Multi-Elemental Analysis of Lithium Aluminum Titanium Phosphate by Automated ICP-OES

Importance of the Topic

The transition to cleaner energy sources and enhanced energy storage technologies has elevated the importance of all-solid-state lithium-ion batteries (ASSBs). Multi-element analysis of solid electrolytes such as lithium aluminum titanium phosphate (LATP) is essential for optimizing ionic conductivity, chemical stability, and mechanical properties. Comprehensive elemental profiling supports material development, quality control, and ensures battery safety and performance.

Study Objectives and Overview

This work presents an automated ICP-OES method for quantifying four major elements (Li, Al, Ti, P) and sixteen trace elements in LATP electrolytes. The study aimed to streamline sample preparation, implement robust calibration, and validate method performance in terms of detection limits, accuracy, and stability using an Agilent 5800 ICP-OES system integrated with an autodilution unit.

Methodology

• Sample Preparation and Digestion:

• Approximately 0.1000 g of LATP powder was digested with a mixture of aqua regia and hydrofluoric acid in a microwave system under a precise temperature program.
• Digests were evaporated, reconstituted to 25 mL with ultrapure water, and prepared for analysis.

• Calibration and Autodilution:

• Stock solutions for major and trace elements were prepared and automatically diluted by the Agilent ADS 2 to generate calibration standards across the required concentration ranges.
• Autocalibration reduced manual handling time and minimized preparation errors.

Used Instrumentation

• Agilent 5800 Vertical Dual View ICP-OES with radial viewing mode.
• MiraMist nebulizer, inert spray chamber, and demountable torch assembly.
• Advanced Valve System (AVS 7) for high-speed sample introduction.
• Advanced Dilution System (ADS 2) for automated standard and sample dilution.
• ICP Expert Pro software with IntelliQuant screening, wavelength star-rating, fitted background correction, and early maintenance feedback.

Main Results and Discussion

• All calibration curves demonstrated excellent linearity (R² > 0.999) over the targeted ranges.
• Method detection limits were below 1 mg/kg for most trace elements, enabling sensitive impurity detection.
• Spike recoveries for 16 trace elements ranged from 91 % to 107 %, confirming method accuracy.
• Quantitation of two LATP batches revealed major constituents and impurities such as Fe, Mg, and Na, with automatic dilution handling overrange signals.
• Stability testing over two hours showed relative standard deviations below 1 % for matrix elements, demonstrating robust performance.

Benefits and Practical Applications

• Fully automated workflow minimizes manual intervention, reduces standard preparation time, and lowers consumable waste.
• Comprehensive multi-element detection supports R&D and quality control in solid-state battery material production.
• High sensitivity and precision enable monitoring of critical doping levels and trace impurities that affect battery life and safety.

Future Trends and Applications

• Integration of automated ICP-OES with data analytics and machine learning for predictive quality control of electrolyte materials.
• Extension of automated multi-element methods to other solid electrolytes and full-cell battery components.
• Development of compact, on-site elemental screening tools for real-time process monitoring in battery manufacturing.

Conclusion

An automated ICP-OES method combining advanced autodilution, robust calibration, and software-driven analytics has been developed for rapid, precise multi-element analysis of LATP solid electrolytes. This approach enhances laboratory efficiency and ensures high-quality control in the development and production of all-solid-state batteries.

References

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