John Blackson

Structures and properties of disordered boron carbide coatings generated by magnetron sputtering

Disordered boron carbide coatings with their high hardness, high lubricity, and low surface friction have become the coatings of choice to enhance the wear performance of many existing products. These coatings have been successfully commercialized using a magnetron sputtering process. In this paper, the effects of one of the critical process parameters, bias voltage, on the chemistry, microstructure, and the properties of the coatings are discussed. In combination with microstructure examination, special emphasis was made on nanoscopic level chemical analyses in order to explain the effects of this process parameter. The substrate bias was found to have strong effects on the hardness and the stress of the coating, but it has little influence on the frictional characteristics of the coating. The results of the examination and the analyses of the coating using FTIR, XPS, TEM, PEELS, and SIMS revealed that the morphology of the coating changed from a columnar structure to a continuous solid structure as the substrate bias voltage increased from 0 to 200 V. Oxide species were found in between the columns, while the columns mainly consisted of boron carbide with a boron to carbon atomic ratio of about 4. The atomic ratio of boron to carbon appeared to be independent of the substrate bias.

In Situ Electron Microscopy Studies of the Sintering of Palladium Nanoparticles on Alumina during Catalyst Regeneration Processes

Sintering of a palladium catalyst supported on alumina (Al2O3) in an oxidizing environment was studied by in situ transmission electron microscopy (TEM). In the case of a fresh catalyst, sintering of Pd particles on an alumina surface in a 500 mTorr steam environment happened via traditional ripening or migration and coalescence mechanisms and was not significant unless heating above 500 degrees C. After the catalyst was used for the hydrogenation of alkynes, TEM coupled with convergent beam electron diffraction and electron energy loss spectroscopy analysis revealed that most of the Pd particles were lifted from the alumina surface by hydrocarbon buildup. This dramatically different morphology totally changed the sintering mechanism of Pd particles during the regeneration process. Catalytic gasification of hydrocarbon around these particles in an oxidizing environment allowed the Pd particles to move around and coalesce with each other at temperatures as low as 350 degrees C. For catalysts heating under 500 mTorr steam at 350 degrees C, steam stripped hydrocarbon catalytically at the beginning, but the reaction stopped after 4 h. Heating in air resulted in both catalytic and noncatalytic stripping of hydrocarbon.

Automated Image Acquisition at High Spatial Resolutions in a Field Emission Gun Scanning Electron Microscope

Extended abstract of a paper presented at Microscopy and Microanalysis 2008 in Albuquerque, New Mexico, USA, August 3 – August 7, 2008