INFM-Istituto Nazionale per la Fisica della Materia


Programme for Research and Technological Development in the Field of Industrial
and Material Technologies


Thematic Network

"NANOPOWDERS: PREPARATION AND PROCESSING" (NANOMAT)

Proposal N o
BET2-592
Project Coordinator:
Istituto Nazionale per la Fisica della Materia (INFM)-IT

PARTICIPANTS:
Belgian Ceramic Research Centre (BCRC)-BE
Dept. of Materials Engineering at the Technical University of Clausthal (IWW)-DE
Commissariat a l'Energie Atomique (CEA)-F
Vlaamse Instelling voor Technologisch Onderzoek (VITO) -BE
Laboratoire de Chimie des Plasmas Universite' de Limoges (ULIMO)-F
Laboratoire d'Etudes et de Recherches sur les Materiaux (LERMAT)-F
Ist. di Ricerca suTecnologie Ceramiche-Consiglio Naz. delle Ricerche (IRTEC-CNR)-IT
Technical University of Wien (UWIEN) AT
Materials Ireland, Joint Coating&Ceramics Research Centre (JCCRC) -IE
Interdisciplinary Research Centre at the Univ. of Birmingham (IRC)-GB
Materials Ireland Research Centre at the Univ. of Limerick (ULIMK)-IE
Dept. of Material Science at the Technical University of Freiberg (BAF)-DE
Ente per le Nuove Tecnologie, l'Energia e l'Ambiente (ENEA)-IT
Morgan Materials Technology LTD (MMT)-GB
Rolls Royce plc(RR)-GB
Metalloceramica Vanzetti S.p.A.(MCV) IT
NeoCeram S.A. BE
Gel Design&Engineering (GDE) IT
L'Air Liquide S.A. F
Howmedica Int. Inc. (HOW) IE

TECHNICAL INTRODUCTION

          Recently, increasing interest has focused on nanostructured materials, which are materials composed of structural units with a size scale below 100 nm, with the hope that their properties could be superior to conventional materials having a phase or grain structure on a coarser size scale. This interest has been stimulated by the possibility of synthesizing a huge variety of one-dimesional (multi-layered materials), bi-dimensional (porous silicon pillars...), and three-dimensional nanostructures (atom clusters in the nanometer size) of interest not only from a fundamental point of view but also with respect to technological issues. Scientific interest is primarily motivated by the possibility of exploring totally new phenomena such as visible emission from silicon nanostructures or transparency in opaque ceramics, whereas the availability of a novel class of materials with properties mainly determined by the tremendously high surface/volume ratio offers the possibility of applications ranging from the field of new catalysts to the fabrication of ceramic nanocomposites with significant property improvement.

          A key target in ceramic research for several decades has been the identification and assessment of methods for improving fracture toughness, ie for avoiding the problems created by sudden brittle failure, which still hinder wider application of ceramic materials. Ceramics have of course won an important market segment as functional components (electronic ceramics, gas sensors..), but a breaktrough into widespread and general use in engineering such as heat engine parts, heat exchangers, fuel cell components will be permitted only by cost effective solutions of the mechanical reliability problem. It is in this context that claims for ceramic nanocomposites with improved mechanical properties at high temperature have been advanced by Prof. K. Niihara of Osaka University (Japan). By his definition, nanocomposites are ceramic materials fabricated by dispersion of nanosized particles within micro-sized matrix grains or at the grain boundaries of the matrix, whereas nano-nanocomposites are formed when also matrix grains are in the nanosize scale. A significant increase in strength (over 1 GPa) and fracture toughness (from 3.25 to 4.70 MPa.m1/2) was reported as resulting from addition of SiC nanoparticles (5vol%) to a microsized Al2O3 matrix, whereas superplastic behavior (that is an exceptionally large tensile elongation during stretching) was observed in SiC/Si3N4 nano-nanocomposites at 1600 °C. In any event, little is known on the specific processing routes used for the fabrication of such composites and, in spite of the impressive results reported by Prof. K. Niihara, it appears that no-one has currently reproduced them. Moreover, the mechanisms behind the strengthening and toughening of nano-composites are not fully understood.

          It is commonly accepted that the starting powder is of critical importance for the fabrication of most advanced ceramic components, with improved thermomechanical properties and reliability as well as reproducible behavior. In the last few years, several new powder synthesis techniques have been developed as alternatives to established methods. A recent development is the availability of chemically pure, nano-sized powders with a narrow size distribution. These materials have proved difficult to handle and densify by use of conventional processing routes and densification methods. Many technical and business issues (including proper packaging and handling, processing powders into components, and high cost) must be resolved before nano-sized powders can be used in commercial applications. Also environmental and health related issues in the production of nano-powders have not yet been assessed.

          In summary, at the present point in time, it is commonly accepted that nanostructured materials are very interesting from a scientific point of view and potentially attractive for applications, but there is a stalemate in their development at industrial level for the following reasons:

- there is a lack of technology in handling and processing nanopowders, so that the fabricated materials show a very fine microstructure, but the mechanical properties are still well below the potential values;

- the cost of fabricating bulk nanoscale materials is very high, thus they are uneconomic for industrial use.

          It follows that R&D on nanostructured materials is highly risky for industries and there is the distinct possibility that European companies will be left behind, whilst in the rest of the world (USA and Japan) nanocomposites are currently under study as a promising class of materials and nanosized powders are commercially available.

          The formation of a wide Network on nanopowder production and processing for the fabrication of innovative ceramic materials would open up the possibility of overcoming the present stalemate in the field of nanostructured materials. Today, about 150 research groups are working in Europe in the field of nanomaterials. Their research potential and expertise are not coordinated enough to take full advantage of their complimentary skills. The participation of European industries is modest because of the high investments and long time required for new material development. Shortening of the development and technology transfer time could be reached by focusing the research efforts among European Universities, Research Institutes and Industries either working in the field of nanopowder production and processing or in the use of advanced ceramics, the latter for steering action. The network should be divided in three groups, each with the aim of answering a crucial question:

          Group 1 : Powder producers . Question: Is it possible to produce nanopowders in quantities sufficient for industrial uses at a reasonable price? Goal: Assessment of a cost effective method of nanopowder production for development of a pilot plant on industrial scale.

          Group 2 : Powder processors. Question: Is it possible to develop innovative nano-powder processing and densification routes in order to produce dense, high performance ceramic nanocomposites suitable for advanced engineering applications? Goal: transfer to European industries the technology for high performance ceramic component production starting from nanopowders.

          Group 3 : Experts in powder and/or material characterization. Question: Is there any real and significant improvement in the mechanical properties of nanocomposites and which is the mechanism responsible for it? Goal: stimulation of industrial interest in the production of nanocomposites for advanced applications. Researchers from industries couid either participate actively in research or provide guidance and help in the definition of targets.

          Researchers from industries could either participate actively in research or provide guidance and help in the definition of targets.



1. OBJECTIVES AND STATE OF THE ART

1.1 Importance to industry

          Advanced ceramic materials constitute an emerging technology with a very broad base of current and potential applications and an ever growing list of material compositions. The major applications and market segments can be categorized as follows:

STRUCTURAL CERAMICS

  • Heat Engine Components
  • Cutting Tools
  • Wear-Resistant Parts
  • Energy and Aerospace related industrial applications
  • Bioceramics

ELECTRONIC CERAMICS

  • Insulators, Substrates and IC Packages
  • Piezoelectric Ceramics

Ferrite Magnets

  • Capacitors
  • Superconductors

CERAMIC COATINGS

  • Auto, Diesel & Land-Based Turbine Engines
  • Heat Exchangers
  • Wear Parts
  • Cutting Tool Inserts

          Business Communications Co. has analysed the current and future U.S. markets for advanced ceramics. Table I summarises BCC's estimates of the size of the 1994 and future market potential for the various advanced ceramics market segments in the U.S. Table I : U.S. Markets for Advanced Ceramic Components from 1994-2000.

Table I : U.S. Markets for Advanced Ceramic Components from 1994-2000.
 
1994
($ mil.)
2000
($ mil.)
AAGR*1994-2000(%)
Structural Ceramics
475
1020
13.5
Electronics Ceramics
3864
6573
9.3
Ceramic Coating
525
940
10.2
Total
4864
8533
9.8
* AAGR: Average Annual Growth Rate

          Electronic ceramics hold the largest share of the ceramic powder market, although the largest growth rate is expected to be for the structural ceramics market. In fact, there is an increasing need for materials suitable for structural applications under severe conditions, for new cutting tool materials and for bioceramics.

