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Determination of Nickel, Cobalt and Manganese in Lithium Nickel–Cobalt–Manganese Oxide Battery Materials by X-Ray Fluorescence Spectrometry with Fusion Preparation

Author(s)

Lei Yu1,2, Yuting Zuo1, Xiao Zhang1,2,*, Yin Yang1, Tian Li1,2, Li Wang2,*, Ruixin Liu2

Affiliation(s)

1China United Test & Certification Co., Ltd., Beijing, China 2Guobiao (Beijing) Testing & Certification Co., Ltd., Beijing, China *Corresponding Author

Abstract

This study established a rapid method for the simultaneous determination of nickel, cobalt, and manganese in lithium nickel–cobalt–manganese oxide (NMC). Sample preparation employed fusion pretreatment using a mixed flux of lithium tetraborate and lithium metaborate (67:33 mass ratio), followed by pre-oxidation at 700 °C for 10 min, fusion at 1150 °C, and artificial synthesis of calibration standards with well-defined concentration gradients from high-purity reference reagents. Quantitative analysis was performed using a wavelength-dispersive X-ray fluorescence (WDXRF) spectrometer. Key analytical parameters—including flux composition, flux-to-sample dilution ratio, excitation voltage and current, and matrix correction-were systematically optimized. Under the optimized conditions, certified reference materials were analyzed. The measured values fell within the certified uncertainty intervals, and the relative standard deviation (RSD) for replicate analyses was less than 2%. The results demonstrate that this method is rapid, accurate, and fully suitable for quality control analysis of lithium nickel–cobalt–manganese oxide battery materials.

Keywords

Lithium Nickel Cobalt Manganate; Cathode Battery Material; X-Ray Fluorescence Spectrometry; Fusion Preparation

References

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