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Electron probe microanalysis (EPMA) measurement of thin-film thickness in the nanometre range
(2002)
The thickness of thin films of platinum and nickel on fused silica and silicon substrates has been determined by EPMA using the commercial software STRATAGEM for calculation of film thickness. Film thickness ranged in the order 10 nm. An attempt was made to estimate the confidence range of the method by comparison with results from other methods of analysis. The data show that in addition to the uncertainty of the spectral intensity measurement and the complicated fitting routine, systematic deviation caused by the underlying model should be added. The scattering in the results from other methods does not enable specification of a range of uncertainty, but deviations from the real thickness are estimated to be less than 20%.
Mechanical properties, i.e. hardness and elastic modulus, of amorphous SiO2 and Si3N4 PE-CVD coatings have been studied for two coating thicknesses (0.1 and 1.0 µm) and two substrate materials (fused silica, i.e. Herasil, and borosilicate glass, i.e., BK7) using low load instrumented indentation. The coating systems are being considered for possible use as reference materials for thin film mechanical property test methods. Single layers of SiO2 and Si3N4 and a multilayer stack consisting of five double layers of SiO2/Si3N4 (individual layer thickness: 0.1 µm) were investigated on both substrate materials. A special plasma pre-treatment of the substrates prior to deposition ensured that coating adhesion exceeded inner film stress for all systems considered. The applied indentation load ranged from 700 down to 0.1 mN and resulted in indentation depths from more than 1 µm to about 15 nm. The influence of coating thickness and the effect of the substrate on the measurement of hardness and elastic modulus of the films are discussed, with emphasis on the effects of indentation depth vs. coating thickness on the observed coating properties. One coatingsubstrate system (1.0 µm Si3N4 on Herasil) out of ten was found to be above a critical threshold for tensile cracking of the coating. In this system, termed overcritical, tensile cracks occurred both prior to, and as a result of, indentation, indicating that Berkovich indentation may also be used to probe residual film stress.