ feedback form, to get a feedback on the usability of the web site and on the interest created by the project.
The public section of the HELM website therefore:
▪ provides a brief project summary in journalistic style highlighting the objectives, the contents and the structure of the HELM Project including the composition of the HELM Consortium.
▪ provides a short profile of each of the HELM Partners and a link to the related web sites;
▪ provides access to the project Public Deliverables and abstracts of selected non-Public Deliverables;
▪ provides copies of publications and presentations done at external conferences;
▪ features a separate events section where events are registered and highlighted. It refers to HELM events such as HELM meetings and workshop, and conferences and external events where HELM had an active role (e.g. presentation of paper(s), organisation of sessions, stands with demos, etc.).
Also, Social Media channels were activated and maintained to increase visibility and thus raise public awareness:
Facebook https://www.facebook.com/pages/HELM-EU-Funded-Project/441410005901081
Linked-in https://www.linkedin.com/groups/8129092
Google+ https://plus.google.com/102803555881338454738
You Tube https://www.youtube.com/channel/UCxziJrpOd6QSa-dhi48r62Q ,
Twitter https://twitter.com/HelmEuFunded
HELM standard Flyer and Poster were issued, published, restyled and distributed throughout the project duration, with the aim to intensify and strengthen the effect of recognition of the Project.
The main objective of the project brochure is to provide our audiences with an attractive and written project overview and a summary of the main project objectives and characteristics. To assist the dissemination effort, an attractive and professionally made brochure has been prepared and published on the project website.
The brochure presents the goals of the project and the main (expected) findings. The text was designed taking in to account not only experts, but also an interested non-specialist. It introduced the main mission and the goals of the project. Furthermore, it included the website address and provides basic information on Consortium. All partners’ logos were also displayed.
The main purpose of the project poster is to catch the audience attention, with a visual representation clear and easily understandable by the target end users. To reach this objective an eye catching poster was designed, then restyled and updated.
With regard to the layout and design, the poster showed the project’s logo and the colours emphasizing the link to the project´s graphic.
From the content point of view, the standard poster illustrated the project objectives and included basic information on the project and on the Consortium, including all partners’ logos. It is possible to download it from the HELM website.
HELM consortium also operated with a proactive approach to the dissemination of the project objectives first and results later.
Press releases on partners’ websites were issued at the beginning of the project. Articles were published on scientific journals (Engineering Applications of Computational Fluid Mechanics, Ceramics International, Ceramic Transactions, Journal of European Ceramic Society, International Journal of Modern Physics, Developments in Strategic Materials and Computational Design, Wetting and Wettability) and more popular magazines (Platinum-on-line) throughout the project duration.
Newsletters were issued periodically, in order to present the project activities and results to interested parties, also through the website.
Posters were presented at relevant conferences and the project results presented orally to congresses and scientific events (also at yearly or periodic conferences such as: ECOS, ICACC, EUROMAT, ENF, HTCMC, NANOTECHITALY). Several sector Stakeholder and Academic representatives were contacted to discuss the project perspectives on all occasions.
Also, a final workshop on "Advanced Processing Technologies – institutional investments, research results and market potential" was organized at the end of the Project, on May 31st 2016, hosted by Consiglio Nazionale delle Ricerca in Pisa (IT). HELM Consortium met academic and industrial stakeholders and interested parties, to discuss research results and future developments of Advanced Processing Technologies. During the final workshop, the CVI Furnace and its results were shown, raising the interest of various industrial entities. Potential synergies and future collaborations were envisaged, to further HELM results in the future.
Ultimately, the Project has capitalized on varied opportunities to disseminate the Project results, in order to increase and cement the exploitation potential.
EXPLOITATION OF RESULTS
HELM was intended as a strategic project from the industrial point of view, considering that industry and market needs are the main drivers of development and integration of the proposed MW/RF thermal processing technologies.
CMCs and EG are advanced materials where Europe has outstanding leadership at global level; indeed some of those leaders are involved in HELM. HELM took into consideration the most significant market niches for C/SiC or SiC/SiC composites and EG, i.e.:
▪ aerospace thermos-structural composites (HERAKLES SA, AIRBUS DEFENCE AND SPACE GMBH)
▪ refractory materials (SCHUNK KOHLENSTOFF-TECHNIK GMBH, CVT GMBH & CO KG)
▪ ceramics for brake systems (BREMBO SGL CARBON CERAMIC BRAKES SPA)
▪ antiballistic applications (PETROCERAMICS SPA),
▪ silicon carbide foams (ERBICOL SA), and
▪ expended graphite production (IMERYS GRAPHITE & CARBON SWITZERLAND LTD).
At the same time, the project involved three innovate SMEs involved in the technical development (ARCHER TECHNICOAT LIMITED, FRICKE UND MALLAH MICROWAVE TECHNOLOGY GMBH and SAIREM IBERICA S.L.) for MW/RF processing of CMCs and GE.
The HELM Consortium therefore addressed the need of new technical solutions for European companies in the field to stay competitive in the market of CMCs and EG, requiring higher performance products at lower cost. Indeed the results obtained showed a relevant potential in reducing processing time and costs, as illustrated in the previous sections.
All partners of HELM owning exploitable results or in any case having acquired useful knowledge planned exploitation in different manners, jointly or individually. Indeed cooperation between the partners, during and after the project, played and plays an essential role in the successful exploitation of the innovations originated in HELM.
Research partners are clearly more oriented to transfer knowledge in academia and technology to interested stakeholders, while industries strongly focus on industrialization and future commercialization of the research products and by-products.
To be noticed that academic and research partners (CONSORZIO INTERUNIVERSITARIO NAZIONALE PER LA SCIENZA E TECNOLOGIA DEI MATERIALI, SCUOLA UNIVERSITARIA PROFESSIONALE DELLA SVIZZERA ITALIANA, FUNDACION TECNALIA RESEARCH & INNOVATION, FUNDACION CIRCE CENTRO DE INVESTIGACION DE RECURSOS Y CONSUMOS ENERGETICOS, BALTIC STATE TECHNICAL UNIVERSITY VOENMEKH, UNIVERSIDAD DE ALICANTE, Steinbeis Advanced Risk Technologies GmbH and CONSIGLIO NAZIONALE DELLE RICERCHE) as well defined further research paths and exploitation plans for the knowledge acquired and technology developed.
Therefore, it is planned to have a full return on the results achieved thanks to the investment from the EC both from the academic and industrial perspective, also joined in one unique approach, through further research, development and industrialization activities.
However, exploitable results and related exploitation plans within HELM are regulated by confidentiality and IPR management rules, therefore no details can be publicly disclosed.
List of Websites:
PROJECT WEBSITE:
http://www.helm-project.eu/
CONTACT DETAILS:
Andrea Lazzeri
andrea.lazzeri@unipi.it
Tel: +39 050-2217807
Fax: +39 050-2217903
Isella Vicini
isella.vicini@warrantgroup.it
Tel: +39 051 9840863
Fax: +39 051 9840885
Cinzia Iacono
cinzia.iacono@warrantgroup.it
Tel: +39 051 9840863
Fax: +39 051 9840885
Summary description of project context and objectives
Lightweight ceramics and fibre reinforced ceramic composites, such as non-oxide Ceramic Matrix Composites (CMCs) and Expanded Graphite (EG), represent very promising solutions for high temperature applications in strategic industrial sectors, such as transport and energy. Huge market opportunities are expected for CMC and EG provided to overcome the three major identified gaps: high cost, difficulty of processing and materials reliability. New and more efficient manufacturing technologies can pave the way to improve material quality, reduce processing time, converge towards near-net shape fabrication, trim energy spent and abate production costs.
HELM addressed these challenges by proposing innovative high-frequency electromagnetic, microwaves (MW) and radiofrequencies (RF), heating technologies for integrating and, in the long term, replacing standard thermal processing routes, i.e.: Chemical Vapour Infiltration (CVI), Liquid Silicon Infiltration (LSI), Polymer Impregnation and Pyrolysis (PIP), and Graphite Exfoliation (GE).
Description of work performed and main results
The activities were organized in three main pillars: pillar I, devoted to MW-CVI technique; Pillar II, devoted to MW assisted LSI and GE; Pillar III, dedicated to Polymer Impregnation and Pyrolysis (PIP). Transversal activities (TA) such as monitoring systems, modelling, LCA and TA, risk assessment, exploitation/dissemination and management were also considered.
The results of Pillar I activities brought to an improved knowledge of MW-CVI process thanks to the design, simulation and assembly of a pilot MW-CVI plant. The new plant was tested and infiltrations performed on three different materials. The investigations performed showed a reduction at one third of the infiltration duration. Some research is still needed for optimizing the properties of CMCs produced by MW-CVI.
The results of Pillar II activities resulted in an improved knowledge in the MW assisted LSI thanks to the building of one lab-scale prototype and the testing activities developed for optimizing both processing conditions and final properties of obtained CMCs. Two industrial pilot plants (one plant for antiballistic plates and brake system and one for SiC foams) were built and tested to obtain prototypes. In antiballistic applications and SiC foams the project reached the highest TRL, with processes and products close to market requirements. In the field of brake and GE expansion the results resulted quite promising, although some more research is needed to achieve materials properties close to the ones on the market.
The results of Pillar III consisted in the improved knowledge of the consortium about the MW/RF assisted pyrolysis and the design and assembly of a new MW/RF pyrolysis pilot plant. Thus, an up-scaled furnace was designed, constructed and validated, but there is still room for significant improvements. Some research is still needed for optimizing the properties of CMCs produced by MW/RF-pyrolysis.
Expected final results and potential impacts
The HELM projects produced results in terms of design, assembly and testing of new plants: innovations were introduced in this field because of the necessity of coupling MW or RF with conventional production processes, thus using alternative materials or modifying the design in order to achieve homogeneous fields and temperature. The produced materials resulted, in general, similar but not identical to the ones produced by conventional techniques. This point requires further research aimed at developing the opportunities evidenced in the HELM project.
Project Context and Objectives:
HELM project aims at designing and testing on a pilot scale advanced processing technologies based on high-frequency electromagnetic (EM) fields - microwaves (MW) and radiofrequencies (RF) – for thermal processing/treatment of CMCs (C/C, C/SiC and SiC/SiC composites for instance) and expanded graphite, such as: Polymer Impregnation and Pyrolysis (PIP), Liquid Silicon Infiltration (LSI), Chemical Vapour Infiltration (CVI), and Graphite Exfoliation (GE).
This project was organized in three main pillars: pillar I, devoted to MW-CVI technique; Pillar II, devoted to MW assisted LSI and GE; Pillar III, dedicated to Polymer Impregnation and Pyrolysis (PIP). Transversal activities (TA) such as monitoring systems, modelling, LCA and TA, risk assessment, exploitation/dissemination and management were also considered. In the following the objectives of the different Work Packages are reported.
