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