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At least 361 records · Page 20

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.↗

Growing Larger Crystals for Neutron Diffraction

Obtaining crystals of suitable size and high quality has been a major bottleneck in macromolecular crystallography. With the advent of advanced X-ray sources and methods the question of size has rapidly dwindled, almost to the point where if one can see the crystal then it was big enough. Quality is another issue, and major national and commercial efforts were established to take advantage of the microgravity environment in an effort to obtain higher quality crystals. Studies of the macromolecule crystallization process were carried out in many labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. While technological improvements are resulting in a diminishing of the minimum crystal size required, neutron diffraction structural studies still require considerably larger crystals, by several orders of magnitude, than X-ray studies. From a crystal growth physics perspective there is no reason why these 'large' crystals cannot be obtained: the question is generally more one of supply than limitations mechanism. This talk will discuss our laboratory s current model for macromolecule crystal growth, with highlights pertaining to the growth of crystals suitable for neutron diffraction studies.

Pusey, Marc↗

Synchrotron X-Ray Diffraction Analysis of Meteorites in Thin Section: Preliminary Results

X-ray diffraction is the pre-eminent technique for mineral identification and structure determination, but is difficult to apply to grains in thin section, the standard meteorite preparation. Bright focused X-ray beams from synchrotrons have been used extensively in mineralogy and have been applied to extraterrestrial particles. The intensity and small spot size achievable in synchrotron X-ray beams makes them useful for study of materials in thin sections. Here, we describe Synchrotron X-ray Diffraction (SXRD) in thin section as done at the National Synchrotron Light Source, and cite examples of its value for studies of meteorites in thin section.

Treiman, A. H.↗

Neutron Diffraction Studies of the Atomic Vibrations of Bulk and Surface Atoms of Nanocrystalline SiC

Thermal atomic motions of nanocrystalline Sic were characterized by two temperature atomic factors B(sub core), and B(sub shell). With the use of wide angle neutron diffraction data it was shown that at the diffraction vector above 15A(exp -1) the Wilson plots gives directly the temperature factor of the grain interior (B(sub core)). At lower Q values the slope of the Wilson plot provides information on the relative amplitudes of vibrations of the core and shell atoms.

Stelmakh, S.↗

Rayleigh-Sommerfield Diffraction vs Fresnel-Kirchhoff, Fourier Propagation and Poisson's Spot

The boundary conditions imposed on the diffraction problem in order to obtain the Fresnel-Kirchhoff (FK) solution are well-known to be mathematically inconsistent and to be violated by the solution when the observation point is close to the diffracting screen 1-3. These problems are absent in the Rayleigh-Sommerfeld (RS) solution. The difference between RS and FK is in the inclination factor and is usually immaterial because the inclination factor is approximated by unity. But when this approximation is not valid, FK can lead to unacceptable answers. Calculating the on-axis intensity of Poisson s spot provides a critical test, a test passed by RS and failed by FK. FK fails because (a) convergence of the integral depends on how it is evaluated and (b) when the convergence problem is xed, the predicted amplitude at points near the obscuring disk is not consistent with the assumed boundary conditions.

RS (RAYLEIGH SOMMERFELD)↗

Remote, Noncontact Strain Sensing by Laser Diffraction Developed

A system was developed at the NASA Glenn Research Center for continually monitoring, in real time, the in-plane strain tensor in opaque solids during high-temperature, long-term mechanical testing. The simple, noncontacting, strain-sensing methodology should also be suitable for measurement in hostile environments. This procedure has obvious advantages over traditional, mechanical, contacting techniques, and it is easier to interpret than moir and speckle interferometric approaches. A two-dimensional metallic grid of micrometer dimensions is applied to a metallographically prepared gauge section on the surface of a tensile test specimen by a standard photolithographic process. The grid on the fixtured specimen is interrogated by an He-Ne laser, and the resulting diffraction pattern is projected backwards onto a translucent screen. A charge-coupled device (CCD) camera is used to image the first-order diffraction peaks from the translucent screen. A schematic representation of the system is shown in the figure.

