Measurement of Lattice Parameter at the Nanometer Scale Using Convergent Beam Microdiffraction from a Thermal Emission Source
Explore the source record for details and available documents.
crystal growth Laue zone atomic level CBM electron↗
SEARCH · Search NASA
Results for “lattice parameters”
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.
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.↗
Ion beam sputtering of in situ superconducting Y-Ba-Cu-O films
Oriented superconducting YBa2Cu3O7 thin films were deposited on yttria stabilized zirconia and SrTiO3 substrates by ion-beam sputtering of a nonstoichiometric oxide target. The films exhibited zero-resistance critical temperatures as high as 83.5 K without post-deposition anneals. Both the deposition rate and the c-lattice parameter data displayed two distinct regimes of dependence on the beam power of the ion source. Low-power sputtering yielded films with large c-dimensions and low Tc. Higher-power sputtering produced a continuous decrease in the c-lattice parameter and increase in critical temperature. Films having the smaller c-lattice parameters were Cu rich. The Cu content of films deposited at beam voltages of 800 V and above increased with increasing beam power.
Klein, J. D.↗
Investigation of the Surface Stress in SiC and Diamond Nanocrystals by In-situ High Pressure Powder Diffraction Technique
The real atomic structure of nanocrystals determines key properties of the materials. For such materials the serious experimental problem lies in obtaining sufficiently accurate measurements of the structural parameters of the crystals, since very small crystals constitute rather a two-phase than a uniform crystallographic phase system. As a result, elastic properties of nanograins may be expected to reflect a dual nature of their structure, with a corresponding set of different elastic property parameters. We studied those properties by in-situ high-pressure powder diffraction technique. For nanocrystalline, even one-phase materials such measurements are particularly difficult to make since determination of the lattice parameters of very small crystals presents a challenge due to inherent limitations of standard elaboration of powder diffractograms. In this investigation we used our methodology of the structural analysis, the 'apparent lattice parameter' (alp) concept. The methodology allowed us to avoid the traps (if applied to nanocrystals) of standard powder diffraction evaluation techniques. The experiments were performed for nanocrystalline Sic and GaN powders using synchrotron sources. We applied both hydrostatic and isostatic pressures in the range of up to 40 GPa. Elastic properties of the samples were examined based on the measurements of a change of the lattice parameters with pressure. The results show a dual nature of the mechanical properties (compressibilities) of the materials, indicating a complex, core-shell structure of the grains.
Palosz, B.↗
Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry
Fundamental limitations, with respect to nanocrystalline materials, of the traditional elaboration of powder diffraction data like the Rietveld method are discussed. A tentative method of the analysis of powder diffraction patterns of nanocrystals is introduced which is based on the examination of the variation of lattice parameters calculated from individual Bragg lines (named the "apparent lattice parameter", alp). We examine the application of our methodology using theoretical diffraction patterns computed for models of nanocrystals with a perfect crystal lattice and for grains with a two-phase, core-shell structure. We use the method for the analysis of X-ray and neutron experimental diffraction data of nanocrystalline diamond powders of 4, 6 and 12 nm in diameter. The effects of an internal pressure and strain at the grain surface is discussed. This is based on the dependence of the alp values oil the diffraction vector Q and on the PDF analysis. It is shown, that the experimental results support well the concept of the two-phase structure of nanocrystalline diamond.
Palosz, B.↗
Thermal expansion behavior of NiSi/NiSi2
The thermal expansion of NiSi/NiSi2 for a range of temperatures from 293 to 1223 K was determined using high-temperature X-ray diffraction. While a linear relation with temperature was found for the lattice parameter of NiSi2, third-order relationships were found for the three lattice parameters of NiSi, with one of the parameters showing a decrease with increasing temperature. The volumetric expansion of both materials exhibited linear relationships.
Wilson, D. F.↗
Defect Structure of Beta NiAl Using the BFS Method for Alloys
The semiempirical BFS method for alloys is generalized by replacing experimental input with first-principles results thus allowing for the study of complex systems. In order to examine trends and behavior of a system in the vicinity of a given point of the phase diagram a search procedure based on a sampling of selected configurations is employed. This new approach is applied to the study of the beta phase of the Ni-Al system, which exists over a range of composition from 45-60 at.% Ni. This methodology results in a straightforward and economical way of reproducing and understanding the basic features of this system. At the stoichiometric composition, NiAl should exist in a perfectly ordered B2 structure. Ni-rich alloys are characterized by antisite point defects (with Ni atoms in the Al sites) with a decrease in lattice parameters. On the Al-rich side of stoichiometry there is a steep decrease in lattice parameter and density with increasing Al content. The presence of vacancies in Ni sites would explain such behavior. Recent X-ray diffraction experiments suggest a richer structure: the evidence, while strongly favoring the presence of vacancies in Ni sites, also suggests the possibility of some vacancies in Al sites in a 3:1 ratio. Moreover, local ordering of vacant sites may be preferred over a random distribution of individual point defects.
