Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “cryogenic electron microscopy”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Cryo-based Structural Characterization and Growth Model of Salt Film on Metal

Metal salt films play a critical role in high rate dissolution processes such as within an active pit. However, structural and compositional characterization of salt films is challenging owing to the dynamic nature of the dissolving interface. Here, the salt film formed on SS304 one-dimensional artificial pit surface was directly characterized using flash freezing and cryo-based focused ion beam/scanning electron microscopy. The salt film exhibits a porous structure. Ni is co-located with Fe in the salt film, indicating the formation of co-precipitated salt containing Fe2+ and Ni2+. Additionally, a salt film growth model is presented based on ion transport.

Salt film, Pitting corrosion, Cryogenic, Cryo-FIB/↗
DOE OSTI2021

Synthesis and characterization of amorphous Fe2.75Dy-oxide thin films demonstrating room-temperature semiconductor, magnetism, and optical transparency

Recently, amorphous/disordered oxide thin films made from Fe and lanthanides like Dy and Tb have been reported to have a rich set of magnetic, optical, and electronic properties, as well as room-temperature magneto-electric coupling with multiferroics [A. Malasi et al., Sci. Rep. 5, 18157 (2015); H. Taz et al., Sci. Rep. 6, 27869 (2016); and H. Taz et al., Sci. Rep. 10, 1–10 (2020)]. Here, we report the synthesis and detailed characterization of Fe2.75Dy-oxide thin films prepared on various substrates using electron beam co-evaporation. The structure, chemistry, electric, magnetic, and optical properties were studied for the as-prepared and annealed (373 K, in air, 1 h) films of thickness 40 nm. High resolution transmission electron microscopy and electron diffraction study showed that the films were amorphous in both the as-prepared and annealed states. The electron energy-loss spectroscopy studies quantified that metal oxygen stoichiometry changed from Fe2.75Dy-O1.5 to Fe2.75Dy-O1.7 upon annealing. Synchrotron-based x-ray absorption spectroscopy investigation confirmed that the as-prepared films were highly disordered with predominantly metallic Fe and Dy states that became slightly oxidized with annealing in air. The as-prepared amorphous films demonstrated significantly high value of ordinary (∼10 cm2/V s) and anomalous (∼102 cm2/V s) Hall mobility and high electrical conductivity of ∼103 S/cm at room temperature. The cryogenic magnetic property measurement shows two-step magnetization below 200 K, suggesting exchange-spring magnetic interaction. The nature of the field cooled and zero-field cooled curves suggested a spin-glass like transition between 78 K and 80 K, with a characteristic broad peak. The Tauc plot analysis from optical transmission spectra confirms the existence of an optical bandgap of ∼2.42 eV that increased slightly to ∼2.48 eV upon annealing. This rich set of transport, optical, and magnetic properties in these thin films is very exciting and points to potential applicability in low-cost multifunctional devices requiring a combination of transparent, semiconducting, and magnetic responses, such as in spintronics.

Prasad Koirala, Krishna (ORCID:000000029137917X)↗
DOE OSTI2022

Exceptional fracture toughness of CrCoNi-based medium- and high-entropy alloys at 20 kelvin

Medium- and high-entropy alloys based on the CrCoNi-system have been shown to display outstanding strength, tensile ductility and fracture toughness (damage-tolerance properties), especially at cryogenic temperatures. Here we examine the J Ic and (back-calculated) K JIc fracture toughness values of the face-centered cubic, equiatomic CrCoNi and CrMnFeCoNi alloys at 20 K. At flow stress values of ~1.5 GPa, crack-initiation K JIc toughnesses were found to be exceptionally high, respectively 235 and 415 MPa√m for CrMnFeCoNi and CrCoNi, with the latter displaying a crack-growth toughness K ss exceeding 540 MPa√m after 2.25 mm of stable cracking, which to our knowledge is the highest such value ever reported. Characterization of the crack-tip regions in CrCoNi by scanning electron and transmission electron microscopy reveal deformation structures at 20 K that are quite distinct from those at higher temperatures and involve heterogeneous nucleation, but restricted growth, of stacking faults and fine nanotwins, together with transformation to the hexagonal closed-packed phase. The coherent interfaces of these features can promote both the arrest and transmission of dislocations to generate respectively strength and ductility which strongly contributes to sustained strain hardening. Indeed, we believe that these nominally single-phase, concentrated solid-solution alloys develop their fracture resistance through a progressive synergy of deformation mechanisms, including dislocation glide, stacking-fault formation, nano-twinning and eventually in situ phase transformation, all of which serve to extend continuous strain hardening which simultaneously elevates strength and ductility (by delaying plastic instability), leading to truly exceptional resistance to fracture.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Simplified feedback control system for scanning tunneling microscopy

