Rechargeable Lithium-Ion Battery Evaluation ─ APPLICATION NOTEBOOK ─

Significance of the Topic

Rechargeable lithium‐ion batteries power a vast range of devices from consumer electronics to electric vehicles. Continuous improvement of their energy density, safety and cycle life depends on detailed understanding of each component—electrode materials, separator, electrolyte and additives—and of the interfaces between them. Advanced analytical methods are essential to guide materials development, quality control and safety assessment in both research and industrial settings.

Objectives and Study Overview

This collection of application notes illustrates a multidisciplinary analytical toolbox applied to lithium‐ion battery components. The key goals are to evaluate thermal stability, moisture content, carbon impurities, additive behavior, gas impurities, and surface chemistry across solid and liquid battery materials. Methods span thermal analysis, carbon analysis, scanning probe microscopy, gas chromatography, mass spectrometry and X‐ray photoelectron spectroscopy.

Methodology and Instrumentation

Multiple techniques and instruments were employed to characterize battery components:

• Thermal Analysis: Differential Scanning Calorimeter DSC‐60 Plus, Macro‐Type Thermogravimetric Analyzer
• Total Organic Carbon (TOC) Analysis: TOC‐LCPH analyzer with SSM‐5000A solid sample combustion unit
• Scanning Probe Microscopy: SPM‐8100FM with electrochemical solution cell for in‐situ interface imaging
• Gas Chromatography: Nexis GC‐2030 with dual BID detectors; Rt‐Msieve 5A and Rt‐Q‐BOND capillary columns; MGS‐2030 gas sampler
• Trace Impurity GC: Tracera GC‐2010 Plus with BID‐2010 Plus detector, Rt‐Msieve 5A and Micropacked ST columns
• MALDI‐TOF Mass Spectrometry: MALDI‐8020 benchtop TOF for molecular weight confirmation of organic semiconductors and electrolytes
• X‐ray Photoelectron Spectroscopy (XPS): Kratos AXIS with high‐energy Ar cluster ion source for depth profiling and chemical‐state mapping

Main Results and Discussion

• Thermal Analysis: DSC revealed exothermic degradation peaks of charged cathode materials above 200 °C. TGA measured moisture content in LiFePO₄ and graphite. DSC and TMA of separators showed melting transitions at 100–150 °C and dimensional changes under heat, informing shutdown behavior.
• Carbon Measurement: TOC solid‐sample analysis quantified trace carbon in LiCoO₂ powders with sub‐percent accuracy across calibration levels (0.2–5 % C).
• Additive Layer Visualization: Frequency‐modulation AFM imaged a 50–100 nm lignin‐lead layer on lead‐acid battery negative electrodes, elucidating additive adsorption that mitigates sulfation.
• GC Cooling‐Rate Effects: Nexis GC‐2030 studies showed that slower oven cooling minimizes liquid‐phase damage in methyl phenyl polysiloxane columns, reducing baseline noise and improving S/N ratios in repeated analyses.
• Simultaneous Inorganic Gas Analysis: Dual‐column GC‐2030 with BID achieved high‐sensitivity separation of H₂, O₂, N₂, CH₄, CO, CO₂ and light hydrocarbons in a single run with repeatable quantification at ppm levels.
• Trace Hydrogen Impurity Analysis: Tracera GC‐2010 Plus with BID and Rt‐Msieve 5A column detected CO down to 0.03 ppm, complying with ISO 14687-2 limits, and Micropacked ST column enabled CO₂ and hydrocarbon analysis.
• MALDI‐TOF MS of Organic Functional Materials: The MALDI‐8020 instrument obtained clear molecular‐ion peaks and isotopic distributions for OLED dyes, organic semiconductors and photovoltaic materials up to 1,300 Da, demonstrating rapid confirmation of synthetic products.
• XPS Depth Profiling of LiPON Films: Cluster‐ion sputter profiling of ALD‐deposited LiPON revealed lithium enrichment near the surface and reliable Li quantification, overcoming light‐ion migration artifacts in monatomic profiling.
• Surface Segregation on Cu Electrodes: Large‐area and stitched XPS imaging mapped lithium perchlorate crystallites on Cu battery electrodes. High‐energy cluster profiling confirmed Li remains confined to the near‐surface region without bulk penetration.

Benefits and Practical Applications of the Methods

• Thermal analysis informs safe operating limits and material selection for electrodes and separators.
• TOC solid‐sample systems provide fast trace carbon quantification for raw‐material quality control.
• High‐resolution AFM under electrochemical conditions reveals additive‐electrode interfaces critical to cycle life.
• Flexible GC cooling programs extend column lifetime and ensure low‐noise analysis in routine laboratory workflows.
• Universal BID detectors allow simultaneous detection of diverse gas species, streamlining gas‐analysis setups.
• Benchtop MALDI‐TOF MS accelerates verification of high‐molecular‐weight organic battery components.
• XPS with cluster depth profiling delivers quantitative, depth‐resolved chemical‐state data for solid electrolytes and electrode films.

Future Trends and Application Possibilities

• Integration of operando analytical techniques (in‐situ thermal, spectroscopic and microscopy) to monitor battery aging in real time.
• Development of new solid‐state electrolyte materials characterized by combined AFM, XPS and ToF‐SIMS profiling.
• Advances in ambient‐pressure XPS and in‐line GC detectors for direct cell analysis under working conditions.
• Machine‐learning‐driven analysis pipelines to correlate multi‐modal data with performance metrics for accelerated materials screening.
• Miniaturized, portable versions of MALDI‐TOF MS and GC‐BID systems for field testing of battery materials and fuels.

Conclusion

A comprehensive suite of analytical methods spanning thermal analysis, carbon quantification, scanning probe microscopy, gas chromatography, mass spectrometry and XPS has been demonstrated for evaluation of battery components and interfaces. These tools deliver critical insights into material stability, impurity levels, additive behavior and surface chemistry, underpinning safer, higher‐performance and longer‐lifetime rechargeable batteries. Collaborative adoption of multi‐technique analysis will drive next‐generation battery innovation.

Použitá instrumentace

• DSC‐60 Plus Differential Scanning Calorimeter
• Macro‐type Thermogravimetric Analyzer
• Shimadzu TOC‐LCPH with SSM‐5000A
• SPM‐8100FM with Electrochemical Solution Cell
• Nexis GC‐2030 with Dual BID Detectors, Rt‐Msieve 5A and Rt‐Q‐BOND Columns
• Tracera GC‐2010 Plus with BID‐2010 Plus and Rt‐Msieve 5A/Micropacked ST Columns
• MALDI‐8020 Benchtop MALDI‐TOF Mass Spectrometer
• Kratos AXIS XPS with 20 kV Ar Cluster Ion Source

Reference

• A. Kozen, A. Pearse, G. Rubloff, C.-F. Lin, M. Noked, Chem. Mater., 2015, 27, 5324.
• Y. Yamamoto, K. Yamamoto, J. Non-Cryst. Solids, 2015, 356, 14.