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At least 1,459 records · Page 81
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Preparation and characterisation of nanoscale α-Al{sub 2}O{sub 3} by precipitation method

Nanometer-scale α-Al{sub 2}O{sub 3} particles have been synthesized by a simple precipitation method from an aqueous solution in the presence of AlCl{sub 3} and NH{sub 3}. The surface morphology and composition of the as-synthesized Al{sub 2}O{sub 3} nanoparticle were characterized by means of scanning electron microscopy (SEM) and X-ray diffraction (XRD). The powder was nanocrystalline in nature having hexagonal structure with unit cell parameters: a=4.76A°, c=12.99A°. The Al{sub 2}O{sub 3} nanocrystallites with an average crystal size of about 86 nm. The powder has been characterized by means of FT-IR, and UV-Vis Study. From these results it is possible to conclude that the precipitation method is a very suitable technique to prepare α-Al{sub 2}O{sub 3} materials. The technique is fast, low cost and produces well defined materials that can be used for dosimetric applications.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The application of inelastic neutron scattering to explore the significance of a magnetic transition in an iron based Fischer-Tropsch catalyst that is active for the hydrogenation of CO

An iron based Fischer-Tropsch synthesis catalyst is evaluated using CO hydrogenation at ambient pressure as a test reaction and is characterised by a combination of inelastic neutron scattering (INS), powder X-ray diffraction, temperature-programmed oxidation, Raman scattering, and transmission electron microscopy. The INS spectrum of the as-prepared bulk iron oxide pre-catalyst (hematite, α-Fe{sub 2}O{sub 3}) is distinguished by a relatively intense band at 810 cm{sup −1}, which has previously been tentatively assigned as a magnon (spinon) feature. An analysis of the neutron scattering intensity of this band as a function of momentum transfer unambiguously confirms this assignment. Post-reaction, the spinon feature disappears and the INS spectrum is characterised by the presence of a hydrocarbonaceous overlayer. A role for the application of INS in magnetic characterisation of iron based FTS catalysts is briefly considered.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Investigation of the commensurate magnetic structure in the heavy-fermion compound CePt 2 In 7 using magnetic resonant x-ray diffraction

In this paper, we investigated the magnetic structure of the heavy-fermion compound CePt 2 In 7 below T N = 5.34 (2) K using magnetic resonant x-ray diffraction at ambient pressure. The magnetic order is characterized by a commensurate propagation vector k 1/2 = (1/2, 1/2, 1/2) with spins lying in the basal plane. Our measurements did not reveal the presence of an incommensurate order propagating along the high-symmetry directions in reciprocal space but cannot exclude other incommensurate modulations or weak scattering intensities. The observed commensurate order can be described equivalently by either a single-k structure or by a multi-k structure. Furthermore we explain how a commensurate-only ordering may explain the broad distribution of internal fields observed in nuclear quadrupolar resonance experiments [Sakai et al., Phys. Rev. B 83, 140408 (2011)] that was previously attributed to an incommensurate order. We also report powder x-ray diffraction showing that the crystallographic structure of CePt 2 In 7 changes monotonically with pressure up to P = 7.3 GPa at room temperature. The determined bulk modulus B 0 = 81.1 (3) GPa is similar to those of the Ce-115 family. Broad diffraction peaks confirm the presence of pronounced strain in polycrystalline samples of CePt 2 In 7 . Lastly, we discuss how strain effects can lead to different electronic and magnetic properties between polycrystalline and single crystal samples.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Crystal growth, differential gas adsorption, high thermal stability, and reversible coordination of two new barium-organic frameworks, Ba(SBA)(DMF){sub 4} and Ba{sub 2}(BTEC)(H{sub 2}O)

Single crystals of two barium-organic framework materials, Ba(SBA)(DMF){sub 4} (CAUMOF-15) and Ba{sub 2}(BTEC)(H{sub 2}O) (CAUMOF-16), have been grown through solvothermal reactions (H{sub 2}SBA=4,4′-sulfonyldibenzoic acid and H{sub 4}BTEC=1,2,4,5-benzenetetracarboxylic acid). The crystal structures of the reported frameworks have been determined by single-crystal X-ray diffraction. The materials have been fully characterized by powder X-ray diffraction (PXRD), elemental analyses, Infrared (IR) spectroscopy, and thermogravimetric analyses (TGA). CAUMOF-15 reveals a three-dimensional open-framework that comprises of an inorganic motif with one-dimensional chains and the SBA linkers. CAUMOF-16 shows another three-dimensional backbone consisting of layers of edge-shared BaO{sub 9} and BaO{sub 10} polyhedra, and BTEC pillars. Both of the 3D frameworks exhibit relatively high thermal stabilities. The PXRD and IR spectral data confirm that CAUMOF-15 and CAUMOF-16 reveal reversible coordinations of the respective solvent molecules, DMF and H{sub 2}O. Gas adsorption properties towards nitrogen, hydrogen, and carbon dioxide have been also investigated. - Graphical abstract: Crystals of two new barium-organic frameworks, Ba(SBA)(DMF){sub 4} and Ba{sub 2}(BTEC)(H{sub 2}O), exhibiting a differential gas adsorption, a high thermal stability, and a reversible coordination of solvent molecules have been grown. - Highlights: • Crystals of two new 3D Ba-MOFs are grown. • The two Ba-MOFs reveal very high thermal stabilities up to ca. 400 °C. • Ba(SBA)(DMF){sub 4} exhibits differential gas adsorption properties. • The two Ba-MOFs show reversible coordination of the solvent molecules.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Experimental Evidence of Negative Linear Compressibility in the MIL-53 Metal-Organic Framework Family

Here, we report a series of powder X-ray diffraction experiments performed on the soft porous crystals MIL-53(Al) and NH 2 -MIL-53(Al) in a diamond anvil cell under different pressurization media. Systematic refinements of the obtained powder patterns demonstrate that these materials expand along a specific direction while undergoing total volume reduction under an increasing hydrostatic pressure. Our results confirm for the first time the negative linear compressibility behaviour of this family of materials, recently predicted from quantum chemical calculations.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Observation of localized heating phenomena during microwave heating of mixed powders using in situ x-ray diffraction technique

In materials processing research using microwave heating, there have been several observations of various phenomena occurring known as microwave effects. One significant example of such a phenomenon is increased reaction kinetics. It is believed that there is a possibility that this might be caused by localized heating, were some reactants would attain a higher than apparent temperature. To examine whether such thermal gradients are indeed possible, mixed powders of two microwave non-absorbers, alumina and magnesia, were mixed with graphite, a known absorber, and heated in a microwave furnace. During microwave irradiation, the local temperatures of the respective sample constituents were measured using an in situ x-ray diffraction technique. In the case of the alumina and graphite sample, a temperature difference of around 100 °C could be observed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1985

X-ray diffraction studies of phase transformations in heavy-metal fluoride glasses

Powder X-ray diffraction and differential scanning calorimetry studies of the crystallization properties of five ZrF4-based glass compositions have indicated that the crystalline phase in Zr-Ba-La-Pb fluoride glass is beta-BaZrF6; no such identification of crystal phases was obtainable, however, for the other glasses. Reversible polymorphic phase transformations occur in Zr-Ba-La-Li and Zr-Ba-La-Na fluoride glasses, upon heating to higher temperatures.

Bansal, N. P.↗
DOE OSTI2024

Critical behavior in monoclinic Cr 3 ⁢Te 4

High-quality monoclinic Cr 3 ⁢Te 4 crystals are synthesized by the chemical vapor transport method and confirmed by synchrotron powder x-ray diffraction. Critical behaviors of Cr 3 ⁢Te 4 are studied by bulk isothermal magnetization measurements around its paramagnetic to ferromagnetic phase transition. From these data, we evaluate the modified Arrott plot, the Kouvel-Fisher plot, and critical isotherms, and estimate critical exponent values of β~0.3827, γ~1.2119, and δ~4.16, and the Curie temperature T C ≈321 K. After the scaling, the isothermal magnetization curves below and above the critical temperatures collapse into two independent universal branches which signifies the reliability of our critical exponent estimation. Finally, the estimated critical exponent values of Cr 3 ⁢Te 4 do not match well with theoretically calculated values of any three-dimensional models.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effect of three bis-pyridyl-bis-amide ligands with various spacers on the structural diversity of new multifunctional cobalt(II) coordination polymers

Three new cobalt(II) coordination polymers [Co{sub 2}(1,4-NDC){sub 2}(3-bpye)(H{sub 2}O)] (1), [Co(1,4-NDC)(3-bpfp)(H{sub 2}O)] (2) and [Co(1,4-NDC)(3-bpcb)] (3) [3-bpye=N,N′-bis(3-pyridinecarboxamide)-1,2-ethane, 3-bpfp=bis(3-pyridylformyl)piperazine, 3-bpcb=N,N′-bis(3-pyridinecarboxamide)-1,4-benzene, and 1,4-H{sub 2}NDC=1,4-naphthalenedicarboxylic acid] have been hydrothermally synthesized. The structures of complexes 1–3 have been determined by X-ray single crystal diffraction analyses and further characterized by infrared spectroscopy (IR), powder X-ray diffraction (PXRD) and thermogravimetric analyses (TGA). Complex 1 is a 3D coordination structure with 8-connected (4{sup 20}.6{sup 8}) topology constructed from 3D [Co{sub 2}(1,4-NDC){sub 2}(H{sub 2}O)]{sub n} framework and bidentate 3-bpye ligands. Complex 2 shows 1D “cage+cage”-like chain formed by 1D [Co{sub 2}(1,4-NDC){sub 2}]{sub n} ribbon chains and [Co{sub 2}(3-bpfp){sub 2}] loops, which are further linked by hydrogen bonding interactions to form a 3D supramolecular network. Complex 3 displays a 3D coordination network with a 6-connected (4{sup 12}.6{sup 3}) topology based on 2D [Co{sub 2}(1,4-NDC){sub 2}]{sub n} layers and bidentate 3-bpcb bridging ligands. The influences of different bis-pyridyl-bis-amide ligands with various spacers on the structures of title complexes are studied. Moreover, the fluorescent properties, electrochemical behaviors and magnetic properties of complexes 1–3 have been investigated. - Graphical abstract: Three multifunctional cobalt(II) complexes constructed from three bis-pyridyl-bis-amide and 1,4-naphthalenedicarboxylic acid have been hydrothermally synthesized and characterized. The fluorescent, electrochemical and magnetic properties of 1–3 have been investigated. - Highlights: • Three multifunctional cobalt(II) complexes based on various bis-pyridyl-bis-amide ligands. • Complex 1 is a 3D coordination structure with 8-connected (4{sup 20}.6{sup 8}) topology. • Complex 2 is a 1D “cage+cage”-like chain. • Complex 3 is a 3D coordination network with a 6-connected (4{sup 12}.6{sup 3}) topology. • The fluorescent, electrochemical and magnetic properties of 1–3 were reported.

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

Melting curve and phase diagram of vanadium under high-pressure and high-temperature conditions

We discuss melting curve and phase diagram of vanadium under high-pressure and high-temperature conditions We report a combined experimental and theoretical study of the melting curve and the structural behavior of vanadium under extreme pressure and temperature. We performed powder x-ray-diffraction experiments up to 120 GPa and 4000 K, determining the phase boundary of the body-centered cubic-to-rhombohedral transition and melting temperatures at different pressures. Melting temperatures have also been established from the observation of temperature plateaus during laser heating, and the results from the density-functional theory calculations. Results obtained from our experiments and calculations are fully consistent and lead to an accurate determination of the melting curve of vanadium. These results are discussed in comparison with previous studies. The melting temperatures determined in this study are higher than those previously obtained using the speckle method, but also considerably lower than those obtained from shockwave experiments and linear muffin-tin orbital calculations. Finally, a high-pressure, high-temperature equation of state up to 120 GPa and 2800 K has also been determined.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Long-range and local crystal structures of the S r 1 - x C a x Ru O 3 perovskites

Here, the crystal structures of the Sr 1–x Ca x RuO 3 (0 ≤ x ≤ 1) perovskites are investigated using both long-range and local structural probes. High-resolution synchrotron powder x-ray-diffraction characterization at ambient temperature shows that the materials have orthorhombic long-range crystal structures to high precision, and we support previous work showing that Ca 2+ substitution for Sr 2+ primarily changes the tilting of rigid corner-sharing RuO 6 octahedra at their shared oxygen vertices. X-ray pair-distribution function analysis for SrRuO 3 , CaRuO 3 , and one intermediate composition show them to display monoclinic symmetry at the local level; when averaged over different domain orientations this yields orthorhombic symmetry in the long range, and no long-range or local phase transitions are observed between 80 and 300 K for materials with intermediate compositions. High-resolution transmission electron microscopy shows that the Sr/Ca distribution is random at the nanoscale. Lastly, we plot magnetic characteristics such as the ferromagnetic T c , Curie-Weiss theta, effective moment, and ambient temperature susceptibility vs the octahedral tilt and unit-cell volume.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Polaronic transport and thermoelectricity in Mn 3 Si 2 Te 6 single crystals

Here, we carried out a comprehensive study of the structural, electrical transport, thermal, and thermodynamic properties in ferrimagnetic Mn 3 Si 2 Te 6 single crystals. Mn and Te K -edge x-ray absorption spectroscopy and synchrotron powder x-ray diffraction were measured to provide information on the local atomic environment and the average crystal structure. The dc and ac magnetic susceptibility measurements indicate a second-order paramagnetic to ferrimagnetic transition at T c ~ 74 K, which is further confirmed by the specific heat measurement. Mn 3 Si 2 Te 6 exhibits semiconducting behavior along with a large negative magnetoresistance of -87% at T c and a relatively high value of thermopower up to ~10 mV/K at 5 K. Besides the rapidly increasing resistivity ρ(T) and thermopower S(T) below 20 K, the large discrepancy between the activation energy for resistivity E ρ and thermopower E S above 20 K indicates the polaronic transport mechanism. Furthermore, the thermal conductivity κ(T) of Mn 3 Si 2 Te 6 is notably rather low, comparable to Cr 2 Si 2 Te 6 , and is strongly suppressed in the magnetic field across T c , indicating the presence of strong spin-lattice coupling, also similar with Cr 2 Si 2 Te 6 .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Equation of state, phase transitions, and band-gap closure in Pb Cl 2 and Sn Cl 2

The equations of state and band-gap closures for Pb Cl 2 and Sn Cl 2 were studied using both experimental and theoretical methods. Here we measured the volume of both materials to a maximum pressure of 70 GPa using synchrotron-based angle-dispersive powder x-ray diffraction. The lattice parameters for both compounds showed anomalous changes between 16–32 GPa, providing evidence of a phase transition from the cotunnite structure to the related Co 2 Si structure, in contrast to the postcotunnite structure as previously suggested. First-principles calculations confirm this finding and predict a second phase transition to a Co 2 Si-like structure between 75– 110 GPa in Pb Cl 2 and 60–75 GPa in Sn Cl 2 . Band gaps were measured under compression to ~70 GPa for Pb Cl 2 and ~66 GPa for Sn Cl 2 and calculated up to 200 GPa for Pb CI 2 and 120 GPa for Sn Cl 2 . We find an excellent agreement between our experimental and theoretical results when using the Heyd-Scuseria-Ernzerhof (HSE06) hybrid functional, which suggests that this functional could reliably be used to calculate the band gap of similar AX 2 compounds. Experimental and calculated band-gap results show discontinuous decreases in the band gap corresponding to phase changes to higher-coordinated crystal structures, giving insight into the relationship between interatomic geometry and metallicity.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Experimental equation of state of 11 lanthanide nitrides (NdN to LuN) and pressure induced phase transitions in NdN, SmN, EuN, and GdN

Through an extensive data analysis of powder X-ray diffraction data obtained at pressures up to at least 78 GPa, we report the experimental equations of state for all lanthanide nitrides between NdN and LuN, excluding the radioactive Pm. By fitting the obtained unit cell volumes as a function of pressure with the third order Birch–Murnaghan equation of state, we find that the bulk modulus increases with an increasing lanthanide number from K 0 = 146(12) GPa for NdN to 182(7) GPa in EuN. Hereafter, the bulk modulus reaches a plateau for the rest of the series except for TmN which has a lower bulk modulus. We find that the first derivative of the bulk modulus is around 4 for all compounds except TbN, which displays a significantly different compression behavior. In addition, we find a B1 to B10 pressure-induced phase transition in NdN, SmN, EuN, and GdN at increasingly higher pressures. In fact, we observe that the onset pressure of the phase transition increases linearly with Ln atomic number. From TbN and onwards, we do not observe any sign of a B1 to B10 transition indicating that the transition pressure exceeds the studied pressure range. Therefore, we believe that, for the heavier lanthanides, the linear relationship between the onset pressure and the lanthanide number does not hold and even higher pressures are needed to observe the transition. This coherent study of the series of lanthanide nitrides offers a unique opportunity for benchmark studies of computational methods applied to compounds with 4f electrons.

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

Structural study of Ca{sub 2}Gd{sub 2}Ge{sub 2}O{sub 9} and optical spectroscopy of the Eu{sup 3+} dopant ion

The new rare earth-based germanate compound Ca{sub 2}Gd{sub 2}Ge{sub 2}O{sub 9} (orthorhombic (Pnma) crystal structure), has been characterized and investigated for the first time, using synchrotron powder X-ray diffraction. From Rietveld refinement calculations on the collected powder pattern we observe an inhomogeneous distribution of the two available cationic sites by Gd{sup 3+} and Ca{sup 2+} ions. In particular, the former prefers the occupation (67.5%) of the site with 8-fold coordination. In addition, we observed a not negligible degree of distortion of the Ge{sub 2}O{sub 7}{sup 6−} unit. Finally, luminescence spectra and decay curves of Eu{sup 3+} doped Ca{sub 2}Gd{sub 2}Ge{sub 2}O{sub 9} were measured and analysed taking into account the structural features of the host. The results reveal that this material shows strong red luminescence upon excitation in the region where blue LEDs emit (470 nm). - Graphical abstract: The structural study on Ca{sub 2}Gd{sub 2}Ge{sub 2}O{sub 9} exploiting synchrotron X-ray diffraction, allows us to determine the detailed geometry of the metal coordination polyhedra, which is closely related to the emission luminescence spectroscopy of the Eu{sup 3+} dopant ion introduced as impurity in this host. - Highlights: • The crystal structure of the Ca{sub 2}Gd{sub 2}Ge{sub 2}O{sub 9} was determined. • Gd{sup 3+} ion is distributed on two crystal sites with different occupation. • A structural study focused on the metal coordination polyhedra was performed. • Two emitting sites are detected for Eu{sup 3+} dopant ion in Ca{sub 2}Gd{sub 2}Ge{sub 2}O{sub 9}. • Strong red luminescence by excitation in the region where blue LEDs emit was found.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Uranium Silicide/Nitride Pellet Fabrication Demonstration: Report on Powder Characteristics (Final CRADA Report)

