Publications

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In ductile metals, sliding contact is often accompanied by severe plastic deformation localized to a small volume of material adjacent to the wear surface. During the initial run-in period, hardness, grain structure and crystallographic texture of the surfaces that come into sliding contact undergo significant changes, culminating in the evolution of subsurface layers with their own characteristic features. Here, a brief overview of our ongoing research on the fundamental phenomena governing the friction-induced recrystallization in single crystal metals, and how these recrystallized structures with nanometer-size grains would in turn influence metallic friction will be presented. We have employed a novel combination of experimental tools (FIB, EBSD and TEM) and an analysis of the critical resolved shear stress (RSS) on the twelve slip systems of the FCC lattice to understand the evolution of these friction-induced structures in single crystal nickel. The later part of the talk deals with the mechanisms of friction in nanocrystalline Ni films. Analyses of friction-induced subsurfaces seem to confirm that the formation of stable ultrafine nanocrystalline layers with 2-10 nm grains changes the deformation mechanism from the traditional dislocation mediated one to that is predominantly controlled by grain boundaries, resulting in significant reductions in the coefficient friction.

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2-Chloroethyl phenyl sulfide (CEPS), a surrogate compound of the chemical warfare agent sulfur mustard, was examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a novel method of producing multiway data using a stepped thermal desorption. Various multivariate analysis schemes were employed to analyze the data. These methods may be able to discern different sources of CEPS. In addition, CEPS was applied to cotton, nylon, polyester, and silk swatches. These swatches were placed in controlled humidity chambers maintained at 23%, 56%, and 85% relative humidity. At regular intervals, samples were removed from each test swatch, and the samples analyzed using TD/GC-MS. The results were compared across fabric substrate and humidity.

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The major focus of this study was to examine the feasibility of applying diamond-like nanocomposite (DLN) coatings on the sidewalls of Ni alloy parts fabricated using lithographie, galvanoformung and abformung (LIGA: a German acronym that means lithography, electroforming, and molding) for friction and wear control. Planar test coupons were employed to understand the friction mechanisms in regimes relevant to LIGA microsytems. Friction tests were conducted on planar test coupons as well as between LIGA-fabricated test structures in planar-sidewall and sidewall-sidewall configurations. Measurements were made in dry nitrogen and air with 50% relative humidity by enclosing the friction tester in an environmental chamber. In contrast to bare metal-metal contacts, minimal wear was exhibited for the DLN-coated LIGA NiMn alloy parts and test coupons. The low friction behavior of DLN was attributed to its ability to transfer to the rubbing counterface providing low interfacial shear at the sliding contact. The coating coverage and chemistry on the sidewalls and the substrate-coating interface integrity were examined by transmission electron microscopy, Automated eXpert Spectral Image Analysis, and electron backscatter diffraction on cross sections prepared by focused ion beam microscopy. The role of novel characterization techniques to evaluate the surface coatings for LIGA microsystems technology is highlighted. © 2009 IEEE.

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Erbium is used as a storage medium for tritium. Microstructural study of helium bubble generation from tritium decay in erbium tritide can provide an unusual example of bubble development with negligible radiation damage. Aged erbium tritide film specimens were found to contain five distinctly different microstructural features. The general structure was of large columnar grains of ErT2. But on a fine scale, precipitates believed to be erbium oxy-tritides and helium bubbles could be identified. The precipitate size was in the range of ∼10 nm and the bubbles were of an unusual planar shape on {111} planes with an invariant thickness of ∼1 nm and a diameter on the order of 10 nm. Also, an outer layer containing no fine precipitate structure and only a few helium bubbles were present on the films. This layer is best described as a denuded zone which probably grew during aging in air. Finally, large embedded Er2O3 particles were found at low density and nonuniformly distributed, but sometimes extending through the thickness of the film. A failure mechanism allowing the helium to escape is suggested by observed cracking between bubbles closer to end of life. Copyright © 2007 by ASTM International.

Er(D,T){sub 2-x} {sup 3}He{sub x}, erbium di-tritide, films of thicknesses 500 nm, 400 nm, 300 nm, 200 nm, and 100 nm were grown and analyzed by Transmission Electron Microscopy, X-Ray Diffraction, and Ion Beam Analysis to determine variations in film microstructure as a function of film thickness and age, due to the time-dependent build-up of {sup 3}He in the film from the radioactive decay of tritium. Several interesting features were observed: One, the amount of helium released as a function of film thickness is relatively constant. This suggests that the helium is being released only from the near surface region and that the helium is not diffusing to the surface from the bulk of the film. Two, lenticular helium bubbles are observed as a result of the radioactive decay of tritium into {sup 3}He. These bubbles grow along the [111] crystallographic direction. Three, a helium bubble free zone, or 'denuded zone' is observed near the surface. The size of this region is independent of film thickness. Four, an analysis of secondary diffraction spots in the Transmission Electron Microscopy study indicate that small erbium oxide precipitates, 5-10 nm in size, exist throughout the film. Further, all of the films had large erbium oxide inclusions, in many cases these inclusions span the depth of the film.

Three-spatial-dimension (3D) time-of-flight-secondary ion mass spectrometry (TOF-SIMS) analysis can be performed if an X-Y image is saved at each depth of a depth profile. In this paper, we will show how images reconstructed from specified depths, depth profiles generated from specific X-Y coordinates, as well as three-spatial-dimensional rendering provide for a better understanding of the sample than traditional depth profiling where only a single spectrum is collected at each depth. We will also demonstrate, for the first time, that multivariate statistical analysis (MVSA) tools can be used to perform a rapid, unbiased analysis of the entire 3D data set. In the example shown here, retrospective analysis and MVSA revealed a more complete picture of the 3D chemical distribution of the sample than did the as-measured depth profiling alone. Color overlays of the MVSA components as well as animated movies allowing for visualization (in 3D) from various angles will be provided. © 2007 American Chemical Society.