Freedman, Marc R.↗

An Efficient Image Recovery Algorithm for Diffraction Tomography Systems

A diffraction tomography system has potential application in ultrasonic medical imaging area. It is capable of achieving imagery with the ultimate resolution of one quarter the wavelength by collecting ultrasonic backscattering data from a circular array of sensors and reconstructing the object reflectivity using a digital image recovery algorithm performed by a computer. One advantage of such a system is that is allows a relatively lower frequency wave to penetrate more deeply into the object and still achieve imagery with a reasonable resolution. An efficient image recovery algorithm for the diffraction tomography system was originally developed for processing a wide beam spaceborne SAR data...

Jin, Michael Y.↗

Liquid crystal devices especially for use in liquid crystal point diffraction interferometer systems

Liquid crystal point diffraction interferometer (LCPDI) systems that can provide real-time, phase-shifting interferograms that are useful in the characterization of static optical properties (wavefront aberrations, lensing, or wedge) in optical elements or dynamic, time-resolved events (temperature fluctuations and gradients, motion) in physical systems use improved LCPDI cells that employ a "structured" substrate or substrates in which the structural features are produced by thin film deposition or photo resist processing to provide a diffractive element that is an integral part of the cell substrate(s). The LC material used in the device may be doped with a "contrast-compensated" mixture of positive and negative dichroic dyes.

Marshall, Kenneth L.↗

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Park, Yoonjoon↗

Multiple-Zone Diffractive Optic Element for Laser Ranging Applications

A diffractive optic element (DOE) can be used as a beam splitter to generate multiple laser beams from a single input laser beam. This technology has been recently used in LRO s Lunar Orbiter Laser Altimeter (LOLA) instrument to generate five laser beams that measure the lunar topography from a 50-km nominal mapping orbit (see figure). An extension of this approach is to use a multiple-zone DOE to allow a laser altimeter instrument to operate over a wider range of distances. In particular, a multiple-zone DOE could be used for applications that require both mapping and landing on a planetary body. In this case, the laser altimeter operating range would need to extend from several hundred kilometers down to a few meters. The innovator was recently involved in an investigation how to modify the LOLA instrument for the OSIRIS asteroid mapping and sample return mission. One approach is to replace the DOE in the LOLA laser beam expander assembly with a multiple-zone DOE that would allow for the simultaneous illumination of the asteroid with mapping and landing laser beams. The proposed OSIRIS multiple-zone DOE would generate the same LOLA five-beam output pattern for high-altitude topographic mapping, but would simultaneously generate a wide divergence angle beam using a small portion of the total laser energy for the approach and landing portion of the mission. Only a few percent of the total laser energy is required for approach and landing operations as the return signal increases as the inverse square of the ranging height. A wide divergence beam could be implemented by making the center of the DOE a diffractive or refractive negative lens. The beam energy and beam divergence characteristics of a multiple-zone DOE could be easily tailored to meet the requirements of other missions that require laser ranging data. Current single-zone DOE lithographic manufacturing techniques could also be used to fabricate a multiple-zone DOE by masking the different DOE zones during the manufacturing process, and the same space-compatible DOE substrates (fused silica, sapphire) that are used on standard DOE s could be used for multiple- zone DOE s. DOEs are an elegant and cost-effective optical design option for spacebased laser altimeters that require multiple output laser beams. The use of multiple-zone DOEs would allow for the design and optimization of a laser altimeter instrument required to operate over a large range of target distances, such as those designed to both map and land on a planetary body. In addition to space-based laser altimeters, this technology could find applications in military or commercial unmanned aerial vehicles (UAVs) that fly at an altitude of several kilometers and need to land. It is also conceivable that variations of this approach could be used in land-based applications such as collision avoidance and robotic control of cars, trains, and ships.

