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DOE OSTI2026

Advanced Manufacturing of Cathode Materials for Lithium-ion Batteries

Original objectives (per the Statement of Project Objectives) centered on developing and translating a continuous pilot process for cathode materials production while targeting (i) a 29% manufacturing cost reduction, (ii) an 82% energy consumption reduction for cathode production, and (iii) a doubling of manufacturing productivity. Planned validation included characterization at appropriate analytical facilities and electrochemical performance evaluation progressing from half-cells to pouch-cell formats, with a pathway to kilogram-scale production of finished cathode materials for representative testing. Scope evolution: During execution, the project team identified that the surfactant-enabled chemistry offered high selectivity for lithium precipitation from brine sources. A formal scope revision shifted the final project year from cathode manufacturing development to direct lithium extraction/lithium recovery, while maintaining the overarching intent of cost reduction and process simplification relevant to the battery supply chain.

25 ENERGY STORAGE↗

DOE OSTI2024

Giant elastocaloric effect at low temperatures in TmVO 4 and implications for cryogenic cooling

Adiabatic decompression of paraquadrupolar materials has significant potential as a cryogenic cooling technology. We focus on TmVO 4 , an archetypal material that undergoes a continuous phase transition to a ferroquadrupole-ordered state at 2.15 K. Above the phase transition, each Tm ion contributes an entropy of k B ln 2 due to the degeneracy of the crystal electric field groundstate. Owing to the large magnetoelastic coupling, which is a prerequisite for a material to undergo a phase transition via the cooperative Jahn–Teller effect, this level splitting, and hence the entropy, can be readily tuned by externally induced strain. Using a dynamic technique in which the strain is rapidly oscillated, we measure the adiabatic elastocaloric response of single-crystal TmVO 4 , and thus experimentally obtain the entropy landscape as a function of strain and temperature. The measurement confirms the suitability of this class of materials for cryogenic cooling applications and provides insight into the dynamic quadrupole strain susceptibility.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS2013

Using Combustion Synthesis to Reinforce Berms and Other Regolith Structures

The Moonraker Excavator and other tools under development for use on the Moon, Mars, and asteroids will be employed to construct a number of civil engineering projects and to mine the soil. Mounds of loose soil will be subject to the local transport mechanisms plus artificial mechanisms such as blast effects from landers and erosion from surface vehicles. Some of these structures will require some permanence, with a minimum of maintenance and upkeep. Combustion Synthesis (CS) is a family of processes and techniques whereby chemistry is used to transform materials, often creating flame in a hard vacuum. CS can be used to stabilize civil engineering works such as berms, habitat shielding, ramps, pads, roadways, and the like. The method is to unroll thin sheets of CS fabric between layers of regolith and then fire the fabric, creating a continuous sheet of crusty material to be interposed among layers of loose regolith. The combination of low-energy processes, ISRU (in situ resource utilization) excavator, and CS fabrics, seems compelling as a general method for establishing structures of some permanence and utility, especially in the role of robotic missions as precursors to manned exploration and settlement. In robotic precursory missions, excavator/ mobility ensembles mine the Lunar surface, erect constructions of soil, and dispense sheets of CS fabrics that are covered with layers of soil, fired, and then again covered with layers of soil, iterating until the desired dimensions and forms are achieved. At the base of each berm, for example, is a shallow trench lined with CS fabric, fired and filled, mounded, and then covered and fired, iteratively to provide a footing against lateral shear. A larger trench is host to a habitat module, backfilled, covered with fabric, covered with soil, and fired. Covering the applied CS fabric with layers of soil before firing allows the resulting matrix to incorporate soil both above and below the fabric ply into the fused layer, developing a very irregular surface which, like sandpaper, can provide an anchor for loose soil. CS fabrics employ a coarse fiberglass weave that persists as reinforcement for the fired material. The fiberglass softens at a temperature that exceeds the combustion temperature by factors of two to three, and withstands the installation process. This type of structure should be more resistant to rocket blast effects from Lunar landers.

