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Inhoudsopgave

1 Introduction ...................................... ........................................................................ 3

2 Program Solar ..................................... ..................................................................... 4 2.1 Introduction ................................................................................................................ 4 2.2 Program 2013 ............................................................................................................ 5 2.3 Results 2013 .............................................................................................................. 6 2.4 Cooperation ............................................................................................................... 6

3 Program Lighting .................................. ................................................................... 8 3.1 Introduction ................................................................................................................ 8 3.2 Program 2013 ............................................................................................................ 9 3.3 Results 2013 ............................................................................................................ 11 3.4 Cooperation ............................................................................................................. 12

4 Program Printing and Additive Manufacturing ....... ............................................ 13 4.1 Introduction .............................................................................................................. 13 4.2 Program 2013 .......................................................................................................... 14 4.3 Results 2013 ............................................................................................................ 15 4.4 Cooperation ............................................................................................................. 16

5 Program Healthcare................................. .............................................................. 17 5.1 Introduction .............................................................................................................. 17 5.2 Program 2013 .......................................................................................................... 18 5.3 Results 2013 ............................................................................................................ 19

6 Program High-Tech Materials ....................... ........................................................ 21 6.1 Introduction .............................................................................................................. 21 6.2 Program 2013 .......................................................................................................... 21 6.3 Results 2013 ............................................................................................................ 24 6.4 Cooperation ............................................................................................................. 26

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1 Introduction

This report describes the developments of TNO‘s VP High-Tech Instrumentation and Materials (HTIM) over the year 2013 with respect to the Topsector High-Tech Systems and Materials (HTSM). This report is part of the 4-yearplan of TNO and the yearly adaptation as prescribed in the TNO law and is part of the lawful obligation of TNO to account for the usage of SMO (Samenwerkings Middelen Onderzoek) by TNO. The VP HTIM has five programs: Solar Equipment, Lighting, Printing and Additive Manufacturing, Healthcare and High-Tech Materials. The first four programs are directly connected to four Shared Research Programs: Solar Equipment with Solliance, Lighting with Snellius, Additive manufacturing with Penrose and Healthcare with van ‘t Hoff. The five programs in HTIM are directly aligned with the respective roadmaps in the Topsector HTSM Solar, Printing, Healthcare and High-Tech Materials. From the Solliance program only the research related to CIGS (cupper-indium-gallium-selenide) is reported here and of the Lighting program only the inorganic LED program of Snellius. This is because all organic electronics programs like OLED (Organic Light Emitting Devices) and OPV (Organic Photo Voltaics) are concentrated in a Shared Research Program at the Holst Centre (a Shared Research Program of TNO with other research partners imec, ECN and many industrial partners) that has its own road mapping and reporting process. As VP arena’s and roadmaps were not yet all aligned in the VP High-Tech Instrumentation and Materials we decided to concentrate particularly on the Shared Research Program meetings and used them as arena’s.

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2 Program Solar

2.1 Introduction

A reliable, affordable, clean and safe energy supply is a prerequisite for the future economic and social development. Amongst others, this requires a change to energy generation by renewable sources, like wind and solar. The Dutch High-Tech Industry is well place to exploit the opportunities arising from this need for renewable energy sources, in particular photovoltaics (PV). The present volume of the solar cell market is 90 billion Euro/year, and the installed capacity of 100 GWp PV power expands at a rate of 40 GWp/year. The market growth of 50%/year over the last decade was enabled by increase in product quality (conversion efficiency) with a simultaneous steep decrease in cost. The final breakthrough for PV energy is realization of grid parity (PV electricity to be competitive with retail electricity prices). Therefore the main driver in the PV industry is the reduction of solar energy generation costs. Although the large reduction of PV module cost seems to be driven by several incidental factors (overcapacity, investment crises and a market consolidation), it is common opinion that there is still an enormous potential for further product improvement and cost reduction, with the potential for a two orders of magnitude market growth up to 2050, and a considerable contribution of PV to the worlds electricity production. A large part is traditional c-Si PV modules, but the market volume and share of thin film-PV devices and in particular CIGS will increase dramatically in the coming decade creating market opportunities for new processes and equipment. Also, it is generally expected that the next leap in efficiency improvement of PV modules will be enabled by combining c-Si and thin film technologies in tandem structures. Europe is leading in this technology development, and Dutch industry has 5% market share of PV equipment production. Both quality improvement and cost reduction are driven by the technological development of low cost, large area (eventually Roll-to-Roll) thin film technology. Using it broader background in large area electronics, thin film technology, material science and high-end equipment, the TNO program is focused on development of equipment and processes for thin film photovoltaics, more specifically on CGIS- and the closely related CTTS –based technology. The overall aim of the solar equipment program is to enable easy, affordable and embedded PV technology through development of world class generic manufacturing equipment and process solutions that: • Close the 5% efficiency gap for CIGS between lab and production using fast

and reliable production methods and equipment to achieve > 20% conversion efficiency modules.

• Move from current vacuum processes to atmospheric processes for large area R2R production; < 10 €c/kWh and > 99% high yield production.

• Allow green production and reduced use of scarce materials. • Enable and validate > 25 year PV module life time. • Facilitate smart and easy PV integration. These aims are in line with priorities defined in the national Dutch Solar Roadmap written for “Topgebied HTSM” and “Topgebied Energie” (both co-authored by TNO), which in turn was based on a critical assessment of international PV Roadmaps. The Solar Roadmap is the guideline for the research topics of the Solliance Initiative, the research collaboration between TNO, ECN, TU/e, Holst Centre, imec

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and Forschungszentrum Jülich. In collaboration with industrial partners and investors Solliance aims to generate new (regional) business through research on three thin film-PV technologies: aSi (managed by ECN), OPV (Holst) and CIGS, which is led by TNO.

