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At least 577 records · Page 32
All sourcesNASA NTRSDOE OSTI
DOE OSTI2011

Quantum control of stability of a discrete electron state coupled with a continuum by external oscillating fields

Numerical and theoretical analysis of electron survival probability is presented for the system where a periodically driven discrete state is coupled with continuum states of the tight-binding model. The stability of the discrete state is examined by analyzing the survival probability in the weak-coupling case. Stable nondecaying states as well as usual unstable decaying states appear in the systems where the oscillating energy of the discrete state and the energy band of the continuum states overlap. Dynamical stable states caused by the energy oscillation are qualitatively explained by an approximate solution of a periodically driven two-level model. The decay is suppressed as a result of vanishing reduced coupling constant at the resonance.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2013

Synthesis and electrical properties of Cu-doped tin oxide nanowires

We report on atmospheric pressure growth of Cu-doped Tin oxide nanowires by thermal evaporation method. Scanning-electron-microscopic analysis shows the growth of wire-like SnO{sub 2} nanostructures (diameter Almost-Equal-To 80 nm and length Almost-Equal-To 70 {mu}m) on gold catalyzed silicon substrate. The as-synthesized Cu-doped SnO{sub 2} nanowires show polycrystalline nature with tetragonal rutile structure. EDX analysis confirms that Cu ( Almost-Equal-To 0.7 at%) have been uniformly doped into SnO{sub 2} nanowires. Electrical measurement of Cu-doped SnO{sub 2} nanowires concludes their resistance of about 5 M{Omega} at room temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Characterization of the Uranium-Bearing Products of the Ammonia Injection Remediation Method - 15707

Commissioned in 1943, the Hanford Site is the home of the world's first full-scale nuclear production facility. After more than 40 years of processing, improper discharge and failed storage tanks have resulted in the contamination of the Hanford vadose zone with radiologically contaminated waste. Remediation methods considered for the area include sequestration of the mobile uranium by injection of ammonia (NH{sub 3}) gas. Injection of this reactive gas increases the pore water pH, promoting the dissolution of soil minerals; a subsequent re-establishment of natural conditions is believed to result in the recrystallization of those soil minerals and the co-precipitation of uranium phases. Characterization of the precipitates formed when the ammonia (NH{sub 3}) injection method, proposed for the Hanford vadose zone, is applied to synthetic pore water on a laboratory scale. This involves: Identification of the uranium-bearing phases; A study of the effect of pore water constitution on the phases produced. Synthetic pore water solutions were prepared to mimic selected constituents of the pore water from the Hanford 200 Area: Varying constituent concentrations; Observations led to modifications to increase relative uranium content: 200 ppm → 500 ppm U; Substituted sodium silicate for silicic acid. Dried samples were analyzed by SEM-EDS and powder X-ray diffraction (XRD). A suspension in ethanol was prepared and analyzed by Transmission Electron Microscope (TEM) with Selective Area Electron Diffraction (SAED). Studied and applied geochemical modeling software (Visual Minteq and Geo-chemist's Workbench) for speciation and prediction of potential species formed. Discussion/Conclusions: - SEM-EDS Analysis: Scanning electron microscopy revealed areas of high average atomic weight which would be confirmed to be uranium-rich by energy dispersive spectroscopy analysis. The samples prepared with a more than two-fold increase in uranium concentration did not show the crystal-like forms spotted in the lower [U] samples. The samples prepared with silicic acid substituted in showed little to no uranium precipitation [not shown]. - Diffraction Analysis: Powder XRD analysis of the low [U] samples confirmed the presence of repeating crystalline patterns in the precipitate samples. Nitratine (NaNO{sub 3}) showed a massive presence, potentially obscuring significant peaks in the low [U] samples. Though it was not predicted, there was a tentative match for cejkaite (Na{sub 4}(UO{sub 2})(CO{sub 3}){sub 3}). Elevated uranium samples showed none of the needle-like crystalline shapes [diffraction data pending]. TEM - SAED confirmed the presence of a polycrystalline phase. Data analysis is complex but a comparison of average d-spacings with those of reference minerals could further support a match with cejkaite. - Geochemical Modeling: The system conditions were input into geochemical modeling software to predict the forms present throughout the reaction process. The model was used to demonstrate that the pH of the system could be increased using [NH{sub 4}{sup +}] in solution to better represent the system. Using the [NH{sub 4}{sup +}] increase, the changes in significant species with increasing pH were observed. Future Work: Repeat samples will be prepared and analyzed to bolster any potential identification. Promising samples will be submitted to the PNNL's EMSL facility, which is better equipped to perform the required analyses. An expanded study on the impact of carbonate (CO{sub 3}{sup 2-}) on the phases produced.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1981

