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At least 325 records · Page 18
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Diffraction Studies from Minerals to Organics - Lessons Learned from Materials Analyses

In many regards the study of materials and minerals by powder diffraction techniques are complimentary, with techniques honed in one field equally applicable to the other. As a long-time materials researcher many of the examples are of techniques developed for materials analysis applied to minerals. However in a couple of cases the study of new minerals was the initiation into techniques later used in materials-based studies. Hopefully they will show that the study of new minerals structures can provide opportunities to add new methodologies and approaches to future problems. In keeping with the AXAA many of the examples have an Australian connection, the materials ranging from organics to battery materials.

Mineralogy↗
DOE OSTI2020

Pseudospin versus magnetic dipole moment ordering in the isosceles triangular lattice material K 3 Er(VO 4 ) 2

Spin- 1 / 2 antiferromagnetic triangular lattice models are paradigms of geometrical frustration, revealing very different ground states and quantum effects depending on the nature of anisotropies in the model. Due to strong spin orbit coupling and crystal field effects, rare-earth ions can form pseudospin- 1 / 2 magnetic moments with anisotropic single-ion and exchange properties. Thus, rare-earth-based triangular lattices enable the exploration of this interplay between frustration and anisotropy. Here we study one such case, the rare-earth double vanadate glaserite material K 3 Er ( VO 4 ) 2 , which is a quasi-two-dimensional (2D) isosceles triangular antiferromagnet. Our specific heat and neutron powder diffraction data from K 3 Er ( VO 4 ) 2 reveal a transition to long range magnetic order at T N = 155 ± 5 mK which accounts for all R ln 2 entropy. Furthermore, we observe what appears to be a coexistence of three-dimensional (3D) and quasi-2D order below T N . The quasi-2D order leads to an anisotropic Warren-like peak profile for ( h k 0 ) reflections, while the 3D order is best-described by layers of antiferromagnetic b -aligned moments alternating with layers of zero moment. Our magnetic susceptibility data reveal that Er 3 + takes on a strong X Y single-ion anisotropy in K 3 Er ( VO 4 ) 2 , leading to vanishing moments when pseudospins are oriented along c . Thus, the magnetic structure, when considered from the pseudospin point of view could comprise of alternating layers of b -axis and c -axis aligned antiferromagnetism.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Crystal structure of pemetrexed disodium heptahydrate, C 20 H 33 N 5 Na 2 O 13 (Alimta)

The crystal structure of pemetrexed disodium heptahydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Pemetrexed disodium heptahydrate crystallizes in space group P2 1 (#4) with a = 11.732 697(27), b = 5.244 195(14), c = 21.689 00(6) Å, β = 92.663 90(20) ° , V = 1333.051(6) Å 3 , and Z = 2. Each of the two ionized carboxylate groups acts as a unidentate ligand to a Na cation. The remaining five positions of the octahedral coordination spheres are occupied by water molecules. The Na octahedra share an edge to form pairs. These pairs share corners to form chains along the b -axis. All of the water molecule hydrogen atoms act as hydrogen bond donors. In addition the hydrogen atoms associated with the nitrogen atoms and amino groups of the pemetrexed anion were also observed to act as hydrogen bond donors. The powder pattern has been submitted to the International Centre for Diffraction Data (ICDD) for inclusion in the Powder Diffraction File ™ .

Kaduk, James A.↗
DOE OSTI2024

Multidimensional Rietveld refinement of high-pressure neutron diffraction data of PbNCN

High-pressure neutron powder diffraction data from PbNCN were collected on the high-pressure diffraction beamline SNAP located at the Spallation Neutron Source (SNS) of Oak Ridge National Laboratory (Tennessee, USA). The diffraction data were analyzed using the novel method of multidimensional (two dimensions for now, potentially more in the future) Rietveld refinement and, for comparison, employing the conventional Rietveld method. To achieve two-dimensional analysis, a detailed description of the SNAP instrument characteristics was created, serving as an instrument parameter file, and then yielding both cell and spatial parameters as refined under pressure for the first time for solid-state cyanamides/carbodiimides. The bulk modulus B 0 = 25.1 (15) GPa and its derivative B ′ 0 = 11.1 (8) were extracted for PbNCN following the Vinet equation of state. Surprisingly, an internal transition was observed beyond 2.0 (2) GPa, resulting from switching the bond multiplicities (and bending direction) of the NCN 2− complex anion. The results were corroborated using electronic structure calculation from first principles, highlighting both local structural and chemical bonding details.

Meinerzhagen, Yannick↗
DOE OSTI2025

Shifting and tilting towards enhanced piezoelectricity in high-temperature ceramics: an average structure study of (1 − x )BiFe 2/8 Ti 3/8 Mg 3/8 O 3 – x PbTiO 3 through X-ray and neutron diffraction

A comprehensive report is provided of the average structure of a high Curie temperature ferroelectric ceramic, (1 − x)BiFe 2/8 Ti 3/8 Mg 3/8 O 3 –xPbTiO 3 (BFTM–xPT) when x = 0.25–0.375 at room temperature. Both neutron and synchrotron X-ray powder diffraction data were collected and combined Rietveld refinements were completed. These data revealed that, of the compositions studied, BFTM–xPT crystallizes as mixed phase material. At x = 0.25–0.275, the average structure of each phase is best described by space groups R3c and Cc. At 0.30 ≥ x ≥ 0.35, a morphotropic phase boundary is present and is best modelled by space groups P4mm and Cc, where space group Cc is the dominant phase. As the concentration of PbTiO 3 increases, the amount of octahedral tilting decreases and x = 0.375 exhibits a loss of octahedral tilting and crystallizes in space groups P4mm and Cm. In conclusion, an updated phase diagram at room temperature of this novel system is given and structural intricacies responsible for its piezoelectric properties are revealed.

high Curie temperature↗
DOE OSTI2015

CIT-7, a crystalline, molecular sieve with pores bounded by 8 and 10-membered rings

A new crystalline molecular sieve, denoted CIT-7, is synthesized using an imidazolium-based diquaternary organic structure directing agent (OSDA). The framework structure is determined from a combination of rotation electron diffraction and synchrotron X-ray powder diffraction data. The structure has 10 crystallographically unique tetrahedral atoms (T-atoms) in the unit cell, and can be described as an ordered arrangement of the [4 2 5 4 6 2 ] mtw building unit and a previously unreported [4 4 5 2 ] building unit. The framework contains a 2-dimensional pore system that is bounded by 10 T-atom rings (10-ring, 5.1 Å × 6.2 Å opening) that are connected with oval 8-rings (2.9 Å × 5.5 Å opening) through medium-sized cavities (~7.9 Å) at the channel intersections. CIT-7 can be synthesized over a broad range of compositions including pure-silica and heteroatom, e.g., aluminosilicate and titanosilicate, containing variants.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Observation of indium ion migration-induced resistive switching in Al/Mg{sub 0.5}Ca{sub 0.5}TiO{sub 3}/ITO

Understanding switching mechanisms is very important for resistive random access memory (RRAM) applications. This letter reports an investigation of Al/Mg{sub 0.5}Ca{sub 0.5}TiO{sub 3} (MCTO)/ITO RRAM, which exhibits bipolar resistive switching behavior. The filaments that connect Al electrodes with indium tin oxide electrodes across the MCTO layer at a low-resistance state are identified. The filaments composed of In{sub 2}O{sub 3} crystals are observed through energy-dispersive X-ray spectroscopy, high-resolution transmission electron microscopy, nanobeam diffraction, and comparisons of Joint Committee on Powder Diffraction Standards (JCPDS) cards. Finally, a switching mechanism resulting from an electrical field induced by In{sup 3+} ion migration is proposed. In{sup 3+} ion migration forms/ruptures the conductive filaments and sets/resets the RRAM device.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2023

Multilevel atomic structural model for interstratified opal materials

The structure of opal has long fascinated scientists. It occurs in a number of structural states, ranging from amorphous to exhibiting features of stacking disorder. Opal-CT, where C and T signify cristobalite- and tridymite-like interstratification, represents an important link in the length scales between amorphous and crystalline states. However, details about local atomic (dis)order and arrangements extending to long-range stacking faults in opal polymorphs remain incompletely understood. Here, a multilevel modeling approach is reported that considers stacking states in correlation with the abundance of C and T segments as a high-level structural parameter (i.e. not each atom). Optimization accounting for inter-tetrahedral bond lengths and angles and the regularity of the silicate tetrahedra is included as lower levels of structural parameters. Together, a set of parameters with both coarse-grained and atomistic features for different levels of structural details is refined. Structural disorder at the ~10–100 Å distance scale is evaluated using experimental pair distribution function and diffraction datasets, comparing peak intensities, widths and asymmetry. Here this work presents a complete multilevel structural description of natural opal-CT and explains many of the unusual features observed in X-ray powder diffraction patterns. This modeling approach can be adopted generally for analyzing layered materials and their assembly into 3D structures.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Fast-current-heating devices to study in situ phase formation in metallic glasses by using high-energy synchrotron radiation

Details of fast-resistive-heating setups, controlled heating ranging from ~10 1 K s –1 to ~10 3 K s –1 , to study in situ phase transformations (on heating and on cooling) in metallic glasses by high-energy synchrotron x-ray diffraction are discussed here. Both setups were designed and custom built at the Leibniz Institute for Solid State and Materials Research Dresden (IFW Dresden) and have been implemented at the P02.1 Powder Diffraction and Total Scattering Beamline and the P21.1 Swedish Materials Science Beamline at PETRA III storage ring, DESY, Hamburg. The devices are interchangeable at both beamlines. Joule heating is triggered automatically and is timed with the incident beam and detector. The crystallization process can be controlled via a feedback circuit by monitoring the change in the time-dependent resistivity and temperature of glasses. Different ambient atmospheres, such as vacuum and inert gases (He and Ar), can be used to control oxidation and cooling. The main focus of these devices is on understanding the crystallization mechanism and kinetics in metallic glasses, which are brittle and for which fast heating gives defined glass–crystal composites with enhanced plasticity. As an example, phase-transformation sequence(s) in a prototyped Cu–Zr-based metallic glass is described on heating, and a crystalline phase beneficial to the plasticity is identified.

47 OTHER INSTRUMENTATION↗
DOE OSTI2015

Ca{sub 2}Cr{sub 0.5}Ga{sub 1.5}O{sub 5}—An extremely redox-stable brownmillerite phase

Investigation of the Ca{sub 2}Cr{sub x}Ga{sub 2−x}O{sub 5} compositional series reveals a maximum chromium solubility of 25%. The most chromium rich composition, Ca{sub 2}Cr{sub 0.5}Ga{sub 1.5}O{sub 5}, adopts a brownmillerite-type anion deficient perovskite structure described in space group Pnma (a=5.368 Å, b=14.547 Å, c=5.593 Å). Neutron powder diffraction data reveals rigorous B-site cation order, with all of the tetrahedral coordination sites occupied exclusively by gallium and the octahedral coordination sites occupied by gallium or chromium. Annealing studies reveals Ca{sub 2}Cr{sub 0.5}Ga{sub 1.5}O{sub 5} is stable in both oxidizing (100% O{sub 2}) and reducing (5% H{sub 2} in N{sub 2}) conditions up to 800 °C, suggesting it could find application as a stable host lattice for fuel cell electrodes or electrolytes with suitable doping to enhance catalytic behaviour and/or anionic conductivity. - Graphical abstract: Ca{sub 2}Cr{sub 0.5}Ga{sub 1.5}O{sub 5}, adopts a brownmillerite-type anion deficient perovskite structure yet it is stable in both oxidizing (100% O{sub 2}) and reducing (5% H{sub 2} in N{sub 2}) conditions up to 800 °C. - Highlights: • Anion deficient oxide stable to both oxidation and reduction up to 800 °C. • Cation-ordered brownmillerite structure determined by powder neutron diffraction. • Low solubility of Cr{sup 3+} in framework due to spherical d{sup 3} electron configuration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

A novel orange-red emitting NaCaVO{sub 4}:Sm{sup 3+} phosphor for solid state lighting

The samarium doped NaCaVO{sub 4} phosphor was synthesized by the combustion method. The X-ray powder diffraction (XRD) analysis confirmed that the phosphor powder crystallized as orthorhombic structure belonging to space group Cmcm. From Williamson-Hall analysis the grain size and microstrain in the powder was estimated. The Fourier- transform infrared (FT-IR) studies further validated the formation of vanadate phase of the phosphor. Photoluminescence (PL) study revealed that the phosphor could be efficiently excited by UV-VIS from 200 nm to 500 nm. The 565 nm, 602 nm, 648 nm and 713 nm emissions were ascribed to {sup 4}G{sub 5/2} to {sup 6}H{sub J} (J = 5/2, 7/2, 9/2 and 11/2) transitions of the Sm{sup 3+} ion. The present material may be explored as a novel phosphor to be excited by UV light emitting diodes (LEDs) chips for solid-state lighting and display applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Chiral properties of the zero-field spiral state and field-induced magnetic phases of the itinerant kagome metal YMn 6 Sn 6

Applying a magnetic field in the hexagonal plane of YMn 6 Sn 6 leads to a complex magnetic phase diagram of commensurate and incommensurate phases, one of which coexists with the topological Hall effect (THE) generated by a unique fluctuation-driven mechanism. Using unpolarized neutron diffraction, we report on the solved magnetic structure for two previously identified, but unknown, commensurate phases. These include a low-temperature, high-field fanlike phase and a room-temperature, low-field canted antiferromagnetic phase. Here, an intermediate incommensurate phase between the fanlike and forced ferromagnetic phases is also identified as the last known phase of the in-plane field-temperature diagram. Additional characterization using synchrotron powder diffraction reveals extremely high-quality, single-phase crystals, which suggests that the presence of two incommensurate magnetic structures throughout much of the phase diagram is an intrinsic property of the system. Interestingly, polarized neutron diffraction shows that the centrosymmetric system hosts preferential chirality in the zero-field double-flat-spiral phase, which, along with the THE, is a topologically nontrivial characteristic.

36 MATERIALS SCIENCE↗
DOE OSTI2017

In Situ Neutron Diffraction Studies of the Ion Exchange Synthesis Mechanism of Li 2 Mg 2 P 3 O 9 N: Evidence for a Hidden Phase Transition

Motivated by predictions made using a bond valence sum difference map (BVS-DM) analysis, the novel Li-ion conductor Li 2 Mg 2 P 3 O 9 N was synthesized in this paper by ion exchange from a Na 2 Mg 2 P 3 O 9 N precursor. Impedance spectroscopy measurements indicate that Li 2 Mg 2 P 3 O 9 N has a room temperature Li-ion conductivity of about 10 –6 S/cm (comparable to LiPON), which is 6 orders of magnitude higher than the extrapolated Na-ion conductivity of Na 2 Mg 2 P 3 O 9 N at this temperature. The structure of Li 2 Mg 2 P 3 O 9 N was determined from ex situ synchrotron and time-of-flight neutron diffraction data to retain the P2 1 3 space group, though with a cubic lattice parameter of a = 9.11176(8) Å that is significantly smaller than the a = 9.2439(1) Å of Na 2 Mg 2 P 3 O 9 N. The two Li-ion sites are found to be very substantially displaced (~0.5 Å) relative to the analogous Na sites in the precursor phase. The non-molten salt ion exchange method used to prepare Li 2 Mg 2 P 3 O 9 N produces a minimal background in powder diffraction experiments, and was therefore exploited for the first time to follow a Li + /Na + ion exchange reaction using in situ powder neutron diffraction. Lattice parameter changes during ion exchange suggest that the reaction proceeds through a Na 2–x Li x Mg 2 P 3 O 9 N solid solution (stage 1) followed by a two-phase reaction (stage 2) to form Li 2 Mg 2 P 3 O 9 N. However, full Rietveld refinements of the in situ neutron diffraction data indicate that the actual transformation mechanism is more complex and instead involves two thermodynamically distinct solid solutions in which the Li exclusively occupies the Li1 site at low Li contents (stage 1a) and then migrates to the Li3 site at higher Li contents (stage 1b), a crossover driven by the different signs of the local volume change at these sites. Finally, in addition to highlighting the importance of obtaining full structural data in situ throughout the ion exchange process, these results provide insights into the general question of what constitutes a thermodynamic phase.

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

Photophysical properties of [Ru(2,2′-bipyridine){sub 3}]{sup 2+} encapsulated within the Uio-66 zirconium based metal organic framework

The ability to encapsulate photo-active guest molecules within the pores of metal organic frameworks (MOFs) affords the opportunity to develop robust photocatalysts as well as solar energy conversion systems. An important criteria for such systems is stability of the new materials towards moisture, high temperatures, etc which preclude the use of many MOF frameworks. Here, the ability to encapsulate [Ru(II)(2,2′-bipyridine){sub 3}]{sup 2+}([Ru(bpy){sub 3}]{sup 2+}) into the cavities of the zirconium based MOF Uio-66 as well as the photophysical properties of the complex are reported. The X-ray powder diffraction data of the orange Uio-66 powder are consistent with the formation of Uio-66 in the presence of [Ru(bpy){sub 3}]{sup 2+}. The steady state emission exhibits a significant bathochromic shift from 603 nm in ethanol to 610 nm in Uio-66. The corresponding emission decay of the encapsulated [Ru(bpy){sub 3}]{sup 2+} complex is biexponential with a fast component of 128 ns and a slower component of 1176 ns (20 deg C). The slow component is consistent with encapsulation of [Ru(bpy){sub 3}]{sup 2+} into cavities with restricted volume that prevents the population of a triplet ligand field transition that is anti-bonding with respect to the Ru-N bonds. The origin of the fast component is unclear but may involve interactions of the [Ru(bpy){sub 3}]{sup 2+} encapsulated within large cavities formed through missing ligand defect sites within the Uio-66 materials. Co-encapsulated quenchers contained within these larger cavities gives rise to the reduced lifetimes of the [Ru(bpy){sub 3}]{sup 2+} complexes. - Graphical abstract: One-pot synthesis of Ru(II)tris(2,2-bipyridine)@Uio-66 (left) and the effects of encapsulation on the excited state energy levels and decay pathways of the Ru(II)tris(2,2-bipyridine) complex (right).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Three-dimensional copper(II) carboxylates based on 4,4′,4″-benzene-1,3,5-triyltris(benzoic acid)

The homochiral coordination polymers [Cu{sub 4}(CH{sub 3}OH)(H{sub 2}O){sub 4}(Hbtb)(S-mal){sub 2}]•4H{sub 2}O and [Cu{sub 4}(CH{sub 3}OH)(H{sub 2}O){sub 4}(Hbtb)(R-mal){sub 2}]•4H{sub 2}O were synthesized by heating S- or R-malic acid (H{sub 3}mal), 4,4′,4″-benzene-1,3,5-triyltris(benzoic acid) (H{sub 3}btb), and copper(II) acetate in an aqueous methanolic solution. The reaction with copper(II) nitrate in aqueous dioxane afforded the coordination framework [Cu{sub 6}(C{sub 4}H{sub 8}O{sub 2}){sub 3}(H{sub 2}O){sub 3}(btb){sub 4}]•4C{sub 4}H{sub 8}O{sub 2}•10H{sub 2}O, which does not contain chiral ligands. The compositions and crystal structures of the new compounds were determined by single-crystal X-ray diffraction and confirmed by X-ray powder diffraction, IR spectroscopy, thermogravimetric and elemental analysis.

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

The assembly of two isomorphous coordination compounds based on 1,4-cyclohexanedicarboxylic acid and 2,4-diamino-6-phenyl-1,3,5-triazine

The compounds [Co(e,a-cis-1,4-chdc)(phdat)]{sub n} (1) and [Cd(e,a-cis-1,4-chdc)(phdat)]{sub n} (2) have been synthesized under hydrothermal method by using 1,4-cyclohexanedicarboxylic acid (1,4-H{sub 2}chdc), 2,4-diamino-6-phenyl-1,3,5-triazine (phdat) as well as CoCl{sub 2}·6H{sub 2}O, CdCl{sub 2}·2.5H{sub 2}O respectively and characterized by IR spectra, X-ray single-crystal diffraction, powder X-ray single-crystal diffraction (PXRD), elemental analyses and thermogravimetric analyses (TGA). The results show the compounds 1 and 2 are isomorphous and exhibit paddle-wheel dinuclear Co{sub 2}(CO{sub 2}){sub 4}/Cd{sub 2}(CO{sub 2}){sub 4} units, which are further connected to 1D chain structures by μ{sub 4}:η{sup 1}:η{sup 1}:η{sup 1}:η{sup 1} 1,4-chdc{sup 2–} ligands and extended into a 3D structures via different hydrogen bonding and π…π stacking interactions. Furthermore, compound 1 exhibits antiferromagnetic behavior and compound 2 displays luminescent behavior at solid state. - Graphical abstract: Two isomorphous coordination compounds 1–2 have been synthesized and characterized by XRD, IR spectra and TGA etc. Compound 1 and 2 display antiferromagnetic behavior and luminescent behavior respectively. - Highlights: • Two novel polymers based on 1,4-cyclohexanedicarboxylic acid have been synthesized. • Compounds 1 and 2 feather 1D chain structure built up from paddle-wheel SBUs. • The magnetism of 2 is investigated. • The electrochemical property and luminescent property of 1 are investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