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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Wavefront Preservation in Soft X-Ray Beamlines for the Advanced Light Source Upgrade

In the 4th generation of X-ray light sources, including Free-Electron Lasers (FEL) and Diffraction-Limited Storage Rings (DLSR), the emittance of the electron beam is small or negligible compared to the emittance of the photon beam produced by insertion devices, thus generating coherent beams of light. Over the next few years, several lightsource facilities will be built or upgraded to produce X-ray beams of unprecedented coherent flux. Delivering these exceptional beams to the sample chambers requires beamline optical systems that are designed to preserve the wavefront properties. Our goal in the Advanced Light Source upgrade project (ALS-U) is to create a new class of beamlines that reach diffraction-limited X-ray optical quality through tightly integrated, efficient optical systems, diagnostics, and adaptive mirrors, thus providing users with new scientific capabilities offered by coherent X-ray light interactions with matter. Herein we describe aspects of the beamlines’ design as they enter the project’s final design phase.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS1995

Laser Light Scattering by Shock Waves

Scattering of coherent light as it propagates parallel to a shock wave, formed in front of a bluff cylindrical body placed in a supersonic stream, is studied experimentally and numerically. Two incident optical fields are considered. First, a large diameter collimated beam is allowed to pass through the shock containing flow. The light intensity distribution in the resultant shadowgraph image, measured by a low light CCD camera, shows well-defined fringes upstream and downstream of the shadow cast by the shock. In the second situation, a narrow laser beam is brought to a grazing incidence on the shock and the scattered light, which appears as a diverging sheet from the point of interaction, is visualized and measured on a screen placed normal to the laser path. Experiments are conducted on shocks formed at various free-stream Mach numbers, M, and total pressures, P(sub 0). It is found that the widths of the shock shadows in a shadowgraph image become independent of M and P(sub 0) when plotted against the jump in the refractive index, (Delta)n, created across the shock. The total scattered light measured from the narrow laser beam and shock interaction also follows the same trend. In the numerical part of the study, the shock is assumed to be a 'phase object', which introduces phase difference between the upstream and downstream propagating parts of the light disturbances. For a given shape and (Delta)n of the bow shock the phase and amplitude modulations are first calculated by ray tracing. The wave front is then propagated to the screen using the Fresnet diffraction equation. The calculated intensity distribution, for both of the incident optical fields, shows good agreement with the experimental data.

Panda, J.↗
DOE OSTI2018

Nd3+ Doping effect on the optical and electrical properties of SnO2 thin films prepared by nebulizer spray pyrolysis for opto-electronic application

Highlights: • High quality, Nd:SnO{sub 2} thin films prepared using simple nebulizer spray pyrolysis technique. • Characterizations of the films confirmed good crystallinity and smooth surface morphology. • High optical transparency with low electrical resistivity in nebulizer spray pyrolysis prepared Nd: SnO{sub 2} thin films is presented. - Abstract: Neodymium doped tin oxide (Nd: SnO{sub 2}) thin films were deposited on heated glass substrates with different Nd concentrations (0, 2, 4 and 6 %) by nebulizer spray pyrolysis method. Effects of Nd doping on structural, optical and electrical properties of the prepared films were investigated. X-ray diffraction study confirmed that all the deposited Nd: SnO{sub 2} films are in polycrystalline tetragonal structure with (211) preferential orientation. FESEM images showed that the prepared SnO{sub 2} particles are in nano-size in spherical shape, completely covering the substrate. AFM topology showed smooth deposition of the films with minimum surface roughness. The films showed maximum optical transmittance 90 % in the visible region with a band gap value 3.67 eV, also showed low refractive index and extinction coefficients. Room temperature photoluminescence (PL) spectrum exhibited a strong UV emission peak at 356 nm for all the films. All the Nd: SnO{sub 2} films displayed n-type conductivity with low electrical resistivity 5.88 × 10{sup −4} (Ω cm) for 4 % Nd doping. As the films showed good figure of merit (ϕ) values, these Nd doped SnO{sub 2} thin films can perform better role in optoelectronic device.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Investigation of gamma-ray irradiation induced phase change from NiO to Ni 2 O 3 for enhancing photocatalytic performance

