Cryogenic Electron Microscopy for Buried Interface Characterization.
Abstract not provided.
Long, Daniel↗
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Cryogenic Electron Microscopy of Beam- and Air-Sensitive Materials.
Abstract not provided.
Long, Daniel↗
Next Generation Cryogenic Electronics for High Energy Physics
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Turowski, Marek↗
Reliability of Electronics for Cryogenic Space Applications Being Assessed
Many future NASA missions will require electronic parts and circuits that can operate reliably and efficiently in extreme temperature environments below typical device specification temperatures. These missions include the Mars Exploration Laboratory, the James Webb Space Telescope, the Europa Orbiter, surface rovers, and deep-space probes. In addition to NASA, the aerospace and commercial sectors require cryogenic electronics in applications that include advanced satellites, military hardware, medical instrumentation, magnetic levitation, superconducting energy management and distribution, particle confinement and acceleration, and arctic missions. Besides surviving hostile space environments, electronics capable of low-temperature operation would enhance circuit performance, improve system reliability, extend lifetime, and reduce development and launch costs. In addition, cryogenic electronics are expected to result in more efficient systems than those at room temperature.
Patterson, Richard L.↗
Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage
Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. In conclusion, this platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.
Charge density wave↗
Structural Complexities in Sodium Ion Conductive Antiperovskite Revealed by Cryogenic Transmission Electron Microscopy
Here we use low-dose cryogenic transmission electron microscopy (cryo-TEM) to investigate the atomic-scale structure of antiperovskite Na 2 NH 2 BH 4 crystals by preserving the room-temperature cubic phase and carefully monitoring the electron dose. Via quantitative analysis of electron beam damage using selected area electron diffraction, we find cryogenic imaging provides 6-fold improvement in beam stability for this solid electrolyte. Cryo-TEM images obtained from flat crystals revealed the presence of a new, long-range-ordered supercell with a cubic phase. The supercell exhibits doubled unit cell dimensions of 9.4 Å × 9.4 Å as compared to the cubic lattice structure revealed by X-ray crystallography of 4.7 Å × 4.7 Å. The comparison between the experimental image and simulated potential map indicates the origin of the supercell is a vacancy ordering of sodium atoms. This work demonstrates the potential of using cryo-TEM imaging to study the atomic-scale structure of air- and electron-beam-sensitive antiperovskite-type solid electrolytes.
36 MATERIALS SCIENCE↗
Identification and demonstration of roGFP2 as an environmental sensor for cryogenic correlative light and electron microscopy
Cryogenic correlative light and electron microscopy (cryo-CLEM) seeks to leverage orthogonal information present in two powerful imaging modalities. While recent advances in cryogenic electron microscopy (cryo-EM) allow for the visualization and identification of structures within cells at the nanometer scale, information regarding the cellular environment, such as pH, membrane potential, ionic strength, etc., which influences the observed structures remains absent. Fluorescence microscopy can potentially be used to reveal this information when specific labels, known as fluorescent biosensors, are used, but there has been minimal use of such biosensors in cryo-CLEM to date. Here we demonstrate the applicability of one such biosensor, the fluorescent protein roGFP2, for cryo-CLEM experiments. At room temperature, the ratio of roGFP2 emission brightness when excited at 425 nm or 488 nm is known to report on the local redox potential. When samples containing roGFP2 are rapidly cooled to 77 K in a manner compatible with cryo-EM, the ratio of excitation peaks remains a faithful indicator of the redox potential at the time of freezing. Using purified protein in different oxidizing/reducing environments, we generate a calibration curve which can be used to analyze in situ measurements. As a proof-of-principle demonstration, we investigate the oxidation/reduction state within vitrified Caulobacter crescentus cells. The polar organizing protein Z (PopZ) localizes to the polar regions of C. crescentus where it is known to form a distinct microdomain. Finally, by expressing an inducible roGFP2-PopZ fusion we visualize individual microdomains in the context of their redox environment.