Rodriquez, Gary↗

DOE OSTI2026

Refining a Novel Process Monitoring Method to Safeguard Continuously Cycling Designs Using Isotopic Ratios

In advanced reactor (AR) designs, a common feature is continuous chemical processing and circulation of the nuclear material. This work bridges a significant measurement gap in safeguarding reactors with circulating fuel or continuous refueling by leveraging and building on the isotope ratio method first developed by our team under an FY21 Advanced Reactors International Safeguards Engagement (ARISE) project (Uribe et al. 2021). In circulating fuel designs, the radioisotope inventory changes from traditional effects (e.g., radioactive decay, fission) but also includes material transport due to pressure and temperature gradients. Such designs may also require regular or continuous additions or removals during operation, which significantly increases the rate of inventory change compared to traditional pressurized water reactor (PWR)s. Thus, directly tracking the nuclear inventory is ineffective since the isotopes are continuously added and removed. The isotope ratio method instead focuses on detecting changes to the input and output flows of radioisotopes. Previous work showed that for well-chosen pairs of isotopes, the isotopic ratio provides a sensitive and lasting indicator of deviation from normal conditions (e.g., startup, shutdown, diversion). The isotope ratio method is a process monitoring method with potential for application in for forward-looking approaches to International Atomic Energy Agency (IAEA) safeguards. The original process monitoring method was developed for a specific case—the decay tank of a thorium-fueled molten salt breeder reactor. In this expanded work, we explored other types of reactors and processes with nonstationary (e.g., flowing) nuclear material, which are difficult to safeguard with traditional methods because of the transient nature of the systems. The goal of the present work is to generalize the isotope ratio method for use in processes with continuously flowing nuclear material. All continuous processes have an average time for isotopes to be replaced in the system. The isotope ratio method works by choosing radioisotopes with half-lives both above and below the processing time. The present work seeks to explore which isotopes are suitable for the method by simulating the nuclear inventory, radioisotope emissions, and detector responses for several classes of advanced reactors. While the method can in principle be applied to other processes (e.g., enrichment or reprocessing facilities), the present work limits scope to ARs with continuously flowing fuel. Section 2 details the mathematics supporting the isotope ratio method, and Section 3 introduces the representative ARs selected for this work. Section 4 discusses how each reactor was analyzed, and Section 5 showcases the results for each representative reactor. Finally, Section 6 provides concluding remarks and suggests pathways for further analysis.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

NASA NTRS1977

Conductive spacecraft materials development program

The objectives of this program are to provide design criteria, techniques, materials, and test methods to ensure control of absolute and differential charging of spacecraft surfaces. The control of absolute and differential charging of spacecraft cannot be effected without the development of new and improved or modified materials or techniques that will provide electrical continuity over the surface of the spacecraft. The materials' photoemission, secondary emission, thermooptical, physical, and electrical properties in the space vacuum environment both in the presence and absence of electrical stress and ultraviolet, electron, and particulate radiation, are important to the achievement of charge control. The materials must be stable or have predictable response to exposure to the space environment for long periods of time. The materials of interest include conductive polymers, paints, transparent films and coatings as well as fabric coating interweaves.

Lehn, W. L.↗

NASA NTRS1974

Pilot cryo tunnel: Attachments, seals, and insulation

Several different tests are described which simulated the actual configuration of a cryogenic wind tunnel operating at pressures up to 5 atmospheres (507 kPa) and temperatures from -320 F (78K) to 120 F (322K) in order to determine compatible bolting, adequate sealing, and effective insulating materials. The evaluation of flange attachments (continuous threaded studs) considered bolting based on compatible flanges, attachment materials, and prescribed bolt elongations. Various types of seals and seal configurations were studied to determine suitability and reusability under the imposed pressure and temperature loadings. The temperature profile was established for several materials used for structural supports.

Wilson, J. F.↗

NASA NTRS1984

Magnetic properties of Martian surface material

The hypothesis that the magnetic properties of the Martian surface material are due to the production of a magnetic phase in the clay mineral nontronite by transient shock heating is examined. In the course of the investigation a magnetic material is produced with rather unusual properties. Heating from 900 C to 1000 C, of natural samples of nontronite leads first to the production of what appears to be Si doped maghemite gamma (-Fe2O3). Although apparently metastable, the growth of gamma -Fe2O3 at these temprtures is unexpected, and its relative persistence of several hours at 1000 C is most surprising. Continued annealing of this material for longer periods promote the crystallization of alpha Fe2O3 and cristobalite (high temperature polymorph of SiO2). All available data correlate this new magnetic material with the cristobalite hence our naming it magnetic ferri cristobalite. Formation of this magnetic cristobalite, however, may require topotactic growth from a smectite precursor.

Hargraves, R. B.↗

NASA NTRS2014

Recent Progress in Adjustable X-ray Optics for Astronomy

Two adjustable X-ray optics approaches are being developed for thin grazing incidence optics for astronomy. The first approach employs thin film piezoelectric material sputter deposited as a continuous layer on the back of thin, lightweight Wolter-I mirror segments. The piezoelectric material is used to correct mirror figure errors from fabrication, mounting/alignment, and any ground to orbit changes. The goal of this technology is to produce Wolter mirror segment pairs corrected to 0.5 arc sec image resolution. With the combination of high angular resolution and lightweight, this mirror technology is suitable for the Square Meter Arc Second Resolution Telescope for X-rays (SMART-X) mission concept.. The second approach makes use of electrostrictive adjusters and full shell nickel/cobalt electroplated replication mirrors. An array of radial adjusters is used to deform the full shells to correct the lowest order axial and azimuthal errors, improving imaging performance from the 10 - 15 arc sec level to ~ 5 arc sec. We report on recent developments in both technologies. In particular, we discuss the use of insitu strain gauges on the thin piezo film mirrors for use as feedback on piezoelectric adjuster functionality, including their use for on-orbit figure correction. We also report on the first tests of full shell nickel/cobalt mirror correction with radial adjusters.

Reid, Paul B.↗

NASA NTRS1992

Development of high T(sub c) (greater than 110 K) Bi, Tl, and Y-based materials as superconducting circuit elements

Experimental work has continued on the development and characterization of bulk and hot pressed powders and tapecast materials in the Bi-Sr-Ca-Cu-O and Tl-Ba-Ca-Cu-O systems. A process for producing warp-free, sintered, superconducting tapes of Bi composition Bi2Sr2Ca2Cu3O(x) with a mixed oxide process was established. This procedure required a triple calcination at 830 C for 24 hours and sintering at 845 C from 20 to 200 hours. Hot pressing the triple calcined powder at 845 C for 6 hours at 5000 psi yielded a dense material which on further heat treatment at 845 C for 24 hours exhibited a Tc of 108.2 K. A further improvement in the processing of the bismuth materials was achieved via a chemical coprecipitation process wherein the starting nitrate materials were coprecipitated with oxalic acid, thus yielding a more chemically homogeneous, more reactive powder. With the coprecipitated powders, only one calcine at 830 C for 12 hours and a final sinter at 845 C for 30 hours was sufficient to produce a bulk superconducting material with a Tc of 108.4 K. SAFIRE-type grounding links were successfully fabricated from sintered, tapecast, coprecipitated BSCCO 2223 powders. Compositional and processing investigations were continued on the Tl-based superconductors. Manganese and lithium additions and sintering temperature and time were examined to determine their influence on superconducting properties. It was found that lithium substitutions for copper enhance the transition temperatures while manganese additions produced deleterious effects on the superconducting properties. A suitable procedure for producing reproducible bulk and tapecast material of Tl composition Tl2Ba2Ca2Cu3O(x) was developed and used in fabricating uniform superconducting tapes. The highest transition temperature for Tl-based tapes was measured at 110.2 K. Thallium superconducting SAFIRE-type grounding links were fabricated from the tapes.

