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Periodic Report Summary 2 - NEWSPEC (New cost-effective and sustainable polyethylene based carbon fibres for volume market applications)

Project Context and Objectives:
Carbon fibres (CFs) are the most efficient reinforcing materials in modern composite applications that require high specific stiffness and strength. A steady increase in future production and consumption of CF is predicted due to increasing demand from classical and new industrial segments such as aerospace, automotive, wind energy, sport goods and other industrial applications such as high pressure gas storage. However, the extensive use of CFs in large volume market applications is severely limited by the current market price of CFs - over 20 euro/kg - that results from the dependence on petroleum-based precursors and the laborious, expensive and often non-environmental friendly conversion processes. The development of cheaper and more sustainable fibres is indeed nowadays of paramount importance and this is further exacerbated by the current high demand for CFs.

NEWSPEC aims at the production of CFs through very promising precursors, such as polyethylene (PE). PE presents interesting technical features like high carbon yield (around 70%), high processability, flexibility and very competitive cost (~2 euro/kg) with respect to PAN precursor that may result into a precursor cost saving of up to 70%. The target technical features of the PE-CFs are: 250 GPa tensile modulus, 2 GPa tensile strength, 1% elongation, 10 microns diameter, and 1.8 g/cm3 density. Considering the overall CF production cycle, the final target cost of PE-CFs will be of 10 euro/kg that means a cost reduction of 30% with respect to comparable PAN based fibres.

For PE stabilisation an original dry oxidation method, assisted by Electron Beam Curing (EBC) that introduces heteroatoms at the precursor stage is proposed. The new approach has technical, economic and ecologic advantages thus ensuring very innovative and flexible development of new CFs. Novel strategies for the reduction of the graphitisation temperature via the use of nucleation agents such as cellulose nanowhiskers (CNWs), CNTs, graphite powders or Graphene Oxide (GO) are envisaged. The partners will also explore the possibility of surface modification via atmospheric plasma techniques and room-temperature grafting with specific surface-attacking chemicals. Online non-destructive laser Raman probe, that can provide in situ information for the development of the various fibre structures during the processing stages. A main attribute of this project is the use of an available pilot scale facility (HPFC) that allows design and optimization of endless CF processing and easy scale up to a larger size industrial plant.

Specific carbon composite prototypes will be manufactured and tested by the end-users during the lifetime of the project to ensure the validation of CF functionality for the final components with this ensuring proper exploitation of results. NEWSPEC involves specialized end-users as manufacturer of carbon composites, both CF reinforced and carbon ceramic matrix composites, in each of above mentioned segments: aerospace, automotive, wind, oil/gas transportation and storage.

To prove overall environmental and economic sustainability LCA and LCC are implemented within all phases of the project.

NEWSPEC brings together the best available expertise in Europe for the development of the PE-CFs up to mature exploitable technology. It consists of RTD performers with well-documented experience in CFs development and industrial end-users who are specialist in the target market segments.

Project Results:
The lab phase of the NEWSPEC project was successfully concluded. Since the beginning of the project the Consortium has investigated different PE precursor materials. The approach was focused on staring material from which the best CFs in terms of mechanical properties can be obtained. The polymers were fully characterized and the best precursor to be used in subsequent pilot phase has been selected.
Four different stabilization methods have been tested in the project and the best stabilization method for continuous process was identified. A novel technology for continuous PE fibres stabilization process has been designed and a new pilot equipment was developed and installed at the HPFC facility. The best stabilization parameters for preparing the PE carbon fibres were identified. The resulting fibres were non-brittle and could be processed without problems even as single filaments. Rest mass in carbonizations is actually about 30%, with calculates to a carbon yield of 75% based on the raw PE. The carbon phase was well oriented. WAXS data showed a well-developed aromatic structure even in the precursor as in the resulting CFs. The mechanical properties of the resulting carbon fibers samples is best for the polymer from type HDPE, which reaches 0.9-1.1 GPa strength and 100-135 GPa of modulus.
One of the activities regards the reduction of the graphitisation temperature via the incorporation of nucleation agents. This work was started with transforming of natural graphite powder (GP) into graphene oxide (GO) using Hummers’ method, several dispersion trials were performed but this method was abandoned because leading to poor results. Cellulose Nanocrystals (CNCs) have been successfully dispersed into the PE matrix. PE master batches with already dispersed Carbon Nanotubes (MWNTs) were acquired from suppliers upon specifications. The dispersion of nanoagents in the PE matrix was verified using a newly developed method based on Raman imaging.
The installation of a prototype system for continuous plasma treatment of CF has been finalised. The equipment is now operational for the surface treatment of endless CFs. The system has been validated using commercial PAN-CF as model material. Innovative surface treatments were also studied. The chemical reaction of epoxidizing the outer surface of the CFs is successful. The process can be applied to these materials. The epoxidation efficiency (as measured by the surface oxygen content) can be tuned and depends on both immersion duration and reagent concentration. The whole procedure (solution preparation and immersion) does not require any form of heating and can be utilized in room temperature. Preliminary results have shown an interface (between epoxidized CF and epoxy matrix) enhancement, compared to non-epoxidized fibres.
The installation, set-up, calibration and testing of the remote Raman probe system for on line monitoring of the CF production process has been completed. Several functional tests were performed using commercially available PAN fibres and the Raman facility is now fully operative. The set-up of measurement protocols is still in progress with mechanical experiments on various commercial fibres and Raman testing of the fibres under tension and compression.
In order to obtain an integrated and quantitative view on environmental and cost impacts across the full life cycle of the developed carbon fibres within NEWSPEC, Life Cycle Assessment (LCA) was combined with Life Cycle Costing (LCC). After a phase of data gathering from different sources and databases, an initial LCA/LCC model has been developed at the scale of 1500 ton/year in order to allow for a comparison with established CFs, such as PAN-CF, for which LCC and LCA data are more readily available.
As part of the exploitation activities of the project, a market overview and an IPR survey was performed. An internal survey that covers both technological and non-technological risks, including innovation and exploitation risks, has been carried out. Risk survey also includes relevant aspects associated with CFs manufacturing, such as safety and environmental risks.
Since the beginning of the project two Summer schools have been organized in the framework of NEWSPEC. The 1st School was organized by FORTH in Patras (Hellas) from 15th to 19th of June 2015; about 50 students from all over the world have attended the course. The 2nd Summer Course was organized by Warrant Group on June 12th-17th 2016 as an itinerant course, students had the unique opportunity to visit the labs and production sites of of Brembo, BSCCB, Petroceramics, Lamborghini and Dallara Automobili SpA. Forty people attended the course and the feedbacks were extremely positive.