          For example, materials that are used in oil and gas exploration and production currently experience some of the most aggressive operating conditions. Such materials must operate for long periods of time without failing, where failure can be caused by excessive corrosion, fracture or degradation properties. Valves used where sandy or dirty gases or fluids are pumped can suffer from excessive wear. The cost in repair and maintenance of worn valves, especially in offshore environments, is extremely high. Furthermore, there is an increasing need for materials that can operate under such conditions on sub-sea installations where they can also experience mechanical loading. The costs of repairing sub-sea equipment that has failed prematurely make material reliability in combination with high strength and good wear properties extremely important.

          New cutting tool materials are required by metal-working industries. For improved productivity, industries need higher cutting speeds and greater tool life, to reduce shut-downs for replacing cutting inserts. The typical characteristics required of cutting tools are toughness and failure resistance on one hand, and high temperature hardness and wear resistance on the other. At the moment, cutting tool materials are mostly based on tungsten carbide bonded with cobalt. Such tooling has reached the limit of its potential, and further improvement can come only from new materials. The most innovative of the new generation of cutting tools are those based on ceramic materials, however such materials are more brittle than tungsten carbide and more prone to catastrophic failure. Improvement in their toughness and strength is mandatory to penetrate the market of automotive industry, aerospace industry and steel-working and machinery industries.

          A number of oxide and non-oxide ceramics are finding increasing applications in a range of clinical applications, particularly where the components are subjected to high stresses generated by mechanical loads and severe wear. For instance, alumina is the bioinert material with the longest medical history in load bearing prosthesis replacement. Unfortunately, the scope of the potential clinical uses is limited by a combination of relatively low fracture toughness and strength, which are generic to many ceramics but could be overcome by developing biomedical components on the basis of advanced ceramics.

          The European abrasives industry suffers from competition by American sol-gel abrasives that could be counteracted by the development of better, innovative abrasive materials. The benefit would be great, but the risk is high.

          During the 'explorative phase' of the T.N. NANOMAT, a number of european industrial Companies were consulted and gave their views on the expectations and perspectives for nanostructured ceramic materials.

          Rolls Royce is considering the future of fuel cells in the context of stationary power generation systems, ship and train propulsion. The Solid Oxide Fuel Cell (SOFC) has been identified as the technology which has the widest range of potential stationary power generation applications. In this context, Rolls Royce is developing a supported electrolyte SOFC: the Integrated Planar SOFC (IP- SOFC). This is a thick film device, which relies on the integrity of dense films of zirconia, and other ceramic materials, to separate the fuel and air streams. Improvement in both thermo-mechanical properties and sintering temperature are crucial and could be won by incorporating nanopowders into the SOFC. The role of Rolls Royce in the Network will be as an advisor to the partners. When appropriate, the possibility to transfer relevant nano-technology into Rolls Royce will be discussed.

          Air Liquide S.A. (which is a part of the Air Liquide Group) is interested in highly performing ceramics for solid electrolyte oxygen pumps and mixed conductors. Their objective is the production of large amounts of high purity nanopowders for pilot plants, if it is demonstrated by the Network that there is a real benefit in fabricating components from nanopowders and technical problems (in processing the nano-powders and shaping the components) are solved. The role of the Company in the partnership is as possible advisor and end-user.

NeoCeram is also interested in the development of advanced materials for the production of pump components. In the framework of a joint Project with some partners of the Network NANOMAT, alumina-SiC nanocomposites with higher wear and strength resistance than conventional materials were produced. However, before using nanoceramics in its pilot test devices, NeoCeram needs an answer to key questions on the real possibility either to produce nanopowders at low cost and to assess reliable and economically viable processing methods. It follows that NeoCeram is willing to encourage the set-up of a Network on nanomaterials and is ready to steer the R&D activity.

          MetalloCeramica Vanzetti (MCV) is involved in the development, manufacturing and industrialisation of cutting tools. At the moment, ceramic cutting tools represent only 5% of the total market, due to limitations in toughness of the presently available products; therefore improvements in toughness and increased reliability are needed in order to offering to the market a real alternative to traditional tools and significantly contribute to cost reduction and quality enhancement of cutting operations. MCV was recently involved in a BRITE-EURAM project on the development of nanocomposite ceramic materials for cutting tool applications. This project has demonstrated the technical feasibility of using ultrafine powders for making ceramic cutting tools, however a number of technical issues related to the difficulty in handling and processing nanopowders remain to be solved. Still open problems concern the optimisation of particle size dimension in relation to the binder type, binder introduction and composition, granulation stage. It was established that control of powder properties is crucial and the particle specific surface area should not exceed 30 m2 gr-1, to minimise the difficulties of processing and achieve good quality materials. MCV will probably present a new Project (under the Innovation Programme) on the industrialisation of nanocomposites for cutting tool applications, thus the Company is highly interested in following and steering the activity of a Network devoted to R&D on nanomaterials.

          As an orthopaedic company routinely selling alumina and zirconia heads, Howmedica is committed to the development of new, improved ceramic materials. The Company will take part in the Network as possible end-user of ceramic materials that have better wear properties, higher flexural strength and especially higher fracture toughness than existing ceramic materials.

          Morgan Material Technology (a R&D Company within the Morgan Group) is involved in the development of a wide variety of ceramic materials including toughened oxide materials, non-oxide ceramics and composites. In the Company, there is a wide expertise in sol-gel chemistry and processing, ceramic fabrication, solid and liquid state oxide synthesis, metal and ceramic processing. As an R & D laboratory supporting a major manufacturer of ceramic components, MMT hopes to obtain results from the network which will enable the Company to develop new cost effective products which can be sold profitably. Both directly and via other Companies in the group, MMT has already been involved in, and supported, projects to develop simpler processing routes for alumina / silicon carbide nano-composites and to develop these materials for wear resistant and other applications. However these have not yet resulted in materials which can be produced by routes, and at costs, which are acceptable in the markets so there has been no return on the Company investment. This early work has been disappointing but MMT still believes that nano-structured materials offer great potential so the network is seen as a way to remain involved in a wide variety of research in this area without having to invest large sums of money in projects which from a commercial point of view have a high risk.

          As a result of the above mentioned consultations, it comes out that there is need for the development on-industrial scale of a new class of ceramic materials with improved mechanical and physichemical properties. It has been claimed that nanostructured ceramics exhibit excellent properties (high strength, good creep, wear and corrosion resistance), making them suitable for structural applications under severe conditions, but as yet there have been no fully commercialised products. It would therefore be of great benefit to industry to form a Thematic Network devoted to answering key questions on R&D of nanocomposite materials, e.g. if there are any real benefits in fabricating components from nanopowders and whether economically viable nanopowder production and processing methods are available.



1.2 State of the art


          Ceramic nanocomposites were first developed in Japan, mainly by K. Niihara (Univ. of Osaka) who claimed that ceramic materials with excellent mechanical properties (strength, toughness, creep resistance) can be obtained through nanocomposite technology. Furthermore, it was stated that nano-nanocomposites show potential for superplasticity, that is they exhibit exceptionally large tensile elongation during stretching. In spite of these impressive results, little or few information is available on the specific processing routes (dispersion of nanoparticles, homogenisation, sintering....) used for the fabrication of such kind of composites. Moreover, very little consistent information is available on the reinforcement mechanism of nanocomposites.

          In order to afford R&D on nanocomposite materials, the availability of nanopowders is of critical importance.

Over the last few years, several new technologies have been developed for the production of submicron, ultrapure powders with a narrow size distribution. Nanopowders are generally produced by condensation of precursors (atoms, molecules or clusters) in a supersaturated gas environment. Such precursors are generated by various processes, such as laser ablation of solid targets or plasma or laser-induced decomposition of gas mixtures. Other methods are related to: evaporation-condensation, ball milling (or mechanical alloying), self-propagating high temperature synthesis, sol-gel, spray-drying of solutions, aerosol pyrolysis, chemical vapor condensation at low pressure.

At present some American and Japanese companies can supply developmental quantities of nanopowders:

  • Nanophase Technologies Corp. has developed a gas condensation process to produce different oxide powders (alumina, titania, zirconia);
  • Nanodyne is focused on the production of cobalt-tungsten carbide to make cutting tools and wear resistant devices;
  • Ultram International produces ceramic and composite powders by a super-high-frequency plasma chemical process;
  • MarkeTech International proposes nanosized silicon carbide, silicon nitride, silicon carbonitride, boron carbide and silica powders obtained by a CO2 laser pyrolysis process;
  • Mitsubishi Mining Cement Co. Ltd. has prepared Si/C/N nanocomposite powders from pyrolysis of an organosilicon compound in a furnace.

