Characterization of solid materials and heterogeneous catalysts: from structure to surface reactivity
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| ISBN: | 3527326871 9783527326877 9783527645329 |
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IMAGE 1
CONTENTS
ABOUT T H E EDITORS X I X
LIST O F CONTRIBUTORS X X I
PREFACE X X V I I
MICHEL CHE A N D JACQUES C. VIDRINE GENERAL INTRODUCTION X X X I MICHEL
CHE A N D JACQUES C. VIDRINE
OVERVIEW O N PHYSICAL TECHNIQUES FOR INVESTIGATING MODEL SOLID CATALYSTS
XLV GERHARD ERTL OVERVIEW O N PHYSICAL TECHNIQUES FOR INVESTIGATING
POROUS CATALYSTS LV JOHN MEURIG THOMAS
VOLUME 1
PART O N E MOLECULAR/LOCAL SPECTROSCOPIES 1
1 INFRARED SPECTROSCOPY 3
FR6D6RIC THIBAULT-STARZYK AND FRANGOISE M A U G I 1.1 INTRODUCTION 3
1.2 PRINCIPLES O F IR SPECTROSCOPY A N D BASIC KNOWLEDGE FOR ITS U S E
1.2.1 IR LIGHT 3
1.2.2 MATTER-RADIATION INTERACTION 4
1.2.3 SPECTROMETRY, INTERFEROMETRY 4
1.2.4 LIMITATIONS O F A N D PROBLEMS WITH T H E FOURIER TRANSFORM 6
1.3 EXPERIMENTAL CONSIDERATIONS 7
1.3.1 TECHNICAL ASPECTS O F T H E FOURIER TRANSFORM 7
1.3.2 PRACTICAL I M P L E M E N T A T I O N 8
1.3.2.1 TRANSMISSION EXPERIMENTS, QUANTITATIVE ASPECTS 8 1.3.2.2 DIFFUSE
REFLECTION 9
1.4 U S E O F IR SPECTROSCOPY TO CHARACTERIZE SOLIDS 11
1.4.1 IR S P E C T R U M A N D STRUCTURE O F A SOLID 11
HTTP://D-NB.INFO/1011200287
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V I I I CONTENTS
1.4.1.1 T H E EXAMPLE O F ZEOLITES 11
1.4.1.2 SUBSTITUTION O F METALS I N T H E STRUCTURE O F ZEOLITES 13
1.4.2 ACTIVATION: CLEANING T H E S A M P L E TO OBSERVE SURFACE SITES 13
1.4.2.1 EXPERIMENTAL ASPECTS 13
1.4.2.2 ACTIVATION - CLEANING T H E S A M P L E TO OBSERVE SURFACE SITES
14 1.4.3 T H E S P E C T R U M O F O H G R O U P S 17
1.4.3.1 O H G R O U P S O N A L U M I N A 18
1.4.3.2 O H G R O U P S I N ZEOLITES 18
1.4.4 CHARACTERIZATION O F ACIDITY WITH PROBE MOLECULES 2 0
1.4.4.1 BREINSTED SITES: H Y D R O G E N BONDING A N D IR SPECTROSCOPY
21 1.4.4.2 MOLECULAR PROBES FOR LEWIS ACIDITY 2 4
1.4.4.3 C O M M O N PROBE MOLECULES FOR ACIDITY 2 4
1.4.5 CHARACTERIZATION O F BASICITY WITH PROBE MOLECULES 3 2
1.4.5.1 C 0 2 A S A PROBE FOR BASIC SITES 3 2
1.4.5.2 PROTIC MOLECULES 33
1.4.5.3 METHANOL 33
1.4.6 PROBES FOR SUPPORTED METAL CATALYSTS 3 4
1.4.7 PROBES FOR SULFIDE CATALYSTS 36
1.4.8 QUANTITATIVE ANALYSIS BY COUPLING IR SPECTROSCOPY WITH GRAVIMETRY
3 8 1.5 APPLICATION TO SURFACE REACTIVITY: OPERANDO SPECTROSCOPY 3 9
1.5.1 EXPERIMENTAL SETUP FOR OPERANDO IR SPECTROSCOPY A N D REACTIONS
CONDITIONS 4 0
1.5.2 EXAMPLES O F OPERANDO IR M E A S U R E M E N T S 4 0
1.6 CONCLUSION 4 5
REFERENCES 4 5
2 RAMAN A N D UV-RAMAN SPECTROSCOPIES 4 9
FENGTAO FAN, ZHAOCHI FENG, AND CAN LI 2.1 INTRODUCTION 4 9
2.1.1 R A M A N SPECTROSCOPY 4 9
2.1.2 FT-RAMAN SPECTROSCOPY 51
2.1.3 UV R A M A N SPECTROSCOPY 5 3
2.1.4 RESONANCE R A M A N SPECTROSCOPY 5 3
2.2 CHARACTERIZATION O F ACTIVE SITES A N D P H A S E STRUCTURE O F
METAL OXIDES 5 5
2.2.1 IDENTIFICATION O F T H E ACTIVE SPECIES O N METAL OXIDES 5 5
2.2.2 PHASE TRANSFORMATION I N T H E SURFACE REGION O F METAL OXIDES 5 6
2.3 CHARACTERIZATION O F SURFACE METAL OXIDE SPECIES O N SUPPORTED
