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DOE OSTI2025

Broadband optical modulation and control at millikelvin temperatures

A universal experimental challenge in studying radiation effects on cryogenic devices is precisely and accurately characterizing the position-dependent device response near the energy detection threshold. Here, we have developed a compact cryogenic optical beam steering system that can be used to generate O (μs) pulses of small numbers of photons over the energy range of 1.3–3.4 eV at room temperature, and deliver those photons via fiber optic to any specified location on the surface of a detector operating at cryogenic temperatures. This new system will allow for robust calibration of any photon-sensitive detector, including superconducting devices. The system can be used efficiently to explore the physics of target materials, quantify the position sensitivity of different sensor designs, measure phonon transport, and study the effects of quasiparticle poisoning on detector operation. We describe the design of this pulsed calibration method and present first results obtained with a second-generation system operated at room temperature and sub-Kelvin temperatures.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Anharmonic Exciton‐Phonon Coupling in Metal‐Organic Chalcogenides Hybrid Quantum Wells

Abstract In contrast to inorganic quantum wells, hybrid quantum wells (HQWs) based on metal‐organic semiconductors are characterized by relatively soft lattices, in which excitonic states can strongly couple to lattice phonons. Therefore, understanding the lattice's impact on exciton dynamics is essential for harnessing the optoelectronic potential of HQWs. Beyond 2D metal halide perovskites, layered metal‐organic chalcogenides (MOCs), which are an air‐stable, underexplored material class hosting room‐temperature excitons, can be exploited as photodetectors, light emitting devices, and ultrafast photoswitches. Here, the role of phonons in the optical transitions of the prototypical MOC [AgSePh] ∞ is elucidated. Impulsive stimulated Raman scattering (ISRS) allows the detection of coherent exciton oscillations driven by Fröhlich interaction with low‐energy optical phonons. Steady state absorption and Raman spectroscopies reveal a strong exciton‐phonon coupling (Huang‐Rhys parameter ≈1.7) and its anharmonicity, manifested as a nontrivial temperature‐dependent Stokes shift. The ab initio calculations support these observations, hinting at an anharmonic behavior of the low‐energy phonons <200 cm −1 . These results untangle complex exciton‐phonon interactions in MOCs, establishing an ideal testbed for room‐temperature many‐body phenomena.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Role of electronic energy loss on defect production and interface stability: Comparison between ceramic materials and high-entropy alloys

High-entropy alloys (HEAs) and some complex alloys exhibit desirable properties and significant structural stability in harsh environments, including possible applications in advanced reactors. Energetic ion irradiation is often used as a surrogate for neutron irradiation; however, the impact of ion electronic energy deposition and dissipation is often neglected. Moreover, differences in recoil energy spectrum and density of cascade events on damage evolution must also be considered. In many chemically complex alloys, the mean free path of electrons is reduced significantly, thus their decreased thermal conductivity and slow dissipation of localized radiation energy can have noticeable effects on displacement cascade evolution that is greatly different from metals with high thermal conductivity. In this work, nanocrystalline HEAs of Ni 20 Fe 20 Co 20 Cr 20 Cu 20 and nonequiatomic (NiFeCoCr) 97 Cu 3 , both having much lower room-temperature thermal conductivity than pure Ni or Fe, are chosen as model HEAs to reveal the role that electronic energy loss during ion irradiation has in complex alloys. The response of nanocrystalline HEAs is investigated under irradiation at room temperature using MeV Ni and Au ions that have different ratios of electronic energy to damage energy, which is the energy dissipated in displacing atoms. Different from previously reported amorphization of nanocrystalline SiC, experimental results on these HEAs show that, similar to the process in nanocrystalline oxide materials, both inelastic thermal spikes via electron–phonon coupling and elastic thermal spikes via collisions among atomic nuclei contribute to the overall grain growth. The growth follows a power law dependence with the total deposited ion energy, and the derived value of the power-exponent suggests that the irradiation-induced instability at and near grain boundaries leads to local rapid atomic rearrangements and consequently grain growth. The high power-exponent value can be attributed to the sluggish diffusion and delayed defect evolution arising from the chemical complexity intrinsic to HEAs. Here, this work calls attention to quantified fundamental understanding of radiation damage processes beyond that of simplified displacement events, especially in simulating neutron environments.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Indirectly probing the structural change in ion-irradiated Zr-Based metallic glasses from small scale mechanical tests

