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At least 523 records · Page 29
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Synthesis and characterization of amorphous Fe2.75Dy-oxide thin films demonstrating room-temperature semiconductor, magnetism, and optical transparency

Recently, amorphous/disordered oxide thin films made from Fe and lanthanides like Dy and Tb have been reported to have a rich set of magnetic, optical, and electronic properties, as well as room-temperature magneto-electric coupling with multiferroics [A. Malasi et al., Sci. Rep. 5, 18157 (2015); H. Taz et al., Sci. Rep. 6, 27869 (2016); and H. Taz et al., Sci. Rep. 10, 1–10 (2020)]. Here, we report the synthesis and detailed characterization of Fe2.75Dy-oxide thin films prepared on various substrates using electron beam co-evaporation. The structure, chemistry, electric, magnetic, and optical properties were studied for the as-prepared and annealed (373 K, in air, 1 h) films of thickness 40 nm. High resolution transmission electron microscopy and electron diffraction study showed that the films were amorphous in both the as-prepared and annealed states. The electron energy-loss spectroscopy studies quantified that metal oxygen stoichiometry changed from Fe2.75Dy-O1.5 to Fe2.75Dy-O1.7 upon annealing. Synchrotron-based x-ray absorption spectroscopy investigation confirmed that the as-prepared films were highly disordered with predominantly metallic Fe and Dy states that became slightly oxidized with annealing in air. The as-prepared amorphous films demonstrated significantly high value of ordinary (∼10 cm2/V s) and anomalous (∼102 cm2/V s) Hall mobility and high electrical conductivity of ∼103 S/cm at room temperature. The cryogenic magnetic property measurement shows two-step magnetization below 200 K, suggesting exchange-spring magnetic interaction. The nature of the field cooled and zero-field cooled curves suggested a spin-glass like transition between 78 K and 80 K, with a characteristic broad peak. The Tauc plot analysis from optical transmission spectra confirms the existence of an optical bandgap of ∼2.42 eV that increased slightly to ∼2.48 eV upon annealing. This rich set of transport, optical, and magnetic properties in these thin films is very exciting and points to potential applicability in low-cost multifunctional devices requiring a combination of transparent, semiconducting, and magnetic responses, such as in spintronics.

Prasad Koirala, Krishna (ORCID:000000029137917X)↗
DOE OSTI2025

Synthesis, Crystal Structure, and Optical Properties of the Barium meta -Pertechnetate Ba[TcO 4 ] 2

High-quality single crystals of the colorless title compound Ba[ 99 TcO 4 ] 2 were prepared from radioactive, isotope-pure 99 TcO 2 by oxidation with H 2 O 2 in an aqueous ammonia solution and subsequent cation metathesis using an ion-exchange column. Single-crystal X-ray diffraction revealed Ba[TcO 4 ] 2 to crystallize isotopically to Ba[MnO 4 ] 2 in the orthorhombic space group Fddd with the lattice parameters a = 747.34(5) pm, b = 1244.08(7) pm, and c = 1511.23(9) pm for Z = 8. Its crystal structure features [BaO 12 ] 22- icosahedra surrounded by ten [TcO 4 ] - tetrahedra connected via two edges and eight corners. The optical properties of Ba[TcO 4 ] 2 investigated by UV-vis spectroscopy show the broad O 2- → Tc 7+ ligand-to-metal charge transfer (2p → 4d) process within these discrete [TcO 4 ]- anions at an absorption maximum of around 350 nm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Synthesis and optical properties of phosphorus doped ZnO: X-ray absorption, X-ray emission, and X-ray excited optical luminescence studies