          In Europe nanopowders are not yet produced on industrial scale, but only on a laboratory scale.

          From the exploratory phase of the Network, it came out that nanopowders are produced in several European Research Laboratories. In the following, the acronyms of Par. 2 will be used to identify the Participants.

          The potential of the laser synthesis process from gas-phase precursors for producing very fine particles (typical diameters <30 nm) of various Si-based materials (SiC, Si3N4, Si/C/N, Si/Ti/C, Si/C/AI....) has been demonstrated by Italian and French research groups (at ENEA-Frascati,lT,and at CEA-Saclay,FR). The rate of production is actually 100 g/h and couid be increased by a factor of ten after scaling-up of the experimentai set-ups. The possibility of using lower cost starting materials (as liquid organometallics or sol-gel precursors) is currently being developed by the CEA group. INFM (through the external services of ICTIMA-CNR as associated partner) could provide new,cost-effective precursors for nano-powder synthesis. Nanoscaled powders are produced at IWW-TU Clausthal by evaporation of different materials with the radiation of a Nd:YAG laser. By use of this process several oxides (Al2O3, ZrO2, CuO, BaTiO3, SnO2), composites as Al2O3/ZrO2 and doped powders (with an average particle size ranging from 14nm to 23nm) can be prepared, but the yield is still low.

          A variety of oxide and non-oxide nanopowders are produced by CO2 laser ablation of solid targets by researchers working at the Univ. of Jena and BAF- T. U. Freiberg.
          At the Univ. of Limoges, ceramic nanopowders of alumina, zirconia and SiC (with particle size ranging from 50-100 nm) are produced in a twin DC plasma arc.

          These nano-powder synthesis techniques are more expensive than the currently established powder manufacturing methods. It is likely that a surge in the market demand for nanosized ceramic powders will push the development of production methods to become more competitive with conventional production techniques. For example, a cheap SiC nano-powder production process has been recently proposed by BAF-T. U. Freiberg (D). This method is based on the conversion of a sugar and silica sol into silicon carbide by thermal treatment under appropriate and well controlled pressure conditions. A solution to the remaining problems of this method (incomplete conversion of the parent substances at low temperature and coarsening of powder particles at higher temperatures) as well as the development of alternative, low cost processes would certainly be accelerated by a strong industrial demand for cheaper nanopowders. However, at the moment, the availability in Europe of nanopowders in quantities sufficient for making prototype ceramic components is a crucial step to start up the programme:

production of nanopowders in developmental quantities
|
production of nanopowders in developmental quantities
|
assessment of nanopowder handling & processing methods
|
production and characterization of prototype components
|
                              evaluation of the benefits           ->
 no stop the activity
          |    yes
development of cost-effective nanopowder production and processing methods
|
transfer of the technology of nanopowder production & processing to industry


          
If nanocomposite ceramics have to be fabricated on industrial scale, it is mandatory to evaluate economically the different processing and fabrication techniques. The following review of the state of art in the field of nanopowders handling & processing came out from the exploratory phase of the Netwok.

          At the IRTEC/CNR preliminary results have been achieved on hot-pressing of Si/C/N nanopowders produced at the ENEA Research Centre of Frascati. A high degree of densification (up to 98.5 of T.D.) was obtained in spite of the low green density and the sintered samples exhibit a very fine microstructure, but the mechanical properties are still unsatisfactory.

          The Belgian Ceramic Research Centre (BCRC) has been involved in the development of nanoceramics based on commercially available nanosized silicon carbide (SiC) in different matrices (alumina, mullite, silicon nitride, cordierite) selected on the base of their thermal expansion coefficient and of their mechanism of densification (solid state, liquidphase, vitrification). High thermomechanical performance materials were densified by hot-pressing. The rupture strength and toughness were largely higher than those of reference materials (+ 50%). A feature of alumina nano-SiC ceramics is their exceptionnally high creep and wear resistance. At the moment, research is focused on alumina as the matrix with a dispersion of nanosized non oxide particles. In cooperation with the Univ. of Valenciennes (F), research is carried out on nanocomposites where both phases are kept within the nanometer scale. after densification. Nanostructured zirconia-alumina composites were obtained, starting from mixed powders synthesised by a hydrothermal route.

          At VITO, research was carried out on manufacturing SiC- Si3N4 nanocomposites, starting from nanopowders supplied by the CEA group. In accordance with the findings of other Network partners, the main characteristics of the nanopowders obtained by laser synthesis were the strong agglomeration and the tendency to hydrolise when exposed to ambient air. Applying proper processing, the material was pressureless sintered into high density, nearly defect free components.

          Interesting results were obtained at the University of Limerick on the development of alumina matrix nanocomposites for wear applications and abrasive grits applications. The nanocomposites have been fabricated by inexpensive processing (water dispersion, pressureless sintering). In addition, results have been obtained on the fabrication of silicon nitride-silicon carbide nanocomposites using commercial powders, economic (aqueous) processing routes and economic densification techniques (gas pressure sintering).

          The recent ceramic nanocomposite research at the IRC in Materials has been focused on the alumina nano-SiC system processing using pressureless sintering. Data were obtained on nanocomposites based on Alcan RA207LS a-alumina powder (d50 = 0.5 mm) as the matrix material and each of two types of SiC powder. The SiC powders were Lonza UF15 ( 15 m2g-1) and ENEA SiC powder (80 m2g-1). The base alumina was sintered in air, while the nanocomposite materials were sintered in a vacuum furnace under an argon atmosphere at 1900°C for 2 hours. The green compacts were produced by the pressure filtration. The sintered densities were 99.0%TD for the alumina, 98.2%TD for the UF15 nanocomposite and 98.9%TD for the ENEA nanocomposite, with the respective maximum room temperature 4-point flexural strengths being 453 MPa, 404 MPa and 540 MPa. The load-extension behaviour at 1400°C of the UF15 nanocomposite versus that of the base alumina demonstrated that the nanocomposite is much more creep-resistant, with the fall-off in strength at elevated temperatures being less rapid.

          At the Univ. of Wien, results were found on the influence of SiC (nano)particle addition on the mechanical properties of hot-pressed alumina. SiC nanopowders with different grain size (10, 20 and 40 nm) were supplied by ENEA. The main problems encountered in processing and densifying the mixed powders were the difficulty to avoid particle agglomeration and achieve a homogeneous distribution of the nanoparticles in the ceramic matrix.

          In conclusion, the microstructure of sintered nanocomposites were excellent, but the mechanical properties were still unsatisfactory, in many cases.

          The first goal of the Network should be to obtain nanocomposites with improved mechanical properties, the second should be to define cost effective nano-powder production & processing techniques.

The main aspects to be considered for the improvement of processing techniques are:

  • conditioning of nanopowders surface to avoid particle agglomeration
  • development of powder treatment methods for the dispersion of the second phase and for the introduction of sintering aids;
  • development of forming techniques to produce green shapes, aiming at the possibility to produce complex shaped components as required by industrial applications;
  • development and improvement of densification techniques, using processing parameters (temperature, atmosphere, pressure) which allow the attainment of the desired shape.

          The assessment of processing and densification techniques will require the availability of several complementary characterization techniques for the control of the raw material,of the intermediate products (slurries, green bodies) and of the densified material.

Characterization techniques are also necessary for understanding the mechanism behind the possible enhancement in the mechanical properties of nanocomposites, aiming at a full exploitation of the potential of this novel class of materials.