Bozzolo, Guillermo↗
Atomistic Modeling of RuAl and (RuNi) Al Alloys
Atomistic modeling of RuAl and RuAlNi alloys, using the BFS (Bozzolo-Ferrante-Smith) method for alloys is performed. The lattice parameter and energy of formation of B2 RuAl as a function of stoichiometry and the lattice parameter of (Ru(sub 50-x)Ni(sub x)Al(sub 50)) alloys as a function of Ni concentration are computed. BFS based Monte Carlo simulations indicate that compositions close to Ru25Ni25Al50 are single phase with no obvious evidence of a miscibility gap and separation of the individual B2 phases.
Gargano, Pablo↗
MC carbide structures in M(lc2)ar-M247
The morphologies and distribution of the MC carbides in Mar-M247 ingot stock and castings were investigated using metallographic, X-ray diffraction and energy-dispersive X-ray analysis techniques. The MC carbides were found to form script structures during solidification. The script structures were composed of three distinct parts. The central cores and elongated arms of the MC carbide script structures had compositions (Ti, Cr, Hf, Ta, W)C and lattice parameters of 4.39 A. The elongated script arms terminated in enlarged, angular "heads". The heads had compositions (Ti, Hf, Ta, W)C and lattice parameters of approximately 4.50 A. The heads had a higher Hf content than the cores and arms. The size of the script structures, as well as the relative amount of head-type to core and arm-type MC carbide, was found to be determined by solidification conditions. No carryover of the MC carbides from the ingot stock to the remelted and cast material was observed.
Wawro, S. W.↗
Analysis of the Defect Structure of B2 Feal Alloys
The Bozzolo, Ferrante and Smith (BFS) method for alloys is applied to the study of the defect structure of B2 FeAI alloys. First-principles Linear Muffin Tin Orbital calculations are used to determine the input parameters to the BFS method used in this work. The calculations successfully determine the phase field of the B2 structure, as well as the dependence with composition of the lattice parameter. Finally, the method is used to perform 'static' simulations where instead of determining the ground state configuration of the alloy with a certain concentration of vacancies, a large number of candidate ordered structures are studied and compared, in order to determine not only the lowest energy configurations but other possible metastable states as well. The results provide a description of the defect structure consistent with available experimental data. The simplicity of the BFS method also allows for a simple explanation of some of the essential features found in the concentration dependence of the heat of formation, lattice parameter and the defect structure.
Bozzolo, Guillermo↗
Redistribution of Ti and Al in deuterium charged TiAl
The redistribution of titanium and aluminum in a single-phase TiAl alloy that has been exposed to a high pressure of deuterium gas at high temperature is studied. The microstructure in the as-received, uncharged condition consisted of single-phase gamma TiAl grains and a random distribution of precipitates. Precipitates were distributed throughout the matrix and along the grain boundaries. The chemistry of the precipitates varied considerably; some were rich in Al, while other were mostly Ti with some Si and Al. The dislocation density in most grains was low, although in a few grains a high dislocation density was observed. FCC deuterides with a lattice parameter of 0.45 nm form in a Ti-52.1Al-2.1Ta (at. pct) alloy after exposure to 1.38 MPa of deuterium gas at 650 C for 213 hr. The structure and lattice parameter are consistent with the formation of Ti(l)D2. The deuterides that form in this alloy are enriched in Ti and deficient in Al and Ta compared to the deuteride-free matrix. Regions of the matrix contiguous with the deuterides have a correspondingly enhanced aluminum and tantalum concentration.
Legzdina, D.↗
Interplay Between Thin Film Ferroelectric Composition, Microstructure and Microwave Phase Shifter Performance
One of the keys to successfully incorporating ferroelectric films into Ku-band (12 to 18 GHz) phase shifters is to establish the composition, microstructure, and thickness required to meet the tuning needs, and tailor the film properties to meet these needs. Optimal performance is obtained when the film composition and device design are such that the device performance is limited by odd mode dielectric losses, and these losses are minimized as much as possible while still maintaining adequate tunability. The parameters required to maintain device performance will vary slightly depending on composition, but we can conclude that the best tuning-to-loss figures of merit (K-factor) are obtained when there is minimal variation between the in-plane and out-of-plane lattice parameters, and the full-width half maximum values of the BSTO (002) peaks are less than approximately 0.04 deg. We have observed that for phase shifters in which the ferroelectric crystalline quality and thickness are almost identical, higher losses are observed in films with higher BaISr ratios. The best performance was observed in phase shifters with Ba:Sr = 30:70. The superiority of this composition was attributed to several interacting factors: the B a: Sr ratio was such that the Curie temperature (180 K) was far removed from room temperature, the crystalline quality of the film was excellent, and there was virtually no difference between the inplane and out-of-plane lattice parameters of the film.