A Scanning Tunneling Microscope (STM) is one of the most important scanning probe tools available to study and manipulate matter at the nanoscale. In a STM, a tip is scanned on top of a surface with a separation of a few Å. Often, the tunneling current between the tip and the sample is maintained constant by modifying the distance between the tip apex and the surface through a feedback mechanism acting on a piezoelectric transducer. This produces very detailed images of the electronic properties of the surface. The feedback mechanism is nearly always made using a digital processing circuit separate from the user computer. Here, we discuss another approach using a computer and data acquisition through the universal serial bus port. We find that it allows successful ultralow noise studies of surfaces at cryogenic temperatures. We show results on different compounds including a type II Weyl semimetal (WTe2), a quasi-two-dimensional dichalcogenide superconductor (2H–NbSe2), a magnetic Weyl semimetal (Co3Sn2S2), and an iron pnictide superconductor (FeSe).

Martín-Vega, Francisco (ORCID:0000000333177833)↗
NASA NTRS1989

Liquid oxygen LOX compatibility evaluations of aluminum lithium (Al-Li) alloys: Investigation of the Alcoa 2090 and MMC weldalite 049 alloys

The behavior of liquid oxygen (LOX) compatibility of aluminum lithium (Al-Li) alloys is investigated. Alloy systems of Alcoa 2090, vintages 1 to 3, and of Martin Marietta Corporation (MMC) Weldalite 049 were evaluated for their behavior related to the LOX compatibility employing liquid oxygen impact test conditions under ambient pressures and up to 1000 psi. The developments of these aluminum lithium alloys are of critical and significant interest because of their lower densities and higher specific strengths and improved mechanical properties at cryogenic temperatures. Of the different LOX impact tests carried out at the Marshall Space Flight Center (MSFC), it is seen that in certain test conditions at higher pressures, not all Al-Li alloys are LOX compatible. In case of any reactivity, it appears that lithium makes the material more sensitive at grain boundaries due to microstructural inhomogeneities and associated precipitate free zones (PFZ). The objectives were to identify and rationalize the microstructural mechanisms that could be relaxed to LOX compatibility behavior of the alloy system in consideration. The LOX compatibility behavior of Al-Li 2090 and Weldalite 049 is analyzed in detail using microstructural characterization techniques with light optical metallography, scanning electron microscopy (SEM), electron microprobe analysis, and surface studies using secondary ion mass spectrometry (SIMS), electron spectroscopy in chemical analysis (ESCA) and Auger electron spectroscopy (AES). Differences in the behavior of these aluminum lithium alloys are assessed and related to their chemistry, heat treatment conditions, and microstructural effects.

Diwan, Ravinder M.↗
DOE OSTI2021

Scanning SQUID microscopy in a cryogen-free dilution refrigerator

We report a scanning superconducting quantum interference device (SQUID) microscope in a cryogen-free dilution refrigerator with a base temperature at the sample stage of at least 30 mK. The microscope is rigidly mounted to the mixing chamber plate to optimize thermal anchoring of the sample. The microscope housing fits into the bore of a superconducting vector magnet, and our design accommodates a large number of wires connecting the sample and sensor. Through a combination of vibration isolation in the cryostat and a rigid microscope housing, we achieve relative vibrations between the SQUID and the sample that allow us to image with micrometer resolution over a 150 μm range while the sample stage temperature remains at base temperature. To demonstrate the capabilities of our system, we show images acquired simultaneously of the static magnetic field, magnetic susceptibility, and magnetic fields produced by a current above a superconducting micrometer-scale device.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

