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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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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Thermal deflection in neutron scattering sample environments at Oak Ridge National Laboratory

The neutron sources at Oak Ridge National Laboratory use a wide suite of sample environment equipment to deliver extreme conditions for a number of experiments. Much of this instrumentation focuses on extremes of temperature, such as cryostats, closed-cycle refrigerators in both low and high temperature configurations, and radiant heating furnaces. When the temperature is controlled across a large range, thermal deflection effects can notably move the sample and affect its alignment in the beam. Here, we combine these sample environments with neutron imaging and machine vision to determine the motion of a representative sample with respect to the neutron beam. We find vertical sample displacement on the order of 1–2 mm and horizontal displacement that varies from near-negligible to 1.2 mm. While these deflections are not relevant for some of the beamlines at the first target station at the spallation neutron source and the high flux isotope reactor, they will become critical for upcoming instrumentation at the second target station, as well as any instruments targeting sub-mm samples, as neutron sources and optics evolve to smaller and more focused beams. We discuss mitigation protocols and potential modifications to the environment to minimize the effect of misalignment due to thermal deflection.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Multimodal Ambient Pressure Sample Environment for the HIPPIE Solid-Gas Endstation at MAX IV Laboratory

The HIPPIE APXPS instruments have undergone several major upgrades, such as developing a dedicated solid gas endstation to specialize in multimodal ambient pressure sample environments centered around X-ray photoelectron spectroscopy. Herein, the technical specifications of the HIPPIE solid gas endstation are detailed; upgrades to the laser heating and gas systems, as well as the addition of an offline 1 bar reactor, are introduced. To demonstrate how the endstation is currently being utilized, scientific examples of all upgrades are presented, as well as science cases using infrared reflection-adsorption spectroscopy. The HIPPIE solid gas endstation is maturing into an instrument offering bespoke sample environments aimed at pushing experimental capabilities, especially in the time-resolved domain.

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

Sample environment effects on synchrotron-measured temperature profiles in an approximant of optical floating zone crystal growth

Even though the growth of crystals using optical floating zone furnaces has had an immense scientific impact, the implementation of this method remains more of an art than a science due to the difficulty of obtaining quantitative information about the sample thermal profile during crystal growth. Building on recent work demonstrating that in situ synchrotron studies can be used to map sample rod temperatures during heating, investigations were carried out to better understand how the sample environment affects the sample temperature profile. Through a combination of experimental studies and modeling efforts, it is shown that the environment in the furnace can strongly influence the sample temperature at the lamp focus, the steepness of the vertical temperature gradient, and the timescale required for sample heating and cooling - effects which can combine to produce a strong history-dependence to sample temperature profiles. It is demonstrated that the furnace effects can be effectively captured in thermal models, allowing both the steady-state and time-dependent behavior of the sample to be accurately reproduced with predictive models, and providing a launching point for improved furnace designs that can more readily deliver desired thermal profiles.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Past, present and future—sample environments for materials research studies in scattering and spectroscopy; a UK perspective

Small Angle X-Ray Scattering (SAXS) and X-Ray Absorption Fine Structure (XAFS) are two techniques that have been employed at synchrotron sources ever since their inception. Over the course of the development of the techniques, the introduction of sample environments for added value experiments has grown dramatically. This article reviews past successes, current developments and an exploration of future possibilities for these two X-ray techniques with an emphasis on the developments in the United Kingdom between 1980-2020.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Soft Matter Sample Environments for Time-Resolved Small Angle Neutron Scattering Experiments: A Review

With the promise of new, more powerful neutron sources in the future, the possibilities for time-resolved neutron scattering experiments will improve and are bound to gain in interest. While there is already a large body of work on the accurate control of temperature, pressure, and magnetic fields for static experiments, this field is less well developed for time-resolved experiments on soft condensed matter and biomaterials. We present here an overview of different sample environments and technique combinations that have been developed so far and which might inspire further developments so that one can take full advantage of both the existing facilities as well as the possibilities that future high intensity neutron sources will offer.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
NASA NTRS1971

Preliminary description of Apollo 15 sample environments

Approximately 78 kg of lunar rock and soil samples were returned by Apollo 15. The rather complete documentation of the locations of nearly all of the samples allows for relating the samples to the specific and detailed geologic environments from which they were collected. This is especially important in an area as geologically complex as the Hadley-Apennine site. All of the material presented was derived from the pre-mission photogeologic maps, lunar surface television video tapes, air-to-ground transcript and crew debriefings, photographs taken on the lunar surface by the Apollo 15 crew, and information supplied by the Lunar Sample Preliminary Examination team from which the samples were categorized into groups consisting of, broadly, basalts and breccias. The breccias are considered loosely in terms of coherent breccias and soil breccias.