Ramos-Izquierdo, Luis A.↗

Fabricating Blazed Diffraction Gratings by X-Ray Lithography

Gray-scale x-ray lithography is undergoing development as a technique for fabricating blazed diffraction gratings. As such, gray-scale x-ray lithography now complements such other grating-fabrication techniques as mechanical ruling, holography, ion etching, laser ablation, laser writing, and electron-beam lithography. Each of these techniques offers advantages and disadvantages for implementing specific grating designs; no single one of these techniques can satisfy the design requirements for all applications. Gray-scale x-ray lithography is expected to be advantageous for making gratings on steeper substrates than those that can be made by electron-beam lithography. This technique is not limited to sawtooth groove profiles and flat substrates: various groove profiles can be generated on arbitrarily shaped (including highly curved) substrates with the same ease as sawtooth profiles can be generated on flat substrates. Moreover, the gratings fabricated by this technique can be made free of ghosts (spurious diffraction components attributable to small spurious periodicities in the locations of grooves). The first step in gray-scale x-ray lithography is to conformally coat a substrate with a suitable photoresist. An x-ray mask (see Figure 1) is generated, placed between the substrate and a source of collimated x-rays, and scanned over the substrate so as to create a spatial modulation in the exposure of the photoresist. Development of the exposed photoresist results in a surface corrugation that corresponds to the spatial modulation and that defines the grating surface. The grating pattern is generated by scanning an appropriately shaped x-ray area mask along the substrate. The mask example of Figure 1 would generate a blazed grating profile when scanned in the perpendicular direction at constant speed, assuming the photoresist responds linearly to incident radiation. If the resist response is nonlinear, then the mask shape can be modified to account for the nonlinearity and produce a desired groove profile. An example of grating grooves generated by this technique is shown in Figure 2. A maximum relative efficiency of 88 percent has been demonstrated.

Mouroulis, Pantazis↗

First X-Ray Diffraction Results from Mars Science Laboratory: Mineralogy of Rocknest Aeolian Bedform at Gale Crater

Numerous orbital and landed observations of the martian surface suggest a reasonably uniform martian soil composition, likely as a result of global aeolian mixing [1, 2]. Chemical data for martian soils are abundant [e.g., 2, 3], and phase information has been provided by lander thermal emission and Moessbauer spectroscopic measurements [3, 4, 5, 6]. However, until now no X-ray diffraction (XRD) data were available for martian soil nor has XRD ever been used on another body apart from Earth. XRD is generally considered the most definitive method for determining the crystalline phases in solid samples, and it is the method of choice for determining mineralogy. CheMin s first XRD analysis on Mars coincided with the 100th anniversary of the discovery of X-ray diffraction by von Laue. Curiosity delivered scooped samples of loose, unconsolidated material ("soil") acquired from an aeolian bedform at the Rocknest locality to instruments in the body of the rover (the laboratory). Imaging shows that the soil has a range of particle sizes, of 1-2 mm and smaller, presumably representing contributions from global, regional, and local sources.

Bish, D. L.↗

Impedance Matched to Vacuum, Invisible Edge, Diffraction Suppressed Mirror

Diffraction suppressed mirrors having an invisible edge are disclosed for incident light at both targeted wavelengths and broadband incident light. The mirrors have a first having at least one discontiguous portion having a plurality of nanostructured apertures. The discontiguous mirror portion impedance matches a relatively high impedance portion of the mirror to a relatively low impedance portion of the mirror, thereby reducing the diffraction edge effect otherwise present in a conventional mirror.

