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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

Development of a liquid-helium free cryogenic sample holder with mK temperature control for autonomous electron microscopy

The automated and autonomous cryogenic transmission electron microscopy (Cryo-EM) demands a sample holder capable of maintaining temperatures below 10 K with precise control, long holding times, and minimal helium use. Rising to this challenge, we initiated an ambitious project to develop a novel closed-cycle cryocooler-based cryogenic sample holder that operates without the use of liquid helium and the consumption of gaseous helium. Here, this article presents the design, construction, and experimental testing of the initial prototype, which achieves an ultimate temperature of 5.6 K with exceptional stability close to 1mK, while providing a wide temperature control range from 295 K to 5.6 K, marking a clear advancement in cryo-EM holder development. While the prototype was not designed for atomic resolution imaging and thus lacks a sturdy support system to mitigate mechanical vibrations from the cryocooler's pulsed tube, this innovative approach successfully demonstrates proof of concept. It offers unprecedented capabilities for state-of-the-art cryogenic microscopy and microanalysis in materials and biological sciences.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2013

Cryogenic Liquid Sample Acquisition System for Remote Space Applications

There is a need to acquire autonomously cryogenic hydrocarbon liquid sample from remote planetary locations such as the lakes of Titan for instruments such as mass spectrometers. There are several problems that had to be solved relative to collecting the right amount of cryogenic liquid sample into a warmer spacecraft, such as not allowing the sample to boil off or fractionate too early; controlling the intermediate and final pressures within carefully designed volumes; designing for various particulates and viscosities; designing to thermal, mass, and power-limited spacecraft interfaces; and reducing risk. Prior art inlets for similar instruments in spaceflight were designed primarily for atmospheric gas sampling and are not useful for this front-end application. These cryogenic liquid sample acquisition system designs for remote space applications allow for remote, autonomous, controlled sample collections of a range of challenging cryogenic sample types. The design can control the size of the sample, prevent fractionation, control pressures at various stages, and allow for various liquid sample levels. It is capable of collecting repeated samples autonomously in difficult lowtemperature conditions often found in planetary missions. It is capable of collecting samples for use by instruments from difficult sample types such as cryogenic hydrocarbon (methane, ethane, and propane) mixtures with solid particulates such as found on Titan. The design with a warm actuated valve is compatible with various spacecraft thermal and structural interfaces. The design uses controlled volumes, heaters, inlet and vent tubes, a cryogenic valve seat, inlet screens, temperature and cryogenic liquid sensors, seals, and vents to accomplish its task.

Mahaffy, Paul↗
DOE OSTI2020

Selective NMR observation of the SEI–metal interface by dynamic nuclear polarisation from lithium metal

While lithium metal represents the ultimate high-energy-density battery anode material, its use is limited by dendrite formation and associated safety risks, motivating studies of the solid–electrolyte interphase layer that forms on the lithium, which is key in controlling lithium metal deposition. Dynamic nuclear polarisation enhanced NMR can provide important structural information; however, typical exogenous dynamic nuclear polarisation experiments, in which organic radicals are added to the sample, require cryogenic sample cooling and are not selective for the interface between the metal and the solid–electrolyte interphase. Here we instead exploit the conduction electrons of lithium metal to achieve an order of magnitude hyperpolarisation at room temperature. We enhance the 7 Li, 1 H and 19 F NMR spectra of solid–electrolyte interphase species selectively, revealing their chemical nature and spatial distribution. These experiments pave the way for more ambitious room temperature in situ dynamic nuclear polarisation studies of batteries and the selective enhancement of metal–solid interfaces in a wider range of systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1979

Trace constituent mixing ratios in the lower stratosphere during the 1977 intertropical convergence zone experiment

Minor constituents in the atmosphere can play an important role as tracers in studies of atmospheric transport and mixing. Simultaneous measurements of the vertical distribution of trace constituents in the troposphere and lower stratosphere were conducted in the region of the Intertropical Convergence Zone (ITCZ). An effort was made to measure the mixing ratios of selected trace constituents. A cryogenic sampling system on board a U-2 aircraft was used to acquire whole-air samples and to cryogenically collect samples at 13.7 to 21.3 km. Simultaneous tropospheric measurements using whole-air sampling canisters on board a Learjet aircraft were also carried out.

