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| 100 | 1 | _ | |a Evertz, Marco |0 P:(DE-HGF)0 |b 0 |
| 245 | _ | _ | |a Matrix-matched standards for the quantification of elemental lithium ion battery degradation products deposited on carbonaceous negative electrodes using pulsed-glow discharge-sector field-mass spectrometry |
| 260 | _ | _ | |a Cambridge |c 2017 |b ChemSoc |
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| 520 | _ | _ | |a In this work an external calibration approach for glow discharge-sector field-mass spectrometry (GD-SF-MS) using matrix-matched self-prepared carbonaceous standards for elemental battery degradation products of LiNi1/3Co1/3Mn1/3O2 (NCM111) positive electrodes like lithium, manganese, cobalt and nickel is adapted. Firstly, the standards were prepared using graphite mixed with increasing contents of NCM111 which was coated on a thin copper foil as a current collector. The homogeneous distribution of NCM111 in the standards was proven via SEM/EDX images and the bulk homogeneity of the electrode sheets was validated via ICP-OES. Afterwards, sufficient linearity could be obtained in a calibration range of 1 mg g−1 to 28 mg g−1 for 7Li with respect to the active material mass. Additionally, the matrix-matched relative sensitivity factors (RSFs) of each element could be calculated. Limits of detection (LODs) ranging from 80 μg g−1 (7Li) up to 393 μg g−1 (58Ni) could be achieved at low (R > 300) and medium (R > 4000) resolutions for the Element GD, respectively. Secondly, we adapted the matrix-matched RSF values in order to investigate cycled electrodes by monitoring the 7Li signal as well as common isotopes from lithium ion batteries – such as 31P and 19F, originating from the conducting salt – and transition metals to conduct depth-resolved analysis. The concentration of transition metals in all of the cycled electrodes was below the LOD of the GD-SF-MS method which was investigated in a previous study, showing a maximum bulk deposition of transition metals of 4.5 mg g−1. As expected, an accumulation of 7Li in the first few minutes (=surface layers) of sputtering was observed in the cycled carbonaceous negative electrodes followed by a decreasing 7Li signal with ongoing sputtering indicating the presence of a solid electrolyte interphase (SEI) passivation layer. |
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| 700 | 1 | _ | |a Schwieters, Timo |0 P:(DE-HGF)0 |b 1 |
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| 700 | 1 | _ | |a Winter, Martin |0 P:(DE-Juel1)166130 |b 3 |u fzj |
| 700 | 1 | _ | |a Nowak, Sascha |0 0000-0003-1508-6073 |b 4 |e Corresponding author |
| 773 | _ | _ | |a 10.1039/C7JA00129K |g Vol. 32, no. 10, p. 1862 - 1867 |0 PERI:(DE-600)1484654-8 |n 10 |p 1862 - 1867 |t Journal of analytical atomic spectrometry |v 32 |y 2017 |x 1364-5544 |
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