2.THE PARTNERSHIP

1 Istituto Nazionale per la Fisica della Materia (INFM))-IT        COORDINATOR
2 Belgian Ceramic Research Centre (BCRC)-BE
3 Dept. of Materials Engineering at the Technical University of Clausthal (IWW)-DE
4 Commissariat a l'Energie Atomique (CEA)-F
5 Vlaamse Instelling voor Technologisch Onderzoek (VITO) -BE
6 Laboratoire de Chimie des Plasmas Universite' de Limoges (ULIMO)-F
7 Laboratoire d'Etudes et de Recherches sur les Materiaux (LERMAT)-F
8 Ist. di Ricerca sulle Tecnologie Ceramiche del Consiglio Nazionale delle Ricerche (IRTEC- CNR)-IT
9 Technical University of Wien (UWIEN) AT
10 Materials Ireland, Joint Coating&Ceramics Research Centre (JCCRC) -IE
11 Interdisciplinary Research Centre at the Univ. of Birmingham (IRC)-GB
12 Materials Ireland Research Centre at the Univ. of Limerick (ULIMK)-IE
13 Dept. of Material Science at the Technical University of Freiberg (IKW)-DE
14 Ente per le Nuove Tecnologie, l'Energia e l'Ambiente (ENEA)-IT
15 Morgan Materials Technology LTD (MMT)-GB
16 Rolls Royce plc(RR)-GB
17 Metalloceramica Vanzetti S.p.A.(MCV) IT
18 NeoCeram S.A. BE
19 Gel Design&Engineering (GDE) IT
20 L'Air Liquide S.A. (AirLiq) F
21 Howmedica Int. Inc. (HOW) IE

OVERVIEW

Partner

Role

   

Group I

Powder suppliers

IWW (EDU)

Oxide nanopowder production by Nd-YAG laser evaporation of solid targets

CEA (ROR)

Si-based nanopowder production by CO 2 laser synthesis of liquid precursors

ULIMO (EDU)

Nanopowder production by thermal plasma evaporation and reaction synthesis

BAF (EDU)

Nanopowder production by CO 2 laser evaporation of solid targets

ENEA (ROR)

Oxide and Si-based nanopowder production by CO 2 laser synthesis

   

Group II

Powder processors

BCRC (ROR)

Development of cost-effective methods for nanocomposite fabrication

IRC (EDU)

Processing of nanocomposites; hydrothermal synthesis of ceramic sols

TU WIEN (EDU)

Hot-pressing or pressureless sintering of alumina and zirconia nanocomposites

VITO (ROR)

Handling&processing of non-oxide nano-powders;

IRTEC (ROR)

Processing of SiC/Si 3 N 4 nanocomposites

ULIMK (EDU)

Optimisation of pressureless sintering routes to produce nanocomposites

   

Group III

Experts in nanopowder and nanoceramic characterisation

JCCRC (ROR)

Characterisation of the mechanical properties of nanoceramics

LERMAT (ROR)

Automatic image analysis of nanopowders and nanoceramics

INFM (ROR)

Microchemical (XPS) and microstructural (AFM) analysis of nanopowders

   
 

Industrial Partners (observers &advisors, possible end-users)

MMT (IND/7)

Ceramic material manufacturer

RR (IND/7)

Industrial Power and AeroSpace Sectors

MCV (SME)

Development, manufacturing and distribution of cutting tools

AirLiq (IND/6)

World leader of industrial gas producers; interested in solid electrolyte pumps

How (IND4)

Manufacturer of hip and knee ceramic joints

GDE (SME)

Development and exploitation of technology in the field of sol-gel

NeoCer (IND/1)

Manufacturer of pump components

1. INFM ( Istituto Nazionale per la Fisica della Materia)- (IT)
INFM promotes, coordinates and performs -through long term programmes and specific projects- basic and applied research within a network of 36 Research Units established in Italian Universities, and in its own national laboratories. Of particular relevance to the present Project is the experience and expertise of the Research Unit at the University of Padova in the area of nanocluster physics and microanalytical and microstructural characterisation. INFM (through CNR-ICTIMA as associated partner) will provide powder suppliers with new, cost-effective organometallic precursors. INFM as coordinator assumes the responsability for project management.

2 BCRC ( Belgian Ceramic Research Centre ) -(BE)
BCRC is a research centre created more than forty years ago with the aim to help the ceramic industry community, involving mainly SME's having increasing need in process adaptation and diversification to new products. BCRC is in charge of several collective, pre-competitive research programmes and is involved in the CEN standardisation committees for advanced ceramics. BCRC will contribute to the Network working in the processing group, on ceramic matrix (alumina, mullite, silicon nitride) nanocomposites. BCRC will use the external services of the Laboratory CRITT (Ceramiques Fines)  at the University of Valenciennes (F) (VAL) to provide hydrpthermally synthesized mixed oxide powders.

3.IWW (Dept. of Materials Engineer. and Technology) at the Univ. of Clausthal (DE)
The chair of Materials Engineering (IWW) at the Univ. of Clausthal (DE)  was established in the early 1970's and first filled in 1977. The creation reflected a shift, which has been experienced in all the major developed nations, namely the increasing need to market high quality products together with industrial expertise. In addition, increasing costs of raw materials and energy demanded an optimisation in the development and application of raw materials. The Department is well equipped and able to carry out fundamental and applied research in a wide range of topics. Some projects are carried out jointly with industry. The role of IWW in the Network will be as oxide ( allumina, zirconia, CuO, SnO 2 ...) nanopowders supplier .

4. CEA (Commissariat a l'Energie Atomique) - (FR)
CEA is a large multidisciplinary R&D Institute involved in fundamental and applied research for nuclear and non-nuclear industries. The "Service des Photons, Atomes et Molecules" from CEA-Saclay  was the first in Europe to develop the process of laser driven synthesis of ultrafine ceramic powders (such as SiC, Si/C/N, WC.....) from gas-phase precursors. Recently, the CEA group has extended the process to liquid organometallic precursors injected into the laser beam in the aerosol form for the synthesis of amorphous Si/C/N nanocomposite powders. Furthermore, silica based powders and oxide composites have been obtained by high power, tunable CO2 laser induced pyrolysis of sol-gel precursors. The CEA group will supply Si-based nanopowders to the processing group for the fabrication of nano-ceramics.

5. VITO (Vlaamse Instelling voor Technologisch Onderzoek ) - (BE)
VITO (acronym for the Flemish Institute for Technological Research) employs over 350 scientists, engineers, technicians and administrative staff, making it the largest multidisciplinary research Centre in the Flanders region. VITO carries out market-oriented technological research and develops innovative products and processes in the field of non-nuclear energy, environmental and bio-technologies and advanced materials. Of interest for the present Project is the expertise of VITO in non-oxide ceramics( SiC, Si 3 N 4 ..) nanopowder handling & processing technology and in sintering of non-oxide nanocomposites.

6. ULIMO (Laboratoire de Chimie des Plasmas Universite’ de Limoges)-F
The Laboratoire de Chimie des Plasmas , Universite’ de Limoges (LIMO), has wide and well documented experience in the field of ceramic nano-powders production in a twin DC plasma arc. The LIMO group will supply the Network with mixed alumina-zirconia nanopowders and with batches of SiC/Si 3 N 4 nanopowders.

7. ISMRA- LERMAT (Laboratoire d' E'tudes et de Recherches sur les Materiaux) -
Caen (FR)
The group at ISMRA- LERMAT is working on the relationship between morphology, microstructure and physical properties of materials, using automatic image analysis, TEM-HREM-EDX and mechanical or electrical testing. There is an increasing emphasis on nanomaterials and nanopowders in the various types of materials investigated (composites materials such as CMC, MMC, PMC, ceramics materials and semiconductors). The role in the Network will be the use of TEM, HREM and nanoanalysis to investigate at atomic level the microstructure of nanoceramics.

8. National Research Institute for Ceramics Technology (IRTEC) of the Italian Research Council
(CNR) - (IT)
IRTEC is an Institute of the Italian Research Council working in the field of processing and of basic science of monolithic and composite ceramic materials with different functional properties and areas of applications, i.e. structural ceramics, electroceramics and bioceramics. IRTEC has facilities for forming and sintering processes, microstructural characterisation, textural analysis of green and dense bodies, evaluation of mechanical and tribological properties, thermophysical and electrical characterisation. IRTEC will cooperate with the Network partners on the processing and characterisation of oxide (alumina/zirconia) and non-oxide (SiC/ Si 3 N 4 ) nanocomposites.

9 Dept. of Oxide Chemistry of TU (Technical University) -Wien (AT).
The Institute of Chemical Technology of Inorganic Materials of the TU-Wien (AT) is divided into 4 Departments (Oxide Chemistry, Powdermetallurgy, Metal Science, Inorganic Materials and Processes). The main research fields at the Department of Oxide Chemistry are on the fabrication and characterization of structural ceramics. Inside the Network, the research activity will be focused on Al O 3 and zirconia nano-powder processing and (hot pressing or pressureless) sintering. Characterisation of the mechanical properties (strength, toughness, hardness...) and of the microstructure of the nano-ceramics will also be performed both on the samples produced ‘in house’ as well as by other Network partners.