Objectives of Work Packages (related to RTD and demonstration activities):
Objectives of WP1- MW assisted CVI (leader INSTM) (Pillar I)
The aim of this WP is the study and development of a hybrid thermal/MW assisted Chemical Vapour Infiltration (CVI) technology to achieve a reduction of about one order of magnitude in manufacturing time (20-30 hrs against 200-300 hrs) of CMCs, compared to conventional Isothermal CVI, by developing a cost-effective process route to build up the SiC matrix in 2D or 3D fibre performs.
Advanced MW heating (frequency combination) will be used to ensure the maximum EM field homogeneity inside the CVI-reactor, in order to achieve a homogeneous heating of samples of CMCs of realistic size based on carbon and silicon carbide fibers in carbon and silicon carbide matrices. A homogeneous heating will also help to reduce the processing time and permit energy saving in the CVI process.
Preforms of complex geometry will be selected for infiltration at operating temperatures between 900 and 1200°C.
Objectives of WP 2 - MW assisted LSI and GE (leader SUPSI) (Pillar II)
The specific objective of WP2 is to develop, assemble, and test a “modular” MW furnace capable for liquid silicon infiltration (LSI) and graphite expansion (GE) manufacturing. In particular the WP2 is devoted to:
• Develop a lab MW furnace for LSI;
• Develop a lab MW furnace for GE expansion;
• Optimize the MW assisted LSI process and product;
• Optimize MW assisted GE process and product.
Objectives of WP 3 - MW/RF assisted Pyrolysis (leader TECNALIA) (Pillar III)
The main objective of the WP3 is the reducing of time-cycle of the pyrolysis process for the manufacture of carbon fibre reinforced SiC and C ceramic composites (C/C and C/SiC), which are affected by high costs because of their long processing times and expensive raw materials. Therefore, it is a promising approach to develop a new process technology for the rapid pyrolysis of carbon fibre reinforced plastics (CFRP). Because of homogeneous heating, a rapid pyrolysis step can be achieved successfully using MW/RF assisted thermal treatment (conventional MW, mixed frequencies MW or RF). The porous C/C preforms can either be later infiltrated with a polymer, or subjected to additional infiltration/pyrolysis cycles until the required porosity is achieved, or siliconized to produce C/SiC composites in WP2. SiC pre-ceramic slurry systems, or SiC precursor polymers will be also considered for the infiltration step. Therefore specific aims of this WP are:
• Investigation of MW/RF assisted thermal treatment with respect to the conventional pyrolysis and PIP process.
• Investigation and evaluation of material properties.
• Proof-of-concept of MW/RF assisted thermal treatment with respect to the pyrolysis and PIP process.
Specific objectives for this task are a 10% improvement in the fracture toughness in comparison to conventional produced C/C and C/SiC. The process time will be reduced to less than 1/10 of the current process time, without shrinkage cracks, geometrical instabilities or other forms of damage due to the heat treatment. Related to the power consumption for MW assisted pyrolysis the objective is to achieve an energy saving of 25 % compared to conventional heating. In terms of cost efficiency, the final aim is to achieve a 25% reduction in production costs.
Objectives of WP4 - Development of new methodologies for high temperature MW/RF processing and process monitoring (leader CNR) (TA)
The goal of WP4 is to develop new methodologies for the homogeneous microwave and radio frequency heating of components of ceramic matrix composites, based on carbon and silicon carbide fibers in carbon and silicon carbide matrices, and for the monitoring of the growth process. In the framework of the WP, the acquisition of the information necessary to achieve this goal, mainly that related to the dielectric and thermal properties of the materials in the interval of temperatures of interest, will be carried out. The use of advanced multiphysics simulations, where the electromagnetic problem and the thermal problem are simultaneously solved, will allow a detailed modelling of the MW/RF and hybrid reactors in the working conditions.
The main objectives of the WP4 are:
• Characterization of the dielectric and thermal properties of the materials at the temperatures of the growth processes;
• Modelling and design of the MW/RF reactors and of the experiments;
• Development of a real-time measurement system of the dielectric properties of the ceramic composite part during the growth process;
• Development of a source system for a uniform MW/RF heating.
Objectives of WP 5 – Modeling and Simulation of Materials Processing (leader SUPSI) (TA)
This WP aims at implementing different modelling strategies in order to address specific aspects of the main processing methods (CVI, CVD, LSI, PIP) developed within the project. In particular, we will focus our attention on those microscale phenomena which can hardly be investigated using experimental tools, but that nonetheless yield a large influence on the final properties of the materials resulting from these processing techniques. Specifically, we intend to perform Density Functional Theory (DFT) and kinetic MonteCarlo (MC) simulations in order to study decomposition/reaction mechanisms in CVI/CVD processes, while we will employ recently developed Molecular Dynamics (MD) empirical potentials to investigate the reactive wetting phenomena taking place during LSI. In both cases, information obtained from these simulations will prove useful for a better understanding of phenomena occurring at the atomic scale during processing, and at the same time they will also serve as input data for further modelling at the mesoscopic scale. Mesoscopic modelling will be carried out by allowing for conjugate heat transfer and multicomponent gas transport in reactive porous media for CVI/CVD, whereas for LSI it will be based on the Lattice Boltzmann method. In this way, we aim at realizing a multiscale framework which can provide important insights about the underlying mechanisms controlling these processes and at the same time produce useful data for an effective calibration of process parameters. As far as PIP is concerned, due to the complexity of the decomposition reactions and to the scarcity of literature dealing with the modelling of this process, we will start from the current state of the art on this subject and intensively exploit DOE techniques of process optimization along with exploring the possibility of modelling such process using available commercial software.
Objectives of WP6 - MW-CVI process scale-up for refractory materials and aerospace (leader SKT) (Pillar I)
It was decided to design, develop and assemble a Hybrid Radiant/MW-CVI technology on a technical industrial level in order to demonstrate improvements in cost efficiency of CVI process of about 25% and reductions in energy consumption of about 25%. It is expected a cycle-time reduction to 1/10 compared to the conventional CVI process and a reduction of investment.
This task will also investigate possible improvements of homogeneity for CVI-produced CMCs like C/C , C/SiC and SiC/SiC and associated improvements in other properties like mechanical, physical or chemical behaviour. This WP will also provide information to WP12 and WP13 for the complete thermoeconomic analysis and process risk-analysis of the Hybrid Radiant/MW-CVI technology.
Objectives of WP7 - MW-LSI process scale-up for braking systems and antiballistic plate production (Leader BSCCB) (Pillar II)
WP7 aims to:
• Develop a pilot scale oven with MW or RF assisted heating for the LSI of SiCp/C and Cf reinforced carbon preform
• Optimize LSI scale process and products
• Technical assessment of CCM brake discs and SiC antiballistic plates produced by MW or EM-assisted
processing
Objectives of WP8 - MW-LSI process scale up for SiC foams production (leader ERBICOL) (PillarII)
WP8 objectives are:
- Reduce current processing time and costs. Because of higher heating rates and smaller heated mass, MW-LSI should allow a faster process and a smaller amount of energy consumption, resulting in time and energy savings.
- Improve material properties. MW-LSI allows processing at higher temperatures, up to 2000 °C, with a more uniform temperature distribution inside samples. This will led to new microstructures and enhanced material properties that will enlarge the application range of the product, actually limited to 1400°C.
- Production of volumetric pieces. Actual production technique, through convective heat transfer, limits the production of pieces with low volume. Through MW-LSI with a uniform heat distribution, the capillary diffusion of silicon is improved and the production of volumetric pieces should no more be a problem.
Objectives of WP 9 - MW assisted GE process scale-up (leader IMERYS) (Pillar II)
The aim of this WP is the up-scaling of the continuous MW assisted Graphite Expansion process. For this purpose, first a deep technical and economical evaluation of the process will be performed (T9.1) based on the results and experience acquired during WP2 and WP4. Following this evaluation a stop or go decision will be taken (MS9.1) on whether to build a demonstrator plant. The decision will also take into account the input from WP12 on life-cycle-analysis as well as from WP13 on process risk-analysis.
In the case the MW-GE process meets the requirement in term of economical efficiency and, especially, material improvement, a demonstrator plant will be designed, developed and installed (T9.2) based on the technical knowledge acquired during WP2 and WP4. All the information acquired will be then transferred to the WP12 and WP13 for completing the life-cycle-analysis as well as the process risk-analysis.
Objectives of WP 10 - MW/RF Pyrolysis process scale-up (leader AGI) (Pillar III)
The aim of this WP is to investigate the feasibility of the MW/RF-PIP technology upscale to fabricate large CMC structures for aerospace applications and of MW pyrolysis to produce preforms for LSI infiltration. To this purpose, first an in-depth technical and economical assessment of the MW/RF-PIP and MW pyrolysis will be performed, based on results of WP3 and a “Stop or Go” decision will be taken on whether to build an up-scaled MW/RF-PIP and/or MW pyrolysis equipment aiming to demonstrate the possibility of a further scale-up at industrial level of these processes. The decision will also take into consideration the input from WP12 on life-cycle-analysis and thermo-economic analysis and from WP13 on process risk-analysis.
In the case of the MW/RF-PIP technology, the implementation of this new technology will be considered successful if improvements in cost efficiency of PIP process of about 25% and reductions in energy consumption of about 25% will be achieved at up-scaled level. It is expected a cycle-time reduction to 1/10 compared to the conventional pyrolysis process. This task will also investigate possible improvements in other properties like mechanical, physical or chemical behaviour. An improvement of about 10% in fracture toughness, tensile strength and banding strength will be considered as a breakthrough in PIP technology. For MW pyrolysis technology, a pilot plant will be designed and built up to be able to process a preform of a brake disc. The implementation of the MW assisted pyrolysis for the manufacture of the brake disk is estimated to allow a reduction in thermal cycle from 48 to 12 h (with 75% time saving).
This WP will also provide information to WP12 and WP13 for the complete thermo-economic analysis and process risk-analysis of the MW/RF-PIP and/or MW pyrolysis technologies.
Objectives of WP11 - Pilot plant start-up and process validation (Demonstration) (leader INSTM) (all Pillars)
This WP collects the demonstration activities related to the WPs 6-7-8-9-10.
This WP will provide information to WP12 and WP13 for the complete LCA, LCC and TA analysis and process risk-analysis of the developed technology, to achieve a complete feasibility study, an overall comparison with the standard state-of-the art process technique and finally full assessment of the developed technologies and processes.
Objectives of WP12 - LCA and TA (Leader CIRCE) (TA)
WP12 aims to accomplish:
• The Assessment of the environmental (LCA), energy and exergy impacts, and associated costs to the new developed production processes compared to the conventional ones. Therefore the success and impact of the project can be measured and valorised.
• The provision of a diagnosis and advisory feedback over lab and demo scale developments. Therefore, potential improvements can be identified and implemented, enhancing the impact of the project.
