Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Powder diffraction”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 379 records · Page 21
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Structural properties of barium stannate

Here BaSnO 3 has attracted attention as a transparent conducting oxide with high room temperature carrier mobility. We report a series of measurements that were carried out to assess the structure of BaSnO 3 over a variety of length scales. Measurements included single crystal neutron and x-ray diffraction, Rietveld and pair distribution analysis of neutron powder diffraction, Raman scattering, and high-pressure x-ray diffraction. Results from the various diffraction probes indicate that both the long-range and local structures are consistent with the cubic symmetry. The diffraction data under pressure was consistent with a robustly cubic phase up to 48.9 GPa, which is supported by density functional calculations. Additionally, transverse phonon velocities were determined from measured dispersion of the transverse acoustic phonon branches, the results of which are in good agreement with previous theoretical estimates and ultrasound measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Controlling superstructural ordering in the clathrate-I Ba 8 M 16 P 30 (M = Cu, Zn) through the formation of metal–metal bonds

Order–disorder–order phase transitions in the clathrate-I Ba 8 Cu 16 P 30 were induced and controlled by aliovalent substitutions of Zn into the framework. Unaltered Ba 8 Cu 16 P 30 crystallizes in an ordered orthorhombic ( Pbcn ) clathrate-I superstructure that maintains complete segregation of metal and phosphorus atoms over 23 different crystallographic positions in the clathrate framework. The driving force for the formation of this Pbcn superstructure is the avoidance of Cu–Cu bonds. This superstructure is preserved upon aliovalent substitution of Zn for Cu in Ba 8 Cu 16– x Zn x P 30 with 0 < x < 1.6 (10% Zn/M total ), but vanishes at greater substitution concentrations. Higher Zn concentrations (up to 35% Zn/M total ) resulted in the additional substitution of Zn for P in Ba 8 M 16+ y P 30– y (M = Cu, Zn) with 0 ≤ y ≤ 1. This causes the formation of Cu–Zn bonds in the framework, leading to a collapse of the orthorhombic superstructure into the more common cubic subcell of clathrate-I ( Pm n ). In the resulting cubic phases, each clathrate framework position is jointly occupied by three different elements: Cu, Zn, and P. Detailed structural characterization of the Ba–Cu–Zn–P clathrates-I via single crystal X-ray diffraction, joint synchrotron X-ray and neutron powder diffractions, pair distribution function analysis, electron diffraction and high-resolution electron microscopy, along with elemental analysis, indicates that local ordering is present in the cubic clathrate framework, suggesting the evolution of Cu–Zn bonds. For the compounds with the highest Zn content, a disorder–order transformation is detected due to the formation of another superstructure with trigonal symmetry and Cu–Zn bonds in the clathrate-I framework. It is shown that small changes in the composition, synthesis, and crystal structure have significant impacts on the structural and transport properties of Zn-substituted Ba 8 Cu 16 P 30 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Designing a hybrid electrode toward high energy density with a staged Li + and PF 6 - deintercalation/intercalation mechanism

Existing lithium-ion battery technology is struggling to meet our increasing requirements for high energy density, long lifetime, and low-cost energy storage. Here, a hybrid electrode design is developed by a straightforward reengineering of commercial electrode materials, which has revolutionized the “rocking chair” mechanism by unlocking the role of anions in the electrolyte. Our proof-of-concept hybrid LiFePO 4 (LFP)/graphite electrode works with a staged deintercalation/intercalation mechanism of Li + cations and PF 6 - anions in a broadened voltage range, which was thoroughly studied by ex situ X-ray diffraction, ex situ Raman spectroscopy, and operando neutron powder diffraction. Introducing graphite into the hybrid electrode accelerates its conductivity, facilitating the rapid extraction/insertion of Li + from/into the LFP phase in 2.5 to 4.0 V. This charge/discharge process, in turn, triggers the in situ formation of the cathode/electrolyte interphase (CEI) layer, reinforcing the structural integrity of the whole electrode at high voltage. Consequently, this hybrid LFP/graphite-20% electrode displays a high capacity and long-term cycling stability over 3,500 cycles at 10 C, superior to LFP and graphite cathodes. Importantly, the broadened voltage range and high capacity of the hybrid electrode enhance its energy density, which is leveraged further in a full-cell configuration.

25 ENERGY STORAGE↗
DOE OSTI2020

High oxygen pressure floating zone growth and crystal structure of the metallic nickelates R4Ni3O10 ( R=La,Pr )

Single crystals of the metallic Ruddlesden-Popper trilayer nickelates R 4 Ni 3 O 10 ( R = La , Pr ) were successfully grown using an optical-image floating zone furnace under oxygen pressure ( p O 2 ) of 20 bar for La 4 Ni 3 O 10 and 140 bar for Pr 4 Ni 3 O 10 . Furthermore, a combination of synchrotron and laboratory x-ray single-crystal diffraction, high-resolution synchrotron x-ray powder diffraction and measurements of physical properties revealed that R 4 Ni 3 O 10 ( R = La , Pr ) crystallizes in the monoclinic P 2 1 / a ( Z = 2 ) space group at room temperature, and that a metastable orthorhombic phase ( Bmab ) can be trapped by postgrowth rapid cooling. Both La 4 Ni 3 O 10 and Pr 4 Ni 3 O 10 crystals undergo a metal-to-metal transition (MMT) below room temperature. In the case of Pr 4 Ni 3 O 10 , the MMT is found at 157.6 K. For La 4 Ni 3 O 10 , the MMT depends on the lattice symmetry: 147.5 K for Bmab vs 138.6 K for P 2 1 / a . Lattice anomalies were found at the MMT that, when considered together with the pronounced dependence of the transition temperature on subtle structural differences between Bmab and P 2 1 / a phases, demonstrate a not insignificant coupling between electronic and lattice degrees of freedom in these trilayer nickelates.

36 MATERIALS SCIENCE↗
NASA NTRS2005

Neutron Diffraction Study Oxygen Dissolution Alpha(sub 2)-Ti3Al

Rietveld refinements of neutron powder diffraction data on alpha(sub 2)-Ti3Al have been performed to determine the crystal structure as a function of interstitial oxygen (O) concentration for three alloys with a Ti/Al ratio of approximately equal to 2.34 and O concentrations of 0.25%, 3.99% and 7.71%. The structures of the allows are hexagonal in space group P6(sub 3)/mmc where Ti and Al atoms populate unique sites with excess Al at the Ti site and O atoms occupy octahedral interstitial sites surrounded by six Ti sites. The length of the c-axis was found to increase linearly as the O occupancy of the interstitial sites increased; this lattice lengthening effect was much less pronounced along the alpha axis. Correspondingly, the increases in the lengths of Ti-Al and Ti-Ti bonds with a major component of their direction parallel to the c-axis were roughly an order of magnitude greater than the increases in the lengths of Ti-al and Ti-Ti bonds more closely aligned with the alpha-axis. Densities calculated form the lattice parameters and occupancy factors fall in the range (4.118 plus or minus 0.004) grams per cubic centimeter to (4.194 plus or minus 0.004) grams per cubic centimeter, and exhibit a nearly linear increase with oxygen concentration. Measured densities of (4.113 plus or minus 0.001) grams per cubic centimeter, (4.146 plus or minus 0.009) grams per cubic centimeter, and (4.191 plus or minus 0.002) grams per cubic centimeter for these alloys agree with the results of the refinements.

Jones, Camille Y.↗
NASA NTRS1999

X-Ray Diffraction Techniques for a Field Instrument: Patterns of Lithologic Provences

Future exploration of Mars will attempt to shed light on the mineralogy of surface materials. Instruments deployed from remote platforms should have the capability to conduct both intensive analyses as well as rapid, reconnaissance surveys while they function in the martian environment as surrogate geologists. In order to accommodate the reconnaissance mode of analysis and to compensate for analytical limitations imposed by the space-flight conditions, data analysis methods are being developed that will permit interpretation of data by recognition of signatures or "fingerprints". Specifically, we are developing a technique which will allow interpretation of diffraction patterns by recognition of characteristic signatures of different lithologic provences. This technique allows a remote vehicle to function in a rapid-scan mode using the lithologic signature to determine where a more thorough analysis is needed. An x-ray diffraction pattern is characterized by the angular positions of diffracted x-rays, x-ray intensity levels and background radiation levels. These elements may be used to identify a generalized x-ray signature. Lithologic signatures are being developed in two ways. A signature is composed using the ideal powder diffraction indices from the mineral assembledge common to a specific lithologic provence. This is then confirmed using a laboratory diffraction pattern of a whole rock powder. Preliminary results comparing the diffraction signatures of the major mineral assembledges common to basalt, carbonate, and evaporite basin deposits indicate that lithologies are differentiable as a "fingerprint". Statistical analyses are being performed to establish the confidence levels of this technique.

Marshall, J.↗
DOE OSTI2020

Unraveling the nature of Fe-doping mediated inter- and intra-chain interactions in Ca 3 Co 2 O 6

The structural and magnetic properties of quasi-one-dimensional (1D) spin-chain compounds Ca 3 Co 2-x Fe x O 6 (x = 0, 0.1, 0.2 and 0.3) synthesized by a sol-gel method have been systematically studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), neutron powder diffraction (NPD), dc and ac magnetization measurements. The samples adopt a rhombohedral crystal structure with the space group R-3c in a temperature range of 5–100 K. Fe ions are found to locate at the trigonal prism Co2 crystallographic sites. Fe doping converts some of low-spin Co 3+ ions at Co1 octahedral sites into Co 2+ ions. For the high-temperature paramagnetic phase, the Curie paramagnetic temperature θp changes its sign from positive to negative at x = 0.2, implying that the dominant magnetic interaction is driven from ferromagnetic (FM) to antiferromagnetic (AFM) upon Fe substitution. A partial low-spin to high-spin state crossover of the Co1 ions is observed at high Fe-doping level x = 0.3. All the samples exhibit a long-range spin-density wave (SDW) AFM ordering below TN, followed by a spin-glass-like transition at Tf. These low-temperature magnetic phases were significantly suppressed upon Fe doping. The Fe substitution in Ca 3 Co 2-x Fe x O 6 weakened both intrachain and interchain magnetic interactions, caused by enhanced magnetic disorder due to the different magnetic characters of Ising Co and Heisenberg Fe spins.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Combustion of Silane-Hydrogen-Nitrous oxide Mixtures: Analysis of Laminar Flame Propagation and Condensed Products

The laminar burning rate, the explosion pressure, and the pressure rise coefficient have been measured for silane-nitrous oxide-argon mixtures using the spherically expanding flame technique in a constant volume combustion chamber. For these three parameters, the values obtained were higher than for hydrogen-nitrous oxide-argon and typical hydrocarbon-based mixtures. As an example, a maximum burning rate of 1800 g/m 2 s was measured at 101 kPa, whereas under similar conditions, a maximum burning rate around 950 g/m 2 s has been reported for hydrogen-nitrous oxide-argon mixtures. Here, the condensed combustion products formed in the silane-nitrous oxide-argon flames were sampled and characterized using electron micrograph, electronic diffraction, energy-dispersive spectroscopy, and X-ray powder diffraction. For all equivalence ratios, silica spherical particles with a mean diameter in the range 200-300 nm were observed. In addition, for mixtures with Φ ≥2.2, silicon nanowires were formed. X-ray diffraction experiments showed that the silicon nanowires are composed of a material referred to as “metal silicon” characterized by a cubic structure (lattice parameter: a = 5.425 Å) with the Fm-3m space group.

42 ENGINEERING↗
DOE OSTI2015

Complementary use of monochromatic and white-beam X-ray micro-diffraction for the investigation of ancient materials

Archaeological artefacts are often heterogeneous materials where several phases coexist in a wide grain size distribution. Most of the time, retrieving structure information at the micrometre scale is of great importance for these materials. Particularly, the organization of different phases at the micrometre scale is closely related to optical or mechanical properties, manufacturing processes, functionalities in ancient times and long-term conservation. Between classic X-ray powder diffraction with a millimetre beam and transmission electron microscopy, a gap exists and structure and phase information at the micrometre scale are missing. Using a micrometre-size synchrotron X-ray beam, a hybrid approach combining both monochromatic powder micro-diffraction and Laue single-crystal micro-diffraction was deployed to obtain information from nanometre- and micrometre-size phases, respectively. Therefore providing a way to bridge the aforementioned gap, this unique methodology was applied to three different types of ancient materials that all show a strong heterogeneity. In Roman terra sigillata, the specific distribution of nanocrystalline hematite is mainly responsible for the deep-red tone of the slip, while the distribution of micrometre-size quartz in ceramic bodies reflects the change of manufacturing process between pre-sigillata and high-quality sigillata periods. In the second example, we investigated the modifications occurring in Neolithic and geological flints after a heating process. By separating the diffracted signal coming from the nano- and the micrometre scale, we observed a domain size increase for nanocrystalline quartz in geological flints and a relaxation of the residual strain in larger detritic quartz. In conclusion, through the study of a Roman iron nail, we showed that the carburation process to strengthen the steel was mainly a surface process that formed 10–20 µm size domains of single–crystal ferrite and nanocrystalline cementite.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of particle size and strain on phase stability of (Li{sub 0.06} Na{sub 0.94}) NbO{sub 3}

Alkaline niobates are most suitable and excellent candidates for lead free piezoceramics, as they exhibit morphotropic phase boundary and have ultra-large piezoresponse similar to them. We provide direct experimental evidence of ferroelectric to paraelectric phase transition in (Li{sub 0.06} Na{sub 0.94})NbO{sub 3} with reduction of particle size using a combination of x-ray and neutron powder diffraction techniques at room temperature. Detailed Rietveld analyses of x-ray data show variation of particle sizes from micrometer to nanometer for sintered, calcined, and ball milled powders. The ferroelectric orthorhombic phase for micron sized powder (∼1.17 μm) is found to transform to paraelectric phase by reducing particle size to ∼10.8 nm. The crystal structure of paraelectric phase has been identified with tetragonal symmetry (P4{sub 2}/mmc) and is found to be a post perovskite phase. The low temperature neutron diffraction studies on the powders with different particle sizes reveal that orthorhombic to rhombohedral phase transition gets suppressed with reducing particle size.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Enhancement of luminescence emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor by Li{sup +} co-doping

This paper demonstrates the effects of Li{sup +} co-doping on the structure, morphology, and luminescence properties of GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor prepared using a high-temperature solid-state chemistry method. The GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} powders synthesized with the Li{sup +} co-dopant (in concentrations of 0, 5, 10, and 15 mol%) are characterized by X-ray powder diffraction, scanning electron microscopy, and photoluminescence spectroscopy. Structural analysis showed that powders co-doped with Li{sup +} have larger crystallite sizes and slightly smaller crystal lattice parameters than powders prepared without Li{sup +} ions. Photoluminescence down-conversion (345-nm excitation) and up-conversion (980-nm excitation) spectra show characteristic Er{sup 3+} emissions, with the most intense bands peaking at 525 nm ({sup 2}H{sub 11/2}→{sup 4}I{sub 15/2} transition) and 552 nm ({sup 4}S{sub 3/2}→{sup 4}I{sub 15/2}). The intensity of up-conversion emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} is enhanced (by a factor of four) by co-doping with 5 mol% of Li{sup +} ions. The mechanisms responsible for this emission enhancement are discussed. - Graphical abstract: UC emission spectra for GdVO{sub 4}:1.5-mol% Er{sup 3+}/20-mol% Yb{sup 3+} powders co-doped with different concentrations of Li{sup +} ions, recorded under 980-nm excitation. - Highlights: • 5-mol% Li{sup +} co-doped powders have 400% enhanced up-conversion emission intensity. • 15-mol% Li{sup +} co-doping produces 40% higher emission in down-conversion. • Li{sup +} co-doped powders have larger crystallite size and smaller lattice parameters.

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

Towards solution and refinement of organic crystal structures by fitting to the atomic pair distribution function

In this study, a method towards the solution and refinement of organic crystal structures by fitting to the atomic pair distribution function (PDF) is developed. Approximate lattice parameters and molecular geometry must be given as input. The molecule is generally treated as a rigid body. The positions and orientations of the molecules inside the unit cell are optimized starting from random values. The PDF is obtained from carefully measured X-ray powder diffraction data. The method resembles `real-space' methods for structure solution from powder data, but works with PDF data instead of the diffraction pattern itself. As such it may be used in situations where the organic compounds are not long-range-ordered, are poorly crystalline, or nanocrystalline. The procedure was applied to solve and refine the crystal structures of quinacridone (β phase), naphthalene and allopurinol. In the case of allopurinol it was even possible to successfully solve and refine the structure in P1 with four independent molecules. As an example of a flexible molecule, the crystal structure of paracetamol was refined using restraints for bond lengths, bond angles and selected torsion angles. In all cases, the resulting structures are in excellent agreement with structures from single-crystal data.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

The order-disorder transition in Cu{sub 2}ZnSnS{sub 4} – A neutron scattering investigation

In this work a series of stoichiometric Cu{sub 2}ZnSnS{sub 4} (CZTS) samples annealed at different temperatures in the range of 473–623 K were investigated. The temperature dependence of the Cu/Zn-order-disorder behavior was analyzed by neutron powder diffraction measurements. Cu fully occupies the 2a and Sn the 2b position within the whole temperature range. For Zn and the remaining Cu on sites 2d and 2c, a clear change from ordered to disordered kesterite structure is found. The critical temperature T{sub c} for this Landau-type second order transition was determined as 552±2 K. It was found that in Cu{sub 2}ZnSnS{sub 4} very long annealing times are necessary to reach equilibrium at low temperatures. - Graphical abstract: The order-disorder transition in Cu{sub 2}ZnSnS{sub 4} was investigated using neutron diffraction techniques on samples annealed in the temperature range of 473–623 K. The critical temperature T{sub c} for this Landau-type second order transition was determined as 552±2 K. Display Omitted - Highlights: • The order-disorder transformation of Cu{sub 2}ZnSnS{sub 4} follows a Landau‐type behavior for a second order transition. • The critical exponent β is 0.57±0.06. • The critical temperature was determined as 552±2 K. • A fully ordered (within the standard deviation) Cu{sub 2}ZnSnS{sub 4} sample was synthesized.

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

Neutron scattering study on cathode LiMn{sub 2}O{sub 4} and solid electrolyte 5(Li{sub 2}O)(P{sub 2}O{sub 5})

