The authors report determination of interlayer composition with subnanometer sensitivity at the buried interfaces using soft x-ray resonant reflectivity technique. Near the absorption edge, fine structure features of energy-dependent atomic scattering factor are sensitive to the composition, and can be exploited for determination of composition at the buried interfaces. This technique is demonstrated for a Mo–Si multilayer system using soft x-ray resonant reflectivity measurement.

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A multilayer structure consisting of alternate layers of W and B4C has been deposited using a magnetron sputtering system. The structure of the as-deposited and vacuum-annealed W/B4C multilayer sample has been characterized using grazing incidence x-ray reflectivity, grazing incidence diffraction, and the normal incidence reflectivity has been measured using synchrotron radiation. A two-layer model consisting of tungsten and boron carbide is presented. The multilayer structure was found to be stable after 800°C annealing. Grazing incidence x-ray diffraction measurements suggested that W is polycrystalline with small grain size. No signature of tungsten carbide or tungsten boride formation could be observed during the annealing treatments. A near normal incidence soft x-ray reflectivity (SXRR) of ~8.3% was obtained at 6.8 nm wavelength. A little drop (~1%) in SXRR after 800°C annealing suggested that there were no compositional changes within the layers during the annealing treatments.

The microstructure and residual stress are investigated in W/B4C x-ray multilayer (ML) mirrors as a function of the number of layer pairs (N) varying from 20 to 400 at a fixed period, d ≈ 1.9 nm. The microstructure is analyzed using the x-ray reflectivity (XRR) and rocking scan methods. The total residual stress in the ML film is derived using the substrate curvature measurement method, whereas the stress in W layers of MLs is separately determined by grazing incidence x-ray diffraction measurements based on the sin2 χ method using synchrotron. The successive order Bragg peaks in XRR measured curves indicate good quality of the ML structure in terms of interface roughness and thickness errors. As N increases, the interface width of B4C and W varies in the range of 0.15–0.22 nm and 0.26–0.44 nm, respectively. The contribution of physical roughness to the interface width is significantly lower (∼sub-angstrom) compared to interfacial diffuseness (angstrom level) along with a small (few nanometers) correlation length in the ML structures as observed by rocking scan measurements. The residual stresses both in the W layers and in the ML film are compressive in nature. The total stress in the ML film decreases from −1.444 GPa to −0.389 GPa with increasing N. Measured residual stress in the ML film and W layers is correlated considering a net combined tensile stress arising from B4C layers and interfaces. The ML film with N = 400 shows the least residual stress and is suitable for large layer pair ML optics. Microstructure and stress are correlated considering the mechanism of film growth at the early stage and is discussed.