Objectives of WP13 - Risk Assessment (leader R-TECH) (TA)
The WP addresses the following main open issues related to risks pertinent to HELM project:
• risks of "open innovation", i.e. risks of obtaining the desired result in terms of processing of ceramic matrix composites and graphite expansion under selected/given starting conditions,
• risks related to uncertainties in material characteristics (cf. ISO/IEC 17025, both the characteristics in the moment of obtaining the material and along its life cycle) and
• risks related to long-term impacts, including the both the HSE and socio-economical impacts as required by the new EU directives.
Project Results:
The scientific and technical results are discussed in this section by considering the different Work Packages, linked to the objectives of the project. The figures and tables referred in the text are reported in the annexed .pdf.
Work Package 1- MW assisted CVI (leader INSTM)
This Work package was dedicated to the design and assembly of a laboratory scale MW-CVI plant. The design activity involved INSTM, ATL, CNR, SKT, CVT and SAIREM. During the first 12 months of the project, the MW/ CVI plant has been designed and, for this purpose, some simulation tests were carried out.
The obtained results showed that, in order to obtain the necessary field uniformity, the size of the chamber of CVI should be larger than that of a laboratory scale furnace. For this reason, it was decided to go directly to the work stage of a pilot plant, expected in WP6, and this has resulted in an up-grade of the design work. The consortium decided of building the chamber in graphite, to avoid any contamination of the material produced and to use similar condition to conventional CVI equipment. Hence, on the basis of the design work described on deliverable D1.3 the assembly of the thermal/MW assisted CVI pilot plant was carried out. The preliminary testing of the plant was conducted in order to verify its functioning. The assembly work and the testing of the MW-CVI plant, built in ATL facilities (UK) was carried out on April 2014 and described in D1.4. The plant was then transferred to Pisa, where a laboratory was organized in the meantime considering all the requirements necessary for security and good working of the plant.
In the meantime ATL, SKT and CVT, on the basis of the knowledge of the state of the art about preparation of suitable preforms for CMCs, prepared and sent preforms based on Silicon Carbide (SiC) or Carbon (C ) to INSTM for allowing the scheduling of the successive infiltration trials. The different preforms shapes and properties were described in D1.5.
Hence the WP1 activity were propedeutic for the successive testing of the pilot plant and production of demonstration samples (WP6 and WP11-T11.1).
Work Package 2 - MW assisted LSI and GE (leader SUPSI)
After an extensive bibliographic research on the state of the art on MW processing, both on liquid silicon infiltration (LSI) and graphite expansion (GE), two documents (D2.1 and D2.2) were issued to give to the furnace manufacturer (FM) the requirements of the two furnaces. Furnaces were designed, manufactured and installed in collaboration with the industrial partners involved in WP2.
The LSI-MW furnace (D2.3) (Fig. 3) consists of a stainless steel vessel with a working zone of 250 mm in diameter and 150 mm in height. The double walls vessel (designed for vacuum levels up to 10-7 mbar) is water-cooled. The steel chamber is connected to four circular waveguides carrying a TM01 mode at 2.45 GHz. Each waveguide is supplied by an independent microwave generator delivering a power of 2 kV. As shown in Fig. 3, the system accounts on several sensors which are sending signals to the control rack. To improve in-plane temperature uniformity, a vertical rotation system is also installed. Angular velocities from 1 to 30 RPM can be selected. Samples’ temperature was measured from the top of the furnace (Fig. 4) with an optical pyrometer (PYROSPOT DSR 10N, DIAS Infrared, Dresden, Germany) equipped with a digital camera.
The infiltration process was carried out placing inside the furnace an original set-up represented in Fig. 5. It consisted in thin (1-2 mm) alumina cylindrical crucible (mostly transparent to MW) hosting the preform, the silicon grains and the susceptor powder bed. Rigid porous carbon felts were used to support the preform and to guide the molten silicon upon its melting. SiC/BN powder bed was uniformly distributed around the preform and the silicon to fill the empty space into the crucible. A boron nitride tube was placed as shown in Figure 3, enabling temperature measurement directly on the preform surface, otherwise covered with the SiC powder. The crucible was closed with a refractory lid of thin alumina with a central hole for the boron nitride tube.
Several pyrolysed micro porous preforms were produced and characterized to be Si-infiltrated by means of MW approach (D2.8).
The materials and the related HELM partners suppliers are here listed:
• C-SiC foams (Erbicol)
• C-SiC plates (Petroceramics)
• C-C preforms (BSCCB)
In a first step screening experiments allowed to asses MW-LSI feasibility. Later on process set-up was refined to increase products quality trough different series of experiments (Fig. 5). MW-LSI was applied successfully to ceramic foams by obtaining infiltrated parts of comparable to conventional products.
Microwave LSI of preforms embedded in powder field modifiers proved to be an effective method with respect to process time and energy consumption. The use of SiC/BN powder beds is an efficient way to convert MW power into heat while keeping temperature fairly uniform and without dispersing molten silicon upon its melting. Si-SiC (Petroceramics), composite (BSCCB) and foams (Erbicol) were successfully infiltrated in minutes (Fig. 6). The achieved product quality was assessed by each industrial partner to be almost the same as their standard industrial products.
A parallel Si-infiltration campaign by means of standard approach was carried by the University of Alicante (UA), in order to make a detailed comparison between the two techniques of infiltration.
UA studied the effect of vacuum, temperature and Si alloying in the synthesis of SiC by reactive infiltration, and compared the results with the standard products.
The design and characteristics of the MW GE (D2.4) furnace was fixed in D2.2. A schematic of the furnace is depicted in Fig. . The main components of the MW furnace are: 4x6 KW MW generators, an inclination system, a rotation system, a water cooling system, a feeder and a container for collecting the product. The MW furnace, as received from F&M, was modified by Imerys to better feed and collect the EG material.
Numerous tests were completed after some technical problems related to continuous processing were solved. More than 50 tests were performed varying the generators power, the feeder dosage, the gas flow, the inclination and the rotation. The time was kept constant for all the experiments at 1 min. After each GE reaction, the material was collected and weighed and the BET surface area and Scott apparent density were measured as control parameters of the process. A design of experiments (DOE) was used to analyse the data and to help to plan new experiments. In all cases it is observed a significant influence of the rotation and inclination parameters.
Results lead to the following conclusions:
• The maximum BET surface area values that were obtained after optimization of the parameters were in all cases ca. 45 m2/g, as compared to ca. 1 m2/g of the raw material.
• The highest BET values are obtained when either low values of inclination and rotation are used at low feeding rates, or a combination of low values of inclination and high values of rotation at higher feeding rates.
• The plots’ shape of the DOE results for the resulting BET when the generators’ power is lower than 90% is similar to the plots presented before with for instance an apparent maximum BET value of 35-40 m2/g when 50% power is used (see D2.7 for details).
• The use in practice of low values of inclination and rotation typically leads to complication in the transportation of the expanded graphite to the product container and lower productivity
The properties of the materials obtained with the MW furnace were comparable to the ones obtained with the current industrial process but still the productivity of the machine is considered as a lab-scale machine or small pilot-plant.
Some modifications to the current equipment were needed, such as a better or alternative gas transportation system, a better/alternative powder collection system and a further optimization of the process parameters, to increase the productivity and the efficiency of the process. Finally further decrease the reflected MW power is needed once the impedance matching (fine tuning of the MW generators) will be optimised.
Work Package 3 - MW/RF assisted Pyrolysis (leader TECNALIA)
The work carried out under WP3 in HELM project mainly consisted of the development of an MW/RF assisted Pyrolysis process suitable for intermediate products of the different industrial sectors of the project. In fact the intermediate samples were provided by BSCCB and PETROCERAMICS. Also final PIP products were prepared for AIRBUS GI and SCHUNK.
A programmatic approach was followed in correlation with WP10, having an up-to-date state-of-the-art and results from early stage of the project, through the workload at the refurbished lab furnace. Materials from four end users above indicated have been procured and processed: PETROCERAMICS (antiballistic protection), AIRBUS GI/SCHUNK (CMCs plates for the aerospace and energy sector) and BSCCBs (automotive brake disk).
The chosen approach for the MW/RF based pyrolysis and the design behind the up-scaled furnace is based on a full MW heating. The advantage is a maximization of the energy consumption and simplification of design, while the disadvantages are the associated high risk on design & development.
WP3, together with WP10 has been part of the Pillar 3 of HELM project. WP10 has been envisaged for the construction and validation of a pilot furnace, where WP3 has covered the research of the processes, the procurement of materials , the development of a lab scale furnace and the design of a pilot plant, which included two version: with quartz chamber and graphite chamber. Further details are given in the frame of WP10 description.
Main resources from Tecnalia in this WP3 package have been allocated on research and design activities to construct a lab furnace and complete the design of the up-scaled MW furnace. Procurement of new material batch has been carried out from BSCCB and AGI. A new material batch was delivered by SCHUNK to be processed by Tecnalia, as well as the new graphite chamber.
Moreover, further crosslink with WP1 (CVI), WP4 (MW processing and monitoring), WP5 (simulation), WP10 (pyrolysis process scale-up), WP12 (LCA-LCC) and WP13 (TRL calculation and risk analysis has been performed).
Work Package 4 - Development of new methodologies for high temperature MW/RF processing and process monitoring
The objectives and results of WP4 can be described according to the tasks composing the WP.
Task 4.1 - High-temperature dielectric characterization
Main objective: determination of the dielectric permittivity of the materials as a function of T.
Main obtained results:
- Construction of a setup capable of measurements up to 1200 °C and measurement times of about 300 ms, with high temperature uniformity over the sample;
- Development of a measurements and analysis methodology capable to extract with high accuracy the dielectric quantities from the cavity parameters, in a wide range of conditions;
- Determination of the dielectric properties of samples of interest for all the pillars (Ps) composing the project, in particular SiC fibers infiltrated by SiC for P1, α-SiC powders, Si powders, and β-SiC powders for P2, green body C/SiC and pyrolyzed C/SiC for P3.
The main task activity was conducted by CNR. FM contributed to the evaluation of the initial state-of-the-art. ATL provided samples for P1; Petroceramics, SUPSI, and BSCCB provided samples for P2; Tecnalia and AGI provided samples for P3.
Task 4.2 - High-temperature thermal properties
Main objective: determination of the thermal properties of the materials as a function of T.
Main obtained results:
- Definition of suited measurement setups and procedures;
- Determination of thermal conductivity, heat capacity, and linear expansion coefficient of samples of interest for all the pillars composing the project, in particular SiC/SiC and C/SiC for P1, C/SiC and Si-SiC for P2, and C/SiC for P3.
The main task activity was conducted by Petroceramics. ATL provided samples for P1, Petroceramic and BSCCB provided samples for P2, and AGI provided samples for P3.
Task 4.3 - Multiphysics simulation and design of experiments
Main objective: numerical simulation of the interrelated electromagnetic and thermal distributions in microwave reactors in operational conditions.