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↗
A cryogenic multichannel electronically scanned pressure module
Consideration is given to a cryogenic multichannel electronically scanned pressure (ESP) module developed and tested over an extended temperature span from -184 to +50 C and a pressure range of 0 to 5 psig. The ESP module consists of 32 pressure sensor dice, four analog 8 differential-input multiplexers, and an amplifier circuit, all of which are packaged in a physical volume of 2 x 1 x 5/8 in with 32 pressure and two reference ports. Maximum nonrepeatability is measured at 0.21 percent of full-scale output. The ESP modules have performed consistently well over 15 times over the above temperature range and continue to work without any sign of degradation. These sensors are also immune to repeated thermal shock tests over a temperature change of 220 C/sec.
Shams, Qamar A.↗
Observation of formation and local structures of metal-organic layers via complementary electron microscopy techniques
Abstract Metal-organic layers (MOLs) are highly attractive for application in catalysis, separation, sensing and biomedicine, owing to their tunable framework structure. However, it is challenging to obtain comprehensive information about the formation and local structures of MOLs using standard electron microscopy methods due to serious damage under electron beam irradiation. Here, we investigate the growth processes and local structures of MOLs utilizing a combination of liquid-phase transmission electron microscopy, cryogenic electron microscopy and electron ptychography. Our results show a multistep formation process, where precursor clusters first form in solution, then they are complexed with ligands to form non-crystalline solids, followed by the arrangement of the cluster-ligand complex into crystalline sheets, with additional possible growth by the addition of clusters to surface edges. Moreover, high-resolution imaging allows us to identify missing clusters, dislocations, loop and flat surface terminations and ligand connectors in the MOLs. Our observations provide insights into controllable MOL crystal morphology, defect engineering, and surface modification, thus assisting novel MOL design and synthesis.
36 MATERIALS SCIENCE↗
Monofluorinated acetal electrolyte for high-performance lithium metal batteries
High degree of fluorination for ether electrolytes has resulted in improved cycling stability of lithium metal batteries due to stable solid electrolyte interphase (SEI) formation and good oxidative stability. However, the sluggish ion transport and environmental concerns of high fluorination degree drive the need to develop less fluorinated structures. Here, we depart from the traditional ether backbone and introduce bis(2-fluoroethoxy)methane (F2DEM), featuring monofluorination of the acetal backbone. High coulombic efficiency and stable long-term cycling in Li||Cu half cells can be achieved with F2DEM even under fast Li metal plating conditions. The performance of F2DEM is further compared with diethoxymethane (DEM) and 2-[2-(2,2-difluoroethoxy)ethoxy]-1,1,1-trifluoroethane (F5DEE). A significantly lower overpotential is observed with F2DEM, which improves energy efficiency and enables its application in high-rate conditions. Comparative studies of F2DEM with DEM and F5DEE in anode-free lithium iron phosphate (LiFePO4) LFP pouch cells and high-loading LFP coin cells further show improved capacity retention of F2DEM electrolyte, demonstrating its practical applicability. More importantly, we also extensively investigate the underlying mechanism for the superior performance of F2DEM through various techniques, including X-ray photoelectron spectroscopy, scanning electron microscopy, cryogenic electron microscopy, focused ion beam, electrochemical impedance spectroscopy, and titration gas chromatography. Overall, F2DEM facilitates improved Li deposition morphology with reduced amount of dead Li. This enables F2DEM to show superior performance, especially under higher charging and slower discharging rate conditions.
25 ENERGY STORAGE↗
Multi-channel electronically scanned cryogenic pressure sensor
A miniature, multi-channel, electronically scanned pressure measuring device uses electrostatically bonded silicon dies in a multielement array. These dies are bonded at specific sites on a glass, prepatterned substrate. Thermal data is multiplexed and recorded on each individual pressure measuring diaphragm. The device functions in a cryogenic environment without the need of heaters to keep the sensor at constant temperatures.
