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NASA NTRS2002

Nanocrystalline CuInS2 And CuInSe2 via Low-Temperature Pyrolysis Of Single-Source Molecular Precursors

Single-source precursors are molecules which contain all the necessary elements for synthesis of a desired material. Thermal decomposition of the precursor results in the formation of the material with the correct stoichiometry, as a nanocrystalline powder or a thin film. Nanocrystalline materials hold potential as components of next-generation Photovoltaic (PV) devices. Presented here are the syntheses of CuInS2 and CuInSe2 nanocrystals from the precursors (PPh3)2CuIn(SEt)4 and (PPh3)2CuIn(SePh)4, respectively. The size of the nanocrystals varies with the reaction temperature; a minimum of 200 C is required for the formation of the smallest CuInS2 crystals (approximately 1.6 nm diameter); at 300 C, crystals are approximately 7 nm.

Castro, Stephanie L.↗
NASA NTRS2003

Application of Powder Diffraction Methods to the Analysis of Short- and Long-Range Atomic Order in Nanocrystalline Diamond and SiC: The Concept of the Apparent Lattice Parameter (alp)

Two methods of the analysis of powder diffraction patterns of diamond and SiC nanocrystals are presented: (a) examination of changes of the lattice parameters with diffraction vector Q ('apparent lattice parameter', alp) which refers to Bragg scattering, and (b), examination of changes of inter-atomic distances based on the analysis of the atomic Pair Distribution Function, PDF. Application of these methods was studied based on the theoretical diffraction patterns computed for models of nanocrystals having (i) a perfect crystal lattice, and (ii), a core-shell structure, i.e. constituting a two-phase system. The models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the shell. X-ray and neutron experimental diffraction data of nanocrystalline SiC and diamond powders of the grain diameter from 4 nm up to micrometers were used. The effects of the internal pressure and strain at the grain surface on the structure are discussed based on the experimentally determined dependence of the alp values on the Q-vector, and changes of the interatomic distances with the grain size determined experimentally by the atomic Pair Distribution Function (PDF) analysis. The experimental results lend a strong support to the concept of a two-phase, core and the surface shell structure of nanocrystalline diamond and SiC.

Palosz, B.↗
NASA NTRS2003

High Pressure X-Ray Diffraction Studies on Nanocrystalline Materials

Application of in situ high pressure powder diffraction technique for examination of specific structural properties of nanocrystals based on the experimental data of SiC nanocrystalline powders of 2 to 30 nrn diameter in diameter is presented. Limitations and capabilities of the experimental techniques themselves and methods of diffraction data elaboration applied to nanocrystals with very small dimensions (< 30 nm) are discussed. It is shown that due to the complex structure, constituting a two-phase, core/surface shell system, no unique lattice parameter value and, consequently, no unique compressibility coefficient can satisfactorily describe the behavior of nanocrystalline powders under pressure. We offer a tentative interpretation of the distribution of macro- and micro-strains in nanoparticles of different grain size.

Palosz, B.↗
NASA NTRS2010

New Insights into the Origin of Magnetite Crystals in ALH84001 Carbonate Disks

Martian meteorite ALH84001 preserves evidence of interaction with aqueous fluids while on Mars in the form of microscopic carbonate disks believed to have formed approx.3.9 Ga ago at beginning of the Noachian epoch. Intimately associated within and throughout these carbonate disks are nanocrystal magnetites (Fe3O4) with unusual chemical and physical properties, whose ori gins have become the source of considerable debate. One group of hypotheses argues that these magnetites are the product of partial thermal decomposition of the host carbonate. Alternatively, the origins of magnetite and carbonate may be unrelated: that is, from the perspective of the carbonate the magnetite is allochthonous. We have sought to resolve between these hypotheses through the detailed characterized of the compositional and structural relationships between the carbonate disks, their associated magnetites and the orthopyroxene matrix in which they are embedded [1]. Comparison of these results with experimental thermal decomposition studies of sideritic carbonates conducted under a range of heating scenarios suggests that the magnetite nanocrystals in the ALH84001 carbonate disks are not the products of thermal decomposition.