2.2 Program 2013

The scope of the research activities in the program includes all PV technologies, but thin film CIGS is chosen as the carrier for the development of knowledge on various generic PV production technologies. The activities in this program have been divided into five work packages governing generic technologies along the various stage of the solar cell manufacturing chain. Work package 1: Solar module demonstration, lifetime prediction and integration Main activities: Development of CIGS reference process for 10x10 cm2 co-evaporated demonstrator cells on rigid glass substrates and development and evaluation of equipment to accelerate lifetime and reliability testing. Highlight: Processes of the CIGS baseline were further improved and efficiencies were increased to a record of 15.2%. An average efficiency over all cells of 13% was established. Subsequently other technologies were used to replace the conventional methods. For example CIGS cells with atomic layer deposited (s-ALD) i-ZnO were made in cooperation of the TU Eindhoven showing improved cell parameters. Besides that the first CIGS cells on flexible stainless steel foil were produced, see picture. Work package 2: Atmospheric photo absorber processing Main activities: Development of atmospheric process CIGS demonstrators at 30x30 cm2 scale for S2S and R2R production, more specifically the development of a precursor electrodeposition and selenisation process for CIGS demonstrator cells with > 15% efficiency together with in situ process sensors for thin film monitoring. Highlight: CIGS solar cells on glass have been produced using electrodeposition of Cu/In/Ga (CIG) precursor stacks and subsequent selenisation in elemental Se with a maximum size of 32.5x32.5 cm2. On a 12.5x12.5 cm2 area an average efficiency of 6.9% was reached and a maximum efficiency of 8.4% on a 0.5 cm2 area for a non-optimized process. This constitutes the baseline process for low-cost CIGS absorber layer processing at atmospheric pressure. Alternatively, CIGS cells with a maximum efficiency of 10.5% on a 0.5 cm2 area were produced from vacuum sputtered CuGa/In precursor stacks and a similar atmospheric selenisation process on 12.5 x 12.5 cm2 glass panels. Work package 3: Light Management

Main activities: Development of s-ALD and AP(PE)CVD equipment and processes for S2S and R2R

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deposition of < 15 ohm/sq ZnO:Al and development of s-ALD, AP(PE)CVD and wet-chemical processes for amorphous TCO deposition. Highlight: A process for spatial ALD deposition of ZnSnO transparent conductive oxide films was developed. The crystallinity and properties of the film can be controlled by varying Sn/(Zn+Sn) in the range from 0 to 30%. At Sn/Zn+Sn is 1%, films have a polycrystalline structure and are highly conductive, 5 mOhm cm, and transparent, 94%, in the visible range and. At Sn/(Zn+Sn) > 16%, films become amorphous and highly resistive. Work package 4: Cell interconnection Main activities: Design of R2R equipment for post-scribing and interconnection of thin film cells. Highlight: A back-end interconnection concept for interconnecting cells in a module was validated on a 10x10 cm CIGS cell produced in the CIGS pilot line. By combining laser scribing and inkjet-printing a CIGS module giving 4.5 V output voltage was demonstrated. Work package 5: New solar cell concepts Highlight: Kesterite (Cu2ZnSnSe4) solar cells from an electrodeposited Cu/Zn/Sn precursor stack were produced. A baseline process for successive electrodeposition of Copper, Tin And Zinc on a 12.5x12.5cm2 Mo-coated glass panels was developed. The as-deposited precursor layer was selenised at imec using a H2Se process and further processed at TNO. Although the obtained cells showed a relative large amount of shunts a solar cell activity was obtained.

2.3 Results 2013

Work package 1: The CIGS baseline installed in 2012 was optimized to a reference process for 10x10 cm2 co-evaporated demonstrators cells on rigid glass substrates and first tests on flexible substrates were done. Work package 2: Baseline processes for CIGS cell production by atmospheric selenisation of sputtered and electrodeposited CuInGa (CIG) precursors were developed. Work package 3: Atmospheric pressure, CVD and s-ALD processes for S2S deposition of crystalline and new amorphous TCOs were developed and demonstrated as planned. Work package 4: Models to assist the design of R2R equipment for post-scribing and interconnection of thin film PV cells were developed and validated in 2013 as planned. Work package 5: A baseline process for electrodeposition of kesterite (Cu2ZnSnSe4) cells was developed and cells were produced.

2.4 Cooperation

A Shared Research Program (SRP) on CIGS as part of the Solliance initiative will be established and expanded in 2014 based on a short list of 20 existing industrial partners that have been approached in 2013 for participation. The technologies

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developed in the various work packages of the solar program are the core of the proposition for participation in the SRP. The CIGS SRP leverages individual partner’s participation fees through multiple partner contributions, matching funds (TKI and SMO) and EU projects. In relation to the Solliance initiative the customer base of industrial partners for commercialization of the project results involves the entire PV manufacturing chain. Partners in 2013 were companies ranging from material suppliers (Umicore, Enthone, DSM), substrate suppliers (AGC, Arcelor Mittal, Fuji) through equipment manufacturers (Meco, Smit Ovens, Singulus, Roth & Rau, IBS) towards solar module manufactures (Nexcis, Scheuten, Bosch, Avancis, Crystasol, Flisom), PV end-users/integrators (Oskomera, Abengoa, Dutch Space) are existing or potential partners for this technology development within the framework of cofi projects (Smit Ovens, MECO), EU projects (HipoCIGS, R2R CGIS) technology programs (TKI Energy, PID) and bilateral projects.

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3 Program Lighting

3.1 Introduction

As lighting design is rapidly changing and has become of a multi-disciplinary nature, the emphasis in design needs to shift. Currently the optical design of lighting systems and luminaire designs are driven by methods as employed for halogen, discharge and CFL type sources. However, the LED sources are of a different nature and act more as point-sources, while the traditional ones act as line or globe sources. As LED’s are more electronics based, the electrical design also has high attention. A good balance between optical, electrical, thermal, and mechanical design, satisfying many other conditions (chemical, moist, UV, …) is still challenging. Fundamental steps are being made in cooperation with TU/e (Group Ivo Adan). These methods are then “translated” in industrial approaches. Although SSL already has a green image because of the energy saving that can be achieved, the environmental impact of the products and manufacturing processes to generate SSL luminaires is not very optimal: the highest environmental impact in this area is reached by the long life time of the products, while the environmental impact per product is actually higher. In the Roadmap Lighting of the Topsector HTSM four main areas of research are defined: A) Lighting component technology improvements B) Improvement of SSL systems C) Human Centric Lighting Solutions D) Maturing the OLED technology

TNO is responsible as the agenda setting party for ‘Improvement of SSL Systems’ and ‘Human Centric Lighting Solutions’. In this respect the Snellius Innovation. The third research program is Smart Lighting Solutions. Partnership started in January 1st, 2013. The relation of Snellius to the Topsector Lighting is given below.

