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At least 73 records · Page 4

Examination of the Atomic Pair Distribution Function (PDF) of SiC Nanocrystals by In-situ High Pressure Diffraction

Key properties of nanocrystals are determined by their real atomic structure, therefore a reasonable understanding and meaningful interpretation of their properties requires a realistic model of the structure. In this paper we present an evidence of a complex response of the lattice distances to external pressure indicating a presence of a complex structure of Sic nanopowders. The experiments were performed on nanocrystalline Sic subjected to hydrostatic or isostatic pressure using synchrotron and neutron powder diffraction. Elastic properties of the samples were examined based on X-ray diffraction data using a Diamond Anvil Cell (DAC) in HASYLAB at DESY. The dependence'of the lattice parameters and of the Bragg reflections width with pressure exhibits a ha1 nature of the properties (compressibilities) of the powders and indicates a complex structure of the grains. We interpreted tws behaviour as originating from different elastic properties of the grain interior and surface. Analysis of the dependence of individual interatomic distances on pressure was based on in-situ neutron diffraction measurements done with HbD diffractometer at LANSCE in Los Alamos National Laboratory with the Paris-Edinburgh cell under pressures up to 8 GPa (Qmax = 26/A). Interatomic distances were obtained by PDF analysis using the PDFgetN program. We have found that the interatomic distances undergo a complex, non-monotonic changes. Even under substantial pressures a considerable relaxation of the lattice may take place: some interatomic distances increase with an increase in pressure. We relate this phenomenon to: (1), changes of the microstructure of the densified material, in particular breaking of its fractal chain structure and, (2), its complex structure resembling that of a material composed of two phases, each with its distinct elastic properties.

Grzanka, E.↗

The Effect of Solution Parameters on Lysozyme Nucleation Rates and Crystal Quality

In the pursuit of strongly diffracting high quality macromolecule crystals of suitable volume, this study investigates how the formation of macromolecules in solution and their growth characteristics effect crystal volume and diffracting quality. We systematically investigated the effect of solution conditions on lysozyme nucleation rates and the volume of crystals produced. Batch crystallization plates were used in combination with a video microscope system to measure nucleation rates and crystal volume. As expected from classical nucleation theory, crystal numbers were found to increase with increases in temperature and supersaturation. Small changes in solution pH, at constant supersaturation values were found, however, to dramatically effect the number of crystals nucleated in the wells varying from 1000s to 10s in the pH range 4.0 to 5.2. Having optimized the conditions required to produce an appropriate number of crystals of a suitable volume for X-ray analysis, a large number of uniform crystals were produced under exactly the same conditions. In the X-ray analysis of more than 50 such crystals there was found a wide variation in crystal lattice parameters and data quality. The variation in X-ray quality crystal samples is thought to be related to the growth rate variation caused by growth rate dispersion seen in lysozyme crystal growth experiments.

Judge, R. A.↗

Geometry of divergent-beam diffraction.

Divergent-beam diffraction geometry for interpretation of Kossel diffraction patterns in space group assignment lattice parameters and structure factor evaluation

CRYSTAL STRUCTURE↗

Crystal structure analysis of intermetallic compounds

Study concerns crystal structures and lattice parameters for a number of new intermetallic compounds. Crystal structure data have been collected on equiatomic compounds, formed between an element of the Sc, Ti, V, or Cr group and an element of the Co or Ni group. The data, obtained by conventional methods, are presented in an easily usable tabular form.

Conner, R. A., Jr.↗

NASA research on refractory compounds.

The behavior and properties of the refractory carbides, nitrides, and borides are being investigated by NASA as part of its research aimed at developing superior heat resistant materials for aerospace applications. Studies of the zirconium-carbon-oxygen system show that zirconium oxycarbides of different compositions and lattice parameters can be formed between 1500 C and 1900 C and are stable below 1500 C. More applied studies show that hot working generally improves the microstructure and therefore the strength of TiC and NbC. Sintering studies on UN indicate that very high densities can be achieved. Hot pressing of cermets of HfN and HfC produces good mechanical properties for high temperature bearing applications. Attempts to improve the impact resistance of boride composites by the addition of a nickel or carbon yarn were not overly successful.

Gangler, J. J.↗

NASA research on refractory compounds.

The behavior and properties of the refractory carbides, nitrides, and borides are being investigated by NASA as part of its research aimed at developing superior heat resistant materials for aerospace applications. Fundamental studies on the electronic and defect structures of the carbides indicate that there is promise for improving the strength and ductility of these materials. Studies of the zirconium-carbon-oxygen system show that zirconium oxycarbides of different compositions and lattice parameters can be formed between 1500 and 1900 C and are stable below 1500 C. More applied studies show that hot working generally improves the microstructure and therefore the strength of TiC and NbC. Sintering studies on UN indicate that very high densities can be achieved. Hot pressing of cermets of HfN and HfC produces good mechanical properties for high temperature bearing applications.

Gangler, J. J.↗

Identification of a new lithium oxide, Li3O2

Lithium oxide (Li3O2) was prepared by decomposing anhydrous lithium hydroxide at 360 C in 48 hours and between 640 and 730 C in times up to 1.3 hours and pressures of about 0.00001 torr. Decompositions were done in nickel, molybdenum, niobium, tantalum, and the T-111 tantalum alloy (Ta - 8-wt.% W - 2 wt.% Hf) containers. This oxide probably belongs to the simple orthorhombic system with the following lattice parameters: a = 108.4 + or - 0.4 nm (10.84 + or - 0.04 A), b = 128.4 + or - 0.5 nm (12.84 + or - 0.05 A), and c = 103.6 + or - 0.4 nm (10.36 + or - 0.04 A).