Swann, G. A.↗
NASA NTRS2004

Comparison of Classical and Charge Storage Methods for Determining Conductivity of Thin Film Insulators

Conductivity of insulating materials is a key parameter to determine how accumulated charge will distribute across the spacecraft and how rapidly charge imbalance will dissipate. Classical ASTM and IEC methods to measure thin film insulator conductivity apply a constant voltage to two electrodes around the sample and measure the resulting current for tens of minutes. However, conductivity is more appropriately measured for spacecraft charging applications as the "decay" of charge deposited on the surface of an insulator. Charge decay methods expose one side of the insulator in vacuum to sequences of charged particles, light, and plasma, with a metal electrode attached to the other side of the insulator. Data are obtained by capacitive coupling to measure both the resulting voltage on the open surface and emission of electrons from the exposed surface, as well monitoring currents to the electrode. Instrumentation for both classical and charge storage decay methods has been developed and tested at Jet Propulsion Laboratory (JPL) and at Utah State University (USU). Details of the apparatus, test methods and data analysis are given here. The JPL charge storage decay chamber is a first-generation instrument, designed to make detailed measurements on only three to five samples at a time. Because samples must typically be tested for over a month, a second-generation high sample throughput charge storage decay chamber was developed at USU with the capability of testing up to 32 samples simultaneously. Details are provided about the instrumentation to measure surface charge and current; for charge deposition apparatus and control; the sample holders to properly isolate the mounted samples; the sample carousel to rotate samples into place; the control of the sample environment including sample vacuum, ambient gas, and sample temperature; and the computer control and data acquisition systems. Measurements are compared here for a number of thin film insulators using both methods at both facilities. We have found that conductivity determined from charge storage decay methods is 102 to 104 larger than values obtained from classical methods. Another Spacecraft Charging Conference presentation describes more extensive measurements made with these apparatus. This work is supported through funding from the NASA Space Environments and Effects Program and the USU Space Dynamics Laboratory Enabling Technologies Program.

Swaminathan, Prasanna↗
NASA NTRS1976

Low cycle fatigue life of two nickel-base casting alloys in a hydrogen environment

Samples of two nickel-base casting alloys, Mar-M-246 (a Martin Company alloy) and 713LC (a low-carbon modification of the alloy 713C developed by International Nickel Company) were tested as candidate materials for the high-pressure fuel and high-pressure oxidizer turbopump turbine nozzles. The samples were subjected to tensile tests and to low cycle fatigue tests in high-pressure hydrogen to study the influence of the hydrogen environment. The Mar-M-246 material was found to have a three times higher cyclic life in hydrogen than the 713LC alloy, and was selected as the nozzle material.

Cooper, R. A.↗
NASA NTRS1983

Stability of silica heat shield materials in the Space Shuttle environment

Sample tiles of Space Shuttle reusable surface insulation (RSI) and fibrous refractory composite insulation (FRCI) have been alternately exposed to simulated mission heating and the Kennedy Space Center launch-pad environment for up to 50 cycles. The two types of tiles were coated with an identical glass composition. The coating on RSI tiles was prone to cracking in the test environment while the same coating on FRCI was not. Absorption of water contaminated with environmental deposits resulted in accelerated devitrification in the RSI tiles. Devitrification in FRCI tiles was significantly less. The rate of environmental degradation of tiles appeared to be dependent on the amount of water absorption.

Ransone, P. O.↗
NASA NTRS1981

Long-time stress relaxation of a filled elastomer in vacuum environments

Samples of a filled elastomeric ablative material were stored at 45 C and 10 to the -6th torr for 7 months. Their tensile stress-relaxation modulus at constant strain was measured throughout the 7 months. Results of the testing are discussed primarily by comparisons of the data to atmospheric-pressure moduli (determined in this work for shorter periods of time) and with moduli predicted from short-time testing. Confirmation of the strengthening effects of vacuum on this composite was obtained. The use of time-temperature superposition techniques as an approximate accelerated testing procedure for this material under these conditions was also verified.