Hagopian, John G.↗

Reaching the Diffraction Limit - Differential Speckle and Wide-Field Imaging for the WIYN Telescope

Speckle imaging allows telescopes to achieve diffraction limited imaging performance. The technique requires cameras capable of reading out frames at a very fast rate, effectively 'freezing out' atmospheric seeing. The resulting speckles can be correlated and images reconstructed that are at the diffraction limit of the telescope. These new instruments are based on the successful performance and design of the Differential Speckle Survey Instrument (DSSI).The instruments are being built for the Gemini-N and WIYN telescopes and will be made available to the community via the peer review proposal process. We envision their primary use to be validation and characterization of exoplanet targets from the NASA, K2 and TESS missions and RV discovered exoplanets. Such targets will provide excellent follow-up candidates for both the WIYN and Gemini telescopes. We expect similar data quality in speckle imaging mode with the new instruments. Additionally, both cameras will have a wide-field mode and standard SDSS filters. They will be highly versatile instruments and it is that likely many other science programs will request time on the cameras. The limiting magnitude for speckle observations will remain around 13-14th at WIYN and 16-17th at Gemini, while wide-field, normal CCD imaging operation should be able to go to much fainter, providing usual CCD imaging and photometric capabilities. The instruments will also have high utility as scoring cameras for telescope engineering purposes, or other applications where high time resolution is needed. Instrument support will be provided, including a software pipeline that takes raw speckle data to fully reconstructed images.

detector↗

Crystallographic Characterization of Extraterrestrial Materials by Energy-Scanning X-ray Diffraction

We have continued our long-term project using X-ray diffraction to characterize a wide range of extraterrestrial samples. The stationary sample method with polychromatic X-rays is advantageous because the irradiated area of the sample is always same and fixed, meaning that all diffraction spots occur from the same area of the sample, however, unit cell parameters cannot be directly obtained by this method though they are very important for identification of mineral and for determination of crystal structures. In order to obtain the cell parameters even in the case of the sample stationary method, we apply energy scanning of a micro-beam of monochromatic SR at SPring-8.

Hagiya, Kenji↗

Curved Diffractive X-ray Optics for X-ray Astronomy

We report on a concept for curved diffractive X-ray optics (CDXO). CDXO would enable potential new optical designs for X-ray instruments, such as a two element spectrometer, in which the secondary element of an X-ray mirror pair is patterned with an X-ray grating. A two-element spectrometer design eliminates the grating assembly, resulting in decreased instrument mass and reduced power requirements. In addition, a two-element spectrometer may realize cost/schedule savings by eliminating a separate grating alignment effort, and yield increased effective area over three element designs. We present a raytrace concept study of a two-element spectrometer compact enough to fit within a sounding rocket payload. We also review the progress made in electron-beam lithography (EBL) techniques that would enable curved diffractive X-ray optics to be patterned, and outline a procedure by which the accuracy of the EBL patterning process can be measured interferometrically.

Casey T. DeRoo↗

Materials Characterization Using X-Ray Diffraction

This talk for the Spring Meeting of the Ohio Section of the American Association of Physics Teachers begins with a brief description of what X-Ray diffraction is, and relates 2D diffraction (grating equation) to 3D (Bragg’s law). Various examples of how XRD can be used to answer a variety of materials science questions will be discussed along with some of how XRD has been used at NASA Glenn.

Laura Wilson↗

Valence Electron Distributions from Sub-Angstrom Convergent Beam Electron Diffraction

Modern aberration-corrected scanning transmission electron microscopes can acquire four-dimensional data sets (“4D STEM”) by recording convergent beam electron diffraction (CBED) patterns, using precisely positioned, sub-angstrom probes. Here, we demonstrate that these patterns can probe the site symmetry, atomic displacements, and valence electron distributions at individual atomic columns. To this end, 4D STEM CBED patterns were acquired from SrTiO 3 single crystals and compared with patterns calculated using scattering potentials derived from density functional theory. Here, we show that an aspherical valence electron charge build-up at the oxygen sites causes intensity asymmetries in the low-angle scattering portion of the patterns. Using strained SrTiO 3 films containing subtle polar displacements within nanometer-sized domains, it is shown that the high-angle scattering portion in each pattern is sensitive to atomic displacements.

36 MATERIALS SCIENCE↗