Thomas-Keptra, Katie L.↗
NASA NTRS2012

The Origin of Magnetite Crystals in ALH84001 Carbonate Disks

Martian meteorite ALH84001 preserves evidence of interaction with aqueous fluids while on Mars in the form of microscopic carbonate disks believed to have formed approx 3.9 Ga ago at beginning of the Noachian epoch. Intimately associated within and throughout these carbonate disks are nanocrystal magnetites (Fe3O4) with unusual chemical and physical properties, whose origins have become the source of considerable debate. One group of hypotheses argues that these magnetites are the product of partial thermal decomposition of the host carbonate. Alternatively, the origins of magnetite and carbonate may be unrelated; that is, from the perspective of the carbonate the magnetite is allochthonous. We have sought to resolve between these hypotheses through the detailed characterized of the compositional and structural relationships between the carbonate disks, their associated magnetites and the orthopyroxene matrix in which they are embedded. Comparison of these results with experimental thermal decomposition studies of sideritic carbonates conducted under a range of heating scenarios suggests that the magnetite nanocrystals in the ALH84001 carbonate disks are not the products of thermal decomposition.

Thomas-Keprta, K. L.↗
NASA NTRS1993

Size distributions in two porous chondritic micrometeorites

Quantitative size measurements of granular units (GUs), and nm-sized minerals in these units, in two porous chondritic micrometeorites are investigated. The matrix of these micrometeorites consist of loosely packed, 0.1 micron-sized, GUs. These objects were a major component of the solar nebula dust that accreted into protoplanets. The matrix in micrometeorite W7010*A2 has a fractal dimension with a small coefficient that supports efficient sticking of carbon-rich GUs during accretion. The fractal nature of the matrix provides a way to calculate the density using the aggregate size. The resulting very low density for porous chondritic micrometeorites is 0.08-0.14 g/cu cm, which supports the view that they are the solid debris from unconsolidated solar system bodies. Chondritic GUs contain ultrafine olivines, pyroxenes, and sulfides, embedded in hydrocarbons and amorphous carbons. Nanocrystals in the micrometeorites W7010*A2 and U2015*B show log normal size distributions. The high incidence of disk-shaped grains, a changeover from disk-shaped to euhedral grains, the unevolved nature of the size distributions, and multiple populations for grains less than 127 nm in size, are consistent with continuous postaccretion nucleation and growth in amorphous GUs, including coarsening via Ostwald ripening.

Rietmeijer, Frans J. M.↗
NASA NTRS1993

Micrometeorite dynamic pyrometamorphism: Observation of a thermal gradient in iron-nickel sulfide

Dynamic pyrometamorphism describes the mineralogical changes in a micrometeorite that occur in response to flash-heating during atmospheric entry. Mineral reactions during this event will be endothermic and act as local sinks for thermal energy which delays a uniform temperature distribution in decelerating micrometeorites. The most common pyrometamorphic reaction is formation of magnetite nanocrystal decorations on Mg,Fe-silicate grains and magnetite or (partial) maghemite rims. Constituent silicates also respond to this thermal event and show formation of olivine-maghemite symplectites and growth of garnet and partial laihunitisation. In continued effort to constrain dynamic pyrometamorphism of unmelted interplanetary dust particles (IDP's), I determined the mineralogical composition, and Fe,Ni-sulfide chemistry, in the sulfide-rich particles L2005C39, L2005E40, and L2006A28 using a JEOL 2000FX analytical electron microscope equipped with a TN5500 energy dispersive spectrometer for in situ microanalysis. Sulfide compositions in these three IDP's are distinctly different from those in silicate-rich particle L2005T13 which might suggest a delicate balance of the fO2/fS2 ratios during dynamic pyrometamorphism.

Rietmeijer, Frans J. M.↗
NASA NTRS1998

Microstructural, Chemical and Mechanical Characterization of Polymer-Derived Hi-Nicalon Fibers with Surface Coatings

Room temperature tensile strengths of as-received Hi-Nicalon fibers and those having BN/SiC, p-BN/SiC, and p-B(Si)N/SiC surface coatings, deposited by chemical vapor deposition, were measured using an average fiber diameter of 13.5 microns. The Weibull statistical parameters were determined for each fiber. The average tensile strength of uncoated Hi-Nicalon on was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. Strength of fibers coated with BN/SiC did not change. However, coat with p-BN/SiC and p-B(Si)N/SiC surface layers showed strength loss of approx. 10 and 35 percent, respectively, compared with as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive x-ray spectroscopy. The BN coating was contaminated with a large concentration of carbon and some oxygen. In contrast, p-BN, p-B(Si)N, and SiC coatings did not show any contamination. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction. Hi-Nicalon fiber consists of the P-SIC nanocrystals ranging in size from 1 to 30 nm embedded in an amorphous matrix. TEM analysis of the BN coating revealed four distinct layers with turbostatic structure. The p-BN layer was turbostratic and showed considerable preferred orientation. The p-B(Si)N was glassy and the silicon and boron were uniformly distributed. The silicon carbide coating was polycrystalline with a columnar structure along the growth direction. The p-B(Si)N/SiC coatings were more uniform, less defective and of better quality than the BN/SiC or the p-BN/SiC coatings.

