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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 109 records · Page 6

Rapid preparation of nanodiscs for biophysical studies

Nanodiscs, which are disc-shaped entities that contain a central lipid bilayer encased by an annulus of amphipathic helices, have emerged as a leading native-like membrane mimic. The current approach for the formation of nanodiscs involves the creation of a mixed-micellar solution containing membrane scaffold protein, lipid, and detergent followed by a time consuming process (3–12 h) of dialysis and/or incubation with sorptive beads to remove the detergent molecules from the sample. In contrast, the methodology described herein provides a facile and rapid procedure for the preparation of nanodiscs in a matter of minutes (<15 min) using Sephadex® G-25 resin to remove the detergent from the sample. A panoply of biophysical techniques including analytical ultracentrifugation, dynamic light scattering, gel filtration chromatography, circular dichroism spectroscopy, and cryogenic electron microscopy were employed to unequivocally confirm that aggregates formed by this method are indeed nanodiscs. We believe that this method will be attractive for time-sensitive and high-throughput experiments.

59 BASIC BIOLOGICAL SCIENCES↗

Freeze It or Leave It? Evaluating the Role of Cryo-Electron Microscopy in Battery Research

Cryogenic electron microscopy (cryo-EM) continues to gain prominence in materials science, particularly in battery research where it has enabled high-resolution, multimodal characterization of electrode materials and interfaces that otherwise degrade quickly under electron beam irradiation. But as anyone who has attempted cryo-EM techniques knows, freezing comes at a cost; cryo-EM experiments are time-consuming, highly sensitive, and carry an increased risk of artifacts due to issues such as frost contamination. Thus, when planning new characterization of battery materials or other beam-sensitive samples, it is critical to consider whether (and which) cryo-EM techniques are appropriate, based on study goals and an understanding of electron beam-sample interactions. Here we review such considerations for battery materials to elucidate the questions of when, why, and how to freeze to achieve high-quality characterization.

25 ENERGY STORAGE↗

Strong-coupling quantum dot microscope

Here, we report the development and fabrication of a novel cryogenic instrument, a scanning quantum dot microscope (SQDM), capable of positioning a quantum dot to within tunneling range of a sample surface. The microscope is strong-coupling in the sense that electron wavefunctions in the quantum dot can directly overlap with electron wavefunctions in the sample, in contrast to probes based on electric-field coupling. The SQDM consists of a sharp glass probe with two asymmetric electrodes leading to an aluminum quantum dot at the apex. One electrode is capacitively coupled to the quantum dot, while the other lead is connected to the dot via a tunneling junction. A charge sensing circuit constructed from a high-electron-mobility transistor is attached to the capacitance lead to measure the charge state of the dot. The last key feature of the design is a tilted-apex geometry. This design feature, in conjunction with the capacitive sensing scheme, results in a robust quantum-dot probe capable of operating within angstrom distances of the sample surface while protecting the single tunnel junction responsible for electron transport onto the quantum dot. We demonstrate that our instrument can detect single-electron tunneling events and can also be operated as a standard scanning tunneling microscope capable of nanometer-scale resolution of the surface topography.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Scaling behavior of low-temperature orthorhombic domains in the prototypical high-temperature superconductor La 1.875 Ba 0.125 CuO 4

Structural symmetry breaking and recovery in condensed-matter systems are closely related to exotic physical properties such as superconductivity (SC), magnetism, spin density waves, and charge density waves (CDWs). The interplay between different order parameters is intricate and often subject to intense debate, as in the case of CDW order and superconductivity. In La 1.875 Ba 0.125 CuO 4 (LBCO), the low-temperature structural domain walls are hypothesized as nanometer-scale pinning sites for the CDWs. Coherent x-ray diffraction techniques have been employed here to visualize the domain structures associated with these symmetry changes directly during phase transition. We have pushed Bragg coherent diffractive imaging (BCDI) into the cryogenic regime where most phase transitions in quantum materials reside. Utilizing BCDI, we image the structural evolution of LBCO microcrystal samples during the high-temperature tetragonal to low-temperature orthorhombic (LTO) phase transition. Our results show the formation of LTO domains close to the transition temperature and how the domain size decreases with temperature. In conclusion, the number of domains follows the secondary order parameter (or orthorhombic strain) measurement with a critical exponent that is consistent with the three-dimensional universality class.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Borderline first-order phase transition and large cryogenic magnetocaloric effect in PrNdIn