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3.2 Program 2013

Human Centric Lighting Solutions The SRP Human Centric Lighting Solutions (HCLS) focusses on the development of evidence based lighting solutions in which a user can perform his or her activities (both visual as non-visual) better, safer and more comfortably while using a minimum of light related energy. The parameters and specifications that define the lighting solutions will be converted into a common set of parameters, guidelines and codes of practice for evidence based lighting solutions, which are still lacking to date. The 2013 objective of the SRP HCLS is to develop a ‘Dynamic Lighting’ solution that uses advanced communication networks that will optimize lighting of infrastructure (outdoor) and rooms (indoor) based on the presence of vehicles or persons, user needs and aspects like weather or glare. To be able to study the effects of a dynamic lighting solution, the hypothesis that it is possible that with the right light the perceived safety and comfort can be increased while saving energy at the same time is studied. A lighting concept that complies with the hypothesis will be designed in 2013, based on key performance indicators and values that are either adopted from state of the art literature or found by lab experiments. The studying and the validation of the concept is done by questioning a large group of users of the lighting system in a field experiment is foreseen to be completed by the end of 2014. The complete work description and background is given in the IBC proposal for the SRP as well as the annex. Smart Lighting Solutions The SRP Smart Lighting Solutions” (SRP SLS) will focus on creating smart (intelligent) technology lighting solutions (HW/SW) which are: 1) easy to install (Plug & Play), 2) easy to use and 3) easy to maintain over lifetime enabling Dynamic-, Personalized- and Integrated Lighting Solutions. This program will research how a common technology platform using a decentralized system approach can be established for indoor and outdoor lighting applications open for multiple vendors and enabling seamlessly integration with Smart Buildings or Smart Cities overcoming the detected technology roadblocks of past intentions to do so. The program in 2013 focussed on getting better insights into the state of the art for networked lighting applications and on defining the detailed technology program including the Technology Roadmap in cooperation with the partners of the program. The research work started with the realization of the first lead user project. This included a) first system architecture and technology platform set up; b) defining and testing a sensor suitable to detect people and cars; c) testing wireless communication system components to enable a distributed wireless lighting system without central controller; d) build a tracking and light planning simulation tool to

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simulate and compare ground ture with the reality. Furthermore a close cooperation was established with the Human Centric Lighting System Program for Q-Park to be cover the needed use cases. The program in 2013 focussed further on creating testing systems and setting up the first modelling approaches. It is foreseen to complete a “loop” including testing and system modelling, firstly being able to work on light flux (i.e., lumen output). Later (2014 and beyond) the performance criteria will be further sharpened to include color shifts, light patterns etc. These future criteria are to be delivered by the human centric program and external sources. These, however, do not exist yet. For 2013, the following activities on the different subjects were foreseen. Human Centric Lighting Solutions: Concept development of a ‘Dynamic Lighting’ solution that aims to increase the level of perceived safety and reduce the lighting related energy consumption based on a car park use case. The necessary functionalities and requirements will be inventoried and the specifications of the lighting system will be defined based on state of the art literature and fundamental research based on small scaled experiments. While making choices during the design (of the experiment), total costs of ownership will be taken into account. The ‘Dynamic Lighting’ concept will be materialized (hardware and software) which will result in a proof of principle. All will be performed in close cooperation with the SRP SLS. An ‘alpha’ test will be performed in the laboratory before going to the proof of principle phase in 2014. The field experiment is designed. A test plan will be drawn up. Preparations for the field test in 2014 are made. To date, there are a lot of different methods available to calculate the total costs of ownership of a lighting system. These methods all provide different results. A common or generic method for TCO is lacking. Also, sustainability becomes more and more a key performance indicator when a lighting system is considered. However, there is no model or method available that can provide an integrated overview of total costs of ownership and the impact on sustainability. Improvement of SSL systems: Define a test bed, define appropriate measurement procedures and instrumentation and execute experiments with different elevated loading regimes; to a) provide data for validation of the theoretical work and b) identify failure modes that may be induced due to interaction of the different components. As LED’s are more electronics based, the electrical design has high attention. A better balance between optical, electrical, thermal, and mechanical design, satisfying many other conditions (chemical, moist, UV, …) has to be established. Fundamental steps are being made in cooperation with TU/e (Group Ivo Adan). These methods are then “translated” in industrial approaches. In a separate project called Bright Light research was planned on the following generic problem: commissioning the system of current smart lighting system is an extensive job performed by specialists. Also the options for optimum personalized light planning are limited. Two objectives were to be investigated: The first objective was to design a technical concept for an adaptive lighting environment; primarily consisting of a sensor network, data management, actuators and controls and making use of (new) light sources and blinds and screens without any concession on scalability. It should furthermore be able to (re)configure fully autonomously, adjust appropriately to the needs of multiple users, plug ‘n play, bring light when and where needed, save more than 30% energy compared to ‘traditional systems’ and has to be suitable/flexible for application in new and retro-fit applications. The second objective was to demonstrate the concept in a (demonstration) environment for indoor (office) and outdoor (road) situations.

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A further separate project the newly started EU project Accus aims at three innovations: • Provide an integration and coordination platform for urban systems to build

applications across urban systems. • Provide an adaptive and cooperative control architecture and corresponding

algorithms for urban subsystems in order to optimize their combined performance.

• Provide general methodologies and tools for creating real-time collaborative applications for systems.