Bansal, Narottam P.↗
NASA NTRS1996

The Ultrafine Mineralogy of a Molten Interplanetary Dust Particle as an Example of the Quench Regime of Atmospheric Entry Heating

Melting and degassing of interplanetary dust particle L2005B22 at approx. 1200 C was due to flash heating during atmospheric entry. Preservation of the porous particle texture supports rapid quenching from the peak heating temperature whereby olivine and pyroxene nanocrystals (3 nm-26 nm) show partial devitrification of the quenched melt at T approx. = 450 C - 740 C. The implied ultrahigh cooling rates are calculated at approx. 105 C/h-106 C/h, which is consistent with quench rates inferred from the temperature-time profiles based on atmospheric entry heating models. A vesicular rim on a nonstoichiometric relic forsterite grain in this particle represents either evaporative magnesium loss during flash heating or thermally annealed ion implantation texture.

Rietmeijer, Frans J. M.↗
NASA NTRS1996

CM-like Interplanetary Dust Particles in Lower Stratosphere During 1989 October and 1991 June/July

The stratospheric interplanetary dust particles L2005T12 and L2011O3 are linked to CM chondrite matrix. Particle L2005T12 is dominated by tabular grains of partially dehydrated greenalite-rich serpentine. Its amorphous matrix contains abundant smectite nanocrystals and annular Fe,Ni,S units. A uniquely stratified (partial) maghemite rim occurs only on S-rich parts of the matrix. Formation of this rim and Mg depletions in the matrix occurred during atmospheric entry heating of this particle. Particle L2011O3 has large iron sulfide and magnesiowustite grains in an amorphous low-Al, ferromagnesiosilica matrix. Hydrous crystallisation of this matrix produced ultrafine-grained smectites and disseminated iron sulfides. Atmospheric entry heating of both particles is indicated by the partial iron oxide rim, vesicular sulfides, and the scatter of matrix compositions due to loss of Mg. While many uncertainties remain, the high incidence of chondritic rough particles, which include an unknown amount of CM-like particles, in the lower stratosphere during 1984, 1989, and 1991 suggests annual variations in their abundances. The timing of lower stratospheric dust samplings is critical to collect these particles.

Rietmeijer, Frans J. M.↗
NASA NTRS1998

Study of the effects of MeV Ag, Cu, Au, and Sn implantation on the optical properties of LiNbO3

The authors present the results of characterization of linear absorption and nonlinear refractive index of Au, Ag, Cu and Sn ion implantation into LiNbO3. Ag was implanted at 1.5 MeV to fluences of 2 to 17 x 17(exp 16)/sq cm at room temperature. Au and Cu were implanted to fluences of 5 to 20 x 10(exp 16)/sq cm at an energy of 2.0 MeV. Sn was implanted to a fluence of 1.6 x 10(exp 17)/sq cm at 160 kV. Optical absorption spectrometry indicated an absorption peak for the Au implanted samples after heat treatment at 1,000 C at approx. 620 nm. The Ag implanted samples absorption peaks shifted from approx. 450 nm before heat treatment to 550 nm after 500 C for 1h. Heat treatment at 800 C returned the Ag implanted crystals to a clear state. Cu nanocluster absorption peaks disappears at 500 C. No Sn clusters were observed by optical absorption or XRD. The size of the Ag and Au clusters as a function of heat treatment were determined from the absorption peaks. The Ag clusters did not change appreciably in size with heat treatment. The Au clusters increased from 3 to 9 nm diameter upon heat treatment at 1000 C. TEM analysis performed on a Au implanted crystal indicated the formation of Au nanocrystals with facets normal to the c-axis. Measurements of the nonlinear refractive indices were carried out using the Z-scan method with a tunable dye laser pumped by a frequency doubled mode-locked Nd:YAG laser. The dye laser had a 4.5 ps pulse duration time and 76 MHz pulse repetition rate (575 nm).