Potential Impact:
In order for Europe to achieve higher independence from imported CFs and fossil oil-based precursors, mainly PAN, it is necessary to invest resources on development of novel strategic CF precursors. This shall bring about novel, technically valid, cheaper and environmentally sustainable materials. NEWSPEC applied research proposes indeed promising materials such as poly-olefin which can be derived from bio-ethanol. The PE-CFs could provide the highest performance/cost ratio than any other precursor currently under investigation. At this PE combines high availability and versatility, since non-fossil alternatives are available at very competitive market prices.

The restrain of climate change reversal, the decrease in energy prices and the energy efficiency are the main drivers for a future sustainable economic growth. For this reason the fuel consumption of air and terrestrial vehicles, and thus their exhaust emissions, has to be cut. It is estimated that each kilogram that can be saved per moving load, can help towards deferral of global warming and, thus, can pave the way for a better future for the planet. Carbon fibre reinforced composites (CFRC) are 80% lighter than steel and 50% lighter than aluminium, while delivering at least twice the strength and stiffness. The reduction of the overall weight of an aircraft by 60% can increase considerably its effective payload and can also yield to significant savings in fuel consumption.

In the automotive industry, there is enormous potential, all the way to new designs, to reduce the mass of many relevant components (body, chassis, interior parts and brake systems) and therefore decrease dramatically fuel consumption and GHG emissions. CF cost still represents the main market barrier for the mass-market penetration of those materials, therefore the primary need of the automotive supply-chain industry is to reduce the cost of CF composites.

The use of CFs in wind energy blades is projected to be the first largest application sector by 2020. New offshore and onshore wind power plants with much higher degrees of efficiency based on CFRC will help generate alternative energy economically in the near future. The increasing dimensions of the wind turbine blades (>1MW), especially in offshore areas, will require the extensive use of CFs due to the enormous tensile loads on rotors with large diameters. Retrofitting of already installed (smaller) turbines is also of considerable interest for the “wind companies”. Here low-cost CFs could be an ideal replacement for classical low module E-glass fibres providing enhanced technical performance at competitive cost.

Enormous opportunities for CFRC application is given by civil and industrial infrastructures building. One such promising field is that of oil/gas transportation and storage (compressed natural gas tanks, offshore oil wells, pipelines and gas turbines). The largest new potential end use for CFRC could be the manufacture of riser pipes, drill risers and choke and kill lines for the offshore oil industry: one single 3000 m CFRC riser string with 100 joints consumes about 60 tonnes of CFs, as 17 large wind blades or 200 sport cars today. The future is also likely to witness the growth of CF in the fuel cell industry for the making of natural gas and hydrogen storage systems.

Low cost CFs will open several new application perspectives and, by consequence will have high industrial, environmental and societal implications. Thus, NEWSPEC will contribute on towards FP7 and Horizon2020 objectives to create growth and jobs, especially for the benefit of SMEs (half of the Consortium partners are European SMEs).

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