Connect battery materials properties to performance through advanced characterization techniques

Understanding electrochemical processes during battery cycling demands specialized analytical tools that go beyond static analysis. Battery Materials Characterization: Advanced Techniques and Applications, written by two searchers with combined publications exceeding 280 papers in energy materials and synchrotron radiation, covers a wide range of battery types and the in situ/operando characterization methods required to link materials properties with electrochemical performance.

The book provides dedicated treatment of XAS, TXM, ND/PDF, RIXS, EPR, TOF-SIMS, DEMS, and Cs-TEM variants applied to battery systems. Each technique is examined through case studies addressing material degradation, interfacial reactions, dynamic structural evolution, and electronic state changes under operational conditions. Coverage extends to multimodal analysis approaches that combine multiple methods for multiscale, multidimensional characterization of battery materials.

The book also covers:

• In situ and operando characterization methods enabling real-time tracking of material dynamics during battery cycling and operation
• Integration of multi-mode characterizations combining spectroscopy, microscopy, and diffraction for multiscale analysis of electrode materials
• Actionable guidance and real-world case studies demonstrating practical application of each analytical technique to battery research
• Machine learning and large-scale data analysis approaches applied to characterization data interpretation and materials discovery
• Emerging ultrafast and high-resolution methods representing future directions in battery materials analysis and electrochemical research

Written for materials scientists, electrochemists, spectroscopists, structural chemists, solid state chemists, and physical chemists, this reference connects advanced characterization techniques with practical battery research applications. It serves researchers and practitioners who require authoritative, technique-specific guidance across multiple battery chemistries and analytical methods.

About the Author ix
Preface xi

1 Fundamentals of Battery Materials and the Evolution of Advanced Characterization Techniques 1
1.1 Global Energy Transition 1
1.2 Basic Principles and Core Composition of Lithium-Ion Batteries 3
1.3 Development Trend and Core Characteristics of Secondary Batteries 7
1.4 Research Trend and Core Bottlenecks of Key Battery Components 11
1.5 Evolution of Characterization Technology 14

2 Neutron Scattering and Pair Distribution Function Analysis for Battery Materials 19
2.1 Introduction 19
2.2 Neutron Facilities: Global Distribution and Specialized Capabilities 21
2.3 Fundamental Comparison: Neutrons vs. Electrons vs. X-rays for Material Characterization 30
2.4 Neutron Scattering Techniques: Principles and Variants 32
2.5 Applications of Neutron Techniques in Energy Storage Materials 40
2.6 Challenges and Future Directions 49

3 X-ray Diffraction and Scattering Techniques: From Crystal Structure to Multiscale Structural Analysis 55
3.1 Fundamentals and Techniques of X-ray Diffraction 55
3.2 Synchrotron Radiation XRD 67
3.3 Small-angle/Wide-angle X-ray Scattering Techniques 72
3.4 Application Cases 77
3.5 Conclusions and Perspectives 89

4 Transmission Electron Microscopy for Atomic Scale and Dynamic Characterization of Battery Materials 95
4.1 Electron Beam Imaging and Basic Configuration of Transmission Electron Microscopy (TEM) 95
4.2 Electron Diffraction 100
4.3 Different Imaging Modes and Contrast Imaging 105
4.4 Diffraction Contrast Images 106
4.5 High-resolution TEM (HRTEM) Images and Phase Contrast 108
4.6 STEM Images 110
4.7 Introduction to New TEM Technologies 111
4.8 Application Cases 113
4.9 Conclusion and Prospective 139

5 Transmission X-ray Microscopy for Multiphysics Imaging of Batteries 143
5.1 Fundamental Principles and Theories 143
5.2 Equipment and Analysis 147
5.3 Introduction to Emerging TXM Technology 158
5.4 Application Cases 165vi Contents
5.5 Conclusion and Prospective 179

6 Synchrotron-based Soft X-ray Absorption Spectroscopy for Electronic and Interfacial Characterization of Battery Materials 185
6.1 Fundamentals and Theory 185
6.2 Equipment and Analysis 193
6.3 Application Cases 202

7 Resonant Inelastic X-ray Scattering for Probing Electronic Excitations in Battery Materials 213
7.1 Fundamentals and Techniques of Resonant Inelastic X-ray Scattering 213
7.2 Instrumentation and Analysis of RIXS 217
7.3 Application Cases 222
7.4 Summary and Perspectives 230

8 Synchrotron-based Hard X-ray Absorption Spectroscopy for Local Structure and Redox Chemistry in Battery Materials 235
8.1 Fundamentals of Hard X-ray Absorption Spectroscopy 235Contents vii
8.2 Equipment and Analysis 246
8.3 Application Cases 254

9 Electron Paramagnetic Resonance Spectroscopy for Defect and Redox Characterization in Battery Materials 265
9.1 Basic Principles 265
9.2 Equipment and Analysis 269
9.3 Introduction of New Technologies 273
9.4 Application Cases 275
9.5 Conclusion and Prospective 286

10 Raman Spectroscopic Characterization of Structural and Interfacial Evolution in Battery Materials 289
10.1 Fundamental Principles and Theory 289
10.2 Instrumentation and Analysis 293
10.3 Advanced Techniques and In-situ Applications 296
10.4 Application of Raman Spectroscopy in the Study of Battery Materials 300
10.5 Summary and Outlook 320

11 Gas Evolution and Surface Chemistry Analysis of Battery Materials by Differential Electrochemical Mass Spectrometry (DEMS) and Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) 323
11.1 Principles and Instrumentation of DEMS 323
11.2 Applications of DEMS