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At least 19 records

Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements

Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here, in this paper, a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focused ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Lastly, our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.

36 MATERIALS SCIENCE↗

Stationary Bragg reflection of laser light in inhomogeneous absorbing plasmas inside inertial confinement fusion Hohlraums

Laser-produced plasma in inertial confinement fusion (ICF) Hohlraums are marked with density non-uniformity whose length scale can go down to micrometers. This scale is of the order of the laser wavelength. The WKB approximation, which is classically used in radiation-hydrodynamic codes to compute the laser trajectory, cannot correctly take into account such small-scale inhomogeneity of the plasma. Going beyond this approximation, we predict a novel mechanism for the laser reflection. Here we show that an electromagnetic plane wave with wave number k resonates with the k B =2 k Fourier component of a multimode perturbation of the background density and generates a reflected wave. It is the first time that this reflection is considered for stationary inhomogeneous ICF plasmas, and the energy absorption is taken into account. This mechanism, which is a form of Bragg reflection, can occur away from the critical surface and generate a drift of the location of the laser absorption. Furthermore, this absorption will be periodically modulated with a k B wave number. The stationary Bragg reflection can explain ongoing discrepancies between experimental and numerical data about laser trajectory and absorption in ICF Hohlraums.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

High Bragg reflectivity of diamond crystals exposed to multi-kW mm –2 X-ray beams

X-ray free-electron lasers in the oscillator configuration (XFELO) are future fully coherent hard X-rays sources with ultrahigh spectral purity. X-ray beams circulate in an XFELO optical cavity comprising diamond single crystals. They function as high-reflectance (close to 100%), narrowband (~10 meV) Bragg backscattering mirrors. The average power density of the X-ray beams in the XFELO cavity is predicted to be as high as ~10 kW mm –2 . Therefore, XFELO feasibility relies on the ability of diamond crystals to withstand such a high radiation load and preserve their high reflectivity. Here the endurance of diamond crystals to irradiation with multi-kW mm –2 power density X-ray beams is studied. It is shown that the high Bragg reflectivity of the diamond crystals is preserved after the irradiation, provided it is performed at ~1 × 10 –8 Torr high-vacuum conditions. In conclusion, irradiation under 4 × 10 –6 Torr results in a ~1 meV shift of the Bragg peak, which corresponds to a relative lattice distortion of 4 × 10 –8 , while the high Bragg reflectivity stays intact.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Holographic reflective Bragg gratings of gain and their role in the operation of high-power pulsed lasers

The influence of reflective Bragg gratings that are formed in an active medium due to the spatial periodic modulation of gain on the spectral properties of lasing are investigated by an example of a pulsed Nd : YAG laser. It is shown that, at a certain choice of the formation regime of reflective gratings of gain, the lasing bandwidth can be reduced by a factor of 3 – 5, with a corresponding increase in the pulse energy and significant improvement of spatial beam quality. (paper)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Oblique diffraction geometry for the observation of several non-coplanar Bragg reflections under identical illumination

A method to determine the strain tensor and local lattice rotation with dark-field X-ray microscopy is presented. Using a set of at least three non-coplanar symmetry-equivalent Bragg reflections, the illuminated volume of the sample can be kept constant for all reflections, facilitating easy registration of the measured lattice variations. This requires an oblique diffraction geometry,i.e.the diffraction plane is neither horizontal nor vertical. We derive a closed analytical expression that allows determination of the strain and lattice rotation from the deviation of experimental observables (e.g.goniometer angles) from their nominal values for an unstrained lattice.

Chemistry↗

Three-dimensional strain imaging of irradiated chromium using multi-reflection Bragg coherent diffraction

Abstract Radiation-induced materials degradation is a key concern in limiting the performance of nuclear materials. The formation of nanoscale void and gas bubble superlattices in metals and alloys under radiation environments can effectively mitigate radiation-induced damage, such as swelling and aid the development of next generation radiation tolerant materials. To effectively manage radiation-induced damage via superlattice formation, it is critical to understand the microstructural changes and strain induced by such superlattices. We utilize multi-reflection Bragg coherent diffraction imaging to quantify the full strain tensor induced by void superlattices in iron irradiated chromium substrate. Our approach provides a quantitative estimation of radiation-induced three-dimensional (3D) strain generated at the microscopic level and predicts the number density of defects with a high degree of sensitivity. Such quantitative evaluation of 3D strain in nuclear materials can have a major impact on predicting materials behavior in radiation environments and can revolutionize design of radiation tolerant materials.