Ion irradiation was applied to tailor the structural heterogeneities in Zr-based metallic glasses at room temperature. Experimental methods of X-ray diffraction, nanoindentation, and micropillar compression were conducted to examine the irradiation effects on their structural and mechanical property changes. It is found that the irradiated materials retained amorphous structure after room-temperature Ni ion irradiation. The reduction of elastic modulus and hardness measured by nanoindentation indicated the irradiation-induced mechanical degradation. A unified statistic model was employed to quantitatively predict the density and strength of irradiation defects, although their specific structural and physical nature is not explicitly included in this model. The transition of non-intersecting shear bands to multiple intersecting shear bands was observed on compression tests of irradiated micropillars with the increase of irradiation dose. Furthermore, the analysis of the displacement excursion of micropillar compression tests indicated a different deformation mode from the unirradiated state. These results from nanoindentation pop-in and micro-pillar compression tests suggested that irradiation eventually leads to a new state with different types and characteristics of structural heterogeneities from violent displacement cascades and non-equilibrium energy deposition/dissipation processes, which also proves ion irradiation as an effective method to tune the structure and mechanical properties of metallic glasses.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Tailoring Negative Thermal Expansion via Tunable Induced Strain in La–Fe–Si-Based Multifunctional Material

Zero thermal expansion (ZTE) composites are typically designed by combining positive (PTE) with negative thermal expansion (NTE) materials acting as compensators and have many diverse applications, including in high-precision instrumentation and biomedical devices. La(Fe 1-x ,Si x )13-based compounds display several remarkable properties, such as giant magnetocaloric effect and very large NTE at room-temperature. Both are linked via strong magnetovolume coupling, which leads to sharp magnetic and volume changes occurring simultaneously across first-order phase transitions; the abrupt nature of these changes makes them unsuitable as thermal expansion compensators. To make these materials more useful practically, the mechanisms controlling the temperature over which this transition occurs and the magnitude of contraction need to be controlled. In this work, ball-milling was used to decrease particles and crystallite sizes and increase the strain in LaFe 11.9 Mn 0.27 Si 1.29 H x alloys. Such size and strain tuning effectively broadened the temperature over which this transition occurs. The material’s NTE operational temperature window was expanded, and its peak was suppressed by up to 85%. This work demonstrates that induced strain is the key mechanism controlling these materials’ phase transitions. This allows the optimization of their thermal expansion towards room-temperature ZTE-applications.

36 MATERIALS SCIENCE↗

NASA NTRS1979

Studies of magnetostriction and spin polarized band structures of rare earth intermetallics

Anisotropic magnetostriction measurements of R6Fe23, R = (Tb, Dy, Ho, and Er) were carried out from 77 K to room temperature. Magnetic fields up to 2.1 Tesla were applied. All the compounds exhibited large magnetostrictions at 77 K, the largest effect being obtained for Tb6Fe23. Saturation magnetostriction values for the compounds were also determined for 77 K and room temperature. Results of the temperature dependence of magnetostriction for Er6Fe23 are in good agreement with Callen and Callen's single ion theory. Therefore, the main sources of magnetostriction in this compound is the Er ion. The spin-up and spin-down electronic energy bands, the density of states and the magnetic moments of YCo5, SmCo5, and GdCo5 were calculated by the spin polarized augmented plane wave technique. The calculations obtained show the origin of the moment, provide good estimates of its magnitude and variation, and the reasons for those variations. They also show the important role of partial charge transfer and of d-d electronic coupling. Calculations for LaNi5 and GdNi5 systems are discussed.