METAL OXIDES 5 9
2.4 E L E C T R O N - P H O N O N COUPLING I N NANOSTRUCTURED MATERIALS
63
2.5 CHARACTERIZATION O F S P 2 C A R B O N MATERIALS 6 4
2.6 CHARACTERIZATION O F TRANSITION METAL-CONTAINING MICROPOROUS A N D
MESOPOROUS MATERIALS 6 7 2.6.1 IDENTIFICATION O F T H E ISOLATED
QUADRIVALENT TRANSITION METAL SITES I N MICROPOROUS A N D MESOPOROUS
MATERIALS 6 7 2.6.2 IDENTIFICATION O F T H E ISOLATED TRIVALENT
TRANSITION METAL SITES
I N MICROPOROUS A N D MESOPOROUS MATERIALS 6 9
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CONTENTS | I X
2.6.3 IDENTIFICATION O F EXTRA-FRAMEWORK ACTIVE SITES I N MICROPOROUS
A N D MESOPOROUS MATERIALS 71 2.7 SYNTHESIS M E C H A N I S M S O F
MOLECULAR SIEVES 7 3
2.7.1 ASSEMBLING ZEOLITES F R O M PREFABRICATED U N I T S 73
2.7.2 ASSEMBLING FE-ZSM-5 FROM ACTIVE CENTERS A N D SILICATE BUILDING
UNITS 74 2.7.3 A REAL-TIME PROBING FOR T H E CRYSTALLIZATION PROCESS: IN
SITU R A M A N SPECTROSCOPY 76
2.8 CONCLUSIONS 8 0
REFERENCES 81
3 ELECTRONIC SPECTROSCOPY: ULTRA VIOLET-VISIBLE A N D N E A R IR
SPECTROSCOPIES 8 9 FRIEDERIKE C.JENTOJT 3.1 INTRODUCTION A N D OVERVIEW
8 9
3.1.1 SCOPE 8 9
3.1.2 HISTORY 8 9
3.1.3 OVERVIEW 9 1
3.2 UV-VIS-NIR SPECTRA 93
3.2.1 SPECTRA REPRESENTATION 93
3.2.1.1 SPECTRAL POSITION O F ABSORPTION FEATURES 93
3.2.1.2 INTENSITY O F ABSORPTION FEATURES 93
3.2.2 SPECTRA PROCESSING 9 8
3.2.3 TRANSITIONS I N MOLECULAR SPECIES 99
3.2.3.1 SELECTION RULES 99
3.2.3.2 INDIVIDUAL MOLECULES 9 9
3.2.3.3 COMPOSITE SPECIES: METAL COMPLEXES 101 3.2.4 TRANSITIONS I N
EXTENDED SOLID STRUCTURES 104
3.2.4.1 BANDGAPS 104
3.2.4.2 METALLIC COLLOIDS: LOCALIZED SURFACE P L A S M O N RESONANCE 106
3.2.5 QUANTITATIVE ANALYSIS 107
3.3 EXPERIMENTAL CONSIDERATIONS 108
3.3.1 INSTRUMENTATION: SPECTROMETERS, SOURCES, A N D DETECTORS 108
3.3.1.1 OVERVIEW O F ESSENTIAL I N S T R U M E N T C O M P O N E N T S
108 3.3.1.2 I N S T R U M E N T SELECTION CRITERIA FOR M E A S U R E M E
N T S O F SOLIDS 110 3.3.2 OPTICAL CONFIGURATION A N D CELLS FOR
CONTROLLED ENVIRONMENTS 110
3.3.2.1 TRANSMISSION M O D E 111
3.3.2.2 CELLS FOR U S E I N T R A N S M I S S I O N M O D E 111
3.3.2.3 DIFFUSE REFLECTION MODE: INTEGRATING SPHERES 112 3.3.2.4 CELLS
FOR U S E WITH INTEGRATING SPHERES 113
3.3.2.5 DIFFUSE REFLECTION MODE: MIRROR OPTICS 115 3.3.2.6 CELLS FOR U S
E WITH MIRROR OPTICS A T T A C H M E N T 116
3.3.2.7 DIFFUSE REFLECTION MODE: FIBER-OPTIC PROBES 117 3.3.2.8 CELLS
FOR U S E WITH FIBER-OPTIC PROBES 118
3.3.2.9 C O M B I N A T I O N O F U V - V I S - N I R W I T H O T H E R
TECHNIQUES 119 3.4 FORMATION A N D ALTERATION O F SOLIDS 120
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X CONTENTS
3.4.1 PRECURSOR ANALYSIS 120
3.4.2 SOLID FORMATION 121
3.4.3 CHARACTERIZATION O F SOLIDS 122
3.4.3.1 I S O M O R P H O U S SUBSTITUTION O F FRAMEWORK CATIONS I N
ZEOLITES 123 3.4.3.2 I O N EXCHANGE I N ZEOLITES 124
3.4.3.3 DISPERSION O F SUPPORTED METAL OXIDE SPECIES 125
3.4.3.4 BANDGAP DETERMINATION I N SEMICONDUCTORS 125 3.4.3.5 SPATIALLY
RESOLVED SPECTROSCOPY O F SPECIMENS WITH COMPOSITIONAL VARIATION O N T H
E MILLIMETER SCALE 127 3.4.3.6 SPATIALLY RESOLVED SPECTROSCOPY O F
SPECIMENS WITH COMPOSITIONAL