Probing the magnetsophere with artificial electron beams

An analysis is conducted of the University of Minnesota Electron Echo experiments, which so far have included five sounding rocket experiments. The concept of the Echo experiment is to inject electron beam pulses from a rocket into the ionosphere at altitudes in the range from 100 to 300 km. The electrons move to the conjugate hemisphere following magnetic field lines and return on neighboring field lines to the neighborhood of the rocket where the pulses may be detected and analyzed. Attention is given to the detection and analysis of echoes, the structure of echoes, and the Echo V experiment. The Echo V experiment showed clearly that detection of remote echo beams by atmospheric fluorescence using low light level TV system is not a viable technique. A future experiment is to use throw-away detectors for direct remote echo detection.

Winckler, J. R.↗
NASA NTRS1974

The protons and electrons trapped in the Jovian dipole magnetic field region and their interaction with Io

Detailed analysis of electrons equal to or greater than 3 MeV and of protons 0.5 to 1.8 MeV and equal to or greater than 35 MeV for both the inbound and the outbound passes of the Pioneer 10 spacecraft. Conclusive evidence is obtained that the trapped radiation in Jupiter's inner magnetosphere is maintained and supplied by inward diffusion from the outer regions of the trapped radiation zone. It is shown that the time required for isotropization of an anisotropic flux by pitch angle scattering inside L approximately equal to 6 is long in comparison with the time required for particles to diffuse inward from L approximately equal to 6 to L approximately equal to 3, that the high-energy protons were not injected at high energies by the Crand (cosmic ray albedo neutron decay) process but were accelerated in the magnetosphere of Jupiter, and that the main conclusions of this analysis are unaffected by use of either the D sub 1 or the D sub 2 magnetic field models. Theoretical studies of the capture of trapped electrons and protons by Io have been carried out, and it is found that the probability of capture by Io depends strongly upon the particle species and kinetic energy.

Simpson, J. A.↗
DOE OSTI2011

The system Ce-Zn-B at 800 deg. C

The isothermal section for the system Ce-Zn-B has been established at 800 deg. C using electron microprobe analysis and X-ray powder diffraction. No ternary compounds exist and mutual solid solubilities of binary phases are negligible. In the concentration range of 10.0-10.5 at% Ce two structural modifications have been confirmed: high temperature {beta}Ce{sub 2}Zn{sub 17} above {approx}750 deg. C with the Th{sub 2}Zn{sub 17} type (R3-bar m, a=0.90916(4) nm, c=1.3286(1) nm) and low temperature {alpha}CeZn{sub 7} (Ce{sub 1-x}Zn{sub 5+2x}; x{approx}0.33) up to 750 deg. C for which we attributed the TbCu{sub 7} type (P6/mmm, a=0.52424(2), c=0.44274(1) nm). The crystal structure of CeZn{sub 7} was derived from the Rietveld refinement of X-ray powder intensities. Precise data on atom site distribution and positional parameters have been furthermore provided from X-ray single crystal refinements for two compounds, for which crystal structures hitherto have only been derived from X-ray diffraction photographs: Ce{sub 3}Zn{sub 11} (Immm, a=0.45242(2) nm, b=0.88942(3) nm, c=1.34754(4) nm) and Ce{sub 3}Zn{sub 22} (I4{sub 1}/amd; a=0.89363(2) nm, c=2.1804(5) nm). - Graphical abstract: Existence of low temperature modification {alpha}CeZn{sub 7} (Ce{sub 1-x}Zn{sub 5+2x}; x{approx}0.33) of Ce{sub 2}Zn{sub 17} has been verified up to 750 deg. C that is attributed with the TbCu{sub 7} type. Highlights: > Isothermal section of system Ce-Zn-B at 800 deg. C. > In System Ce-Zn, X-ray single crystal intensity data refinement of Ce{sub 3}Zn{sub 11} and Ce{sub 3}Zn{sub 22} and Rietveld refinement of Ce{sub 13}Zn{sub 58}. > Two temperature modifications of Ce{sub 2}Zn{sub 17}, rhombohedral {beta}Ce{sub 2}Zn{sub 17} (hT) and of hexagonal {alpha}CeZn{sub 7} (lT). > No ternary compound in the System Ce-Zn-B (<50 at% Ce) at 800 deg. C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Electrochemical performance studies of MnO{sub 2} nanoflowers recovered from spent battery

