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@PHDTHESIS{Dellen:829751,
      author       = {Dellen, Christian},
      title        = {{Q}uantitative {A}nalyse der {L}ithiumverteilung in
                      {K}athoden und {E}lektrolyt-{D}ünnschichten für
                      {F}estkörperbatterien},
      volume       = {363},
      school       = {Universität Bochum},
      type         = {Dr.},
      address      = {Jülich},
      publisher    = {Forschungszentrum Jülich GmbH Zentralbibliothek, Verlag},
      reportid     = {FZJ-2017-03385},
      isbn         = {978-3-95806-214-6},
      series       = {Schriften des Forschungszentrums Jülich Reihe Energie $\&$
                      Umwelt / Energy $\&$ Environment},
      pages        = {vi, 161 S.},
      year         = {2017},
      note         = {Universität Bochum, Diss., 2016},
      abstract     = {When searching for new powerful energy storage systems for
                      mobile consumer electronics and a sustainable energy supply,
                      the development in the field of lithium ion batteries was
                      highly pushed in last years. As part of this development the
                      so called solid state batteries have recently attracted a
                      lot of attention as a promising energy storage system for
                      future applications. In a solid state battery the
                      combustible liquid electrolyte, which is used in
                      conventional lithium ion batteries, is replaced by a solid
                      state li ion conductor. Hereby the safety and the
                      performance of the battery system can be increased
                      tremendously. Within this work the quantitative analysis of
                      the lithium distribution in cathode and electrolyte thin
                      films for solid state batteries is addressed as one major
                      issue of the current battery research. The lithium
                      distribution can be regarded as a crucial parameter within
                      the processing of battery materials as well as in the
                      operation of the whole battery system. Unfortunately lithium
                      cannot be quantified by the commonly used characterization
                      techniques. Therefore secondary ion mass spectrometry (SIMS)
                      was used in this work to derive depth resolved concentration
                      profiles of lithium containing thin films. As model systems
                      for the quantitative analysis of lithium, thin films of the
                      cathode material LiCoO$_{2}$ and the solid state electrolyte
                      Li$_{6.6}$La$_{3}$Zr$_{1.6}$Ta$_{0.4}$O$_{12}$ were
                      selected. These were prepared by magnetron sputtering and
                      characterized with a variety of analytical techniques. In
                      addition to the SIMS as the primary analytical method,
                      further techniques like nuclear reaction analysis (NRA),
                      Rutherford backscattering (RBS) and glow discharge optical
                      emission spectroscopy (GDOES) were employed. In case of the
                      LiCoO$_{2}$ thin films, the lithium distribution was
                      investigated as a function of the cathode’s state of
                      charge. Therefore the thin films were first cycled in the
                      voltage range from 3.0 V to 4.1 V vs. Li/Li$^{+}$ and
                      afterwards the elemental composition was analyzed. These
                      measurements revealed a stepwise lithium profile in the
                      charged LiCoO$_{2}$ thin films, showing a delithiated area
                      close to the electrolyte facing surface and a fully
                      lithiated area in the proximity of the substrate. In
                      addition, quantitative SIMS concentration profiles were
                      calculated with relative sensitivity factors (RSF), derived
                      from NRA reference measurements. These profiles showed that
                      the surface area of the charged thin film cathodes is
                      delithiated below the reversible limit of
                      Li$_{0.5}$CoO$_{2}$, which is well known for bulk
                      LiCoO$_{2}$ cathodes. The elemental distribution within the
                      Li$_{6.6}$La$_{3}$Zr$_{1.6}$Ta$_{0.4}$O$_{12}$ thin films
                      was analysed as a function of the deposition temperature.
                      The combined SIMS and NRA analysis of thin films deposited
                      in the temperature range between 150 $^{\circ}$C and 800
                      $^{\circ}$C revealed an increasing lithium concentration
                      with temperature. At elevated temperatures, the formation of
                      an Al$_{2}$O$_{3}$ interlayer on top of the used FeCrAlY
                      substrates was observed as well as the reaction of this
                      interlayer with lithium from the
                      Li$_{6.6}$La$_{3}$Zr$_{1.6}$Ta$_{0.4}$O$_{12}$. The measured
                      elemental distribution was also affected by a surface
                      reaction of the lithium rich
                      Li$_{6.6}$La$_{3}$Zr$_{1.6}$Ta$_{0.4}$O$_{12}$ thin films.
                      In principle, the quantitative SIMS analyses were able to
                      visualize the depth resolved changes in the lithium
                      concentration. But in comparison to the NRA results, the
                      SIMS analyses systematically overestimated the absolute
                      lithium content.},
      cin          = {IEK-1},
      cid          = {I:(DE-Juel1)IEK-1-20101013},
      pnm          = {131 - Electrochemical Storage (POF3-131)},
      pid          = {G:(DE-HGF)POF3-131},
      typ          = {PUB:(DE-HGF)3 / PUB:(DE-HGF)11},
      url          = {https://juser.fz-juelich.de/record/829751},
}