VARIATION O N T H E MICROMETER SCALE 127 3.4.4 PROBING O F SURFACE
PROPERTIES 129
3.4.5 DYNAMIC EXPERIMENTS 129
3.4.5.1 DEHYDRATION 129
3.5 SURFACE REACTIVITY A N D CATALYSIS 130
3.5.1 OXIDATION STATE A N D COORDINATION C H A N G E S 130
3.5.1.1 OXIDATION STATE O F TRANSITION METALS I N SUPPORTED M O X M O I
E T I E S O R SOLID SOLUTIONS 130
3.5.1.2 SUPPORTED METALS: OXIDATION STATE A N D PARTICLE SIZE A N D
SHAPE 131
3.5.2 HYDROCARBON SPECIES O N SURFACES 133
3.5.2.1 REFERENCE SPECTRA 133
3.5.2.2 SURFACE HYDROCARBON POOL U N D E R REACTION CONDITIONS 137
3.5.2.3 DEACTIVATION A N D REGENERATION 138
3.6 CONCLUSIONS 139
REFERENCES 140
4 PHOTOLUMINESCENCE SPECTROSCOPY 149
MASAYA MATSUOKA, MASAKAZU SAITO, A N D MASAKAZU ANPO 4.1 INTRODUCTION
149
4.2 BASIC PRINCIPLES O F PHOTOLUMINESCENCE 150
4.3 GENERAL ASPECTS O F PHOTOLUMINESCENCE M E A S U R E M E N T S 153
4.3.1 STEADY-STATE PHOTOLUMINESCENCE M E A S U R E M E N T S 153 4.3.2
TIME-RESOLVED PHOTOLUMINESCENCE M E A S U R E M E N T S 154 4.4
CHARACTERIZATION O F CATALYSTS BY P H O T O L U M I N E S C E N C E A N
D
TIME-RESOLVED PHOTOLUMINESCENCE SPECTROSCOPY 156 4.4.1 I N SITU
PHOTOLUMINESCENCE O F MICROCRYSTALLINE M G O 156
4.4.2 IN SITU PHOTOLUMINESCENCE O F BULK T I 0 2 P H O T O C A T A L Y S
T S 159
4.4.3 IN SITU PHOTOLUMINESCENCE O F HIGHLY DISPERSED TRANSITION METAL
IONS A N D OXIDES 163
4.4.3.1 V-CONTAINING BEA ZEOLITE CATALYSTS 163 4.4.3.2 A G + / M F I
CATALYSTS 165
4.5 INVESTIGATIONS O F T H E DYNAMICS O F PHOTOCATALYSIS B Y
TIME-RESOLVED PHOTOLUMINESCENCE SPECTROSCOPY 165
IMAGE 5
CONTENTS X I
4.5.1 DYNAMICS O F PHOTOCATALYTIC REACTIONS O N T I 0 2
P H O T O C A T A L Y S T S 1 6 6
4.5.2 DYNAMICS O F PHOTOCATALYTIC REACTIONS O N HIGHLY DISPERSED
TRANSITION METAL ION A N D OXIDE CATALYSTS 169 4.5.2.1 CU +/ZEOLITE
CATALYSTS 169
4.5.2.2 TI OXIDE/ZEOLITE CATALYSTS 175
4.5.2.3 M O 0 X I D E / S I 0 2 CATALYSTS 177
4.6 CONCLUSION 182
REFERENCES 182
5 NEUTRON SCATTERING 185
HERVI JOBIC
5.1 INTRODUCTION 185
5.2 INTRODUCTION TO T H E THEORY 186
5.2.1 PROPERTIES O F N E U T R O N S 186
5.2.2 SCATTERING CROSS-SECTIONS 187
5.2.3 C O H E R E N T A N D I N C O H E R E N T SCATTERING 188
5.3 EXPERIMENTAL 190
5.4 STRUCTURE 192
5.5 DYNAMICS 194
5.5.1 VIBRATIONAL SPECTROSCOPY 195
5.5.2 DIFFUSIVE MOTIONS 197
5.5.2.1 N E U T R O N SPIN-ECHO TECHNIQUE 198
5.5.2.2 ROTATIONAL MOTION 201
5.5.2.3 TRANSLATIONAL MOTION 2 0 2
5.6 CONCLUSION 208
REFERENCES 208
6 S U M FREQUENCY GENERATION A N D INFRARED REFLECTION ABSORPTION
SPECTROSCOPY 211 KARIN FDTTINGER, CHRISTIAN WEILACH, AND CIINTHER
RUPPRECHTER 6.1 INTRODUCTION 211
6.2 THEORETICAL BACKGROUND O F SFG 213
6.2.1 SFG SIGNAL INTENSITY A N D SELECTION RULES 2 1 5
6.2.2 SURFACE CONCENTRATION (COVERAGE) A N D SFG SIGNAL INTENSITY 216
6.3 SPECTROMETER SETUP 2 1 7
6.3.1 MODES O F OPERATION 2 1 8
6.4 CASE STUDIES 221
6.4.1 METAL SINGLE-CRYSTAL SURFACES 221
6.4.2 BIMETALLIC SURFACES 2 2 8
6.4.3 OXIDE SURFACES 233
6.4.4 METAL NANOPARTICLES O N OXIDE SURFACES 240
6.5 CONCLUSION 2 4 5
REFERENCES 245
IMAGE 6
X I I | CONTENTS
7 INFRA RED REFLECTION ABSORPTION SPECTROSCOPY A N D POLARISATION
MODULATION-IRRAS 2 5 5 CHRISTOPHE MITHIVIER A N D CLAIRE-MARIE PRADIER
7.1 INTRODUCTION 2 5 5