Highlights: • MnO{sub 2} is recovered from spent zinc–carbon batteries as nanoflowers structure. • Recovered MnO{sub 2} nanoflowers show high specific capacitance. • Recovered MnO{sub 2} nanoflowers show stable electrochemical cycling up to 900 cycles. • Recovered MnO{sub 2} nanoflowers show low resistance in EIS data. - Abstract: The electrochemical performance of MnO{sub 2} nanoflowers recovered from spent household zinc–carbon battery is studied by cyclic voltammetry, galvanostatic charge/discharge cycling and electrochemical impedance spectroscopy. MnO{sub 2} nanoflowers are recovered from spent zinc–carbon battery by combination of solution leaching and electrowinning techniques. In an effort to utilize recovered MnO{sub 2} nanoflowers as energy storage supercapacitor, it is crucial to understand their structure and electrochemical performance. X-ray diffraction analysis confirms the recovery of MnO{sub 2} in birnessite phase, while electron microscopy analysis shows the MnO{sub 2} is recovered as 3D nanostructure with nanoflower morphology. The recovered MnO{sub 2} nanoflowers exhibit high specific capacitance (294 F g{sup −1} at 10 mV s{sup −1}; 208.5 F g{sup −1} at 0.1 A g{sup −1}) in 1 M Na{sub 2}SO{sub 4} electrolyte, with stable electrochemical cycling. Electrochemical data analysis reveal the great potential of MnO{sub 2} nanoflowers recovered from spent zinc–carbon battery in the development of high performance energy storage supercapacitor system.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Pre-Irradiation Comparison of W-Based Alloys for the PHENIX Campaign: Microstructure, Composition, and Mechanical Properties

Tungsten is the material of choice as the plasma-facing material in future plasma-burning fusion reactors. During operation, plasma-facing materials will be simultaneously exposed to 14-MeV neutrons, low-energy D/He particles, and high heat loads. Neutron irradiation of tungsten results in bulk material damage, including knock-on damage causing loops and voids, and transmutation reactions leading to the transmutation of tungsten to rhenium and osmium. Under irradiation to high dose, Re and Os atoms can amalgamate into precipitates that drastically alter the material properties, noticeably increasing the hardness. However, the early-stage development of Re and Os precipitates under a fast neutron spectrum has not been investigated.In this work, the microstructure and hardening behavior of W-Re alloys containing 0 to 2.2 wt% Re, TiC-doped W, and powder-injection-molded W are investigated prior to neutron irradiation at 500ºC and 800ºC to ~0.1 displacement per atom in the High Flux Isotope Reactor (HFIR) to establish a baseline understanding of the starting microstructures.Transmission electron microscopy analysis indicates a dislocation-heavy microstructure, and scanning transmission electron microscopy–energy dispersive spectroscopy shows no spatial segregation of Re and W. Similarly, surface compositional studies performed with electron backscatter diffraction and X-ray photoelectron spectroscopy showed no presence of Re, indicating the Re did not segregate or form new phases during fabrication. Here, the alloys in their as-fabricated state showed no Re segregation or second-phase development, with no significant differences between their microstructures and Vickers hardness values.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Metal–organic frameworks assembled from lanthanide and 2,5-pyridinedicaboxylate with cubane-like [Ln{sub 4}(OH){sub 4}] building units