10.JCCRC (Materials Ireland, Joint Coating&Ceramics Research Centre)- (IE)
JCCRC is a government research and industrial development organisation. JCCRC's strategic interest is to develop state of the art expertise in advanced ceramic technology. This know-how will then be used to support JCCRC's role in the development and transfer of technology into industry. The role of JCCRC inside the Network will be focused on the analysis of nanoparticles (particle size and shape analysis, determination of physical properties such as porosimetry, density, chemical composition, BET area...). The effect of chemical and firing treatment on particle properties will also be investigated.

11 IRC-(Interdisciplinary Research Centre) at the Univ. of Birmingham-( GB )
The University was founded in 1900 to train and educate the people who would create and manage the burgeoning businesses and industries of the Midlands. The IRC in Materials for High Performance Applications was established in October 1989 for the development of new materials, novel materials processing and manufacturing technologies and the subsequent use of computer-aided materials engineering to allow their efficient transfer to industry. IRC will participate in the activity of the Processing Group of both non-oxide and oxide containing composites. Of great interest for the Network is the expertise of IRC in the hydrothermal synthesis of ceramic sols from pure precursor chemicals and their use in the processing of nanocomposite materials.

12.ULIMK ( Materials Ireland Research Centre at the Univ. of Limerick) (IE)
The  Materials Ireland Research Centre at the Univ. of Limerick (IE) was established in 1981 with the aim of coordinating research activity in the field of metallurgy, polymers and composites, advanced ceramics and glasses, semiconductor technology and biomaterials. The Centre aims to assist Irish industry to grow.by providing both the facilities and necessary expertise to carry out research and development programmes in the fields of metals, polymers, composites, coatings, glasses and ceramics. The work of ULIM will concentate on the fabrication of nanocomposites, by developping economic processing routes and densification techniques. Within the Materials Ireland Research Centre prototyping, processing and manufacturing  state of the art capabilities exist and test as well as characterisation facilities (including mechanical testing equipment) are available for the Network partners.

13. BAF (Dept. of Material Science and Material Technology) of the the TU (Technical University) of Freiberg (D).
  The research group on ceramic nanopowders at BAF has a wide experience in the synthesis of nano-powders by CO2 laser ablation (in cooperation with the University of Jena). A synthesis route of SiC and sugar was tested recently. The Institute is well equipped with devices for particle characterisation, for chemical and structural investigations and for ceramic materials preparation. The main tasks in the Network are the production of oxide (mixed and doped) nano-powders by laser ablation and the manufacture of nanosized SiC and boron carbide powders by cheap methods.

14. ENEA (IT)
ENEA (Ente Nazionale per le Nuove Tecnologie, l'Energia e l'Ambiente) is the Italian Council for Innovative Technologies, Energy and Environment. Employment at ENEA amounts to approximately 4000 and the agency operates in various research centres distributed throughout the national territory. One of its major responsabilities is to promote advanced technology and to integrate its own research results into the national productive system, with the objective to renewing Italian industry. Of particular relevance to the present project is the experience and expertise in the area of CO 2 laser synthesis, characterisation (surface sensitive analysis techniques, morphological and chemical analyses) and processing of ceramic nano-powders. Nanopowders will be deliverd to the Network and powders produced by other partners as well as ‘in house’ will be characterised.

15. Morgan Materials Technology LTD (MMT)-GB
Morgan Material Technology (a R&D Company within the Morgan Group) is involved in the development of a wide variety of ceramic materials including toughened oxide materials, non-oxide ceramics and composites. In the Company, there is a wide expertise in sol-gel chemistry and processing, ceramic fabrication, solid and liquid state oxide synthesis, metal and ceramic processing. MMT has already been involved in projects to develop alumina /SiC nanocomposites for wear resistant and other applications. Their interest in the Network is motivated by the perspective to develop new cost-effective materials The participation of Morgan Material Technology to the Network would consist both in “steering” the programme and in performing some amount of ‘work in-house’ to characterise and test products of the partners which can be of interest for the Company .

16. Rolls Royce plc (RR)-GB
The Rolls-Royce Industrial Power Group manufactures a wide range of power plant, ranging from 30-1000 MW steam turbines to 10-40 MW industrial derivative gas turbines. The Rolls Royce Aerospace Group manufacture gas turbines for a wide range of airframes. The Rolls Royce Applied Science Lab. serves both the Rolls-Royce Industrial Power and Aerospace interests of Rolls Royce. It is the home for the Solid Oxide Fuel Cell (SOFC) programme . Improvement in both thermo-mechanical properties and sintering temperature could be won by incorporating nanopowders into the SOFC. The role of Rolls Royce in the Network will be as an advisor to the partners. When this is appropriate, representative from Rolls Royce will discuss with the other partners the possibility to transfer relevant nano-technology into Rolls Royce.

17. Metalloceramica Vanzetti S.p.A.(MCV) IT
MCV is a SME involved in the development, manufacturing and distribution of cutting tools. Metalworking operations are making use of ceramic cutting tools, but limitations in toughness of available products prevent significant market penetration. MCV will probably present a Project (in the framework of the INNOVATION Programme) on the development and industrialisation of nanocomposites for cutting tool applications, thus the Company is highly interested in following and steering the activity of a Network devoted to R&D on nanomaterials.

18. NeoCeram S.A. BE
NeoCeram S.A. is a Belgian SME producing alumina and zirconia wear parts (pump components). Altough these materials are satisfactory for many applications, better performing materials (with higher wear and strength resistance) are needed for advanced applications. NeoCeram is interested in following the research performed inside the Network and offers to test nanoceramics in its pilot test devices.

19 Gel Design&Engineering SRL(GDE) IT
GDE is an Italian Company established in 1992 to develop and commercially exploit technology related to hard materials of high and/or extremely high thermal resistance in the field of sol-gel. The Company strategy is based on the identification and commercial exploitation of applications that maximize benefits derived from intrinsic properties of its materials and processes. GDE is fully interested in the subject covered by NANOMAT and will take an active role in the Network.

20. L’Air Liquide S.A. F
L’Air Liquide S.A is a French SA company created in 1902 which is part of the Air Liquide Group present in more than 60 countries world-wide (28000 people, 31 billion FF sales). In 1996, it had employed 4000 people and its sales were over 7.7 billion FF. The Air Liquide Group appears as the world leader of the industrial gases producers. Air Liquide handles several research centres (about 500 persons) devoted to gas production and applications and masters the different technologies of production of industrial gases as cryo-distillation, adsorption on molecular sieves and permeation through organic membranes. Interest in the Network is related to the possibility of having access to better performing ceramics for solid electrolyte pumps or mixed conductors. The role of Air Liquide will be both as advisor and possible end-user.

21. Howmedica Int. Inc.(HOW) IE
Howmedica International was established in 1971 for the manufacture of orthopaedic implants. Today, the Company (which is part of the Pfizer Group) is a world leader of man-made surgical implants for total replacement of hip and knee joints. As an orthopaedic company routinely selling alumina and zirconia ceramic heads, Howmedica is committed to the development of new improved ceramic materials and is interested in producing ceramic materials that have better wear properties, higher flexural strength and especially higher fracture toughness than existing ceramic materials. Thus the Al2O3/SiC and Al2O3/zirconia systems to be studied in the NANOMAT Network are of great interest for the Company The role of Howmedica will be both as advisor and possible end-user.




3. WORK CONTENT

3.1 Ongoing Research

          A proposal for the formation of a Thematic Network on Nano-powder Production & Processing was circulated at the beginning of 1996 among 20-25 research groups operating in the field of innovative ceramic materials at Universities, Research Centres and Industries of various European countries. Most of the groups gave a positive response motivated by the following reasons:
  • nano-powder producers are strongly interested in a feedback from groups having expertise in powder processing and willing to face all the problems arising from a product that is promising but impractical to handle and difficult to press;
  • groups with expertise either in powder processing & densification or in material characterisation are intrigued by the possibility to investigate nanocomposite properties, but they are often limited by the difficulty in purchasing or obtaining the raw-material (nanopowders) in developmental quantities;
  • researchers from industry think that the present cost of fabricating nano-scale materials is too high and the benefits of the material are not fully demonstrated, however they are extremely interested in steering a research activity that could lead to the production of cost effective, high performance ceramic nanostructured materials.

          The general opinion was that there is a stalemate in R&D on nanostructured materials caused by both the high cost of the raw material and the sceptimism about the real benefits of fabricating components from nanopowders, after the failure in reproducing the results claimed by K. Niihara. However, everybody is convinced that there is a growing need for advanced ceramic materials and that R&D on nanostructured materials should not be abandoned before having tried novel nanopowder processing and densification routes.