Main obtained results:
- Setup of suited simulation strategies for the investigation of reactor loaded by static and rotating samples, heated by means of a single port or multiport microwave excitation;
- Determination of the electromagnetic field and temperature distributions in the reactor and sample as a function of time;
- Analysis of the temperature uniformity in the sample volume. Optimization of the temperature uniformity by means of a combination of sample rotation and multiport microwave excitation.
The main task activity was conducted by CNR. Data from T4.1 T4.2 and T4.4 were employed.
Task 4.4 - Development of a source system for a uniform MW heating
Main objective: design of the microwave parts of the pilot-scale hybrid radiant/MW CVI reactor
Main obtained results:
- Definition of the most suited design approach, based on a closed oversized resonant structure;
- Design of the microwave reactor chamber, including a sample holder, a movable plate for the frequency tuning, and rotating waveguides for a continuous control over the MW polarization;
- Analysis of the most suited MW polarization as a function of the sample dielectric properties.
The main task activity was conducted by CNR. Sairem contributed to the design of the microwave excitation channels. INSTM contributed to the conceptual development.
Task 4.5 - Development of a Real-Time Monitoring System
Main objective: design and construction of a system for the real-time and in situ monitoring of the sample processing
Main obtained results:
- Construction and implementation of the system in the pilot-scale hybrid radiant/MW CVI reactor;
- Test and setup of the real-time monitoring system.
The main task activity was conducted by CNR. INSTM contributed to the conceptual development and to the test and setup of the system.
Work Package 5 – Modeling and Simulation of Materials Processing (SUPSI)
Task 5.1.1 – CVI/CVD Modeling – Atomistic Simulations. Objective: simulating decomposition and reaction mechanisms in CVI, in order to improve synthesis protocols. Results: (i) a reactive force field for describing the chemistry of MTS decomposition under hydrogen; (ii) the kinetic parameters of reaction mechanisms and successive reaction of the thus produced radical species with a growing SiC surface; (iii) an integrated computational protocol to simulate SiC CVI growth under steady-state conditions, in which DFT- and MD-based atomistic mechanisms are combined with statistical (kinetic Monte Carlo, kMC) sampling; (iv) a simulation of the long time scales relevant to experimental growth and prediction of growth rates as a function of environmental variables (temperature and reactant pressures)
Task 5.1.2 – CVI/CVD Modeling – Mesoscopic Modeling. Objective: finding process conditions which combine material performance with minimal infiltration time using simulation. Results: (i) a numerical algorithm and software package for 2D simulations allowing study of MW assisted CVI processes, allowing analysis of the flow pattern, thermal field and distributions of species concentrations in the gas region of the reactor and in the porous preform and evaluation of degree of densification; (ii) a parametric study of different modifications of CVI processes (including Isothermal, Thermal Gradient and Forced Flow CVI processes); (iii) a study of the temperature distribution in a MW CVI reactor and particularly in the bulk of the preform for different values of heating power of both MW and conventional heaters; all major mechanisms of heat transfer were considered: conductive, convective and radiative; (iv) a numerical study of flow pattern, thermal field and distributions of species concentrations in the gas region of the reactor and in the porous perform and evolution in time of the structure of the preform porous medium in the long-term MW assisted CVI process; (v) a numerical study of the long-term MW assisted CVI process for the final design of the plant with porous sample holder and a parametric study of effect of process parameters
Task 5.2.1 – LSI Modeling – Atomistic Simulations. Objective: evaluating different MD potentials with respect to their ability of describing reactive wetting phenomena in LSI. Results: (i) a study of the performance of different forcefields (ReaxFF, Tersoff, S-W) for the simulation of silicon melting using the Z-method; (ii) a MD protocol for the simulation of silicon droplets on different substrates (graphite, amorphous carbon, silicon carbide) and using different software (LAMMPS, MDCASK) and forcefields (Tersoff, ReaxFF)
Task 5.2.2 – LSI Modeling – Mesoscale Modeling. Objective: provide information on fundamental parameters controlling reactive infiltration by developing a LB code. Results: (i) a LB code for 2D simulations of capillary infiltration of structured channels and packing structures, including surface growth phenomena; (ii) a GPU implementation of the code, allowing a statistically accurate description of reaction wetting phenomena during silicon infiltration of carbon preforms; (iii) a parametric study of the influence of different factors in the infiltration process of channels (pore size and shape, liquid silicon velocity, growth rate); (iv) a direct comparison to experimental results obtained in the infiltration of mm-sized channels; (v) a parametric study of reactive wetting and infiltration of different packing structures (variable particle size and shape distributions) during LSI, allowing for the identification of factors and phenomena which determine the quality of the infiltration and the resulting material (e.g. porosity)
Task 5.3.1 – PIP Simulations – State of the Art of PIP Simulation. Objective: conducting a review on the state of the art methods for atomistic and mesoscopic simulation of PIP. Results: (i) a state of the art of available modeling and simulation methods for the study of the PIP process.
Task 5.3.2 – PIP Simulations – DOE for PIP Simulations. Objective: finding process conditions which combine material performance with minimal infiltration time. Results: (i) a screening of factors affecting the PIP process; (ii) the identification of the optimal process conditions (heating ramp duration, intermediate temperature) for MOR and weight loss; (iii) a factorial design for the analysis of the current experimental furnace obtaining a reduction of the time-cycle and the best mechanical performances of the material.
Work Package 6 - MW-CVI process scale-up for refractory materials and aerospace (leader SKT)
It was decided to design, develop and assemble a Hybrid Radiant/MW-CVI technology on a technical industrial level within WP 6. The main objective within this task was the set-up and test of a pilot Hybrid Radiant/MW-CVI plant at INSTM in Pisa (Subtask 6.2). This objective could completely be fulfilled. The set up of the plant was particularly complex for logistic reasons (installation of the necessary safety equipment) and technical reasons. The MW-CVI pilot plant was equipped with safety devices to take into account the different risks, such as explosion risks.
During test operations at high temperature the breakage of quartz windows occurred. The damages were caused by the decomposition of o-rings at high temperature and successive overheating. Hence many modifications to the plant were made in order to avoid this issue, introducing a cooling system, a Magic T system, reducing the wall thickness of graphite waveguide, adding graphite foil rings at end of graphite waveguide, using larger windows, changing the O-ring material, inserting a double quartz window and introducing a flow meter.
Conditions for SiC deposition were thus selected and the obtained deposited material was characterized. The deposited material is SiC, probably containing carbon. This testing and optimization activities related to the MW-CVI plant were described in D6.2.
After the set up of conditions it was possible to make a program of infiltrations aimed at assessing the working of the plant and its efficiency in different systems. A SiC preform, a C preinfiltrated preform and a preform consisting in knitted SiC Nicalon fabrics were the systems investigated. Several successive infiltrations were made on each system by varying processing parameters, such as pressure and gases flows. A systematic approach allowed the storage of all the information related to trials: (1) mass and parameters information; (2) Temperature profile along the trial; (3) pH profile in the scrubber; (4) Chamber temperature profile. The data of infiltration rate and also the data of efficiency were investigated in order to correlate with processing parameters. The shape and chemical composition of the preform influenced the infiltration rate. The characterization of materials allowed evidencing that the main compounds present in the composites matrix is SiC. However also some presence of minor components such as silica or nitrides was evidenced.
Some important limits must be overcome: the inhomogeneity of the infiltration (due to the inhomogeneity in heating), that can be overcome by proper rotation, and the deposition of powders in the graphite chambers or also in the furnace chamber resulting in quartz window periodical darkening to microwaves.
The MW-CVI plant can be used by INSTM for future activities and further parameter optimizations. Some problems could be already solved during installation like optimization of wave guides, cooling of flanges and improved optical ports. A preliminary technical and economical assessment of the Hybrid Radiant MW-CVI technology was thus possible. There exists still some open problems in order to enable a complete densification via MW/CVI technique. One open problem is the formation of dust. This dust formation results in a limitation of the maximum infiltration time of approximately 3 h in total. Further improvements of the quartz glass windows are necessary. The windows have to be modified by using a purge gas to avoid dust deposition on the windows. Furthermore, the sample holder has to be equipped with a rotation system in order to improve the homogeneity of the MW assisted CVI process.
The WP 6 enabled SKT to develop an isothermal CVI-SiC densification technique for high performance composites. In past SKT applied the CVI process only for mixed matrix systems or with a lower degree of densification for thermal insulation parts. The progress made in WP6 have shown further potentials for CVI optimizations at SKT, which will be used in future. Furthermore, CVT has improved their own rapid CVI-SiC densification method by optimization steps within WP 6. These two techniques were used for producing samples for comparative analysis. The processing data as well as their characteristics were described in D6.1.
Therefore, the objective of the optimization of the MW-CVI pilot plant is in a good progress, but not yet completed. This subtask (6.3) is an ongoing work, which will be continued by INSTM after the project. One open issue is the observed formation of impurities in the MW-CVI based SiC-matrix. The CVI matrix contained Silica as well as Silicon Nitrides. The reason for these impurities are not yet fully known and will be investigated after the project.
A second issue was the limitation in CVI densification due to the above mentioned dust formation. This incomplete densification as well as these impurities of the matrix did not allow to compare the mechanical, physical and microstructural properties of the MW-CVI based materials with conventional isothermal CVI densified samples.
Nevertheless, it could be demonstrated within WP 6 as well as WP 11 that the targets of energy efficiency of 25 % and expected cycle time reduction to 20% in comparison to isothermal CVI densifications seem to be feasible.
Work Package 7- MW-LSI process scale-up for braking systems and antiballistic plate production (Leader BSCCB)
In the frame of WP7, the task 7.1 was devoted to the technical evaluation of MW-LSI process to obtain braking systems (BSCCB) and antiballistic plates (Petroceramics).
The tested materials (Si-SiC samples for antiballistic and carbon ceramic samples for braking rotors purposes) have been made on small scale in WP2.
Petroceramics Si-SiC analysis
The lab scaled SiC plates Si-infiltrated by means of MW showed diffused small pores and local defects for every experimental setup and processing conditions. Anyway large areas of the samples were well infiltrated. The material well infiltrated has comparable values of flexural strength than the standard one, and the values of Young modulus are in line with the target for both well infiltrated and porous material.
BSCCB carbon ceramic analysis
Only small samples of carbon ceramic composite were made in the frame of WP2, not big enough to obtain specimens suitable to perform mechanical tests. As a consequence the material has been evaluated only in terms of the chemical-physical properties. The best thermal ramps and setups of LSI driven by means of MW entailed a carbon ceramic materials in line with the targets in terms of density, silicon uptake and microstructure.
Outcomes
LSI by means of MW approach seems a suitable way both for Si-SiC antiballistic plates and carbon ceramic brake rotors; on the basis of these evidences the scaled-up furnace building has been pursued.
In Task 7.2 Petroceramics designed and built a MW oven with a cavity able to Si-Infiltrate full scaled antiballistic plates and carbon ceramic rotors. The assembly was successfully completed and the functionality test of the components concluded. Operating at atmospheric pressure no plasma was observed at P=100%. On the basis of these evidences the experimental activity was perfomed and drove to the results reported in WP11 task 11.2.