Lanthanide–organic frameworks based on 2,5-pyridinedicaboxylate (25p) ligand, formulated as [Yb{sub 4}(OH){sub 4}(25p){sub 4}(H{sub 2}O){sub 3}]·H{sub 2}O (25pYb), [Y{sub 4}(OH){sub 4}(25p){sub 4}(H{sub 2}O){sub 3}]·H{sub 2}O (25pY-1) and [Y{sub 6}(OH){sub 8}(25p){sub 5}(H{sub 2}O){sub 2}] (25pY-2), have been obtained as single phases under hydrothermal conditions. 25pYb and 25pY-1 are isostructural, and crystallize in the triclinic space group, P-1, with a=8.6075(5) Å, b=14.8478(7) Å, c=15.9164(9) Å, α=86.277(4)°, β=80.196(5)°, γ=81.785(4)°, and a=8.7166(6) Å, b=14.966(1) Å, c=15.966(1) Å, α=86.260(6)°, β=80.036(6)°, γ=81.599(6)°, respectively. 25pY-2 crystallizes in the monoclinic space group, P2{sub 1}/c, with a=24.9117(17) Å, b=13.7340(8) Å, c=14.3385(10) Å, β=100.551(7)°. 25pYb and 25pY-2 have been structurally characterized by single-crystal X-ray diffraction. The 25pYb structure is based on tetranuclear cubane-like [Yb{sub 4}(OH){sub 4}]{sup 8+} clusters, which are interconnected to eight neighbouring clusters through teen surrounding 25p ligands leading to neutral 3D framework, while the structure of 25pY-2 is based on two independent cuban-like [Y{sub 4}(OH){sub 4}]{sup 8+} clusters, which are joined together through Y1 cation leading to the formation of hexanuclear [Y{sub 6}(OH){sub 8}]{sup 10+} clusters, which in turn are joined via Y2 cation resulting in infinite inorganic chain extending along c-axis, and each chain is interconnected to six adjacent chains through 25p ligands leading finally to 3D framework. The luminescence properties of Eu{sup 3+} and Tb{sup 3+} doped 25pY-1 and 25pY-2 compounds have also been investigated. All materials has been characterized by powder X-ray diffraction, thermal analyses (TG–SDTA–MS), FTIR spectroscopy, C–H–N elemental analysis, scanning electron microscopy (SEM-EDX), and powder X-ray thermodiffraction. - Graphical abstract: Nowadays, lanthanide–organic frameworks (LOFs) attract tremendous attention due to the unique characteristic of lanthanide cations, such as variable coordination numbers and geometries which often lead to novel complex structures, and also to their magnetic and photoluminescence properties. Herein, three LOFs formulated as [Ln{sub 4}(OH){sub 4}(25p){sub 4}(H{sub 2}O){sub 3}]·H{sub 2}O (Ln=Y, Yb) and [Y{sub 6}(OH){sub 8}(25p){sub 5}(H{sub 2}O){sub 2}] have been obtained by hydrothermal method and characterized, and the photoluminescence properties of the Eu and Tb doped compounds are discussed. - Highlights: • Three novel LnOFs has been synthesized and characterized. • Crystal structures are based on tetranuclear cuban-like [Ln{sub 4}(OH){sub 4}]{sup 8+} clusters. • 25pYb and 25pY-1 are based on isolated [Ln{sub 4}(OH){sub 4}]{sup 8+} clusters. • 25pY-2 is based on infinite inorganic chains built up from [Y{sub 4}(OH){sub 4}]{sup 8+} clusters. • Photoluminescence studies show strong red and green light emissions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Feld-induced modulation of two-dimensional electron gas at LaAlO 3 /SrTiO 3 interface by polar distortion of LaAlO 3

Since the discovery of two-dimensional electron gas at the LaAlO 3 /SrTiO 3 interface, its intriguing physical properties have garnered significant interests for device applications. Yet, understanding its response to electrical stimuli remains incomplete. Our in-situ transmission electron microscopy analysis of a LaAlO 3 /SrTiO 3 two-dimensional electron gas device under electrical bias reveals key insights. Inline electron holography visualized the field-induced modulation of two-dimensional electron gas at the interface, while electron energy loss spectroscopy showed negligible electromigration of oxygen vacancies. Instead, atom-resolved imaging indicated that electric fields trigger polar distortion in the LaAlO 3 layer, affecting two-dimensional electron gas modulation. This study refutes the previously hypothesized role of oxygen vacancies, underscoring the lattice flexibility of LaAlO 3 and its varied polar distortions under electric fields as central to two-dimensional electron gas dynamics. These findings open pathways for advanced oxide nanoelectronics, exploiting the interplay of polar and nonpolar distortions in LaAlO 3 .

36 MATERIALS SCIENCE↗
NASA NTRS1978

Luna 24 - Lateral heterogeneity in the lunar crust

Results of petrological investigations of Luna 24 soil samples are compared with data from Apollo and other Luna missions in order to determine the large scale composition of the lunar surface and crust. Modal analysis of the 90 to 150 micron soil fraction and electron microprobe analysis of glass spheres and fragments of the Luna 24 core sample are presented. High and low MgO mare basalt compositional clusters are found, suggesting the derivation of southern Mare Crisium basalts from two magmas. A model of Luna 24 soils as being composed of a mixture of glass-poor mare material and glass-rich highland material is found to be consistent with glass and agglutinate modal abundances. Comparisons show that potassium, and by inference all lithophile trace elements, are depleted on the eastern limb of the moon relative to the central nearside. The observed depletion is interpreted to be characteristic of the underlying crust and mantle as well as the surface.

