Continuous hydrothermal synthesis is still in its infancy, in terms of the scope of materials that can be produced and the control over particle size and shape. The project also allowed researchers to specifically focus on expanding the ‘repertoire’ of the process. Partners were able to demonstrate how metals, mixed metal oxides, sulphides, perovskites, phosphates and even metal organic frameworks could be produced. In addition to simple ‘production’, much of the work was around how the size and shape of the products themselves could be altered by changing process variables e.g. pressure, temperature, flow, concentration and precursor type. Most of this work is now published, with a significant number of publications in preparation. These will be added periodically.
These publications include the following papers.
Reactor Design and Simulation;
1. Thomas Huddle, Ammar Al-Atta, Ed Lester, Pseudo Fluid Modelling used in the Design of Continuous Flow - Supercritical Water Oxidation Reactors with improved Corrosion Resistance Journal of Supercritical Fluids 120, pp. 355-365
2. Jose Sierra-Pallares, Juan Garcia Serna, Maria Cocero, Fidel Mato, Thomas Huddle, Ed Lester Prediction of residence time distributions in supercritical hydrothermal reactors working at low Reynolds numbers Chemical Engineering Journal
299, pp. 373-385
3. Jose Sierra-Pallares, Juan Garcia Serna, Olaf Luebben, Igor Shvets, Maria Cocero, Fidel Mato, Thomas Huddle, Ed Lester Understanding the bottom up synthesis of nanoparticles via continuous hydrothermal synthesis using empirical measurement and computational simulation Nano Research, 9, (11), p3377-3387
4. Housley, D., et al., The use of dimensionless groups to analyse the mixing of streams with large density differences in sub- and supercritical water. Chemical Engineering Journal, 2016. 287: p. 350-358.
5. Tom Huddle, Ed Lester. Paul Langston, Bayesian Deconvolution of Vessel Residence Time Distribution, accepted in the International Journal of Chemical Reactor Engineering (IJCRE)
New Materials Discovery
I. Dunne, P. W., Starkey, C. L., Munn, A. S., Sikder, M., Luebben, O., Shvets, I., Lester, E. H., Transition metal doped anatase nanocrystals: continuous flow hydrothermal synthesis and photocatalytic activity. Accepted in Journal of Environmental Chemical Engineering 2016.
II. Dunne, P. W., Starkey, C. L., Munn, A. S., Tang, S. V. Y., Luebben, O., Shvets, I., Ryder, A. G., Casamayou-Boucau, Y., Morrison, L., Lester, E. H., Bench- and pilot-scale continuous-flow hydrothermal production of barium strontium titanate nanopowders. Chemical Engineering Journal, 2016, 289, 433-441.
III. Dunne, P. W., Starkey, C. L., Munn, A. S., Huddle, T. A., Lester, E. H., Continuous-flow supercritical hydrothermal synthesis of inorganic nanomaterials. Philosophical Transactions of the Royal Society of London A: Mathematical, Physical and Engineering Sciences, 2015, 373, 2057.
IV. Dunne, P. W., Munn, A. S., Starkey, C. L., Lester, E. H., The sequential continuous-flow hydrothermal synthesis of molybdenum disulphide. Chemical Communications, 2015, 51, 4048-4050.
V. Dunne, P. W., Starkey, C. L., Gimeno-Fabra, M., Lester, E. H., The rapid size- and shape-controlled continuous hydrothermal synthesis of metal sulphide nanomaterials. Nanoscale, 2014, 6 (4), 2406-2418.
VI. Gimeno-Fabra, M., et al., Continuous synthesis of dispersant-coated hydroxyapatite plates. CrystEngComm, 2015. 17(32): p. 6175-6182.
VII. Munn, A.S., Dunne P, Lester E., Large-scale continuous hydrothermal production and activation of ZIF-8. Chemical Communications, 2015. 51(64): p. 12811-12814
Characterisation and metrology
I. Wang, C., Huddle T, Mathews J, Lester E., Quantifying Curvature in High-Resolution Transmission Electron Microscopy Lattice Fringe Micrographs of Coals. Energy & Fuels, 2016
II. Mariusz Cierech, Jacek Wojnarowicz, Dariusz Szmigiel, Bohdan Bączkowski, Anna Grudniak, Katarzyna Wolska, Witold Łojkowski, Elżbieta Mierzwińska-Nastalska Preparation and characterization of ZnO-PMMA resin nanocomposites for denture bases, has been finally accepted for publication in Acta of Bioengineering and Biomechanics (IF=0.894). DOI assigned: 10.5277/ABB-00232-2014-04.