We report a large cryogenic magnetocaloric effect stemming from an unconventional borderline first-order magnetic phase transition with negligibly small thermomagnetic hysteresis in a rare-earth-based intermetallic compound PrNdIn. The sample exhibits maximum magnetic field-induced entropy change as large as –10 J/Kg K (for 20 kOe magnetic field change) near the boiling point of oxygen. Magnetocaloric properties of PrNdIn are comparable to those of other known potential magnetocaloric materials with operating temperatures ranging between 50 and 125 K. Here, the magnetic properties of the present sample are qualitatively reminiscent of those of the binary Pr 2 In and Nd 2 In, including the emergence of a second low-temperature anomaly in the temperature dependence of magnetization.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Characterization of Two Fast-Turnaround Dry Dilution Refrigerators for Scanning Probe Microscopy

Low-temperature scanning probe microscopes (SPMs) are critical for the study of quantum materials and quantum information science. Due to the rising costs of helium, cryogen-free cryostats have become increasingly desirable. However, they typically suffer from comparatively worse vibrations than cryogen-based systems, necessitating the understanding and mitigation of vibrations for SPM applications. Here, in this work, we demonstrate the construction of two cryogen-free dilution refrigerator SPMs with minimal modifications to the factory default and we systematically characterize their vibrational performance. We measure the absolute vibrations at the microscope stage with geophones and use both microwave impedance microscopy and a scanning single-electron transistor to independently measure tip-sample vibrations. Additionally, we implement customized filtering and thermal anchoring schemes and characterize the cooling power at the scanning stage and the tip electron temperature. This work serves as a reference to researchers interested in cryogen-free SPMs, as such characterization is not standardized in the literature or available from manufacturers.

36 MATERIALS SCIENCE↗

Metallic support films reduce optical heating in cryogenic correlative light and electron tomography

Super-resolved cryogenic correlative light and electron tomography is an emerging method that provides both the single-molecule sensitivity and specificity of fluorescence imaging, and the molecular scale resolution and detailed cellular context of tomography, all in vitrified cells preserved in their native hydrated state. Technical hurdles that limit these correlative experiments need to be overcome for the full potential of this approach to be realized. Chief among these is sample heating due to optical excitation which leads to devitrification, a phase transition from amorphous to crystalline ice. Here, in this work, we show that much of this heating is due to the material properties of the support film of the electron microscopy grid, specifically the absorptivity and thermal conductivity. We demonstrate through experiment and simulation that the properties of the standard holey carbon electron microscopy grid lead to substantial heating under optical excitation. In order to avoid devitrification, optical excitation intensities must be kept orders of magnitude lower than the intensities commonly employed in room temperature super-resolution experiments. We further show that the use of metallic films, either holey gold grids, or custom made holey silver grids, alleviate much of this heating. For example, the holey silver grids permit 20× the optical intensities used on the standard holey carbon grids. Super-resolution correlative experiments conducted on holey silver grids under these increased optical excitation intensities have a corresponding increase in the rate of single-molecule fluorescence localizations. This results in an increased density of localizations and improved correlative imaging without deleterious effects from sample heating.

