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Phase evolution in a yttria-partially-stabilized zirconia (Y-PSZ) thermal barrier coating (TBC) was studied by using quantitative electron probe x-ray mapping combined with microbeam x-ray diffraction. The as-sprayed coating contains a single t' phase with the composition of the feedstock material. After annealing at 1400 °C for 1 hour, the yttria content of the t' phase increases slightly to compensate for the formation of 0.06 mass fraction of a t phase containing 0.01 mole fraction YO1.5. These results are in contrast to those determined by bulk x-ray and neutron diffraction, and therefore highlight the need for multiple techniques of phase analysis in Y-PSZ.
The use of digital electron microprobe x-ray compositional mapping with wavelength dispersive spectrometers to understand the microstructure of yttria stabilized zirconia thermal barrier coatings is described. Data from quantification of element x-ray maps can be utilized to infer what phase or phases are present. Analysis of a plasma-sprayed coating prepared from a fused and crushed feedstock is compared to an annealed specimen of the same material.
Bulk silicon-germanium (SiGe) alloys and two SiGe thick films (4 and 5 μm) on Si wafers were tested with the electron probe microanalyzer (EPMA) using wavelength dispersive spectrometers (WDS) for heterogeneity and composition for use as reference materials needed by the microelectronics industry. One alloy with a nominal composition of Si0.86Ge0.14 and the two thick films with nominal compositions of Si0.90Ge0.10 and Si0.75Ge0.25 on Si, evaluated for micro- and macroheterogeneity, will make good microanalysis reference materials with an overall expanded heterogeneity uncertainty of 1.1% relative or less for Ge. The bulk Ge composition in the Si0.86Ge0.14 alloy was determined to be 30.228% mass fraction Ge with an expanded uncertainty of the mean of 0.195% mass fraction. The thick films were quantified with WDS-EPMA using both the Si0.86Ge0.14 alloy and element wafers as reference materials. The Ge concentration was determined to be 22.80% mass fraction with an expanded uncertainty of the mean of 0.12% mass fraction for the Si0.90Ge0.10 wafer and 43.66% mass fraction for the Si0.75Ge0.25 wafer with an expanded uncertainty of the mean of 0.25% mass fraction. The two thick SiGe films will be issued as National Institute of Standards and Technology Reference Materials (RM 8905).