Processing of Nanostructured Ceramics
Lead Research Organisation:
Loughborough University
Department Name: Materials
Abstract
The appeal of nanocrystalline ceramics arises from their potential to offer unusual physical and mechanical properties, which, depending on the material, can include superplasticity at elevated temperatures, optical transparency for normally opaque materials and a range of other electrical, optical and magnetic properties as well as potentially higher strengths, toughnesses and hardness.Although some commercial nanopowders are now produced in relatively large quantities, consolidation into dense nanostructured components by industrially-viable routes is needed to take full advantage of the potential offered. If this can be achieved there is the potential to use the materials for a very wide range of applications. Advanced ceramics are the active material in many electronics devices, fuel cells, magnets, sensors and biomaterials, as well as a very wide range of structural components. This means that they are used in almost every type of industry, including power generation, aerospace, transportation and military applications as well as in the manufacture of other materials. Such applications are vital to maintaining global competitiveness, decreasing energy consumption and minimising pollution. Their estimated world market was >$20B in 2000, with an annual growth rate of 7.2%. Of this, the electronics sector was ~65% of the market, the rest falling into the chemical processing, coatings and advanced structural mechanics sectors.The primary objective of this research proposal is to develop a number of recent developments at Loughborough Univ. that have been achieved under previous EPSRC grants. Specifically:* Whilst it is now possible to slip cast very homogeneous and high density compacts from nanosuspensions, there is currently a major problem with drying those made from high solids content suspensions (which yield the best bodies) - it can take several days even using a humidity drier. The structure of these bodies need understanding as a function of the processing conditions used, particularly the solids content of the suspension. This then gives us a chance to control the situation and perhaps improve it so that drying times can be much faster without sacrificing the properties of the body.* Similarly, it is now possible to dry press homogeneous and high density compacts from powders that have been formed by spray-freeze drying the nanosuspensions (the same process used to make instant coffee granules). Once again, however, the high solids content suspensions (which yield the highest densities) provide problems, this time with hard agglomerates that don't crush. Very similar work needs performing as above to allow us to understand why this is happening and what can be done about it.* Both types of compact need firing in furnaces to produce fully dense ceramics whilst retaining an extremely fine, sub 100 nm, average grain size. Whilst this can now also be done using a novel pressureless (and hence low cost) process, the understanding of how this process works is still not perfect and we also need to scale up to make larger components.* Finally, as we near the point where we can exploit these developments commercially, we really need to develop a better understanding of industry's requirements. Just how close are we to developing process routes that they can use on their factory floors? Which ceramic systems are they most interested in? Which companies are really ready to embrace the new 'nanotechnology' and which are keen to sit on the sidelines for a bit longer yet. These issues, and others, will all be addressed in the final task of the programme.
Organisations
- Loughborough University (Lead Research Organisation)
- Valve Solutions (Collaboration)
- Dynamic-Ceramic Ltd (Collaboration)
- MEL Chemicals Inc (Collaboration)
- Rolls Royce Group Plc (Collaboration)
- Rolls-Royce (United Kingdom) (Project Partner)
- CoorsTek (United Kingdom) (Project Partner)
- QinetiQ Nanomaterials Ltd (Project Partner)
- Luxfer Group (United Kingdom) (Project Partner)
Publications
Binner J
(2008)
Dense nanostructured zirconia by two stage conventional/hybrid microwave sintering
in Journal of the European Ceramic Society
Binner JGP
(2008)
Manufacture of nanostructured ceramics
in Proceedings of ICC2 - Global Roadmap for Ceramics
Liang Y
(2008)
Effect of triblock copolymer non-ionic surfactants on the rheology of 3mol% yttria stabilised zirconia nanosuspensions
in Ceramics International
Santacruz I
(2009)
Wet forming of concentrated nano-BaTiO3 suspensions
in Journal of the European Ceramic Society
Santacruz I
(2010)
Dispersion and Rheology of Aqueous Suspensions of Nanosized BaTiO 3
in International Journal of Applied Ceramic Technology
Santacruz I
(2009)
Gel casting of aqueous suspensions of BaTiO3 nanopowders
in Ceramics International
Sun J
(2020)
3D printing of zirconia via digital light processing: optimization of slurry and debinding process
in Journal of the European Ceramic Society
Vaidhyanathan B
(2010)
Microwave Sintering of Multilayer Integrated Passive Devices
in Journal of the American Ceramic Society
Vaidhyanathan B.