59 BASIC BIOLOGICAL SCIENCES↗

Progress towards the FRIB-EDM 3 -Frontend: A tool to provide radioactive molecules from isotope harvesting for fundamental symmetry studies

The under-construction FRIB-EDM 3 -instrument was designed to study polar radioactive molecules (such as RaF) in transparent cryogenic solids by laser spectroscopy. The instrument is divided into a frontend- and a backend section. The frontend accepts an aqueous sample from isotope harvesting and provides a mass-separated molecular ion beam in an ultra-high vacuum environment. In the backend, the ions are guided into alkali-metal vapor and the resulting neutrals are co-deposited in a solid argon matrix to perform laser spectroscopy. Here, this work addresses the frontend of the instrument. The efficient ionization of harvested radioisotopes from aqueous samples is achieved with a spray-ionization method. Subsequently, the molecular ion beam is analyzed by mass-to-charge ratio by a quadrupole mass filter. To verify the feasibility of the approach, numerical simulations with the COMSOL and SIMION packages have been conducted. While the former was applied to study transport in ion funnels, the latter was used to investigate ion beam transmission through the lower pressure sections. Following promising simulation results, a first experimental setup is under construction.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

ODU Optimization of Nb3Sn supttering on SRF structures

High efficiency Superconducting radio-frequency (SRF) cavities are the key technology to cost-effective Continuous Wave (CW) SRF accelerators. Recent advances in Nb3Sn coatings on the inner surface of SRF cavities showed the potential for this material to significantly cut the capital and operating cost of SRF accelerators. The best results are presently achieved with Nb3Sn films coated by using the so-called vapor diffusion technique. Several alternative approaches have been and are being investigated such as electrochemical deposition, bronze routes, and sputtering. Among these techniques, magnetron sputtering is a versatile technique, which has been demonstrated to deposit Nb3Sn films on SRF cavities. The technique requires further development to compete with the results demonstrated on the cavities coated with the vapor diffusion techniques. The team to develop the novel technique includes a graduate student from Old Dominion University (ODU) and other experts. ODU Prof. Elsayed-Ali directs the graduate student to coat samples and cavities in the new coating system and analyze samples with different surface science techniques. Dr. Grigory Eremeev from Fermilab assists with 2.6 GHz cavities for coating, cavity characterization at cryogenic temperature, and result analysis. The research is funded by the Office of High Energy Physics at the US Department of Energy at both Fermilab and ODU

43 PARTICLE ACCELERATORS↗

Determination of the enthalpy of adsorption of hydrogen in activated carbon at room temperature

The development of high-performance materials for hydrogen storage by adsorption requires detailed understanding of the adsorbate-adsorbent interactions, e.g., the enthalpy of adsorption ΔH, which measures the interaction strength. The determination of ΔH for a weakly adsorbing gas such as hydrogen in a carbonaceous porous material is difficult experimentally, normally requiring measuring two cryogenic adsorption isotherms. Here we demonstrate a calculation of ΔH based on ca. room temperature adsorption isotherms at 273 K and 296 K using the Clausius-Clapeyron equation. This requires an estimation of the volume of the adsorbed film (~40%, ~12% of the total pore volume at 77 K, 296 K, respectively) obtained from fits of the excess adsorption isotherms to an Ono-Kondo model with the auxiliary use of a fixed point corresponding to the saturation film density (estimated as 100 ± 20 g/L) which appears to be remarkably sample and temperature independent, i.e., a property of the adsorbate. The calculated room temperature enthalpy of adsorption ΔH = 8.3 ± 0.4 kJ/mol is in excellent agreement with the low-coverage cryogenic determination of ΔH. The methodology hereby proposed facilitates reliable calculations of the enthalpy of adsorption at room temperatures for weakly-adsorbing gases.

08 HYDROGEN↗

Probing soft X-ray induced photoreduction of a model Mn-complex at cryogenic conditions

Soft X-ray absorption spectroscopy of first row transition elements at their respective L -edges provides important information about the oxidation and spin states of the metal centers. However, the associated sample damage in radiation-sensitive samples substantially alters the electronic and chemical structures of redox-active metal centers. Here, we measure the soft X-ray spectrum of the model Mn III (acac) 3 complex containing a redox-active Mn III metal center in an octahedral environment with a superconducting transition-edge sensor detector. To reduce the secondary damage resulting primarily from the diffusion of radicals and electrons, the spectra are collected at 30 K and 80 K on solid samples. Starting from the first scan, we detect the contribution of X-ray induced sample damage leading to a change in the Mn II intensity. However, at low temperatures, particularly at 30 K, we do not observe a gradual increase in the radiation damage with successive scans with the X-ray beam at the same spot. At our estimated dose of 90 kGy, we find 62% of Mn III (acac) 3 is still intact at 30 K. However, at room temperature, we see a gradual increase in radiation damage with increasing numbers of scans at the same spot, which is consistent with the possibility of increased diffusion rates of secondary radicals and electrons as noted in other studies.