Warner, J. L.↗
NASA NTRS1986

High-frequency waves generated by auroral electrons

Measurements of marginally unstable electron distribution functions and high-frequency plasma waves were made on a sounding rocket flight through a quiet auroral arc. The waves appeared near the electron plasma frequency and had a large parallel electric field component such that k-parallel is greater than k-perpendicular. The appearance of these waves was correlated with the presence of marginally unstable parallel electron distributions. Analysis has shown that the waves were produced by parallel electron distribution function greater than 0 rather than the small perpendicular electron distribution function greater than 0 features. Wave levels and growth rates inside the arc were small, and nonlinear wave-wave and wave-particle interactions appear to have been minimal.

Mcfadden, J. P.↗
DOE OSTI2015

The solubility and site preference of Fe{sup 3+} in Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnets

A series of Fe{sup 3+}-bearing Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnets was synthesized using solid-state synthesis methods. The synthetic products were characterized compositionally using electron microprobe analysis and inductively coupled plasma optical emission spectroscopy (ICP-OES) and structurally using X-ray powder diffraction and {sup 57}Fe Mössbauer spectroscopy. A maximum of about 0.25 Fe{sup 3+} pfu could be incorporated in Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnet solid solutions. At Fe{sup 3+} concentrations lower than about 0.16 pfu, both tetragonal and cubic garnets were obtained in the synthesis experiments. X-ray powder diffraction analysis showed only a garnet phase for syntheses with starting materials having intended Fe{sup 3+} contents lower than 0.52 Fe{sup 3+} pfu. Back-scattered electron images made with an electron microprobe also showed no phase other than garnet for these compositions. The lattice parameter, a{sub 0}, for all solid-solution garnets is similar with a value of a{sub 0}≈12.98 Å regardless of the amount of Fe{sup 3+}. {sup 57}Fe Mössbauer spectroscopic measurements indicate the presence of poorly- or nano-crystalline FeLaO{sub 3} in syntheses with Fe{sup 3+} contents greater than 0.16 Fe{sup 3+} pfu. The composition of different phase pure Li{sub 7−3x}Fe{sub x}La{sub 3}Zr{sub 2}O{sub 12} garnets, as determined by electron microprobe (Fe, La, Zr) and ICP-OES (Li) measurements, give Li{sub 6.89}Fe{sub 0.03}La{sub 3.05}Zr{sub 2.01}O{sub 12}, Li{sub 6.66}Fe{sub 0.06}La{sub 3.06}Zr{sub 2.01}O{sub 12}, Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12}, and Li{sub 6.19}Fe{sub 0.19}La{sub 3.02}Zr{sub 2.04}O{sub 12}. The {sup 57}Fe Mössbauer spectrum of cubic Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12} garnet indicates that most Fe{sup 3+} occurs at the special crystallographic 24d position, which is the standard tetrahedrally coordinated site in garnet. Fe{sup 3+} in smaller amounts occurs at a general 96h site, which is only present for certain Li-oxide garnets, and in Li{sub 6.54}Fe{sub 0.12}La{sub 3.01}Zr{sub 1.98}O{sub 12} this Fe{sup 3+} has a distorted 4-fold coordination. - Graphical abstract: Cubic nominally Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnet is a promising candidate to be used as a solid electrolyte in Li-ion batteries. A series of Fe{sup 3+}-bearing LLZO garnets was synthesized and characterized compositionally and structurally. {sup 57}Mössbauer measurements were made to determine where Fe is incorporated in the crystal structure. X-ray diffraction, electron microprobe, ICP-OES and {sup 57}Mössbauer measurements are needed to obtain a full description of the synthetic products, some of which contain small amounts of nano- or poorly crystalline FeLaO{sub 3}. - Highlights: • A series of Fe{sup 3+}-bearing Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} (LLZO) garnets was synthesized and characterized compositionally and structurally. • {sup 57}Mössbauer measurements were made to determine where Fe is incorporated in the crystal structure. • Most Fe{sup 3+} substitutes for Li{sup +} in LLZO at the 24d and 96h sites in the cubic phase (Ia-3d). • No more than about 0.25 Fe{sup 3+} pfu can be incorporated into the LLZO garnet structure. • X-ray powder diffractions measurements indicate the presence of both cubic and tetragonal garnets phases in some syntheses. • The probable presence of small amounts of poorly or nano-crystalline FeLaO3 can only be identified by Mössbauer spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

