Preface Light Microscopy X-ray Diffraction Methods

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1 Preface xi 1 Light Microscopy Optical Principles Image Formation Resolution Depth of Field Aberrations Instrumentation Illumination System Objective Lens and Eyepiece Specimen Preparation Sectioning Mounting Grinding and Polishing Etching Imaging Modes Bright-Field and Dark-Field Imaging Phase Contrast Microscopy Polarized Light Microscopy Nomarski Microscopy Fluorescence Microscopy Confocal Microscopy Working Principles Three-Dimensional Images 41 References 43 Questions 43 2 X-ray Diffraction Methods X-ray Radiation Generation of X-rays X-ray Absorption Theoretical Background of Diffraction Diffraction Geometry Diffraction Intensity 56

2 vi Contents 2.3 X-ray Diffractometry Instrumentation Samples and Data Acquisition Distortions of Diffraction Spectra Applications Wide Angle X-ray Diffraction and Scattering Wide Angle Diffraction Wide Angle Scattering 74 References 76 Questions 76 3 Transmission Electron Microscopy Instrumentation Electron Sources Electromagnetic Lenses Specimen Stage Specimen Preparation Pre-Thinning Final Thinning Image Modes Mass-Density Contrast Diffraction Contrast Phase Contrast Selected Area Diffraction Selected Area Diffraction Characteristics Single-Crystal Diffraction Multi-Crystal Diffraction Kikuchi Lines Images of Crystal Defects Wedge Fringe Bending Contours Dislocations 115 References 118 Questions Scanning Electron Microscopy Instrumentation Optical Arrangement Signal Detection Probe Size and Current Contrast Formation Electron Specimen Interactions Topographic Contrast Compositional Contrast Operational Variables Working Distance and Aperture Size 134

3 vii Acceleration Voltage and Probe Current Astigmatism Specimen Preparation Preparation for Topographic Examination Preparation for Micro-Composition Examination Dehydration 142 References 143 Questions Scanning Probe Microscopy Instrumentation Probe and Scanner Control and Vibration Isolation Scanning Tunneling Microscopy Tunneling Current Probe Tips and Working Environments Operational Modes Typical Applications Atomic Force Microscopy Near-Field Forces Force Sensors Operational Modes Typical Applications Image Artifacts Tip Scanner Vibration and Operation 168 References 169 Questions X-ray Spectroscopy for Elemental Analysis Features of Characteristic X-rays Types of Characteristic X-rays Comparison of K, L and M Series X-ray Fluorescence Spectrometry Wavelength Dispersive Spectroscopy Energy Dispersive Spectroscopy Energy Dispersive Spectroscopy in Electron Microscopes Special Features Scanning Modes Qualitative and Quantitative Analysis Qualitative Analysis Quantitative Analysis 191 References 195 Questions 195

4 viii Contents 7 Electron Spectroscopy for Surface Analysis Basic Principles X-ray Photoelectron Spectroscopy Auger Electron Spectroscopy Instrumentation Ultra-High Vacuum System Source Guns Electron Energy Analyzers Characteristics of Electron Spectra Photoelectron Spectra Auger Electron Spectra Qualitative and Quantitative Analysis Qualitative Analysis Quantitative Analysis Composition Depth Profiling 221 References 222 Questions Secondary Ion Mass Spectrometry for Surface Analysis Basic Principles Secondary Ion Generation Dynamic and Static SIMS Instrumentation Primary Ion System Mass Analysis System Surface Structure Analysis Experimental Aspects Spectrum Interpretation SIMS Imaging Generation of SIMS Images Image Quality SIMS Depth Profiling Generation of Depth Profiles Optimization of Depth Profiling 246 References 250 Questions Vibrational Spectroscopy for Molecular Analysis Theoretical Background Electromagnetic Radiation Origin of Molecular Vibrations Principles of Vibrational Spectroscopy Normal Mode of Molecular Vibrations Infrared and Raman Activity 261

5 ix 9.2 Fourier Transform Infrared Spectroscopy Working Principles Instrumentation Fourier Transform Infrared Spectra Examination Techniques Fourier Transform Infrared Microspectroscopy Raman Microscopy Instrumentation Fluorescence Problem Raman Imaging Applications Interpretation of Vibrational Spectra Qualitative Methods Quantitative Methods 297 References 299 Questions Thermal Analysis Common Characteristics Thermal Events Instrumentation Experimental Parameters Differential Thermal Analysis and Differential Scanning Calorimetry Working Principles Experimental Aspects Measurement of Temperature and Enthalpy Change Applications Thermogravimetry Instrumentation Experimental Aspects Interpretation of Thermogravimetric Curves Applications 328 References 331 Questions 331 Index 333