7.1.1 S O M E HISTORY 256
7.2 PRINCIPLE O F IRAS 258
7.3 PRINCIPLE O F PM-IRAS 261
7.4 APPLICATIONS O F IRAS A N D PM-IRAS 263
7.4.1 FORMATION O F SELF-ASSEMBLED MONOLAYERS 2 6 3
7.4.2 ADSORPTION O F ORGANIC SMALL MOLECULES A N D CHIRALITY 266
7.4.3 MONITORING SURFACE REACTIVITY A N D CATALYSIS 2 6 8
7.4.3.1 OXIDATION O F C O O N R U 268
7.4.3.2 C O HYDROGENATION O N R U 2 7 0
7.4.3.3 VINYL ACETATE SYNTHESIS REACTION O N P D 2 7 0
7.4.3.4 OXIDATION O F N H 3 A N D REDUCTION O F N 2 0 BY N H 3 O N C U 2
7 2
7.4.3.5 DECOMPOSITION O F METHANOL O N P D 2 7 5
7.4.3.6 DISSOCIATION O F N O O N R H 2 7 5
7.4.3.7 REACTIVITY/STORAGE O F N O O N METAL A N D OXIDE SURFACES 2 7 7
7.4.4 SURFACE FUNCTIONALIZATION A N D ELABORATION O F SENSORS 281
7.4.5 PM-IRAS I N T H E L I Q U I D PHASE 282
7.5 CONCLUSION 285
REFERENCES 286
8 NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY 289
LYNN F. GLADDEN, MICHAL LUTECKI, A N D JAMES MCGREGOR 8.1 INTRODUCTION A
N D HISTORICAL PERSPECTIVE 289
8.2 THEORY 291
8.2.1 BASIC PRINCIPLES O F N M R 291
8.2.1.1 Z E E M A N INTERACTION 292
8.2.1.2 DIPOLAR INTERACTION 2 9 2
8.2.1.3 CHEMICAL SHIFT INTERACTION 2 9 3
8.2.1.4 Q U A D R U P O L A R INTERACTION 2 9 3
8.2.1.5 INDIRECT ELECTRON COUPLED INTERACTION 294
8.2.2 RELAXATION T I M E S 2 9 4
8.2.3 APPLICATION O F MAGNETIC FIELD GRADIENTS 2 9 5
8.2.3.1 MAGNETIC RESONANCE I M A G I N G 2 9 5
8.2.3.2 MEASURING FLOW A N D DIFFUSION 296
8.3 POPULAR N M R TECHNIQUES FOR STUDYING SOLIDS 2 9 7
8.3.1 GENERAL TECHNIQUES FOR BULK A N D SURFACE CHARACTERIZATION 298
8.3.2 STUDYING Q U A D R U P O L A R SYSTEMS W I T H I ' / 2 2 9 9
8.3.3 TECHNIQUES FOR M E A S U R I N G H E T E R O N U D E A R DIPOLAR
COUPLINGS 3 0 0
8.4 CHARACTERIZATION O F HETEROGENEOUS CATALYSTS 3 0 2
8.4.1 SILICA-AND ALUMINA-CONTAINING MATERIALS 303
8.4.1.1 P U R E SILICAS A N D A L U M I N A S 303
8.4.1.2 ZEOLITES A N D ALUMINOSILICATES 3 0 4
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CONTENTS X I I )
8.4.2 VANADIUM-CONTAINING MATERIALS 3 0 5
8.4.3 SURFACE ACIDITY A N D BASICITY 306
8.5 POROSITY, ADSORPTION, A N D TRANSPORT PROCESSES 3 0 8
8.5.1 POROSITY 3 0 8
8.5.1.1 129XE N M R 308
8.5.1.2 TI A N D T2 RELAXOMETRY 3 0 9
8.5.1.3 MAGNETIC RESONANCE I M A G I N G 3 1 0
8.5.2 ADSORPTION 311
8.5.3 DIFFUSION 3 1 2
8.6 "IN SITU" N M R 313
8.6.1 EXPERIMENTAL APPARATUS 3 1 4
8.6.1.1 BATCH CONDITIONS 314
8.6.1.2 FLOW CONDITIONS 3 1 5
8.6.2 APPLICATIONS 3 1 7
8.6.2.1 BATCH CONDITIONS 3 1 7
8.6.2.2 FLOW CONDITIONS 3 2 2
8.6.2.3 COUPLING WITH A SECOND TECHNIQUE 3 2 5
8.7 TOWARDS "OPERANDO" STUDIES 3 2 9
8.8 CONCLUSION A N D OUTLOOK 331
REFERENCES 3 3 2
9 ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY 343
PIOTR PIETRZYK, ZBIGNIEW SOJKA, A N D ELIO CIAMELLO 9.1 INTRODUCTION 343
9.1.1 INTERACTION O F MATTER WITH A MAGNETIC FIELD 343
9.1.2 EXPERIMENTAL APPROACHES I N EPR 344
9.2 PRINCIPLES O F EPR 3 4 5
9.2.1 T H E Z E E M A N EFFECT A N D T H E RESONANCE P H E N O M E N O N
346
9.2.2 SPIN RESONANCE A N D SPIN RELAXATION 3 4 8
9.3 ELECTRON-NUCLEUS HYPERFINE INTERACTION 3 5 0
9.3.1 T H E H Y D R O G E N A T O M (S = 1/2 A N D 1= 1/2) 3 5 3
9.3.2 HYPERFINE INTERACTION I N POLYNUCLEAR SYSTEMS 3 5 5
