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Results for “lattice parameter determination”

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Precision lattice parameter determination from transmission diffraction of thick specimens with irregular cross sections

Accurate determination of lattice parameters from X-ray diffraction requires that the diffraction angles be measured very precisely, and significant errors result if the sample–detector separation differs from that assumed. Transmission diffraction from bones, which have a complex cross section and must be left intact, is a situation where this separation is difficult to measure and it may differ from position to position across the specimen. Here, this article describes a method for eliminating the effect of variable sample cross section. Diffraction patterns for each position on the specimen are collected before and after 180° rotation about an axis normal to the cross section of interest. This places the centroid of the diffracting mass at the center of rotation and provides the absolute lattice parameters from the average apparent lattice parameters at the two rotation angles. Diffraction patterns were collected across the cross section of three specimens: a 3D-printed elliptical cylinder of Hyperelastic Bone (HB), which is composed primarily of synthetic hydroxyapatite (hAp), a 3D-printed HB model of the second metacarpal bone (Mc2), and a modern human Mc2 containing nanocrystalline carbonated apatite (cAp). Rietveld refinement was used to determine precise unit-cell parameters a apparent and c apparent for each pattern of each scan, and these values determined the actual average < a > and < c > for each sample. In conclusion, the results indicate that the 0°/180° rotation method works well enough to uncover variations approaching 1 × 10 -3 Å in cAp unit-cell parameters in intact bones with irregular cross sections.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Determination of lattice parameters, strain state and composition in semipolar III-nitrides using high resolution X-ray diffraction

In group-III-nitride heterostructures with semipolar or nonpolar crystal orientation, anisotropic lattice and thermal mismatch with the buffer or substrate lead to a complex distortion of the unit cells, e.g., by shearing of the lattice. This makes an accurate determination of lattice parameters, composition, and strain state under assumption of the hexagonal symmetry impossible. In this work, we present a procedure to accurately determine the lattice constants, strain state, and composition of semipolar heterostructures using high resolution X-ray diffraction. An analysis of the unit cell distortion shows that four independent lattice parameters are sufficient to describe this distortion. Assuming only small deviations from an ideal hexagonal structure, a linear expression for the interplanar distances d{sub hkl} is derived. It is used to determine the lattice parameters from high resolution X-ray diffraction 2ϑ-ω-scans of multiple on- and off-axis reflections via a weighted least-square fit. The strain and composition of ternary alloys are then evaluated by transforming the elastic parameters (using Hooke's law) from the natural crystal-fixed coordinate system to a layer-based system, given by the in-plane directions and the growth direction. We illustrate our procedure taking an example of (112{sup ¯}2) Al{sub κ}Ga{sub 1−κ}N epilayers with Al-contents over the entire composition range. We separately identify the in-plane and out-of-plane strains and discuss origins for the observed anisotropy.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Diffuse multiple scattering

A new form of diffraction lines similar to Rutherford, Kikuchi and Kossel lines has been identified. They can be used to eliminate the need for sample/source matching in Lonsdale’s triple convergent line method in lattice-parameter determination. A new form of diffraction lines has been identified, similar to Rutherford, Kikuchi and Kossel lines. This paper highlights some of the properties of these lines and shows how they can be used to eliminate the need for sample/source matching in Lonsdale’s triple convergent line method in lattice-parameter determination.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1996

Transmission Electron Microscope Measures Lattice Parameters

Convergent-beam microdiffraction (CBM) in thermionic-emission transmission electron microscope (TEM) is technique for measuring lattice parameters of nanometer-sized specimens of crystalline materials. Lattice parameters determined by use of CBM accurate to within few parts in thousand. Technique developed especially for use in quantifying lattice parameters, and thus strains, in epitaxial mismatched-crystal-lattice multilayer structures in multiple-quantum-well and other advanced semiconductor electronic devices. Ability to determine strains in indivdual layers contributes to understanding of novel electronic behaviors of devices.

