碳材料科学与工程:表征 内容简介

碳材料由于其结构多样性，导致其性能多样化，因而应用领域广阔，碳材料研究已受到全球材料科学界、物理学界、化学界的广泛关注。本书系统介绍了碳材料表征技术及应用。包括X射线粉末衍射、小角X射线散射、透射电镜、扫描电子显微镜、图像分析、拉曼光谱、X射线光电子能谱、磁电阻、电化学性能、气体吸附/解吸等温线、热分析、表面官能团滴定测定、程序升温脱附技术。本书读者对象为材料领域的科技人员、研究生和高校教师。本书以英文著述，并与Elsevier出版集团合作，已在海外出版。

碳材料科学与工程:表征 本书特色

碳材料由于其结构多样性，导致其性能多样化，因而应用领域广阔，碳材料研究已受到全球材料科学界、物理学界、化学界的广泛关注。本书系统介绍了碳材料表征技术及应用，包括 X射线粉末衍射、小角X射线散射、透射电镜、扫描电子显微镜、图像分析、拉曼光谱、X射线光电子能谱、磁电阻、电化学性能、气体吸附/解吸等温线、热分析、表面官能团滴定测定、程序升温脱附技术。本书读者对象为材料领域的科技人员、研究生和高校教师。本书以英文著述，并与 Elsevier出版集团合作已在海外出版。