9.4 EXPERIMENTAL BACKGROUND 3 5 6
9.5 ANISOTROPY O F MAGNETIC INTERACTIONS I N EPR: T H E G, A , A N D D
TENSORS 3 5 9
9.5.1 T H E G TENSOR 361
9.5.2 T H E A TENSOR 3 6 2
9.5.3 T H E ELECTRON-ELECTRON INTERACTIONS I N S 1/2 SYSTEMS: T H E D
TENSOR 3 6 3
9.5.4 T H E SPIN-HAMILTONIAN 3 6 6
9.6 EPR SPECTRA A N D T H E SOLID STATE: SINGLE CRYSTAL VERSUS POWDERS 3
6 6
9.6.1 POWDER EPR SPECTRA 3 6 7
9.7 GUIDELINES TO INTERPRETATION O F EPR SPECTRA 3 6 8
9.7.1 CLASSIFICATION O F EPR SPECTRA A N D D E T E R M I N A T I O N O F
SPECTRAL PARAMETERS 3 6 8
IMAGE 8
X I V CONTENTS
9.7.2 U N U S U A L SPECTRAL FEATURES A N D PUZZLING LINESHAPES 3 7 2
9.7.3 DYNAMIC LINESHAPE EFFECTS A N D PARTIALLY AVERAGED SIGNALS 376 9.8
C O M P U T E R SIMULATION O F POWDER SPECTRA 378
9.9 MOLECULAR INTERPRETATION O F PARAMETERS 3 8 0
9.9.1 G-TENSOR 3 8 0
9.9.2 HYPERFINE TENSOR 383
9.10 Q U A N T U M CHEMICAL CALCULATIONS O F MAGNETIC
PARAMETERS 386
9.11 ADVANCED EPR TECHNIQUES 3 8 8
9.11.1 ELECTRON SPIN ECHO-BASED TECHNIQUES 388
9.12 CHARACTERISTICS O F EPR TECHNIQUES I N APPLICATION TO CATALYSIS A N
D SURFACES 3 8 9
9.12.1 DISTINCTION BETWEEN SURFACE A N D BULK SPECIES 3 9 0
9.12.2 POORLY RESOLVED SPECTRA - MULTIFREQUENCY APPROACH 3 9 2 9.12.3
OVERLAPPING SIGNALS 394
9.12.4 STRAIN BROADENING A N D S M E A R I N G O F FEATURES WITH H I G H
ANGULAR ANISOTROPY 3 9 5 9.12.5 U S E O F PROBE MOLECULES A N D SPIN
LABELS 3 9 6
9.13 INTERFACIAL A N D SURFACE CHARGE-TRANSFER PROCESSES 398
9.14 IN SITU A N D OPERANDO EPR TECHNIQUES 399
9.15 CONCLUSIONS A N D PROSPECTS 403
REFERENCES 403
10 MOSSBAUER SPECTROSCOPY 4 0 7
LORENZO STIEVANO A N D FRIEDRICH E. WAGNER 10.1 INTRODUCTION 4 0 7
10.2 T H E M O S S B A U E R EFFECT 4 0 9
10.3 RADIATION SOURCE 411
10.4 M O S S B A U E R ABSORBERS 4 1 4
10.5 HYPERFINE INTERACTIONS 414
10.5.1 ELECTRIC MONOPOLE INTERACTION 415
10.5.2 MAGNETIC DIPOLE INTERACTION 4 1 7
10.5.3 ELECTRIC Q U A D R U P O L E INTERACTION 419
10.6 EXPERIMENTAL SETUPS 421
10.6.1 TRANSMISSION MOSSBAUER SPECTROSCOPY 421 10.6.2 SURFACE-SENSITIVE
MOSSBAUER SPECTROSCOPY 422 10.6.3 EMISSION MOSSBAUER SPECTROSCOPY 423
10.7 EVALUATION O F EXPERIMENTAL DATA 4 2 4
10.7.1 SPECTRA FOLDING 424
10.7.2 SPECTRA FITTING 4 2 4
10.8 THEORETICAL CALCULATION O F M O S S B A U E R PARAMETERS 426
10.9 C O M M O N MOSSBAUER-ACTIVE TRANSITIONS 4 2 7
10.9.1 T H E 14.4KEV M O S S B A U E R TRANSITION O F 57FE 427
10.9.2 T H E 89.4 KEV M O S S B A U E R TRANSITION O F " R U 4 2 9
10.9.3 T H E 23.9 KEV M O S S B A U E R TRANSITION O F U 9 S N 4 3 0
IMAGE 9
10.9.4
10.9.5 10.9.6 10.10
10.10.1
10.10.1.1
10.10.1.2
10.10.1.3
10.10.1.4
10.10.2 10.10.2.1
10.10.2.2
10.10.2.3
10.10.3 10.11
N
11.1 11.2 11.2.1 1 1 . 2 . 2
11.3
11.3.1 11.3.2 11.4 11.4.1 11.4.2
11.4.3 11.5 1 1 . 6
1 1 . 6 . 1
1 1 . 6 . 2
11.6.3
11.6.4 11.6.4.1
CONTENTS X V
T H E 37.1 KEV MOSSBAUER TRANSITION O F 121SB 4 3 2
T H E 73.0 KEV M O S S B A U E R TRANSITION O F 1 9 3 I R 4 3 2 T H E
77.3 KEV M O S S B A U E R TRANSITION O F 197AU 433 SURVEY O F
APPLICATIONS O F T H E MOSSBAUER EFFECT I N T H E STUDY O F CATALYTIC
MATERIALS 434
197AU M O S S B A U E R SPECTROSCOPY I N T H E STUDY O F GOLD
CATALYSTS 4 3 5
ELECTRONIC PROPERTIES: A U / A 1 2 0 3 O X I D A T I O N CATALYSTS 4 3 5