3.3 Results 2013

Human Centric Lighting Solutions The SRP HCLS started in Q1 2013 with two partners on board. The goal for Q1 was to define and script an use case (based on a car park scenario) to develop a dynamic lighting solution by means of interactive stakeholder workshops in which the necessary functionalities and functional specifications of the lighting solution were inventoried and described. The results of the stakeholder sessions were to frame the inventory of a state of the art research/literature on relevant topics that was scheduled in Q2. However, the interactive stakeholder workshop could take place no earlier than July 2013. Therefore as preliminary work: a document was prepared on the methods and techniques to obtain data for relevant parameters, statistically based data from participants and the external factors that have to be taken into account when studying a (indoor or outdoor) lighting concept in a field test. This report (Measuring the impact of environmental studies on human behaviour in public spaces. Practical guide for a field study) serves as an underlay for the actual design of the lighting concept and the design of the experiment to test the concept in practise in order to demonstrate the functioning of the concept. In Q2, two meetings with intended lead user Q-park were set up to inform them about the program, to formulate the hypothesis that would be tested and to set up the contours of the use case. Also preparations were made for the interactive stakeholder workshop that took place in Q3. In Q2 and Q3, also exploratory talks took place with intended lead users and the state of the art in relevant literature was studied in order to define the necessary threshold levels of relevant key performance indicators like illuminance level, uniformity and responding time of system. The review shows that there is very little research done on the topic of enhancing perceived safety and comfort while saving energy at the same time. In Q3, possibilities for implementation in four Dutch Q-park parking garages were studied and one was selected. In close cooperation with the SLS SRP, the lighting concept was developed and materialized. Lab experiments were set up to give information on the size of the activity spot, required light levels and uniformity and the definition of the gradual decrease of the light levels. Also, with the parking garage that will host the field test known, the actual study design was made. Improvement of SSL systems A test system consisting of luminaires, drivers and a controller was composed. The appropriate measurement procedures and instrumentation were developed and applied to the system. Obtained test data were combined with an overview of potential failure modes and their consecutive acceleration models. An FMEA of the test system was executed in cooperation with the partners. The FMEA formed the basis to set up a failure event tree, that is to be implemented in systems reliability software. A failure tree data set from previous projects was used (CSSL/ESiP) for verification. The failure tree of the test systems will be implemented in 2014.

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A scaling tool for linear luminaires, based on LEDNED’s EasyLine, was developed. A similar tool for controllers is under investigation. The base ingredients for a “mission profile”, i.e., the full scope of possible loadings, were defined. In literature, standard and norms the different loading aspects were investigated. Based on the mission profile definition (to be finalized soon) and the investigations we can now support our partners in defining the appropriate loading profiles for their systems. Smart Lighting Systems A comprehensive state of the art document with 42 networked lighting systems was compiled including detailed view on a) the application area (use); b) system maturity (technology) and c) level of autonomy (smartness of the system). A detailed Technology Roadmap was built for the 4 focus area’s: Detection for Lighting, Data Fusion for Lighting, System Architecture & Platform Development and Quality of Light to be able to start the research work establishing the first generation technology projects in a structured way. A detailed requirement document for the future System Architecture has been made to develop the distributed lighting system solution for Q-Park and beyond. Test of several sensor types has been executed on a parking site to detect and characterize if the objects are a car or a person enabling dedicated light planning for the objects. A broad wireless communication test has been executed to verify multiple nodes can operate in a relative small area without delay and loss of communication influencing the light planning. And finally a simulation tool has been developed to do effective tracking and light planning using different sensors and light sources which can be done both real time as for reproducing occurred situations. In the separate Lighting project a first step in an inventory of available tools an methods was performed. The inventory shows there are a lot of different methods and tools available to calculate a ‘total costs of ownership’ of a lighting system. Two more generic and well used models can be identified and were reviewed further: ‘Rekenhulp Openbare Verlichting Agentschap NL’ and ‘LCC by BOO tool’. Based on this review the improved cost of ownership model developed in this project will be the first (national/European) model that will be supported by relevant stakeholders and that will give improved insight in relevant actual costs of ownership and the impact on sustainability of a lighting system in different application areas. It can be used as instrument to optimize the engineering process by bringing the (required) strengths and opportunities of the system to light.

3.4 Cooperation

The following knowledge institutes cooperate in the Snellius Program: Vito, KU Leuven and TU Delft. The following industrial partners cooperate in the program: LedNed, Maiken, DCD and Sense OS. In the EU projects in the Lighting Program TNO closely cooperate with the partners Philips, Valopaa, Besi/Fico, City Of Eindhoven and Thales. TNO is part of the Roadmap Team for the Topsector HTSM and contributes to the update of the present Roadmap.

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4 Program Printing and Additive Manufacturing

4.1 Introduction

With respect to manufacturing, we aim at new technologies covered by the technical term Additive Manufacturing (AM), more popularly known as 3D printing. We aim at enabling the aplication of AM technologies as a production technology, by the development of AM based, high end, flexible production systems. The use of these technologies opens a vast window of opportunities, unimaginable to establish with traditional manufacturing principles. For instance the freedom of design, personalization of products and local production sites with on demand production. Nevertheless, commercially available AM processes are mainly seen as a fast method to create visual prototypes. Positively, the awareness of the potential of additive manufacturing is boosted by early adaptors placing the first pioneering direct manufactured products on the market. The drivers for acceptance of the technology in a production environment are evident, with a continuously existing demand for improvement. Production costs should be low and production speed should be as high as possible, products become increasingly complex without compromising reliability. To make AM an attractive need-to-have tool in modern manufacturing, for example in high-tech industry value chain with suppliers and OEM companies, the following challenges need to be addressed: • Improved equipment performance by increasing manufacturing speed, increasing the build/product volume and size, increasing the object resolution (feature size), improving the surface quality and guaranteeing material performance and specifications (required material properties). • Extending the portfolio of materials towards high-tech plastics, ceramics, metals and hybrid materials; increased strength and durability (ceramics, metal), compatibility with other materials (biomedical, biocompatible, electronic components), multi-material printing and direct printing of conductive tracks and functionalities like sensors or actuators. • Incorporation of technology in the manufacturing chain; pre- and post-processing, industrial standards, reliability, integration with pick and place technology of components, and the introduction of design for function at the start of product development. To develop AM into a mature manufacturing technology for high-tech applications, mid-to-long term developments along the axis of process capabilities (in particular with new materials and advanced technologies), process control (with in line monitoring and advanced printing strategies) and advanced design (for light and stiff or functional designs) are required. This development space is given in figure 1 and represents the core of SRP Penrose. The research activities in Penrose can be visualized in a development space for the next years, see figure 1, with new process capabilities; process control and advanced design along the three axes.