Pike, William T.↗
DOE OSTI2018

The Effect of Silver Ion Occupancy on Hollandite Lattice Structure

The effect of tunnel cations on tunnel size in α-MnO 2 structured (hollandite, cryptomelane) materials has long been of interest, as the tunnel size effects catalytic and transport properties. Previous research on the tunnel size has focused on potassium cryptomelane (K x Mn 8 O 16 ). This paper uses synthetic control of silver content in Ag x Mn 8 O 16 to investigate the effect that tunnel silver occupancy has on the lattice parameters. Materials with silver (x) content between 1.14 and 1.66 were synthesized, synchrotron diffraction and Rietveld Refinement was used to determine lattice parameters. The lattice parameters were found to contract as silver content increases (from 9.774 Å to 9.738 Å), in contrast to previous investigations of other tunnel cations.

36 MATERIALS SCIENCE↗
DOE OSTI2015

X-ray studies of dynamic aging in an aluminum alloy subjected to severe plastic deformation

In this work, X-ray scattering methods were applied for a quantitative characterization of the microstructure of an aluminum alloy of the Al–Mg–Si system during dynamic aging realized through the high pressure torsion technique. A qualitative and quantitative phase analysis of the alloy was performed, together with Al alloy lattice parameter determination. From the reflections broadening the effective size of the coherent scattering domains and the lattice microstrain were determined in the framework of the Halder–Wagner approach. Using the method of small-angle X-ray scattering, the quantitative characteristics of the size, shape and spatial distribution of the secondary phase particles formed in the Al alloy during dynamic aging were established. In order to validate the obtained results, the method of small-angle X-ray scattering was preliminarily tested on similar samples after artificial aging and compared with the results from small-angle neutron diffraction widely known in literature. - Highlights: • Spherical fcc β-Mg2Si precipitates formed in Al 6201 alloy during dynamic aging in the course of severe plastic deformation. • The size, shape and distribution of the precipitates due to artificial and dynamic aging were revealed by SAXS method. • Monoclinic needle-like β' precipitates and Al5FeSi intermetallic phase were detected in 6201 alloy after T6 treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2026

High energy X-ray characterization of the microstructure of PuGa alloy samples at macroscopic depths and non-ambient conditions

High energy (95 keV) X-rays were utilized to characterize the microstructure of eight PuGa alloy samples at room temperature and during cooling to ∼10 K. The samples had different Ga content (nominally 0-3.4 at.%), age, and history. A ninth sample, similarly characterized with neutron diffraction, was included to extend the Ga range to 7 at.%. The samples span the range from single phase α (monoclinic) to δ (face-centered cubic) PuGa, as well as a two-phase α′/δ sample. The crystallographic textures, phase fractions, lattice parameters and dislocation densities of each sample were evaluated through distinct analysis techniques. The textures of the samples were modest. In each case, the dislocation densities were relatively high, comparable to cold worked metals and metals exposed to similar radiation dose. At room temperature, the lattice parameters determined in the predominantly single-phase samples were larger than expected based on the nominal Ga concentration. The observed lattice thermal expansions of the single-phase δ samples to 10 K are self-consistent across the samples and consistent with previous measurements reported in the literature. Significantly larger thermal lattice strain is observed in the δ phase of the two-phase material due to mechanical constraint from the α′ phase, which has a three times larger thermal expansion and is much harder than the δ phase. In conclusion, the results demonstrate the unique value of high-energy X-rays for relatively routine microstructural characterization of Pu alloy samples.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Thermodynamic re-modelling of the Cu–Nb–Sn system: Integrating the nausite phase