Work Package 8 - MW-LSI process scale up for SiC foams production (leader ERBICOL)
During work package 8 a technical and economical assessment of the MW-LSI process for SiC foams was performed (task 8.1) and a pilot scale MW-furnace was designed and constructed. The work package was following WP2 where the concepts were performed at a laboratory scale and provided the input for the assessment.
The technical and economic evaluation of the MW-LSI process for SiC foams was performed in order to compare the conventional induction based process with the newly developed MW-LSI and understand if a pilot scale furnace was valuable both technically and economically. Following conclusions were drawn from the analysis:
- The process is much faster than conventional LSI, expected to be 50% faster at a pilot scale;
- The faster processing cycle increases equipment throughput, which means for a comparable investment the payback period is faster.
- Lower mass heated is the main performance advantage compare to induction heating;
- At full capacity, an overall cost saving of 20% can be expected;
- Product properties are lower than state of the art, but acceptable for non-structural applications.
Following the techno-economical evaluation of task 8.1 and the outcomes of lab-scale work package 2 for the liquid silicon infiltration of SiC foams, a pilot-scale MW-furnace of 30 L volume has been designed and built. Compared to the lab-scale furnace, the upscaling was done with more standard materials and power sources to keep costs competitive to conventional heating, and particular attention has been dedicated to the magnetron positioning to achieve an homogeneous field distribution inside the chamber. As a summary, following has been achieved:
- Modular design of the pilot-scale furnace (semi-continuous)
- Design of the cavity with asymmetric magnetron distribution to avoid high field heterogeneity
- Construction and assembly of the pilot scale MW-furnace for LSI of SiC foams
- Successful test runs up to a temperature of 1600°C in inert atmosphere
The assembled and tested furnace represents the successful end of work package 8 and the starting point for the test cycles and performance analysis of work package 11.
Work Package 9 - MW assisted GE process scale-up (leader IMERYS)
The aim of this WP was the up-scaling of the continuous MW assisted Graphite Expansion (GE) process. First a technical and economical evaluation of the process was performed based on the results and experience acquired during WP2 to decide whether to build a demonstrator plant or not.
Various parts of the initial set-up needed to be modified in order to make it run continuously and without leakages. In this context, the reactor tube rotation system was optimized and new O-rings were used at the inlet and the outlet for improving gas tightness. Different reaction parameters such as generators’ power, feeding, inclination, rotation and gas flow were modified to find optimum parameters to increase the surface area of the final product and decreasing the apparent density without blocking the reactor tube. During these tasks interactions with mainly SUPSI and F&M were essential to achieve the goals.
After all these optimizations, an economical evaluation of the process was performed taking into account a reaction using optimized parameters. The GE process by MW would need at this point of the project ca. 3 times more energy and it would cost ca. 5 times more than the industrial process. The properties of the materials obtained with the MW furnace are comparable to the ones obtained with the current industrial process but still the productivity of the machine is considered as a lab-scale machine or small pilot-plant.
It was decided not to construct a new industrial-scale pilot oven, but to modify/optimize the existing lab-scale machine to build a small lab-pilot furnace. In this context, the outlet of the equipment was modified in order to improve the material and gas transportation and product collection. A new filter-cyclone apparatus was installed using a plastic bag of container to collect the expanded graphite product. Moreover, two gas entrances were installed at the outlet to control the gas supply together with a suction valve to facilitate the transportation of the expanded graphite from the MW furnace to the filter/cyclone.
The previous design of the MW furnace for GE has been modified to make a lab/pilot scale MW equipment with increased EG productivity. The performance of the optimized lab-pilot MW furnace is a compromise between the properties and the productivity desired. The MW expanded graphite shows comparable electrical properties in a composite material as the industrially produced one with only slight differences depending on the treatment applied. A productivity of ca. 8kg/h with optimal material properties has been achieved at this point of the project. The process was be validated with focus on energy and cost reduction in order to be competitive with the industrial process (WP11).
Work Package 10 - MW/RF Pyrolysis process scale-up (leader AGI)
The objective of WP 10 was to investigate the feasibility of the MW/RF-PIP technology upscale to fabricate large CMC structures for aerospace applications and of MW pyrolysis to produce preforms for LSI infiltration. For this purpose, first an in-depth technical and economical assessment of the MW/RF-PIP and MW pyrolysis, based on results of WP3, was performed (Subtask 10.1). After a Go decision, up-scaled MW/RF-PIP and/or MW pyrolysis equipment aiming to demonstrate the possibility of a further scale-up at industrial level of these processes had to be build-up (Subtask 10.2 and 10.3).
The new technologies are considered successful if improvements in cost efficiency of about 25% and reductions in energy consumption of about 25% are achieved at up-scaled level. A cycle-time reduction to 1/10 compared to the conventional pyrolysis process was expected. The chosen approach for the MW/RF based pyrolysis was based on a full MW heating. The advantage is a maximization of the energy consumption and simplification of design, while the disadvantages are the associated high risk on design & development. A programmatic approach was followed, having results from early stage of the project, through the workload at the refurbished lab furnace. Materials from 4 end-users were processed: for Petroceramics materials excellent results were achieved at the lab furnace with quartz chamber (1 tile for each test). The set-up of the graphite chamber enables to process at least 4 tiles. It was possible to reach 600ºC within 2h without any oxidation signal. These tests enabled to validate the design of the graphite chamber. For AGI and SKT materials no arching was detected, as the MW field was designed to be perpendicular to fiber architectures. It was able to process large samples of about 300 x 300 mm2. However, the high ceramization temperature of e.g. 1600°C for PIP could not be reached due to some unsolved open problems (max. reached temperature was 600°C only). Hence, a complete ceramization process via MW/RF-PIP technology could not be performed within the project by Tecnalia, therefore there is still need of better MW adaptation in the near future.
BSCCB materials have been processed in a step-wise approach: at lab with no chamber, at lab with quartz chamber, up-scaled with quartz chamber and up-scaled with graphite chamber which was manufactured and delivered by SKT for the up-scaled MW/RF-PIP pilot plant according the design of Tecnalia. Two tests of pyrolysis with the up-scaled MW furnace have been performed on full scaled brake rotors. Due to issues related to the new equipment (too high temperature recorded on some equipment components), the tests were stopped at temperatures lower to the target one (that is over 600°C). The best trial entailed a weight loss of 16,7%, too low than expected (20wt%) but good enough to liquid silicon infiltrate the so pyrolyzed rotor by means of standard way. At present the reliability at full scale level was not completely tested but the good results fulfilled working at small scale seem to show that the MW approach seems promising also to pyrolyze a full rotor. Due to the lack of full rotors pyrolyzed by means of MW, not still available, at present it is not possible to make a reliable estimation of the costs and the energy consumption of the MW assisted pyrolysis. It can be highlighted that an up-scaled furnace was designed, constructed and validated, but there is still room for significant improvements, such as the optimization of the efficiency on BSCCB full rotors (max. pyrolysis temperature), better temperature homogeneity and integration of the second frequency 5.8 GHz to reach ceramization temperatures for the PIP technology.
Therefore it can be concluded, that the objective of the optimization of the pilot plant is in a good progress, but not yet completed. This subtask is an ongoing work, which will be continued by Tecnalia after the project. Main open issue is to reach the high ceramization temperature for the PIP technology which was not yet achieved. Consequently, it was not possible to compare the mechanical, physical and microstructural properties of the MW-PIP based materials with conventional PIP material samples. This target of WP 10 as well as WP 11 (subtask 11.5) could not be fulfilled within the project time. Tecnalia will work on this after the official project time. Nevertheless, it could be demonstrated within WP 10 as well as WP 11 that the target of expected cycle time reduction down to 1/10 in comparison to conventional processing seems to be feasible. A complete technical and economical evaluation of the MW/RF-Pyrolysis and PIP technology with conventional ones is only feasible, if all open issues are solved. All material data of the conventional processed material samples are available for comparison. Finally, it can be stated, that in WP10 there was an excellent collaboration and interaction among the involved partners.
Work Package 11 - Pilot plant start-up and process validation (Demonstration) (leader INSTM)
This WP collects the demonstration activities related to the WPs 6-7-8-9-10. The results are here summarized by considering the five different tasks of this WP.
Task 11.1 Hybrid radiant MW-CVI (task leader SKT)
Task 11.1 was aimed to compare the hybrid Radiant MW-CVI technology developed in the project with the more traditional CVI technologies. Because only a reduced number of experiments with a duration lower than three hours was possible by the new MW-CVI plant, a work of modelling was carried out to make a prediction about the potential reduction of processing time achievable by this new technique. All the predictions showed a remarkable reduction of processing time. Moreover, four infiltration trials were conducted in the same condition of CVT partner and on the same preforms provided by CVT on C based preforms preinfiltrated with SiC. The time of processing necessary for obtaining an increase in density from 0,71 to 0,91 g/cm3 was 15 hours by Rapid CVI and only 5,2 hours by MW-CVI. Hence, a reduction of time at one third of its value was achieved. Considering that the plant working was still not optimized (as described in D 6.3) and the system examined was the most difficult to process, because C-preforms do not heat easily through MWs, this result seems quite promising. Further optimization of the plant is necessary for a more definite assessment of the new technique.
Task 11.2 MW-LSI for braking system and anti-ballistic plates- pilot plant start-up and process validation (task leader BSCCB)
In this task the MW-LSI pilot scale furnace was set up for industrial production of anti-abllistic plates and 5 different setup configurations were tested to optimize materials heating. In the case of antibalistic plates prototypes production for demonstration 10 total runs of production for three different products were carried out. Mechanical properties of torso plate of some samples resulted comparable to those of well densified samples by standard heating process. In single shot test on some samples of torso plates the bullet was retained with a reduced trauma of baking layer. The analysis of the morphology showed that the properties of the MW-LSI plate was similar to the ones observed for conventional LSI, but some residual porosity could be noticed in the former. The total energy saving was 13% and time saving is also achieved.
For the production of demonstration prototypes of brake disks seven total MW_LSI runs for 1one disk size were carried out. The mechanical properties of four disks resulted close to the target but the porosity is higher than standard product and the thermal conductivity is far from the specification (<30-40%). For the production of brakes some optimization are still necessary to reduce the properties gap between the conventional and MW-LSI disks.
Task 11.3 MW-LSI for SiC foam- Pilot plant start-up and process validation (task leader ERBICOL)
The pilot MW-LSI furnace has been operated to validate process and equipment and compare it to the currently used induction furnace. Several demo samples has been produced and the furnace operations didn’t produce any serious problems or failures. Through the operation of the furnace, it was possible to demonstrate the compatibility of MW-LSI with SiSiC foam manufacturing, and collect process data to rank the MW-LSI furnace against the conventional one.
Total process energy savings of 38% have been achieved with MW-LSI, and an equipment productivity increase of 50% has been measured. Provided the MW-LSI equipment is 30% more expensive, a total 20% cost saving can be expected.