Williams, E. K.↗
NASA NTRS2000

Mechanical, Chemical and Microstructural Characterization of Monazite-Coated Silicon Carbide Fibers

Tensile strengths of as-received Hi-Nicalon and Sylramic fibers and those having monazite surface coatings, deposited by atmospheric pressure chemical vapor deposition, were measured at room temperature and the Weibull statistical parameters determined. The average tensile strengths of uncoated Hi-Nicalon and Sylramic fibers were 3.19 +/- 0.73 and 2.78 +/- 0.53 GPa with a Weibull modulus of 5.41 and 5.52, respectively. The monazite-coated Hi-Nicalon and Sylramic fibers showed strength loss of approx. 10 and 15 percent, respectively, compared with the as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive X-ray spectroscopy. The LaPO4 coating on Hi-Nicalon fibers was approximately stoichiometric and about 50 nm thick. The coating on the Sylramic fibers extended to a depth of about 100 to 150 nm. The coating may have been stoichiometric LaPO4 in the first 30 to 40 nm of the layer. However, the surface roughness of Sylramic fiber made this profile somewhat difficult to interpret. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Hi-Nicalon fiber consists of fine beta-SiC nanocrystals ranging in size from 1 to 30 mn embedded in an amorphous matrix. Sylramic is a polycrystalline stoichiometric silicon carbide fiber consisting of submicron beta-SiC crystallites ranging from 100 to 300 nm. Small amount of TiB2 nanocrystallites (approx. 50 nm) are also present. The LaPO4 coating on Hi-Nicalon fibers consisted of a chain of peanut shape particles having monazite-(La) structure. The coating on Sylramic fibers consisted of two layers. The inner layer was a chain of peanut shape particles having monazite-(La) structure. The outer layer was comprised of much smaller particles with a microcrystalline structure.

Bansal, N. P.↗
NASA NTRS2002

Superhard Nanocrystalline Homometallic Stainless Steel on Steel for Seamless Coatings

The objective of this work is to deposit nanocrystalline stainless steel onto steel substrates (homometallic) for enhanced wear and corrosion resistance. Homometallic coatings provide superior adhesion, and it has been shown that ultrafine-grained materials exhibit the increased hardness and decreased permeability desired for protective coatings. Nanocrystals will be produced by controlling nucleation and growth and use of an ion beam during deposition by e-beam evaporation or sputtering. Phase I is depositing 31 6L nanocrystalline stainless steel onto 31 6L stainless steel substrates. These coatings exhibit hardnesses comparable to those normally obtained for ceramic coatings such ZrO2, and possess the superior adhesion of seamless, homometallic coatings. Hardening the surface with a similar material also enhances adhesion, by avoiding problems associated with thermal and lattice mismatch. So far we have deposited nanocrystalline homometallic 316L stainless steel coatings by varying the ions and the current density of the ion beams. For all deposition conditions we have produced smooth, uniform, superhard coatings. All coatings exhibit hardness of at least 200% harder than that of bulk materials. Our measurements indicate that there is a direct relationship between nanohardness and the current density of the ion beam. Stress measurements indicate that stress in the films is increasingly proportional to current density of the ion beam. TEM, XPS, and XRD results indicate that the coated layers consist of FCC structure nanocrystallites with a dimension of about 10 to 20 nm. The Ni and Mo concentration of these coating are lower than those of bulk 316L but the concentration of Cr is higher.

Tobin, Eric J.↗
NASA NTRS2004

Determination of the Three-Dimensional Morphology of ALH84001 and Biogenic MV-1 Magnetite: Comparison of Results from Electron Tomography and Classical Transmission Electron Microscopy

Dated at approximately 3.9 billion years of age, carbonate disks, found within fractures of the host rock of Martian meteorite ALH84001, have been interpreted as secondary minerals that formed at low temperature in an aqueous medium. Heterogeneously distributed within these disks are magnetite nanocrystals that are of Martian origin. Approximately one quarter of these magnetites have morphological and chemical similarities to magnetite particles produced by magnetotactic bacteria strain MV-1, which are ubiquitous in aquatic habitats on Earth. Moreover, these types of magnetite particles are not known or expected to be produced by abiotic means either through geological processes or synthetically in the laboratory. The remaining three quarters of the ALH84001 magnetites are likely products of multiple processes including, but not limited to, precipitation from a hydrothermal fluid, thermal decomposition of the carbonate matrix in which they are embedded, and extracellular formation by dissimilatory Fe-reducing bacteria. We have proposed that the origins of magnetites in ALH84001 can be best explained as the products of multiple processes, one of which is biological. Recently the three-dimensional (3-D) external morphology of the purported biogenic fraction of the ALH84001 magnetites has been the subject of considerable debate. We report here the 3-D geometry of biogenic magnetite crystals extracted from MV-1 and of those extracted from ALH84001 carbonate disks using a combination of high resolution classical and tomographic transmission electron microscopy (TEM). We focus on answering the following questions: (1) which technique provides adequate information to deduce the 3-D external crystal morphology?; and, (2) what is the precise 3-D geometry of the ALH84001 and MV-1 magnetites?

