Rechargeable Lithium-Ion Battery Evaluation ─ APPLICATION NOTEBOOK ─

Significance of the Topic

• Rechargeable lithium-ion batteries underpin today’s consumer electronics, electric vehicles and future energy storage, demanding ever-higher safety, power density and cycle life.
• Detailed component analysis—from molecular composition to interfacial phenomena—is critical to optimize performance and prevent hazards such as thermal runaway or electrode degradation.

Goals and Overview of the Article Collection

• Illustrate diverse analytical approaches applied to Li-ion battery R&D and quality control.
• Cover thermal behavior of electrodes and separators, carbon quantification in active materials, visualization of electrolyte additives, gas-phase impurity analysis, organic material verification, and interfacial chemistry in solid electrolytes.

Methodology and Instrumentation

• Thermal Analysis: Differential Scanning Calorimetry (DSC-60 Plus) and Thermogravimetric Analysis (macro TGA) to assess electrode and separator stability.
• Total Organic Carbon (TOC) Analysis: Shimadzu TOC-LCPH with SSM-5000A combustion unit for precise carbon measurement in LiCoO₂ powders.
• High-Resolution Surface Imaging: Shimadzu SPM-8100FM with electrochemical cell to map lignin-lead layers at negative electrodes.
• Gas Chromatography: Nexis GC-2030 with variable cooling rates and dual BID detectors for analysis of inorganic gases and light hydrocarbons.
• Trace Impurity GC: Tracera (GC-2010 Plus & BID-2010 Plus) with micropacked and molecular sieve columns for sub-ppm CO, CO₂, CH₄ in H₂.
• MALDI-TOF MS: Benchtop MALDI-8020 for rapid molecular weight confirmation of OLED, OPV and polymer precursors.
• XPS & Depth Profiling: Kratos AXIS with Arₙ⁺ clusters for LiPON thin films and Li salt distribution on Cu electrodes.

Main Results and Discussion

• DSC/TGA revealed exothermic decomposition of charged cathode materials above 200 °C and separator melting transitions (100–150 °C), informing safer component selection.
• TOC solid sample system achieved accurate quantification of added carbon in LiCoO₂ down to 0.2 % with linear calibration.
• SPM cross-sectional imaging visualized a 50–100 nm lignin-Pb interfacial layer, demonstrating additive adsorption that may mitigate sulfation.
• GC column cooling experiments showed slower oven cooldown preserves liquid phase coating, reducing baseline noise by >75 % and improving S/N ratios.
• Dual-BID GC achieved simultaneous analysis of H₂, O₂, N₂, CO, CO₂ and hydrocarbons in under 9 min with detection limits in the low ppm range.
• Trace‐impurity analysis in H₂ met ISO 14687‐2 requirements, detecting CO at 0.03 ppm (S/N = 3) and simultaneous quantification of CO₂, CH₄, C₂H₄, C₂H₂, C₂H₆.
• MALDI-TOF MS measurements confirmed synthesis of functional organic materials up to 1 400 Da with clear isotopic patterns, facilitating rapid product verification.
• XPS imaging and Arₙ⁺ depth profiling showed Li segregation in LiPON surfaces (~30 at. %) and identified LiClO₄ crystallites on Cu electrodes, clarifying interfacial chemistry.

Benefits and Practical Applications

• Improved battery safety by pinpointing thermal events and separator shrinkage behavior.
• Reliable material purity control in electrode powders through fast TOC analysis.
• Direct nanoscale observation of electrolyte additives guiding formulation improvements.
• Enhanced GC column lifetime and data quality via optimized cooling protocols.
• Rapid multi-gas profiling for production-line monitoring of battery manufacturing gases and fuel-cell hydrogen.
• Expedited development cycles for organic battery materials using benchtop MALDI-TOF MS.
• Deep insight into solid electrolyte interfaces via XPS, supporting design of next-generation all-solid-state batteries.

Future Trends and Utilization Possibilities

• Integration of high-throughput thermal and spectroscopic screening for novel electrode and separator chemistries.
• In situ TOC and AFM probes for real-time monitoring during battery cycling.
• Advanced AFM and XPS imaging to reveal dynamic interphases at the nanoscale.
• Machine-learning-driven GC parameter optimization to further compress analysis times.
• Expanded use of MALDI-TOF MS for macromolecular and composite battery material analysis.
• Wider application of argon cluster depth profiling across emerging metal-ion battery alloys and electrolytes.

Conclusion

Comprehensive application of thermal, carbon, imaging, chromatographic and spectroscopic techniques provides a multidimensional understanding of lithium-ion battery components and interfaces. These analytical insights support safer, higher-performance batteries and are vital for the advancement of solid-state and next-generation energy storage technologies.

References

• Shimadzu Application Note T151: Thermal Analysis of Li-Ion Battery Components (Jun 2016)
• Shimadzu Application Note O72: Carbon Measurement of LiCoO₂ Powder (Dec 2018)
• Shimadzu Application Note S41: Visualization of Additive Layer by SPM-8100FM (Sep 2019)
• Shimadzu Application Note G302: Column Cooling Effects with Nexis GC-2030 (May 2018)
• Shimadzu Application Note G288: Dual BID System GC-2030 Analysis (Jun 2017)
• Shimadzu Application Note G283: Trace Impurity Analysis in H₂ (May 2015)
• Shimadzu MALDI-8020 Whitepaper: Confirmation of Organic Functional Materials (Jun 2019)
• Kratos XPS Note MO435: LiPON Surface and Interface Analysis
• Kratos XPS Note MO448A: Li Salt Distribution on Cu Electrodes