Search

Indentation tests were performed to assess the influence of compositional changes on the mechanical properties of several half-Heusler compounds with the general composition Zr0.5Hf0.5Co1-xIrxSb0.99Sn0.01 (x=0.0,0.1,0.3,0.5,0.7). These samples were synthesized by high temperature solid-state reactions and were consolidated by hot-pressing. Indentation measurements were obtained using both microhardness testing (Vickers) and depth-sensing nanoindentation. These measurements were used to determine the microhardness and the elastic modulus of each half-Heusler compound. The Vickers hardness values were found to range between 876 and 964. A slight increase in hardness was observed with the addition of iridium. The elastic stiffness values ranged from 229 GPa to 246 GPa. Here, a slight decrease in stiffness was observed with the addition of iridium.

Samples with a composition ZrNiSn were synthesized by a combination of mechanical alloying (MA) and consolidation by either Spark Plasma Sintering (SPS) or hot pressing (HP). Appropriate stoichiometric ratios of the starting materials were milled under an inert atmosphere in a high energy ball mill for 6 hours, achieving a half-Heusler phase. X-Ray diffraction patterns of as milled powders and consolidated samples were compared and analyzed for phase purity. Thermal conductivity, electrical conductivity and Seebeck coefficient were measured as a function of temperature in the range 300 K to 800 K and compared with measurements reported for high temperature solid state reaction synthesis of this compound. HP samples, compared to SPS samples, demonstrate increased grain growth due to longer heating times. Reduced grain size achieved by MA and SPS causes increased phonon scattering due to the increased number of grain boundaries, which lowers the thermal conductivity without doping the base system with addition phonon scattering centers.

Nd80Fe20 alloys were prepared by copper mold casting and directional solidification (DS) to obtain a coarse microstructure, which can be identified unambigously. The mold-cast samples exhibit a fine globular eutectic structure and show high room temperature coercivity (∼ 5 kOe). Transmission electron microscopic (TEM) investigations reveal the presence of fcc (a = 5.32 Å) Nd-rich and nanocrystalline non-cubic Fe-rich phases. The directionally solidified (DS) samples exhibit large grains (composition close to NdFe2). The NdFe2 grains (formed in the DS samples) show clear magnetic domains with uniaxial anisotropy indicating that the NdFe2-type phase observed in the present samples is not a cubic phase. X-ray absorption spectroscopy (XAS) was used to analyze the local configuration around Fe atoms in the mold-cast samples. The XAS patterns do not match with the bcc and fcc standards, which supports the presence of NdFe2 phase with uniaxial symmetry in the DS samples.

EXAFS and XANES analysis have been applied in a study of ball-milled nano-crystalline iron-nickel alloys prepared with overall compositions spanning the two-phase region. EXAFS analysis was used to determine bond distances for like and unlike atom pairs in single phase face-centered cubic Fe-Ni alloys, demonstrating the presence of bond dilation for unlike neighbors. Using XANES analysis, the compositions of the two coexisting solid solutions were determined to characterize the ball-milled two-phase region. The compositions of the coexisting face-centered and body-centered cubic phases were found to be consistent with the overall composition of the mixture. The results obtained for the negative heat-of-mixing Fe-Ni system were used for comparison to the positive heat-of-mixing Fe-Cu system.

An x-ray microprobe beamline was recently developed and commissioned at the Center for Advanced Microstructures and Devices (CAMD), Louisiana State University. It achieves a moderate horizontal and vertical focal spot size of 18.8 µm × 7.0 µm (σ), respectively. The beamline and end-station are designed and optimized to perform (i) spatially-resolved x-ray fluorescence spectroscopy (spectro-microscopy) using the broad intense spectrum of the white synchrotron radiation, and (ii) spatially-resolved x-ray absorption spectroscopy (micro-spectroscopy) in the energy region of 2100eV to 12000 eV. These dual capabilities enable K-edge measurements and mapping, in non-vacuum conditions, of low-Z elements down to Cl, S, and P that are of both environmental interest and technological importance. In this paper, an application of this novel synchrotron tool to elucidate the elemental distribution (microstructure) and chemical state (speciation) of Mn, Cl, S, and P-containing particulates emitted from automobile engines burning methylcyclopentadienyl manganese tricarbonyl- (MMT-) added fuel will be discussed in detail. Future opportunities of this microbeam technique in materials science and materials characterization will also be outlined.

