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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Depth profile characterization of Zn-TiO_2 nanocomposite films by pulsed radiofrequency glow discharge-optical emission spectrometry
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Depth profile characterization of Zn-TiO_2 nanocomposite films by pulsed radiofrequency glow discharge-optical emission spectrometry

机译：脉冲射频辉光放电-光发射光谱法表征Zn-TiO_2纳米复合薄膜的深度剖面

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摘要

In recent years particular effort is being devoted towards the development of radiofrequency (rf) pulsed glow discharges (GDs) coupled to optical emission spectrometry (OES) for depth profile analysis of materials with technological interest. In this work, pulsed rf-GD-OES is investigated for the fast and sensitive depth characterization of Zn-TiO_2 nanocomposite films deposited on conductive substrates (Ti and steel). The first part of this work focuses on assessing the advantages of pulsed GDs, in comparison with the continuous GD, in terms of analytical emission intensities and emission yields. Next, the capability of pulsed rf-GD-OES for determination of thickness and compositional depth profiles is demonstrated by resorting to a simple multi-matrix calibration procedure. A rf forward power of 75 W, a pressure of 600 Pa, 10 kHz pulse frequency and 50% duty cycle were selected as GD operation parameters.Quantitative depth profiles obtained with the GD proposed methodology for Zn-TiO_2 nanocomposite films, prepared by the occlusion electrodeposition method using pulsed reverse current electrolysis, have proved to be in good agreement with results achieved by complementary techniques, including scanning electron microscopy and inductively coupled plasma-mass spectrometry. The work carried out demonstrates that pulsed rf-GD-OES is a promising tool for the fast analytical characterization of nanocomposite films.
机译：近年来，人们特别致力于开发射频（rf）脉冲辉光放电（GDs）和光学发射光谱仪（OES），以对具有技术兴趣的材料进行深度剖面分析。在这项工作中，研究了脉冲rf-GD-OES对沉积在导电基底（Ti和钢）上的Zn-TiO_2纳米复合膜的快速灵敏的深度表征。这项工作的第一部分着重于评估脉冲式GD与连续GD相比在分析排放强度和排放产量方面的优势。接下来，通过采用简单的多矩阵校准程序，证明了脉冲rf-GD-OES用于确定厚度和成分深度轮廓的能力。 GD工作参数选择为75 W的射频前向功率，600 Pa的压力，10 kHz脉冲频率和50％的占空比。GD提出的方法制备的Zn-TiO_2纳米复合薄膜的深度深度分布图是通过咬合法制备的事实证明，使用脉冲反向电流电解的电沉积方法与包括扫描电子显微镜和电感耦合等离子体质谱法在内的互补技术所获得的结果非常吻合。进行的工作表明，脉冲rf-GD-OES是用于快速分析表征纳米复合膜的有前途的工具。

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