Continuous Hydrothermal Synthesis of Nanomaterials: From Laboratory to Pilot Plant

Lead Research Organisation: University College London
Department Name: Chemical Engineering


Summary: A novel laboratory scale continuous hydrothermal flow synthesis (CHFS) system has been developed for the controlled synthesis of inorganic nano-materials (particles <100nm) with potential commercial applications from sunscreens and battery materials to fuel cell components and photocatalysts. The CHFS system has many advantages; it is a green technology (using supercritical water as the reagent), which utilises inexpensive precursors (metal nitrate salts) and can controllably produce high quality, technologically important functional nano-materials in an efficient single step (or fewer steps than conventionally). This project seeks to move the existing laboratory scale CHFS system (developed over the past few years at QMUL) towards a x10 pilot scale-up (nano-powder production of up to 500g per 12h depending on variables). The proposed research will initially compare the ability to control particle characteristics of the CHFS system at the laboratory scale over a large range of process variables (flow rates, temperatures, pressures, etc), building full operational envelopes that will describe reactor variables versus particle properties for each material. In particular, we will utilise process analytical technology (PAT)and the data will help develop univariate and multivariate understanding of the temporal operational spaces and interactions between process variables and product quality. PATand chemometrics incorporated with combined computational fluid dynamics modelling of hydrodynamics/mixing and population balance modelling of particle size evolution via nano-precipitation will be used to study alternative nozzles designs and other potential bottleneck factors. This will lead to a generic strategy for scaling up and controlled manufacture of nanomaterials with consistent, reproducible and predictable quality. The scale up quantities of nano-powders from the pilot plant will allow industrial partners to perform prototyping or comprehensive commercial evaluation of nano-powders in a range of applications which they have hitherto not been able to conduct due to lack of sufficient high quality material. Importantly, the know-how acquired on the project and the proposed feasibility studies will reduce the risk and commercial barriers for industry that might consider building a larger industrial scale CHFS plant in the future.
Description this was probably the most improtant grant of my carreer and helped develpoed a pilot plant which has put my reesarch group in a strong position as we are able to make large amounts of nanomaterials. this has supported many research projects now including innovate uk projects. A patented mixer was also developed in the grant which has solved a major technological problem of blocking of the flow reactors and this is a way to make the process commercilisable
Exploitation Route the pilot plant is now supporting multiple projects in moving nano materials applications up the technology readiness levels and we are trying to form a spin out the technology and form a advanced materials company.
the pilot plant has now been involved in the following
EP/P510385/1 Low cost high energy density anode for stationary energy storage (P)
EP/M014045/1 Electrodes by Design - Microstructural Engineering of High Performance Electrodes for Solid Oxide Fuel Cells (C)
EP/M009394/1 ELEVATE (ELEctrochemical Vehicle Advanced TEchnology) (C)
EP/K035355/2 Bio-inspired sulfide nanocatalysts: From proof of concept to 'real' catalysis (C)
EP/M008754/1 Sustainable Oxidation Catalysts for the Production of Solar Hydrogen and Chlorine from Brine (P)
EP/L017709/1 Sustainable Manufacturing of Transparent Conducting Oxide (TCO) Inks and Thin Films (C)
EP/K035355/1 Bio-inspired sulfide nanocatalysts: From proof of concept to 'real' catalysis (C)
EP/J500136/1 Nanocrystalline Water Splitting Photodiodes II; Device Engineering, Integration and Scale-up (C)
EP/H046313/1 Bio-inspired (Fe,Ni)S nano-catalysts for CO2 conversion (C)
ESPRC Faraday Fast Start project "Towards a Comprehensive Understanding of Degradation Processes in EV Batteries" Grant ref: FIRG001 (PI Clare Grey, Cambridge) and also ESPRC grant; ISCF Wave 1: The JUICED Hub [Joint University Industry Consortium for Energy (Materials) and Devices Hub (EP/R023662/1) and also Discovery to use grant "Developing inkjet printable electronics inks and coatings" worth £100k from UCL with £100k in kind matching funding from QinetiQ and also Impact studentship for Charles Footer on "electromagnetic shielding applications" (£45k cash contribution from QinetiQ) and also Innovate UK funding "Low cost high energy density anode for stationary energy" with Sharp UK Ltd (EPSRC ref EP/P510385/1)
Sectors Aerospace, Defence and Marine,Chemicals,Education,Electronics,Energy,Manufacturing, including Industrial Biotechology,Security and Diplomacy,Transport

Description amalyst collaboration 
Organisation Amalyst Ltd
Country United Kingdom 
Sector Private 
PI Contribution we have made and tested a range of new catalysts for brine splitting and water splitting
Collaborator Contribution they have supplied training and expertise and advice related to
Impact one paper trained pdras in use of methods for assessment of catalysts
Start Year 2016
Description impact acceleration funding "Maximising Impact of an EPSRC Funded Pilot Plant Production Facility 
Organisation Qinetiq
Department QinetiQ (Farnborough)
Country United Kingdom 
Sector Private 
PI Contribution Our group developed coated nanoparticles with a range of different dispersions, we investigated the various process conditions in a flow reactor. Then we evaluated the different nanomaterials in ink formulations. we conducted a series of spin coated films that were then heat treated to give the final transparent films. These films were characterized for pertinent properties.
Collaborator Contribution The partner was reponsbile for
Impact The collaboration has led to a full funded phd student charles footer to work on electromagnetic absorbing nanomaterials a phd student Yiana Shakespeare was also supported in supercaps (with in kind funding and access to facilities). They have also funded 2 x 1 years placements in chemistry which are now linked to my group. They are also funding 40k matching funding for a inkjet printer and plasma coater (UCL matching funding). They have also written support letters on several projects funded by epsrc, incluidng offering in kind on all of them, which include Faraday Hub core bid, Faraday fast start degradation project, UCL's JUICED hub which is £1.8M, and a forthcoming bid is also being supported (£5M programme grant led by Sheffield)
Start Year 2016
Description johnson matthey new collaboration 
Organisation Johnson Matthey
Country United Kingdom 
Sector Private 
PI Contribution we have developed new catalysts for splitting brine at low current densities
Collaborator Contribution they have supported the research with access to testing facilities for testing of the catalyst surfaces suing gas adsorption kit attended regular meetings and advised us on the project
Impact a paper has been published the researcher has been trained in use of analytical facilities (multidisciplinary)
Start Year 2016
Title A new mixer for making nanoparticles via hydrothermal flow 
Description this is a confined jet mixer that allow mixing of supercritical water and metal salts at room temperature in water. This prevents bloacking and is a major development that is highly scalable and still makes very good quality nanoceramics 
IP Reference EP2576036 
Protection Patent granted
Year Protection Granted 2015
Licensed No
Impact its allowed me to develop the process so well that we have continued to get industry and academic funding to carry out nanomaterials research and develop new research areas