Wallace, W. E.↗

NASA NTRS1990

A novel electron tunneling infrared detector

The pneumatic infrared detector, originally developed by Golay in the late 1940s, uses the thermal expansion of one cm(exp 3) of xenon at room temperature to detect the heat deposited by infrared radiation. This detector was limited by thermal fluctuations within a 10 Hz bandwidth, but suffered from long thermal time constants and a fragile structure. Nevertheless, it represents the most sensitive room temperature detector currently available in the long wavelength infrared (LWIR). Fabrication of this type of detector on smaller scales has been limited by the lack of a suitably sensitive transducer. Researchers designed a detector based on this principle, but which is constructed entirely from micromachined silicon, and uses a vacuum tunneling transducer to detect the expansion of the trapped gas. Because this detector is fabricated using micromachining techniques, miniaturization and integration into one and two-dimensional arrays is feasible. The extreme sensitivity of vacuum tunneling to changes in electrode separation will allow a prototype of this detector to operate in the limit of thermal fluctuations over a 10 kHz bandwidth. A calculation of the predicted response and noise of the prototype is presented with the general formalism of thermal detectors. At present, most of the components of the prototype have been fabricated and tested independently. In particular, a characterization of the micromachined electron tunneling transducer has been carried out. The measured noise in the tunnel current is within a decade of the limit imposed by shot noise, and well below the requirements for the operation of an infrared detector with the predicted sensitivity. Assembly and characterization of the prototype infrared detector will be carried out promptly.

Kenny, T. W.↗

NASA NTRS2013

Superconductors Enable Lower Cost MRI Systems

The future looks bright, light, and green, especially where aircraft are concerned. The division of NASA s Fundamental Aeronautics Program called the Subsonic Fixed Wing Project is aiming to reach new heights by 2025-2035, improving the efficiency and environmental impact of air travel by developing new capabilities for cleaner, quieter, and more fuel efficient aircraft. One of the many ways NASA plans to reach its aviation goals is by combining new aircraft configurations with an advanced turboelectric distributed propulsion (TeDP) system. Jeff Trudell, an engineer at Glenn Research Center, says, "The TeDP system consists of gas turbines generating electricity to power a large number of distributed motor-driven fans embedded into the airframe." The combined effect increases the effective bypass ratio and reduces drag to meet future goals. "While room temperature components may help reduce emissions and noise in a TeDP system, cryogenic superconducting electric motors and generators are essential to reduce fuel burn," says Trudell. Superconductors provide significantly higher current densities and smaller and lighter designs than room temperature equivalents. Superconductors are also able to conduct direct current without resistance (loss of energy) below a critical temperature and applied field. Unfortunately, alternating current (AC) losses represent the major part of the heat load and depend on the frequency of the current and applied field. A refrigeration system is necessary to remove the losses and its weight increases with decreasing temperature. In 2001, a material called magnesium diboride (MgB2) was discovered to be superconducting. The challenge, however, has been learning to manufacture MgB2 inexpensively and in long lengths to wind into large coils while meeting the application requirements.

