Advancing Research of Lithium-Ion Batteries Using the Agilent Cary 630 FTIR Spectrometer

Significance of the Topic

The rapid growth of electric vehicles and renewable energy storage has intensified the need for advanced lithium ion batteries with higher capacity, faster charging, improved safety, and lower cost. Infrared spectroscopy provides crucial molecular level insights into battery materials that guide the development of novel electrodes, electrolytes, and separators. Compact and flexible FTIR tools enable routine characterization in research and industrial labs, accelerating innovation in battery chemistry and engineering.

Study Objectives and Overview

This white paper highlights how the Agilent Cary 630 FTIR spectrometer supports lithium ion battery research by offering:

• Versatile sampling modules for diverse material forms
• Intuitive software for rapid qualitative and quantitative analysis
• Compact design suitable for controlled environments

Detailed examples illustrate applications in material synthesis, electrolyte monitoring, polymer coatings, and advanced analytical methods.

Methodology

FTIR spectroscopy identifies functional groups and monitors chemical changes by measuring absorbance across mid infrared wavelengths. Key methodological features include:

• Interchangeable sampling modules such as attenuated total reflectance for solids, liquids, and films
• Automated spectral comparison against libraries for compound identification
• Quantitative analysis of electrolyte salts and polymer components through peak integration
• Compatibility with glovebox operation to control moisture and oxygen interference

Used Instrumentation

The primary instrumentation comprises:

• Agilent Cary 630 FTIR spectrometer with modular sampling interfaces
• Attenuated Total Reflectance module for sheet and film materials
• Germanium ATR accessory for electrolyte and polymer analysis
• Agilent MicroLab software for guided workflows and automated data processing
• MicroLab Expert software for advanced spectral visualization and custom processing

Key Results and Discussion

Representative research applications include:

1. Fabrication of vertically aligned graphene oxide films by pulse freezing showing enhanced ion and electron transport, confirmed through disappearance of hydroxyl peaks in FTIR spectra
2. Investigation of lithiation induced vibrational shifts in magneto-ionic cathode materials, tracking C≡N bond changes during charge–discharge cycles
3. Synthesis of ZIF-67 derived Co–Sn composites with N-doped nanoporous carbon anodes, where FTIR revealed bonding environments responsible for structural stability
4. Evaluation of polymeric CO2-absorbing coatings on aluminum foils, monitoring epoxy group conversion and degradation under thermal stress
5. Development of dispersion-mediated grafting of polymer shells onto Li4Ti5O12 particles, using FTIR to identify characteristic CH2 stretching signals
6. Machine learning assisted quantification of LiPF6, EC, EMC, DMC, and DEC in electrolyte mixtures from FTIR spectral features with precision comparable to ICP-OES methods
7. Assessment of solid polymer electrolytes reinforced with graphene oxide nanosheets, determining lithium salt dissociation fractions via peak area ratios

Benefits and Practical Applications

The Cary 630 FTIR system delivers:

• Rapid sample analysis with minimal user training through picture-driven software
• High reproducibility and uptime in multi-user laboratory settings
• Portable footprint enabling integration into gloveboxes or compact workstations
• Qualitative and quantitative insights that accelerate material screening and formulation

Future Trends and Potential Applications

Emerging directions for FTIR in battery research include:

• In situ and operando studies to monitor electrode reactions during cycling
• Integration with machine learning for automated feature extraction and predictive modeling
• Development of infrared imaging and mapping for spatially resolved chemical analysis
• Expansion of spectral libraries for novel electrolyte salts, solid-state materials, and electrode coatings

Conclusion

The Agilent Cary 630 FTIR spectrometer, combined with intuitive MicroLab software, offers a flexible and robust analytical platform for advancing lithium ion battery research. Its modular design, ease of use, and compatibility with controlled environments make it an indispensable tool for characterizing a broad range of materials and accelerating the development of safer, higher performance battery systems.

References

• Masias A, Marcicki J, Paxton WA. Opportunities and Challenges of Lithium Ion Batteries in Automotive Applications, ACS Energy Letters 2021, 6(2), 621–630
• Liu Y et al. Highly Aligned Graphene Oxide for Lithium Storage in Lithium-Ion Battery Through A Novel Microfluidic Process The Pulse Freezing, Advanced Materials Interfaces 2023, 10, 2201612
• Hu Y et al. Lithiating Magneto-Ionics in a Rechargeable Battery, Proceedings of the National Academy of Sciences USA 2022, 119(25), e2122866119
• Ashraf S et al. ZIF-67 Derived Co–Sn Composites with N-Doped Nanoporous Carbon as Anode Material for Li-Ion Batteries, Materials Chemistry and Physics 2021, 270, 124824
• Daigle JC et al. Novel Polymer Coating for Chemically Absorbing CO2 for Safe Li-Ion Battery, Scientific Reports 2020, 10(1), 10305
• Daigle JC et al. A Versatile Method for Grafting Polymers onto Li4Ti5O12 Particles Applicable to Lithium-Ion Batteries, Journal of Power Sources 2019, 421, 116–123
• Ellis LD et al. A New Method for Determining the Concentration of Electrolyte Components in Lithium-Ion Cells Using FTIR and Machine Learning, Journal of The Electrochemical Society 2018, 165, A256
• Yuan M et al. High Performance Solid Polymer Electrolyte with Graphene Oxide Nanosheets, RSC Advances 2014, 4, 59637
• Buteau S et al. User-Friendly Freeware for Determining the Concentration of Electrolyte Components in Lithium-Ion Cells Using FTIR, Beer’s Law, and Machine Learning, Journal of The Electrochemical Society 2019, 166, A3102