DETERMINATION O F CHEMICAL COMPOSITION: SUPPORTED A U P D ALLOYS 436
DETERMINATION O F L A M B - M O S S B A U E R / F A C T O R S FOR
QUANTITATIVE
ANALYSES: AU/ACTIVATED C A R B O N CATALYSTS FOR T H E HYDROCHLORINATION
O F ACETYLENE 4 3 7
IDENTIFICATION O F SURFACE SPECIES: GOLD NANOPARTICLES E M B E D D E D
I N MYLAR 438
57FE MOSSBAUER SPECTROSCOPIC STUDY O F IRON-CONTAINING CATALYSTS 4 3 9
S U P E R P A R A M A G N E T I S M A N D T H E DETERMINATION O F
PARTICLE SIZES: F E / C CATALYSTS FOR C O HYDROGENATION 4 4 0 IN SITU
MEASUREMENTS: IRON-BASED FISCHER-TROPSCH CATALYSTS 443 EMISSION M O S S
B A U E R SPECTROSCOPY: COBALT-BASED FISCHER-TROPSCH
CATALYSTS 4 4 4
U 9 S N MOSSBAUER STUDY O F BIMETALLIC TIN-CONTAINING CATALYSTS 4 4 6
CONCLUSION 4 4 7
REFERENCES 448
LOW ENERGY ION SCATTERING A N D SECONDARY ION M A S S SPECTROMETRY 453
NORBERT KRUSE AND SERGEY CHENAKIN
INTRODUCTION 453
SECONDARY I O N MASS SPECTROMETRY 4 5 7 BASIC PRINCIPLES 457 POTENTIAL O
F SIMS 4 5 9
LOW-ENERGY ION SCATTERING (ION SCATTERING SPECTROSCOPY) 461 M A I N
CONCEPTS 461
POTENTIALITIES O F LE1S 463 SINGLE-CRYSTAL A N D POLYCRYSTALLINE METAL
SURFACES 4 6 5 SURFACE DEFECTS A N D ADSORPTION O F SIMPLE MOLECULES 4 6
5 ADSORPTION O F ORGANIC MOLECULES 469
OXIDATION A N D CORROSION 4 7 0 A M O R P H O U S METALLIC ALLOYS 4 7 2
FROM MODEL TO REAL CATALYSTS 4 7 4 STRUCTURAL EFFECTS 4 7 4
DISPERSION EFFECTS 4 7 7 PREPARATION A N D ACTIVATION EFFECTS 4 8 0
COMPOSITIONAL EFFECTS I N VARIOUS CATALYTIC REACTIONS 4 8 4
C O HYDROGENATION 4 8 4
IMAGE 10
CONTENTS
11.6.4.2 HYDROCARBON OXIDATION 486
11.6.4.3 HYDROGENATION A N D OXIDATIVE DEHYDROGENATION 489 11.6.5 P R O
M O T I O N A N D POISONING EFFECTS 4 8 9
11.6.5.1 C O HYDROGENATION TO METHANOL 4 9 0
11.6.5.2 C O OXIDATION 4 9 0
11.6.5.3 HYDROCARBON PARTIAL A N D TOTAL OXIDATION 4 9 2 11.6.5.4
CRACKING 4 9 4
11.6.5.5 B E C K M A N N R E A R R A N G E M E N T 4 9 4
11.6.5.6 ALDOSE OXIDATION 4 9 5
11.6.5.7 NITRITE A N D NITRATE REDUCTION 4 9 5
11.6.5.8 CL-RELATED EFFECTS I N VARIOUS REACTIONS 4 9 6 11.6.6 ACTIVE
SITES 4 9 7
11.7 CONCLUSION 501
REFERENCES 5 0 2
12 X-RAY ABSORPTION SPECTROSCOPY 511
CHRISTOPHE CEANTET A N D CHRISTOPHE PICHON 12.1 INTRODUCTION 511
12.2 HISTORY O F X-RAY ABSORPTION SPECTROSCOPY 511
12.3 PRINCIPLE O F X-RAY ABSORPTION SPECTROSCOPY; XANES, EXAFS 5 1 2
12.4 EXPERIMENTATION A N D DATA PROCESSING 5 1 5
12.5 APPLICATION T O OXIDE MATERIALS 521
12.6 APPLICATIONS TO T H E STUDY O F SULFIDE CATALYSTS 5 2 4
12.6.1 STRUCTURE O F T H E ACTIVE PHASE 524
12.6.2 ACTIVATION O F SULFIDE CATALYSTS 525
12.7 APPLICATION TO METAL CATALYSTS 527
12.7.1 STRUCTURE A N D SIZE O F (BI-)METALLIC PARTICLES 5 2 8
12.7.2 EVOLUTION O F T H E BIMETALLIC STRUCTURE U N D E R REACTION O R
POISONING C O N D I T I O N S 5 3 0
12.8 CONCLUSION A N D PERSPECTIVES 533
REFERENCES 5 3 4
13 AUGER ELECTRON, X RAY A N D UV PHOTOELECTRON SPECTROSCOPIES 5 3 7
WOLFGANG CRUNERT
13.1 INTRODUCTION 537
13.1.1 T H E RELATION BETWEEN XPS, UPS, A N D AES 5 3 7
13.1.2 A G L I M P S E AT HISTORY 539
13.2 SOURCES O F ANALYTICAL INFORMATION 5 4 0
13.2.1 XPS BINDING ENERGIES 5 40
13.2.1.1 PARAMETERS AFFECTING XPS BINDING ENERGIES 5 4 0 13.2.1.2