Source record↗

NASA NTRS2003

High-Temperature Switched-Reluctance Electric Motor

An eight-pole radial magnetic bearing has been modified into a switched-reluctance electric motor capable of operating at a speed as high as 8,000 rpm at a temperature as high as 1,000 F (=540 C). The motor (see figure) is an experimental prototype of starter-motor/generator units that have been proposed to be incorporated into advanced gas turbine engines and that could operate without need for lubrication or active cooling. The unique features of this motor are its electromagnet coils and, to some extent, its control software. Heretofore, there has been no commercial-off-the-shelf wire capable of satisfying all of the requirements for fabrication of electromagnet coils capable of operation at temperatures up to 1,000 F (=540 C). The issues addressed in the development of these electromagnet coils included thermal expansion, oxidation, pliability to small bend radii, micro-fretting, dielectric breakdown, tensile strength, potting compound, thermal conduction, and packing factor. For a test, the motor was supported, along with a rotor of 18 lb (.8-kg) mass, 3-in. (.7.6-cm) diameter, 21-in. (.53-cm) length, on bearings packed with high-temperature grease. The motor was located at the mid span of the rotor and wrapped with heaters. The motor stator was instrumented with thermocouples. At the time of reporting the information for this article, the motor had undergone 14 thermal cycles between room temperature and 1,000 F (.540 C) and had accumulated operating time >27.5 hours at 1,000 F (=540 C). The motor-controller hardware includes a personal computer equipped with analog-to-digital input and digital-to-analog output cards. The controller software is a C-language code that implements a switched-reluctance motor-control principle: that is, it causes the coils to be energized in a sequence timed to generate a rotating magnetic flux that creates a torque on a scalloped rotor. The controller can operate in an open- or closed-loop mode. In addition, the software has been modified to enable the simultaneous operation of the prototype motor or another, similar apparatus as both a motor and a magnetic bearing. Combined bearing/motor operation has been demonstrated at room temperature but had not yet been demonstrated at high temperature at the time of reporting the information for this article.

Montague, Gerald↗

DOE OSTI2020

High oxygen pressure floating zone growth and crystal structure of the metallic nickelates R4Ni3O10 ( R=La,Pr )

Single crystals of the metallic Ruddlesden-Popper trilayer nickelates R 4 Ni 3 O 10 ( R = La , Pr ) were successfully grown using an optical-image floating zone furnace under oxygen pressure ( p O 2 ) of 20 bar for La 4 Ni 3 O 10 and 140 bar for Pr 4 Ni 3 O 10 . Furthermore, a combination of synchrotron and laboratory x-ray single-crystal diffraction, high-resolution synchrotron x-ray powder diffraction and measurements of physical properties revealed that R 4 Ni 3 O 10 ( R = La , Pr ) crystallizes in the monoclinic P 2 1 / a ( Z = 2 ) space group at room temperature, and that a metastable orthorhombic phase ( Bmab ) can be trapped by postgrowth rapid cooling. Both La 4 Ni 3 O 10 and Pr 4 Ni 3 O 10 crystals undergo a metal-to-metal transition (MMT) below room temperature. In the case of Pr 4 Ni 3 O 10 , the MMT is found at 157.6 K. For La 4 Ni 3 O 10 , the MMT depends on the lattice symmetry: 147.5 K for Bmab vs 138.6 K for P 2 1 / a . Lattice anomalies were found at the MMT that, when considered together with the pronounced dependence of the transition temperature on subtle structural differences between Bmab and P 2 1 / a phases, demonstrate a not insignificant coupling between electronic and lattice degrees of freedom in these trilayer nickelates.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Investigation to develop a method to apply diffusion barrier to high strength fibers

A radio frequency powered ion plating process was used to apply the diffusion barriers of aluminum oxide, yttrium oxide, hafnium oxide and titanium carbide to a substrate tungsten fiber. Each of the coatings was examined as to its effect on both room temperature strength and tensile strength of the base tungsten fiber. The coated fibers were then overcoated with a nickel alloy to become single cell diffusion couples. These diffusion couples were exposed to 1093 C for 24 hours, cycled between room temperature and 1093 C, and given a thermal anneal for 100 hours at 1200 C. Tensile testing and metallographic examinations determined that the hafnium oxide coating produced the best high temperature diffusion barrier for tungsten of the four coatings.

