Rapid Production of Micro- and Nano-particles Using Supercritical Water

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. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .