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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 577 records · Page 32
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Metal–insulator transition tuned by magnetic field in Bi 1.7 V 8 O 16 hollandite

A metal–insulator transition tuned by application of an external magnetic field occurs in the quasi-one dimensional system Bi1.7V8O16, which contains a mix of S = 1 and S = 1/2 vanadium cations. Unlike all other known vanadates, the magnetic susceptibility of Bi1.7V8O16 diverges in its insulating state, although no long-range magnetic ordering is observed from neutron diffraction measurements, possibly due to the frustrated geometry of the triangular ladders. Magnetotransport measurements reveal that the transition temperature is suppressed upon application of an external magnetic field, from 62.5 K at zero field to 40 K at 8 T. This behavior is both hysteretic and anisotropic, suggesting t2g orbital ordering of the V3+ and V4+ cations drives a first-order structural transition. Single crystal X-ray diffraction reveals a charge density wave of Bi3+ cations with a propagation vector of 0.846c*, which runs parallel to the triangular chain direction. Neutron powder diffraction measurements show a first-order structural transition, characterized by the coexistence of two tetragonal phases near the metal–insulator transition. Finally, we discuss the likelihood that ferromagnetic V–V dimers coexist with a majority spin-singlet state below the transition in Bi1.7V8O16.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Long-range three-dimensional magnetic structures of the spin S =1 hexamer cluster fedotovite-like A 2 Cu 3 O ( SO 4 ) 3 ( A 2 = K 2 , NaK, Na 2 ): A neutron diffraction study

The crystal and magnetic structures of the spin S = 1 hexamer cluster fedotovite-like A 2 Cu 3 O(SO 4 ) 3 (A 2 = K 2 , NaK, Na 2 ) were studied by neutron powder diffraction at temperatures 1.6–290 K. The crystal structures in all compounds are well refined in the monoclinic space group C2/c. The basic magnetic units of the compounds are copper hexamers, which are coupled by weak superexchange interactions giving rise to three-dimensional long-range magnetic order below 3.0 < T N < 4.7 K. We have found that for A 2 = K 2 and NaK the propagation vector of the magnetic structure is k = [0,0,0], and the coupling of the Cu hexamers is ferromagnetic (FM) along the ab diagonal and antiferromagnetic along the bc diagonal. In contrast, for A = Na the propagation vector is k = [0,1,0], and the Cu hexamers are coupled antiferromagnetically (AFM) along the ab diagonal. Further, the hexamers are formed by three Cu pairs arranged along the b axis. The calculated spin expectation values $\langle s \rangle$ for the simplest symmetric spin Hamiltonian (obtained from inelastic neutron spectroscopy) of the isolated hexamers in the mean field amounted to $\langle s \rangle$ = 3/8 for the side spins Cu1 and Cu2 and $\langle s \rangle$ = 1/4 for Cu3 in the middle. The Cu spins are FM coupled in pairs and AFM between neighboring pairs. The experimental magnetic moments of the Cu 2+ ions turn out to be not completely collinear due to spin frustrations within the weak interhexamer interactions. The sizes of magnetic moments of Cu in the hexamers determined from the diffraction data are in fair agreement with the calculated values.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

XRD and FTIR structural investigation of gadolinium-zinc-borate glass ceramics

X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy measurements have been employed to investigate the (Gd{sub 2}O{sub 3}){sub x}⋅(B{sub 2}O{sub 3}){sub (60−x)}⋅(ZnO){sub 40} glass ceramics system, with 0 ≤ x ≤ 15 mol%. After heat treatment applied at 860 °C for 2 h, some structural changes were observed and new crystalline phases appeared in the structure of the samples. In these glass ceramics four crystalline phases were identified using powder diffraction files (PDF 2), namely ZnB{sub 4}O{sub 7}, Zn{sub 4}O(B{sub 6}O{sub 12}), Zn{sub 3}(BO{sub 3}){sub 2} and GdBO{sub 3}. From the XRD data, the average unit-cell parameter and the quantitative ratio of the crystallographic phases in the studied samples were evaluated. FTIR data revealed that the BO{sub 3}, BO{sub 4} and ZnO{sub 4} are the main structural units of these glass ceramics network. The compositional dependence of the different structural units which appear in the studied samples was followed.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Lifting the geometric frustration through a monoclinic distortion in “114” YBaFe{sub 4}O{sub 7.0}: Magnetism and transport

The possibility to lift the geometric frustration in the “114” stoichiomeric tetragonal oxide YBaFe{sub 4}O{sub 7.0} by decreasing the temperature has been investigated using neutron and synchrotron powder diffraction techniques. Besides the structural transition from tetragonal to monoclinic symmetry that appears at T{sub S}=180 K, a magnetic transition is observed below T{sub N}=95 K. The latter corresponds to a lifting of the 3D geometric frustration toward an antiferromagnetic long range ordering, never observed to date in a cubic based “114’” oxide. The magnetic structure, characterized by the propagation vector k{sub 1}=(0,0,½), shows that one iron Fe2 exhibits a larger magnetic moment than the three others, suggesting a possible charge ordering according to the formula YBaFe{sup 3+}Fe{sub 3}{sup 2+}O{sub 7.0}. The magnetic M(T) and χ′(T) curves, in agreement with neutron data, confirm the structural and magnetic transitions and evidence the coexistence of residual magnetic frustration. Moreover, the transport measurements show a resistive transition from a thermally activated conduction mechanism to a variable range hopping mechanism at T{sub S}=180 K, with a significant increase of the dependence of the resistivity vs. temperature. Mössbauer spectroscopy clearly evidences a change in the electronic configuration of the iron framework at the structural transition as well as coexistence of several oxidation states. The role of barium underbonding in these transitions is discussed. - Graphical abstract: Atomic displacements at the tetragonal-monoclinic transition in YBaFe{sub 4}O{sub 7}. Display Omitted - Highlights: • The structural and magnetic phase transitions of YBaFe{sub 4}O{sub 7} were studied below room temperature. • The tetragonal to monoclinic transition, characterized by NPD and SXRD, was studied using mode crystallography approach. • Monoclinic distortion allows the lifting of the geometrical frustration on the iron sublattice, leading to AF order at T=95 K.

36 MATERIALS SCIENCE↗
DOE OSTI2011

X-ray diffraction from intact tau aggregates in human brain tissue

We describe an instrument to record X-ray diffraction patterns from diseased regions of human brain tissue by combining an in-line visible light fluorescence microscope with an X-ray diffraction microprobe. We use thiazine red fluorescence to specifically label and detect the filamentous tau protein pathology associated with Pick's disease, as several laboratories have done previously. We demonstrate that thiazine red-enhanced regions within the tissue show periodic structure in X-ray diffraction, which is not observed in healthy tissue. One observed periodicity (4.2 {angstrom}) is characteristic of cross-beta sheet structure, consistent with previous results from powder diffraction studies performed on purified, dried tau protein.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2015

Effect of pressure on the structural properties of Li[Li{sub 0.1}Ni{sub 0.35}Mn{sub 0.55}]O{sub 2}

Li-rich cathode material Li[Li{sub 0.1}Ni{sub 0.35}Mn{sub 0.55}]O{sub 2} was synthesized by a sol-gel method. The morphology and a-NaFeO{sub 2} type structure of the material at ambient conditions were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The high-pressure behavior of the material was studied at pressure up to 19.7 GPa by using angle dispersive synchrotron X-ray powder diffraction (ADXD). The studies affirmed that the a-NaFeO{sub 2} type structure existed up to at least 19.7 GPa. Rietveld refinement analysis indicated that the c/a lattice parameter ratio decreased and the Li-O bond length shrunk with the increasing pressure, however, the Li{sup +}/Ni{sup 2+} ions exchange increased under elevated pressure. The pressure-volume data of the material were fitted to the third-order Birch-Murnaghan equation of state and bulk modulus obtained upon compression from the fitting was 117 (1) GPa.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Determination of a Two-Phase Structure of Nanocrystals: GaN and SiC

The properties of nano-crystalline materials are critically dependent on the structure of the constituent grains. Experimental conditions necessary to perform structural analysis of nanocrystalline materials as a two-phase core-surface shell system are discussed. It is shown, that a standard X-ray diffraction measurements and analysis are insufficient and may lead to incorrect conclusions as to the real structure of the materials. A new method of evaluation of powder diffraction data based on the analysis of the shift of the Bragg reflections from their perfect-lattice positions was developed. "Apparent lattice parameters" quantity, alp, was introduced and calculated from the actual positions of each individual Bragg reflection. The alp values plotted versus diffraction vector (Q) show characteristic features that are used for evaluation of the experimental results. The study was based on modeling of nano-grains and simulations of theoretical intensity profiles using the Debye functions. The method was applied to the analysis of synchrotron X-ray diffraction data of GaN and SiC nanocrystals. A presence of strained surface shell and a considerable internal pressure (GaN) in the nanoparticles was concluded.

Palosz, W.↗
DOE OSTI2010

Nanoparticles of La{sub 0.8}Ca{sub 0.2}Fe{sub 0.8}Ni{sub 0.2}O{sub 3-{delta}} perovskite for solid oxide fuel cell application

Polycrystalline samples of La{sub 0.8}Ca{sub 0.2}Fe{sub 0.8}Ni{sub 0.2}O{sub 3-{delta}} (LCFN) with perovskite type structure have been prepared by combustion, freeze drying, citrate-gel process and liquid mix method. The analysis of X-ray powder diffraction indicated that the samples were single phase and crystallized in an orthorhombic (space group, Pnma no. 62) structure. Transmission electron microscopy (TEM) analysis on the synthesized powder at 600 {sup o}C by liquid mix method showed clusters of 150 nm formed by nanoparticles of 20 nm. Electrochemical performance of LCFN cathodes, which are used for intermediate temperature solid oxide fuel cells, were investigated. The polarization resistance was studied using two different electrolytes: Y-doped zirconia (YSZ) and Sm-doped ceria (SDC). The dc four-probe measurement exhibits a total electrical conductivity, over 100 S cm{sup -1} at T {>=} 600 {sup o}C, pointing out that strontium can be substituted for the cheaper calcium cation without destroying the electrochemical properties. Experimental results indicate that nanoparticles have more advantages in terms of smaller particle size and better electrochemical performance.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Phase stability study of Bi{sub 0.15}Sr{sub 0.85-x}Ae{sub x}CoO{sub 3-{delta}} (x = 0 and Ae = Ba{sub 0.28}; Ca{sub 0.17}) perovskites by in-situ neutron diffraction

The oxygen deficient perovskites, Bi{sub 0.15}Sr{sub 0.85-x}Ae{sub x}CoO{sub 3-{delta}}, x = 0 and Ae{sub x} = Ba{sub 0.28}, Ca{sub 0.17}, were studied with in-situ neutron powder diffraction and combined TGA/DSC in order to investigate their behaviour at elevated temperatures in oxidising conditions. The phase stability of the I4/mmm supercell structure adopted by Bi{sub 0.15}Sr{sub 0.85}CoO{sub 3-{delta}} is shown to be dependent on temperature and the oxygen content of the phase, with three structural events, at T {approx} 250, 590 and 880 {sup o}C, detected. The first transition occurs as the perovskite supercell vanishes due to oxygen absorption; the second transition is also associated with oxidation and involves the decomposition of the perovskite phase via an exothermic process to yield a dominant hexagonal phase. Finally, at T {approx} 900 {sup o}C the perovskite phase re-forms. For the Ba and Ca containing materials the decomposition to the hexagonal phase occurs at T {approx} 600 {sup o}C and {approx} 650 {sup o}C respectively. The presence of Ca at the A-site is found to stabilise the I4/mmm supercell structure in the range RT - 650 {sup o}C. The antiferromagnetic to paramagnetic transitions occur at T{sub N} {approx} 250 {sup o}C, T{sub N} {approx} 175 {sup o}C and T{sub N} {approx} 145 {sup o}C for the samples with Ae{sub x} = Ba{sub 0.28}, x = 0 and Ae{sub x} = Ca{sub 0.17}, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Spectroscopic and X-ray Diffraction Study of Structural Disorder in Cryomilled and Amorphous Griseofulvin

Structural disorder induced by cryogenic milling and by heating to the amorphous phase in the active pharmaceutical ingredient Griseofulvin has been studied using Raman spectroscopy, X-ray powder diffraction (XRPD), and fluorescence spectroscopy. A broad, exciting-frequency-independent scattering background in the Raman spectra and changes in intensities and splitting of some of the Raman lines due to lattice and molecular modes have been observed. In the cryomilled samples this strong background is deconvoluted into two components: one due to lattice disorder induced by cryomilling and the other due to Mie scattering from nanosized crystallites. A single-component background scattering attributed to lattice disorder is seen in the Raman spectrum of the amorphous sample. Fluorescence measurements showed an intrinsic fluorescence signal in as-received Griseofulvin that does not correspond to the inelastic background in the Raman spectra and, moreover, decreases in intensity upon cryomilling, thus excluding an assignment of the Raman background intensity to impurity- or molecular-defect-induced fluorescence. Wide-angle XRPD measurements on cryomilled Griseofulvin shows a broad two-component background consistent with the background-scattering component in the Raman data associated with lattice disorder, but at longer correlation lengths. Persistence of this disorder to even longer lengths is evident in small-angle synchrotron XRPD data on micronized Griseofulvin taken as a function of temperature from the crystalline to the amorphous phase.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2010