36 MATERIALS SCIENCE↗

Electronic Melting of Silicon in Nanostructures using X-ray Forbidden Bragg Reflections

Abstract We carried out a short beamtime at the Pohang Accelerator Laboratory x-ray Free Electron Laser to perform a pump-probe (PP) laser excitation diffraction experiment on the silicon (222) forbidden Bragg peak. To limit the x-ray penetration, we used a “device layer” silicon film wafer bonded to a silicon substrate. The sample, specially fabricated by MEMC Electronic Materials, had a Si(100) substrate bonded to a 170 nm Si(100) film rotated at 45° for crystallographic isolation. A second sample was reactive-ion-etched down to 52 nm thickness. In the silicon lattice, the covalent bonds are seen exclusively at the 222 reflection. Upon laser excitation, these electrons are expected to be excited to the valence band on femtosecond electronic time scales. The Si(222) reflection is therefore expected to be extinguished on this fast time scale, while the electron–phonon coupled acoustic response is determined by the lattice dynamics. The latter is determined by the speed of sound over the device thickness, which is in the mid-picosecond range.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Simultaneous Multi-Bragg Peak Coherent X-ray Diffraction Imaging

The simultaneous measurement of two Bragg reflections by Bragg coherent X-ray diffraction is demonstrated on a twinned Au crystal, which was prepared by the solid-state dewetting of a 30 nm thin gold film on a sapphire substrate. The crystal was oriented on a goniometer so that two lattice planes fulfill the Bragg condition at the same time. The Au 111 and Au 200 Bragg peaks were measured simultaneously by scanning the energy of the incident X-ray beam and recording the diffraction patterns with two two-dimensional detectors. While the former Bragg reflection is not sensitive to the twin boundary, which is oriented parallel to the crystal–substrate interface, the latter reflection is only sensitive to one part of the crystal. The volume ratio between the two parts of the twinned crystal is about 1:9, which is also confirmed by Laue microdiffraction of the same crystal. The parallel measurement of multiple Bragg reflections is essential for future in situ and operando studies, which are so far limited to either a single Bragg reflection or several in series, to facilitate the precise monitoring of both the strain field and defects during the application of external stimuli.

47 OTHER INSTRUMENTATION↗

Narrow-band fibre reflector based on a fibre Bragg grating reflection interferometer

Narrow-band filtering in reflected light using a reflection interferometer with a fibre Bragg grating (FBG) as its back mirror is demonstrated for the first time. The reflection interferometer is made in SMF-28e single-mode fibre, and the faces of its front mirror, which includes a thin metallic film, differ in reflectance. The reflection bandwidth of a test sample is 0.5 pm (62 MHz) at a wavelength of 1556 nm (Q-factor of 3 × 10{sup 6}), its maximum reflectance is 0.21, and its contrast is 10{sup 2}. The use of a narrow-band FBG instead of thin-film broadband mirrors allows spectral selection to be significantly improved owing to an increase in the length of the interferometer base. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Quartz conditioning crystal for X-ray rocking curve topography

A large α-quartz crystal designed to condition the monochromatic beam at beamline 1-BM of the Advanced Photon Source is presented. The purpose of this crystal was to provide a precise match to the Bragg angle of quartz crystals that are commonly used to make analyzers for plasma diagnostics. In order to characterize these analyzers, area detectors need to be positioned at distances from the analyzer at upwards of 1000 mm. As a result of this precise matching, a Bragg-reflected beam from such an analyzer is precisely parallel to the beam incident on the conditioning crystal. This situation alleviates the need to adjust the position of the area detector as the distance between the analyzer and the area detector is varied. That is, there is no need to account for vertical displacement of the diffracted-beam image as a function of this distance. Additionally, verification that the analyzer is set to the correct Bragg reflection is obtained by scanning this distance, because only for a spurious reflection will there be a vertical displacement. This is a very useful check. To commission the conditioning crystal, diffraction from a high-quality flat quartz crystal was mapped using a CCD. Bragg diffraction from the 40$\bar{40}$ reflection at 8.5 keV was studied over an area of 23 × 31 mm. The theoretical Darwin width of the flat sample in this case was 4.7 µrad. An FWHM value near 6 µrad was measured over almost the entire mapped area. These data demonstrate that the resolution function for this four-crystal arrangement is ~4 µrad. Data are also presented for a 0.1 mm-thick α-quartz wafer pressed into a concave form, having a nominal radius of 500 mm and intended for use as an analyzer. Because analyzers are bent crystals, diffraction occurs in narrow bands. When a multiple exposure is made as a function of rocking angle a striped pattern is obtained, which is commonly referred to as a zebra-stripe pattern. A series of zebra stripes from the 30$\bar{33}$ Bragg reflection of the bent wafer over its 25 mm-diameter area were recorded on a CCD. The zebra-stripe pattern was analyzed to show a uniform bending to a radius of 497.0 ± 0.3 mm, in support of the nominal value. An r.m.s. slope error of 7 µrad was also obtained from this analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Correct interpretation of diffraction properties of quartz crystals for X-ray optics applications

