Contributors ................................................... ix
Preface ........................................................ xi
1. Applications of Photoluminescence Spectroscopy to the
Investigation of Oxide-Containing Catalysts in the
Working State ................................................ 1
Masakazu Anpo, Stanislaw Dzwigaj, and Michel Che
1. Introduction .............................................. 3
2. Characterization of Catalytically Active Sites by PL
Spectroscopy .............................................. 4
3. Characterization of Acidic and Basic Sites by Means
of Probe Molecules and Photoluminescence Spectroscopy .... 21
4. Photoluminescence Investigations of Photocatalytic
Processes Involving Bulk Semiconductor TiO2-
Containing Photocatalysts ................................ 23
5. Effect of Pressure on Photoluminescence Spectra .......... 28
6. Effect of Temperature on Photoluminescence Spectra ....... 32
7. Use of Photoluminescence Spectroscopy in High-
Throughput Experiments ................................... 34
8. Conclusions and Outlook .................................. 35
Acknowledgments ............................................. 38
References .................................................. 39
2. Structural Characterization of Operating Catalysts
by Raman Spectroscopy ....................................... 43
Miguel A. Banares and Gerhard Mestl
1. Introduction ............................................. 45
2. Advanced Raman Spectroscopy for Characterization
of Samples in Reactive Environments ...................... 47
3. Raman Scattering ......................................... 48
4. Raman Investigations of Catalysts Under Controlled
Environments ............................................. 65
5. Perspective and Conclusions ............................. 113
Acknowledgments ............................................ 115
References ................................................. 115
3. Ultraviolet-Visible-Near Infrared Spectroscopy in
Catalysis: Theory, Experiment, Analysis, and Application
Under Reaction Conditions .................................. 129
Friederike С. Jentoft
1. Introduction ............................................ 132
2. Theoretical Background .................................. 134
3. Experimental: Optical Accessories for UV-vis-NIR
Spectroscopy in Transmission Mode ....................... 148
4. Experimental: Optical Accessories for UV-vis-NIR
Spectroscopy in Reflection Mode ......................... 149
5. Cells for Measurements in Controlled Environments ....... 160
6. Data Acquisition and Analysis ........................... 167
7. Examples ................................................ 176
8. Conclusions ............................................. 203
Acknowledgments ............................................ 205
References ................................................. 205
4. X-Ray Photoelectron Spectroscopy for Investigation
of Heterogeneous Catalytic Processes ....................... 213
Axel Knop-Gericke, Evgueni Kleimenov, Michael
Hävecker, Raoul Blume, Detre Teschner, Spiros
Zafeiratos, Robert Schlögl, Valerii I. Bukhtiyarov,
Vasily V. Kaichev, Igor P. Prosvirin, Alexander I.
Nizovskii, Hendrik Bluhm, Alexei Barinov, Pavel
Dudin, and Maya Kiskinova
1. Introduction ............................................ 216
2. History of XPS Applied at Substantial Pressures ......... 218
3. Description of XPS Apparatus ............................ 221
4. Interaction of CO with Pd(lll) .......................... 229
5. Dehydrogenation and Oxidation of Methanol on Pd(lll) .... 234
6. Ethene Epoxidation Catalyzed by Silver .................. 240
7. Methanol Oxidation Catalyzed by Copper .................. 247
8. CO Oxidation Catalyzed by Ru(0001) ...................... 256
9. Outlook ................................................. 266
Acknowledgments ............................................ 267
References ................................................. 267
5. X-ray Diffraction: A Basic Tool for Characterization of
Solid Catalysts in the Working State ....................... 273
Robert Schlögl
1. Introduction ............................................ 274
2. Objectives of XRD in Catalyst Characterization .......... 275
3. Static Versus Dynamic Analysis .......................... 284
4. Observations of Catalysts in Reactive Atmospheres ....... 287
5. Cost of Powder Diffraction Under Catalytic Conditions ... 288
6. Aim and Scope of Powder Diffraction Experiments ......... 289
7. Scattering Phenomena .................................... 289
8. Nanostructures and Diffraction .......................... 296
9. Phases in Working Catalysts ............................. 303
10.Applications of XRD to Working Catalysts ................ 307
11.Combination of XRD Data with Auxitiary Information ...... 309
12.Instrumentation ......................................... 310
13.Case Studies ............................................ 313
14.Summary and Conclusions ................................. 330
References ................................................. 332
6. Characterization of Catalysts in Reactive Atmospheres
by X-ray Absorption Spectroscopy ........................... 339
Simon R. Bare and Thorsten Ressler
1. Introduction ............................................ 342
2. Importance of XAFS Spectroscopy to Catalyst
Characterization in Reactive Atmospheres ................ 349
3. Catalytic Reactors that Serve as Cells .................. 369
4. XAFS Spectroscopy of Samples in Reactive Atmospheres
Under Static Conditions ................................. 404
5. XAFS Spectra Measured Under Dynamic Conditions .......... 428
6. Look to the Future ...................................... 446
7. Concluding Remarks ...................................... 456
Acknowledgment ............................................. 456
References ................................................. 456
Index ......................................................... 467
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