This report details experimental procedures and results of work at the Idaho National Lab to fabricate U 3 Si 2 and UN ceramic powders from their basic elements. The reaction procedure centers on arc melting using a cold, copper hearth. The reacted "buttons" are then ground into powder, and the powder is characterized. The preliminary experiments utilized feeding pieces of metallic U and Si (in the proper ratio) into the arc-melting furnace for melting into "buttons." This melting was repeated several times with the intent of homogenizing the reaction to produce phase pure U 3 Si 2 powder. However, sintering of the pressed-powder at over 1400C showed partial melting and slumping of the pellets. Characterization of the powder using x-ray diffraction (XRD) indicated the crystalline portion of the powder was U 3 Si 2 . However, further investigations indicated a significant portion (12.4%) of the powder was amorphous Si that was transformed into crystalline Si after a period of annealing. Therefore, a greatly improved method of powder fabrication was developed using mixing fine powders of U and Si together, pressing into a pellet, followed by arc melting and grinding into U 3 Si 2 powder. This method was highly successful in producing high phase purity (>98.5% U 3 Si 2 ) powder. One feature of this method is that the fine U powder is made by a hydride/de-hydride cycle. The equipment available at INL only allows for fabrication of relatively small batches, and the method (using INL equipment) is somewhat labor intensive. The powder was used to successfully press and sinter U 3 Si 2 pellets ("Final Report on Pellet Fabrication," INL/LTD-13-29465). A limited attempt was made to fabricate high purity UN powder using the fine U powder made at INL (hydride/de-hydride method) and heating it under flowing nitrogen gas. X-ray diffraction was used to characterize the resulting powder, and a Rietveld refinement was performed on the data. The refinement showed a result of 70.0% UN and 30.0% U 2 N 3 . It is thought that the UN content can be easily increased

Source record↗
DOE OSTI2023

Linker Vacancy Engineering of a Robust ftw–type Zr–MOF for Hexane Isomers Separation

Discrimination of physically similar molecules by porous solids represents an important yet challenging task in industrially relevant chemical separations. Precisely controlled pore dimension and/or tailored pore surface functionality are crucial to achieve high-efficiency separation. Metal-organic frameworks (MOFs) are promising candidates for these challenging separations in light of their structural diversity as well as highly adjustable pore dimension/functionality. We report here a microporous, ftw-type Zr-based MOF structure, HIAM-410 (HIAM=Hoffmann Institute of Advanced Materials), built on hexanuclear Zr 6 cluster and pyrene-1,3,6,8-tetracarboxylate (ptc 4– ). Its crystallographic structure has been determined using continuous rotation electron diffraction (cRED) technique combined with Rietveld refinement against powder X-ray diffraction data, aided by low-dose high-resolution transmission electron microscopy (HRTEM) imaging. The compound features exceptional framework stability that is comparable to the prototype MOF UiO-66. Interestingly, the linker vacancies in the pristine MOF structure could be partially restored by post-synthetic linker insertion. Its separation capability of hexane isomers is enhanced substantially upon the linker vacancy engineering. As a result, the restored structure exhibits efficient splitting of monobranched and dibranched hexane isomers at both room temperature and industrially relevant temperature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Magnetic structure and spin dynamics of the quasi-two-dimensional antiferromagnet Zn-doped copper pyrovanadate

We report magnetic properties of the antiferromagnet Zn x Cu 2-x V 2 O 7 (ZnCVO) with x ≈ 0.06 have been thoroughly investigated on powder and single-crystal samples. The crystal structure determination using powder x-ray and neutron diffraction confirms that our ZnCVO samples are isostructural with β-Cu 2 V 2 O 7 (β-CVO) with a small deviation in the lattice parameters. Macroscopic magnetic property measurements also confirm the similarity between the two compounds. The Cu 2+ spins were found to align along the crystallographic c axis, antiparallel to their nearest neighbors connected by the leading exchange interaction J 1 . Spin dynamics reveals a typical symmetric spin-wave dispersion with strong interactions in the bc plane and weak interplane coupling. The exchange interaction analysis indicates that the spin network of ZnCVO is topologically consistent with the previous DFT prediction but the values of leading exchange interactions are contradictory. Furthermore, rather than the predicted 2D honeycomb structure, the spin network in ZnCVO could be better described by the anisotropic 2D spin network composed of J 1 , J 5 , and J 6 interactions, four bonds per one spin site, coupled by weak interplane interactions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