碳材料科学与工程:表征 目录

ListofContributors.................................................................................Preface...............................................................................................Acknowledgments................................................................................CHAPTER 1 Introduction............................................................ 1Michio Inagaki, Feiyu Kang1.1 Carbon Materials............................................................... 11.2 Characterization of Carbon Materials.................................... 31.3 Structure of the Present Book.............................................. 5References.............................................................................. 6CHAPTER 2 X-ray Powder Diffraction ......................................... 7Norio Iwashita2.1 Introduction...................................................................... 72.2 X-ray Diffraction Pattern of Carbon Materials........................ 82.3 Parameters Determined by X-ray Diffraction.........................102.4 Instrumentation ................................................................112.5 Specifications for Measurement ..........................................142.5.1 Preparation of Sample for X-ray Measurements............ 142.5.2 Measurement and Intensity Correction of DiffractionProfiles.................................................................. 142.5.3 Correction of Diffraction Angle With InternalStandard ................................................................ 162.5.4 Determination of Full Width at Half MaximumIntensity ................................................................ 172.5.5 Accuracy of the Values Determined............................ 182.6 Degree of Graphitization ...................................................182.7 Key Issues for Measurement...............................................212.7.1 Diffraction Pattern................................................... 212.7.2 Use of Internal Standard........................................... 212.7.3 Use of Thin Sample Holder....................................... 222.7.4 Indexing the Diffraction Line .................................... 232.7.5 Separation into Component Profiles............................ 232.8 Concluding Remarks.........................................................24References.............................................................................24 CHAPTER 3 Small-Angle X-ray Scattering..................................27Katsuya Fukuyama, Yoshikiyo Hatakeyama3.1 Introduction.....................................................................273.2 Fundamentals ..................................................................283.3 Key Issues for the Measurements ........................................333.4 Applications for Carbon Materials.......................................353.4.1 Porous Carbon Fibers............................................... 353.4.2 Glass-Like Carbons ................................................. 363.4.3 Mesocellular Foam Carbons (Silica-TemplatedCarbons)................................................................ 383.4.4 Open Pores Formed by Air Oxidation......................... 403.5 Concluding Remarks.........................................................42References.............................................................................42CHAPTER 4 Transmission Electron Microscopy..........................45Sylvie Bonnamy, Agne`s Oberlin4.1 Introduction.....................................................................454.2 Modes of Transmission Electron Microscopy ........................464.2.1 Diffracting Mode..................................................... 474.2.2 Imaging Modes....................................................... 474.3 Key Issues for Observation ................................................484.3.1 Object Thickness (Weak Phase Object) ....................... 484.3.2 Contrast Transfer Function of the TransmissionElectron Microscope................................................ 494.3.3 Diffusion Contrasts.................................................. 544.3.4 Fresnel Fringes, ie, Edge Fringes ............................... 544.5 Applications for Carbon Materials.......................................564.5.1 Transmission Electron Microscopy Modes to StudyCrystallinity of Carbon Materials ............................... 564.5.2 Transmission Electron Microscopy Modes inthe Study of Carbonization and Graphitization ............. 624.6 Conclusions.....................................................................69References.............................................................................69Further Reading......................................................................70CHAPTER 5 Scanning Electron Microscopy ...............................71Akira Yoshida, Yutaka Kaburagi, Yoshihiro Hishiyama5.1 Introduction.....................................................................715.2 Instrumentation and Resolving Power ..................................725.2.1 Instrumentation....................................................... 735.2.2 Magnification and Resolving Power of theScanning Electron Microscope................................... 755.2.3 Edge Effects Appearing in SE Mode Images................ 76 5.3 Specimen Preparation........................................................775.4 Observation With the Out-Lens Objective Lens System ..........795.5 Observation With the Snorkel Objective Lens System.............815.6 Observation With the In-Lens System..................................825.7 Electron Channeling Effect ................................................835.7.1 Electron Channeling Effect for Kish Graphite .............. 835.7.2 Electron Channeling Pattern for Kish Graphiteand HOPG Specimens.............................................. 865.7.3 Mapping and Crystal Grain Size Evaluation................. 885.8 Concluding Remarks.........................................................91References.............................................................................92CHAPTER 6 Image Analysis ......................................................95Kyoichi Oshida6.1 Introduction.....................................................................956.2 Image Analysis Methods ...................................................966.2.1 Process of Image Analysis ........................................ 966.2.2 Analysis of Space Frequency..................................... 976.2.3 Three-Dimensional Transmission ElectronMicroscopy ...........................................................1006.2.4 Software for the Analysis ........................................1006.3 Structure Analysis Through Transmission ElectronMicroscopy ................................................................... 1016.3.1 Cup-Stacked Type Carbon Nanotubes ........................1016.3.2 Carbon Nanotubes Loaded With Metal Particles ..........1046.3.3 Thin Graphite ........................................................1086.3.4 Disordered Carbon .................................................1086.4 Texture Analysis Through Scanning ElectronMicrographs .................................................................. 1136.5 Texture Analysis Through Optical Micrographs................... 1166.6 Concluding Remarks....................................................... 120References........................................................................... 121CHAPTER 7 Raman Spectroscopy............................................ 125Yutaka Kaburagi, Akira Yoshida, Yoshihiro Hishiyama7.1 Introduction................................................................... 1267.2 Fundamentals ................................................................ 1267.3 Key Issues for the Measurements ...................................... 1297.3.1 Laser Probe Sampling Depth....................................1297.3.2 Polarization of Laser Light ......................................1297.3.3 Sampling Area.......................................................1317.3.4 Temperature ..........................................................1327.3.5 Elimination of Background Intensity .........................132 7.3.6 Excitation Energy Dependence of D Band..................1337.3.7 Calibration of Raman Frequency...............................1347.3.8 Equipment ............................................................1367.4 As a Measure for Structure Characterization ....................... 1387.4.1 G Band.................................................................1387.4.2 D and D0 Bands .....................................................1417.5 Concluding Remarks....................................................... 149References........................................................................... 150CHAPTER 8 X-ray Photoelectron Spectroscopy ........................ 