Veltri, R. D.↗

NASA NTRS2014

Carbon-Based Regenerable Sorbents for the Combined Carbon Dioxide and Ammonia Removal for the Primary Life Support System (PLSS)

Results are presented on the development of reversible sorbents for the combined carbon dioxide and trace-contaminant (TC) removal for use in Extravehicular Activities (EVAs). Since ammonia is the most important TC to be captured, data on TC sorption presented in this paper are limited to ammonia, with results relevant to other TCs to be reported at a later time. The currently available life support systems use separate units for carbon dioxide, trace contaminants, and moisture control, and the long-term objective is to replace the above three modules with a single one. Furthermore, the current TC-control technology involves the use of a packed bed of acid-impregnated granular charcoal, which is non-regenerable, and the carbon-based sorbent under development in this project can be regenerated by exposure to vacuum at room temperature. The objective of this study was to demonstrate the feasibility of using carbon sorbents for the reversible, concurrent sorption of carbon dioxide and ammonia. Several carbon sorbents were fabricated and tested, and multiple adsorption/vacuum-regeneration cycles were demonstrated at room temperature, and also a carbon surface conditioning technique that enhances the combined carbon dioxide and ammonia sorption without impairing sorbent regeneration.

Wojtowicz, Marek A.↗

DOE OSTI2023

Size‐Dependent Dispersion of Rhodium Clusters into Isolated Single Atoms at Low Temperature and the Consequences for CO Oxidation Activity

Abstract Understanding the dynamic structural evolution of supported metal clusters under reaction conditions is crucial to develop structure reactivity relations. Here, we followed the structure of different size Rh clusters supported on Al 2 O 3 using in situ/operando spectroscopy and ex situ aberration‐corrected electron microscopy. We report a dynamic evolution of rhodium clusters into thermally stable isolated single atoms upon exposure to oxygen and during CO oxidation. Rh clusters partially disperse into single atoms at room temperature and the extent of dispersion increases as the Rh size decreases and as the reaction temperature increases. A strong correlation is found between the extent of dispersion and the CO oxidation kinetics. More importantly, dispersing Rh clusters into single atoms increases the activity at room temperature by more than two orders of magnitude due to the much lower activation energy on single atoms (40 vs. 130 kJ/mol). This work demonstrates that the structure and reactivity of small Rh clusters are very sensitive to the reaction environment.

Albrahim, Malik A.↗

DOE OSTI2023

Size‐Dependent Dispersion of Rhodium Clusters into Isolated Single Atoms at Low Temperature and the Consequences for CO Oxidation Activity

Albrahim, Malik A.↗

DOE OSTI2022

A Fast‐Charging and High‐Temperature All‐Organic Rechargeable Potassium Battery

Abstract Developing fast‐charging, high‐temperature, and sustainable batteries is critical for the large‐scale deployment of energy storage devices in electric vehicles, grid‐scale electrical energy storage, and high temperature regions. Here, a transition metal‐free all‐organic rechargeable potassium battery (RPB) based on abundant and sustainable organic electrode materials (OEMs) and potassium resources for fast‐charging and high‐temperature applications is demonstrated. N‐doped graphene and a 2.8 m potassium hexafluorophosphate (KPF 6 ) in diethylene glycol dimethyl ether (DEGDME) electrolyte are employed to mitigate the dissolution of OEMs, enhance the electrode conductivity, accommodate large volume change, and form stable solid electrolyte interphase in the all‐organic RPB. At room temperature, the RPB delivers a high specific capacity of 188.1 mAh g −1 at 50 mA g −1 and superior cycle life of 6000 and 50000 cycles at 1 and 5 A g −1 , respectively, demonstrating an ultra‐stable and fast‐charging all‐organic battery. The impressive performance at room temperature is extended to high temperatures, where the high‐mass‐loading (6.5 mg cm −2 ) all‐organic RPB exhibits high‐rate capability up to 2 A g −1 and a long lifetime of 500 cycles at 70–100 °C, demonstrating a superb fast‐charging and high‐temperature battery. The cell configuration demonstrated in this work shows great promise for practical applications of sustainable batteries at extreme conditions.

