University of Oviedo, Department of Physical and Analytical Chemistry, Julian Claveria, 8, 33006 Oviedo, Spain.
Talanta. 2011 Apr 15;84(2):572-8. doi: 10.1016/j.talanta.2011.01.076. Epub 2011 Feb 4.
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.
近年来，人们特别致力于开发射频（rf）脉冲辉光放电（GD）与光谱发射（OES）相结合的方法，以对具有技术意义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 用于快速和灵敏地分析具有技术意义的材料的深度剖面，这些材料是在导电基底（Ti 和钢）上沉积的 Zn-TiO2 纳米复合材料薄膜。这项工作的第一部分主要评估了与连续 GD 相比，在分析发射强度和发射产率方面，脉冲 GD 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 用于确定厚度和组成深度剖面的能力。选择射频正向功率为 75 W、压力为 600 Pa、脉冲频率为 10 kHz 和占空比为 50%作为 GD 操作参数。采用提出的 GD 方法获得的 Zn-TiO2 纳米复合材料薄膜的定量深度剖面与互补技术（包括扫描电子显微镜和电感耦合等离子体质谱）的结果非常吻合。所进行的工作表明，脉冲 rf-GD-OES 是快速分析纳米复合材料薄膜的一种很有前途的工具。
