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Summary
Experts must be able to analyze and distinguish all materials, or combinations of materials, in use today - whether they be metals, ceramics, polymers, semiconductors, or composites. To understand a material's structure, how that structure determines its properties, and how that material will subsequently work in technological applications, researchers apply basic principles of chemistry, physics, and biology to address its scientific fundamentals, as well as how it is processed and engineered for use. Emphasizing practical applications and real-world case studies, Materials Characterization Techniques presents the principles of widely used, advanced surface and structural characterization techniques for quality assurance, contamination control, and process improvement.
Table of Contents
| Preface | p. xiii |
| Introduction | p. 1 |
| Contact Angle in Surface Analysis | p. 3 |
| Introduction | p. 3 |
| Measuring Contact Angle | p. 6 |
| Static and Dynamic Sessile Drop Method | p. 7 |
| Static Contact Angle | p. 8 |
| Dynamic Contact Angle | p. 8 |
| Dynamic Wilhelmy Method | p. 10 |
| Captive Air Bubble Method | p. 11 |
| Capillary Rise Method | p. 11 |
| Tilted-Drop Measurement | p. 11 |
| Determining Surface Energy of a Homogeneous Solid Surface | p. 11 |
| Surface Tension Component | p. 13 |
| Zisman | p. 13 |
| Fowkes | p. 14 |
| Owens-Wendt-Kaelble | p. 15 |
| Lifshitz-van der Waals/Acid-Base (van Oss) | p. 16 |
| Wu | p. 16 |
| Equation of State | p. 18 |
| Antonow's Rule | p. 18 |
| Berthelot's Rule | p. 18 |
| Work Examples | p. 19 |
| Fowkes | p. 19 |
| Case Study-Surface Energy of Amorphous Carbon | p. 21 |
| Summary | p. 23 |
| References | p. 24 |
| X-ray Photoelectron Spectroscopy and Auger Electron Spectroscopy | p. 27 |
| Introduction | p. 27 |
| Atomic Model and Electron Configuration | p. 28 |
| Energy Levels | p. 30 |
| Spin-Orbit Splitting | p. 31 |
| Mean Free Path | p. 33 |
| Principles of XPS and AES | p. 34 |
| Photoionization | p. 34 |
| Auger Electron Generation | p. 36 |
| Background Subtraction | p. 39 |
| Chemical Shift in XPS | p. 42 |
| Quantitative Analysis | p. 44 |
| Line Shape | p. 52 |
| Depth Profiling | p. 55 |
| Instrumentation | p. 56 |
| The Vacuum System | p. 57 |
| X-ray Sources | p. 57 |
| Monochromator | p. 59 |
| Generation of Electron Beam | p. 60 |
| Analyzers | p. 62 |
| Electron Detectors | p. 63 |
| Channel Electron Multipliers | p. 64 |
| Channel Plates | p. 64 |
| Samples | p. 64 |
| Accessories | p. 65 |
| Routine Limits of XPS | p. 65 |
| Quantitative Accuracy | p. 65 |
| Analysis Times | p. 66 |
| Detection Limits | p. 66 |
| Analysis Area Limits | p. 66 |
| Sample Size Limits | p. 66 |
| Degradation During Analysis | p. 66 |
| Comparison Between AES and XPS, Energy-Dispersive X-ray Spectroscopy | p. 67 |
| XPS Applications and Case Studies | p. 67 |
| Determination of Doping Effect | p. 68 |
| Chemical Reaction Determination | p. 70 |
| Determination of Chemical Valence | p. 73 |
| Depth Profiling | p. 74 |
| Overlapping Problem | p. 81 |
| Determination of Film Composition | p. 82 |
| AES Applications | p. 85 |
| Surface Element Determination | p. 85 |
| Concentration and Stoichiometry Determination | p. 85 |
| Intensity-Time Curve | p. 86 |
| Chemical Shift | p. 87 |
| Line Shape Changes | p. 88 |
| Depth Profiling | p. 88 |
| Summary | p. 89 |
| References | p. 90 |
| Scanning Tunneling Microscopy and Atomic Force Microscopy | p. 95 |
| Introduction | p. 95 |