Hence, during the demo WP11.3 the furnace was successfully operated without major failures. The infiltration of SiC/C preforms was possible in a faster timeframe and delivering satisfying product properties. Summarizing, following conclusions can be drawn:
- The MW-LSI process is suitable for SiSiC foam processing and is faster than conventional LSI;
- The infiltration quality dependence on samples geometry has been overcome;
- Fully loaded MW-LSI furnaces have been processed delivering repeatable results and consistent product quality;
- The product properties of MW-LSI processed products are not as good as standard processed products, but the economic advantages of MW-LSI make the process a viable solution for a faster and cheaper liquid silicon infiltrations
Task 11.4 MW plant for GE production – pilot plant start-up and process validation (task leader IMERYS)
Several demonstration samples have been produced after modifying the equipment to be able to work at increased capacity. However, it was observed that the properties of the materials decrease when working at higher capacity. Therefore, as explained in D11.8 there are two possible scenarios that can be considered depending on the production capacity/energy/cost balance and the material properties.
The scale of the current plant is in fact too much small for achieving a good exploitation of the process developed in the HELM project for GE expansion based on MW. A scale-up machine based on the design used in HELM would probably help in optimizing the process/material properties and increase the production capacity. This possibility will be evaluated in the future.
The GE by the MW furnace build in the HELM project has shown, on a technical point of view, its potential to expand graphite in a way comparable to the industrial process. After optimization of the reaction parameters and accepting a compromise in the materials properties, a potential reduction in energy saving and production costs would be achievable. Final compatibility tests of the EG as filler in polymers and acceptance by clients would determine the potential of the process. Further increase of energy and cost saving could be realized with the scale-up of the process.
Task 11.5 MW-RF-PIP Pilot plant start-up and process validation (task leader SKT)
Several activities, trials and characterization performed at the pyrolysis and PIP up-scale equipment including a graphite chamber towards the development of a MW based PIP process. The technology has not been fully demonstrated at the up-scaled furnace. Nevertheless with the support of SUPSI (project partner) the technology has been demonstrated (in two separate steps) and a partial comparison of the technology has been feasible.
As a main conclusion, the MW/RF-PIP technology is quite promising for ~90% process time savings of std process (heating phase, excl. cooling down phase).
Work Package 12 - LCA and TA (Leader CIRCE)
A Life Cycle Analysis (LCA) can give very valuable information to assess the goodness of a solution with respect to different environmental categories. The reference impact categories chosen to refer the life cycle impact are carbon footprint in kg CO2-eq/kg and €/kg for the LCC. The main recommendations given for future improvements in the furnaces and processes using those furnaces, from an environmental and thermo-economic point of view, are summarized here below:
MW Furnaces.
1. The environmental impact of the furnace in the total process environmental impact is relatively small. The impact of the new equipment is usually higher as most of the components are made up of metallic parts with low batch manufacturing techniques. Furthermore, these furnaces are not fully optimized since the main purpose in the project is to prove feasibility.
2. For the final version of the MW industrial demonstrators, the absolute carbon footprint impact for the manufacturing of 1 unit of furnace, the relative allocation of this impact to each kg of material treated by the equipment (no energy included) and the LCC per kg (energy included) is represented in the table 1.
Processes
The results of Carbon footprint at every stage of the project for every pillar starting from the conventional process, then the lab scale testing, then the scale up testing, and finalizing with the improvement scenarios, are shown in the table 2.
With the exception of GE and CVI, all process show an improvement in carbon footprint when run with the new MW scale up furnaces in comparison with the conventional processes. The difference in GE is not very significant and in CVI, it could be cancelled out with a lower consumption of the MTS gas. These improvements could be part of further research. In all cases except GE, the efficiency in energy usage is much higher with the MW processes.
Besides the life cycle studies, exergy balances and thermoeconomic analyses were performed in order to assess the efficiency of the new technology from this novel approach. Although it is known that relevant energy savings are achieved with the new heating method (because the processing time is reduced), it is important to quantify this reduction and detect in which parts the processes have potentials of improvement.
Results showed that most of these conventional processes have low energy and exergy efficiency. A big amount of exergy is destroyed into the furnace systems and besides, there are large exergy losses in the by-products streams that could be recovered.
The new MW-systems were able to improve the conventional results for all processes from a thermoeconomic viewpoint (table below). Using the new heating mode, exergy yield has increased for all processes, especially in the most energy demanding processes, CVI and LSI. On the other hand, both the unit exergy consumption and the unit exergy cost have also improved for the five processes, and therefore, one of the main goals of the project has been successfully achieved. It must be taken into account that these MW-results were obtained from processes that they are not still completely optimized, and therefore, it is expected they will keep improving as the new systems are optimized.
Work Package 13 - Risk Assessment (leader R-TECH)
The work carried out by R-Tech represents an approach for appraisal of R&D technological and non-technological risks from an “open innovation” perspective. The approach developed is described as the ORnAMENT framework.
The ORnAMENT framework addresses the technological risks which are derived from the material and process characterization activities, OSHA and HSE identified risks. ORnAMENT framework is integrates a TRL calculator and tackle different issues identified and discussed in D13.1 by systematic method for risk comparison on the basis of quantitative scores. The framework represents an effective means to support r decisions concerned with investments in certain R&D efforts to reduce uncertainties in technological performance, avoid deviations from the project schedule or budget, and encourage technology exploitation.
The ORnAMENT methodology/tool developed afterwards was applied to the six HELM R&D efforts: 1) Chemical Vapour Infiltration; 2) Liquid Silicon Infiltration; 3) Graphite Exfoliation; 4) Pyrolysis for LSI; 5) Pyrolysis for ceramization of SiC/SiC; 6) Pyrolysis for ceramization of Cf/SiC. The risk of failure of each of them was calculated as function of the risk of failure to reach the required level of technological readiness and the sum of technology-specific risks potentially emerging from each R&D effort. These technological risks were integrated with non-technological (e.g. partnership, market, legal and regulatory) risks related to project management, external factors and the market into the HELM overall risk of failure. Preliminary results on the application of the ORnAMENT tool to the pillars of the project are detailed in the D13.6.
In order to collect information on the maturity of the HELM technologies and the probability and consequence of their risks, a survey was distributed to a group of 15 experts selected from the HELM Consortium, including the Coordinator, the Project Manager, Leaders of the technology pillars, the main contributing partners and the potential end-users of the developed technologies. The responses to this survey were complemented with information obtained by R-Tech from an analysis of the project deliverables and were used as inputs to the ORnAMENT methodology/tool, which was applied to assess the HELM R&D&I risks in months 24 (See D13.3 D13.4) and 47 (See D13.5 D13.6) of the project.
ORnAMENT proved to be a robust risk analysis tool, able to transparently provide adequate information for risk management decision making. Nevertheless, there is room for improving it. In order to achieve a more comprehensive appraisal of R&D project risks we recommend that the future version of the tool includes criteria and models to directly assess whether the project meets its schedule, cost, and performance success criteria, something that is only indirectly addressed by the current version of the tool.
GENERAL REMARKS ABOUT SCIENTIFIC AND TECHNICAL RESULTS OF THE HELM PROJECT
HELM project allowed demonstrating the feasibility of several processes for producing CMCs.
The Three pillars of the project (I-CVI, II-LSI and GE, III-PIP) corresponded to the most important industrial techniques actually used in industry to prepare CMCs and they were innovated thanks to the introduction of MW or RF.
The figure 11 shows the three different technical pillars related with the final applications considered in the project
First macro-result: a network of new innovative plants for CMCs production in Europe
The main objective of the HELM project was developing alternative techniques to produce CMCs by using microwaves and radio frequencies in order to reduce time and costs related to the processing of these materials. In this field, as described in the state of the art of the HELM proposal, new research was necessary as not many progresses were achieved in the last decades, despite of the enormous interests for these materials because their advanced performances and durability.
As reported in table 4, the project allowed in the first part the building of a totally new laboratory plant for MW-LSI, whereas laboratory scale tests were performed in refurbished existing plant for GE and PIP. Thanks to the design related to simulation and modelling it was possible to avoid the building of a laboratory scale plant for MW-CVI plant, skipping to the pilot phase. In the first phase of the project, carried out at a laboratory scale, three plants were thus used.
The further step was the building of pilot scale plants and this phase allowed the building of 4 new plants: one for MW-CVI infiltration of C and SiC preforms, one for Liquid silicon infiltration of brake and antiballistic plates, one for production of SiC foams and one for polymer infiltration and pyrolysis.
The building of the plants resulted a complex work because of technical difficulties, mainly due to plasma formation in the extreme conditions of the treatments, not easily predictable in some cases by the thorough work of simulation and modelling performed during the project (WP5).
Two of the new pilot plants were built in Italy, one in Spain and one in Switzerland, involving UK, Spain and Germany equipment producers involved in the project. This aspect evidences the European dimension of the developed network.
Many innovations were introduced in the plants and they were necessary for coupling the MW or RF techniques by the conventional techniques. Thanks to the collaboration among the consortium partners, ideas about design and used materials were shared in the consortium, thus boosting an easy application. The interdisciplinary feature of the consortium, involving experts of physics, chemistry, engineering and material science, and the use of the transversal activities, such as monitoring (WP4), modelling (WP5), LCA/LCC analysis (WP12) and risk analysis (WP13), resulted essential for reaching so many objectives in the project.
Second macro-result: new CMCs products based on the new MW-LSI technologies
The applications in the field of antiballistic plates and SiSiC foams were those in which a higher TRL, of at least 5, was achieved.
In particular mechanical properties of torso plate of some samples resulted comparable to those of well densified samples by standard heating process. In single shot test on some samples of torso plates the bullet was retained with a reduced trauma of back layer. The analysis of the morphology showed that the properties of the MW-LSI plate was similar to the ones observed for conventional LSI, but some residual porosity could be noticed in the former. The total energy saving was 13% and time saving is also achieved.
Moreover, it was possible to demonstrate the compatibility of MW-LSI with SiSiC foam manufacturing. In particular, the following conclusions can be drawn:
- The MW-LSI process is suitable for SiSiC foam processing and is faster than conventional LSI;
- The infiltration quality dependence on samples geometry has been overcome;
- Fully loaded MW-LSI furnaces have been processed delivering repeatable results and consistent product quality;
- The product properties of MW-LSI processed products are not as good as standard processed products, but the economic advantages of MW-LSI make the process a viable solution for a faster and cheaper liquid silicon infiltrations.
Demonstration prototypes of brake disks were also produced. The mechanical properties of four disks resulted close to the target but the porosity is higher than standard product and the thermal conductivity is far from the specification (<30-40%). For the production of brakes some optimization are still necessary to reduce the properties gap between the conventional and MW-LSI disks.
Third macro-result: new industry oriented knowledge in the production of CMCs
In all the pillars important knowledge results were achieved. The assistance of the monitoring techniques (WP4) applied to the different plants was fundamental for developing a knowledge about the processes.