          On this premiss, a proposal was presented to UE for the formation of a wide Network on nanopowder production and processing with the aim of overcoming the present stalemate in the field of nanostructured materials. About 20 research groups (including industrial research groups) declared their interest in the ‘explorative phase’ of the Project. Due to the large number of partners involved in the Network, it was decide to facilitate the preparation of the final proposal by organising a workshop on the following topics:

  • -to review of the state of art and inventory of research activities in the field developped by each partner;
  • -to discuss the feasibility of a Network on nanopowder production & processing;
  • -to hear the point of view of researchers from industry about the reason for the actual stalemate in the development and production of nanomaterials at industrial level and the advice for overcoming the actual difficulties;
  • -to define a provisional network plan for the ‘ implementation phase’.

The representatives of 14 European Research Groups and 4 European Industries participated in the Workshop that was held in Frascati on May 16-17, 1997.

As a result of the discussions held in the Workshop, it came out that the formation of a Thematic Network on nanopowder production and processing involving nano-powder producers, processors and end-users would make the R&D activity on nanostructured materials easier and would minimize the risks and costs involved to the research groups and companies. It was a general opinion that the formation of a Network on nanopowder production & processing is feasible and of great interest for all the participants. Researchers from industry can either partecipate to the activity of a group or provide guidance in their area of interest.

          On the basis of the discussions held during the Workshop and further contacts among the partners, a workplan was outlined as follows:

Workplan

Research Activities Represented in the Network

          Due to the large number of participants (21 groups) it was decided to form a vertically integrated Network comprising: powder producers (Group I), powder processors (Group II), experts in powder and/or material characterisation (Group III).

Group I: Nano-powder Preparation.

Various materials were selected on the basis of the following criteria:

  • interest for industry;
  • availability of precursors;
  • interest and expertise of the partners of Group II in handling&processing these systems.


Table I : Selected Nanopowders for Production

Company

ENEA

IWW

BAF

CEA

ULIM

Production Method

CO 2 Laser synthesis

Nd-YAG laser evaporation

CO 2 laser evaporation reaction synthesis

CO 2 Laser synthesis

Thermal plasma evaporation + reaction synthesis

SiC

YES

 

YES

YES

 

Si/C/N

YES

   

YES

 

Al 2 O 3

YES

YES

YES

YES

YES

ZrO 2

 

YES

YES

 

YES

TiO 2

       

YES

possibility of dopant/binder addition

yes

yes

 

yes

yes

The acronyms of Par. 2 were used to idetify the participants.

Group II: Nano-powder Processing.

Selection of systems

Various systems were selected on the basis of the following criteria:

  • interest for industry;
  • availability of nanosized powders, i.e. from the raw materials group or directly from the processing group;
  • nature of the matrix and the dispersed phase, i.e. oxide-oxide or oxide-non-oxide, particle-paricle or fibre-particle;
  • interaction between matrix and dispersed phase, i.e. chemical interaction or physical interaction (thermal and elastic).

          Table 2 summarises the selected materials systems. For each group of materials, i.e. monolithic ceramics, oxide or non-oxide dispersed nanosized particles and fibre reinforced nanosized matrix, the following information is given: materials system, participants in the research (the acronyms of Par.2 have been used). For oxide composites, nano-size powders mixtures will be synthesized using hydrothermal methods.
           Table 3 shows the role of each participant of the Network processing group in the different preparation and shaping tasks.


Characterisation
The processing group will contribute to the characterisation of densified products using specific techniques:

  • thermomechanical testing (strength, toughness, elastic moduli, hardness versus temperature)
  • wear assessment (friction, erosion, abrasion..).

When available, standard testing procedures will be used, otherwise specific protocols will be developed to allow comparison of results obtained in the different network laboratories.


Table 2 : Selected Nano-systems for Investigation

Type

Raw Material Supplier

Materials Systems

Materials Systems N°

Academic Participant

Industrial Participant

Monolithic

Raw materials Group

Al 2 O 3

ZrO 2

1

2

BCRC,VITO

IRC,VITO

HOW

RR, HOW

Non-oxide containing  composites

Raw materials Group

SiC+Al 2 O 3

SiC+Si 3 N 4

3

4

UWIEN,IRC

BCRC,ULIMK

VITO,ULIMK

IRTEC,

MCV,MMT NEOCERAM HOW

MCV,MMT

Oxide Composites

IRC to supply ZrO 2 and mullite precursor

BCRC (VAL) to supply ZrO 2

and Al 2 O 3 precursor

ZrO 2 +mullite

Al 2 O 3 +ZrO 2

5

6

IRC

ULIMK,

UWIEN,IRC

IRTEC

RR

NEOCERAMMMT,MCV

Table 3: Partition of Tasks between the Participants of the Network Processing Group.

Participant :

IRC

ULIMK

BCRC

UWIEN

VITO

IRTEC

Task:

           

Slurries *

2,3,5,6

3,4,6

1,3,6

1,3,4

4

4,6

Plastic Mixtures *

2,3,5,6

 

3,6

     

Spray drying

X

 

X

     

Freeze drying

X

X

X

 

X

X

Die Pressing

 

X

 

X

X

X

CIP

 

X

X

 

X

X

Slip Casting

X

 

X

   

X

Extrusio

X

 

X

     

Tape Casting

           

CMC fabrication

X

     

X

 

(*) Figures refer to the material systems of table 2.

Group III: Nano-powder and Material Characterisation

I t is essential for the Project, to determine the following properties of nanopowders:

- Particle size and shape of non-agglomerated particles
- Composition of surface
- Crystalline phases.

          For each topic, in the following, information is given on the type of diagnostics and the laboratory in charge of performing it.

Particle size and shape analysis

TEM (Transmission Elictron Microscopy)/EDX

ISMRA-LERMAT

SFM (Scanning Force Microscopy)

INFM

X-ray Diffraction Analysis, BET (specific surface detemination)

JCCRC, ENEA


Analysis of the surface chemical composition

XPS (X-ray Photo-electron Spectroscopy)

ENEA, INFM

surface ‘PH’

JCCRC


Crystalline phases determination

TEM (Transmission Elictron Microscopy)/EDX

ISMRA-LERMAT

X-ray Diffraction Analysis

JCCRC, ENEA


Characterisation of the Properties of Nanostructured Materials

Mechanical properties (strength, hardness, toughness, .. )

ISMRA-LERMAT

wear assesment

JCCRC

When possible, the densification group will contribute to the characterisation of the densified products, using specific techniques.

            In general, standard testing procedures will be used. When standard procedures are not available, specific protocols will be developped by the Network participants to allow comparison of results obtained in the different Network laboratories. ‘Round Robin’ tests of selected samples will be organised between the Laboratories involved in the Network. 


Workplan for the first year of activity

Research Activities to be represented in the Network

Task 1: Preparation of Al 2 O 3 nanoceramics .

Subtask 1.1: Al 2 O 3  powder production

Partner

Activity (1 year)

IWW
ENEA

-------------

-------------

-------------

-------------


Subtask 1.2: Al 2 O 3 processing

Partner

Activity (1 year)

T.U.Wien

   

-------------

 


Subtask 1.3: Al 2 O 3  characterisation

Partner

Activity (1 year)

ENEA
ISMRA-LERMAT
JCCRC

   

-------------

-------------

-------------


Task 2: Preparation of ZrO
2 nanoceramics

Subtask 2.1: ZrO 2  production

Partner

Activity (1 year)

IWW
BAF

-------------
-------------
-------------
-------------


-------------

 


Subtask 2.2: ZrO 2  processing

Partner

Activity (1 year)

IRC

------------- -------------

-------------

 


Subtask 2.3: ZrO 2  characterisation

Partner

Activity (1 year)

JCCRC
ISMRA-LERMAT

   

-------------
-------------

-------------
-------------


Task3: Preparation of SiC/Al
2 O 3 nanocomposites

Subtask 3.1: SiC/Al 2 O 3  nanopowder production

Partner

Activity (1 year)

ENEA
BAF

  -------------

-------------
-------------


-------------


Subtask 3.2: SiC/Al 2 O 3   processin

Partner

Activity (1 year)

WIEN
ULIMK

-------------
-------------
-------------

-------------
-------------

-------------
-------------


Subtask 3.3: SiC/Al 2 O 3  characterisation

Partner

Activity (1 year)

ULIMK+BCRC


 

 

-------------

Task 4: Preparation of SiC/Si 3 N 4 nanocomposites

Subtask 4.1: SiC/Si 3 N 4 production

Partner

Activity (1 year)