Vedder, J. F.↗
DOE OSTI2023

Towards resolving protein structures at the atomic scale using atom probe tomography

In the field of Structural Biology, Atom Probe Tomography (APT) is in the nascent stages of development wherein coarse-grained visuals of proteins have been captured. The characterization of organic samples or biomolecules through the technique is currently limited to the detection of a few dominant signatures. The problem of indecipherable characterization can inherently be traced back to multiple forms of technique-specific responses to organic samples and consequent triggers leading to organic-sample and sample-medium interactions. While it is possible for captured manifestations of protein reconstructions to seemingly appear intact from a basic visual purview, the parameter-protein associative responses throughout the structure as a direct consequence of the inherent workings of the technique (until harmonized with organic sample complexity and behavior) and field evaporation-based factors make non-aberrative atomic associations infeasible. The work focused on identifying and theorizing the (above stated and other) fundamental mechanisms that stronghold the study of intricate atomic to higher order associations in proteins through APT. Attempts at structure elucidation of the cryogenic sample under study, through indirect associations (and methods) based on other imaging techniques, further revealed the distinct and highly distortive nature at the atomic scale deterring structural tunability and thus characterization of APT based cryogenic samples under analysis. As a direct counter to the atomic scale characterization problem, by taking the experiment-specific uncertainties, and probable APT-centric organic sample-based variabilities into account, a basic result is extracted and presented. Through mass-spectrometric and computational analysis, specific individual amino acids (Sulfur-containing protein-bound amino acids) in proteins and aspects of protein structure (probable backbone fragments, partial sequence - partial backbone portions) have been identified and characterized. Under analysis considerations, a few of the simplest known and easily inferable segments that favor structural deteriorations in the reconstructions are stated. Additionally, to overcome technique-specific deterrents to the characterization of biomolecules in cryogenic sample medium, the development of a protein-labeling strategy tailored to APT is suggested.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS2018

Lunar Sample Return Entry Systems Analysis

The Lunar Prospector and Clementine missions have revealed deposits of water-ice located at the South Pole-Aitken Basin of the lunar surface. Due to the scarce amount of previous successful sample return missions and the recent discovery of water-ice, the National Research Council (NRC) Decadal Survey recommended prioritizing the development of a Lunar Sample Return Mission Architecture. The NRC Decadal survey ranked the return of cryogenic samples that could potentially aid in current scientific investigations and identify sites for in-situ resource utilization to support future exploration missions. This study aims to identify the key technical challenges and operational constraints involved in returning cryogenic samples in pristine condition. A detailed classification of defined ground rules and assumptions, justification of mission events and high level functional requirements reinforces the proposed concept of operations. In support of the drafted architecture, a comprehensive analysis on design and environmental constraints are documented for the Earth return vehicle, sample container and thermal protection entry system. The design and thermal analysis is comprised of quantitative dimensions for mass and volume, flight performance parameters and thermal system performance limitations. Further refinement of the high level functional requirements is imperative for determining the optimal approach for returning cryopreserved lunar samples.

Lunar Sample Return↗
NASA NTRS2009

Apparatus Measures Thermal Conductance Through a Thin Sample from Cryogenic to Room Temperature

An apparatus allows the measurement of the thermal conductance across a thin sample clamped between metal plates, including thermal boundary resistances. It allows in-situ variation of the clamping force from zero to 30 lb (133.4 N), and variation of the sample temperature between 40 and 300 K. It has a special design feature that minimizes the effect of thermal radiation on this measurement. The apparatus includes a heater plate sandwiched between two identical thin samples. On the side of each sample opposite the heater plate is a cold plate. In order to take data, the heater plate is controlled at a slightly higher temperature than the two cold plates, which are controlled at a single lower temperature. The steady-state controlling power supplied to the hot plate, the area and thickness of samples, and the temperature drop across the samples are then used in a simple calculation of the thermal conductance. The conductance measurements can be taken at arbitrary temperatures down to about 40 K, as the entire setup is cooled by a mechanical cryocooler. The specific geometry combined with the pneumatic clamping force control system and the steady-state temperature control approach make this a unique apparatus.