Abstract Over the past decades, zinc oxide semiconductor and its derivatives have been extensively developed because of its optoelectronic properties. Since ZnO is an intrinsic n-type semiconductor, how to synthesize high-quality p-type ZnO semiconductors and investigate their optoelectronic properties and local chemical structures are important and necessary. In this article, two studies of synthesizing both undoped and phosphorus-doped ZnO nanostructures by hydrothermal method and chemical vapor deposition (CVD) technique are presented. Scanning electron microscopy (SEM) and laboratory X-ray diffraction (XRD) are used to track the surface morphology and the crystalline structure of both undoped and phosphorus doped ZnO nanostructures, respectively. X-ray absorption near edge structures (XANES), X-ray emission spectroscopy (XES) and X-ray excited optical luminescence (XEOL) are also used to determine the local chemical information of both undoped and phosphorus-doped ZnO nano/microstructures such as local symmetry and optical properties. It is found that the phosphorus is successfully doped into the surface of ZnO and substituted the Zn. The phosphorus-doped ZnO products have better crystallinity and less oxygen vacancies on the surface. These two are correlated as one leads to the other. The XEOL results suggest that the average bandgap for undoped and phosphorus doped ZnO is the same, 3.24 eV. The second derivative of the absorption-emission spectra yields the fundamental bandgap for undoped ZnO and phosphorus-doped ZnO is 3.25 eV. The implication of this observation is discussed.

Chemistry↗
DOE OSTI2022

Super-Resolution Airy Disk Microscopy of Individual Color Centers in Diamond

Super-resolution imaging techniques enable nanoscale microscopy in fields such as physics, biology, and chemistry. However, many super-resolution techniques require specialized optical components, such as a helical-phase mask. In this work, we present a novel technique, super-resolution Airy disk microscopy, that can be used in a standard confocal microscope without any specialized optics. We demonstrate this technique, in combination with ground state depletion, to image and control nitrogen-vacancy (NV) centers in bulk diamond below the diffraction limit. A greater than 14-fold improvement in resolution compared to the diffraction limit is achieved, corresponding to a spatial resolution of 16.9(8) nm for a 1.3 NA microscope with 589 nm light. We make use of our enhanced spatial resolution to control the spins states of individual NV centers separated from each other by less than the diffraction limit, including pairs sharing the same orientation that are indistinguishable with a conventional electron spin resonance measurement.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Indications for Lifshitz transitions in the nodal-line semimetal ZrSiTe induced by interlayer interaction

The layered material ZrSiTe is currently extensively investigated as a nodal-line semimetal with Dirac-like band crossings protected by nonsymmorphic symmetry close to the Fermi energy. A recent infrared spectroscopy study on ZrSiTe under external pressure found anomalies in the optical response, providing hints for pressure-induced phase transitions at ≈4.1 and ≈ 6.5GPa. By pressure-dependent Raman spectroscopy and x-ray diffraction measurements combined with electronic band structure calculations we find indications for two pressure-induced Lifshitz transitions with major changes in the Fermi surface topology in the absence of lattice symmetry changes. These electronic phase transitions can be attributed to the enhanced interlayer interaction induced by external pressure. Overall, our findings demonstrate the crucial role of the interlayer distance for the electronic properties of layered van der Waals topological materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Ultrafast perturbation of magnetic domains by optical pumping in a ferromagnetic multilayer

Ultrafast optical pumping of spatially nonuniform magnetic textures is known to induce far-from-equilibrium spin transport effects. Here, we use ultrafast x-ray diffraction with unprecedented dynamic range to study the laser-induced dynamics of labyrinth domain networks in ferromagnetic CoFe/Ni multilayers. We detected azimuthally isotropic, odd order, magnetic diffraction rings up to fifth order. The amplitudes of all three diffraction rings quench to different degrees within 1.6 ps. In addition, all three of the detected diffraction rings both broaden by 15% and radially contract by 6% during the quench process. We are able to rigorously quantify a 31% ultrafast broadening of the domain walls via Fourier analysis of the order-dependent quenching of the three detected diffraction rings. Here, the broadening of the diffraction rings is interpreted as a reduction in the domain coherence length, but the shift in the ring radius, while unambiguous in its occurrence, remains unexplained. In particular, we demonstrate that a radial shift explained by domain-wall broadening can be ruled out. With the unprecedented dynamic range of our data, our results provide convincing evidence that labyrinth domain structures are spatially perturbed at ultrafast speeds under far-from-equilibrium conditions, albeit the mechanism inducing the perturbations remains yet to be clarified.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Small Bragg-plane slope errors revealed in synthetic diamond crystals