153Hidetaka Konno8.1 Introduction................................................................... 1538.2 Practical Side of Measurements ........................................ 1548.3 State Analysis................................................................ 1568.3.1 Determination of Binding Energy..............................1568.3.2 Background Subtraction ..........................................1588.3.3 Peak Separation .....................................................1598.3.4 State Analysis Using Chemical Shift .........................1648.4 Semiquantitative Analysis................................................ 1668.5 Concluding Remarks....................................................... 168References........................................................................... 169CHAPTER 9 Magnetoresistance............................................... 173Yoshihiro Hishiyama, Yutaka Kaburagi, Michio Inagaki9.1 Introduction................................................................... 1749.2 General Scheme of Dr/r0 Change With Graphitization ......... 1749.3 Measurement of Magnetoresistance ................................... 1789.3.1 Specimen Shape.....................................................1789.3.2 Magnetic Field Orientation Schemes .........................1799.3.3 Instruments ...........................................................1829.4 Magnetoresistance Parameters for Coke ............................. 1859.4.1 Coke B and Gilsonite Coke......................................1859.4.2 Coke Prepared From Hydrogenated EthyleneTar Pitch...............................................................1869.5 Magnetoresistance Parameters for Carbon Fibersand Extruded Coke......................................................... 1899.5.1 Benzene-Derived Vapor-Grown Carbon Fiberand Extruded Coke.................................................1899.5.2 Other Carbon Fibers ...............................................1919.6 Magnetoresistance Parameters for Highly CrystallizedGraphite Materials.......................................................... 192 9.7 Concluding Remarks....................................................... 194Supplement: Background of the Characterization of CarbonMaterials With Dr/r0 ............................................................ 195S-1 Origin of the Sign of Dr/r0............................................... 195S-2 Microtexture .................................................................. 197S-3 Relationship Between Microtexture and Magnetoresistance.... 199References........................................................................... 203CHAPTER 10 Electrochemical Performance............................. 205Soshi Shiraishi10.1 Introduction................................................................. 20510.2 Fundamentals............................................................... 20610.2.1 Capacitance .......................................................20610.2.2 Construction of Measurement Cell.........................20810.2.3 Electrochemically Analytical Mode .......................20910.2.4 Differential Capacitance and IntegralCapacitance .......................................................21110.2.5 Definition of Specific Capacitance.........................21210.3 Measurement Procedure................................................. 21410.3.1 Measurement Cell...............................................21410.3.2 Preparation of Carbon Electrode............................21610.3.3 Aqueous Acid Electrolyte System(by Three-Electrode Cell).....................................21810.3.4 Organic Electrolyte System(by Three-Electrode Cell).....................................21910.3.5 Organic Electrolyte System(by Two-Electrode Cell) ......................................22110.4 Concluding Remarks..................................................... 224References........................................................................... 224CHAPTER 11 Gas Adsorption/Desorption Isothermfor Pore Structure Characterization..................... 227Yoko Nishi, Michio Inagaki11.1 Introduction................................................................. 22811.2 Fundamentals............................................................... 22911.3 Key Issues for the Measurements and Analyses ................. 23211.3.1 Sample Amount for the Measurement ....................23211.3.2 Pretreatment of Sample........................................23211.3.3 BrunauereEmmetteTeller Method ........................23311.3.4 as Plot ..............................................................23411.3.5 BarretteJoynereHalenda Method..........................235 11.3.6 DubinineRadushkevich Method............................23711.3.7 Density Functional Theory Method........................23811.4 Application to Carbon Materials ..................................... 23911.4.1 Microporous Carbons ..........................................23911.4.2 Mesoporous Carbons...........................................24111.4.3 Measurements Using Various Gases as Adsorbate ....24311.4.4 Gravimetric Measurement of Adsorption/Desorption of CO2 ..............................................24411.5 Concluding Remarks..................................................... 245References........................................................................... 246CHAPTER 12 Thermal Analysis ............................................... 249Ming-ming Chen12.1 Introduction................................................................. 24912.2 Fundamentals in Thermal Analyses ................................. 25012.3 Key Issues for the Measurements .................................... 25212.4 Applications of TG and DTG for Carbon Materials ............ 25612.4.1 Biomasses .........................................................25612.4.2 Pitches..............................................................25812.4.3 Organic Polymers ...............................................25812.4.4 Measurements in Oxygen.....................................26312.5 Applications of DTA and DSC for Carbon Materials .......... 26512.5.1 Pitches..............................................................26512.5.2 Organic Polymers ...............................................26712.5.3 Intercalation Reactions ........................................26912.6 Concluding Remarks..................................................... 269References........................................................................... 270CHAPTER 13 Titration Method for the Identificationof Surface Functional Groups.............................. 273Yern Seung Kim, Chong Rae Park13.1 Introduction................................................................. 27313.2 Basic Concept of Titration Method.................................. 27613.3 Instrumentation ............................................................ 27913.4 Specification for the Methodology................................... 27913.4.1 Reaction Step.....................................................28013.4.2 Filtration Step ....................................................28113.4.3 Titration Step.....................................................28113.5 Analysis of the Titration Results ..................................... 28113.6 Key Points for the Titration Measurements ....................... 284 13.6.1 Preparation of the Reaction Mixture for the ReactionStep..................................................................28413.6.2 Agitation Method and Period................................28413.6.3 Titration Condition and End Point Determination.....28513.7 Concluding Remarks..................................................... 285References........................................................................... 285CHAPTER 14 Temperature Programmed Desorption.................. 287Takafumi Ishii, Takashi Kyotani14.1 Introduction................................................................. 28714.2 TPD Experimental Conditions and Apparatus.................... 28814.3 Assignment of TPD Peaks to Surface FunctionalGroups........................................................................ 29114.4 Secondary Reactions During a TPD Run .......................... 29614.5 Effect of Air Exposure on TPD Patterns ........................... 29914.6 Effect of Inorganic Matter in Carbons.............................. 30014.7 Concluding Remarks..................................................... 302References........................................................................... 302Index...................................................................................................307

碳材料科学与工程:表征 作者简介

Michio Inagaki教授，日本北海道大学荣休教授。担任过日本碳素学会主席，JSPS117委员会主席，Carbon杂志副主编。获得过美国和中国碳素学会、日本陶瓷学会学术贡献奖。出版8本书，发表700多篇学术论文。Feiyu Kang（康飞宇），教授，清华大学深圳研究生院院长。现任SCI刊物《Carbon》顾问编委，SCI刊物《新型炭材料》副主编，层间化合物系列国际会议（ISIC）国际顾问委员会委员。曾获国家发明奖等多项奖励。出版中英文专著5部，在国内外发表论文200多篇。