Comparative Insights Into the Accuracy of Quantitative Phase Analysis of Lithium‐Ion Battery Recycling Slags
- 1Institute for Geosciences and Geography Martin‐Luther‐University Halle‐Wittenberg Halle (Saale) Germany
- 2Institute for Geosciences University of Potsdam Potsdam‐Golm Germany
- 3ITEL – Institute for Technologies and Economics of Lithium GmbH Halle (Saale) Germany
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 Li2O 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.
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BibTeX
@article{gantz2026comparative,
title = {{Comparative Insights Into the Accuracy of Quantitative Phase Analysis of Lithium‐Ion Battery Recycling Slags}},
author = {Peter Cornelius Gantz and Charlize Alexia Senkyr and Rüdiger Kilian and Maximilian Korges and Hans Roggendorf and Ralf Wehrspohn and Stefan Stöber and Christiane Stephan‐Scherb},
journal = {Advanced Energy \& Sustainability Research},
year = {2026},
month = oct,
doi = {10.1002/aesr.70289},
url = {https://doi.org/10.1002/aesr.70289},
note = {CC BY},
}
RIS
TY - JOUR
TI - Comparative Insights Into the Accuracy of Quantitative Phase Analysis of Lithium‐Ion Battery Recycling Slags
AU - Peter Cornelius Gantz
AU - Charlize Alexia Senkyr
AU - Rüdiger Kilian
AU - Maximilian Korges
AU - Hans Roggendorf
AU - Ralf Wehrspohn
AU - Stefan Stöber
AU - Christiane Stephan‐Scherb
PY - 2026
DA - 2026/10/28
JO - Advanced Energy & Sustainability Research
DO - 10.1002/aesr.70289
UR - https://doi.org/10.1002/aesr.70289
AB - 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 Li2O 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.
SN - 2699-9412
ER -