Currently available Cu–Nb–Sn phase diagrams lack the recently discovered nausite phase (Cu,Nb)Sn 2 , which is an important intermediate in the course of thermal processing of superconducting Nb 3 Sn wires. Processing decisively determines the resulting microstructure of Nb 3 Sn and, thus, its superconducting properties. Lack of suitable and complete phase diagrams, however, obstructs rational design of such thermal processing procedures. To close this gap and to obtain valid knowledge of homogeneity and stability range of nausite, various Cu–Nb–Sn samples, which are heat-treated between 300 °C and 500 °C, are investigated. By means of energy-dispersive X-ray spectroscopy (EDX), a temperature-dependent homogeneity range of nausite is observed, which covers average mole fractions of Cu between 0.09 and 0.15. This is correlated with a change in the mean atomic volume and can be seen in the lattice parameters determined by X-ray diffraction (XRD). Additionally performed first-principles calculations on different CuSn 2 and NbSn 2 model structures confirm this trend. Furthermore, the peritectic decomposition of nausite to NbSn 2 and liquid at 586 °C is determined by means of in situ XRD and differential scanning calorimetry (DSC). By using the CALPHAD (CALculation of PHase Diagrams) approach, all these findings are used to extend a previous thermodynamic description of the Cu–Nb–Sn system by including the nausite as an additional phase. Finally, with this noteworthy integration, the updated modelling of the Cu–Nb–Sn system can be used for optimizing the multistage heat-treatment steps during processing superconducting Nb 3 Sn wires.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Surface speciation and interactions between adsorbed chloride and water on cerium dioxide

Abstract: Ceria particles with different specific surface areas were contaminated with chloride and water, then heat treated at 500 and 900 °C, to investigate the sorption behaviour onto the metal oxide. The association of chloride with the particles was investigated using electron microscopy and energy dispersive x-ray analysis. Results from xray photoelectron spectroscopy, x-ray absorption spectroscopy (XAS) and infrared spectroscopy show that the amount of chloride and water adsorbed on the particles increases with surface area. These species are mostly removed upon heat treatment, from 6.3 to 0.8 at% Cl- on high specific surface area, and 1.4 to 0.4 at% on low specific surface area particles. Lattice parameters determined by x-ray diffraction reveal that chloride is not incorporated into the bulk ceria structure, but crystal size does increase upon contamination. Sintering of contaminated high specific surface area particles occurs with heat treatment at 900 °C, until they resemble low specific surface area particles synthesised at this temperature. The Ce L-edge XAS of ceria particles shows that chloride is not present in the first co-ordination sphere around Ce(IV) ions, so is not directly bonded to Ce as a chloride in the bulk structure.

Sutherland-Harper, Sophie↗
DOE OSTI2016

Investigations of cations distributions and morphology of cobalt ferrite magnetic nanoparticles

Cobalt ferrite nanoparticles were synthesized by co-precipitation method and structural properties was investigated by X-ray diffraction (XRD) at room temperature. X-ray diffraction data was used to determine lattice parameter, X-ray density, distributions of cations among tetrahedral and octahedral sites, site radii, ionic radii and bond length of inverse spinel cobalt ferrite. XRD analysis revealed crystallinity and high intense peak correspond to cubic inverse spinel structure with average crystalline size measured by X-ray line profile fitting was found to be 13nm for most intense peak (311). The surface morphology and microstructural feature was investigated by TEM analysis which revealed that particle size varying from 12-22 nm with selected electron diffraction pattern (SAED).

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS2002

Effect of the Chemical State of the Surface on the Relaxation of the Surface Shell Atoms in SiC and GaN Nanocrystals

The effect of the chemical state of the surface of nanoparticles on the relaxation in the near-surface layer was examined using the concept of the apparent lattice parameter (alp) determined for different diffraction vectors Q. The apparent lattice parameter is a lattice parameter determined either from an individual Bragg reflection, or from a selected region of the diffraction pattern. At low diffraction vectors the Bragg peak positions are affected mainly by the structure of the near-surface layer, while at high Q-values only the interior of the nano-grain contributes to the diffraction pattern. Following the measurements on raw (as prepared) powders we investigated powders cleaned by annealing at 400C under vacuum, and the same powders wetted with water. Theoretical alp-Q plots showed that the structure of the surface layer depends on the sample treatment. Semi-quantitative analysis based on the comparison of the experimental and theoretical alp-Q plots was performed. Theoretical alp-Q relations were obtained from the diffraction patterns calculated for models of nanocrystals with a strained surface layer using the Debye functions.

