The Sol-Gel Handbook: Synthesis, Characterization and Applications, 3-Volume Set

1557 Pages·2015·197.104 MB·English

by  David Levy, Marcos Zayat

Editedby
DavidLevyand
MarcosZayat
TheSol-GelHandbook
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Edited by
David Levy and
Marcos Zayat
The Sol-Gel Handbook
Volume 1: Synthesis and Processing
Volume 2: Characterization and Properties
of Sol-Gel Materials
Volume 3: Application of Sol-Gel Materials
TheEditors AllbookspublishedbyWiley-VCHarecarefully
produced.Nevertheless,authors,editors,and
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V
Contents
Preface XXXI
ListofContributors XXXIII
VolumeOne: SynthesisandProcessing
PartOne Sol–GelChemistryandMethods 1
1 ChemistryandFundamentalsoftheSol–GelProcess 3
UlrichSchubert
1.1 Introduction 3
1.2 HydrolysisandCondensationReactions 4
1.2.1 Silica-BasedMaterials 4
1.2.1.1 Precursor(s) 9
1.2.1.2 Catalyst(pH) 9
1.2.1.3 AlkoxoGroup/H ORatio(R ) 9
2 w
1.2.1.4 Solvent 10
1.2.1.5 Electrolytes 10
1.2.2 MetalOxide-BasedMaterials 11
1.3 Sol–GelTransition(Gelation) 17
1.3.1 HydrolyticSol–GelProcesses 17
1.3.2 NonhydrolyticSol–GelProcesses 22
1.3.3 Inorganic–OrganicHybridMaterials 22
1.4 AgingandDrying 24
1.5 PostsynthesisProcessing 26
1.6 ConcludingRemarks 26
References 27
2 NonhydrolyticSol–GelMethods 29
RupaliDeshmukhandMarkusNiederberger
2.1 Introduction 29
2.2 NonaqueousSol–GelRoutestoMetalOxideNanoparticles 31
2.2.1 Surfactant-AssistedSynthesis 31
VI Contents
2.2.2 Solvent-ControlledSynthesis 33
2.2.2.1 BenzylAlcoholRoute 33
2.2.2.2 tert-ButylAlcoholRoute 37
2.2.2.3 EtherRoute 37
2.2.2.4 AcetophenoneRoute 38
2.2.2.5 CarboxylicAcidRoute 39
2.2.2.6 BenzylamineRoute 39
2.2.3 Microwave-AssistedSynthesis 40
2.3 NonaqueousSol–GelSynthesisbeyondMetalOxides 43
2.3.1 Composites 43
2.3.2 Organic–InorganicHybridMaterials 44
2.3.3 MetalSulfides 46
2.3.4 Metals 47
2.4 ChemicalReactionandCrystallizationMechanisms 48
2.4.1 Introduction 48
2.4.2 OverviewoftheMainChemicalReactions 49
2.4.3 ClassicalandNonclassicalCrystallizationMechanisms 51
2.4.4 SelectedExamples 51
2.5 AssemblyandProcessing 56
2.5.1 Introduction 56
2.5.2 NanoparticleArraysandSuperlattices 57
2.5.3 OrientedAttachmentandMesocrystals 59
2.5.4 Films 60
2.6 SummaryandOutlook 63
References 63
3 IntegrativeSol–GelChemistry 71
M.Depardieu,N.Kinadjian,D.Portehault,R.Backov,andClémentSanchez
3.1 Introduction 71
3.2 Designof0DStructures 72
3.2.1 AerosolProcessing 72
3.2.2 Capsules 75
3.2.2.1 SimpleEmulsionsPreparation 76
3.2.2.2 MineralizationoftheWaxDispersion 76
3.2.2.3 Temperature-TriggeredRelease 77
3.2.2.4 IntroducingaHydrophilicCompartment 79
3.2.2.5 Water@Wax@WaterEmulsionFormulation 80
3.2.2.6 Water@Wax@WaterEmulsionMineralization 80
3.2.2.7 Temperature-TriggeredRelease 81
3.2.2.8 Wax@Water@OilEmulsionFormulation 83
3.2.2.9 Wax@Water@OilEmulsionMineralization 84
3.2.2.10 Temperature-TriggeredRelease 85
3.3 Designof1DMacroscopicStructures 88
3.3.1 Electrospinning 89
3.3.1.1 AFirstCase:TiO FibersforDye-SensitizedSolarCells 89
2
Contents VII
3.3.1.2 CouplingSol–GelReactionsandElectrospinning 90
3.3.2 Extrusion 93
3.3.2.1 V O FibersasAlcoholSensor 94
2 5
