Technical University of Berlin , Institute of Optics and Atomic Physics, Hardenbergstraße 36, D-10587 Berlin, Germany.
Humboldt University of Berlin , School of Analytical Sciences Adlershof (IRIS-Building), Unter den Linden 6, D-10099 Berlin, Germany.
Anal Chem. 2017 Feb 7;89(3):1965-1971. doi: 10.1021/acs.analchem.6b04449. Epub 2017 Jan 10.
Grazing incidence and grazing emission X-ray fluorescence spectroscopy (GI/GE-XRF) are techniques that enable nondestructive, quantitative analysis of elemental depth profiles with a resolution in the nanometer regime. A laboratory setup for soft X-ray GEXRF measurements is presented. Reasonable measurement times could be achieved by combining a highly brilliant laser produced plasma (LPP) source with a scanning-free GEXRF setup, providing a large solid angle of detection. The detector, a pnCCD, was operated in a single photon counting mode in order to utilize its energy dispersive properties. GEXRF profiles of the Ni-L line of a nickel-carbon multilayer sample, which displays a lateral (bi)layer thickness gradient, were recorded at several positions. Simulations of theoretical profiles predicted a prominent intensity minimum at grazing emission angles between 5° and 12°, depending strongly on the bilayer thickness of the sample. This information was used to retrieve the bilayer thickness gradient. The results are in good agreement with values obtained by X-ray reflectometry, conventional X-ray fluorescence and transmission electron microscopy measurements and serve as proof-of-principle for the realized GEXRF setup. The presented work demonstrates the potential of nanometer resolved elemental depth profiling in the soft X-ray range with a laboratory source, opening, for example, the possibility of in-line or even in situ process control in semiconductor industry.
掠入射和掠出射 X 射线荧光光谱学(GI/GE-XRF)是一种能够对元素深度分布进行非破坏性、定量分析的技术,其分辨率可达纳米级。本文提出了一种软 X 射线 GE-XRF 测量的实验室装置。通过将高亮度激光产生等离子体(LPP)源与无扫描 GE-XRF 装置相结合,可以实现合理的测量时间,从而提供大的探测立体角。探测器是一个 pnCCD,以单光子计数模式运行,以利用其能量色散特性。对具有横向(双)层厚度梯度的镍-碳多层样品的 Ni-L 线的 GE-XRF 谱进行了在几个位置的记录。理论谱线的模拟预测,在掠出射角为 5°至 12°之间会出现显著的强度最小值,这强烈依赖于样品的双层厚度。该信息用于获取双层厚度梯度。结果与通过 X 射线反射测量、常规 X 射线荧光和透射电子显微镜测量获得的值非常吻合,证明了所实现的 GE-XRF 装置的原理。本文的工作展示了使用实验室光源对软 X 射线范围内的纳米分辨元素深度分布进行探测的潜力,例如为半导体工业中的在线或甚至原位过程控制开辟了可能性。