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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Grazing-incidence diffraction reveals cellulose and pectin organization in hydrated plant primary cell wall

Abstract The primary cell wall is highly hydrated in its native state, yet many structural studies have been conducted on dried samples. Here, we use grazing-incidence wide-angle X-ray scattering (GIWAXS) with a humidity chamber, which enhances scattering and the signal-to-noise ratio while keeping outer onion epidermal peels hydrated, to examine cell wall properties. GIWAXS of hydrated and dried onion reveals that the cellulose ( $$110/1\overline{1}0$$ 110 / 1 1 ¯ 0 ) lattice spacing decreases slightly upon drying, while the (200) lattice parameters are unchanged. Additionally, the ( $$110/1\overline{1}0$$ 110 / 1 1 ¯ 0 ) diffraction intensity increases relative to (200). Density functional theory models of hydrated and dry cellulose microfibrils corroborate changes in crystalline properties upon drying. GIWAXS also reveals a peak that we attribute to pectin chain aggregation. We speculate that dehydration perturbs the hydrogen bonding network within cellulose crystals and collapses the pectin network without affecting the lateral distribution of pectin chain aggregates.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Spin waves above and below the Verwey transition in TbBaFe 2 O 5

TbBaFe 2 O 5+δ (TBFO) is a mixed valence compound with an antiferromagnetic order (T N =450K) that changes along with the crystal structure and conductivity upon cooling below a Verwey-like transition (TV=280K). This type of double-cell-layered perovskite is useful to study putative charge ordering in fractional valence systems because the crystal structure develops unique sites for the different valence states. While the evolution of the static magnetic structure in the different charge ordered states of TBFO is known, in this study we investigate the effect of charge ordering on the magnetic interactions. Dispersive magnetic excitations measured using single crystal inelastic neutron scattering experiments at T=4K V and T=320K>T V are modeled with linear-spin-wave theory to extract anisotropy and superexchange parameters. Below T V , we observe a sizable magnon gap due to an easy-axis magnetic anisotropy that closes above T V due to the evolution of easy-plane anisotropy. The magnetic interactions are found to be highly three-dimensional and change across T V . Above T V , where the conductivity is greater, a damping term is required to model the spin waves that suggests a coupling to valence fluctuations.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

SMART Perovskite Growth: Enabling a Larger Range of Process Conditions

Cost-effective, high-throughput industrial applications of metal-halide perovskites require a highly tolerant method (i.e., wide process window) that produces high-quality materials with a short annealing time. Here, we introduce a Seed Modulation for ARTificially controlled nucleation (SMART) process that enables rapid fabrication of high-quality perovskite films under a wide set of initial input parameters. Additionally, we characterized the thin-film evolution from the perspective of crystallinity, surface potential, diffusivity, surface carrier dynamics, and interfacial recombination. We find that surface and subsurface defects primarily determine the performance of materials and devices. By modulating the seeds for perovskite nucleation, we were able to improve the overall crystallization. We achieved a >20% power conversion efficiency using only a 5 min annealing step, and we found that the annealing window is widened such that differing initial conditions achieve similar quality. Furthermore, we demonstrated reproducibility and performance improvement in larger-area perovskite cells by incorporating the SMART process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2022