In the MW-CVI process the use of a graphite furnace was demonstrated to be successful. The occurring of arching and plasma was demonstrated to be an issue during infiltration. Hence the conditions for infiltration must be found in pressure ranges where plasma formaton is suppressed and a peculiar configuration for sample holder is necessary for avoiding arching.
The resistance of materials employed in plants building to the high temperature generated by MW was found to be important and the necessity of cooling the coupling system (flanges) connecting the MW waveguides with the furnace was fundamental.
In the MW-LSI process the use of SiC powder susceptor for enhancing MW heating was found to be important and this result was the object of a publication. The results achieved at a laboratory scale were promising and the following scaling up into the two pilot plants of Pillar II allowed including peculiar design of magnetrons distribution keeping into account the preliminary results achieved in the laboratory plant.
In the MW/RF based pyrolysis Pillar the design behind the up-scaled furnace is based on a full MW heating keeping into account the results achieved in laboratory trials and with the aim of increasing the homogeneity of the magnetic field thanks to the peculiar waveguides distribution. The advantage is a maximization of the energy consumption and simplification of design, while the disadvantages are the associated high risk on design & development.
Dissemination activities (in particular related to scientific papers) indicate the achievement of excellent results during the project activities period. As the interdisciplinary approach typical of HELM project, being a pioneering one, is usually slow in giving a fast scientific production in terms of publications number, it can be reasonably predicted that the scientific advance of this project will be spread much also in the next years’ scientific publications about CMCs production and it will give further knowledge in the advanced ceramic materials sector. This knowledge is both of high scientific relevance and easily upheld by the market, as directly involving researchers of academy and companies.
Open issues and opportunities
Some still open issues were evidenced in the HELM project.
The objective of the optimization of the MW-CVI pilot plant is in a good progress, but not yet completed. This work will be continued by INSTM after the project. One open issue is the observed formation of impurities in the MW-CVI based SiC-matrix. The CVI matrix contained Silica as well as Silicon Nitrides. The reason for these impurities are not yet fully understood. A second issue was the limitation in CVI densification due to the dust formation on quartz windows, making impossible the realization of an infiltration longer than 3 hours up to now. This incomplete densification as well as these impurities of the matrix did not allow up to now to compare the mechanical, physical and microstructural properties of the MW-CVI based materials with conventional isothermal CVI densified samples.
The interests of HELM partners and stakeholders present at the final workshop can be addressed to a further optimization work in collaboration with INSTM and CNR, hosting the MW-CVI plant in Pisa.
In the case of MW-PIP it can be highlighted that an up-scaled furnace was designed, constructed and validated, but there is still room for significant improvements, such as the optimization of maximum pyrolysis temperature, better temperature homogeneity and integration of a second frequency to reach ceramization temperatures for the PIP technology. Therefore, the objective of the optimization of the pilot MW-PIP plant is in a good progress, but not yet completed. This subtask is an ongoing work, which will be continued by TECNALIA after the project. Main open issue is to reach the high ceramization temperature for the PIP technology which was not yet achieved. Consequently, it was not possible to compare the mechanical, physical and microstructural properties of the MW-PIP based materials with conventional PIP material samples.
Potential Impact:
POTENTIAL IMPACT
Ceramic Matrix Composites (CMCs) occupy a fundamental position in the transport sector (e.g. for elements of combustion engines of aircrafts, valve-trains, turbine blades, exhaust systems, cars braking systems) and energy sector (e.g. refractory materials for silicon foundry furnaces, energy reactors, gas burners and high pressure heat exchangers).
Regarding the technical impacts of the project, as explained in the “General remarks about Scientific and technical results of the HELM project”, interesting results were achieved in two products, both developed by the MW-LSI technique. In all the cases materials with lower properties than the conventional counterpart were obtained and this can be attributed also to the not complete optimization of the new techniques. However, in the production of antiballistic plates and SiSiC foams the MW-LSI technique was demonstrated to result in CMCs with properties similar to conventional counterparts, thus allowing predicting a fast impact on the market of these new technologies. The production of CMCs by the other techniques is also promising, but some more research is required for achieving the complete fulfilments of mechanical requirements of the developed materials.
Regarding the impacts on industrial manufacturing the building of the new plants suggested new industrial strategies for obtaining CMCs reducing processing time and energy consumption, in agreement with the objectives of the project. Companies involved in several applications of CMCs were directly impacted by the project activities.
Aerospace materials
In the HELM project the aerospace materials involve HERAKLES and AIRBUS (AGI).
HERAKLES is one of the world’s leaders in the design and production of solid rocket motors for missiles and space launchers. For more than 30 years, HERAKLES has been using thermostructural composites, designed to withstand very high loads in extreme environments and has focused his industrial efforts on CVI technology for producing CMCs for aerospace applications.
The HELM project impacted HERAKLES industrial activities thanks to the knowledge and deeper understanding of phenomena associated with MW assisted CVI. The project provided also some preliminary results about the feasibility to build MW-CVI furnaces. The reduction of processing time achieved in the project is quite promising.
AIRBUS Group is interested in all the 3 main standard process routes for the fabrication of non-oxide CMC: Polymer Infiltration Pyrolysis (PIP), Liquid Silicon Infiltration and Chemical Vapour Infiltration (CVI). However, the main commitment of AGI in HELM is to investigate the hybrid or MW/RF assisted PIP to demonstrate its feasibility (proof-of-concept) as a cost-effective process route to manufacture SiC matrix CMC materials with C and/or SiC fibre 2D/3D performs. PIP process manufactured C/SiC is currently used in AGI for Thermal Protection Systems (TPS) and Hot
Structures (HS), for instance for re-entry vehicles as well as for propulsion parts because of excellent material characteristics. HELM project contributed to demonstrating the suitability of MW/RF techniques to manufacture components, although an optimization of the pilot scale plant is still necessary.
Refractory materials
SKT is one of the leading enterprises in the field of CVI and CVD processes for graphites and composites worldwide. These manufacturing methods are all based on PIP, silicon modifications (e. g. LSI), CVI and CVD techniques as well as heat treatments for pyrolysis and graphitization treatments. The SKT main business is the manufacture of CMC-structural components for industrial plants for polysilicon production: heaters; thermal insulations; heat shields; crucibles; tools. All these applications require highest purity (low carbon contamination), toughness, thermal resistance up to 2000 °C, cost efficient, low methanisation rate, oxidation/corrosion resistance against SiO2. To this, CVI technique is the most suitable one.
The HELM project enabled SKT to develop an isothermal CVI-SiC densification technique for high performance composites. In past SKT applied the CVI process only for mixed matrix systems or with a lower degree of densification for thermal insulation parts. The progress made in WP6 have shown further potentials for CVI optimizations at SKT, which will be used in future.
Rapid CVI processing
CVT has more than 25 years experience in CVD and CVI and holds the patented process of rapid-CVI (r-CVI), well defined and high reproducible CVI procedure in house. The r-CVI is a fast and reliable techniques for manufacturing carbon-carbon (C/C) and carbon-silicon carbide (C/SiC) materials which allows densification of carbon fiber preforms within days (less than 30% wrt traditional method). For this specific competence, CVT is technology partner of SKT and AGI for r-CVI manufacturing of high purity materials with also high density, extremely uniform densification and adjustable matrix regarding texture of infiltrated carbon. CVT has improved their own rapid CVI-SiC densification method by optimization steps within WP 6.
Carbon-ceramic brake disks
BSCCB, a joint venture between Brembo SpA and SGL Brakes GmbH, is a world leader in the sector of carboceramic rotors manufacturing for high performance brake systems. Automotive brake disks are representing the first large scale application of CMC materials.
The role of BSCCB in HELM was to exploit newly developed MW-LSI and MW/RF assisted pyrolysis for the production of ceramic carbon-ceramic brake disks.
Demonstration prototypes of brake disks were produced and the mechanical properties of four disks resulted close to the target but the porosity is higher than standard product and the thermal conductivity is far from the specification (<30-40%). For the production of brakes some optimization are still necessary to reduce the properties gap between the conventional and MW-LSI disks.
Preliminary promising results were achieved also by RW-PIP technologies. Also in this case further optimizations, mainly in processing, are needed.
Antiballistic materials
PETROCERAMICS has experience in the production of antiballistic ceramics made of carbides, nitrides and carbon pre-forms densified via liquid silicon infiltration (LSI) process. Thanks to HELM project a MW-LSI pilot plant was built and tested. Mechanical properties of torso plates produced in HEM project by MW-LSI pilot plant resulted comparable to those of well densified samples by standard heating process. In single shot test on some samples of torso plates the bullet was retained with a reduced trauma of back layer. The analysis of the morphology showed that the properties of the MW-LSI plate was similar to the ones observed for conventional LSI, but some residual porosity could be noticed in the former. The total energy saving was 13% and time saving is also achieved.
SiC foams
ERBICOL is active since in the production of porous ceramics made of silicon infiltrated silicon carbide for components working in high temperature, harsh environments, where are needed materials with high thermal conductivity, high thermal shock resistance and high corrosion resistance. Such products are gas burners, radiation plates, fuel cell reformers, catalyst support and many more.
Thanks to the HELM project activities it was possible to build a MW-LSI pilot plant for foams and demonstrate the compatibility of MW-LSI with SiC foam manufacturing. In particular, the following conclusions can be drawn:
- The MW-LSI process is suitable for SiSiC foam processing and is faster than conventional LSI;
- The infiltration quality dependence on samples geometry has been overcome;
- Fully loaded MW-LSI furnaces have been processed delivering repeatable results and consistent product quality;
- The product properties of MW-LSI processed products are not as good as standard processed products, but the economic advantages of MW-LSI make the process a viable solution for a faster and cheaper liquid silicon infiltrations.
Expanded graphite
IMERYS produces high quality expanded graphite for energy applications, electrochemical storage devices, fuel cells and solar ovens, with about 2,500 t/year production and 11 Mio€ revenues annually for this segment
worldwide. The GE by the MW furnace built in the HELM project has shown, on a technical point of view, its potential to expand graphite in a way comparable to the industrial process. After optimization of the reaction parameters and accepting a compromise in the materials properties, a potential reduction in energy saving and production costs would be achievable. Final compatibility tests of the EG as filler in polymers and acceptance by clients would determine the potential of the process. Further increase of energy and cost saving could be realized with the scale-up of the process.
Impact on SMEs innovation and technology
The HELM project provided the three SMEs (ATL, FM, SAIREM) with a new technology portfolio for MW/RF processing of CMCs and GE. The expected outcome will bring development of new knowledge, new technologies and economic revenues for these SME participants.
ATL developed a hybrid/MW assisted CVI plant that will be included in his catalogue, while SAIREM and FM have the know-how on advanced MW and RF heating and can thus enrich their catalogue of products: FM
developed ovens for MW assisted LSI and GE, SAIREM developed MW componente for MW-CVI plant and RF furnace for Pyrolysis.