(2010)
Microwave assisted large scale sintering of multilayer electroceramic devices
in Ceramic Engineering and Science Proceedings
Description | The primary objective of this research proposal was to develop a number of recent developments at Loughborough Univ. that have been achieved under previous EPSRC grants. Specifically: * It has been learnt how to slip cast bodies as large as 60 mm in diameter (dried green body) without cracking. In part this is down to the rheology of the slip used (60 wt% solid content, 0.2 Pa s nanosuspension), to the choice of grade of plaster of Paris and to the drying conditions used. The green bodies formed are typically ~55% of theoretical density, which is sufficient to be able to sinter them to full density without undue grain growth. * It has been learnt how to produce a flowable, completely crushable granulated nanopowder. The flowability matches that of a benchmark, commercial, submicron yttria stablised zirconia; the granules now crush at as little as 200 MPa (previously at least 380 MPa). The new, lower strength granules are now well within range of existing ceramic processing equipment on the factory floor. The primary key has been the introduction of an agent designed to introduce flaws into the granules and hence weaken their strength. A patent application was filed on this process (Oct 08). * We are now able to densify both the above green bodies to at least 99.5% of theoretical density whilst retaining a mean grain size anything from ~65 nm up to ~200 nm. These results have given us the ability to actually measure the properties of these ceramics. In brief, we have discovered that they are as strong as commercial ceramics (measurements made by NPL - strengths of ~1 GPa); they can be a lot more damage resistant (indentation toughness measurements up to 14.5 MPa m-1/2) and they can be entirely resistant to hydrothermal ageing (3 weeks at 250oC, 4 bar; conventional YSZ disintegrates completely within 1 hr under these conditions). A patent has been filed (Nov 08) on the properties. * A full market survey has been completed by an independent body, viz. CERAM Research in the UK. Undertaken before we could release the property data, it provided confirmation of the significant interest in our work. Numerous companies were interested provided a) the properties were good (we now know that they are) and b) the various steps can be scaled up (they can). |
Exploitation Route | The work undertaken here has been further extended via a Collaboration Fund programme and was subsequently licensed to MEL Chemicals in February 2012. Commercialisation is expected during 2012/13. |
Sectors | Energy |
Description | This research led to a series of subsequent research grants and the processes developed have been licensed by MEL Chemicals. |
First Year Of Impact | 2009 |
Sector | Aerospace, Defence and Marine,Energy,Environment |
Impact Types | Economic |
Description | EPSRC Collaboration Fund - Manufacture of prototype nanostructured ceramic components |
Amount | £100,780 (GBP) |
Funding ID | EP/I500227/1 |
Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
Sector | Public |
Country | United Kingdom |
Start | 04/2010 |
End | 12/2011 |
Description | HIRF - Manufacture of nanostructured ceramics |
Amount | £16,309 (GBP) |
Organisation | ENVEO |
Sector | Private |
Country | Austria |
Start | 09/2007 |
End | 02/2008 |
Description | KTA - Nanostructured ceramics for dental applications |
Amount | £48,312 (GBP) |
Organisation | Loughborough University |
Sector | Academic/University |
Country | United Kingdom |
Start | 09/2011 |
End | 10/2012 |
Description | Loughborough Univ - Enterprise Fellowship |
Amount | £16,296 (GBP) |
Organisation | Loughborough University Enterprises Ltd |
Sector | Private |
Country | United Kingdom |
Start | 12/2007 |
End | 11/2008 |
Description | Loughborough Univ Enterprise Office - Bridging funds for postdoc |
Amount | £8,487 (GBP) |
Organisation | Loughborough University |
Sector | Academic/University |
Country | United Kingdom |
Start | 12/2011 |
End | 03/2012 |
Description | Loughborough Univ Enterprise Support - patent costs |
Amount | £25,000 (GBP) |
Organisation | Loughborough University Enterprises Ltd |
Sector | Private |
Country | United Kingdom |
Start | 03/2008 |
End | 09/2008 |
Description | Loughborough Univ research studentship - Transparent nanocrystalline YAG |
Amount | £51,570 (GBP) |
Organisation | Loughborough University |