An Irradiated nickel oxide (NiO) thin film was deposited onto glass substrates at 723 K by the spray pyrolysis using nickel chloride as precursors. The obtained films were irradiated by gamma-radiation doses varying from 180 Gy to 10 kGy. The structure and optical properties of the samples were examined by X-ray diffraction, UV-vis spectrometer and photoluminescence measurement. Un-irradiated and irradiated NiO thin films have a cubic structure with the same preferred orientation along the plane (111). XRD investigation shows that, the intensity of preferred orientation and crystallite size depend on gamma-radiation dose. For a study of the dose effect, it is very important to optimize the precursor concentration. With a concentration of 5.10(-2) M precursor NiCl 2 and a dose of 10 kGy, we obtain a thin film of Ni 2 O 3 . With a 10 kGy dose we obtain a new dominant phase, Ni 2 O 3 , which induced an activation of the visible range under the effect of gamma rays. This improved the photocatalytic performance under gamma rays treatment. Moreover, the PL quenching effect shows an improvement of photocatalytic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Soft X-ray flat-field VLS spectrographs

We have analysed the capabilities of flat-field spectrometers with concave VLS reflection gratings from the standpoint of spectral imaging in the soft X-ray range. Two types of such instruments are shown to exist: spectrographs with as flat as possible a portion of the focal surface (of Harada spectrograph type) and those with a nearly constant distance from the grating centre to the focal surface, which permits reaching a high spatial resolution with the use of a crossed focusing mirror (without a loss in spectral resolution). Three 0.25, 0.5, and 1.5-m long spectrographs of Harada type were calculated for operation in the ranges 90 – 250, 50 – 200, and 20−110 A-ring , respectively. We show that each of the calculated instruments may be converted to an instrument of the second type for operation in the second and fourth diffraction orders without significant changes in scheme geometry. In this case, the theoretical spatial resolution is equal to ∼10 μm throughout the optimisation range. (x-ray optics)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Atomic Structure, Dynamics, Changes in Chemical Bonding and Semiconductor-Metal Transition in Sb 2 Se 3 : A Remarkable Material for Quantum Networks and Energy Applications

Antimony sesquiselenide has become an outstanding functional material for photovoltaics, energy storage and transformation, memory and photonic applications. Sb 2 Se 3 is one of the most successful emerging solar light absorbers and has also been identified as a highly promising ultralow-loss phase-change material (PCM) for next-generation coherent nanophotonic processors, photonic tensor cores, quantum and neuromorphic networks. Unlike benchmark telluride PCMs, Sb 2 Se 3 features a quasi-one-dimensional (1D) crystalline structure consisting of (Sb 4 Se 6 ) ∞ ribbons, lacks the typical PCM chemical bonding, and undergoes an extended semiconductor-metal transition above the melting point. Consequently, the origin of high optical contrast between crystalline (SET) and amorphous (RESET) logic states remains elusive and presents a significant challenge. Using high-energy X-ray diffraction and Raman spectroscopy over a wide temperature range, supported by first-principles simulations and complemented by thermal, optical and electrical measurements, as well as by 121 Sb-Mossbauer spectroscopy, the quasi-1D network of orthorhombic antimony sesquiselenide was found to undergo significant evolution in amorphous and supercooled Sb 2 Se 3 , leading to lower coordination, shorter interatomic distances and a higher p-electron density on antimony, indicating changes in chemical bonding. The observed novel Sb 2 Se 3 nanocrystalline polymorph, characterized by trigonal antimony coordination and more isolated Sb-Se ribbons, could help reduce multiple trapping defect states in the bandgap, which are typical of orthorhombic Sb 2 Se 3 , thereby enhancing the power-conversion efficiency of photovoltaic devices. Semimetallic and metallic liquid Sb 2 Se 3 exhibit a gradual transformation into a denser 2D and/or 3D network with higher antimony coordination. Localized electron states in the pseudogap are becoming extended, leading to an increase in electronic conductivity σ following the relationship σ ∝ N(E F ) 2 . Liquid Sb 2 Se 3 also appears to be strongly fragile, with a nonmonotonic change in viscosity and higher atomic mobility in the metallic liquid. Furthermore, these results explain extraordinary functionalities of Sb 2 Se 3 for photonic and energy applications.

antimony↗
DOE OSTI2015

Synthesis and photocatlytic performance of nano-sized TiO{sub 2} materials prepared by dealloying Ti–Cu–Pd amorphous alloys