Haertling, Gene H.↗

NASA NTRS1995

Removal of Burkholderia cepacia biofilms with oxidants

Iodine is used to disinfect the water system aboard US space shuttles and is the anticipated biocide for the international space station. Water quality on spacecraft must be maintained at the highest possible levels for the safety of the crew. Furthermore, the treatment process used to maintain the quality of water on research must be robust and operate for long periods with minimal crew intervention. Biofilms are recalcitrant and pose a major threat with regard to chronic contamination of spacecraft water systems. We measured the effectiveness of oxidizing biocides on the removal and regrowth of Burkholderia (Pseudomonas) cepacia biofilms. B. cepacia, isolated from the water distribution system of the space shuttle Discovery, was grown in continuous culture to produce a bacterial contamination source for biofilm formation and removal studies. A 10(7) CFU ml-1 B. cepacia suspension, in distilled water, was used to form biofilms on 3000 micrometers2 glass surfaces. Rates of attachment were measured directly with image analysis and were found to be 7.8, 15.2, and 22.8 attachment events h-1 for flow rates of 20.7, 15.2, and 9.8 ml min-1, respectively. After 18 h of formation, the B. cepacia biofilms were challenged with oxidants (ozone, chlorine, and iodine) and the rates of biofilm removal determined by image analysis. Fifty percent of the biofilm material was removed in the first hour of continous treatment with 24 mg l-1 chlorine or 2 mg l-1 ozone. Iodine (48 mg l-1) did not remove any measurable cellular material after 6 h continuous contact. After this first removal of biofilms by the oxidants, the surface was allowed to refoul and was again treated with the biocide. Iodine was the only compound that was unable to remove cellular debris from either primary or secondary biofilms. Moreover, treating primary biofilms with iodine increased the rate of formation of secondary biofilms, from 4.4 to 5.8 attachment events h-1. All the oxidants tested inactivated the B. cepacia associated with both primary and secondary biofilms. The amount of biocide needed to inactivate 50% of planktonic B. cepacia in 10 min at 25 degrees C was 8.4, 0.5, and 0.2 mg l-1 for iodine, chlorine, and ozone, respectively. The data suggest that iodine maynot be the best chemical for treating of biofilms when removal of cellular material is required.

NASA Discipline Environmental Health↗

NASA NTRS2015

Investigating the Effects of Temperature on the Signatures of Shocks Propagated Through Impacts into Minerals Found in Comets and Asteroids

Comets and asteroids are subjected to extremely cold conditions throughout their lifetimes. During their sojourns in the solar system, they are subjected to collisions at speeds that are easily capable of generating shock waves in their constituent materials. In addition to ices, more common silicate minerals such as olivines and pyroxenes are important components of these objects. The collision-induced shocks could affect the spectral signatures of those mineral components, which could in turn be detected telescopically. We have embarked on a project to determine how impact-generated shock might affect the reflectance spectra and structures of select silicates as both impact speed and target temperature are varied systematically. While the effects of impact speed (in the form of shock stress) on numerous materials have been and continue to be studied, the role of target temperature has received comparatively little attention, presumably because of the operational difficulties it can introduce to experimentation. Our experiments were performed with the vertical gun in the Experimental Impact Laboratory of the Johnson Space Center. A liquid-nitrogen system was plumbed to permit cooling of the target container and its contents under vacuum to temperatures as low as -100 C (173 K). Temperatures were monitored by thermocouples mounted on the outside of the target container. Because those sensors were not in contact with the target material at impact, the measured temperatures are treated as lower limits for the actual values. Peridot (Mg-rich olivine) and enstatite (Mg-rich orthopyroxene) were used as targets, which involved the impact of alumina (Al2O3) spheres at speeds of 2.0 - 2.7 km s(exp -1) and temperatures covering 25 C to -100 C (298 K to 173 K). We have begun collecting and analyzing data in the near to mid-IR with a Fourier-transform infrared spectrometer, and preliminary analyses show that notable differences in absorption-band strength and position occur as functions of both impact speed (peak shock stress) and initial temperature.