Wavefront-preserving X-ray diamond crystal optics are essential for numerous applications in X-ray science. Perfect crystals with flat Bragg planes are a prerequisite for wavefront preservation in Bragg diffraction. However, this condition is difficult to realize in practice because of inevitable crystal imperfections. Here, X-ray rocking curve imaging is used to study the smallest achievable Bragg-plane slope errors in the best presently available synthetic diamond crystals and how they compare with those of perfect silicon crystals. It is shown that the smallest specific slope errors in the best diamond crystals are about 0.08 (3) µrad mm -2 . These errors are only 50% larger than the 0.05 (2) µrad mm -2 specific slope errors measured in perfect silicon crystals. High-temperature annealing at 1450°C of almost flawless diamond crystals reduces the slope errors very close to those of silicon. Further investigations are in progress to establish the wavefront-preservation properties of these crystals.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Modulating the optoelectronic properties of hybrid Mo-thiolate thin films

In this study, hybrid MoS 2 -based molybdenum thiolate thin films with selected organic motifs are grown using molecular layer deposition (MLD), allowing for tunable optoelectronic film properties. The thin films are deposited at 170°C using the metal precursor molybdenum hexacarbonyl and one of the three organic precursors: 1,2-ethanedithiol, 1,4-butanedithiol, and 1,4-benzenedithiol. The resulting Mo-ethanethiolate, Mo-butanethiolate, and Mo-benzenethiolate films show saturating growth with a growth per cycle of 1.2, 1.0, and 1.5 Å/cycle, respectively. Fourier transform infrared spectroscopy, x-ray photoelectron spectroscopy, Raman spectroscopy, x-ray absorption spectroscopy, and x-ray diffraction are used to characterize the as-deposited films. Results show that by changing the organic precursor, the film composition as well as the optical and electronic properties can be tuned. The Mo-thiolate films grown with benzenedithiol exhibit the lowest resistivity, which at 12 mΩ cm is ~400 times more conductive than Mo-thiolates grown with aliphatic organic linkers. All three backbone chemistries of the Mo-thiolates show an optical bandgap between 2.3 and 2.4 eV and mild photoconductivity response. The MLD of these Mo-thiolate films demonstrates the synthesis of transition metal-organosulfur thin films with tunable properties.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Subnanosecond phase transition dynamics in laser-shocked iron

Iron is one of the most studied chemical elements due to its sociotechnological and planetary importance; hence, understanding its structural transition dynamics is of vital interest. By combining a short pulse optical laser and an ultrashort free electron laser pulse, we have observed the subnanosecond structural dynamics of iron from high-quality x-ray diffraction data measured at 50-ps intervals up to 2500 ps. We unequivocally identify a three-wave structure during the initial compression and a two-wave structure during the decaying shock, involving all of the known structural types of iron (α-, γ-, and ε-phase). In the final stage, negative lattice pressures are generated by the propagation of rarefaction waves, leading to the formation of expanded phases and the recovery of γ-phase. Our observations demonstrate the unique capability of measuring the atomistic evolution during the entire lattice compression and release processes at unprecedented time and strain rate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Airy light-sheet Raman imaging

Light-sheet fluorescence microscopy has greatly improved the speed and overall photostability of optically sectioning cellular and multi-cellular specimens. Similar gains have also been conferred by light-sheet Raman imaging; these schemes, however, rely on diffraction limited Gaussian beams that hinder the uniformity and size of the imaging field-of-view, and, as such, the resulting throughput rates. Here, we demonstrate that a digitally scanned Airy beam increases the Raman imaging throughput rates by more than an order of magnitude than conventional diffraction-limited beams. Overall, this, spectrometer-less, approach enabled 3D imaging of microparticles with high contrast and 1 µm axial resolution at 300 msec integration times per plane and orders of magnitude lower irradiation density than coherent Raman imaging schemes. We detail the apparatus and its performance, as well as its compatibility with fluorescence light-sheet and quantitative-phase imaging towards rapid and low phototoxicity multimodal imaging.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Simulation of X-ray Hartmann wavefront sensing with the Synchrotron Radiation Workshop