3.3.2.2 CompositeFibersPreparedwiththeHelpofPolymerDehydration/
Reticulation 96
3.4 DesignofExtended2DStructures 99
3.5 DesignofExtended3DStructures 99
3.5.1 Foams 99
3.5.1.1 SilicaFoams:Si-(HIPE) 101
3.5.1.2 Eu3+@Organo-Si-(HIPE):PhotonicProperties 101
3.5.1.3 Pd@Organo-Si-(HIPE):CyclingHeckCatalysisReactions 103
3.5.1.4 Enzyme@Organo-Si-(HIPE):HighEfficiencyBiocatalysts 104
3.5.1.5 Si-(HIPE)asHardTemplatetoCarbonaceousFoamsand
Applications 106
3.5.1.6 Carbon-(HIPE)asLiIonNegativeElectrodes 107
3.5.1.7 LiBH4@Carbon-(HIPE)forHydrogenStorageandRelease 107
3.5.2 Aerogels 112
3.5.3 DenseNanostructuredMonoliths 112
3.6 Conclusions 113
References 115
4 SyntheticSelf-AssemblyStrategiesandMethods 121
AlexandraZamboulis,OlivierDautel,andJoëlJ.E.Moreau
4.1 Introduction 121
4.2 TemplatedSynthesisofInorganicMaterials 122
4.2.1 Self-AssemblyofMesoporousSilicas 123
4.2.2 HydrothermalRearrangementandPostsynthesisTreatment 125
4.2.3 Self-AssemblyofThinFilms 126
4.2.4 Self-AssemblyofFunctionalizedMesoporousSilicas 127
4.3 Self-AssembledOrganosilicas 128
4.3.1 ControlofthePoreStructure:TemplatedSynthesisofMesoporous
BridgedSilsesquioxanes 129
4.3.2 Self-OrganizedOrganosilicas 132
4.3.3 Self-AssemblySyntheticStrategiesforOrganosilicaswithOptical
Properties 139
4.3.3.1 TowardanH-Aggregation/CardPackStacking 141
4.3.3.2 FromaJ-toanH-Aggregation 149
4.3.3.3 TranscriptionoftheJ-AggregationfromthePrecursortothe
Material 153
4.4 Conclusions 154
References 154
5 ProcessingofSol–GelFilmsfromaTop-DownRoute 165
PlinioInnocenziandLucaMalfatti
5.1 Introduction 165
VIII Contents
5.2 Top-DownProcessingbyUVPhotoirradiation 167
5.2.1 UVCuringofOxides 167
5.2.2 UVCuringofHybridSol–GelFilms 169
5.2.3 UVPhotoirradiationofMesoporousFilms 170
5.2.4 NanocompositeSo–GelFilmsbyUVPhotoirradiation 173
5.3 LaserIrradiationandWriting 174
5.3.1 Thermal-InducedEffects 174
5.3.2 Laser-InducedMicrofabrication 175
5.3.3 NanofabricationbyTwo-orMultiphotonAbsorption 177
5.4 ElectronBeamLithography 178
5.5 Top-DownProcessingbyHardX-Rays 181
5.6 SoftX-RayLithography 184
References 186
6 Sol–GelPrecursors 195
VadimG.Kessler
6.1 Introduction 195
6.2 SimpleSiliconAlkoxides 196
6.3 FunctionalandMixedLigandSiliconAlkoxidesforMoreFacile
Hydrolysis 197
6.4 FunctionalSiliconAlkoxides:PrecursorsofHybridMaterials 198
6.5 SimpleMetalAlkoxides 200
6.5.1 CommerciallyAvailableSimpleMetalAlkoxide 202
6.5.2 CustomarySynthesisofMetalAlkoxidePrecursors 209
6.5.2.1 InteractionofMetalswithAlcohols 209
6.5.2.2 AlcoholysisofComplexesDerivedfromVolatileAcidsWeakerThan
Alcohols 209
6.5.2.3 BasicAlcoholysisofMetalHalides:MetathesisReaction 210
6.5.2.4 AlcoholysisofMetalOxides 210
6.5.2.5 ElectrochemicalOxidationofMetalsinAlcohols 211
6.5.2.6 AlcoholInterchangeReaction 211
6.6 FunctionalandMixedLigandMetalAlkoxidesforMoreFacile
HydrolysisandStabilizationofResultingColloids 212
6.7 PrecursorandSolventChoiceforNonhydrolyticSol–GelProcesses 213
6.8 SynthesisofComplexMaterials:Single-SourcePrecursorApproach 214
6.9 Sol–GelPrecursorsforSpecialApplications:Biomedicaland
Luminescent 215
Abbreviations 216
References 216
PartTwo Sol–GelMaterials 225
7 NanoparticlesandComposites 227
GuidoKickelbick
7.1 Introduction 227