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@ARTICLE{Evertz:851129,
      author       = {Evertz, Marco and Schwieters, Timo and Börner, Markus and
                      Winter, Martin and Nowak, Sascha},
      title        = {{M}atrix-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},
      journal      = {Journal of analytical atomic spectrometry},
      volume       = {32},
      number       = {10},
      issn         = {1364-5544},
      address      = {Cambridge},
      publisher    = {ChemSoc},
      reportid     = {FZJ-2018-04831},
      pages        = {1862 - 1867},
      year         = {2017},
      abstract     = {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.},
      cin          = {IEK-12},
      ddc          = {540},
      cid          = {I:(DE-Juel1)IEK-12-20141217},
      pnm          = {131 - Electrochemical Storage (POF3-131)},
      pid          = {G:(DE-HGF)POF3-131},
      typ          = {PUB:(DE-HGF)16},
      UT           = {WOS:000414347800003},
      doi          = {10.1039/C7JA00129K},
      url          = {https://juser.fz-juelich.de/record/851129},
}