Tuttle, James G.↗
NASA NTRS1997

Thermal Design and Analysis for the Cryogenic MIDAS Experiment

The Materials In Devices As Superconductors (MIDAS) spaceflight experiment is a NASA payload which launched in September 1996 on the Shuttle, and was transferred to the Mir Space Station for several months of operation. MIDAS was developed and built at NASA Langley Research Center (LaRC). The primary objective of the experiment was to determine the effects of microgravity and spaceflight on the electrical properties of high-temperature superconductive (HTS) materials. The thermal challenge on MIDAS was to maintain the superconductive specimens at or below 80 K for the entire operation of the experiment, including all ground testing and 90 days of spaceflight operation. Cooling was provided by a small tactical cryocooler. The superconductive specimens and the coldfinger of the cryocooler were mounted in a vacuum chamber, with vacuum levels maintained by an ion pump. The entire experiment was mounted for operation in a stowage locker inside Mir, with the only heat dissipation capability provided by a cooling fan exhausting to the habitable compartment. The thermal environment on Mir can potentially vary over the range 5 to 40 C; this was the range used in testing, and this wide range adds to the difficulty in managing the power dissipated from the experiment's active components. Many issues in the thermal design are discussed, including: thermal isolation methods for the cryogenic samples; design for cooling to cryogenic temperatures; cryogenic epoxy bonds; management of ambient temperature components self-heating; and fan cooling of the enclosed locker. Results of the design are also considered, including the thermal gradients across the HTS samples and cryogenic thermal strap, electronics and thermal sensor cryogenic performance, and differences between ground and flight performance. Modeling was performed in both SINDA-85 and MSC/PATRAN (with direct geometry import from the CAD design tool Pro/Engineer). Advantages of both types of models are discussed. Correlation of several models to ground testing and flight data (where available) is presented. Both SINDA and PATRAN models predicted the actual thermal performance of the experiment well, even without post-flight correlation adjustments of the models.

Amundsen, Ruth McElroy↗
DOE OSTI2022

CRADA Number NFE-19-07867 with Neptune Fluid Flow Systems (CRADA Final Report)

Neptune Fluid Flow Systems is a rising engineering firm with a technology focus in improving cryogenic sample preparation for cryogenic-transmission electron microscopy (cryo-TEM) studies. To advance the R&D of its innovative cryogenic preparation method, Neptune has teamed up with the Center for Nanophase Materials Science (CNMS) at Oak Ridge National Laboratory (ORNL) to achieve the following aims: (1) validate the technical feasibility of CryoSheet sample prep method, (2) design, fabricate and test the cryo-stage support, and (3) experiment and achieve success with the novel sample preparation method on different soft matters.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Commissioning of a two-target DC cylindrical magnetron sputter coater for depositing Nb 3 Sn film on Nb superconducting radiofrequency cavities

A DC cylindrical magnetron sputter coater was commissioned and used to coat Nb 2.6 GHz superconducting radiofrequency (SRF) cavity with Nb 3 Sn. The sputter coater has two identical cylindrical magnetrons that can move, with a controlled speed, along the axis of the SRF cavity to coat the inside surface of the cavity. The design of the sputter coater is discussed, along with its performance. Initially, a sample holder that allows coating on flat substrates at positions similar to the equator and beam tubes of a 2.6 GHz SRF cavity was used to test conditions for fabricating Nb 3 Sn layers. Multilayers of Nb and Sn were sequentially sputtered on flat Nb and sapphire substrates mounted on the equivalent positions of the cavity's beam tubes and the equator using the two identical cylindrical magnetrons. Then, the Nb/Sn multilayers were annealed at 950 °C for 3 h. Here, the ~1.2 μm thick Nb 3 Sn film did not show any other Nb–Sn compounds and had a superconducting transition temperature of 17.61–17.76 K. The 2.6 GHz SRF cavity was coated using similar conditions as flat samples. Cryogenic RF testing of the Nb 3 Sn-coated cavity demonstrated a quality factor of 3.2 × 10 8 at an accelerating gradient of 5 MV/m at 4.4 K.

43 PARTICLE ACCELERATORS↗
DOE OSTI2021

Electrical and Thermal Properties of Cold-Sprayed Bulk Copper and Copper-Tungsten Samples at Cryogenic Temperatures

The de­vel­op­ment of high ther­mal con­duc­tiv­ity coat­ings with pure cop­per or cop­per-tung­sten alloy could be ben­e­fi­cial to im­prove the heat trans­fer of bulk Nb cav­i­ties for con­duc­tion cool­ing ap­pli­ca­tions and to in­crease the stiff­ness of bulk Nb cav­i­ties cooled by liq­uid he­lium. Cold-spray is an ad­di­tive man­u­fac­tur­ing tech­nique suit­able to grow thick coat­ings of ei­ther Cu or CuW on a Nb sub­strate. Bulk (~5 mm thick) coat­ings of Cu and CuW were de­posited on stan­dard 3 mm thick, high-pu­rity Nb sam­ples and smaller sam­ples with 2 mm x 2 mm cross sec­tion were cut for mea­sur­ing the ther­mal con­duc­tiv­ity and the resid­ual re­sis­tiv­ity ratio. The sam­ples were sub­jected to an­neal­ing at dif­fer­ent tem­per­a­tures and a max­i­mum RRR of ~130 and ~40 were mea­sured for the Cu sam­ples and CuW sam­ples, re­spec­tively.