25 ENERGY STORAGE↗

DOE OSTI2020

Raman and X-ray diffraction study of pressure-induced phase transition in synthetic Mg 2 TiO 4

Synthetic Mg 2 TiO 4 qandilite was investigated to 50 and 40.4 GPa at room temperature using Raman spectroscopy and X-ray diffraction, respectively. The Raman measurements showed that cubic Mg 2 TiO 4 spinel transforms to a high pressure tetragonal (I4 1 /amd, No.141) phase at 14.7 GPa. Owing to sluggish kinetics at room temperature, the spinel phase coexists with the tetragonal phase between 14.7 and 24.3 GPa. In the X-ray diffraction experiment, transformation of the cubic Mg 2 TiO 4 to the tetragonal structure was complete by 29.2 GPa, ~5 GPa higher than the transition pressure obtained by Raman measurements, owing to slow kinetics. The obtained isothermal bulk modulus of Mg 2 TiO 4 spinel is K T0 = 148(3) GPa when K T0 ’ = 6.6, or K T0 = 166(1) GPa when K T0 ’ is fixed at 4. The isothermal bulk modulus of the high-pressure tetragonal phase is calculated to be 209(2) GPa and V 0 = 270(2) Å 3 when K T0 ’ is fixed at 4, and the volume reduction on change from cubic to tetragonal phase is about 9%. The calculated thermal Grüneisen parameters (γ th ) of cubic and tetragonal Mg 2 TiO 4 phases are 1.01 and 0.63. Based on the radii ratio of spinel cations, a simple model is proposed to predict post-spinel structures.

36 MATERIALS SCIENCE↗

NASA NTRS1983

Hypergravic fields and parallel controllers for thermoregulation

To test the proposal that mammals have parallel neurocontrollers for temperature regulation, Long-Evans hooded male rats were exposed to cold while in a 3-G field. When exposed to cold, these rats consumed 35 percent less oxygen/min at 3 G than they did when exposed to cold at 1 G. However, rats acclimated for 6 wk to 5 C consumed oxygen at the same rate during cold exposure at 3 G as at 1 G. Because cold-acclimated rats generate heat primarily by nonshivering thermogenesis while rats acclimated to room temperature rely to a greater extent on shivering, the 35 percent decrease in oxygen consumption of cold-exposed room-temperature rats in 3-G fields may reflect an inactivation of shivering. These oxygen consumption measurements, together with measurements of core and tail temperatures of rats in 3-G fields, are consistent with the proposal that neurocontrollers for thermoregulation are arranged in parallel and can be uncoupled by hypergravic fields.

Monson, C. B.↗

NASA NTRS1999

Novel Ultraviolet-Light-Curable Polyimides

Polyimides have found broad application in fiber-reinforced composites for aerospace components and as thin films for electronics packaging. Typical routes to processing these materials require temperatures above 200 C. As a result, tooling costs for fabricating components from these composites can be quite high. Recent efforts within the Polymers Branch at the NASA Lewis Research Center have been aimed at developing radiationcurable (with light or electron beams) polyimides. Such materials may enable the processing of polymers and composites at or near room temperature, leading to reduced tooling requirements and costs. A new Diels-Alder route to polyimides has been developed that employs ultraviolet light (UV), rather than heat, to effect polymerization. This approach, which can be carried out at room temperature, is based on a well-known photochemical reaction--the photoenolization of o-methylphenyl ketones. Irradiation of o-methylphenyl ketones, such as 1 in the preceding figure, with UV wavelengths above 300 nm produces a photoenol, 2. This photoenol is unstable, but it persists long enough to undergo Diels-Alder reactions with good dienophiles, such as maleimide, 3. By utilizing a diketone, such as 2,5-dibenzoylp-xylene, 5, and a bismalemide, 6, this chemistry has been used to make a number of polyimides, 7.

Meador, Michael A.↗