Structural and chemical complexity of minerals: An update

The complexities of chemical composition and crystal structure are fundamental characteristics of minerals that have high relevance to the understanding of their stability, occurrence and evolution. This review summarises recent developments in the field of mineral complexity and outlines possible directions for its future elaboration. The database of structural and chemical complexity parameters of minerals is updated by H-correction of structures with unknown H positions and the inclusion of new data. The revised average complexity values (arithmetic means) for all minerals are 3.54(2) bits/atom and 345(10) bits/cell (based upon 4443 structure reports). The distributions of atomic information amounts, chemIG and strIG, versus the number of mineral species fit the normal modes, whereas the distributions of total complexities, chemIG,total and strIG,total, along with numbers of atoms per formula and per unit cell are log normal. The three most complex mineral species known today are ewingite, morrisonite and ilmajokite, all either discovered or structurally characterised within the last five years. The most important complexity-generating mechanisms in minerals are: (1) the presence of isolated large clusters; (2) the presence of large clusters linked together to form three-dimensional frameworks; (3) formation of complex three-dimensional modular frameworks; (4) formation of complex modular layers; (5) high hydration state in salts with complex heteropolyhedral units; and (6) formation of ordered superstructures of relatively simple structure types. The relations between symmetry and complexity are considered. The analysis of temporal dynamics of mineralogical discoveries since 1875 with the step of 25 years show the increasing chemical and structural complexities of human knowledge of the mineral kingdom in the history of mineralogy. In the Earth’s history, both diversity and complexity of minerals experience dramatic increases associated with the formation of Earth’s continental crust, initiation of plate tectonics and the Great Oxidation event.

complexity↗
DOE OSTI2024

Magnetic ordering in Eu 2 In and Eu 2 Sn

Eu 2 In and Eu 2 Sn crystallize in the orthorhombic Co 2 Si-type structure (oP12, Pnma, No. 62) with In and Sn atoms occupying one 4c site and the Eu atoms filling two other 4c sites. Eu 2 In has a nearly ideal first-order magnetostructural transition (FOMT) at 55 K with a hysteresis of less than 0.1 K, a large entropy change and an adiabatic temperature change of 5.0 K in a field of 2 T. The anhysteretic nature of the FOMT is likely due to there being no change in cell symmetry and relatively small changes in the lattice parameters. There is no magnetostructural transition in Eu2Sn. In this work we present the results of powder neutron diffraction, magnetization, and Eu Mössbauer spectroscopy aimed to investigate the nature of magnetic order for both Eu 2 In and Eu 2 Sn. The Eu Mössbauer spectrum of Eu 2 In at 5 K shows two equal area components, consistent with Eu occupying two equal multiplicity crystallographic sites. However, the different hyperfine fields (B) of 27 T and 17 T suggest that the magnetic environments of the Eu moments on the two 4c sites are different. Neutron diffraction data at 2.5 K show that in Eu 2 In the order is ferromagnetic, with Eu moments on both Eu sites oriented parallel to the a-axis; moment values of 6.8 μB and 6.5 μB were found. For Eu 2 Sn measurements find two antiferromagnetic transitions, which are corroborated by neutron diffraction. Analysis of density-functional theory calculations shows negligible energy difference between differing magnetic configurations, indirectly supporting stability of multiple magnetic structures observed experimentally. While the transition at T N1 = 30 K corresponds to the formation of a simple k 1 = 0 antiferromagnetic structure with Eu-moments pointing along the b-axis, at T N2 = 13 K a coexisting second magnetic order with k 2 = [0, ½, ½] appears.

36 MATERIALS SCIENCE↗
NASA NTRS1980

Gaalas/Gaas Solar Cell Process Study

Available information on liquid phase, vapor phase (including chemical vapor deposition) and molecular beam epitaxy growth procedures that could be used to fabricate single crystal, heteroface, (AlGa) As/GaAs solar cells, for space applications is summarized. A comparison of the basic cost elements of the epitaxy growth processes shows that the current infinite melt LPE process has the lower cost per cell for an annual production rate of 10,000 cells. The metal organic chemical vapor deposition (MO-CVD) process has the potential for low cost production of solar cells but there is currently a significant uncertainty in process yield, i.e., the fraction of active material in the input gas stream that ends up in the cell. Additional work is needed to optimize and document the process parameters for the MO-CVD process.

Almgren, D. W.↗
NASA NTRS1996

Investigation of Polymer Liquid Crystals

The positron annihilation lifetime spectroscopy (PALS) using a low energy flux generator may provide a reasonably accurate technique for measuring molecular weights of linear polymers and characterization of thin polyimide films in terms of their dielectric constants and hydrophobity etc. Among the tested samples are glassy poly arylene Ether Ketone films, epoxy and other polyimide films. One of the proposed techniques relates the free volume cell size (V(sub f)) with sample molecular weight (M) in a manner remarkably similar to that obtained by Mark Houwink (M-H) between the inherent viscosity (eta) and molecular wieght of polymer solution. The PALS has also demonstrated that free-volume cell size in thermoset is a versatile, useful parameter that relates directly to the polymer segmental molecular weight, the cross-link density, and the coefficient of thermal expansion. Thus, a determination of free volume cell size provides a viable basis for complete microstructural characterization of thermoset polyimides and also gives direct information about the cross-link density and coefficient of expansion of the test samples. Seven areas of the research conducted are reported here.

Han, Kwang S.↗
NASA NTRS2008

Role of Hf on Phase Formation in Ti45Zr(38-x)Hf(x)Ni17 Liquids and Solids

Hafnium and zirconium are very similar, with almost identical sizes and chemical bonding characteristics. However, they behave differently when alloyed with Ti and Ni. A sharp phase formation boundary near 18-21 at.% Hf is observed in rapidly-quenched and as-cast Ti45Zr38-xHfxNi17 alloys. Rapidly-quenched samples that contain less than 18 at.% Hf form the icosahedral quasicrystal phase, whiles samples containing more than 21 at.% form the 3/2 rational approximant phase. In cast alloys, a C14 structure is observed for alloys with Hf lower than the boundary concentration, while a large-cell (11.93 ) FCC Ti2Ni-type structure is found in alloys with Hf concentrations above the boundary. To better understand the role of Hf on phase formation, the structural evolution with supercooling and the solidification behavior of liquid Ti45Zr38-xHfxNi17 alloys (x=0, 12, 18, 21, 38) were studied using the Beamline Electrostatic Levitation (BESL) technique using 125keV x-rays on the 6ID-D beamline at the Advanced Photon Source, Argonne National Laboratory. For all liquids primary crystallization was to a BCC solid solution phase; interestly, an increase in Hf concentration leads to a decrease in the BCC lattice parameter in spite of the chemical similarity between Zr and Hf. A Reitveld analysis confirmed that as in the cast alloys, the secondary phase that formed was the C14 below the phase formation boundary and a Ti2Ni-type structure at higher Hf concentrations. Both the liquidus temperature and the reduced undercooling change sharply on traversing the phase formation boundary concentration, suggesting a change in the liquid structure. Structural information from a Honeycutt-Anderson index analysis of reverse Monte Carlo fits to the S(q) liquid data will be presented to address this issue.

Wessels, V.↗
DOE OSTI2021

The influence of hydrostatic pressure and annealing conditions on the magnetostructural transitions in MnCoGe

In this work, the phase transitions of stoichiometric MnCoGe alloys were studied by systematically varying the annealing conditions and applying hydrostatic pressure. First-order martensitic structural transitions from the Ni2In-type hexagonal austenite phase to the TiNiSi-type orthorhombic martensite phase spanned a wide temperature window (>200 K) as a result of quenching the samples at temperatures ranging from the solid phase at 700 °C to the liquid phase at 1150 °C. Despite the large variation in their structural transition temperatures, the changes in cell parameters across the structural transitions and the Curie–Weiss temperatures of the martensite/austenite phase were relatively small. For the sample quenched from 800 °C, coupled magnetostructural transitions were observed, and the largest maximum magnetic entropy change was found to be -ΔS max = 33:6 J/kg K for a 7-T field change. The coupled magnetostructural transitions and the corresponding magnetic entropy enhancements were found to also be achievable by applying hydrostatic pressures. Meanwhile, as the quenching temperatures or hydrostatic pressures increased, the first-order martensitic structural transition shifted toward lower temperature until it was ultimately absent, in which case only the crystal structure and magnetic transition of the Ni 2 In-type hexagonal austenite phase were present.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
NASA NTRS2000

A Technique for Rapidly Deploying a Concentration Gradient with Applications to Microgravity

The latter half of the last century has seen rapid advancements in semiconductor crystal growth powered by the demand for high performance electronics in myriad applications. The reduced gravity environment of space has also been used for crystal growth tests, especially in instances where terrestrial growth has largely been unsuccessful. While reduced gravity crystal growth affords some control of the gravity parameter, many crystals grown in space, to date, have structural flaws believed to result from convective motions during the growth phase. The character of these instabilities is not well understood but is associated with thermal and solutal density variations near the solidification interface in the presence of residual gravity and g-jitter. In order to study these instabilities in a separate, controlled space experiment, a concentration gradient would first have to be artificially established in a timely manner as an initial condition. This is generally difficult to accomplish in a microgravity environment because the momentum of the fluid injected into a test cell tends to swirl around and mix in the absence of a restoring force. The use of magnetic fields to control the motion and position of liquids has received growing interest in recent times. The possibility of using the force exerted by a non-uniform magnetic field on a ferrofluid to not only achieve fluid manipulation but also to actively control fluid motion makes it an attractive candidate for space applications. This paper describes a technique for quickly establishing a linear or exponential fluid concentration gradient using a magnetic field in place of gravity to stabilize the deployment. Also discussed is a photometric technique for measuring the concentration profile using light attenuation. Results of the ground-based experiments indicate that the concentration distribution is within 3% of the predicted value. Although any range of concentations can be realized, photometric constraints are discussed which impose some limitations on measurements.

Leslie, Fred↗
NASA NTRS1990

The Spacelab J mission

This paper describes Spacelab J (SL-J), its mission characteristics, features, parameters and configuration, the unique nature of the shared reimbursable cooperative effort with the National Space Development Agency (NASDA) of Japan and the evolution, content and objectives of the mission scientific experiment complement. The mission is planned for launch in 1991. This long module mission has 35 experiments from Japan as well as 9 investigations from the United States. The SL-J payload consists of two broad scientific disciplines which require the extended microgravity or cosmic ray environment: (1) materials science such as crystal growth, solidification processes, drop dynamics, free surface flows, gas dynamics, metallurgy and semiconductor technology; and (2) life science including cell development, human physiology, radiation-induced mutations, vestibular studies, embryo development, and medical technology. Through an international agreement with NASDA, NASA is preparing to fly the first Japanese manned, scientific, cooperative endeavor with the United States.

Cremin, J. W.↗
NASA NTRS2005

NASA Tech Briefs, April 2005

Gas-Tolerant Device Senses Electrical Conductivity of Liquid Nanoactuators Based on Electrostatic Forces on Dielectrics Replaceable Microfluidic Cartridges for a PCR Biosensor CdZnTe Image Detectors for Hard-X-Ray Telescopes High-Aperture-Efficiency Horn Antenna Full-Circle Resolver-to-Linear-Analog Converter Continuous, Full-Circle Arctangent Circuit Advanced Three-Dimensional Display System Automatic Focus Adjustment of a Microscope Topics covered include: FastScript3D - A Companion to Java 3D; Generating Mosaics of Astronomical Images; Simulating Descent and Landing of a Spacecraft; Simulating Vibrations in a Complex Loaded Structure; Rover Sequencing and Visualization Program; Software Template for Instruction in Mathematics; Support for User Interfaces for Distributed Systems; Nanostructured MnO2-Based Cathodes for Li-Ion/Polymer Cells; Multi-Layer Laminated Thin Films for Inflatable Structures; Two-Step Laser Ranging for Precise Tracking of a Spacecraft; Growing Aligned Carbon Nanotubes for Interconnections in ICs; Multilayer Composite Pressure Vessels; Texturing Blood-Glucose-Monitoring Optics Using Oxygen Beams; Fault-Tolerant Heat Exchanger; Atomic Clock Based on Opto-Electronic Oscillator; Microfocus/Polycapillary-Optic Crystallographic X-Ray Sys; Depth-Penetrating Luminescence Thermography of Thermal- Barrier Coatings; One-Dimensional Photonic Crystal Superprisms; Measuring Low-Order Aberrations in a Segmented Telescope; Mapping From an Instrumented Glove to a Robot Hand; Application of the Hilbert-Huang Transform to Financial Data; Optimizing Parameters for Deep-Space Optical Communication; and Low-Shear Microencapsulation and Electrostatic Coating.

Source record↗
NASA NTRS1986

Crystal growth and furnace analysis

A thermal analysis of Hg/Cd/Te solidification in a Bridgman cell is made using Continuum's VAST code. The energy equation is solved in an axisymmetric, quasi-steady domain for both the molten and solid alloy regions. Alloy composition is calculated by a simplified one-dimensional model to estimate its effect on melt thermal conductivity and, consequently, on the temperature field within the cell. Solidification is assumed to occur at a fixed temperature of 979 K. Simplified boundary conditions are included to model both the radiant and conductive heat exchange between the furnace walls and the alloy. Calculations are performed to show how the steady-state isotherms are affected by: the hot and cold furnace temperatures, boundary condition parameters, and the growth rate which affects the calculated alloy's composition. The Advanced Automatic Directional Solidification Furnace (AADSF), developed by NASA, is also thermally analyzed using the CINDA code. The objective is to determine the performance and the overall power requirements for different furnace designs.

Dakhoul, Youssef M.↗
DOE OSTI2025

Thermal expansion of LaB 6 from 298 to 998 K

We propose LaB 6 as a temperature calibration standard for high-temperature (HT) X-ray diffractometry owing to its high temperature stability. Such HT applications require a reliable HT lattice parameter or, equivalently, peak position data, which have not been readily accessible to the diffraction community to date. As such, the thermal expansion behavior of NIST SRM 660a LaB6 was assessed in the temperature range 298–998 K using HT Bragg–Brentano parafocusing θ:θ X-ray diffractometry in conjunction with Rietveld analysis. Data were collected in the 2θ range 20–150° at a data collection rate of 0.5° θ min −1 in air and at 1 atm. The temperature was stepped in 50 K increments. The cubic unit-cell lattice parameter [a(T)] of LaB 6 in Å was found to vary as a(T) = 4.15678 (±0.00001) + Ξ(T − 298 K) + Ψ(T − 298 K) 2 , where Ξ = 2.4645 × 10 −5 (±4.8904 × 10 −8 ) Å K −1 and Ψ = 1.0325 × 10 −8 (±6.7376 × 10 −11 ) Å K −1 . The isobaric volume thermal expansion coefficient (TEC) was obtained as α V P = (5.9291 × 10 −6 ) + (4.9680 × 10 −9 )(T − 298 K) K −1 , from which the corresponding linear TEC was obtained as α L P = (1.9764 × 10 −6 ) + (1.6560 × 10 −9 )(T − 298 K) K −1 . The 3 × 3 matrix representations of the single-crystal isobaric linear TEC and the volume expansivity were obtained for the cubic crystal class to which LaB 6 belongs. Also, the temperature dependence of the lattice parameter data of this study was compared with past landmark studies on LaB 6 by Dutchak et al. [Inorg. Mater. (1972), 8, 1877–1880] and Aivazov et al. [Inorg. Mater. (1979), 15, 1015–1016].

LaB6 standard material↗
DOE OSTI2023

Reactor physics characterization of triply periodic minimal surface-based nuclear fuel lattices

Triply periodic minimal surface (TPMS) lattices are receiving substantial attention in numerous engineering fields due to their impressive topology-driven physical characteristics. TPMS lattices are periodic structures of two distinct intertwined volume domains separated by an area-minimizing surface or wall. TPMS lattices have been observed in nature, such as biological membranes, skeletons, block copolymers, sea urchins, butterfly wings, and equipotential surfaces in crystals. Intriguingly, the topology of TPMS lattices can be easily parametrized via level-set equations and thus are heavily numerically and experimentally studied. Here, a significant research effort is currently applying TPMS lattices for heat exchangers and sinks. This paper extends TPMS lattice applications to nuclear reactor fuel designs, with a focus on identifying relevant TPMS geometric parameters controlling neutronics characteristics, such as reactivity, neutron spectrum, and heat removal properties. We found that fuel surface-area-to-volume ratios for TPMS lattices can be two orders of magnitude larger than current cylindrical fuel rods. Further, the selected TPMS lattice and its implicit equation, the unit cell pitch, wall thickness, and structure porosity are design parameters enabling neutronics optimization for both thermal and fast spectrum configurations, paving the way for exceptionally compact and dense nuclear core concepts.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2021

Ferrotorryweiserite, Rh 5 Fe 10 S 16 , a New Mineral Species from the Sisim Placer Zone, Eastern Sayans, Russia, and the Torryweiserite–Ferrotorryweiserite Series

Ferrotorryweiserite, Rh 5 Fe 10 S 16 , occurs as small grains (≤20 µm) among droplet-like inclusions (up to 50 μm in diameter) of platinum-group minerals (PGM), in association with oberthürite or Rh-bearing pentlandite, laurite, and a Pt-Pd-Fe alloy (likely isoferroplatinum and Fe-Pd-enriched platinum), hosted by placer grains of Os-Ir alloy (≤0.5 mm) in the River Ko deposit. The latter is a part of the Sisim placer zone, which is likely derived from ultramafic units of the Lysanskiy layered complex, southern Krasnoyarskiy kray, Russia. The mineral is opaque, gray to brownish gray in reflected light, very weakly bireflectant, not pleochroic to weakly pleochroic (grayish to light brown tints), and weakly anisotropic. The calculated density is 5.93 g·cm –3 . Mean results (and ranges) of four WDS analyses are: Ir 18.68 (15.55–21.96), Rh 18.34 (16.32–20.32), Pt 0.64 (0.19–1.14), Ru 0.03 (0.00–0.13), Os 0.07 (0.02–0.17), Fe 14.14 (13.63–14.64), Ni 13.63 (12.58–14.66), Cu 4.97 (3.42–6.41), Co 0.09 (0.07–0.11), S 29.06 (28.48–29.44), and total 99.66 wt.%. They correspond to the following formula calculated for a total of 31 atoms per formula unit: (Rh 3.16 Ir 1.72 Pt 0.06 Ru 0.01 Os 0.01 ) Σ 4.95 (Fe 4.48 Ni 4.11 Cu 1.38 Co 0.03 ) Σ10.00 S 16.05 . The results of synchrotron micro-Laue diffraction studies indicate that ferrotorryweiserite is trigonal; its probable space group is $R\bar{3}m$ (#166) based on its Ni-analog, torryweiserite. The unit-cell parameters refined from 177 reflections are a = 7.069 (2) Å, c = 34.286 (11) Å, V = 1484 (1) Å 3 , and Z = 3. The c:a ratio is 4.8502. The strongest eight peaks in the X-ray diffraction pattern derived from results of micro-Laue diffraction study [d in Å(hkil)(I)] are 2.7950 ($20\bar{2}5$) (100); 5.7143 (0006) (60); 1.7671 ($22\bar{4}0$) (44.4); 3.0486 ($20\bar{2}1$) (39.4); 5.7650 ($10\bar{1}2$) (38.6); 2.5956 ($20\bar{2}7$) (37.8); 3.0058 ($11\bar{2}6$) (36.5); and 1.5029 ($4\bar{2}\bar{2}12$) (35.3). Ferrotorryweiserite and the associated PGM crystallized from microvolumes of residual melt at late stages of crystallization of grains of Os- and Ir-dominant alloys occurred in lode zones of chromitites of the Lysanskiy layered complex. In a particular case, the residual melt is disposed peripherally around a core containing a disequilibrium association of magnesian olivine (Fo 72.9–75.6 ) and albite (Ab 81.6–86.4 ), with the development of skeletal crystals of titaniferous augite: Wo 40.8–43.2 En 26.5–29.3 Fs 20.3–22.6 Aeg 6.9–9.5 (2.82–3.12 wt.% TiO 2 ). Ferrotorryweiserite represents the Fe-dominant analog of torryweiserite. We also report occurrences of ferrotorryweiserite in the Marathon deposit, Coldwell Complex, Ontario, Canada, and infer the existence of the torryweiserite–ferrotorryweiserite solid solution in other deposits and complexes.