Highlights: • TiO{sub 2} nanospindles were synthesized by dealloying Ti–Cu–Pd amorphous alloy. • Pd significantly enhanced the exposure of high-energy (0 0 1) facet of TiO{sub 2}. • TiO{sub 2} with high-energy (0 0 1) facet showed good photocatalytic activity. - Abstract: TiO{sub 2} nanospindles with exposed (0 0 1) facet were synthesized through a simple dealloying reaction. The rutile photocatalysts were characterized by X-ray diffraction, scanning electron microscope and transmission electron microscope, inductively coupled plasma optical emission spectrometry and ultraviolet–visible spectrophotometer. A Rhodamine B dye (RhB) was used to detect the photocatalytic activity of TiO{sub 2} under full light irradiation. The presence of Pd in the original amorphous alloy reduced the surface free energy of TiO{sub 2}, stabilized the (0 0 1) facet. The Pd8-TiO{sub 2} sample exhibited the largest crystal size along the direction which is perpendicular to the (0 0 1) facet. The photocatalytic degradation rate of RhB was improved due to the Pd addition in the original amorphous alloy. This indicated that the exposure of (0 0 1) facets could enhance the activity of TiO{sub 2} photocatalyst. In addition, the presence of isolated Pd atoms on the surface of TiO{sub 2} would be another probable reason for the improvement of photocatalytic activity.

36 MATERIALS SCIENCE↗
NASA NTRS1999

Rectangular Relief Diffraction Gratings for Coherent Lidar Beam Deflection

LIDAR systems require a light transmitting system for sending a laser light pulse into space and a receiving system for collecting the retro-scattered light, separating it from the outgoing beam and analyzing the received signal for calculating wind velocities. Currently, a shuttle manifested coherent LIDAR experiment called SPARCLE (SPAce Readiness Coherent Lidar Experiment) includes a silicon wedge (or prism) in its design in order to deflect the outgoing beam 30 degrees relative to the incident direction. The intent of this paper is to present two optical design approaches that may enable the replacement of the optical wedge component (in future, larger aperture, post-SPARCLE missions) with a surface relief transmission diffraction grating. Such a grating could be etched into a lightweight, flat, fused quartz substrate. The potential advantages of a diffractive beam deflector include reduced weight, reduced power requirements for the driving scanning motor, reduced optical sensitivity to thermal gradients, and increased dynamic stability.

Cole, H. J.↗
DOE OSTI2015

Controlled synthesis and magnetic properties of monodispersed ceria nanoparticles

In the present study, monodispersed CeO{sub 2} nanoparticles (NPs) of size 8.5 ± 1.0, 11.4 ± 1.0 and 15.4 ± 1.0 nm were synthesized using the sol-gel method. Size-dependent structural, optical and magnetic properties of as-prepared samples were investigated by X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), high resolution transmission electron microscopy (HR-TEM), ultra-violet visible (UV-VIS) spectroscopy, Raman spectroscopy and vibrating sample magnetometer (VSM) measurements. The value of optical band gap is calculated for each particle size. The decrease in the value of optical band gap with increase of particle size may be attributed to the quantum confinement, which causes to produce localized states created by the oxygen vacancies due to the conversion of Ce{sup 4+} into Ce{sup 3+} at higher calcination temperature. The Raman spectra showed a peak at ∼461 cm{sup -1} for the particle size 8.5 nm, which is attributed to the 1LO phonon mode. The shift in the Raman peak could be due to lattice strain developed due to variation in particle size. Weak ferromagnetism at room temperature is observed for each particle size. The values of saturation magnetization (Ms), coercivity (Hc) and retentivity (Mr) are increased with increase of particle size. The increase of Ms and Mr for larger particle size may be explained by increase of density of oxygen vacancies at higher calcination temperature. The latter causes high concentrations of Ce{sup 3+} ions activate more coupling between the individual magnetic moments of the Ce ions, leading to an increase of Ms value with the particle size. Moreover, the oxygen vacancies may also produce magnetic moment by polarizing spins of f electrons of cerium (Ce) ions located around oxygen vacancies, which causes ferromagnetism in pure CeO{sub 2} samples.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Measuring the Burgers vector of dislocations with dark-field X-ray microscopy