Thomas-Keprta, Kathie L.↗
NASA NTRS2003

Quantum dots as strain- and metabolism-specific microbiological labels

Biologically conjugated quantum dots (QDs) have shown great promise as multiwavelength fluorescent labels for on-chip bioassays and eukaryotic cells. However, use of these photoluminescent nanocrystals in bacteria has not previously been reported, and their large size (3 to 10 nm) makes it unclear whether they inhibit bacterial recognition of attached molecules and whether they are able to pass through bacterial cell walls. Here we describe the use of conjugated CdSe QDs for strain- and metabolism-specific microbial labeling in a wide variety of bacteria and fungi, and our analysis was geared toward using receptors for a conjugated biomolecule that are present and active on the organism's surface. While cell surface molecules, such as glycoproteins, make excellent targets for conjugated QDs, internal labeling is inconsistent and leads to large spectral shifts compared with the original fluorescence, suggesting that there is breakup or dissolution of the QDs. Transmission electron microscopy of whole mounts and thin sections confirmed that bacteria are able to extract Cd and Se from QDs in a fashion dependent upon the QD surface conjugate.

NASA Center JPL↗
NASA NTRS2004

Diffraction Studies of the Atomic Vibrations of Bulk and Surface Atoms in the Reciprocal and Real Spaces of Nanocrystalline SiC

To describe and evaluate the vibrational properties of nanoparticles it is necessary to distinguish between the surface and the core of the particles. Theoretical calculations show that vibrational density of states of the inner atoms of nanograins is similar to bulk material but shifted to higher energies which can be explained by the fact that the gain core is stressed (hardened) due to the presence of internal pressure. Theoretical calculations also show that there is a difference between vibrational properties of a crystal lattice of the grain interior in isolated particles and in a dense (sintered) nanocrystalline material. This is probably due to a coupling of the modes inside the grains via the grain boundaries in dense nanocrystalline bodies. We examined strains present in the surface shell based on examination of diamond and Sic nanocrystals in reciprocal (Bragg-type scattering) and real (PDF analysis) space analysis of neutron diffraction data. Recently we examined the atomic thermal motions in nanocrystalline Sic based on the assumption of a simple Einstein model for uncorrelated atomic notions. According to this model, the Bragg intensity is attenuated as a function of scattering angle by the Debye-Waller factor. Based on this assumption overall temperature factors were determined from the Wilson plots.

Stelmakh, S.↗
NASA NTRS2005

Thermal Characterization of Fe3O4 Nanoparticles Formed from Poorly Crystalline Siderite

Increasing interest in environmental geochemistry has led to the recognition that crystals with sizes in the nanometer range (e.g., colloids and nanoscale precipitates) and poorly crystalline compounds (e.g., ferrihydrites) may comprise the majority of reactive mineral surface area near the Earth s surface. When the diameters of individual particles are in the range of 100 nm or less, the surface energy contribution to the free energy modifies phase stability. This results in stabilization of polymorphs not normally encountered in the macrocrystal domain. These phases potentially have very different surface-site geometries, adsorptive properties, and growth mechanisms, and exhibit size-dependent kinetic behavior. Thus nanophases dramatically modify the physical and chemical properties of soils and sediments. In a more general sense, the characteristics of nanocrystals are of intense technological interest because small particle size confers novel chemical, optical, and electronic properties. Thus, nanocrystalline materials are finding applications as catalytic substrates, gas phase separation materials, and even more importantly in the field of medicine. This is an opportune time for mineral physicists working on nanocrystalline materials to develop collaborative efforts with materials scientists, chemists, and others working on nanophase materials of technological interest (e.g., for magnetic memories). Our objective in this study was to synthesize submicron (<200 nm) magnetite and to study their thermal and particle size properties.

Lauer, H. V., Jr.↗