THEORETICAL PREDICTION O F XPS BINDING ENERGIES 5 4 5 13.2.1.3 PRACTICAL
ASPECTS 5 47
13.2.2 T H E ANALYTICAL POTENTIAL O F XPS LINESHAPES 548
13.2.2.1 S P I N - O R B I T SPLITTING 548
13.2.2.2 C H A R G E TRANSFER SATELLITES 5 4 9
IMAGE 11
CONTENTS X V I I
13.2.2.3 O T H E R SHAKE-UP TYPE SATELLITES 5 5 0
13.2.2.4 MULTIPLET SPLITTING 551 13.2.3 SURFACE SENSITIVITY; WORKING
WITH XPS INTENSITIES 553 13.2.3.1 H O M O G E N E O U S A N D I N H O M
O G E N E O U S S A M P L I N G REGION 5 5 3 13.2.3.2 INCREASING T H E
SURFACE SENSITIVITY O F XPS 5 5 7 13.2.3.3 D E T E R M I N I N G XPS
INTENSITIES - LINESHAPES A N D SIGNAL
BACKGROUNDS 5 6 0
13.2.4 XAES A N D XPS - STRUCTURAL SENSITIVITY VIA T H E AUGER P A R A M
E T E R 5 6 2 13.2.5 ULTRAVIOLET PHOTOELECTRON SPECTROSCOPY 5 6 5 13.2.6
XPS A N D O T H E R METHODS 566
13.3 I N S T R U M E N T A T I O N 5 6 7
13.3.1 CONVENTIONAL XPS 5 6 7
13.3.2 LATERAL RESOLUTION, I M A G I N G 5 6 9
13.3.3 AMBIENT-PRESSURE PHOTOELECTRON SPECTROSCOPY (APPES) 5 7 0 13.4
CASE STUDIES 571
13.4.1 COMBINATION O F METHODS: STRONG METAL-SUPPORT INTERACTION I N A A
G / T I 0 2 CATALYST 571 13.4.2 DEPTH RESOLUTION: T H E SURFACE C O M P
O S I T I O N O F STOICHIOMETRIC BULK MIXED VANADATES A N D MOLYBDATES
573 13.4.3 APPES: O N T H E DOORSTEP O F A N E W AGE O F XPS 5 7 4
13.5 OUTLOOK 5 7 8
REFERENCES 5 7 9
14 SINGLE MOLECULE SPECTROSCOPY 585
TIMO LEBOLD, JENS MICHAELIS, THOMAS BEIN, A N D CHRISTOPH BRDUCHLE 14.1
INTRODUCTION 585
14.2 DESCRIPTION O F T H E METHOD 5 8 6
14.3 EXPERIMENTAL CONSIDERATIONS A N D CONSTRAINTS 591
14.4 MESOPOROUS SILICA MATERIALS 5 9 2
14.5 SELECTED STUDIES 5 9 3
14.5.1 CORRELATING DYNAMIC A N D STRUCTURAL INFORMATION BY C O M B I N I
N G SINGLE-MOLECULE MICROSCOPY A N D HIGH-RESOLUTION T R A N S M I S S I
O N ELECTRON MICROSCOPY 5 9 3
14.5.2 ANALYZING T H E DIFFUSION DYNAMICS W I T H I N A SILICA MESOPORE
WITH ONE-CHANNEL ACCURACY U S I N G SINGLE-MOLECULE MICROSCOPY A N D
SINGLE-PARTICLE TRACKING 5 9 5
14.5.3 ANALYZING ORIENTATIONAL A N D SPECTRAL DYNAMICS AT ADSORPTION
SITES INSIDE A CTAB TEMPLATED T H I N MESOPOROUS SILICA FILM 5 9 8
14.5.4 VISUALIZATION O F T H E M E C H A N I S M S GOVERNING T H E
STRUCTURE FORMATION O F MESOPOROUS SILICA N A N O C H A N N E L S 601
14.6 CONCLUSION 605
REFERENCES 605
IMAGE 12
X V I I I J CONTENTS
VOLUME 2
PART TWO MACROSCOPIC TECHNIQUES 609
15 X-RAY DIFFRACTION A N D SMALL ANGLE X-RAY SCATTERING 611
MATTE BEHRENS A N D ROBERT SCHLDGL
16 TRANSMISSION ELECTRON MICROSCOPY 6 5 5
JOHN MEURIG THOMAS A N D CATERINA DUCATI
17 SCANNING PROBE MICROSCOPY A N D SPECTROSCOPY 703
TOMOAKI NISHINO
18 THERMAL METHODS 7 4 7
ADRIEN MEKKI-BERRADA A N D ALINE AUROUX
19 SURFACE AREA/POROSITY, ADSORPTION, DIFFUSION 853
PHILIP L. LLEWELLYN, EMILY BLOCH, A N D SANDRINE BOURRELLY
PART THREE CHARACTERIZATION O F T H E FLUID P H A S E (CAS A N D / O R
LIQUID) 881
2 0 M A S S SPECTROMETRY 883
SANDRA ALVES AND JEAN-CLAUDE TABET
21 CHROMATOGRAPHIC METHODS 953
FABRICE BERTONCINI, DIDIER THIEBAUT, MARION COURTIADE, A N D THOMAS
DUTRIEZ
22 TRANSIENT TECHNIQUES: TEMPORAL ANALYSIS O F PRODUCTS A N D
STEADY STATE ISOTOPIC TRANSIENT KINETIC ANALYSIS 1013 ANGELOS M.