Lederer, Susan M.↗

NASA NTRS1990

Satellite material contaminant optical properties

The Air Force Wright Research and Development Center and the Arnold Engineering Development Center are continuing a program for measuring optical effects of satellite material outgassing products on cryo-optic surfaces. Presented here are infrared (4000 to 700 cm(-1)) transmittance data for contaminant films condensed on a 77 K geranium window. From the transmittance data, the contaminant film refractive and absorptive indices (n, k) were derived using an analytical thin-film interference model with a nonlinear least-squares algorithm. To date 19 materials have been studied with the optical contents determined for 13 of those. The materials include adhesives, paints, composites, films, and lubricants. This program is continuing and properties for other materials will be available in the future.

Wood, B. E.↗

NASA NTRS2003

Instrument for Measuring Cryo CTE

Coefficient of thermal expansion is an integral part of the performance of optical systems, especially for those, which operate at cryogenic temperatures. The measurement of the coefficient of relevant materials has been of continuous interest. Besides commercial measurement sources, development of one-of-a-kind tools have always been of interest due to local needs. This paper describes one such development at the University of Alabama in Huntsville (UAH). The approach involves two vertical rods (one sample and one reference) on a flat platform. A probe bar is held horizontally atop the two samples. A temperature change will generally cause rotation of the probe bar. A mirrored surface on one end of the probe bar is used to measure the rotation using the reflection of an incident laser beam upon it. A position-sensing detector measures the change of the reflected beam spot position. Using other known quantities, the change determines the coefficient of thermal expansion of the sample material as a function of temperature. A parallel measurement of the rotation of the sample support platform is also performed to account for any unwanted background effects. This system has been demonstrated in a cryogenic chamber at the NASA Marshall Space Flight Center X-ray Calibration Facility (XRCF). We present the system details, achievable sensitivity, and up-to-date experimental performance.

Vikram, Chandra S.↗

NASA NTRS2014

Material and Thickness Grading for Aeroelastic Tailoring of the Common Research Model Wing Box

This work quantifies the potential aeroelastic benefits of tailoring a full-scale wing box structure using tailored thickness distributions, material distributions, or both simultaneously. These tailoring schemes are considered for the wing skins, the spars, and the ribs. Material grading utilizes a spatially-continuous blend of two metals: Al and Al+SiC. Thicknesses and material fraction variables are specified at the 4 corners of the wing box, and a bilinear interpolation is used to compute these parameters for the interior of the planform. Pareto fronts detailing the conflict between static aeroelastic stresses and dynamic flutter boundaries are computed with a genetic algorithm. In some cases, a true material grading is found to be superior to a single-material structure.