Chapman, John J.↗
Power control electronics for cryogenic instrumentation
In order to achieve a high-efficiency high-density cryogenic instrumentation system, the power processing electronics should be placed in the cold environment along with the sensors and signal-processing electronics. The typical instrumentation system requires low voltage dc usually obtained from processing line frequency ac power. Switch-mode power conversion topologies such as forward, flyback, push-pull, and half-bridge are used for high-efficiency power processing using pulse-width modulation (PWM) or resonant control. This paper presents several PWM and multiresonant power control circuits, implemented using commercially available CMOS and BiCMOS integrated circuits, and their performance at liquid-nitrogen temperature (77 K) as compared to their room temperature (300 K) performance. The operation of integrated circuits at cryogenic temperatures results in an improved performance in terms of increased speed, reduced latch-up susceptibility, reduced leakage current, and reduced thermal noise. However, the switching noise increased at 77 K compared to 300 K. The power control circuits tested in the laboratory did successfully restart at 77 K.
Ray, Biswajit↗
Current Density Regulated Atomic to Nanoscale Process on Li Deposition and Solid Electrolyte Interphase Revealed by Cryogenic Transmission Electron Microscopy
Current density has been perceived to play a critical rule for controlling Li deposition morphology and solid electrolyte interphase (SEI). However, the atomic level mechanism of current density on Li deposition and the SEI remains unclear. In this work, based on cryogenic transmission electron microscopy imaging combined with energy dispersive X-ray spectroscopy and electron energy loss spectroscopy electronic structure analyses, we reveal the atomic level correlation of Li deposition morphology and SEI with current density. We discover that increasing current density leads to increased overpotential for Li nucleation and growth, leading to the transition from growth-limited to nucleation-limited mode for Li dendrite. Independence of current density, the electrochemically deposited Li metal (EDLi) exhibits crystalline whisker-like morphology. The SEI formed at low current density (0.1 mA cm -2 ) is monolithic amorphous; while, a current density of above 2 mA cm -2 leads to a mosaic structured SEI, featuring an amorphous matrix with Li 2 O and LiF dispersoids, and the thickness of the SEI increases with the increase of current density. Uniquely, the Li 2 O particles is spatially located at the top surface of the SEI, while LiF is spatially adjacent to the Li-SEI interface. These results highlight the possible tuning of crucial structural and chemical features of EDLi and SEI through altering deposit conditions and consequently direct correlation with electrochemical performance.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Designing Antifouling and Antimicrobial Interfaces: Structural Characterization using CryoEM, Automated Microscopy, and AI Image Segmentation
The design of functionalized surfaces for interactions with biological systems is critical across sectors such as healthcare, energy, and agriculture. Tailoring materials for specific applications, such as antifouling and antimicrobial surfaces, demands a comprehensive understanding of topology and chemistry across multiple length and time scales on both biological and materials systems. This work presents the development and characterization of nanostructured surfaces with controlled topographies and chemistries that enhance bacterial membrane disruption, reduce biofilm formation, and improve antimicrobial and antifouling capabilities. Two specific use cases will be presented - the use of cellulose nanocrystals (CNCs) for bacterial growth inhibition and the development of antifouling surfaces to prevent protein and bacterial adsorption [1-4]. By leveraging large language models (LLMs) for image segmentation and training [5], we enable automated analysis of terabyte-scale cryogenic electron microscopy (cryoEM) datasets. This analysis provides statistical insights into the biotic/abiotic interface and facilitates automated electron microscopy experiments to mitigate time and dose. The integration of cryogenic electron tomography (cryoET) and cryogenic focused ion beam (cryoFIB) milling enables high-resolution, near-native-state imaging and 3D reconstructions of bio/material interfaces [6]. Orthogonal characterization techniques and computational modeling further enhances our understanding, offering a robust platform for the design and optimization of next-generation functional surfaces [7].
