Thisbookistalkingabouthowtousesupercriticalwater(SCW)torapidlyproduce micro- and nano-particles of metal oxides, inorganic salts, metals and organics. Itcoversbasicprinciples, experimentalmethodologiesandreactors, particlep- duction, characterizationsandapplicationsaswellastherecentadvancement. Fine particlescanbeproducedbybothchemicalandphysicalprecipitationofproducts from SCW. They can be used as catalysts, materials in ceramics and electronic devices andcompositematerials. Particlesareeasilyproduced continuouslyina owreactorinshortreactiontimes(0. 4s?2min)butcanalsobesynthesizedin batchreactorsforlongreactiontimes(e. g.,12h). Theycanbeeasilystudiedin-situ microscopically(optical/IR/Raman/SR-XRD)inanopticalmicro-reactor, diamond anvilcell. Thesize, sizedistribution, crystalgrowth&structure, andmorphologyof particlescanbecontrolledbychangingtheconcentrationsofstatingmaterials, pH, pressures, temperatures, heating&coolingrates, organicmodi cations, reducingor oxidizingatmospheres, owratesandreactiontimes. Thisisthe rstbooktosystematicallyintroduceusingSCWforproductionof neparticles. Itisanidealreferencebookforengineers, researchersandgraduate studentsinmaterialscienceandengineering. vii Acknowledgments I would like to thank Drs. T. Ogi & T. Minowa (Biomass Technology Research Center, NationalInstituteofAdvancedIndustrialScienceandTechnology, Japan), and Profs. K. Arai, H. Inomata, R. L. Smith Jr. and T. Adschiri (Chemical Engineering, TohokuUniversity, Japan), whoinitiallyintroducedthehydrothermal andsupercritical uidsareastomewhenIworkedinJapanfrom1996to1999. Thanks are also due to Profs. J. A. Kozinski, R. I. L. Guthrie (Materials Engineering, McGillUniversity, Canada)andI. S. Butler(Chemistry, McGill)for theirguidanceinmyworkonhydrothermalprocessduringmyworkinCanadafrom 1999to2007. Profs. W. Bassett (Geological Sciences, Cornell University) and D. Baker (Earth&PlanetarySciences, McGill)forinstructionsregardingDAC, Dr. I-Ming Chou(U. S. GeologicalSurvey)forusefuldiscussionsofthepressurecalculation procedure. Drs. M. Watanabe and T. Sato (Research Center of Supercritical Fluid Technology, Tohoku University, Japan) for discussions about the experimental set-upofthebatchand owreactors. Drs. S. Xu, H. Assaaoudi, R. HashaikehandA. Sobhy, whoworkedwithmeat McGillinCanada. ix Contents 1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 1. 1 Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 1. 2 RapidExpansionofSupercriticalSolution(RESS)Process . . . 4 1. 3 SupercriticalAntisolvent(SAS)Process . . . . . . . . . . . . . 4 1. 4 OtherPhysicalProcesses . . . . . . . . . . . . . . . . . . . . . 5 1. 5 SupercriticalWaterProcess . . . . . . . . . . . . . . . . . . . . 5 References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 2 Supercritical Water Process. . . . . . . . . . . . . . . . . . . . . . 11 2. 1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11 2. 2 BatchReactor . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 2. 3 FlowReactor. . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 2. 4 DiamondAnvilCell(DAC). . . . . . . . . . . . . . . . . . . . 20 References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 3 Metal Oxides Synthesis. . . . . . . . . . . . . . . . . . . . . . . . . 29 3. 1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 3. 2 Boehmite(AlOOH) . . . . . . . . . . . . . . . . . . . . . . . . 30 3. 3 Ferrites. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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This book shows how to use supercritical water (SCW) to synthesize nano- and micro- oxides, inorganic salts and metal particles and its recent advancement. Also polymer/biomass particles can be produced by using the method of precipitation of solutes from SCW. The particles can be used as catalysts for biomass conversions, materials in ceramics & electronic devices and composite materials. Particles are easily produced continuously in a flow reactor in short reaction times or synthesized in a batch reactor in long reaction times. Besides the synthesis process, the book also present studies of the properties of these materials. The size, size distribution, crystal growth & structure, and morphology of particles produced by supercritical water can be controlled by the feed concentrations, pH, pressures, temperatures, heating & cooling rates, organic modifications, reducing or oxidizing atmospheres, flow rates and reaction times.
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