Sector | Academic/University |
Country | United Kingdom |
Start | 09/2010 |
End | 09/2013 |
Description | Manufacturing nanostructured ceramics: new process for concentrating nanosuspensions via an industrially viable route |
Amount | £12,983 (GBP) |
Organisation | Loughborough University |
Sector | Academic/University |
Country | United Kingdom |
Start |
Description | Morganite Electrical Carbon Ltd - Transparent nanocrystalline YAG |
Amount | £45,000 (GBP) |
Organisation | Morgan Advanced Materials |
Department | Morganite Electrical Carbon Ltd |
Sector | Private |
Country | United Kingdom |
Start | 09/2010 |
End | 09/2013 |
Description | Nano transparent alumina |
Amount | $66,000 (USD) |
Organisation | ONRG Office of Naval Research Global |
Sector | Public |
Country | United States |
Start | 09/2012 |
End | 03/2015 |
Description | Nano transparent alumina |
Amount | £50,000 (GBP) |
Organisation | Defence Science & Technology Laboratory (DSTL) |
Sector | Public |
Country | United Kingdom |
Start | 09/2012 |
End | 03/2015 |
Description | Nanoplant |
Amount | £358,390 (GBP) |
Funding ID | EP/L024780/1 |
Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
Sector | Public |
Country | United Kingdom |
Start | 04/2014 |
End | 04/2017 |
Description | Royal Soc - Scaling up the production of nanostructured ceramics |
Amount | £29,375 (GBP) |
Organisation | The Royal Society |
Department | Brian Mercer Feasibility Award |
Sector | Charity/Non Profit |
Country | United Kingdom |
Start | 04/2009 |
End | 02/2011 |
Description | TSB - Nanostructured advanced ceramics |
Amount | £218,811 (GBP) |
Funding ID | TS/G000891/1 |
Organisation | Innovate UK |
Sector | Public |
Country | United Kingdom |
Start | 09/2008 |
End | 12/2011 |
Description | TSB - Nanozirconia for ceramic implants |
Amount | £206,020 (GBP) |
Organisation | Innovate UK |
Sector | Public |
Country | United Kingdom |
Start | 09/2011 |
End | 09/2013 |
Description | Dynamic-Ceramic Ltd |
Organisation | Dynamic-Ceramic Ltd |
Country | United Kingdom |
Sector | Private |
PI Contribution | Further collaboration was undertaken utilising the following funding: EPSRC Collaboration Fund EP/I500227/1 Royal Society Brian Mercer Feasibility Award Loughborough University funding KTA funding Direct industrial funding All of which extended this project further. Partners included MEL Chemicals, Dynamic Ceramic Ltd and Valve Solutions amongst others. |
Collaborator Contribution | Dynamic-Ceramic put our nanopowder through their production line to make ceramics - it worked. |
Impact | None to date. |
Start Year | 2007 |
Description | MEL Chemicals |
Organisation | MEL Chemicals Inc |
Country | United States |
Sector | Private |
PI Contribution | Further collaboration was undertaken utilising the following funding: EPSRC Collaboration Fund EP/I500227/1 Royal Society Brian Mercer Feasibility Award Loughborough University funding KTA funding Direct industrial funding All of which extended this project further. Partners included MEL Chemicals, Dynamic Ceramic Ltd and Valve Solutions amongst others. |
Collaborator Contribution | They provided the precursor nanosuspension |
Impact | They have commercialised their process |
Start Year | 2007 |
Description | Rolls-Royce Fuel Cell Systems Ltd |
Organisation | Rolls Royce Group Plc |
Department | Rolls-Royce Fuel Cell Systems Limited |
Country | United Kingdom |
Sector | Private |
Start Year | 2007 |
Description | Valve Solutions |
Organisation | Valve Solutions |
Country | United Kingdom |
Sector | Private |
PI Contribution | Further collaboration was undertaken utilising the following funding: EPSRC Collaboration Fund EP/I500227/1 Royal Society Brian Mercer Feasibility Award Loughborough University funding KTA funding Direct industrial funding All of which extended this project further. Partners included MEL Chemicals, Dynamic Ceramic Ltd and Valve Solutions amongst others. |
Collaborator Contribution | Valve Solutions tested the final product. |
Impact | None to date. |
Start Year | 2007 |
Title | METHOD FOR CONCENTRATING NANOSUSPENSIONS |
Description | A method for concentrating a nanosuspension comprising nanopowder particles suspended in a liquid comprises reducing the liquid content of the nanosuspension and controlling the dispersion of the nanopowder particles in the liquid. |
IP Reference | WO2006136780 |
Protection | Patent granted |
Year Protection Granted | 2006 |
Licensed | Yes |
Impact | Sales are beginning to happen. |