Materials Syntheses: A Practical Guide / Edition 1

Materials Syntheses: A Practical Guide / Edition 1

by Ulrich Schubert, Nicola H?sing, Richard Laine
     
 

ISBN-10: 3211751246

ISBN-13: 9783211751244

Pub. Date: 07/19/2008

Publisher: Springer Vienna

Materials syntheses are generally more complex than syntheses of inorganic or organic compounds and specific characterization methods play a more important role. Materials synthesis protocols often suffer from unclarities, irreproducibility, lack in detail and lack in standards. The need to change this situation is the main motivation for this book. It collects a

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Overview

Materials syntheses are generally more complex than syntheses of inorganic or organic compounds and specific characterization methods play a more important role. Materials synthesis protocols often suffer from unclarities, irreproducibility, lack in detail and lack in standards. The need to change this situation is the main motivation for this book. It collects a number of detailed protocols, ranging from organic polymers to carbonaceous and ceramic materials, from gels to porous and layered materials and from powders and nanoparticles to films. Preparation methods include intercalation and flux methods, sol-gel processing, templating methods for porous materials, sonochemistry or spray pyrolysis. Each contribution provides detailed and unambiguous descriptions of the hardware, specific characteristics of the procedure, scope of applicability as well as methods that unequivocally identify and characterize the material and allow checking whether the synthesis was successful. Written for: Researchers and graduate students in inorganic, organic, physical organic chemistry as well as material sciences studies

Product Details

ISBN-13:
9783211751244
Publisher:
Springer Vienna
Publication date:
07/19/2008
Edition description:
2008
Pages:
228
Product dimensions:
6.20(w) x 9.40(h) x 0.80(d)

Table of Contents

Preface 1

List of Contributors 3

Controlling Size and Morphology of Zeolite L 9

Large Zeolite L Crystals 11

Medium-sized Disc-shaped Zeolite L Crystals 13

Nano-sized Zeolite L Crystals 15

Medium-sized Cylindrical-shaped Zeolite L Crystals 16

Zeolite A and ZK-4 21

Zeolite A Crystals 25

ZK-4 Crystals 26

Nano-sized Zeolite A Crystals (Fig. 4) 27

Mesostructured Silica Thin Films 29

Preparation of the Coating Sol 32

Film Deposition 33

Post Treatment 33

Organically Modified Monolithic Silica Aerogels 39

Preparation of 3-Methacryloxypropyl-substituted Silica Aerogel 41

Preparation of 2-Aminoethyl-3-aminopropyl-substituted Silica Aerogel 44

Porous Silica Gel by Acid Leaching of Metakaolin 47

Preparation of Metakaolins 49

Preparation of the Acid-activated Solids 49

Zirconia-Pillared Clays 53

Preparation of Zr-pillared Clays Using Zirconyl Chloride as Precursor 55

Preparation of Zr-pillared Clays Using Zirconium Acetate as Precursor 57

Montmorillonites with Mixed Aluminum-Lanthanide Oxide Pillars 59

Preparation of the Pillaring Agent 60

Pillaring Process 61

Birnessite-type Manganese Oxide by Redox Precipitation 65

Redox Precipitation 67

Hydrothermal Treatment 68

Templated Carbon from Pyrolysis of Pyrene in Pillared Clay Matrices 71

Preparation of Pillared Clay 73

Loading of the Pillared Clay with Organic Compounds 74

Pyrolysis, and Removal of the Inorganic Matrix 75

Fiberous Carbon from Sepiolite Clay and Propylene 77

Preparation of Propylene-loaded Sepiolite 79

Pyrolysis and Dissolution of the Propylene-loaded Sepiolite 81

Aerosol Spray Synthesis of Porous Molybdenum Sulfide Powder 83

Preparation of Low-porosityMoS[subscript 2] 86

Preparation of Porous MoS[subscript 2] 86

Sonochemically Prepared Molybdenum Sulfide 89

Preparation in Glove Box 91

Reaction in Fume Hood 92

Product Isolation 92

Doped Manganites 95

Preparation of La[subscript 0.5]Ba[subscript 0.5]MnO[subscript 3] 97

Preparation of La[subscript 0.5]Sr[subscript 0.5]MnO[subscript 3] 100

Lithium Manganese Oxide Prepared by Flux Methods 103

Growth of LiMn[subscript 2]O[subscript 4] Spinel Single Crystals in a LiCl-Mn(NO[subscript 3])[subscript 2] Flux 105

Growth of LiMn[subscript 2]O[subscript 4] Spinel Single Crystals in a LiCl-MnCl[subscript 2] Flux 107

Nanoscale Magnesium Oxide 111

Nanostructured Pt-doped Tin Oxide Films 117

Preparation of Tetra(tert-butoxy)tin 119

Preparation of the Sol for Coating 119

Film Deposition and Annealing 121

Organically Functionalized Silica Nanoparticles 127

Synthesis of SiO[subscript 2] Nanoparticles 129

Preparation of 2-[4-(Chloromethyl)phenyl]ethyltriethoxysilane 130

Functionalization of the Silica Particles 130

Copper Nanoparticles in Silica 135

Sol-Gel Processing of Alkoxysilyl-substituted Metal Complexes 138

Oxidation 139

Reduction 140

Copper Nanocrystals 143

Assembly of TOPO-Capped Silver Nanoparticles to Multilayered Films 149

Preparation of Silver Hydrosols 151

Transfer of the Silver Nanoparticle Sol into Organic Solvents 151

Multilayered Film Synthesis 152

Colloidal Dispersion of Gold Nanoparticles 155

Preparation of HAuCl[subscript 4 middle dot]3H[subscript 2]O 157

Preparation of Gold Nanoparticles Colloidal Suspension 158

One-dimensional Nanorods and Nanowires 163

Preparation of Gold Seeds 164

Preparation of Growth Solution 164

Preparation of Gold Nanorods and Wires 165

Monolithic Tin-doped Silica Glass 169

Sol Preparation 171

Sol-Gel Transition and Drying 171

Thermal Treatment and Glass Formation 172

Sintering Process A 172

Sintering Process B 173

Octaphenyloctasilsesquioxane and Polyphenylsilsesquioxane for Nanocomposites 179

Synthesis of Phenyltriethoxysilane (PTES) 182

Synthesis of OPS and its Polymeric Analog PPS from PTES 182

Polysilsesquicarbodiimide Xerogels 193

Polyaniline - A Conducting Polymer 199

Preparation of Polyaniline Hydrochloride 201

Preparation of Polyaniline Base 204

Allyl- and Hydroxytelechelic Poly(isobutylenes) 209

Syntheses of Allyl-telechelic PIB (1) 213

Syntheses of Hydroxyl-telechelic PIBs (2) 215

Symmetrically and Unsymmetrically Substituted Phthalocyanines 217

Procedure A 221

Procedure B 223

Index 227

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