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  6. Technical Information Magazine 201910-03 In-situ Heating Method

Technical Information Magazine 201910-03 In-situ Heating Method

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last updated:Mar 24, 2025

東レリサーチセンター
東レリサーチセンター
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The technical information magazine The TRC News provides the latest information on analytical techniques that are useful for research and development, solving production troubles, and quality control.

**Abstract** Regarding the LIB positive electrode active material LiCoO2, gas analysis using TPD-MS and two in-situ heating methods (in-situ heating TEM) were employed to investigate the relationship between the gases emitted from LiCoO2 particles during heating and the changes in morphology, organization, and structure. The results demonstrated that gas generation is closely related to structural changes. Changes similar to charge-discharge behavior were also observed, and a series of measurements with temperature as a parameter provided important insights for analyzing actual materials. Additionally, it was shown that microscopic structural changes (such as the formation of domain structures), which cannot be detected without high resolution (approximately 40 nm field of view), can be visualized and quantitatively analyzed using ASTAR* (with *ASTAR being a registered trademark of NanoMEGAS) at a field of view of over 1 μm. **Table of Contents** 1. Introduction 2. Experimental Methods 3. Observation of Gas Generation Behavior Using TPD-MS 4. Observation of Structural Changes by in-situ Heating TEM 4-1. Observation of Morphological and Organizational Changes in STEM Images 4-2. Observation of Crystal Structure Changes in HRSTEM Images 4-3. Observation of Morphological, Organizational, and Structural Changes Above 650°C 5. Conclusion

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Technical Information Magazine 201910-03 In-situ Heating Method

TRC News 201910-03.jpg
TRC News 201910-03.jpg
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Technical Information Magazine The TRC News "Investigation of the Relationship Between Gas Generation and Structural Changes in Cathode Materials Using in-situ Heating Method" 【Table of Contents】 Introduction Experimental Methods Observation of Gas Generation Behavior Using TPD-MS Observation of Structural Changes Using in-situ Heating TEM Method Observation of Morphological and Structural Changes in STEM Images Observation of Crystal Structure Changes in HRSTEM Images Observation of Morphological, Structural, and Organizational Changes Above 650℃ Summary 【Figures and Tables】 Figure 1 to Figure 9 MS Curves for CO2, CO, and O2 in TPD-MS Measurement Results of LiCoO2 HAADF-STEM Observation Results of LiCoO2 Using in-situ Heating TEM Method High-Resolution HAADF-STEM Observation Results of LiCoO2 [100] Incidence Using in-situ Heating TEM Method BF-STEM Observation Results of LiCoO2 Using in-situ Heating TEM Method at Each Temperature Point from Room Temperature (23℃) to 650℃ and Unique Grain Map HAADF-STEM Observation Results of LiCoO2 Using in-situ Heating TEM Method at Each Temperature Point from 700℃ to 1000℃ TEM Observation Results of Cathode Active Material LiCoO2 Particles Extracted from Disassembled Swollen Battery Cell

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At Toray Research Center, Inc., we provide technical support through analytical techniques and physical property analysis to address various challenges in research and development as well as production fields via contract analysis. Based on our long-standing achievements and extensive experience in analysis and physical property evaluation, we continue to strive to meet the advanced and diverse needs of our customers.

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