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QUANTIHEAT Report Summary

Project ID: 604668
Funded under: FP7-NMP
Country: France

Periodic Report Summary 2 - QUANTIHEAT (QUANTItative scanning probe microscopy techniques for HEAT transfer management in nanomaterials and nanodevices.)

Project Context and Objectives:
The QUANTIHEAT project is aimed at addressing the problem of thermal metrology at the nano-scale and at delivering validated standards, methods and modeling tools for nanothermal design and measurements.
Control of heat flow is central to a large number of technologies. Indeed, modern material science and technology are increasingly devoted to the control of matter at the nanoscale. However, usual methods for modeling and designing experiments in macroscopic systems are completely inappropriate and no effective and quantitative tool for thermal measurement at the nanoscale currently exists.
The key promising technique for thermophysical properties measurements at the nanoscale is Scanning Thermal Microscopy (SThM), but this technique remains highly non-quantitative. The need is for a complete thermal measurement and modeling technology for use at the nanoscale.
The main expected outputs of the project are to be useful as practical standards in the real world. Accordingly, the project includes applications where materials are modified at the nanoscale during manufacturing processes due to thermo-dependent effects or have to be thermally characterized and optimized. These applications include thermal and UV-nano-imprint lithography (NIL), novel nanostructured micro-particle based interconnects materials, atomic layer deposition (ALD) and novel generation of nanostructured thermoelectric (TE) and thermal interface (TI) materials.
The QUANTIHEAT Consortium gathers 20 partners, from 9 different countries that are leading experts in their fields (attachment1): 10 academic leading groups in thermal nanoscience and nanoengineering, thermal nano-measurements and nanofabrication, and thermal nanometer-scale instrumentation, 3 National Metrology Institutes (NMIs) and 7 industrials developing materials and fabrication processes or characterization equipment.
The key objectives of the project are to:
• Establish a consistent and rigorous terminology in the vocabulary for nanoscale thermal metrology,
• Characterize existing microscale SThM measurement methods and traceably quantify their repeatability and reproducibility,
• Develop new metrology tools, including calibration, reference and test samples as well as modelling tools; derive test protocols for the most promising methods and push the dimensional limits of thermal metrology down to 50 nm,
• Use these validated metrology tools to characterize the physical mechanisms of micro and nanoscale energy transfer between two solid objects (probe and sample). The results will be used to refine existing models of thermal transport at the nanoscale. The models will then be used to acquire a new quantitative understanding of heat transfer at the scale of nano-contacts such as those operating inside nano-crystalline, nano-composite or nanoporous materials,
• Apply the newly developed tools to the design and optimization of new SThM nano-sensors, benchmark these tools and sensors in the frame of specific relevant applications involving: nano-composite and nanostructured materials.
To reach these objectives in a hierarchical way, the project is divided into 6 R&D parts corresponding to five sub-projects (SP) and a new technology application work package (WP) (attachment2). Each SP is divided into two goal-oriented WPs, which are divided into different tasks. Technical work is supported by 2 management WPs and 1 dissemination and exploitation WP.
The project will lead to a large number of Deliverables (70 deliverables including 58 for the technical work) associated with 21 Milestones. Thus, the progress of the work is reported step by step and is regularly checked by all the partners involved in the project.
QUANTIHEAT is coordinated by CNRS. The scientific management is led by CNRS with the support of SP&WP leaders who compose the project executive and scientific boards. Moreover, an external advisory board, composed of 4 members from Academia and Industry, was created to provide advice and guidance to the Consortium.

