Microstructural study of aluminide surface coatings on single crystal nickel base superalloy substrates

Aluminide diffusion coatings are frequently employed to enhance the oxidation resistance of nickel base superalloys. However, there is a concern that the presence of an aluminide coating could influence the properties of the coated superalloy, especially in respect of fatigue behaviour. To understand the nature of the effects of surface coatings on the fatigue properties of superalloys, an understanding of microstructural development within both the coating and the coating/substrate interfacial zone during high temperature fatigue testing is necessary. This paper is concerned with microstructural changes in aluminide diffusion coatings on single crystal γ′ strengthened superalloy substrates during the course of high temperature fatigue testing. The 'edge on' transmission electron microscopy technique is employed to study cross-sections of two stage (aluminization plus diffusion treatment) coated superalloy samples. The paper examines the degradation of the coating produced by phase transformations induced by loss of aluminum from the coating and/or aging of the coating. Aluminum removal both by interdiffusion with the substrate and by oxidation of the coating surface is considered. Microstructural development in the portion of the substrate influenced by interdiffusion with the coating is also discussed.

Microstructural development in aluminide diffusion coatings on nickel-base superalloy single crystals

An investigation has been made of the microstructural stability of aluminide diffusion coatings during post-coating thermal exposure. This study has employed edge-on transmission electron microscopy to examine high-activity pack aluminised single crystals of a gamma prime strengthened nickel-base superalloy. The influence of exposure temperature, duration and atmosphere as well as the initial coating thickness has been assessed. Two major processes have been found to contribute to microstructural changes in the coating. These are, firstly, the transformation of the coating matrix (β-phase, nominally NiAl) to other Ni-Al based phases, especially γ' (nominally Ni3(Al, Ti)) and, secondly, the precipitation of chromium containing phases. The work has enabled the roles of three processes contributing to γ formation, namely: oxidation of the coating surface, interdiffusion with the substrate and ageing of the coating, to be understood. In addition, the factors leading to the formation of a sequence of chromium-containing phases have been identified.

Physicochemical properties of WOx/ZrO2 catalysts for palmitic acid esterification

A series of WOx/ZrO2 with various tungsten loadings was prepared via incipient-wetness impregnation of zirconium hydroxide. The resulting thermally processed materials were characterised by XRD, XPS, porosimetry, NH3-TPD and pyridine FTIR spectroscopy to elucidate their composition, morphology and acidity, and subsequently tested in the esterification of palmitic acid with methanol. Catalytic performance was strongly dependent upon calcination temperature and W surface density. Esterification activity increased with increasing surface W density, reaching a maximum at 8.9Wnm-2 corresponding to near monolayer coverage. Subsequent growth of crystalline WO3 lowered activity, consistent with a decrease in the density of active surface sites. Calcination temperatures as high as 800°C increased surface acidity and hence catalytic activity. The formation of polymeric tungstate species on zirconia is necessary to generate the Brönsted acid sites responsible for palmitic acid esterification under mild conditions. © 2014 Elsevier B.V.

High activity, templated mesoporous SO4/ZrO2/HMS catalysts with controlled acid site density for α-pinene isomerisation

Highly active mesoporous SO4/ZrO2/HMS (hexagonal mesoroporous silica) solid acid catalysts with tuneable sulphated zirconia (SZ) content have been prepared for the liquid phase isomerisation of α-pinene. The mesoporous HMS framework is preserved during the grafting process as evidenced by the X-ray diffraction (XRD) and porosimetry with all SO4/ZrO2/HMS materials possessing average pore-diameters ∼20 Å. XRD confirms the presence of a stabilized tetragonal phase of nanoparticulate ZrO2, with no evidence for zirconia phase separation or the formation of discrete crystallites, consistent with a uniform and highly dispersed SZ coating. The activity towards α-pinene isomerisation scales linearly with Zr loading, while the specific activities are an order of magnitude greater than attainable by conventional methodologies (∼1 versus 0.08 mol h−1 g Zr−1).

Nanoscratch and nanowear testing of TiN coatings on M42 steel

Constant load, progressive load and multipass nanoscratch (nanowear) tests were carried out on 500 and 1500 nm TiN coatings on M42 steel chosen as model systems. The influences of film thickness, coating roughness, scratch direction relative to the grinding grooves on the critical load in the progressive load test and number of cycles to failure in the wear test have been determined. Progress towards the development of a suitable methodology for determining the scratch hardness from nanoscratch tests is discussed. © 2011 W. S. Maney & Son Ltd.