58 GEOSCIENCES↗
DOE OSTI2024

A contactless in situ EFISH method for measuring electrostatic potential profile of semiconductor/electrolyte junctions

In photoelectrochemical cells, promising devices for directly converting solar energy into storable chemical fuels, the spatial variation of the electrostatic potential across the semiconductor–electrolyte junction is the key parameter that determines the cell performance. In principle, electric field induced second harmonic generation (EFISH) provides a contactless in situ spectroscopic tool to measure the spatial variation of electrostatic potential. However, the total second harmonic generation (SHG) signal contains the contributions of the EFISH signals of semiconductor space charge layer and the electric double layer, in addition to the SHG signal of the electrode surface. The interference of these complex quantities hinders their analysis. In this work, to understand and deconvolute their contributions to the total SHG signals, bias-dependent SHG measurements are performed on the rutile TiO2(100)–electrolyte junction as a function of light polarization and crystal azimuthal angle (angle of the incident plane relative to the crystal [001] axis). A quadratic response between SHG intensity and the applied potential is observed in both the accumulation and depletion regions of TiO2. The relative phase difference and amplitude ratio are extracted at selected azimuthal angles and light polarizations. At 0° azimuthal angle and s-in–p-out polarization, the SHG intensity minimum has the best match with the TiO2 flatband potential due to the orthogonal relative phase difference between bias-dependent and bias-independent SHG terms. We further measure the pH-dependent flatband potential and probe the photovoltage under open circuit conditions using the EFISH technique, demonstrating the capability of this contactless method for measuring electrostatic potential at semiconductor–electrolyte junctions.

Chemistry↗
DOE OSTI2020

A fixed-target platform for serial femtosecond crystallography in a hydrated environment

For serial femtosecond crystallography at X-ray free-electron lasers, which entails collection of single-pulse diffraction patterns from a constantly refreshed supply of microcrystalline sample, delivery of the sample into the X-ray beam path while maintaining low background remains a technical challenge for some experiments, especially where this methodology is applied to relatively low-ordered samples or those difficult to purify and crystallize in large quantities. This work demonstrates a scheme to encapsulate biological samples using polymer thin films and graphene to maintain sample hydration in vacuum conditions. The encapsulated sample is delivered into the X-ray beam on fixed targets for rapid scanning using the Roadrunner fixed-target system towards a long-term goal of low-background measurements on weakly diffracting samples. As a proof of principle, we used microcrystals of the 24 kDa rapid encystment protein (REP24) to provide a benchmark for polymer/graphene sandwich performance. The REP24 microcrystal unit cell obtained from our sandwiched in-vacuum sample was consistent with previously established unit-cell parameters and with those measured by us without encapsulation in humidified helium, indicating that the platform is robust against evaporative losses. While significant scattering from water was observed because of the sample-deposition method, the polymer/graphene sandwich itself was shown to contribute minimally to background scattering.

36 MATERIALS SCIENCE↗