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Figure 1 Penrose Development space In a horizontal plane the playing field is enlarged for instance by the development of processes for more than one material in a product or by improving process control leading to a higher yield. Design capabilities are used to develop new products. In this way a cross fertilization is enabled: technologies developed in the horizontal plane will lead to a technology push, resulting in new designs; while products developed along the vertical axis will result in a market pull leading to further manufacturing technology development. Directly related to topics and goals mentioned for the Roadmap Mechatronics and Manufacturing, the activities at TNO contributing to the Printing Roadmap of the Topsector HTSM aim at achieving market readiness for Additive Manufacturing (AM). We thereby address the application domain “3D Printing & Additive Manufacturing”, all subjects classified as technological challenges and the priorities “Printheads & functional materials” and “Print Platform Architectures” as mentioned in the Roadmap document. Printing (EU projects APPLE, ROPAS) APPLE: Creating added value and new business for the paper industry. The project focuses on the development of new functional materials (paper, fibers, inks), new functional components (battery, sensors, display, memory) and innovative, flexible and cost-effective manufacturing processes based on printing and embedding techniques for the integration of all these functional components on the smart paper substrate. The APPLE products make extended use of the specific properties of both fiber based products and (nano)fibers individually. TNO creates temperature sensors and H2S sensors to create added value to the paper. ROPAS integrates electronics on paper by printing (Printed electronics, PE) to create added value to paper. Also ROPAS creates demonstrators by integration of sensors on the paper. The sensors foreseen are a pressure sensitive switch, a humidity and a temperature sensor. The demonstrators are: security tag, smart label for anti-counterfeiting and environmental monitoring and track and trace envelope. Paper makes the product affordable and recyclable, electronic components should be integrated on the paper.

4.2 Program 2013

Additive Manufacturing (SRP Penrose and EU projects): • To develop AM into a mature manufacturing technology for high-tech applications, mid-to-long term developments along the axis of process capabilities

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(in particular with new materials and advanced technologies), process control (with in line monitoring and advanced printing strategies) and advanced design (for light and stiff or functional designs) are required. • Develop new material capabilities: Vat photo-polymerization for dentures (cofi project with Vertex), translucent alumina parts for burners in HID lighting (cofi with Philips Lighting) and piezo transducers for use in medical ultrasound applications (cofi with Boston Scientific and Oldelft). • To develop additive manufacturing, in line control and integration technologies for next generation (hybrid) manufacturing. Following program and project activities related to these goals were envisaged: Kick-off Penrose SRP Program, definition of program lines, roadmapping, selection of strategic partners, workplan activities. Further development of baseline for ceramic printing. Finalization of the cofi projects on Al2O3 printing (with Philips Lighting) and piezo materials (with Boston Scientific and Oldelft). All technical objectives of the US probe 3D printing project and the AM of Al2O3 project were realized in 2012. Execution of the cofi project with Vertex on the development of resins for additive manufacturing via photo-polymerization of dental prostheses and implants. Requirement specifications for the next generation PrintValley platform (Hyproline), integration of commercial print head systems for continuous printing. Developing a methodology for defining Key Technology Challenges KTCs with 2D and 3D digital printing technology. Draft Roadmap for Digital Fabrication. Printing (EU projects APPLE, ROPAS) APPLE: Create H2S measurement set up, create Cu complexes, verify reaction of Cu with H2S, create printing ink, create sensor set up (electronic design), create temperature measurement set up, create NTC thermistors, verify α, create printing ink, create sensor set up (electronic design). ROPAS: In 2013, focus of the ROPAS project was to integrate components in the demonstrators. No actively develops and uses the printed materials/components developed in the previous periods. The components are battery, antenna and sensor switch, which are printed on a modified paper surface. The demonstrators are a security tag (electrically activated sensor with LED communication), smart label (electrically activated humidity and temperature sensor with electronic display) and wireless envelop with electronically activated pressure switch. In the table each demonstrator idea is displayed from print use case to electronic scheme to print- plate product and standard component attachment. TNO is responsible for: 1) The development of the electronically activated sensor switch. Thereto conductive chemicals are encapsulated using the encapsulating printer. The development of the electronic switch was foreseen to be developed in 2012, but was not successful. New switches are foreseen by embossing the paper. Also humidity sensors are created by printing PI and temperature sensors by printing Fe2CuO4. 2) Inventorying of chip integrating methods to paper using conductive adhesives. 3) Concept validation. 4) Flash curing on paper.

4.3 Results 2013

Late 2012, the scope of the Shared Research Program Penrose was defined. In 2013, the technical annexes with technical scope and market studies were generated. The collaboration with ITRI, including the definition of a metal print tool,

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was established. Within this collaboration, a work plan was delivered and the specification for the laser print tool was generated (tool to be built by ITRI). The two projects on ceramics did not continue to the next phase because of strategic choices within Philips PLU (AM Al2O3) and Boston Scientific (US Probe 3D printing). Baseline processes for Vat photo-polymerization ceramic slurries were established, both for Al2O3 and piezo materials. Both projects did not continue to the next phase. The first phase of the cofi project with Vertex was successfully executed. Within the project, three resins candidate for dental prostheses and medical implant applications were successfully developed. Recipes for photo-polymerization were developed and tested on the LEPUS 1 print platforms. The developed resins were further evaluated for biocompatibility at Vertex. The first phase cofi was successfully transferred into a multiple year participation in the Penrose Program. The PrintValley platform was further prepared for integration in the Hyproline project, with interfacing to multi-nozzle printing, post-processing and metal parts building. In addition, first metal parts with material from Hoganas and stereolithography were realized, opening new opportunities for the LEPUS technology. Activities at roadmapping and standardization were executed. EU Printing projects APPLE, ROPAS APPLE: A H2S sensor was developed and successfully tested. The sensor on paper was tested for humidity changes for a reference and a loaded (with H2S) situation. In addition, a CuFe2O4 temperature sensor was integrated in the devices and successfully tested. ROPAS: Development of a demonstrator roadmap. A print design was made and printed on paper. Printed demonstrators with integrated components were made. The smart label does not contain all the printed components yet. The temperature sensor however is already in place but not yet integrated. The result of the CuFe2O4temperature sensor was within specifications.

4.4 Cooperation

Collaboration within Penrose started per November 2013 with the partners Schultheiss and Vertex, joint development agreement with ITRI was established in Q2 2013. The collaboration with Vertex in the cofi project was successfully transferred to the participation in the SRP. Partners in APPLE and ROPAS are Varta, CTP, CEA, VTT, Bioage, Labeltech, Polypore, SBA, Océ, MPS, ELEP, Starcke and Enfucell.

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5 Program Healthcare

5.1 Introduction

A Shared Research Program (SRP) for the medical world, based on the open innovation model has started January 1st, 2012. This SRP has the aim to combine public foundations and industrial companies as paying partners but also hospitals, insurance companies and doctors in either research and/or advisory boards. Research will be based on applying optical principles and for medical applications. TNO’s excellence in optical technologies makes her the ideal candidate to start such an initiative and gives confidence in future success. The SRP follows a matrix structure with technical programs (TPs) developing generic research platforms and technical integration program (TIPs) integrating the TP results according to the needs of a specific application. The matrix structure can be seen below with, currently three TPs and two TIPs.