The subsurface dynamics of dislocations are essential to many properties of bulk crystalline materials. However, it is challenging to characterize a bulk crystal by conventional transmission electron microscopy (TEM) due to the limited penetration depth of electrons. A novel X-ray imaging technique – dark-field X-ray microscopy (DFXM) – was developed to image hierarchical dislocation structures in bulk crystals. While today's DFXM can effectively map the line structures of dislocations, it is still challenging to quantify the Burgers vectors, the key characterization governing the dislocation behaviors. Here, we extend the 'invisibility criterion' formalism from the TEM theory to the geometrical-optics model of DFXM and demonstrate the consistency between DFXM and dark-field TEM using multi-diffraction-peak imaging for a single edge dislocation. Due to the practical difficulty of multi-peak DFXM experiments, we further study how the Burgers vector effect is encoded for a single-peak DFXM experiment. Using the geometrical-optics DFXM simulation, we explore the asymmetry of rocking tilt scans at different rolling tilts and develop a new method to characterize the Burgers vector. The conclusions of this study advance our understanding of the use of DFXM in characterizing individual dislocations, enabling the connection from bulk DFXM imaging to dislocation mechanics.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Intense Reactivity in Sulfur–Hydrogen Mixtures at High Pressure under X-ray Irradiation

Superconductivity near room temperature in the sulfur–hydrogen system arises from a sequence of reactions at high pressures, with X-ray diffraction experiments playing a central role in understanding these chemical–structural transformations and the corresponding S:H stoichiometry. Here we document X-ray irradiation acting as both a probe and as a driver of chemical reaction in this dense hydride system. We observe a reaction between molecular hydrogen (H 2 ) and elemental sulfur (S 8 ) under high pressure, induced directly by X-ray illumination, at photon energies of 12 keV using a free electron laser. The rapid synthesis of hydrogen sulfide (H 2 S) at 0.3 GPa was confirmed by optical observations, spectroscopic measurements, and microstructural changes detected by X-ray diffraction. These results document X-ray induced chemical synthesis of superconductor-forming dense hydrides, revealing an alternative production strategy and confirming the disruptive nature of X-ray exposure in studies on high-pressure hydrogen chalcogenides, from water to high-temperature superconductors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Growth mechanism of Cobalt(II) Phthalocyanine(CoPc) thin films on SiO{sub 2} and muscovite substrates

Thin films of Cobalt(II) Phthalocyanine (CoPc) were grown by thermal evaporation technique on two different substrates namely SiO{sub 2} and atomically cleaned muscovite mica(001) at various substrate temperatures. Deposition rate has been maintained to 0.3Å/sec during the growth of the films. The growth process is studied by means of atomic force microscopy (AFM). Films on SiO{sub 2} exhibit only three-dimensional islands and uniformity of these islands improved with substrate temperatures, whereas films on mica (001) consist of long oriented percolated structures. The results revealed that the growth mechanism of CoPc strongly depends on substrate temperatures as well as nature of substrate used. Optical properties were characterized by UV-Visible spectroscopy and structural properties were studied using X-ray diffraction.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Laser and optical transport line for laser-based ion beam diagnostics and control in the SNS linear accelerator

We report our recent upgrade of the laser and optical transport line for the laser-based ion beam diagnostics (laser wire) system at the linear accelerator (linac) of the Spallation Neutron Source (SNS). A new light source based on diodepumped solid-state laser amplifiers has been developed to provide near diffraction-limited laser beam with a variety of pulse structures. The free-space optical transport line has been modified to include image relay optics with remote control, which greatly improved the laser beam quality and position stability at individual measurement stations. The upgraded system enables novel beam diagnostics/control capabilities including longitudinal profile measurement and high-energy proton beam extraction from the SNS linac.

Liu, Yun↗
NASA NTRS2007

[Overview of the GSFC Effort to Build Microwave Detectors for CMB Polarization]

Filled arrays of bolometers are currently being employed for use in astronomy from the far-infrared through millimeter portion of the electromagnetic spectrum. Because of the large range of wavelengths for which such detectors are applicable, the size of a pixel (p) relative to the wavelength (lambda) will vary according to the specific application of a given available technology. As the pixel size becomes comparable to a wavelength of the absorbed radiation, correlations in the radiation field at the pixel can affect the imaging properties of the system independent of the correlations introduced by the front-end optics. We study the dependence of image fidelity and induced polarization on the size of the pixel by employing a formalism in which diffraction due to the pixel boundary is treated by propagating the second-order statistical correlations of the radiation field through a model optical system. We construct simulated polarized images of square pixels for various ratios of p lambda. For the limit in which few modes are supported by the pixel (p lambda lesssiml), we find that the diffraction due to the pixel edges is non-negligible and hence must be considered along with the telescope diffraction pattern in modeling the ultimate spatial resolution of an imaging system. For the case in which the pixel is over-moded (p lambda ggl), the geometric limit is approached as expected. This technique provides a quantitative approach to understand and optimize the imaging properties of planar detectors in the few-mode limit.