A critical factor in the characterization of two-phase binary alloy systems is the determination of the phase fractions and compositions of the two coexisting solid solutions for any given overall composition of the two-phase mixture. In some systems, for example nanocrystalline alloys formed by high-energy ball-milling, these parameters are difficult to attain by traditional techniques like x-ray diffraction. A new technique has been developed to obtain these quantities indirectly from x-ray absorption near edge structure (XANES) data collected at the two relevant absorption edges, with the formulation of this technique presented here in detail. The technique has been tested using Fe-Ni fcc and bcc standards and the results indicate that the method is accurate to within 5%. This method has been applied to two-phase (f.c.c. and b.c.c.) binary alloys formed by ball-milling of Cu100-xFex(x = 50-80).

Extended x-ray absorption fine structure (EXAFS) and Raman spectroscopy measurements have been performed in a series of liquid polymer electrolytes prepared using poly(tetramethylene glycol) (PTMG), and copolymer poly(tetramethylene glycol/poly(ethylene glycol) (PTMG/PEG), as matrices, and ZnCl2or COCl2 as dopants in the concentration range of n = 30 to 90, where n is the molar ratio of Oxigen/Metal cation. EXAFS results have shown the presence of Co-O and Co-Cl coordination shells for PTMG/CoCl2 and PTMG/PEG/CoCl2 systems. Zn-based systems have shown only Zn-Cl bonds in all the concentration range studied. The presence of ZnCl2 and COCl2 species was confirmed by Raman measurements, by the presence of bands characteristic of CI-Zn-Cl and Co-Cl stretching modes.

The understanding of the physical, chemical and mechanical properties of materials used in micro-electromechanical systems (MEMS) is essential for the successful application. For the characterization of such materials, it is often necessary to utilize a probe which can gather information on the same scale as the devices themselves. Based on these needs, x-ray microprobe analysis has been employed to perform spatially resolved measurements on several problems related to the fabrication of MEMS devices. These include spatially resolved transmission measurements of the homogeneity of transmitted flux through a graphite mask, micro-fluorescence measurements to assess elemental distributions, and micro-XANES measurements to follow the breakdown of new sulfone-based x-ray resists. These studies demonstrate the value of such an instrument in the characterization of micro-systems.

An X-ray absorption beamline has been developed recently at the electron storage ring of the LSU Center for Advanced Microstructures and Devices. Using Extended X-ray Absorption Fine Structure (EXAFS) and X-ray Absorption Near Edge Structure (XANES), we have studied the local atomic environments in immiscible mixtures processed by high-energy ball milling, a mechanical alloying technique involving heavy deformation. By examining the local coordination and bond distances, it is concluded that atomic-level alloying can indeed be induced between Cu and Fe through milling at room temperature, forming substitutional fcc and bcc solid solutions. In addition to single-phase regions, a two-phase region consisting of fcc/bcc solutions has been found after milling at both room temperature and liquid nitrogen temperature. In contrast to the Cu-Fe system, solid solution formation is not detectable in milled Ag-Fe and Cu-Ta mixtures. This work demonstrates the power of synchrotron EXAFS/XANES experiments in monitoring nonequilibrium alloying on the atomic level. At the same time, the results provide direct experimental evidence of the capability as well as limitations of high-energy ball milling to form alloys in positive-heat-of-mixing systems.

Electroplating is a key technology in the LIGA process (German acronym for Lithographie (Lithography), Galvano (Electroplating) and Abformung (Moulding)). The electroplating process determines the physical, chemical, and mechanical properties of a device. In the macro environment, the process is empirically understood arid electroplating results are fairly well predictable. For use in the micro environment, in particular in microfabrication of LIGA components with high-aspect-ratios, effects like delamination from the substrate, inhomogeneous material distribution, pores in the material and large grain sizes have to be avoided. It is, therefore, important to investigate the structure and composition of such materials. Various electroplated Permalloy foils have been prepared, which are of interest because of their soft magnetic behaviour and use as materials for microsensors and microactuators. X-ray absorption fine structure (XAFS) and x-ray absorption near edge structure (XANES) have been recorded at the Nickel and Iron K-edges (8333 and 7112 eV respectively) for electroplated Permalloy.