Heterometallic M/Mn (M=Cu, Co, Zn) acetate complexes as precursors for binary oxides

A facile one-pot procedure, or so-called 'direct synthesis,' was used to prepare the novel heterometallic complexes [M{sub 2}Mn(OAc){sub 6}(bpy){sub 2}], where M=Cu (1), Co (2), Zn (3), bpy=2,2'-bipyridyl, with high yields via oxidative dissolution of pure metals in a liquid phase. The complexes were characterized by an elemental analysis, single crystal X-ray diffraction method and FTIR. These complexes are proposed as precursors, whose thermal degradation may lead to the formation of solids possessing nano- to microsize levels of dispersity. The thermal behavior of the complexes obtained was studied by thermal analysis (TG/DTA/DTG) in both air and N{sub 2} and also by TPD mass-spectrometry in vacuo. The FTIR, X-ray powder diffraction (PXRD) and thermoanalytical data were used for the identification of the solid products of thermal degradation. The morphology and microstructure of the solid residues were analyzed, using scanning electron microscopy with energy dispersive X-ray microanalysis (SEM/EDX) at mkm and sub-micro levels. -- Graphical abstract: The novel heterometallic complexes [M{sub 2}Mn(OAc){sub 6}(bpy){sub 2}] (M=Cu, Co, Zn, bpy=2,2'-bipyridyl) were isolated and used as precursors for low-temperature synthesis of binary oxides. Single crystal X-ray diffraction, FTIR, TG/DTA/DTG, TPD-MS, PXRD, SEM/EDX analysis was performed on complexes and powders. Display Omitted

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Synthesis and Characterization of Metastable Cobalt Honeycomb KCoAsO 4

The Kitaev model has served as a long-sought-after target in the realization of a quantum spin liquid that could host Majorana Fermions. Such non-Abelian anyons could revolutionize quantum computing if properly implemented to overcome decoherence. A 3d 7 electronic configuration, like Co 2+ , has been explored by theory and experimental work to design Kitaev materials. Here, in this study, we report the synthesis of a new cobaltate honeycomb material KCoAsO 4 . The compound is synthesized through a low-temperature solution route and crystallized in space group R¯3 with lattice parameters a = 5.0394(1) and c = 28.6790(1) as determined by neutron powder diffraction. The crystal structure follows motifs similar to those of the honeycomb compound BaCo2(AsO 4 ) 2 but presents differing magnetic behavior. Magnetization/heat capacity measurements on the powder show antiferromagnetic transition T N = 14 K. Two lower-temperature transitions are present in susceptibility at low field that resemble spin reorientations. Magnetization data as a function of field have curvature indicative of metamagnetic behavior below the magnetic ordering temperature, with the magnetic ordering suppressed upon application of a higher magnetic field. Computational studies suggest the presence of a weak nearest-neighbor Kitaev term, K 1 , consistent with related honeycomb cobaltates. Together, the data suggest that this material should present a new platform for developing Kitaev quantum spin liquids.

cobaltate↗
DOE OSTI2011

Application of Rietveld Method to the Structural Characteristics of some Bulk and Nanocrystalline Materials

In recent years, the full pattern structure refinement using Rietveld Method, with the advent of increased performance of powder diffractometers has allowed enormous progress in the analysis of powder diffraction data. In the full pattern structure refinement, with the possibility of varying peak shape parameters and site occupancies along with the structural and instrumental parameters, provides information not only on the crystal and magnetic structure, but also gives precise knowledge of the particle size and micro-structural strain. In this report Rietveld profile refinement of some bulk and nano crystalline materials has been presented.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Structural studies of the rhombohedral and orthorhombic monouranates: CaUO{sub 4}, α-SrUO{sub 4}, β-SrUO{sub 4} and BaUO{sub 4}

