Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Clavería 8, 33006 Oviedo, Spain.
Anal Chim Acta. 2011 Jan 17;684(1-2):38-44. doi: 10.1016/j.aca.2010.10.039. Epub 2010 Nov 4.
In recent years particular effort is being devoted towards the development of pulsed GDs because this powering operation mode could offer important analytical advantages. However, the capabilities of radiofrequency (rf) powered glow discharge (GD) in pulsed mode coupled to optical emission spectrometry (OES) for real depth profile quantification has not been demonstrated yet. Therefore, the first part of this work is focussed on assessing the expected advantages of the pulsed GD mode, in comparison with its continuous mode counterpart, in terms of analytical emission intensities and emission yield parameters. Then, 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 50 W, a pressure of 600 Pa, 1000 Hz pulse frequency and 50% duty cycle were selected. The quantification procedure used was validated by analysing conductive layers of thicknesses ranging from a few tens of nanometer up to about 20 μm and varied compositions (hot-dipped zinc, galvanneal, back contact of thin film photovoltaic solar cells and tinplates).
近年来，人们特别致力于开发脉冲 GD，因为这种供电操作模式可以提供重要的分析优势。然而，射频 (rf) 供电辉光放电 (GD) 在与光发射光谱 (OES) 结合的脉冲模式下的能力，尚未在实际深度剖面定量方面得到证明。因此，这项工作的第一部分侧重于评估与连续模式相比，在分析发射强度和发射产率参数方面，脉冲 GD 模式的预期优势。然后，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。选择的射频正向功率为 50 W，压力为 600 Pa，脉冲频率为 1000 Hz，占空比为 50%。所使用的定量程序通过分析厚度从几十纳米到约 20 μm 不等且组成不同的导电层（热浸镀锌、锌铁合金、薄膜光伏太阳能电池的背接触和镀锡板）进行了验证。