III. Y. Wu, M. I. Breeze, G. J. Clarkson, F. Millange, D. O’Hare, R. I. Walton “Exchange of Coordinated Solvent During Crystallisation of a Metal-Organic Framework Observed by In Situ High Energy X-ray Diffraction”, 2016 Angew. Chem. Int. Ed., 10.1002/anie.201600896
IV. H.H.-M. Yeung, Y. Wu, S. Henke, A.K. Cheetham, D. O'Hare, R.I. Walton “In-situ Observation of Successive Crystallizations and Metastable Intermediates in Metal-Organic Framework Formation”, 2016 Angew. Chem. Int. Ed., 55, 2012
V. G. Kieslich, A. C. Forse, S. Sun, K. Butler, S. Kumagai, Y. Wu, M. R. Warren, A. Walsh, C.P. Grey, A. K. Cheetham “Amine-cavity interactions in determining the structure and mechanical properties of the ferroelectric perovskite framework [NH3NH2]Zn(HCOO)3”, 2016 Chem. Mater., 28, 312
VI. C. Chen, C. F. H. Byles, J.-C. Buffet, N. H. Rees, Y. Wu, D. O’Hare, “Core-shell Zeolite@Aqueous Miscible Organic-Layered Double Hydroxide”, 2016 Chem. Sci., 7, 1457
VII. S. J. Moorhouse, Y. Wu, D. O’Hare “In Situ Study of Resin-Assisted Solvothermal Metal-Organic Framework Synthesis”, 2015 J. Solid State Chem., doi:10.1016/j.jssc.2015.07.035
VIII. Y. Wu, S. J. Moorhouse, D. O’Hare, “Time-Resolved In Situ Diffraction Reveals a Solid-State Rearrangement During Solvothermal MOF Synthesis”, 2015 Chem. Mater., 27, 7236
IX. I. Wang, C., Huddle T, Huang C.H, Lester E., Mathews J,Improved quantification of curvature in high-resolution transmission electron microscopy lattice fringe micrographs of soots. Carbon, 117 p174-181
Life Cycle Analysis
I. Freiberg, F. - Vlachý, J.: LCC Analysis and its Application. Manažment podnikov, 2014, vol. 11, no. 3, pp. 167-174. ISSN 1338-410
II. Stieberová, B. - Žilka, M. - Tichá, M. - Freiberg, F. - Hošek, J.: Comparative study of nanoparticle production technologies focused on environmental aspects. In NANOCON 2014 Conference Proceedings. Ostrava: TANGER spol. s r.o., 2014, ISBN 978-80-87294-55-0. Accessible from: http://konsys-t.tanger.cz/files/proceedings/20/reports/3086.pdf
III. Tichá, M. - Freiberg, F. - Žilka, M. - Stieberová, B.: Comparative LCA study on photocatalytic coating and air purifier. In SETAC 20th LCA Case Study Symposium. Novi Sad: University of Novi Sad, Faculty of Technical Sciences, 2014, vol. 1, art. no. 53, p. 48. ISSN 2310-3191. Accessible from: tp://lcanovisad.setac.eu/embed/LCANoviSad/files/programmebook_v5.pdf
IV. Tichá, M. - Freiberg, F. - Žilka, M. - Stieberová, B.: Life Cycle Assessment comparison of photocatalytic coating and air purifier. Integrated Environmental Assessment and Management [online]. 2015. ISSN 1551-3793.
V. Vlachý, J.: A Chemical Engineering Case of Life Cycle Costing. In Economics and Business Management in the 21st Century. Ostrava: VŠB-TU, 2014, pp. 283-292. ISBN 978-80-248-3520-4. Accessible from: http://www.ekf.vsb.cz/export/sites/ekf/erp21/.content/galerie-dokumentu/proceedings.pdf
VI. Vlachý, J. - Freiberg, F.: Deriving an Economic Model for the Production of New Materials. Applied Mechanics and Materials, 2014, vol. 11, no. 718, pp. 3-8. ISSN 1662-7482 Accessible from: http://www.scientific.net/AMM.718.3
The SHYMAN website (www.shyman.eu) has had over 10,000 visits during the 4 years and the videos posted on the video diary page (mainly accessed via YouTube links) have had over 250,000 views. The Project coordinator has also given several radio interviews on nanotechnology and its significance in society.