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DDC: 540 × Subject: Laser ablation ×

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    Investigating the electrochemical stability of Li7La3Zr2O12 solid electrolytes using field stress experiments
    (London [u.a.] : RSC, 2021) Smetaczek, Stefan; Pycha, Eva; Ring, Joseph; Siebenhofer, Matthäus; Ganschow, Steffen; Berendts, Stefan; Nenning, Andreas; Kubicek, Markus; Rettenwander, Daniel; Limbeck, Andreas; Fleig, Jürgen
    Cubic Li7La3Zr2O12 (LLZO) garnets are among the most promising solid electrolytes for solid-state batteries with the potential to exceed conventional battery concepts in terms of energy density and safety. The electrochemical stability of LLZO is crucial for its application, however, controversial reports in the literature show that it is still an unsettled matter. Here, we investigate the electrochemical stability of LLZO single crystals by applying electric field stress via macro- and microscopic ionically blocking Au electrodes in ambient air. Induced material changes are subsequently probed using various locally resolved analysis techniques, including microelectrode electrochemical impedance spectroscopy (EIS), laser induced breakdown spectroscopy (LIBS), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), and microfocus X-ray diffraction (XRD). Our experiments indicate that LLZO decomposes at 4.1–4.3 V vs. Li+/Li, leading to the formation of Li-poor phases like La2Zr2O7 beneath the positively polarized electrode. The reaction is still on-going even after several days of polarization, indicating that no blocking interfacial layer is formed. The decomposition can be observed at elevated as well as room temperature and suggests that LLZO is truly not compatible with high voltage cathode materials.
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    Residual Layer Removal of Technical Glass Resulting from Reactive Atmospheric Plasma Jet Etching by Pulsed Laser Irradiation
    (Dordrecht : Springer Science + Business Media B.V., 2020) Kazemi, Faezeh; Arnold, Thomas; Lorenz, Pierre; Ehrhardt, Martin; Zimmer, Klaus
    Ultrahigh-precision machining of glass is indispensable for optical component fabrication and therefore for applications. In this regard, plasma jet assisted chemical etching technologies enable new fabrication processes for enhanced optical functionalities due to their deterministic localized machining capabilities. This technique has been successfully applied to fused silica and silicon. However, applications require specific glass properties are related to complex material compositions of the glass. Hence, reactive plasma etching of these optical glasses is a challenging task. For instance, etching of metal oxide containing glass like N-BK7 by a fluorine-based reactive atmospheric plasma jet (RAPJ) exhibits currently limitations due to the formation of non-volatile reaction products that remain on the glass surface as a layer. Therefore, a procedure consisting of RAPJ etching and laser ablation is proposed for the machining of N-BK7. The capability of laser-based removal of residual layers is compared to water-based solving of the residual layer. After RAPJ etching of N-BK7 using a CF4–O2 gas mixture with an average microwave power of 16 W, the samples are cleaned either by a water-based solvent or by the ablation with a nanosecond-pulsed ultraviolet laser. The laser irradiation with fluences of 2.8 J/cm2 results in a localized removal of the residual layer. It is demonstrated that the roughness of the laser-cleaned N-BK7 surface is similarly low as solvent-based cleaned samples but the pulsed laser enhanced cleaning allows a dry processing at atmospheric pressure as well as a localized processing with a high lateral resolution.