Project Results:
The tasks of the first step of the project (SP1: Specification and methodology) were achieved in P1, providing the basis for the other R&D activities that started within SP2- SP5 (attachment2).
The industrial application oriented specimens to be studied and the requirements for new generations of nanomaterials and processes were defined in detail. The thermal characterization techniques and methodologies available within the consortium for multi-scale analysis of heat transport at different length scales were specified. This enabled the identification of measurement and modeling pathways linking thermophysical measurements with industry specified materials.
A review of definitions and terminology currently used in the micro and nano-scale measurement community was undertaken and recommendations were made for terms and definitions applicable to SThM measurements. Uncertainty budget analysis methodologies were developed by NMIs. The requirements for calibration, test and scientific samples to be developed for evaluating SThM measurement were specified and test plans for experimental research to be carried out were established.
On this basis, in P2, first passive calibration, test and scientific samples as well as first sets of industrial samples (NIL resist thin films, ALD, TE and TI materials) were fabricated and disseminated to partners for their measurements by means of various characterization methods including SThM techniques (attachment3). At this stage of the project characterization results have been mainly aimed at improving the first sets of passive test samples. In accordance with the test plans to be performed with the samples selected by the consortium for thermal calibration and thermomechanical calibration of SThM techniques, interlaboratory comparisons and SThM measurements were initiated. Study of the first sets of industrial samples allowed refining the thermal characterization techniques to be developed and/or to be applied to solve critical aspects related to manufacturing processes, materials and characterization. Material and manufacturing process were developed, supported by characterization results for NIL resist, ALD and interface materials. The fabrication process for the first version of four categories of active devices was completed and devices were characterized through modeling and measurements for the development of temperature reference and heater devices for the calibration of SThM tip temperature and for thin film characterization using the 3-omega method. Measurements following the test plans established for temperature measurements started.
Supporting modeling activity provided BTE-based simulations of the thermal distributions of thin films and confined geometries heated with localized heat source and numerical codes for heat conduction issues in many classes of nanomaterials with varying levels of details were developed. Based on an overview of the available probe-sample interaction modeling approaches methodologies for treatment of more complex tip-sample geometries were established. Fast modeling tools were developed for speedup of experimental data analysis and for building more complex models.
First SThM measurements with the new instruments developed were demonstrated. This include new and evolved SThM probes, new SThM-based techniques combining SThM with Scanning Electron Microscopy and Infra-Red radiometry, a novel SThM technique calibrated in a liquid environment and a novel thermal–force imaging mode.
The evaluation of SThM methods was initiated with the establishment of draft of calibration protocols for SThM measurement of (i) thermal conductance, (ii) surface temperature and, (iii) phase change temperatures and the assessment of measurement uncertainties.
Beyond scientific work, the Consortium participated in 153 dissemination actions. To promote the exploitation of the project’s results, our exploitation plan is continuously refined under the advice of an ESIC Expert from the EC.

Potential Impact:
QUANTIHEAT’s main outcome is the establishment and implementation of a new metrology technology based on scanning thermal probing to characterize the thermal properties of nanomaterials and devices at the nanoscale. Expected results in metrology include (attachment4):
• Measurement methods, reference and calibration samples, measurement procedures, and good practice guides,
• Modeling and simulation tools,
leading to the creation of standards in the field of research on nanoscale thermal properties.
The focus on standardization ensures the greatest possible industrial applicability. An emphasis on validated modeling is of particular relevance to the needs of SMEs for whom extensive experiment-based development cycles are impractical.
It is intended that the developed terminology for SThM measurements will be submitted for normalization to the European Committee for Standardization (CEN: Comité Européen de Normalisation) or, preferably, to the International Standards Organization (ISO) with adoption by CEN under the Vienna Agreement. The latter option provides opportunities for more effective European influence over the global market via the standardization process, as well as promoting a wider international feedback to the project. Depending on the type of reference samples and project results, a certification process for calibration samples may be also implemented.
Good-practice guidance and Standards for calibration and SThM measurements will be provided and will form the basis for submission of New Work Item Proposals for standardization through ISO or CEN.
For dissemination within the atomic force microscopy (AFM) community of the developed SThM techniques, the unification of SThM cantilever holders and electronics for different AFM models is of primary importance.
The project will develop traceable measurement methods and will seek to establish them as potential standards. The establishment of internationally-agreed calibration standards and models will enable rational design and will provide an agreed basis of communication between designers, manufacturers and users of nanomaterials.

The Project will also guide, enable and advance the development of (attachment4):
• new-generation nanomaterials for NIL and TI materials,
• new processes such as those for semiconductor manufacturing industry, NIL mask coating, Graphene coating, but also for semiconductor, energy (TE materials)).
Complete thermal measurement at appropriate scales will provide a check on the design process and allow design optimization to better address thermal management needs. This will result in improved lifetime and reliability of the devices with reduced production costs and need for testing.
Knowledge of the thermal performance of new nanomaterials is an essential prerequisite for use in many industrial sectors. The project will provide technology and tools to perform the required characterizations, and provide important information enabling customers to select their materials.
SMEs will benefit from the QUANTIHEAT project results in many ways in terms of applications and products. The project will then enable an increase of industrial competitiveness through strengthened capabilities in innovative products and services.

Furthermore, the increasing demands of European industry and research sectors for qualified human resources in the area of heat transfer management for nanotechnologies are addressed in the project by several means: the project will contribute to the training of scientists and engineers in leading European industrial and research laboratories working on nanoscale heat transfer measurement, modeling and management (attachment4). The organization of events by consortium such as the QUANTIHEAT scientific school (December 2014) and sessions specific to the project at international events (THERMINIC 2015 in Paris, EUROTHERM108 2016 in Greece) contribute to improve the basic know-how of scientists in these research areas.

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