The structures of some AUO{sub 4} (A=Ca, Sr, or Ba) oxides have been determined using a combination of neutron and synchrotron X-ray diffraction, supported by X-ray absorption spectroscopic measurements at the U L{sub 3}-edge. The smaller Ca cation favours a rhombohedral AUO{sub 4} structure with 8-coordinate UO{sub 8} moieties whilst an orthorhombic structure based on UO{sub 6} groups is found for BaUO{sub 4}. Both the rhombohedral and orthorhombic structures can be stabilised for SrUO{sub 4}. The structural studies suggest that the bonding requirements of the A site cation play a significant role in determining which structure is favoured. In the rhombohedral structure, Bond Valence Sums demonstrate the A site is invariably overbonded, which, in the case of rhombohedral α-SrUO{sub 4}, is compensated for by the formation of vacancies in the oxygen sub-lattice. The uranium cation, with its flexible oxidation state, is able to accommodate this by inducing vacancies along its equatorial coordination site as demonstrated by neutron powder diffraction. - Graphical abstract: Diffraction studies of AUO{sub 4} (A = Ca, Sr, or Ba) oxides reveal the importance of the bonding requirements of the A site cation in determining whether the structure is rhombohedral or orthorhombic. - Highlights: • Structures of AUO{sub 4} ( A = Ca Sr, Ba) refined against X-ray and Neutron diffraction. • The alkali cations size has a dramatic effect on the crystal structure. • Smaller cations favouring a rhombohedral structure. • Oxygen vacancies to stabilise the rhombohedral structure in SrUO{sub 4}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Structural, Magnetic and Magnetocaloric Properties of High-Energy Ball-Milled Gd{sub 5}Si{sub 2}Ge{sub 2}B{sub 0.05} Alloy

Structural, magnetic and magnetocaloric properties of Gd{sub 5}Si{sub 2}Ge{sub 2}B{sub 0.05} alloy, ball milled for different time intervals in the range of 2–50 h were studied. The x-ray powder diffraction analysis of the alloy prior to milling revealed the presence of mixed orthorhombic and monoclinic phases at room temperature. For a milling duration up to 15 h, the alloy powder displayed crystalline nature. Upon further milling, the alloy powder started to lose the crystallinity and after 50 h of milling, the alloy powder displayed amorphous nature. The average particle size of milled samples was found to decrease with increase in milling time. The saturation magnetization value of the bulk alloy 80 emu/g was found to decrease with increase in milling time due to structural disorder. The transition temperature of the milled alloy powder was found to be around 295 K and the transition was found to become broader with increase in milling time. A maximum isothermal entropy change (ΔS{sub max}) of ∼12 J/kg K was obtained in bulk alloy. For a milling duration of 2 h, a marginal decrease of ΔS{sub max} (∼11 J/kg K) was obtained. Whereas, for higher milling durations, (≥ 15 h) a significant decrease in ΔS{sub max} values were observed. However, the broad operating temperature range of the milled powders can be exploited for magnetic refrigeration applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Neutron diffraction study of the formation of ordered antiphase domains in cubic titanium carbide TiC{sub 0.60}

A series of superstructural reflections (described within the sp. gr. Fd3m) are found to be split into three symmetric parts in the neutron powder diffraction pattern of titanium carbide TiC{sub 0.60} annealed at a temperature of 600 Degree-Sign C. No splitting of superstructural reflections is observed in the neutron diffraction pattern of TiC{sub 0.60} annealed at relatively high temperatures (780 Degree-Sign C). This phenomenon can be explained by that fact that the ordering of carbon atoms at relatively high temperatures (780 Degree-Sign C) is accompanied by the formation of randomly oriented rather large antiphase domains (APDs) (450 A). At relatively low temperatures (600 Degree-Sign C), stacking faults arise in the arrangement of partially ordered carbon atoms. In this case, relatively small ordered APDs (290 A) are formed, along with disordered ones.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Characterization of nanosized Al{sub 2}(WO{sub 4}){sub 3}

Graphical abstract: TEM method allows to detect small quantities of impurities not detectable by other methods. In our case impurities of W{sub 5}O{sub 14} are detected in Al{sub 2}(WO{sub 4}){sub 3} nanopowder. Highlights: {yields} Nanosized Al{sub 2}(WO{sub 4}){sub 3} by simple co-precipitation method. {yields} Spherical particles with mean size of 22 nm distributed between 10 and 40 nm at 630 {sup o}C. {yields} XRD, DTA and TEM confirm well defined products with perfect structure. {yields} TEM locality allows detection of impurities not detectable by XRD and DTA. -- Abstract: Nanosized aluminum tungstate Al{sub 2}(WO{sub 4}){sub 3} was prepared by co-precipitation reaction between Na{sub 2}WO{sub 4} and Al(NO{sub 3}){sub 3} aqueous solutions. The powder size and shape, as well as size distribution are estimated after different conditions of powder preparation. The purity of the final product was investigated by XRD and DTA analyses, using the single crystal powder as reference. Between the specimen and the reference no difference was detected. The crystal structure of Al{sub 2}(WO{sub 4}){sub 3} nanosized powder was confirmed by TEM (SAED, HRTEM). In additional, TEM locality allows to detect some W{sub 5}O{sub 14} impurities, which are not visible by conventional X-ray powder diffraction and thermal analyses.

36 MATERIALS SCIENCE↗