Microstructural investigations of optical coatings by backscattering spectrometry, electron diffraction, and spectrophotometry.

Abstract

Backscattering spectrometry with MeV ⁴He ion beams is investigated as a tool for determining composition with applications to optical coatings. Equations for the compositional analysis of thin films are reviewed. The effect of nuclear charge screening on compositional analysis by MeV ⁴He beams is discussed and examples involving the lanthanide trifluorides illustrate the importance of this correction to avoid possibly erroneous conclusions about sample composition. High probe beam energy is also briefly discussed as a method of reducing the overlap of peaks in backscattering spectra which reduces the technique's accuracy. Complications such as non-Rutherford scattering cross sections for light elements are addressed and an example given. The application of backscattering spectrometry to the depth profiling of elemental constituents in thin films is discussed. It is found that the backscattering spectrum itself provides a reasonable depth profile; however, its depth resolution is limited by the energy resolution of the detection system and energy straggling of the probe beam in the solid. In addition, the depth profile suffers from considerable noise. A method is derived using the principle of maximum likelihood which allows hypothetical depth profiles to be tested and the effects of energy straggling and detection system resolution to be separated from the depth profile. Several examples involving two hypothetical depth profile models are presented. Finally, backscattering spectrometry is combined with scanning electron microscopy, transmission electron microscopy, electron diffraction, x-ray photoelectron spectroscopy, and spectrophotometry in a microstructural survey of hafnium dioxide optical coatings deposited by electron beam evaporation and ion-assisted deposition (IAD). It is found that hafnium dioxide films deposited at temperatures below 300°C are amorphous and exhibit a negative optical inhomogeneity. The refractive index as well as the inhomogeneity are strongly influenced by the oxygen present during film deposition. The inhomogeneity can be removed by IAD which also increases the refractive index of the film. In addition, low energy IAD is found to increase the refractive of the films without affecting the inhomogeneity. This is explained by the preferential sputtering of hydroxide from the growing film surface by the bombarding ions.