Mueller, Carl H.↗
Equivalent crystal theory of alloys
Equivalent Crystal Theory (ECT) is a new, semi-empirical approach to calculating the energetics of a solid with defects. The theory has successfully reproduced surface energies in metals and semiconductors. The theory of binary alloys to date, both with first-principles and semi-empirical models, has not been very successful in predicting the energetics of alloys. This procedure is used to predict the heats of formation, cohesive energy, and lattice parameter of binary alloys of Cu, Ni, Al, Ag, Au, Pd, and Pt as functions of composition. The procedure accurately reproduces the heats of formation versus composition curves for a variety of binary alloys. The results are then compared with other approaches such as the embedded atom and lattice parameters of alloys from pure metal properties more accurately than Vegard's law is presented.
Bozzolo, Guillermo↗
Comparison of gamma-gamma Phase Coarsening Responses of Three Powder Metal Disk Superalloys
The phase microstructures of several powder metal (PM) disk superalloys were quantitatively evaluated. Contents, chemistries, and lattice parameters of gamma and gamma strengthening phase were determined for conventionally heat treated Alloy 10, LSHR, and ME3 superalloys, after electrolytic phase extractions. Several of long term heat treatments were then performed, to allow quantification of the precipitation, content, and size distribution of gamma at a long time interval to approximate equilibrium conditions. Additional coarsening heat treatments were performed at multiple temperatures and shorter time intervals, to allow quantification of the precipitation, contents and size distributions of gamma at conditions diverging from equilibrium. Modest differences in gamma and gamma lattice parameters and their mismatch were observed among the alloys, which varied with heat treatment. Yet, gamma coarsening rates were very similar for all three alloys in the heat treatment conditions examined. Alloy 10 had higher gamma dissolution and formation temperatures than LSHR and ME3, but a lower lattice mismatch, which was slightly positive for all three alloys at room temperature. The gamma precipitates of Alloy 10 appeared to remain coherent at higher temperatures than for LSHR and ME3. Higher coarsening rates were observed for gamma precipitates residing along grain boundaries than for those within grains in all three alloys, during slow-moderate quenching from supersolvus solution heat treatments, and during aging at temperatures of 843 C and higher.
Superalloys↗
Modeling of gamma/gamma-prime phase equilibrium in the nickel-aluminum system
A theoretical model is proposed for the determination of phase equilibrium in alloys, taking into consideration dissimilar lattice parameters. Volume-dependent pair interactions are introduced by means of phenomenological Lennard-Jones potentials and the configurational entropy of the system is treated in the tetrahedron approximation of the cluster variation method. The model is applied to the superalloy-relevant, nickel-rich, gamma/gamma-prime phase region of the Ni-Al phase diagram. The model predicts reasonable values for the lattice parameters and the enthalpy of formation as a function of composition, and the calculated phase diagram closely approximates the experimental diagram.
Sanchez, J. M.↗
Prediction of structures and magnetic orientations in solid alpha and beta-O2
A quasi-harmonic-lattice-dynamics method coupled with a pattern-recognition optimization scheme is used to determine the minimum energy structures and magnetic orientations of solid oxygen. It is shown that the magnetic interaction is responsible for the stability of alpha-O2 with respect to beta-O2 at zero temperature and pressure. The calculated alpha-O2 lattice parameters, magnetic orientations, and sublimation energy are in good agreement with experiment. Phonon dispersion curves are calculated at vector k not equal to zero and the acoustic sound velocities are determined. The rms translational and orientational fluctuations from equilibrium are also calculated. The beta-O2 phase is described by constraining the magnetic moments so that the magnetic Hamiltonian preserves the hexagonal symmetry of the crystal. The calculated lattice parameters are in good agreement with the experiments, and a three-sublattice, quasi-helical magnetic orientation is predicted from structural and energetic considerations.
Etters, R. D.↗
Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED
The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.
Source record↗
X-ray measurements of stresses and defects in EFG and large grained polycrystalline silicon ribbons
The Bond method was employed to measure the lattice parameter in an area of 0.4 mm in diameter of EFG Si-ribbons to an accuracy of + or - 0.00008 A. A Bond goniometer was built which included a goniostat with a special specimen holder to mount ribbons 1 m in length and 75 mm in width which could be rotated about two orthogonal axes, and a Leitz microscope for precision alignment of a particular area into the center of the goniostat and the small primary X-ray beam. The (321) planes were found to be parallel to the surface of the ribbons with an angular spread of about 15 deg. The poles of the (111) planes clustered about an angle of 25 deg away from the surface normal, again with a spread of 10 deg. The lattice parameter of a small piece of ribbon material was found to be a sub o = 5.43075 A. A maximum stress of 115 MPa was observed in a fractured ribbon which corresponded to the fracture stress of single crystals of Si.
Wagner, C. N. J.↗