Palosz, B.↗
NASA NTRS2003

The Traps of using Conventional Methodology of Evaluation of Powder Diffractograms for Determination of the Lattice Parameters of Nanocrystals

Inherent errors introduced by the algorithm of standard procedures of evaluation of powder diffractograms when applied for nanopowders are shown. The implications of the errors are discussed in connection with some results reported in the literature. Alternate methodology of evaluation of powder diffractograms of nanocrystals is presented.

Curreri, Peter A.↗
DOE OSTI2016

X-Ray diffraction on large single crystals using a powder diffractometer

Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is sufficient to determine one lattice parameter or the lattice spacing along a certain, high- symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegard’s rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 μm up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimization of the alignment are discussed in detail. Finally, in particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

Crystal structure and thermal expansion of a CsCe{sub 2}Cl{sub 7} scintillator

We used single-crystal X-ray diffraction data to determine crystal structure of CsCe{sub 2}Cl{sub 7}. It crystallizes in a P112{sub 1}/b space group with a=19.352(1) Å, b=19.352(1) Å, c=14.838(1) Å, γ=119.87(2)°, and V=4818.6(5) Å{sup 3}. Differential scanning calorimetry measurements combined with the structural evolution of CsCe{sub 2}Cl{sub 7} via X-ray diffractometry over a temperature range from room temperature to the melting point indicates no obvious intermediate solid–solid phase transitions. The anisotropy in the average linear coefficient of thermal expansion of the a axis (21.3×10{sup –6}/°C) with respect to the b and c axes (27.0×10{sup –6}/°C) was determined through lattice parameter refinement of the temperature dependent diffraction patterns. These findings suggest that the reported cracking behavior during melt growth of CsCe{sub 2}Cl{sub 7} bulk crystals using conventional Bridgman and Czochralski techniques may be largely attributed to the anisotropy in thermal expansion. - Graphical abstract: Three-dimensional quadric surface of thermal expansion coefficient of CsCe{sub 2}Cl{sub 7} at room temperature (sphere – isotropic) and near melting point (ellipsoid – anisotropic). - Highlights: • Crystal structure of CsCe{sub 2}Cl{sub 7} was solved through X-ray diffraction. • Linear coefficients of thermal expansion were determined from in-situ XRD in 25–650 °C. • Anisotropy of the a axis with respect to b and c axes (21.3 vs 27.0×10{sup –6}/°C) was found. • No solid–solid phase transitions were observed via XRD and thermal analysis.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Shear strength of a refractory high entropy alloy MoNbTaVW under high pressure

Radial X-ray diffraction (R-XRD) was performed in situ using a Panoramic Diamond Anvil Cell on the refractory high entropy alloy MoNbTaVW. The lattice parameters were determined through a Le Bail fit using a body centered cubic (BCC) lattice of symmetry $Im$$\overline{3}$$m$ (international space group number 229). Upper and lower bounds to the shear strength were determined up to 80 GPa nonhydrostatically using copper as a pressure standard. The equation of state was derived at the magic angle ψ = 54.7° and yielded a bulk modulus of K 0 = 220.8 ± 1.65 GPa. The experimental lattice parameters and bulk modulus match closely with corresponding density functional theory (DFT) calculations. The BCC phase remains stable up to the highest pressure of 80 GPa studied and is shown to be elastically anisotropic. The shear strength was found to saturate around 70 GPa with a value of τ = 1.75 GPa, and the shear moduli are presented in different limits of iso-strain and iso-stress.

36 MATERIALS SCIENCE↗