X-ray wavefront measurement is an important beam diagnostic tool, especially for the diffraction-limited X-ray beam. These in situ diagnostics give a better understanding of beam imperfections, and they enable feedback for possible corrections and/or optical alignment improvements. Hartmann wavefront sensing is one of the promising techniques to perform in situ X-ray wavefront measurements. In this work, a simulation tool of the X-ray Hartmann Wavefront Sensor (HWS) is developed under the Synchrotron Radiation Workshop (SRW) framework. Using this new simulation capability, one can take advantage of the full SRW package to simulate Hartmann wavefront sensing with the beam traveling from the X-ray source to the sample through different X-ray optical components. This SRW HWS simulation tool can help to optimize the wavefront sensor parameters for a specific X-ray energy range. It can also simulate an in situ wavefront measurement experiment with a particular beamline optical layout and predict the expected results of the wavefront measurement under different beamline configurations.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Accelerated microwave-assisted synthesis and in situ X-ray scattering of tungsten-substituted vanadium dioxide (V 1-x W x O 2 )

Vanadium dioxide (VO 2 ) has been widely studied due to its metal-insulator phase transition at 68°C, below which it is a semiconducting monoclinic phase, P2 1 /c, and above it is a metallic tetragonal phase, P4 2 /mnm. Substituting vanadium with transition metals allows transition temperature tunability. An accelerated microwave-assisted synthesis for VO 2 and 5d tungsten substituted VO 2 presented herein decreased synthesis time by three orders of magnitude while maintaining phase purity, particle size, and transition character. Tungsten substitution amount was determined using inductively coupled plasma-optical emission spectroscopy. Differential scanning calorimetry, superconducting quantum interference device measurements, and in-situ heating and cooling experiments monitored through synchrotron x-ray diffraction (XRD) confirmed the transition temperature decreased with increased tungsten substitution. Scanning electron microscopy analyzed through the line-intercept method produced an average particle size of 3 – 5 μm. Average structure and local structure phase purity was determined through Rietveld analysis of synchrotron XRD and least-squares refinement of pair-distribution function data.

36 MATERIALS SCIENCE↗
DOE OSTI2024

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↗
DOE OSTI2024

Crystal growth, physical and optical properties of TlSr 2 Cl 5 and TlSr 2 Br 5

Small diameter (Ø 16 mm) TlSr 2 Cl 5 and TlSr 2 Br 5 crystals were grown by the Vertical Bridgman method. X-ray diffraction measurements show that both have the monoclinic crystal structure with space group P21/c. TlSr 2 Cl 5 and TlSr 2 Br 5 have a density of 4.14 g/cm 3 and 5.03 g/cm 3 , respectively. The effective Z of TlSr 2 Cl 5 and TlSr 2 Br 5 is 63.7 and 58.6, respectively. Radioluminescence spectra of TlSr 2 Cl 5 and TlSr 2 Br 5 feature a broad emission band peaking at 440 and 445 nm, respectively. As a result the light yield of TlSr 2 Cl 5 and TlSr 2 Br 5 was estimated to be 17,000 and 45,000 ph/MeV, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Optical, structural and aging properties of Al/Sc-based multilayers for the extreme ultraviolet

This manuscript presents the structural characterization of Al/Sc-based periodic multilayer coatings for the extreme ultraviolet (EUV) spectral range. Based on transmission electron microscopy and electron diffraction as well as grazing-incidence and large-angle x-ray diffraction, a model for the layer structure and the interfacial effects of Al/Sc coatings is built. The onset of crystallization in nanoscale Al and Sc layers as a function of thickness is also revealed in these characterizations. The Al/Sc layer model is validated and further refined by fitting in-band and out-of-band EUV reflectance measurements across 5 orders of magnitude in an extended wavelength range from 17 to 80 nm. Here, the same type of EUV reflectance measurements is used to test the Al/Sc aging properties and to demonstrate the spectral response of optimized two- and tri-material multilayers including Al/Sc, Al/Sc/SiC and Mo/Al/Sc.