Chuss, David↗
DOE OSTI2016

Structural and optical properties of nano-structured CdS thin films prepared by chemical bath deposition

Cadmium sulfide (CdS) thin films have been deposited on conducting glass substrates by chemical bath deposition (CBD) technique. The effect of precursor concentration on the structural, morphological, compositional, and optical properties of the CdS films has been studied. Crystal structure of these CdS films is characterized by X-ray diffraction (XRD) and it reveals polycrystalline structure with mixture of cubic and wurtzite phases with grain size decreasing as precursor concentration is increased. Optical studies reveal that the CdS thin films have high transmittance in visible spectral region reaching 90% and the films possess direct optical band gap that decreases from 2.46 to 2.39 eV with decreasing bath concentration. Our study suggests that growth is nucleation controlled.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi, Sn): High Chemical Flexibility Resulting in Good Nonlinear-Optical Properties

Seven acentric sulfides Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi, Sn) were grown by a high-temperature salt flux method. The crystal structures of the Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi, Sn) compounds were determined by single-crystal X-ray diffraction with the aid of solid-state NMR spectroscopy. The Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi) compounds are isostructural and crystallize in the Ba 6 Ag 4 Sn 4 S 16 structure type. The Sn-containing compound exhibits high structural similarity to Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi) with the presence of an interstitial atomic position partially occupied by Sn atoms. The chemical bonding characteristics of Ba 6 (Cu 2.9 Sn 0.4 )Sn 4 S 16 were understood with electron localization function calculations coupled with crystal orbital Hamilton population calculations. The Ba–S and Cu–S interactions are dominantly ionic, but the Sn–S interactions consist of strong covalent bonding characteristics in Ba 6 (Cu 2.9 Sn 0.4 )Sn 4 S 16 . The monovalent Cu atoms, mixed with certain metals with various oxidation states, significantly shift the optical properties of the Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi) compounds. This results in a good balance between the second-harmonic-generation (SHG) response and laser damage threshold (LDT). Ba 6 (Cu 1.9 Zn 1.1 )Sn 4 S 16 possesses a high SHG response and a high LDT of 2.8 × AGS and 3 × AGS, respectively. Here, a density functional theory calculation revealed that CuS 4 and SnS 4 tetrahedra significantly contribute to the SHG response in Ba 6 (Cu 2 Mg)Sn 4 S 16 , which also confirmed that CuS 4 tetrahedra are crucial for the stability and optical properties of the Ba 6 (Cu x Z y )Sn 4 S 16 (Z = Mg, Mn, Zn, Cd, In, Bi, Sn) compounds revealed by electronic structure analysis.

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

Synthesis, morphology and optical properties of LaFeO{sub 3} nanospheres

LaFeO{sub 3} nanospheres have been successively synthesized via hydrothermal method. Structural, morphological and optical properties of the prepared nanopowder were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV–Vis absorption spectroscopy. The UV–Vis shows strong absorption at 475 nm which has excellent visible light absorption ability. Band gap energy of the prepared nanosphere was found to be 2.60 eV. The results indicate that the LaFeO{sub 3} nanospheres prepared by this method could be a kind of photocatalytic material.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Temperature dependent structural, optical and hydrophobic properties of sputtered deposited HfO{sub 2} films

Hafnium oxide being high-k dielectric has been successfully utilized in electronic and optical applications. Being thermodynamically stable and having good mechanical strength, it can be used as a protective coating for outdoor HV insulators which are suffering from surface flashover problem due to contamination. In this paper, we are investigating the effect of substrate temperature on structural, optical and hydrophobic properties of hafnium oxide coating deposited over glass insulators by DC magnetron sputtering. X-ray diffraction is applied to determine the crystalline phase and crystallite size of the film. The morphology of the samples is examined using atomic force microscopy. The optical properties are studied using UV-vis-NIR spectrophotometer. The wettability of the film is investigated using contact angle meter. The thickness is measured using surface profilometer and verified through optical data. The relationship between substrate temperature with grain size, roughness, refractive index, and hydrophobicity is manifested. The maximum contact angle for HfO{sub 2} film was found to be 106° at 400°C.

36 MATERIALS SCIENCE↗