Pokhrel, H.↗
DOE OSTI2022

Streptavidin Affinity Grids for the Preparation of Biological Samples for Cryogenic Electron Microscopy (CRADA Final Report)

Currently, cryo-EM is the most powerful tool for structural analysis of large biomacromolecules, but there are still problems in that biomacromolecules are denatured at the air-interface and their orientations are limited in a specific orientation. We solved this problem at LBL by developing a streptavidin-coated EM grid. Use of such affinity-binding grids can minimize exposure to air-interface by keeping biomacromolecules bound to streptavidin. It is urgently needed to make such grids readily available to the cryo-EM community, but they are somewhat difficult to make. The goal of the CRADA with Hummingbird company was to mass-produce the streptavidin grids so that they would become readily available to the cryo-EM community. Our contribution to the CRADA was to first help Hummingbird to replicate the manual process that we use, and this was completed successfully.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

Electrical and Thermal Properties of Cold-Sprayed Bulk Copper and Copper-Tungsten Samples at Cryogenic Temperatures

The de­vel­op­ment of high ther­mal con­duc­tiv­ity coat­ings with pure cop­per or cop­per-tung­sten alloy could be ben­e­fi­cial to im­prove the heat trans­fer of bulk Nb cav­i­ties for con­duc­tion cool­ing ap­pli­ca­tions and to in­crease the stiff­ness of bulk Nb cav­i­ties cooled by liq­uid he­lium. Cold-spray is an ad­di­tive man­u­fac­tur­ing tech­nique suit­able to grow thick coat­ings of ei­ther Cu or CuW on a Nb sub­strate. Bulk (~5 mm thick) coat­ings of Cu and CuW were de­posited on stan­dard 3 mm thick, high-pu­rity Nb sam­ples and smaller sam­ples with 2 mm x 2 mm cross sec­tion were cut for mea­sur­ing the ther­mal con­duc­tiv­ity and the resid­ual re­sis­tiv­ity ratio. The sam­ples were sub­jected to an­neal­ing at dif­fer­ent tem­per­a­tures and a max­i­mum RRR of ~130 and ~40 were mea­sured for the Cu sam­ples and CuW sam­ples, re­spec­tively.

Pokhrel, H.↗
NASA NTRS1982

Precursor gases of aerosols in the Mount St. Helens eruption plumes at stratospheric altitudes

Nineteen stratospheric samples from the eruption plumes of Mount St. Helens were collected in five flight experiments. The plume samples were collected at various altitudes from 13.1 to 20.7 km by using the Ames cryogenic sampling system on board the NASA U-2 aircraft. The enriched, cryogenically collected samples were analyzed by chromatography. The concentrations of aerosols precursor gases (OCS, SO2, and CS2), CH3Cl, N2O, CF2Cl2, and CFCl3 were measured by gas chromatography. Large enhancement of the mixing ratio of SO2 and moderate enhancement of CS2 and OCS were found in the plume samples compared with similar measurement under pre-volcanic conditions. A fast decay rate of the SO2 mixing ratio in the plume was observed. Measurement of Cl(-), SO2(2-), and NO3(-) by ion chromatography was also carried out on water solutions prepared from the plume samples. The results obtained with this technique imply large mixing ratios of HCl, (NO + NO2 + HNO3), and SO2, in which these constituents are the respective sources of the anions. Measurement of the Rn222 concentration in the plume was made. Other stratospheric constituents in the plume samples, such as H2O, CO2, CH4, and CO, were also observed.

Inn, E. C. Y.↗
NASA NTRSDate not supplied

Titan Sample Return Using In Situ Propellants: NIAC Phase I Study Status

Status of NIAC Phase I study for NIAC Symposium (remote). An overview of the Insitu Titan Sample Return concept. The Compass team developed a concept to return 3 kg of cryogenic samples from the surface of Saturn's moon Titan by gathering ~3000 kg of ice and methane to fuel an inflatable, 3 stage launch vehicle to propel a return vehicle and aeroshell back to earth. Note: This presentation does not include voice information and is not available for this record.

Titan↗
NASA NTRS1983

Sample Holder for Cryogenic Adhesive Shear Test

Five samples tested in one cooldown. Holder mounted in testing machine. Submerged in cryogenic liquid held in cryostat. Movable crosshead of testing machine moves gradually downward. Samples placed under tension, one after another, starting with top one; each sample fails in turn before next is stressed.

Ledbetter, F. E.↗