Neutron scattering is very important technique in order to investigate the energy storage materials such as lithium-ion battery. The unique advantages, neutron can see the light atoms such as Hydrogen, Lithium, and Oxygen, where those elements are negligible by other corresponding X-ray method. On the other hand, the energy storage materials, such as lithium ion battery is very important for the application in the electric vehicles, electronic devices or home appliances. The battery contains electrodes (anode and cathode), and the electrolyte materials. There are many challenging to improve the existing lithium ion battery materials, in order to increase their life time, cyclic ability and also its stability. One of the most scientific challenging is to investigate the crystal structure of both electrode and electrolyte, such as cathodes LiCoO{sub 2}, LiMn{sub 2}O{sub 4} and LiFePO{sub 4}, and solid electrolyte Li{sub 3}PO{sub 4}. Since all those battery materials contain Lithium ions and Oxygen, the used of neutron scattering techniques to study their structure and related properties are very important and indispensable. This article will review some works of investigating electrodes and electrolytes, LiMn{sub 2}O{sub 4} and 5(Li{sub 2}O)(P{sub 2}O{sub 5}), by using a high resolution powder diffraction (HRPD) at the multipurpose research reactor, RSG-Sywabessy of the National Nuclear Energy Agency (BATAN), Indonesia.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Materials Characterization Techniques Lecture Series: X-Ray Diffraction, A Summary of LANL's Materials Capabilities in MPA-11 [Slides]

This presentation provides an overview on X-Ray Diffraction (XRD) to cover background, fundamentals, limitations, best practices, applications, analysis, software, and resources. To summarize: XRD is a great tool for characterizing solid crystalline samples. X-Rays are E-Mag radiation and generate diffraction profiles based on the phase of the sample. Diffraction patterns are unique to the phase of the sample. Powder diffraction gives us better diffraction profiles. We can obtain both qualitative and quantitative data. Analysis requires us to know a little about our sample and a lot about our diffractometer.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The crystal structure of a new calcium aluminate phase containing formate

A new calcium aluminate phase containing formate ions was synthesized and its crystal structure determined. This new phase is indicated as M-phase and was firstly observed in Portland cement pastes hydrated in presence of Ca-formate and in excess of water. The crystal structure of the M-phase was successfully solved in the R-3 space group of the trigonal system on the basis of synchrotron X-ray single crystal diffraction data. The structural model was confirmed by Rietveld refinement of the powder diffraction data acquired on the synthesized pure sample. The crystal structure of the M-phase is similar to that of ettringite, being characterized by columns of AlO{sub 6} octahedra alternating with groups of three edge-sharing CaO{sub 7} polyhedra. The formate ions (HCOO){sup −} share two oxygens with Ca polyhedra and are located in the interspace between the columns. The crystal structure of the M-phase testifies the strong interaction occurring between small organic molecules as formate and the calcium aluminate components of Portland cement.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Synthesis, reversibility and mechanism of the dehydration of monoclinic CaZn{sub 2}(PO{sub 4}){sub 2}·2H{sub 2}O

Highlights: • Reversibility of dehydration of synthetic monoclinic CaZn{sub 2}(PO{sub 4}){sub 2}·2H{sub 2}O to CaZn{sub 2}(PO{sub 4}){sub 2}·H{sub 2}O is proven. • Morphological changes upon dehydration to mono- and anhydrate are investigated. • The diffraction pattern of the monohydrate is presented and indexed. • Lattice constants up to the monohydrate are derived from in-situ XRD measurements. • A topotactic dehydration mechanism is deduced. - Abstract: The reversibility of the dehydration of monoclinic CaZn{sub 2}(PO{sub 4}){sub 2}·2H{sub 2}O to the corresponding monohydrate is proven and the dehydration enthalpy determined by combination of thermal analysis and X-ray diffraction. The mechanism of the monohydrate formation is investigated by scanning electron microscopy (SEM) and temperature dependent in situ X-ray powder diffraction. Mechanistic impact on the powder bulk properties are deduced. As for the orthorhombic dimorph, a crystalline monohydrate species is identified and firstly indexed. Thermal induced changes of the lattice parameters up to the formation of the monohydrate are analyzed. A linear elongation of the lattice parallel to the directions [100] and [001] is found. The corresponding elongation coefficients and the volumetric expansion of the unit cell are determined. With regard to the option of synthetic production of the compound, a possible application of the material for thermochemical energy storage and conversion is conceivable. The relevance of fundamental mechanistic features on the bulk behaviour upon cyclic de- and rehydration is discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