Environmental impact
The full LCA, LCC and TA performed in the HELM project definitively showed the benefits of proposed technologies in terms of using optimal amounts of raw materials, energy consumption and other energy saving
features.
Moreover, the spreading of CMCs in more sectors can allow the use of more durable materials, thus immediately decreasing generation of waste.
Another indirect good environmental impact consists of the development of materials for more efficient engines, allowing a reduction of fuel consumption and thus reducing not renewable resources consumption and related pollution/greenhouse effects.
Socio-economic impact
HELM project allowed the development of innovative technologies in manufacturing advanced materials to improve EU economy. By boosting the use of new processes it promoted the introduction of advanced materials on the market thus directly promoting new job opportunities in Europe. Moreover, these job opportunities are opened in the field of advanced manufacturing, considered strategic in research and innovation action strategies for SMART specializations by the Tuscany region (Italy). Smart Specialisation Strategy means the national or regional innovation strategies which set priorities in order to build competitive advantage by developing and matching research and innovation own strengths to business needs in order to address emerging opportunities and market developments in a coherent manner, while avoiding duplication and fragmentation of efforts” (Regulation 1301/2013 of the European Parliament and of the Council of 17 December 2013 ). Hence these new job places contribute to the convertion to SMART economy promoted by EC.
DISSEMINATION STRATEGY
The objective of the dissemination strategy applied was to identify and organise the activities to be performed in order to maximise the influence of the project and to promote commercial and other exploitation of the project results.
In more detail, the objectives of the dissemination were:
I. To raise public awareness about the project, its expected results and progress within defined target groups using effective communication means and tools;
II. To disseminate the fundamental knowledge, the methodologies and technologies developed during the project;
III. To pave the way for a successful commercial and non-commercial exploitation of the project outcomes.
In accordance with the Grant Agreement indications, every possible opportunity was embraced by individual partners or on collective basis through joint appearance to make HELM known among professionals and general public as well.
Ensuring effective internal communication and dissemination among the Consortium partners represented an important key success element for the Project. Periodic Meetings and TELCOs and the set-up of a Project Collaborative space were used as means to ensure a constant and effective of internal dissemination.
External dissemination targeted Academic and research community, Industrial sector, Industrial Associations, Government bodies and policy makers as well as Media and public community, at national, European and International level.
Dissemination activities in HELM project were deeply linked with the intellectual property (IP) rights protection. All issues regarding Intellectual property use and dissemination were specifically regulated by the EC-GA Articles II.26-II.34. Practical application of IP rights protection, and dissemination procedures agreed among HELM project partners were regulated also by the Consortium Agreement.
DISSEMINATION ACTIVITIES
A common graphic identity was defined at the beginning of the Project to allow for better visibility and recognition as well as branding of the HELM project, paying specific attention to the EC funding acknowledgement. Indeed all publications based on work funded by EC within the activities of the HELM Project acknowledged their affiliation to HELM and bear recognition of the EC funding.
To ensure maximum visibility to the HELM objectives and results a project website was set up registering in the “eu” domain and with intuitive URL to increase hit rates: http://www.helm-project.eu/
The design of the website built upon the following criteria, taking into account suggestions given in the EU Project Websites – Best Practice Guidelines (EC, 2010):
i. visual communication: use of colours and/or photos, web pages are easy to browse, information is kept short and links are included to websites, publications, and so on.
ii. verbal communication: the website uses simple phrasing, no jargon is used in order to attract the widest possible audience, e-devices are user friendly.
iii. visibility: maximum use of free or affordable methods to increase page ranking on search engines, Webmaster Tools provided by search engines to check indexing status, good cross-linking between the different pages of your site and other sites, add keywords to the web page metadata; use frequently used keyword search phrases both in the metadata and in the contents pages.
iv. regular update of contents: the website was maintained and the update regularly done by the Webmaster upon inputs from the partners; social media were also used.
v. Monitoring and feedback tools: the website includes a counter of visitors to measure the number of visits; a visitors’ feedback form, to get a feedback on the usability of the web site and on the interest created by the project.
The public section of the HELM website therefore:
▪ provides a brief project summary in journalistic style highlighting the objectives, the contents and the structure of the HELM Project including the composition of the HELM Consortium.
▪ provides a short profile of each of the HELM Partners and a link to the related web sites;
▪ provides access to the project Public Deliverables and abstracts of selected non-Public Deliverables;
▪ provides copies of publications and presentations done at external conferences;
▪ features a separate events section where events are registered and highlighted. It refers to HELM events such as HELM meetings and workshop, and conferences and external events where HELM had an active role (e.g. presentation of paper(s), organisation of sessions, stands with demos, etc.).
Also, Social Media channels were activated and maintained to increase visibility and thus raise public awareness:
Facebook https://www.facebook.com/pages/HELM-EU-Funded-Project/441410005901081
Linked-in https://www.linkedin.com/groups/8129092
Google+ https://plus.google.com/102803555881338454738
You Tube https://www.youtube.com/channel/UCxziJrpOd6QSa-dhi48r62Q ,
Twitter https://twitter.com/HelmEuFunded
HELM standard Flyer and Poster were issued, published, restyled and distributed throughout the project duration, with the aim to intensify and strengthen the effect of recognition of the Project.
The main objective of the project brochure is to provide our audiences with an attractive and written project overview and a summary of the main project objectives and characteristics. To assist the dissemination effort, an attractive and professionally made brochure has been prepared and published on the project website.
The brochure presents the goals of the project and the main (expected) findings. The text was designed taking in to account not only experts, but also an interested non-specialist. It introduced the main mission and the goals of the project. Furthermore, it included the website address and provides basic information on Consortium. All partners’ logos were also displayed.
The main purpose of the project poster is to catch the audience attention, with a visual representation clear and easily understandable by the target end users. To reach this objective an eye catching poster was designed, then restyled and updated.
With regard to the layout and design, the poster showed the project’s logo and the colours emphasizing the link to the project´s graphic.
From the content point of view, the standard poster illustrated the project objectives and included basic information on the project and on the Consortium, including all partners’ logos. It is possible to download it from the HELM website.
HELM consortium also operated with a proactive approach to the dissemination of the project objectives first and results later.
Press releases on partners’ websites were issued at the beginning of the project. Articles were published on scientific journals (Engineering Applications of Computational Fluid Mechanics, Ceramics International, Ceramic Transactions, Journal of European Ceramic Society, International Journal of Modern Physics, Developments in Strategic Materials and Computational Design, Wetting and Wettability) and more popular magazines (Platinum-on-line) throughout the project duration.
Newsletters were issued periodically, in order to present the project activities and results to interested parties, also through the website.
Posters were presented at relevant conferences and the project results presented orally to congresses and scientific events (also at yearly or periodic conferences such as: ECOS, ICACC, EUROMAT, ENF, HTCMC, NANOTECHITALY). Several sector Stakeholder and Academic representatives were contacted to discuss the project perspectives on all occasions.
Also, a final workshop on "Advanced Processing Technologies – institutional investments, research results and market potential" was organized at the end of the Project, on May 31st 2016, hosted by Consiglio Nazionale delle Ricerca in Pisa (IT). HELM Consortium met academic and industrial stakeholders and interested parties, to discuss research results and future developments of Advanced Processing Technologies. During the final workshop, the CVI Furnace and its results were shown, raising the interest of various industrial entities. Potential synergies and future collaborations were envisaged, to further HELM results in the future.
Ultimately, the Project has capitalized on varied opportunities to disseminate the Project results, in order to increase and cement the exploitation potential.
EXPLOITATION OF RESULTS
HELM was intended as a strategic project from the industrial point of view, considering that industry and market needs are the main drivers of development and integration of the proposed MW/RF thermal processing technologies.
CMCs and EG are advanced materials where Europe has outstanding leadership at global level; indeed some of those leaders are involved in HELM. HELM took into consideration the most significant market niches for C/SiC or SiC/SiC composites and EG, i.e.:
▪ aerospace thermos-structural composites (HERAKLES SA, AIRBUS DEFENCE AND SPACE GMBH)
▪ refractory materials (SCHUNK KOHLENSTOFF-TECHNIK GMBH, CVT GMBH & CO KG)
▪ ceramics for brake systems (BREMBO SGL CARBON CERAMIC BRAKES SPA)
▪ antiballistic applications (PETROCERAMICS SPA),
▪ silicon carbide foams (ERBICOL SA), and
▪ expended graphite production (IMERYS GRAPHITE & CARBON SWITZERLAND LTD).
At the same time, the project involved three innovate SMEs involved in the technical development (ARCHER TECHNICOAT LIMITED, FRICKE UND MALLAH MICROWAVE TECHNOLOGY GMBH and SAIREM IBERICA S.L.) for MW/RF processing of CMCs and GE.
The HELM Consortium therefore addressed the need of new technical solutions for European companies in the field to stay competitive in the market of CMCs and EG, requiring higher performance products at lower cost. Indeed the results obtained showed a relevant potential in reducing processing time and costs, as illustrated in the previous sections.
All partners of HELM owning exploitable results or in any case having acquired useful knowledge planned exploitation in different manners, jointly or individually. Indeed cooperation between the partners, during and after the project, played and plays an essential role in the successful exploitation of the innovations originated in HELM.
Research partners are clearly more oriented to transfer knowledge in academia and technology to interested stakeholders, while industries strongly focus on industrialization and future commercialization of the research products and by-products.
To be noticed that academic and research partners (CONSORZIO INTERUNIVERSITARIO NAZIONALE PER LA SCIENZA E TECNOLOGIA DEI MATERIALI, SCUOLA UNIVERSITARIA PROFESSIONALE DELLA SVIZZERA ITALIANA, FUNDACION TECNALIA RESEARCH & INNOVATION, FUNDACION CIRCE CENTRO DE INVESTIGACION DE RECURSOS Y CONSUMOS ENERGETICOS, BALTIC STATE TECHNICAL UNIVERSITY VOENMEKH, UNIVERSIDAD DE ALICANTE, Steinbeis Advanced Risk Technologies GmbH and CONSIGLIO NAZIONALE DELLE RICERCHE) as well defined further research paths and exploitation plans for the knowledge acquired and technology developed.
Therefore, it is planned to have a full return on the results achieved thanks to the investment from the EC both from the academic and industrial perspective, also joined in one unique approach, through further research, development and industrialization activities.
However, exploitable results and related exploitation plans within HELM are regulated by confidentiality and IPR management rules, therefore no details can be publicly disclosed.
List of Websites:
PROJECT WEBSITE:
http://www.helm-project.eu/
CONTACT DETAILS:
Andrea Lazzeri
andrea.lazzeri@unipi.it
Tel: +39 050-2217807
Fax: +39 050-2217903
Isella Vicini
isella.vicini@warrantgroup.it
Tel: +39 051 9840863
Fax: +39 051 9840885
Cinzia Iacono
cinzia.iacono@warrantgroup.it
Tel: +39 051 9840863
Fax: +39 051 9840885