ULIMK+BCRC


 

 

-------------

Subtask 4.2: SiC/Si3N4 processing

Partner

Activity (1 year)

VITO
IRTEC
CEA


-------------
-------------

 

-------------
-------------
-------------

Subtask 4.3: SiC/Si3N4 characterisation

Partner

Activity (1 year)

ENEA
ISMRA-LERMAT
JCCRC


 

-------------

-------------


-------------



Task 5: Preparation of zirconia/mullite nanocomposites

Subtask 5.1: zirconia/mullite synthesis

Partner

Activity (1 year)

IRC

-------------
-------------

 

 

Subtask 5.2: zirconia/mullite processing

Partner

Activity (1 year)

IRC


 

-------------

-------------

Subtask 5.3: zirconia/mullite characterisation

Partner

Activity (1 year)

INFM
ISMRA-LERMAT
JCCRC


 

-------------

-------------


-------------


Task 5: Preparation of zirconia/mullite nanocomposites

Subtask 5.1: zirconia/mullite synthesis

Partner

Activity (1 year)

IWW
BCRC
LIMO


-------------

-------------
-------------



-------------

-------------

-------------

Subtask 6.2: zirconia/allumina processing

Partner

Activity (1 year)

VITO
IRTEC
CEA


 

-------------
-------------

-------------
-------------
-------------

Subtask 6.3: zirconia/allumina characterisation

Partner

Activity (1 year)

INFM
ISMRA-LERMAT
JCCRC


 

-------------

-------------


-------------

3.2 Network Activities

            - Organisation of Meetings:

                        The first goal of the Network will be to obtain nanocomposites with improved mechanical properties, the second will be to define cost effective nano-powder production & processing techniques..Due to the large number of partners (21 groups) ,it was decided to form three working groups: powder producers (Group I), powder processors (Group II), experts in powder and/or material characterisation (Group III). A Steering Committee will be formed in order to guarantee a coherent effort and integration of the three Groups and an effective flow of information between all the participants.

            The Steering Committee will meet every six months. The purpose of the Steering Committee meetings is to review past work and results and to plan and coordinate future activities. A summary of the discussions and decisions taken at these meetings will be written as minutes and circulated to all partners for comments.

            The Group leaders will organise task meetings with the involved partners following the work requirements. The minutes of the task meetings will be circulated to the Steering Committee members to facilitate the follow-up and monitoring of the research activity of all the participants.

            All partners will meet once a year. One of the six-monthlyl Steering Committee meetings will take place at the end of the General Meeting. The meetings will be organised in turn at the premises of a guest partner so that the participants will have the opportunity to visit the laboratories involved in the Network. Group leaders will be appointed during the general meetings and the position may be turned over every year.

- Establishment of  a review of the state of art and the market for advanced ceramics (see 3.3);

- Identification of other scenarios in which nanotechnology developped for the Network may find applications (see 3.3).


Deliverables:

  A full progress report (including the contribution of each participant) will be delivered every twelve months.

  A report including brief progress notes by each of the three Groups on main achievements and difficulties will be delivered at the intermediate six months.

  At the end of the second year, the progress report will include the analysis of the results and the cost-benefit evaluation for the preparation of the selected nanoceramics. At this point a decision will be taken wether to stop the activity or to develop and optimise cost-effective nanomaterial production methods aiming at transferring the technology of nanopowder production & processing to industry.

  At the end of the fourth year, the final report and a report on exploitation of results on nanocomposites will be delivered.


3.3 State of Art and Market Review

           Advanced ceramic materials constitute an emerging technology with a broad base of current and potential applications and an ever growing list of material compositions. New technologies are emerging among which nanotechnology promises to yield important advances with applications in many different areas.

           In terms of market for advanced ceramics, the largest growth rate in the next years is expected to be for the structural ceramics market and recently there was a surge of interest in nanosized ceramic powders.

          The core of nanotechnology, which is relevant to most of the application areas, consists of fabrication techniques and instrumentation at nanometre scale. Recently it has been recognised that nanotechnology, altough intrinsically multi-disciplinary, suffers from a lack of coordination between nanotechnology RTD infrastructure and researchers in different disciplines, and between the applications for which these resources could be used.

          For these reasons, the Network will devote resources (1.5 man-months/year) to: - establish a review of the state of art and the market for advanced ceramics; - to identify other scenarios in which nanotechnology developped for the Network may find applications.

          In this framework, the Network will devote some resources to explore the potentials of nanotechnology in high added value applications such as the preparation of silica containing luminescent Si nanocrystallites for applications in opto-electronics. A team will be formed by ENEA (with expertise in preparing Si nanoparticles by CO2 laser synthesis), LERMAT (with expertise in magnetic field-assisted nanopowder co-deposition), INFM (with expertise in preparation and characterisation of of nanocomposites for non-linear optics), GDE (with expertise in cold sol gel processes for the preparation of Si doped silica) with the task to develop and evaluate processes leading to the production of innovative nanocomposites for application in opto-electronics.

          In case the first two years of activity will terminate with the demonstration that there are not clear benefits in the fabrication of nanocomposites for structural applications, (see Par.4), some partners of the Network could decide to continue the activity by devoting most of the resources to R&D of nanocomposites for application in opto-electronics. This would clearly require a deep re-organisation of the partnership and revision of the workplan.

Workplan for the first year of activity

Task 7 : State of art and market review
Partner

Man/months

Activity (1 year)

INFM

0.5


 

-------------

-------------

Subtask 5.2: zirconia/mullite processing
Partner

Man/months

Activity (1 year)

INFM, ENEA, GDE, LERMAT

1.0


 

-------------

-------------

Deliverables:
- Annual report on the state of art and market review of nanotechnology.


3.3 State of Art and Market Review

          Advanced ceramic materials constitute an emerging technology with a broad base of current and potential applications and an ever growing list of material compositions. New technologies are emerging among which nanotechnology promises to yield important advances with applications in many different areas.

          In terms of market for advanced ceramics, the largest growth rate in the next years is expected to be for the structural ceramics market and recently there was a surge of interest in nanosized ceramic powders.

          The core of nanotechnology, which is relevant to most of the application areas, consists of fabrication techniques and instrumentation at nanometre scale. Recently it has been recognised that nanotechnology, altough intrinsically multi-disciplinary, suffers from a lack of coordination between nanotechnology RTD infrastructure and researchers in different disciplines, and between the applications for which these resources could be used.

          For these reasons, the Network will devote resources (1.5 man-months/year) (see 3.2) to: - establish a review of the state of art and the market for advanced ceramics; - to identify other scenarios in which nanotechnology developped for the Network may find applications.

          In this framework, the Network will devote some resources (see 3.2) to explore the potentials of nanotechnology in high added value applications such as the preparation of silica containing luminescent Si nanocrystallites for applications in opto-electronics. A team will be formed by ENEA (with expertise in preparing Si nanoparticles by CO2 laser synthesis), LERMAT (with expertise in magnetic field-assisted nanopowder co-deposition), INFM (with expertise in preparation and characterisation of of nanocomposites for non-linear optics), GDE (with expertise in cold sol gel processes for the preparation of Si doped silica) with the task to develop and evaluate processes leading to the production of innovative nanocomposites for application in opto-electronics.

          In case the first two years of activity will terminate with the demonstration that there are not clear benefits in the fabrication of nanocomposites for structural applications, (see Par.4), some partners of the Network could decide to continue the activity by devoting most of the resources to R&D of nanocomposites for application in opto-electronics. This would clearly require a deep re-organisation of the partnership and revision of the workplan.

4. MILESTONES AND DELIVERABLES

According to the Project flow chart, a milestone is identified at the end of the second year of activity.

Project flow chart

Beginning of the Project: production of nanopowders in developmental quantities
|
assessment of nanopowder handling & processing methods
|
production and characterization of prototype components
|
End of the second year: evaluation of the benefits        -> no stop the activity
      | yes
development of cost-effective nanopowder production and processing methods
|
transfer of the technology of nanopowder production & processing to industry
|
End of the fourth year.


The following items will be delivered to the UE:

  • A full progress report (including the contribution of each participant) will be delivered every twelve months.
  • A report including brief progress notes by each of the three Groups on main achievements and difficulties will be delivered at the intermediate six months.
  • At the end of the second year, the progress report will include the analysis of the results and the cost-benefit evaluation for the preparation of the selected nanoceramics. At this point a decision will be taken wether to stop the activity or to develop and optimise cost-effective nanomaterial production methods aiming at transferring the technology of nanopowder production & processing to industry.
  • At the end of the fourth year, the final report and a report on exploitation of results on nanocomposites will be delivered.