EFSTATHIOU, JOHN T. CLEAVES, AND GREGORY S. YABLONSKY
PART FOUR ADVANCED CHARACTERIZATION 1075
23 TECHNIQUES COUPLING FOR CATALYST CHARACTERISATION 1077
ANDREW M. BEALE, MATTHEW C. O'BRIEN, A N D BERT M. WECKHUYSEN
2 4 Q U A N T U M CHEMISTRY METHODS 1119
PHILIPPE SAUTET
CONCLUSIONS 1147 MICHEL CHE AND JACQUES C. VDDRINE
INDEX 1153 |
| any_adam_object | 1 |
| building | Verbundindex |
| bvnumber | BV039727640 |
| classification_rvk | UH 6300 UH 6320 UM 3200 VE 7040 VE 9350 VG 8900 |
| classification_tum | WER 020f CHE 194f WER 700f CHE 167f CHE 236f |
| ctrlnum | (DE-599)DNB1011200287 |
| discipline | Chemie / Pharmazie Physik Werkstoffwissenschaften Chemie |
| format | Book |
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| id | DE-604.BV039727640 |
| illustrated | Not Illustrated |
| indexdate | 2024-07-21T00:16:56Z |
| institution | BVB |
| isbn | 3527326871 9783527326877 9783527645329 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-024575606 |
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| publisher | Wiley-VCH |
| record_format | marc |
| spelling | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity Weinheim Wiley-VCH txt rdacontent n rdamedia nc rdacarrier Werkstoffkunde (DE-588)4079184-1 gnd rswk-swf Katalysator (DE-588)4029919-3 gnd rswk-swf Spektroskopie (DE-588)4056138-0 gnd rswk-swf Strukturaufklärung (DE-588)4183788-5 gnd rswk-swf Katalysator (DE-588)4029919-3 s Strukturaufklärung (DE-588)4183788-5 s Spektroskopie (DE-588)4056138-0 s DE-604 Werkstoffkunde (DE-588)4079184-1 s Che, Michel Sonstige oth Erscheint auch als Online-Ausgabe, EPUB 978-3-527-64533-6 Erscheint auch als Online-Ausgabe, MOBI 978-3-527-64535-0 Erscheint auch als Online-Ausgabe, PDF 978-3-527-64534-3 X:MVB text/html http://deposit.dnb.de/cgi-bin/dokserv?id=3718066&prov=M&dok_var=1&dok_ext=htm Inhaltstext DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=024575606&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity Werkstoffkunde (DE-588)4079184-1 gnd Katalysator (DE-588)4029919-3 gnd Spektroskopie (DE-588)4056138-0 gnd Strukturaufklärung (DE-588)4183788-5 gnd |
| subject_GND | (DE-588)4079184-1 (DE-588)4029919-3 (DE-588)4056138-0 (DE-588)4183788-5 |
| title | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_auth | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_exact_search | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_full | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_fullStr | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_full_unstemmed | Characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_short | Characterization of solid materials and heterogeneous catalysts |
| title_sort | characterization of solid materials and heterogeneous catalysts from structure to surface reactivity |
| title_sub | from structure to surface reactivity |
| topic | Werkstoffkunde (DE-588)4079184-1 gnd Katalysator (DE-588)4029919-3 gnd Spektroskopie (DE-588)4056138-0 gnd Strukturaufklärung (DE-588)4183788-5 gnd |
| topic_facet | Werkstoffkunde Katalysator Spektroskopie Strukturaufklärung |
| url | http://deposit.dnb.de/cgi-bin/dokserv?id=3718066&prov=M&dok_var=1&dok_ext=htm http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=024575606&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT chemichel characterizationofsolidmaterialsandheterogeneouscatalystsfromstructuretosurfacereactivity |