Synchrotron radiation-based x-ray reflection and scattering techniques for dimensional nanometrology

Abstract

Nanoobjects have at least one dimension in the range from 1 to 100 nm. Thus, if radiation is used for dimensional metrology, it should preferably have a wavelength in or below this range. For example, x-ray reflectometry (XRR) using x-ray tubes with Cu Kα radiation is widely used for layer thickness measurements with relative uncertainties of about 1%. By using different monochromator beamlines in the laboratory of PTB at the synchrotron radiation facility BESSY II, any x-ray wavelength from several nanometers down to about 0.1 nm can be selected for dimensional measurements in the nanometer range. Here, XRR is performed at wavelengths in the vicinity of an absorption edge of the chemical elements involved in order to enhance the contrast for layer systems like SiO2/Si which are difficult to resolve with Cu Kα radiation. By using longer wavelengths of around 2 nm, even an oxide layer and a thin carbonaceous contamination layer on a strongly curved spherical surface were separated, as required for measurements at 95 mm diameter silicon spheres within the international Avogadro project for the new definition of the kilogram. For nanoparticles in suspension, small angle x-ray scattering (SAXS) is the method of choice for dimensional metrology. This ensemble technique requires intense, monochromatic x-rays of low divergence. From the scattering pattern, the particle diameter and the size distribution are obtained. Moreover, the dimensional properties of nanostructured surfaces and nanoparticles on surfaces have been studied by grazing incidence SAXS (GISAXS), combining small angle scattering with the reflection geometry known from XRR. The diameters of gold nanoparticles obtained by SAXS and GISAXS are in very good agreement.