Stecura, S.↗

Observation of oxide particles below the apparent oxygen solubility limit in tantalum

The apparent solubility of oxygen in polycrystalline tantalum as determined by the X-ray diffraction lattice parameter technique is about 1.63 atomic percent at 820 C. However, oxide particles were identified in samples containing as low as 0.5 atomic percent of oxygen. These oxide particles were present at the grain boundaries and within the grains. The number of oxide particles increased with increasing oxygen concentration in tantalum. The presence of oxide particles suggests that the true solubility of oxygen in the polycrystalline tantalum metal is probably significantly lower than that reported in the literature.

Stecura, S.↗

Fabrication of cermet bearings for the control system of a high temperature lithium cooled nuclear reactor

The techniques used to fabricate cermet bearings for the fueled control drums of a liquid metal cooled reference-design reactor concept are presented. The bearings were designed for operation in lithium for as long as 5 years at temperatures to 1205 C. Two sets of bearings were fabricated from a hafnium carbide - 8-wt. % molybdenum - 2-wt. % niobium carbide cermet, and two sets were fabricated from a hafnium nitride - 10-wt. % tungsten cermet. Procedures were developed for synthesizing the material in high purity inert-atmosphere glove boxes to minimize oxygen content in order to enhance corrosion resistance. Techniques were developed for pressing cylindrical billets to conserve materials and to reduce machining requirements. Finishing was accomplished by a combination of diamond grinding, electrodischarge machining, and diamond lapping. Samples were characterized in respect to composition, impurity level, lattice parameter, microstructure and density.

Yacobucci, H. G.↗

Observation of oxide particles below the apparent oxygen solubility limit in tantalum

The apparent solubility of oxygen in polycrystalline tantalum as determined by the X-ray diffraction lattice parameter technique is about 1.63 at. pct at 820 C. However, oxide particles were identified in samples containing as low as 0.5 at. pct oxygen. These particles were present at the grain boundaries and within the grains. The number of oxide particles increased with increasing oxygen concentration in tantalum. The presence of oxide particles suggests that the true solubility in the polycrystalline tantalum metal is probably lower than that reported in the literature.

Stecura, S.↗

Research for preparation of cation-conducting solids by high-pressure synthesis and other methods

It was shown that two body-centered-cubic skeleton structures, the Im3 KSbO3 phase and the defect-pyrochlore phase A(+)B2X6, do exhibit fast Na(+)-ion transport. The placement of anions at the tunnel intersection sites does not impede Na(+)-ion transport in (NaSb)3)(1/6 NaF), and may not in (Na(1+2x)Ta2 5F)(Ox). The activation energies are higher than those found in beta-alumina. There are two possible explanations for the higher activation energy: breathing of the bottleneck (site face or edge) through which the A(+) ions must pass on jumping from one site to another may be easier in a layer structure and/or A(+)-O bonding may be stronger in the cubic structures because the O(2-) ion bonds with two (instead of three) cations of the skeleton. If the former explanation is dominant, a lower activation energy may be achieved by optimizing the lattice parameter. If the latter is dominant, a new structural principle may have to be explored.

Goodenough, J. B.↗

Research on metal solidification in zero-g state

The containerless solidification of several pure metals and metallic alloys was studied in a low gravity environment. The tests were performed in the MSFC 4.2 s drop tower using a rapid wire melting apparatus designed and built for this purpose. Pure iron and nickel, and alloys of iron-nickel, iron-carbon, nickel-aluminum and tungsten-rhenium were all melted and solidified at a gravity level of approximately 100.000/-4 g. Interpretation of the results has led to an appreciation of the factors controlling the successful execution of this drop test experiment and to a delineation of the limits of applicability of the apparatus. Preliminary metallurgical evaluations are presented of the overall shapes, lattice parameters, surface microstructure,, cross-sectional microstructures, solidification and transformation sequences, evaporative segregation, and localized solute redistribution observed in the low-gravity specimens. The effects of low gravity on metallic solidification are discussed with particular emphasis on observations of spontaneous undercooling and evaporative segregation in uncontained melts.

Papazian, J. M.↗

Kinetics of the phase transformation in a Ti-15Mo-5Zr-3Al alloy as studied by X-ray diffraction

The purpose of the study is to make the T-T-T diagram available and to describe the X-ray diffraction techniques used to determine the fraction of transformed phase in the Ti-15Mo-5Zr-3Al metastable beta-alloy which decomposes into the hexagonal alpha-phase and the bcc beta-phase of a higher Mo concentration. The sheet material studied for this study is not ideal for an X-ray examination because of both a rolling and annealing texture as well as grain size problems. These difficulties are overcome using special X-ray techniques. Equations are given that indicate the approximations to be accepted if pole figure data are disregarded. Lattice parameter data from the beta phase enables one to obtain an approximate phase diagram.

Rao, V. B.↗

Universal binding energy curves for metals and bimetallic interfaces

We provide evidence for a universal relationship between metallic binding energies and lattice parameters. By a simple scaling of a universal relationship, one can obtain binding energies as a function of atomic separation for bimetallic interfaces and bulk metals.

Rose, J. H.↗