Stanford, Bret K.↗

NASA NTRS2012

Geologic Structures in Crater Walls on Vesta

The Framing Camera (FC) on the Dawn spacecraft has imaged most of the illuminated surface of Vesta with a resolution of apporpx. 20 m/pixel through different wavelength filters that allow for identification of lithologic units. The Visible and Infrared Mapping Spectrometer (VIR) has imaged the surface at lower spatial resolution but high spectral resolution from 0.25 to 5 micron that allows for detailed mineralogical interpretation. The FC has imaged geologic structures in the walls of fresh craters and on scarps on the margin of the Rheasilvia basin that consist of cliff-forming, competent units, either as blocks or semi-continuous layers, hundreds of m to km below the rims. Different units have different albedos, FC color ratios and VIR spectral characteristics, and different units can be juxtaposed in individual craters. We will describe different examples of these competent units and present preliminary interpretations of the structures. A common occurrence is of blocks several hundred m in size of high albedo (bright) and low albedo (dark) materials protruding from crater walls. In many examples, dark material deposits lie below coherent bright material blocks. In FC Clementine color ratios, bright material is green indicating deeper 1 m pyroxene absorption band. VIR spectra show these to have deeper and wider 1 and 2 micron pyroxene absorption bands than the average vestan surface. The associated dark material has subdued pyroxene absorption features compared to the average vestan surface. Some dark material deposits are consistent with mixtures of HED materials with carbonaceous chondrites. This would indicate that some dark material deposits in crater walls are megabreccia blocks. The same would hold for bright material blocks found above them. Thus, these are not intact crustal units. Marcia crater is atypical in that the dark material forms a semi-continuous, thin layer immediately below bright material. Bright material occurs as one or more layers. In one region, there is an apparent angular unconformity between the bright material and the dark material where bright material layers appear to be truncated against the underlying dark layer. One crater within the Rheasilvia basin contains two distinct types of bright materials outcropping on its walls, one like that found elsewhere on Vesta and the other an anomalous block ~200 m across. This material has the highest albedo; almost twice that of the vestan average. Unlike all other bright materials, this block has a subdued 1 micron pyroxene absorption band in FC color ratios. These data indicate that this block represents a distinct vestan lithology that is rarely exposed.

Mittlefehldt, David W.↗

NASA NTRS1987

Fatigue Lives of Materials Cut by Lasers

Laser machining helps to balance high-speed rotating machinery. Report describes continuing studies of fatigue lives of materials cut by lasers. One long-term objective of such studies is use of laser machining to balance rotors operating at high speeds. To achieve objective, necessary to know relationship between effects of conventional and laser machining on fatigue lives of machined materials.

Martin, Michael R.↗

NASA NTRS1980

Argon/UF6 plasma experiments: UF6 regeneration and product analysis

An experimental and analytical investigation was conducted to aid in developing some of the technology necessary for designing a self-critical fissioning uranium plasma core reactors (PCR). This technology is applicable to gaseous uranium hexafluoride nuclear-pumped laser systems. The principal equipment used included 1.2 MW RF induction heater, a d.c. plasma torch, a uranium tetrafluoride feeder system, and batch-type fluorine/UF6 regeneration systems. Overall objectives were to continue to develop and test materials and handling techniques suitable for use with high-temperature, high-pressure, gaseous UF6; and to continue development of complementary diagnostic instrumentation and measurement techniques to characterize the effluent exhaust gases and residue deposited on the test chamber and exhaust system components. Specific objectives include: a development of a batch-type UF6 regeneration system employing pure high-temperature fluorine; development of a ruggedized time-of-flight mass spectrometer and associated data acquisition system capable of making on-line concentration measurements of the volatile effluent exhaust gas species in a high RF environment and corrosive environment of UF6 and related halide compounds.

Roman, W. C.↗

NASA NTRS1999

Thermal-Mechanical Stability of Single Crystal Oxide Refractive Concentrators for High-Temperature Solar Thermal Propulsion

Single crystal oxides such as yttria-stabilized zirconia (Y2O3-ZrO2), yttrium aluminum garnet (Y3Al5O12, or YAG), magnesium oxide (MgO) and sapphire (Al2O3) are candidate refractive secondary concentrator materials for high temperature solar propulsion applications. However, thermo-mechanical reliability of these components in severe thermal environments during the space mission sun/shade transition is of great concern. Simulated mission tests are important for evaluating these candidate oxide materials under a variety of transient and steady-state heat flux conditions, and thus provide vital information for the component design. In this paper, a controlled heat flux thermal shock test approach is established for the single crystal oxide materials using a 3.0 kW continuous wave CO2 laser, with a wavelength 10.6 micron. Thermal fracture behavior and failure mechanisms of these oxide materials are investigated and critical temperature gradients are determined under various temperature and heating conditions. The test results show that single crystal sapphire is able to sustain the highest temperature gradient and heating-cooling rate, and thus exhibit the best thermal shock resistance, as compared to the yttria-stabilized zirconia, yttrium aluminum garnet, and magnesium oxide.

Zhu, Dongming↗