The van ‘t Hoff Program is a collaborative research program amongst industry, government, and non-profit foundations. The aim of the van ‘t Hoff Program is to enhance medical diagnosis and therapy by means of optical and spectroscopic approaches to develop medical applications for biological tissue recognition and human fluid component analysis. This will result in technology that enables less invasive surgical procedures, better screening of diseases in asymptomatic stages and better and/or personalized treatment for dialyses patients, leading to reduced healthcare costs and improved healthcare. For instance, during haemodialysis an optical sensor will measure the amount of sodium, potassium and calcium (electrolytes) present in the cleansing fluid of an artificial kidney. This kind of optical electrolyte sensor is crucial in the realisation of a portable artificial kidney that contains only a few litres of rinsing fluid that is reused during dialysis. So it is essential for the amount of sodium, potassium and calcium to be constantly measured during the dialysis so that the procedure can be adjusted to the excess or lack of electrolytes. Currently it is not possible to measure during the dialysis, only retrospectively. TNO is initiator of the program and collaborates with Dutch health foundations such as the Kidney Foundation, Diabetes Foundation, Alzheimer’s Foundation, Parkinson Foundation and the Brain Foundation and several industrial partners (such as Tornado Medical Systems Inc.) in the field of optical sensing and diagnostics.

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Although costs for this research are high, many companies are interested and the precompetitive nature makes it very suitable for open innovation wherein risks, costs, facilities and data are shared between all participants.

5.2 Program 2013

The program has several long term goals: In the “fiber-optic sensor” program the long term goal is to develop a modular fiber-optic sensing platform that allows real time minimally-invasive characterization and identification of relevant tissue structures (e.g. nerves, blood vessels, tumors) through needles and endoscopes. The key challenges are to miniaturize the technologies, reduce the costs, improve the robustness of the technologies with respect to disturbances such as pressure, bleeding, and movement artefacts, and to develop tissue recognition algorithms (target: 80% confidence, depending on application) based on robust clinical data. As part of the technical integration program ‘Fluids’ the ‘Neurodegenerative Disease’ program in the long term goal aims to develop a simple screening technology for safe, accurate and cost-effective diagnosis and monitoring of neurodegenerative diseases (e.g. Alzheimer’s disease, Parkinson’s Disease). The key challenges in this program are: identification of biomarkers or biomarker signatures for neurodegenerative diseases (for early diagnosis and for monitoring progression) and development of optical technologies for detection and analyses of the identified biomarkers in cerebrospinal fluid and blood. In the “non- and minimally-invasive glucose measurement” program the long term goal is to develop a commercially available non- or minimally-invasive glucose sensor. The key challenges are: to achieve a clinically acceptable accuracy and reliability [A/B zone of Clarke Error grid; 0,5 mmol/l]. A specific challenge is to achieve a sufficiently high specificity with respect to other blood components. To reach our goals we will focus on technology assessment and hardware optimization combined with state-of-the-art signal processing. In the “selective ion measurement in dialysate” program the goal is to develop a miniaturised selective ion sensor for sodium, potassium and calcium that can be integrated in a portable kidney and has sufficient accuracy to validate reuse of dialysate. The key challenges we face are developing a sensor with sufficient accuracy for reuse of spent dialysate and of portable size; the accuracy on normal sized sensors is now 5%, which is sufficient, but miniaturizing the sensor may substantially decrease the accuracy. Furthermore, the clinical value of selective ion measurements in dialysate needs to be established. In the “surgical imaging” program our long term goal is to develop a hyperspectral imaging device that allows wide-field real time imaging and identification of relevant tissue structures (nerves, vessels, tumour borders) during surgery and other medical procedures. Key challenges are: development of tissue recognition algorithms capable of >50% confidence level, improve signal-to-noise ratio to characterize and locate tissue structures (also in depth), reliably identify borders of tissue structures with low endogenous contrast and/or embedded under diffuse tissue layers (>3mm thick) within a distance of 30% of the width of the structure and the development of a fast

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(video-rate >15fps) hyperspectral spatial frequency domain imaging device. The wavelength range that is most promising for tissue structure recognition needs to be investigated in a clinical setting. If that range turns out to be above wavelengths of 1000 nm, Silicon based detectors that are currently used in the state-of-the-art are not suitable and different detectors (e.g. based on InGaAs) must be exploited, which will pose new challenges on signal and image processing.

5.3 Results 2013

In the “fiber-optic sensor” program user requirements research and documents for specific cases and benchmarks i.e. CSF and breast cancer have been made. Analytical models for light transport in tissue were developed based on the diffusion approximation to the radiative transfer equation and a multi-fiber setup with automated position scanning was developed. Testing on liquid phantoms to investigate the applicability of diffusion approximation based models is in progress. In the “Neurodegenerative Disease” program the feasibility of optical detection of specific biomarkers (proteins) for Alzheimer’s disease was explored with various techniques (RAMAN, NIR, fluorescence spectroscopy and ring resonator (RR) technology). RR technology shows promising results, other tested methods appear to have insufficient specificity for low concentration protein detection in a complex matrix. CSF samples of Parkinson disease patients were collected and first attempts with FTIR measurements were performed. The results are promising, but no conclusive results have been obtained yet. In the “non- and minimally-invasive glucose measurement” program, user requirements for non- and minimally-invasive glucose measurements were obtained based on requirements from users and experts combined with official regulatory guidelines. Analysis of error sources for glucose measurements has been performed: sources are identified, but quantification still needs to be done; specific hardware/software solutions need to be chosen first. A pulsating phantom setup was built that can be used for dynamic in vitro measurements, e.g. for absorption spectroscopy measurements.

Ideas for implementation of non-invasive sensor:

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In the “selective ion measurement in dialysate” program, the principle of measuring ions selectively in dialysate has been proven, specification for a Functional Model (FuMo) have been determined, the optical device was composed which was delayed a month due to ordering problems. Sodium, potassium and calcium in correct concentrations were measured with validated concentrations and accuracy.