Ward, T. C.↗
DOE OSTI2022

PIONEER, a high-resolution single-crystal polarized neutron diffractometer

PIONEER is a high Q-resolution, single-crystal, polarized neutron diffractometer at the Second Target Station (STS), Oak Ridge National Laboratory. It will provide the unprecedented capability of measuring tiny crystals (0.001 mm 3 , i.e., x-ray diffraction size), ultra-thin films (10 nm thickness), and weak structural and magnetic transitions. PIONEER benefits from the increased peak brightness of STS cold-neutron sources and uses advanced Montel mirrors that are able to deliver a focused beam with a high brilliance transfer, a homogeneous profile, and a low background. Monte Carlo simulations suggest that the optimized instrument has a high theoretical peak brilliance of 2.9 × 10 12 n cm -2 sr -1 Å -1 s -1 at 2.5 Å at the sample position, within a 5 × 5 mm 2 region and a ±0.3° divergence range. The moderator-to-sample distance is 60 m, providing a nominal wavelength band of 4.3 Å with a wavelength resolution better than 0.2% in the wavelength range of 1.0–6.0 Å. PIONEER is capable of characterizing large-scale periodic structures up to 200 Å. With a sample-to-detector distance of 0.8 m, PIONEER accommodates various sample environments, including low/high temperature, high pressure, and high magnetic/electric field. Additionally, a large cylindrical detector array (4.0 sr) with a radial collimator is planned to suppress the background scattering from sample environments. Bottom detector banks provide an additional 0.4 sr coverage or can be removed if needed to accommodate special sample environments. We present virtual experimental results to demonstrate the scientific performance of PIONEER in measuring tiny samples.

47 OTHER INSTRUMENTATION↗
NASA NTRS2018

Potential High Priority Subaerial Environments for Mars Sample Return

Subaerial environments of interest for Mars Sample Return include surface or near-surface sites not covered by a body of water, but having direct access to water from precipitation, snow melt, or ambient-temperature groundwater. This includes soils, wetlands, ephemeral ponds, cold springs, and periglacial/glacial environments, with paleosol profiles as a high priority collection site. Such soils can be topped by aqueously deposited sediments and precipitates from wetlands, ephemeral ponds, and springs. The composition and morphology of paleosols preserve evidence of past climate, aqueous conditions, and life. Key topics addressed by samples collected from subaerial environments include: 1) Constrain the duration of interaction with liquid water by investigating a weathering profile from the surface to unaltered parent material. 2) Assess the characteristics of past liquid water, and how it has changed through time. 3) Investigate weathered materials such as soils, paleosols, sediments, weathering rinds or rock coatings to assess past climate. 4) Examine characteristics of past aeolian and atmospheric processes.

Source record↗
DOE OSTI2021

Probing Phase Transitions and Magnetism in Minerals with Neutrons

We report the development of sophisticated sample environments to control temperature, pressure, and magnetic field has grown in parallel with neutron source and instrumentation development. High-pressure apparatus, with high- and low-temperature capability, novel designs for diamond cells, and large volume presses are matched with next-generation neutron sources and moderator designs to provide unprecedented neutron beam brightness. Recent developments in sample environments are expanding the pressure–temperature space accessible to neutron scattering experiments. Researchers are using new capabilities and an increased understanding of the fundamentals of structural and magnetic transitions to explore new territories, including hydrogenous minerals (e.g., ices and hydrates) and magnetic structural phase diagrams.

58 GEOSCIENCES↗
DOE OSTI2024

Advanced manufacturing provides tailor-made solutions for crystallography with x-ray free-electron lasers

Serial crystallography at large facilities, such as x-ray free-electron lasers and synchrotrons, evolved as a powerful method for the high-resolution structural investigation of proteins that are critical for human health, thus advancing drug discovery and novel therapies. However, a critical barrier to successful serial crystallography experiments lies in the efficient handling of the protein microcrystals and solutions at microscales. Microfluidics are the obvious approach for any high-throughput, nano-to-microliter sample handling, that also requires design flexibility and rapid prototyping to deal with the variable shapes, sizes, and density of crystals. Here, we discuss recent advances in polymer 3D printing for microfluidics-based serial crystallography research and present a demonstration of emerging, large-scale, nano-3D printing approaches leading into the future of 3D sample environment and delivery device fabrication from liquid jet gas-dynamic virtual nozzles devices to fixed-target sample environment technology.

36 MATERIALS SCIENCE↗