| Working Principle | p. 97 |
| Scanning Tunneling Microscopy | p. 97 |
| Atomic Force Microscopy | p. 98 |
| Instrumentation | p. 100 |
| Tip and Cantilever | p. 101 |
| Piezoelectric Scanner | p. 101 |
| Vibration Isolation | p. 104 |
| Resolution | p. 104 |
| Modes of Operation | p. 106 |
| Scanning Tunneling Microscopy | p. 106 |
| Constant Current Mode | p. 106 |
| Constant Height Mode | p. 106 |
| Atomic Force Microscopy | p. 106 |
| Contact Mode | p. 106 |
| Noncontact Mode | p. 107 |
| Tapping Mode | p. 108 |
| Differences between STM and AFM | p. 109 |
| Applications | p. 110 |
| STM Studies | p. 112 |
| AFM Studies | p. 115 |
| References | p. 120 |
| X-ray Diffraction | p. 125 |
| X-ray Characteristics and Generation | p. 125 |
| Lattice Planes and Bragg's Law | p. 127 |
| Powder Diffraction | p. 131 |
| Thin Film Diffraction | p. 134 |
| Texture Measurement | p. 142 |
| Grazing Angle X-ray Diffraction | p. 145 |
| Acknowledgments | p. 149 |
| References | p. 149 |
| Transmission Electron Microscopy | p. 153 |
| Basics of Transmission Electron Microscopes | p. 153 |
| Reciprocal Lattice | p. 155 |
| Specimen Preparation | p. 160 |
| Bright-Field and Dark-Field Images | p. 167 |
| Electron Energy Loss Spectroscopy | p. 170 |
| Acknowledgments | p. 175 |
| References | p. 175 |
| Scanning Electron Microscopy | p. 177 |
| Introduction to Scanning Electron Microscopes | p. 177 |
| Historical Background | p. 177 |
| Scanning Electron Microscopy Principles | p. 178 |
| The Electron Gun | p. 180 |
| The Condenser and Objective Lenses | p. 181 |
| Scanning Coils | p. 183 |
| Specimen Chamber | p. 184 |
| Electron Beam-Specimen Interaction | p. 184 |
| Backscattered Electrons | p. 187 |
| Secondary Electrons | p. 188 |
| Characteristic X-ray and Auger Electron Production | p. 188 |
| SEM Operating Parameters | p. 190 |
| General Aspects | p. 190 |
| SEM Characteristics | p. 190 |
| Resolution | p. 190 |
| Depth of Field | p. 191 |
| SEM Operational Parameters | p. 192 |
| Applications | p. 193 |
| Application of SEM in the Synthesis of Diamond Films | p. 193 |
| Applications of SEM in Electronic Devices | p. 196 |
| Fabrication of Diamond Microcantilevers | p. 196 |
| Fabrication of Field Emitters | p. 197 |
| Application of SEM in the Synthesis of SiC Coatings | p. 197 |
| SEM Analysis of Diamond-Coated WC-Co Substrate | p. 200 |
| References | p. 205 |
| Chromatographic Methods | p. 207 |
| Introduction | p. 207 |
| General Principles of Chromatography | p. 209 |
| Classification of Chromatography | p. 211 |
| Normal-Phase and Reverse-Phase Chromatography | p. 211 |
| Separation Modes and Mechanisms | p. 212 |
| Adsorption Chromatography | p. 212 |
| Partition Chromatography | p. 212 |
| Bonded-Phase Chromatography | p. 213 |
| Ion Exchange Chromatography | p. 213 |
| Affinity Chromatography | p. 213 |
| Size Exclusion Chromatography | p. 214 |
| Fundamentals About Partition and Retention | p. 214 |
| Partition and Partition Theory | p. 214 |
| Ion Exchange Chromatography | p. 217 |
| Factors Affecting Separation by IEC | p. 218 |
| Separating Proteins | p. 219 |
| Gel Permeation Chromatography | p. 220 |
| Molecular Weights and Molecular Weight Distribution | p. 221 |
| Operation of GPC | p. 222 |
| Polymer Standards and Calibration Curve | p. 223 |
| Sample Preparation | p. 224 |
| GPC for Water-Soluble Polymers | p. 225 |
| Gel Electrophoresis Chromatography | p. 225 |
| Capillary Electrophoresis | p. 226 |
| Gel Electrophoresis | p. 226 |
| Molecular Weight Markers | p. 229 |
| DNA Electrophoresis | p. 229 |