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6 Program High-Tech Materials

6.1 Introduction

The development of advanced materials and their application can be accelerated with predictive methods for relevant material structures and properties in relation to the relevant processing routes. Multi-scale modelling of materials is a major materials science field that attracts interest from academia, R&D laboratories and industries. This field promotes the development of predictive materials research tools to understand the structure and properties of materials at all scales. The field also strives to use these predictive tools to design and process materials with novel properties. Multi-scale modelling also allows the analysis of structures made with advanced materials whose behaviour in all environments may not yet be known. By its very nature, the field of multi-scale modelling of materials transcends the boundaries between materials science, mechanics, and physics and chemistry of materials. At present, the knowledge on multi-scale material modelling for different material classes and the industrial use of these predictive tools, e.g. in combination with geometrical optimisation like DFT, MD, meso/nano, continuum and device level are not common goods within TNO. As the academic use of multi-scale material modelling techniques has matured in the last decade within Dutch organisations having a strong academic position in multi-scale modelling (3TU, AMOLF), the time is there to absorb these techniques into TNO for industrial application and to expand their use in TNO, towards groups that are already working on systems and devices. By the nature of materials the multi-scale domain interacts with the multi-physics domain. Although in the mechanical world the use and benefits of multi-scale techniques are obvious, i.e., the strength of structures is determined by the weakest link at the material level, more functions are integrated into one structure. E.g., certain parts in high-tech machines should not only be light weight and strong, but also efficient in the heat management. This requires different “layers” of physics in the multi-scale approaches. The transitions of the scales may be different for the different physical parameters, which puts additional challenges to finding unified approaches. It is foreseen that multiple solution “routes” may exist or must be employed to keep it computationally efficient. At TNO the aim is to develop know-how in the field of multi-scale materials modeling to bridge the gap between fundamental modeling expertise and advanced materials and device development. The developed new knowledge should be exemplified by cases that prove that TNO has added value in bridging this gap, preferably in cooperation with other stakeholders in the particular material field, such as Dutch academia (modeling) and at a later stage customers (materials and devices).

6.2 Program 2013

Toxicology and sensors The focus is on molecular mechanics and molecular dynamics at the Angstrom-nanometer scale, concerning molecules in their environment. After the initial setup of models and gain of experience, the following cases will be investigated: development of predictive QSAR and/or classification models for a specific

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biological outcome. An illustrative example is shown below, displaying the clustering of structurally similar compounds in order to predict structure-related toxicity.

The development of nano-specific descriptors, and predictive QSAR and QSPR (p for properties) are studied with the aim to use them in the context of safe design, risk assessment and integrated testing strategies. An illustrative example is shown below, showing a graphical view of calculated toxicity of nanoparticle.

Core This work aims at creating a better understanding of the relation between the macroscopic functional properties and the intrinsic microscopic material and interface properties. The object and structures are on a millimeter to centimeter scale, but materials properties on a micrometer level determine the ultimate capabilities. In 2012 the focus was on mechanical (ultimate) properties and stiffness optimization. In 2012 a CORE model has been established to facilitate a single interface for all four interested work packages. The CORE model will be used in 2013 to get a better understanding of the mechanical properties, link the theory with experimental demonstrators and ultimately predict properties and design the materials system. Asphalt This year the attention for asphalt modeling was focused on introducing the thermo-mechanical aspects on the asphalt mortar scale that are responsible for the actual asphalt performance. Microstructures of asphalt are highly dependent on the

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specific components and their correlations/interaction with other parameters. This makes studying the microstructure very complex and makes it hard to study due to the difficulty of isolating certain parameters. Therefore, for this year’s demonstrator, a more constructed microstructure was conceived. Ballistic Future materials for ballistic protection must be 20 – 50% lighter and multi threat resistant. To meet these requirements new materials have to be designed and produced. The developments in material technology offer the possibilities to engineer the material structure to obtain the required material properties. Key is the modification of the material structure and properties at the smaller length scale (nano, micro, meso) and control the interaction with and effect on the larger length scale. Which means that for ballistic impact the response and the damage development in the material have to be controlled from the micro length scale up to the macro scale, so the bulk performance can be related to micro structure. Experimental and computational tools are needed to design the optimal geometry and properties at the micro-level to meet the macroscopic requirements. To provide ballistic protection a range of load conditions have to be resisted. Starting at the shock loads dominated by hydrostatic stresses in the order of GPa’s leading to failure and disintegration of the material, but still confined by the surrounding material. Then, the induced stress waves expand, the amplitude reduces and at some distance the material strength and properties become relevant. The response and failure modes occur due to dynamic stress conditions and the dynamic material properties at the various stages mentioned. Weight reduction as well as increased performance at reasonable costs are the goals of international ballistic R&D. Very promising are the development in nano-structured materials, functionally graded materials and hybrid material concepts. TNO decided to invest in the design and development of advanced armour ceramics, i.e. the design of the micro-structure, as well as the diagnostic and modeling techniques to analyze the ballistic performance and support the design of new materials and material concepts. In order to focus the research, it was decided to invest no research effort on production techniques in 2013. In the CMS project the research effort is on the mechanical response of the ceramic microstructure as well as the macro response at ballistic impact. The scheme of the ballistic work package is given in the figure below with focus on computational research embedded in experimental research. The latter is mainly performed in the program of the market theme Force Protection. Additional tests to fill the gaps are part of the CMS project while diagnostic techniques are part of the ETP 2013 Materials Program. Steel As ferritic steel moves from room temperature to lower temperatures, it undergoes a strong transition from failing in a safe (ductile) way to a brittle (cleavage) failure mode. This brittle failure mechanism is responsible for some high profile historical disasters like the Titanic and the Liberty Ships (see below), but it continues to claim steel structures (including but not limited to maritime and offshore applications) even today. Steels are designed to prevent cleavage fracture, but steel makers lack basic understanding about what microstructural features to choose in order to prevent cleavage fracture. For example, the effect of prior austenite grain size on cleavage is not known. At the same time, rules have been designed to prevent cleavage fracture, but they are based on empirical fits and historical experience, so they are decreasingly relevant to the steels that are being developed today. A new understanding of cleavage fracture is necessary to move to the next level of modeling cleavage fracture of steel.