The structure and properties of single-layer and gradient-layered coatings of the Ti–Al–Si–Cr–Mo–S–N system

Using the method of microprobe analysis and transmission electron microscopy, the influence of obtaining conditions upon particular elemental composition and growth structure coatings of Ti–Al–Si–Mo–S–N system was studied. The possibility of formation and characteristics of the structural and elastic-stress state single-layer coatings with nanoscale columnar or equiaxed grains and gradient-layered, combining two types of selected structure, was defined. On the basis of hardness, tribological properties and coating hardness, a conclusion was made about the relative prospects of its use as wear-resistant coatings with a nanocrystalline structure.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Understanding Biases in Sample Preparation Techniques for Coupled Scanning Electron Microscopy and MAMA PuO 2 Morphological Analysis

In this project, the scanning electron microscopy (SEM) sampling method used during the statistical design study (SDS) was investigated to determine if any sampling biases were present in the analyzed data. Using standard particle size distribution powders from the National Institute of Standards and Technology (NIST 1984 standard reference material) with the origin wet dispersion method, it was determined that a bias to smaller particles was present. This was supported by theoretical calculations using Stokes’ law to determine the settling rate of spherical particles of roughly the same size and mass as those found in the SDS. Based on the theoretical calculations, it was determined that the settling rate for each of the 76 powder sets in the SDS could be unique based on specific particle shape and mass distributions, making a universal correction factor/formula not applicable. Therefore, priority shifted to developing an improved wet dispersion method that significantly reduced the particle settling rate for all particle size and shapes. This was achieved by replacing the original solvent (isopropyl alcohol) with a heavy liquid (lithium heteropolytungstates), which dramatically slowed the settling rate and allowed for the capture of a suitable homogeneous aliquot. SEM imaging and Morphological Analysis for Material Attribution (MAMA) software analysis were conducted on the NIST standard, and the SEM/MAMA data were compared to data captured by a dynamic image analysis particle size analyzer. The resulting data confirmed that the new wet dispersion method does indeed deliver an improved representative aliquot to the SEM stub. For instance, in the NIST certificate, the average particle size is ~17.1 µm ± 2.2 µm with a normal distribution. The initial wet dispersion method resulted in a drastically reduced average particle size of 6.1 µm in addition to a non-representative heavy bi-modal distribution whereas the improved LST wet dispersion method resulting in an average particle size that was much closer to the NIST certificate (12.7 µm) with a similar normal distribution. Although the improved method was still short of the NIST certificate average, atomic force microscopy analysis determined that the resulting ~20-25% reduction in size was due to particles sinking into the carbon sticky tape used for SEM imaging. It is believed that that this bias can be calibrated in a much more predicable manner than the original settling rate bias. In addition, the matching normal distribution curves between the NIST certificate and the heavy liquid method indicate a much-improved representative aliquot has been sampled and imaged. A surrogate CeO 2 powder was used to reflect PuO 2 more accurately and to aid in implementing radiological controls and shielding. The resulting data sets from the SEM/MAMA method and the particle size analyzer give almost identical average particle sizes and particle distribution statistics. Future work will re-analyze several select runs from the SDS to determine if morphological signatures can be found with the improved sampling method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1984

Tribological applications of surface analysis

For some years, surface analysis was used in fundamental studies of solid-solid contacts existing in tribological systems. Analysis was used to detect material transfer in sliding contacts. The effects of surface films on the adhesion of contacts was monitored. Finally electron spectroscopic analysis of interfaces has shed some light on the fundamental electronic nature of the interfacial bond. More recently, surface analysis was applied to many tribological engineering problems. In particular, identification of chemical films formed during the sliding contact of lubricated systems and study of the surface chemistry of lubricant additives were active areas of research. One or more of four properties of the analytical technique will be important in determining its utility. The four are: lateral resolution, specimen damage, depth resolution and the availability of chemical information. In each of the applications discussed here, the important factors are brought out.

Wheeler, D. R.↗