5. NETWORK MANAGEMENT

          INFM ( Istituto Nazionale per la Fisica della Materia) as coordinator assumes the responsability for Project management.

          Due to the large number of participants (21 partners) it was decided to form a vertically integrated Network comprising: powder producers (Group I), powder processors (Group II), experts in powder and/or material characterisation (Group III).

          A steering committee will be formed in order to guarantee a coherent effort and integration of the three Groups and an effective flow of information between all the participants. The Steering Committee will provide technical and financial planning and control. For each Group the participants will appoint one responsible Group leader who will report directly to the Coordinator. Within the Steering Committee each partner will be represented by his Group leader. Members of the Steering Committee will also be the industrial partners acting as endorsers & observers. The Steering Committee will meet every six months. The purpose of the Steering Committee meetings is to review past work and results and to plan and coordinate future activities. A summary of the discussions and decisions taken at these meetings will be written as minutes and circulated to all partners for comments. The Group leaders will organise task meetings with the involved partners following the work requirements. The minutes of the task meetings will be circulated to the Steering Committee members to facilitate the follow-up and monitoring of the research activity of all the participants.

          All partners will meet once a year. One of the six-monthlyl Steering Committee meetings will take place at the end of the General Meeting. The meetings will be organised in turn at the premises of a guest partner so that the participants will have the opportunity to visit the laboratories involved in the Network. Group leaders will be appointed during the general meetings and the position may be turned over every year.

          INFM will appoint Dr. E. Borsella as project coordinator, who will be the Chairman of the Steering Committee

          Dr. E. Borsella obtained her degree in Physics cum Laude at the Univ. of Naples,Italy (July 24, 1974). After joining ENEA from the Univ. of Naples (where from 1975 to 1977 she had been research fellow ) she worked in the area of laser processing and diagnostics. From 1978 to 1985, she focussed her research activity on laser isotope separation of U, S and C molecular compounds. Since 1986 she has been responsible for research in the field of laser induced processes in molecules for ultrafine powders and thin films production. From 1994 to 1996 Dr. E. Borsella was Leader of the Division of Spectroscopy, Laser Applications and Innovative Materials of the Department for Innovativative Technologies at the ENEA Research Centre of Frascati (Rome), Italy. Since October 1996 , she is on leave of absence at the INFM Unit of the University of Padova, where she is involved in research on the physics of nanoclusters. She has supervised several National and International Projects in the field of laser assisted deposition of innovative materials and optical diagnostics of laser induced processes. From 1988 to 1989 she was visiting scientist at the Max Planck Inst. for Quantum Optics ( Garching- FRG). Her wide experience in the field of laser interaction with matter is witnessed by publications on Int. Journals (more than 75), contributions to Int. Conferences (more than 65) and invited talks (9).

          Dr. E. Borsella has got experience in coordinating programmes in the framework of several National and International cooperation projects with Industries and Research Institutes for the production of innovative materials through laser assisted processes. She has got experience in participation to EC Programmes acting as scientific official of ENEA in the BRITE EURAM II Project N° 5147/91: "Development and Industrialization of Nanocomposite Ceramic Materials for Cutting Tool Applications" and in the EC-Human Capital & Mobility Research Network for Scientific and Technical Cooperation entitled: "Heterostructures on Si for Integrated Microelectronics" (ERB4050PL930528). In 95-96, Dr. E. Borsella was coordinator of the INTAS Project "Nucleation, Growth and Spectroscopy of Ceramic and Metallic Clusters in Laser Driven Synthesis" (N°93-1236).


6.FINANCIAL INFORMATION

See the enclosed Form B4.

7. EUROPEAN DIMENSION AND RELATED BENEFITS

          The proposed Network will bring together 21 European partners (14 research groups from 7 Member States and 7 companies from 5 Member States) on the technological objective of developping cost-effective methods for the production of nanocomposite materials with superior thermo-mechanical properties.

          The ceramic market is expanding slowly, but continuously in Europe and there a demand for higher performance ceramic materials in several sectors (see Par. 2). It is commonly accepted that nanostructured materials are very interesting from a scientific point of view and potentially attractive for applications, but there is a stalemate in their development at industrial level for the lack of technology in handling and processing nanopowders and for the high costs involved.

          It follows that R&D on nanostructured materials is highly risky for industries and there is the distinct possibility that European companies will be left behind, whilst in the rest of the world (USA and Japan) nanocomposites are currently under study as a promising class of materials and nanosized powders are commercially available

          The formation of a wide Network on nanopowder production and processing for the fabrication of innovative ceramic materials would open up the possibility of overcoming the present stalemate in the field of nanostructured materials. Shortening of the development and technology transfer time could be reached by focusing the research efforts among the European Universities, Research Institutes and Industries involved in the proposed Network.

          If the initial targets will be achieved, European end-users could benefit of a significant improvement in the performance of nanocomposite ceramic materials.

          An economic feasible level of production of nanocomposite materials for structural applications (Heat Engine Components, Wear-Resistant Parts, Energy and Aerospace related industrial applications, Cutting Tools, Bioceramics) requires from the beginning at least an European wide market impact.

8. LIST OF REFERENCES

          Most of the partners of the proposed Network are involved in other European or National Projects related to R&D of nanocomposite materials.

          BCRC and ULIMK are involved in the Programme BRE3.CT96.0212 entitled "Nanocomposite alumina caramics for advanced technical applications" (NACATA).

          IWW is developping research on nanopowders production and processing in the framework of the BRITE EURAM Project SMOGLESS for the production of gas sensors.

          CEA and VITO were recently involved in the BREU-0555 Programme on "Cost effective laser synthesized nanoscale powders and case of thermomechanical applications" (1992-1996).

          ENEA takes part in the BRITE-EURAM III Project entitled: " Integration of conventional polymers with ceramic nanoparticles to produce structural composites" and in a Project for the development of SiC/SiC fiber nanocomposites by chemical infiltration with polymeric precursors in the framework of the EC-Long Term Fusion Technology Programme.

          ULIMK is involved in a TMR Project entitled "Comparison of the effects of nanodispersed second phase particles in Al2O3 and Si3N4 Matrices in ceramics for high performance applications"

          MCV and ENEA were recently involved in a BRITE-EURAM Project on the "Development and industrialisation of nanocomposite ceramic materials for cutting tool applications" that will originate a new Project under the INNOVATION Programme.

          Rolls Royce is interested in the development of nanocomposite materials in the framework of the Programme SOFC (Solid Oxide Fuel Cell).



LIST OF RELEVANT REFERENCES:

1) S. Komarneni : Nanocomposites, J. Mater. Chem. 2(12), 1219-1230 (1992)

2) R. Dagani: Nanostructured materials promise to advance range of technologies, Chem. & Eng. News 18-24, 23 Nov. 1992.

3) R. S. Averbek, H. J. Hofler, R. Tao: Processing of nano-grained materials, Mater. Sc.Eng. A66 169-177 (1993).

4) R. D. Shull: Viewpoint: nanocrystalline and nanophase materials, NanoStructured Materials 2, 213-216 (1993).

5) L. Sheppard: Advances in nanophase ceramics, Adv. Mater. Proc. 10, 25-27 (1994).

6) R. W. Siegel : Nanophase Materials: synthesis, structure and properties, Springer Series in Material Sciences, Vol. 27, ed. F. E. Fujita 65-105 (1994).

7) H. Gleiter: Nanostructured Materials: state of the art and perspectives, Z. Metallkd. 86, 78-83, (1995).

8) C. Suryanarayana: Nanocrystalline Materials, International Materials Reviews 40, 41-64 (1995).

9) K. Niihara: New Design Concept of Structural Ceramics- Ceramic Nanocomposites, J.Ceram.Soc. Jap., the Centennial Memorial Issue, 99 (10), 974-982 (1992).

10) M. Sternitzke: Review: Structural Ceramic Nanocomposites, Journal of the European Ceramic Society 17, 1061-1082 (1997).

11) "Advanced Ceramic Powders & Nanosized Ceramic Powders- Technologies, Applications, New Developments and Market Opportunities", Published by BCC, 1994.

12) M. Ruhle "Microscopy of Structural Ceramics" Adv. Mater. 9, 195-217 (1997).

13) I. Malsch "The Importance of Interdisciplinary Approaches: The case of Nanotechnology" The IPTS Reports, 13, 36-40, 1997




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