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From prior studies, it is well-known that cleavage is a multi-part process, initiating with dislocation pileup at carbides, carbide cracking (size on the order of 10-8 to 10-6 m), then a sudden crack running through the adjacent grains (size on the order of 10-7 to 10-8 m) (see below). Another important factor is the likelihood of a crack overcoming the boundary of the adjacent grain. Current models take these factors into effect when creating a phenomenological model of cleavage fracture based on a limited state of parameters (affected volume, first principal stress). However, it is appearing increasingly frequently in the literature that additional parameters (e.g. far-field plastic strain, stress triaxiality) must be included. However, the relationships are not well understood. This gives a problem for performing macro-level simulations or for creating new rules.

To answer the above basic questions, CMS-steel is interested in creating an RVE of the steel microstructure to understand how stresses drive the probability of fracture in carbides.

6.3 Results 2013

Toxicology and sensors A predictive model was built for the OATP1B1 transporter, which is of importance for drug-drug interactions and the therapeutic window of a drug. Inhibition data were measured for 640 drugs by Kinetics in research for food and pharma (TNO, Zeist). The corresponding structural data of the investigated compounds was mined from public data. Subsequently, a set of molecular properties of each compound was calculated with the software package Pipeline Pilot. The dataset was divided in a training and a test set. The former was used to build a Bayesian model that predicts 1OATP1B1 inhibition by correlating molecular properties and biological data. The latter was used to internally validate the model. Validation was subsequently performed with an external dataset of 32 drugs mined from the literature. The performance of the model was assessed by the ROC score, and was > 0.89 for each of the datasets (training and test). Thus a satisfactory prediction model was made.

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Four mechanistic models were developed for profiling the potential biological and toxicological effects of oxide nano-materials. The models describe the reactivity, protein adsorption, membrane adhesion and bio-persistence processes of a large range of oxide materials and are based on properties either calculated from experimental data or obtained by statistical regression methods. The information provided can be used to describe and predict the molecular initiating events that can lead to different toxicity and fate profiles of nano-materials. The theoretical framework underlying each model and its predictions are discussed and evaluated in relation to experimental data. It is suggested to use this information collectively with in vitro models in a weight-of-evidence approach to hazard assessment. Core Microstructural representative volume elements (RVEs) are at the heart of many homogenization schemes. An RVE is a model of a material microstructure on which a “virtual experiment” is performed in order to resolve its effective material behavior. The RVE needs to be sufficiently large to accurately determine overall mechanical or physical properties. Moreover, if particular corresponding microstructural phenomena, e.g. microstructural evolution, are of interest, the RVE should also be representative with respect to particular (evolving) microfields as well. The generation of these RVEs sometimes can be challenging and time consuming task. Also the definition of a proper RVE requires multi-disciplinary expertise. At the moment RVE models on geometry generation, interface modelling in heterogeneous materials, kinematical constraints imposed on microstructures have been successfully obtained. Asphalt Based on the CORE script the suggested morphology, with elastic particles (filler/sand particles) and the binder’s micro-phases, can be generated such that a wide distribution of particles can be implemented in the bitumen microstructure. The included mineral particles (partly) substitute one of the binder phases (peri- and perpetua phase).Subsequently the mastic morphology can be generated as function of temperature (binder effect) and filler particle concentration, sizes and distributions. Hence different morphologies can be generated as function of particle sizes, size distribution and temperature. Ballistic The aim of the CMS-ballistic work package is to enable and support material optimization. Parallel to the CMS work layered and graded ceramic armours are developed within the program of the TNO theme Force Protection (FP). To enhance the cooperation between the mainly experimental FP research and support the armour development research, the gained CMS knowledge was applied in a model for ballistic impact on layered systems. The model helps to analyze the dependency of the ballistic response on the material model parameters. General trends are obtained. However, the available material data is insufficient for the elementary input parameters required for the material. A basic, generic problem for many advanced material models. Within the ballistic work package, the general trends for the ballistic response of layered systems has been analyzed. Furthermore, the standardized indentation test was modeled using the advanced material model, in order to study the possibilities to derive the model parameters by inverse engineering from test data. These preliminary CMS results will be used to support the FP research on graded armour systems scheduled for 2014. A PhD project has been defined on ceramics to relate elementary macro model material parameters to experimental data and the relation with the ceramic micro structure. The project has been granted.

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Steel Cleavage fracture of steel is governed by the behavior of microscopic particles that are approximately one micron in diameter. A number of methods of analyzing them on the meso-scale exist, but these are encountering increasing difficulties. This work package aims to use microstructural modeling to serve two goals: Understand the effects of steel microstructure on the cleavage failure mode and better model the cleavage failure mode on the meso-scale. The first goal reflects the fact that there a number of micro scale parameters that affect fracture mechanical behavior that material manufacturers and control in their process, yet don’t yet know what is desirable. This work package would help material and weld process designers to understand what a good target microstructure is to achieve their fracture requirements. The second goal will help designers and analysts to design better structures by giving them more accurate models that are applicable on the meso-scale. Both of these goals will be answered with just one end deliverable: an equation that relates the various microstructural quantities and far-field stress state to the cleavage failure probability of a steel at low temperatures. The overarching approach to creating the above stated deliverable is to create an RVE of the microstructure, then subject it to a number of different conditions to find out the fundamental response of the microstructure is to loading. The ability to review the RVE and find localized stress concentrations will give new insight into the cleavage failure mode that has historically not been available. This overarching approach has been executed in various phases of CMS. In CMS 2012, an RVE of sub-structure was developed based on micro-scale observations and measurements on a real steel of interest to the offshore and maritime industry. In 2013, the RVE will be exercised in a more rigorous and systematic way. If existing phenomenological models are not able to capture the behavior demonstrated by the RVE, then a new one will be given. If 3-D RVE’s are supported by the CORE, then the 2-D RVE of 2012 will be extended into 3-D. (Note that this will require additional scientific developments to generalize inherently 2-D observations, such as SEM micrographs into 3-D extrapolations). If supported by the CORE, the RVE will also be updated to include sub-grain Martensite islands, especially lathe structures. The demonstrator tasks for the steel RVE are planned for a time after 2013.

6.4 Cooperation

The EU projects Photosens and Insight are connected to the Materials Program. In Photosens where the goal is to develop a multi-parameter sensor platform, we work together with VTT, University of Southampton, Momentive and Nanocomp. In Insight, where the goal is to obtain information of size, distribution, chemical composition engineered nanoparticles which are synthesized in dispersion in coatings, we work together with INM and 6 SME companies.