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Deposition of HfO2 was undertaken by dip coating and CVD. Dip coated HfO2 was considered to be a relatively higher risk, but potentially lower cost approach for the coating system. The HfO2 dip coating process was pursued in collaboration with ORNL, who used their expertise to design the slurry system so as to obtain dense, crack-free coatings of HfO2. Figure 4.2.9 shows the cross-section obtained from slurry formulations using pure HfO2 powders. After heat treatment to densify the layer, the coatings were substantively free of cracks and porosity. Although the HfO2 coatings appeared to be well adhered to the underlying silicon layer, there were significant issues associated with maintaining coating adhesion after thermal cycling. Also, the coating was not gas tight and subsequent efforts for top layer coatings were focused on CVD HfO2. Figure 4.2.9: Dip coated HfO2 on CVD Si. (a) Top view and (b) Cross section UTRC worked in collaboration with Ultramet to develop and optimize a novel CVD process that would produce dense hafnium dioxide coatings of the appropriate microstructure, phase, and thickness. Early trials showed the coatings to be very thin (due to slow growth) or to have excessive thickness as shown in Figure 4.2.10. Optimized deposition parameters were developed and these CVD HfO2 coatings survived over 100 furnace thermal cycles to 2400F (1315C). Early attempts at steam testing the CVD HfO2 coatings showed further work needed to be done to provide steam resistance required of the full coating system. Yttrium silicate CVD Si Si3N4 Figure 4.2.10: Coating trials aimed at producing a “full EBC” system. 91 CVD HfO2PDF Image | ADVANCED MICROTURBINE SYSTEMS Final Report for Tasks 1 Through 4 and Task 6
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