Quartz has hundreds of strong Bragg reflections that may offer a great number of choices for making fixed-angle X-ray analyzers and polarizers at virtually any hard X-ray energies with selectable resolution. However, quartz crystals, unlike silicon and germanium, are chiral and may thus appear in two different forms of handedness that are mirror images. Furthermore, because of the threefold rotational symmetry along the c axis, the { h 1 h 2 h 3 L } and { h 2 h 1 h 3 L } Bragg reflections may have quite different Darwin bandwidth, reflectivity and angular acceptance, although they have the same Bragg angle. The design of X-ray optics from quartz crystals therefore requires unambiguous determination of the orientation, handedness and polarity of the crystals. The Laue method and single-axis diffraction technique can provide such information, but the variety of conventions used in the literature to describe quartz structures has caused widespread confusion. The current studies give detailed guidelines for design and fabrication of quartz X-ray optics, with special emphasis on the correct interpretation of Laue patterns in terms of the crystallography and diffraction properties of quartz. Furthermore, the quartz crystals examined were confirmed by X-ray topography to have acceptably low densities of dislocations and other defects, which is the foundation for developing high-resolution quartz-based X-ray optics.

36 MATERIALS SCIENCE↗

K-space algorithmic reconstruction (KAREN): a robust statistical methodology to separate Bragg and diffuse scattering

Diffuse scattering occurring in the Bragg diffraction pattern of a long-range-ordered structure represents local deviation from the governing regular lattice. However, interpreting the real-space structure from the diffraction pattern presents a significant challenge because of the dramatic difference in intensity between the Bragg and diffuse components of the total scattering function. In contrast to the sharp Bragg diffraction, the diffuse signal has generally been considered to be a weak expansive or continuous background signal. In this paper, using 1D and 2D models, it is demonstrated that diffuse scattering in fact consists of a complex array of high-frequency features that must not be averaged into a low-frequency background signal. To evaluate the actual diffuse scattering effectively, an algorithm has been developed that uses robust statistics and traditional signal processing techniques to identify Bragg peaks as signal outliers which can be removed from the overall scattering data and then replaced by statistically valid fill values. This method, described as a 'K-space algorithmic reconstruction' (KAREN), can identify Bragg reflections independent of prior knowledge of a system's unit cell. KAREN does not alter any data other than that in the immediate vicinity of the Bragg reflections, and reconstructs the diffuse component surrounding the Bragg peaks without introducing discontinuities which induce Fourier ripples or artifacts from underfilling `punched' voids. The KAREN algorithm for reconstructing diffuse scattering provides demonstrably better resolution than can be obtained from previously described punch-and-fill methods. The superior structural resolution obtained using the KAREN method is demonstrated by evaluating the complex ordered diffuse scattering observed from the neutron diffraction of a single plastic crystal of CBr 4 using pair distribution function analysis.

36 MATERIALS SCIENCE↗

Combining Laue diffraction with Bragg coherent diffraction imaging at 34-ID-C

Measurement modalities in Bragg coherent diffraction imaging (BCDI) rely on finding a signal from a single nanoscale crystal object which satisfies the Bragg condition among a large number of arbitrarily oriented nanocrystals. However, even when the signal from a single Bragg reflection with ( hkl ) Miller indices is found, the crystallographic axes on the retrieved three-dimensional (3D) image of the crystal remain unknown, and thus localizing in reciprocal space other Bragg reflections becomes time-consuming or requires good knowledge of the orientation of the crystal. Here, the commissioning of a movable double-bounce Si (111) monochromator at the 34-ID-C endstation of the Advanced Photon Source is reported, which aims at delivering multi-reflection BCDI as a standard tool in a single beamline instrument. The new instrument enables, through rapid switching from monochromatic to broadband (pink) beam, the use of Laue diffraction to determine crystal orientation. With a proper orientation matrix determined for the lattice, one can measure coherent diffraction patterns near multiple Bragg peaks, thus providing sufficient information to image the full strain tensor in 3D. The design, concept of operation, the developed procedures for indexing Laue patterns, and automated measuring of Bragg coherent diffraction data from multiple reflections of the same nanocrystal are discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Measurement and Interpretation of Diffuse Scattering in X-Ray Diffraction for Macromolecular Crystallography

X-ray diffraction from macromolecular crystals includes both sharply peaked Bragg reflections and diffuse intensity between the peaks. The information in Bragg scattering reflects the mean electron density in the unit cells of the crystal. The diffuse scattering arises from correlations in the variations of electron density that may occur from one unit cell to another, and therefore contains information about collective motions in proteins.