L-edge spectroscopy↗

Angle- and polarization-resolved luminescence from suspended and hexagonal boron nitride encapsulated MoSe 2 monolayers

The polarized photoluminescence from atomically thin transition metal dichalcogenides is a frequently applied tool to scrutinize optical selection rules and valley physics, yet it is known to sensibly depend on a variety of internal and external material and sample properties. In this work, we apply combined angle- and polarization-resolved spectroscopy to explore the interplay of excitonic physics and phenomena arising from the commonly utilized encapsulation procedure on the optical properties of atomically thin M o S e 2 . We probe monolayers prepared in both suspended and encapsulated manners. We show that the hBN encapsulation significantly enhances the linear polarization of exciton photoluminescence emission at large emission angles. This degree of linear polarization of excitons can increase up to ∼ <#comment/> 17 % <#comment/> in the hBN encapsulated samples. As we confirm by finite-difference time-domain simulations, it can be directly connected to the optical anisotropy of the hBN layers. In comparison, the linear polarization at finite exciton momenta is significantly reduced in a suspended M o S e 2 monolayer, and becomes notable only in cryogenic conditions. This phenomenon strongly suggests that the effect is rooted in the k-dependent anisotropic exchange coupling inherent in 2D excitons. Our results have strong implications on further studies on valley contrasting selection rules and valley coherence phenomena using standard suspended and encapsulated samples.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Origin and Suppression of Beam Damage-Induced Oxygen-K Edge Artifact from γ-Al 2 O 3 using Cryo-EELS

Gamma-alumina (γ-Al 2 O 3 ), like other low-Z oxides, is readily damaged when exposed to an electron beam. This typically results in the formation of a characteristic pre-edge peak in the oxygen-K edge of electron energy-loss spectra (EELS) acquired during or after the damage process. This artifact can mask the presence of intrinsic O-K edge fine structure that would reveal chemical properties of the material; therefore, its suppression is key. In this work, we systematically investigate the conditions that give rise to the damage-induced O-K pre-edge peak and show that it can be effectively suppressed by performing EELS experiments at cryogenic (cryo) temperatures. Prolonged exposure of γ-Al 2 O 3 to a focused electron beam results in a hole bored through the sample; this was used as a reproducible beam damage condition. O-K edge EELS spectra were collected from a single-crystal γ-Al 2 O 3 sample both during and after focused 2 electron beam hole drilling, and at room and cryo temperatures, using a monochromated scanning transmission electron microscope (STEM). Furthermore, the characteristic 531 eV pre-edge peak visible in the room temperature EELS spectra was completely suppressed in the cryo-EELS spectra, even in the presence of a visible drilled hole. We then correlated these experimental observations with multiple-scattering EELS simulations to determine the likely atomistic origin of the damage-induced O-K pre-edge peak. The findings indicate that the pre-edge peak is caused primarily by the presence of surface O dimer (O-O) bonds formed during beam damage, and that operating at cryo temperature suppresses the formation of surface O-O bonds, thus preventing formation of the O-K pre-edge peak. Additionally, Al-L 2,3 edge EELS spectra revealed Al loss primarily from tetrahedral sites during hole drilling.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Inexpensive Superinsulation for Cryogenic and Highly Insulating Applications (CRADA Final Report)

This effort will use our novel insulation formed into effective “solid” (as compared to powder) insulating panels and/or wraps to demonstrate important technical achievements including scaling appropriate crosslinking to directly and cost effectively address vacuum insulated panel (VIP) applications and cryogenic component wrapping to help reduce energy use. This project will improve and scale-up processes (from 3” diameter disks) to make larger samples (e.g., 12” x 12” x 1”) Wow, cfor external evaluation and testing.