| High-Performance Liquid Chromatography | p. 229 |
| Why HPLC? | p. 230 |
| Isocratic Elution Versus Gradient Elution | p. 231 |
| Modes of HPLC | p. 232 |
| Main Detectors of HPLC | p. 234 |
| Limitations of HPLC | p. 234 |
| Applications of HPLC | p. 234 |
| Gas Chromatography | p. 234 |
| Modes of GC | p. 235 |
| Distribution Ratio and Temperature Effect in GC | p. 235 |
| Retention in GC | p. 236 |
| Carrier Gas | p. 236 |
| Columns and Stationary Phases | p. 236 |
| Detectors | p. 237 |
| Factors Affecting GC Separations | p. 238 |
| Features of GC | p. 239 |
| Use of GC | p. 239 |
| Quantitative Analysis Methods | p. 240 |
| Area/Height Percent | p. 240 |
| External Standard Method | p. 242 |
| Internal Standard Method | p. 244 |
| References | p. 245 |
| Infrared Spectroscopy and UV/Vis Spectroscopy | p. 247 |
| Infrared Radiation Spectroscopy | p. 247 |
| Molecular Vibration | p. 247 |
| Resonance | p. 248 |
| IR Spectroscopy | p. 250 |
| Fourier Transform Infrared Spectrometer | p. 252 |
| Interferometer | p. 252 |
| Fourier Transformation | p. 253 |
| Advantages of FTIR | p. 254 |
| Sample Preparation | p. 255 |
| Case Studies-Interactions Between Water and the Polyurethane Thermoresponsive Shape Memory Polymer | p. 256 |
| Ultraviolet/Visible Spectroscopy | p. 257 |
| UV Absorption | p. 257 |
| Beer-Lambert Law | p. 260 |
| UV/Visible Spectra | p. 260 |
| UV/Visible Spectroscopy | p. 263 |
| Case Studies | p. 264 |
| References | p. 265 |
| Macro and Micro Thermal Analyses | |
| Macro and Micro Differential Scanning Calorimetry | p. 267 |
| Differential Scanning Calorimetry | p. 267 |
| Sample Preparation and Effect of Sample Size | p. 269 |
| Effects of Heating Rate | p. 270 |
| Effect of Thermal History | p. 271 |
| Effect of Atmosphere | p. 272 |
| Temperature Calibration for DSC | p. 272 |
| Observation of Thermal Transitions (Using Semicrystalline Polymers as Examples): T[subscript m], T[subscript c], and T[subscript g] | p. 273 |
| Melting | p. 273 |
| Crystallization | p. 275 |
| Glass Transition | p. 276 |
| Micro Differential Scanning Calorimeters | p. 277 |
| Isothermal Titration Calorimetry | p. 282 |
| Thermogravimetric Analysis | p. 286 |
| Principle of TGA | p. 286 |
| Sample Preparation | p. 287 |
| Factors Affecting TGA Curves | p. 287 |
| Effect of Sample Holder | p. 288 |
| Effect of Sample Mass | p. 288 |
| Effect of Heating Rate | p. 289 |
| Effect of Furnace Atmosphere | p. 289 |
| Typical Applications of TGA | p. 290 |
| Thermal Stability | p. 290 |
| Compositional Analysis | p. 290 |
| Oxidative Stability | p. 292 |
| References | p. 292 |
| Laser Confocal Fluorescence Microscopy | p. 295 |
| Fluorescence and Fluorescent Dyes | p. 295 |
| Fluorescence Microscopy | p. 298 |
| Laser Confocal Fluoresence Microscopy | p. 300 |
| What Is Confocal? | p. 300 |
| How LCFM Works | p. 302 |
| Optical Sectioning and 3D Imaging | p. 302 |
| Two-Channel LCFM | p. 304 |
| Commonly Used Fluorophores (Fluorescent Dyes) | p. 305 |
| Photobleaching | p. 306 |
| Resolution of LCFM and Selection of Objective Lenses | p. 308 |
| Objective Lenses | p. 309 |
| Dry Lenses and Immersion Oil Lenses | p. 310 |
| Sample Preparation for LCFM | p. 311 |
| Limitations of LCFM | p. 312 |
| Applications of LCFM | p. 313 |
| Imaging of Cells and Cell Structures | p. 314 |
| Morphological Studies of Polymer Blends | p. 315 |
| References | p. 317 |
| Index | p. 319 |
| Table of Contents provided by Ingram. All Rights Reserved. |
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