59 BASIC BIOLOGICAL SCIENCES↗

Graded Buffer Bragg Reflectors with High Reflectivity and Transparency for Metamorphic Optoelectronics

A graded buffer Bragg reflector (GBBR) is a bifunctional device component that provides the reflection of a distributed Bragg reflector and the adjustable lattice constant of a compositionally graded buffer. Prior work showed that these properties can be combined with low threading dislocation density and high reflectivity. Here, we design and demonstrate complex GBBRs for specific metamorphic solar cell applications. We design buffers that provide (1) high reflectivity over a narrow bandwidth, for quantum well solar cells, (2) reflectivity over a wide bandwidth, for optically thin solar cells, and (3) low sidelobe reflection, for multijunction devices that demand low out-of-band reflection. Apodized and triple GBBRs are demonstrated, and transparency is always considered, requiring designs with carefully engineered material combinations. A GBBR with a reflection of 99% is demonstrated, as well as a triple GBBR that has over 80% reflection for 100?nm of the spectrum around 800?nm. We also analyze potential deviations in a baseline GBBR from that of a perfect DBR using transmission electron microscopy to analyze imperfections in the material and modeling to analyze the impact of imperfect refractive index data for lattice-mismatched AlGaInAs. Minimal crosshatch roughness and unintentional thickness variation occur throughout the buffer, which likely influences reflection slightly. Small deviations between the calculated AlGaInAs and utilized AlGaAs refractive index exist, giving methods for future GBBR improvement. While the GBBR designs are intended for metamorphic solar cells, the broad and high reflection may also be useful for other optoelectronic devices such as light-emitting diodes or lasers.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Structural Peculiarities of the Intermediate Phase in Zr-Rich Lead Zirconate Titanate

This paper presents the results of X-ray diffraction studies on a single crystal of lead zirconate titanate PbZr{sub 0.993}Ti{sub 0.007}O{sub 3} in the region of existence of an intermediate ferroelectric phase. In addition to the known superstructure reflections of the M type q{sub M} = {(1/2),(1/2),0} and the first-order satellite reflections q{sub M} + {δ, δ, δ}, unknown second-order satellites have been observed near q{sub M} and near the Bragg reflections. Structural model of regular system of antiphase domains is used for diffraction calculation. The model is shown to describe the first- and second-orders satellite reflections in the vicinity of q{sub M}, but it cannot explain the appearance of satellites around the main Bragg peaks. A possible origin of the system of the superstructures observed in the intermediate phase is discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

X-ray optics for the cavity-based X-ray free-electron laser

A cavity-based X-ray free-electron laser (CBXFEL) is a possible future direction in the development of fully coherent X-ray sources. CBXFELs consist of a low-emittance electron source, a magnet system with several undulators and chicanes, and an X-ray cavity. The X-ray cavity stores and circulates X-ray pulses for repeated FEL interactions with electron pulses until the FEL reaches saturation. CBXFEL cavities require low-loss wavefront-preserving optical components: near-100%-reflectivity X-ray diamond Bragg-reflecting crystals, outcoupling devices such as thin diamond membranes or X-ray gratings, and aberration-free focusing elements. In the framework of the collaborative CBXFEL research and development project of Argonne National Laboratory, SLAC National Accelerator Laboratory and SPring-8, we report here the design, manufacturing and characterization of X-ray optical components for the CBXFEL cavity, which include high-reflectivity diamond crystal mirrors, a diamond drumhead crystal with thin membranes, beryllium refractive lenses and channel-cut Si monochromators. All the designed optical components have been fully characterized at the Advanced Photon Source to demonstrate their suitability for the CBXFEL cavity application.

47 OTHER INSTRUMENTATION↗

Optical Anisotropy of Photonic Crystals of Cubic Symmetry Induced by Multiple Diffraction of Light

The optical spectra of Bragg reflection from opal-like photonic crystals under conditions of the resonant enhancement of the multiple diffraction of light have been studied experimentally and theoretically using the photonic crystal structures prepared of monodisperse polystyrene globules. It is shown that the reflection signal registered in mutually orthogonal configurations of the polarizer and analyzer is related to the intrinsic optical anisotropy of the crystals and is a specific manifestation of the multiple Bragg diffraction in three-dimensional photonic crystals.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