36 MATERIALS SCIENCE↗

High-bandwidth frequency domain multiplexed readout of transition-edge sensors for neutrinoless double beta decay searches

The next-generation of cryogenic neutrinoless double-beta decay experiments require increasingly fast readout in order to improve background discrimination. These experiments, operated as cryogenic calorimeters at ∼ 10 mK, are usually read out by high-impedance neutron transmutation doped (NTD) thermistors, which provide good energy resolution, but are limited by ∼ 1 ms response times. Superconducting detectors, such as transition-edge sensors (TESs) with a time resolution of ∼ 100 μs, offer superior timing performance over NTD semiconductor bolometers. To make this technology viable for an application to a thousand or more channels, multiplexed readout is necessary in order to minimize the thermal load and radioactive contamination induced by the readout. Frequency-domain multiplexing readout (fMUX) for TESs, previously developed at Berkeley Lab and McGill University, is currently in use for mm-wave telescopes with detector sampling rates in the order of 100 Hz. We demonstrate a new readout system, based on the McGill/Berkeley digital fMux readout, to satisfy the higher bandwidth and noise requirements of the next generation of TES-instrumented cryogenic calorimeters. Each multiplexing readout module comprises 10 superconducting resonators in the 1–5 MHz range and a DC superconducting quantum interference device (DC-SQUID), interfaced to high-speed field programmable gate array (FPGA)-based electronics for digital signal processing and low-latency SQUID feedback. The new readout samples detectors at 156 kHz, three orders of magnitude faster than its cosmology-oriented predecessor, and demonstrates a stable feedback bandwidth of 3 kHz in a real TES-based system.

47 OTHER INSTRUMENTATION↗

Operando Freezing Cryogenic Electron Microscopy of Active Battery Materials

Abstract Understanding structural and chemical evolution of battery materials during operation is critical to achieving safe, efficient, and long-lasting energy storage. Cryogenic electron microscopy (cryo-EM) has become a valuable tool in battery characterization, leveraging low temperatures to improve stability of sensitive materials under electron beam irradiation. However, typical cryo-EM sample preparations leave extended time between the electrochemical point of interest and ex situ freezing of samples, during which active structures may relax, degrade, or otherwise evolve. Here, we detail a method for operando freezing cryo-EM to preserve and characterize native electrode and interfacial structures that arise during battery cycling, based on an operando plunge freezer and cold sample removal process. We validate the method on multiple electrode materials and quantify and discuss the freezing rate achieved. Operando freezing cryo-EM can be used to directly visualize transient features that arise at active electrochemical interfaces, to enable deeper understanding of structural evolution and interfacial chemistry in batteries and other electrochemical systems.

25 ENERGY STORAGE↗

Cryogenic probe for low-noise, high-frequency electronic measurements

The design and performance of a low-noise, modular cryogenic probe, which is applicable to a wide range of measurements over a broad range of working frequencies, temperatures, and magnetic fields, is presented. The design of the probe facilitates the exchange of sample holders and sample-stage amplifiers, which, combined with its characteristic low transmission and reflection loss, make this design suitable for high precision or low sensitivity measurements. The specific example of measuring the shot noise of magnetic tunnel junctions is discussed. We highlight various design characteristics chosen specifically to expand the applicability of the probe to measurement techniques such as nuclear magnetic resonance.

47 OTHER INSTRUMENTATION↗

An in-situ movable calibration source for cryogenic particle detectors

A prototype device capable of moving a radioactive calibration source to multiple positions was operated at millikelvin temperatures using a modified commercial stepper motor. It was developed as an in-situ calibration strategy for cryogenic dark matter detectors. Data taken by scanning a calibration source across multiple radial positions of a prototype dark matter detector demonstrated its functionality. Construction, heat load, and operation of the device are discussed, as is the effect of the motor on the detector operation. A sample dataset taken over multiple positions of a SuperCDMS detector is presented as an example of the utility of such a device.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