36 MATERIALS SCIENCE↗
DOE OSTI2025

A Flat Analyzer Polycapillary Spectrometer for X-ray Absorption Spectroscopy of Dilute Transition Metals at X-ray-Free Electron Lasers

X-ray absorption spectroscopy (XAS) coupled with highly intense pulses from an X-ray-free electron laser (XFEL) can be used to track ultrafast chemical dynamics. Nonetheless, measurements for dilute samples (≤1 mM) have been exceptionally challenging, as scattering background signals dominate over the sample’s X-ray fluorescence. We show that femtosecond time-resolved XAS measurements of sub-millimolar transition metal solutions are now possible at the Linac Coherent Light Source (LCLS) using a high-throughput polycapillary XAS spectrometer, designed, developed, and commissioned at LCLS and the Stanford Synchrotron Radiation Lightsource (SSRL). The instrument integrates three polycapillary optics that collect and collimate X-ray fluorescence emitted from the interaction point with a high solid angle. X-ray collimated fluorescence is then selectively diffracted by coupled graphite analyzer crystals. As a result, the contribution of scattered photons is suppressed. Experiments at the Pt L 3 -edge on 0.1 mM aqueous K 2 PtCl 6 (delivered via a 100 μm liquid jet) were successfully performed in the laser pump X-ray probe configuration at the LCLS XCS and XPP instruments. We report the transient spectra of hexachloroplatinate within the first 10 ps after a 266 nm photoexcitation. We observed a short-lived reduced intermediate (≈2 ps). The polycapillary X-ray spectrometer at LCLS now enables the efficient study of the dynamics of ultradilute transition metals in solution. This capability opens the door to investigating plasmonic systems, photocatalysts, enzymes, and other scarce and dilute samples.

LCLS↗
DOE OSTI2024

Direct neutron-diffraction-based measurement of magnetic order in brownmillerite SrCoO 2.5 and La 0.5 Sr 0.5 CoO 2.5 thin films

Epitaxial cobaltites have emerged as exemplary materials for electrochemical gating, in large part due to their topotactic perovskite (P) ↔ brownmillerite (BM) transformations. SrCoO 3-δ , for example, can be cycled between metallic ferromagnetic P SrCoO 3 and insulating BM SrCoO 2.5 , realizing exceptional modulation of electronic, thermal, and optical properties. It is often presumed that such cycling also generates ferromagnetic–antiferromagnetic (F-AF) modulation due to the G-type AF order in bulk SrCoO 2.5 . Little is understood about magnetism in thin-film BM SrCoO 2.5 , however, meaning that the true magnetic property modulation is unclear. We address this here through a neutron diffraction study of BM La 1-x Sr x CoO 2.5 films at x = 0.5 and 1.0. Lightly compressively strained SrCoO 2.5 films are shown to retain G-type AF order, albeit with suppressed Néel temperature (~340 K). Of high interest for AF spintronics, room-temperature F–AF cycling is thus possible across the SrCoO 3-δ P ↔ BM transformation. At x = 0.5, however, BM La 0.5 Sr 0.5 CoO 2.5 films are found to exhibit no detectable G-type AF order but instead weak F order (Curie temperature ~115 K), unveiling a La 0.5 Sr 0.5 CoO 3-δ phase diagram with two distinct F phases. These results thus uncover new, unanticipated magnetic phase behavior in these materials, in addition to being directly relevant to cobaltite-based magnetoionics.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Acceleration of Crystallization Kinetics in Ge‐Sb‐Te‐Based Phase‐Change Materials by Substitution of Ge by Sn

Abstract Thin films of (Ge 1– x Sn x ) 8 Sb 2 Te 11 are prepared to study the impact of Sn‐substitution on properties relevant for application in phase‐change memory, a next‐generation electronic data storage technology. It is expected that substitution decreases the crystallization temperature, but it is not known how the maximum crystallization rate is affected. Ge 8 Sb 2 Te 11 is chosen from the (GeTe) y (Sb 2 Te 3 ) 1– y system of phase‐change materials as a starting point due to its higher crystallization temperature as compared to the common material Ge 2 Sb 2 Te 5 . In situ X‐ray diffraction at 5 K min −1 heating rate is performed to determine the crystallization temperature and the resulting structure. To measure the maximum crystallization rate, femtosecond optical pulses that heat the material repetitively and monitor the resulting increase of optical reflectance are used. Glasses over the entire composition range are prepared using a melt‐quenching process. While at x = 0, 97, subsequent pulses are required for crystallization, one single pulse is enough to achieve the same effect at x = 0.5. The samples are further characterized by optical ellipsometry and calorimetry. The combined electrical and optical contrast and the ability to cycle between states with single femtosecond pulses renders Ge 4 Sn 4 Sb 2 Te 11 promising for photonics applications.

Zalden, Peter↗