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X-ray photoelectron spectroscopy: A perspective on quantitation accuracy for composition analysis of homogeneous materials
Journal of Vacuum Science & Technology A ( IF 2.4 ) Pub Date : 2020-06-26 , DOI: 10.1116/1.5143897
Christopher Richard Brundle 1 , Bruce Vincent Crist 2
Affiliation  

We present a perspective on the use of XPS relative peak intensities for determining composition in homogeneous bulk materials. Nonhomogenous effects, such as composition variation with depth or severe topography effects (e.g., in nanoparticles), are not discussed. We consider only the use of conventional laboratory-based instruments with x-ray sources, Alkα or Mgkα. We address accuracy (not precision, which is much more straightforward) using relative sensitivity factors, RSFs, obtained either empirically from standards (e-RSF) or from the use of theoretical cross sections, σ, (t-RSF). Issues involved are (1) the uncertainty of background subtraction of inelastically scattered electrons, (2) the accuracy of the RSFs, and (3) the role of XPS peak satellite structure, which affects both (1) and (2) above. The XPS of materials tends to fall into two broad classes: where the signals being used for quantification are “main” peaks, which are narrower and more symmetric, followed by a relatively low background with only weak satellite structure and where the “main” peaks are broader and often asymmetric, followed by backgrounds that are higher and have a stronger satellite structure. The former generally will yield better accuracy, more easily, than the latter. The latter comprises all compounds containing elements with open valence shell electrons. These are mostly the 3d, 4d, and 5d transition metals, the lanthanides, and the actinides. Compounds involving only the first row elements, Li to F, where the 1s binding energy is used for quantitation, are those where the best accuracy is potentially achievable. We specifically address the issue of long-claimed serious discrepancies between e-RSFs and t-RSFs, which were interpreted as indicating calculated σs, used as a parameter in t-RSFs, were seriously in error. We conclude this claim to be untrue and that, if done correctly, there is no disagreement between the two approaches within the limits of accuracy claimed. Finally, we suggest protocols for rapid element composition analysis by obtaining relative XPS signal intensities using only low energy resolution.

中文翻译:

X射线光电子能谱:均质材料成分分析的定量精度透视

我们介绍了使用XPS相对峰强度确定均质散装材料中成分的观点。没有讨论非均匀的影响,例如随着深度的成分变化或严重的形貌影响(例如,在纳米颗粒中)。我们只考虑用的X射线源使用传统的基于实验室仪器,ALK α或MGK α。我们使用相对敏感度系数RSF(从标准(e-RSF)或通过使用理论横截面σ(t-RSF)凭经验​​获得)来解决精度(不是精度,要简单得多)。涉及的问题是(1)非弹性散射电子的背景扣除的不确定性;(2)RSF的准确性;(3)XPS峰值卫星结构的作用,这会影响上述(1)和(2)。材料的XPS倾向于分为两大类:用于量化的信号是“主”峰,这些峰较窄且更对称,其次是背景相对较低且卫星结构较弱的“主”峰,以及“主”峰范围更广且通常不对称,其次是背景更高且具有更强卫星结构的背景。前者通常会比后者更容易获得更好的精度。后者包括所有含有具有开放价壳电子的元素的化合物。这些主要是3d,4d和5d过渡金属,镧系元素和the系元素。仅使用第一行元素Li至F的化合物(其中1s的结合能用于定量)是那些有可能实现最佳准确度的化合物。我们专门解决了长期以来人们一直认为e-RSF与t-RSF之间存在严重差异的问题,这些差异被解释为表明计算出的σs(用作t-RSF中的参数)存在严重错误。我们得出的结论是不真实的,并且,如果正确完成,则在所要求的精度范围内,这两种方法之间不会存在分歧。最后,
更新日期:2020-07-09
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