Williams, Alexis [ORNL] (ORCID:0000000252835822)↗
Cryogenically-Operable Electronics for Surviving the Lunar Night
Current solar-powered robotic lunar landers and rovers have not demonstrated survivability of the extreme cold temperatures seen during the 354-hour lunar night. To address this capability gap, we have been investigating the feasibility of a passive hibernation approach to enable low-cost solar- and battery-powered missions to operate over multiple lunar cycles. This strategy relies on isolating the batteries from the main bus during the lunar night and allowing cells to freeze as temperatures descend as low as 50K. The entire power architecture remains in a hibernation state with no electrical activity until lunar dawn. When the sun returns over the horizon, the now-illuminated solar arrays begin generating power. In order to manage the array power, architecture consisting of cryogenically-operable COTS electronics must be utilized. This architecture will distribute and control power to subsystems - importantly controlling heaters to bring the frozen lithium-ion battery cells to normal operating conditions. This alternative approach to lunar operations will enable low-cost commercial lunar landers and payloads to passively survive the night and continue to operate over multiple lunar cycles without a significant impact to cost or payload mass. Research last year focused on creating a power supply that was capable of operation at cryogenic temperatures. At the end of FY23, our team successfully designed and manufactured a Sequential Switching Shunt Regulator (S3R) that is operational in a cryogenic vacuum chamber. It is capable of full operation down to the coldest lunar night temperatures (~50K). Our presentation will provide an overview of the Lunar Hibernation strategy but will focus mainly on the technical details of this cryogenically-operable shunt regulator and test results.
Cryogenic↗
CryoTRANS: predicting high-resolution maps of rare conformations from self-supervised trajectories in cryo-EM
Cryogenic electron microscopy (cryo-EM) has revolutionized structural biology, enabling efficient determination of structures at near-atomic resolutions. However, a common challenge arises from the severe imbalance among various conformations of vitrified particles, leading to low-resolution reconstructions in rare conformations due to a lack of particle images in these quasi-stable states. We introduce CryoTRANS, a method that predicts high-resolution maps of rare conformations by constructing a self-supervised pseudo-trajectory between density maps of varying resolutions. This trajectory is represented by an ordinary differential equation parameterized by a deep neural network, ensuring retention of detailed structures from high-resolution density maps. By leveraging a single high-resolution density map, CryoTRANS significantly improves the reconstruction of rare conformations and has been validated on four real-world datasets: alpha-2-macroglobulin, actin-binding protein complexes, SARS-CoV-2 spike glycoprotein, and the 70S ribosome. CryoTRANS can also predict high-resolution structures in cryogenic electron tomography maps using a high-resolution cryo-EM map.Cryogenic electron microscopy (cryo-EM) has revolutionized structural biology, enabling efficient determination of structures at near-atomic resolutions. However, a common challenge arises from the severe imbalance among various conformations of vitrified particles, leading to low-resolution reconstructions in rare conformations due to a lack of particle images in these quasi-stable states. We introduce CryoTRANS, a method that predicts high-resolution maps of rare conformations by constructing a self-supervised pseudo-trajectory between density maps of varying resolutions. This trajectory is represented by an ordinary differential equation parameterized by a deep neural network, ensuring retention of detailed structures from high-resolution density maps. By leveraging a single high-resolution density map, CryoTRANS significantly improves the reconstruction of rare conformations and has been validated on four real-world datasets: alpha-2-macroglobulin, actin-binding protein complexes, SARS-CoV-2 spike glycoprotein, and the 70S ribosome. CryoTRANS can also predict high-resolution structures in cryogenic electron tomography maps using a high-resolution cryo-EM map.
47 OTHER INSTRUMENTATION↗
Multi-Channel Electronically Scanned Cryogenic Pressure Sensor And Method For Making Same
A miniature, multi-channel, electronically scanned pressure measuring device uses electrostatically bonded silicon dies in a multi-element array. These dies are bonded at specific sites on a glass, pre-patterned substrate. Thermal data is multiplexed and recorded on each individual pressure measuring diaphragm. The device functions in a cryogenic environment without the need of heaters to keep the sensor at constant temperatures.
Chapman, John J.↗