Work

Comparative Insights Into the Accuracy of Quantitative Phase Analysis of Lithium‐Ion Battery Recycling Slags

Year: 2026

Type: article

Abstract: Slags from pyrometallurgical lithium‐ion battery (LIB) recycling can be thermochemically conditioned to form lithium‐bearing engineered artificial minerals (EnAM), increasing recyclability. Accurate quantification of the lithium‐bearing EnAM is crucial to evaluate the results of the conditioning and assess valorization. However, reliably quantifying the phase assemblage in slag remains challenging due to its chemical and microstructural properties. Here, a conditioned LIB‐recycling slag is investigated using complementary bulk, local, and structural analytical methods. Rietveld analysis‐based phase quantification, employing internal standard method, spiking, and micronizing, is directly compared with quantitative image analysis of backscattered electron images. The bulk and local chemical composition of the slag is investigated by wavelength‐dispersive X‐ray fluorescence spectroscopy, inductively coupled plasma optical emission spectroscopy, and electron probe microanalysis. The slag exhibits an average Li 2 O content of 3.33 mass%. Rietveld quantification yields 26.2 mass% of β‐eucryptite, the present lithium‐bearing EnAM, with a low random error, calculated using standard addition. However, quantitative image analysis returned 20.8 mass% ±2.5 mass% (2σ) β‐eucryptite. The overestimation by Rietveld method may be attributed to microabsorption effects caused by differences in X‐ray attenuation between phases. These findings highlight the importance of cross‐validating quantification results particularly in systems with highly varying mass attenuation coefficients.

Source: Advanced Energy and Sustainability Research

DOI: 10.1002/aesr.70289