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Title Inorganic micro- and nanomaterials : synthesis and characterization / edited by Angela Dibenedetto, Michele Aresta
Published Berlin : Walter de Gruyter GmbH & Co. KG, [2013]
Table of Contents
 Introduction: Nano- (and micro-)materials and human wellbeing1
1.Coating antibacterial nanoparticles on textiles: Towards the future hospital in which all textiles will be antibacterial3
1.1.Introduction: Application of nanotechnology for "smart" textiles3
1.2.Sonochemical method for the synthesis of nanostructured materials and their adherence to solid substrates6
1.3.Ultrasound assisted deposition of metal nano-oxides on textiles and their antibacterial properties8
1.3.1.Synthesis and deposition of CuO nanoparticles8
1.3.2.Finishing of textiles with crystalline TiO2 nanoparticles via a one-step process10
1.3.3.Synthesis and deposition of ZnO16
1.3.4.Enzymatic pretreatment as a means of enhancing antibacterial activity and stability of ZnO nanoparticles sonochemically coated on cotton fabrics22
1.3.5.Size dependence of the antibacterial activity of ZnO NPs28
1.4.Conclusion28
 Bibliography29
2.Automated solutions for high-throughput experimentation in heterogeneous catalyst research35
2.1.Introduction35
2.2.The preparation of solid catalysts37
2.3.Automation challenges examples37
2.3.1.Integration of commercially available devices38
2.4.A fully-automated solution39
2.4.1.SOPHAS-CAT HT39
2.4.2.The loading39
2.4.3.The synthesizer40
2.4.4.Extrudate preparation41
2.4.5.Impregnation and drying41
2.4.6.Calcination42
2.4.7.Scraping and pelletizing42
2.4.8.Grinding43
2.4.9.Sieving43
2.5.Conclusion44
 Bibliography45
3.Insights from XPS on nanosized inorganic materials47
3.1.Introduction47
3.2.XPS in the nanodomain47
3.3.Conclusions53
 Bibliography55
4.Single crystal and powder XRD techniques: An overview57
4.1.The single crystal XRD technique57
4.1.1.Basics of the radiation-matter interaction58
4.1.2.Basics of crystallography and X-ray diffraction by crystal61
4.1.3.Solving the phase problem by direct methods69
4.2.The powder XRD technique74
4.2.1.Indexation74
4.2.2.Space group determination76
4.2.3.Profile decomposition and intensity extraction77
4.2.4.Structure solution79
4.2.5.Rietveld refinement84
4.2.6.Examples85
4.3.Conclusions88
 Bibliography89
5.Structural and electronic characterization of nanosized inorganic materials by X-ray absorption spectroscopies93
5.1.Introduction93
5.2.XAS spectroscopy: Basic background93
5.2.1.Theoretical background of XAS spectroscopy94
5.2.2.The XANES region96
5.2.3.The EXAFS region96
5.2.4.Advantages and drawbacks of the technique99
5.3.CuCl2/Al2O3-based catalysts for ethylene oxychlorination100
5.3.1.Industrial relevance of the CuCl2/Al2O3 system100
5.3.2.Preliminary in situ XAFS experiments101
5.3.2.1.The determination of the Cu-aluminate phase: How to avoid possible pitfalls in the EXAFS data analysis101
5.3.2.2.Catalyst reactivity with the separate reactants: In situ XAFS experiments103
5.3.3.Operando experiments and criteria used to face the presence of more than one phase in the sample105
5.4.Structural and electronic configuration of Cp2Cr molecules encapsulated in PS and Na-Y zeolite and their reactivity towards CO109
5.4.1.Structure of Cp2Cr encapsulated in PS and Na-Y zeolite matrices109
5.4.2.Determination of the electronic structure of Cp2Cr by combined UV-Vis and XANES spectroscopies111
5.4.3.Reactivity of Cp2Cr hosted in PS and in Na-Y zeolite towards CO: IR and XAFS results114
5.5.Transition metal complexes in solution: The [cis-Ru(bpy)2(py)2]2+ case study117
5.5.1.Structure refinement of cis-[Ru(bpy)2(py)2]2+ in aqueous solution by EXAFS spectroscopy118
5.5.2.Advanced details of the EXAFS structure refinement of cis-[Ru(bpy)2(py)2]2+ complex120
5.6.EXAFS study on MOFs of the UiO-66/UiO-67 family: comparison with XRPD and ab initio investigations122
5.7.Applications of X-ray micro beams: Electroabsorption modulated Alaser for optoelectronic devices127
 Bibliography129
6.Lens-less scanning X-ray microscopy with SAXS and WAXS contrast137
6.1.Introduction137
6.2.X-ray microscopes138
6.3.Small-angle and wide-angle scattering contrast (SAXS and WAXS)143
6.4.Applications149
 Bibliography154
7.Characterization of inorganic nanostructured materials by electron microscopy157
7.1.Introduction157
7.2.Electron microscopy158
7.2.1.Working principles159
7.3.Scanning electron microscopy161
7.3.1.Magnification and resolution of SEM163
7.3.2.Interaction of the electron beam with the sample: elastic and inelastic scattering163
7.3.2.1.Secondary electrons and their detection164
7.3.2.2.Backscattered electrons and their detection166
7.3.23.Energy loss167
7.4.Transmission electron microscopy167
7.4.1.The instrument168
7.4.2.Image formation process169
7.5.Sample preparation for electron microscopy174
7.5.1.SEM sample preparation174
7.5.1.1.Casting174
7.5.1.2.Ion sputtering175
7.5.2.Sample preparation for TEM175
7.6.Inorganic nanocrystal investigation by SEM177
7.7.Inorganic nanocrystal investigation by TEM186
7.7.1.Bright field mode186
7.7.2.Dark field contrast mode189
7.7.3.Diffraction mode -- electron diffraction190
7.7.3.1.Selected area diffraction191
7.7.3.2.Convergent beam electron diffraction191
7.733.Investigating crystalline structure: High-resolution TEM192
7.8.Chemical analysis by electron microscopy193
7.8.1.Energy dispersion spectroscopy (EDS)193
7.8.2.Electron energy loss spectroscopy (EELS)194
7.8.3.Energy-filtered transmission electron microscopy (EFTEM)195
7.8.4.Some examples of chemical analysis in electron microscopy195
7.9.Conclusions197
 Bibliography197
8.Nanosized particles: questioned for their potential toxicity, but some are applied in biomedicine199
8.1.Introduction199
8.2.Nanoparticles classification199
8.3.Nanoparticles and biosystems201
8.4.Stability and toxicity202
8.5.Fields of application of engineered nanoparticles203
8.6.Access to bio-organisms and toxicity to organisms204
8.7.Applications of nanoparticles in biomedicine205
8.8.Measurement of the concentration206
8.9.Conclusions206
 Bibliography207
 Index211
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Description 1 online resource
Summary The demand for new materials with novel properties on the micro- and nano-scale continues to grow. This book provides an overview of state-of-the-art techniques for the synthesis and characterization of inorganic nanomaterials including techniques such as XPS, XAS, single crystal X-ray diffraction, X-ray microimaging, electron microscopy, and solid state NMR. Essential for all researchers in nanoscience
Bibliography Includes bibliographical references and index
Notes Print version record
Subject Chemistry, Inorganic.
Nanostructured materials.
Form Electronic book
Author Aresta, Michele, 1940- editor
Dibenedetto, Angela, editor
ISBN 1306091837 (electronic bk.)
1680152556 (electronic bk.)
3110306875 (electronic bk.)
9781306091831 (electronic bk.)
9781680152555 (electronic bk.)
9783110306873 (electronic bk.)