The self-annealing of irradiation induced defects in magnetite Fe 3 O 4 : Revealing reversible irradiation-induced disorder transformation through in situ TEM

This work reports heavy ion-irradiation effects in polycrystalline Fe 3 O 4 . For this matter, Fe/Fe 3 O 4 heterostructures were irradiated in situ in a transmission electron microscopy with 1 MeV Kr ions at 50 K. Evidence of cubic to monoclinic transformation (a.k.a Verwey transition) was recorded in some magnetite grains upon cooling the sample (around 90 K); however, most of the oxide grains retain their cubic spinel structure. Irradiation effects were analyzed in the cubic phase up to a maximum dose of 38 dpa without the sign of amorphization. The extinction of first-order reflections was recorded at doses below 1 dpa, indicating the formation of a new (metastable) phase with half of the lattice parameters compared to the unirradiated Fe 3 O 4 crystal. The formation of the new crystalline phase, which also presents a high resistance to amorphization, is related to the disordering of the cation lattice and the high mobility of the cation interstitials. The metastable phase readily recovers around 225 K during the natural warming of the sample from 50 K to room temperature.

Atom irradiation effects↗
DOE OSTI2023

Infrared nano-imaging of Dirac magnetoexcitons in graphene

Magnetic fields can have profound effects on the motion of electrons in quantum materials. Two-dimensional electron systems subject to strong magnetic fields are expected to exhibit quantized Hall conductivity, chiral edge currents and distinctive collective modes referred to as magnetoplasmons and magnetoexcitons. Generating these propagating collective modes in charge-neutral samples and imaging them at their native nanometre length scales have thus far been experimentally elusive. Here we visualize propagating magnetoexciton polaritons at their native length scales and report their magnetic-field-tunable dispersion in near-charge-neutral graphene. Imaging these collective modes and their associated nano-electro-optical responses allows us to identify polariton-modulated optical and photo-thermal electric effects at the sample edges, which are the most pronounced near charge neutrality. Our work is enabled by innovations in cryogenic near-field optical microscopy techniques that allow for the nano-imaging of the near-field responses of two-dimensional materials under magnetic fields up to 7 T. In conclusion, this nano-magneto-optics approach allows us to explore and manipulate magnetopolaritons in specimens with low carrier doping via harnessing high magnetic fields.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Evolution of Metastable Phases During Mg Metal Corrosion: An In Situ Cryogenic X-ray Photoelectron Spectroscopy Study

Magnesium and its alloys are potential structural materials candidates for a wide variety of applications due to their high strength-to-weight ratio. However, ductility and poor corrosion resistance under ambient environmental conditions are the bottleneck for industrial deployment. Designing passivation layers and/or corrosion resistant alloys requires fundamental understanding of the corrosion process. The traditional ex-situ spectroscopic measurements of polycrystalline metal surface with ubiquitous surface impurities and grain boundaries only provided an indistinct view of the corrosion process. To clearly distinguish the mechanism and sequence of corrosion process, we employed in-situ cryo-based x-ray photoelectron spectroscopy (XPS) measurements on Mg single crystal surface exposed to aqueous salt solution. Clean Mg (0001) surfaces were exposed to pure D2O and NaCl aqueous solution (5 wt% NaCl+95 wt% D2O). The interfacial reactions were studied using multimodal analysis including XPS, x-ray diffraction (XRD) and scanning electron microscopy (SEM). In contrast to previous studies, our experiments demonstrated the formation of magnesium chloride hydroxide hydrate during aqueous salt corrosion processes. Evidence of metastable ClO* radicals were also found during the initial aqueous salt solution exposure.

Shutthanandan, Vaithiyalingam↗
NASA NTRS2002

Time-Temperature-Precipitation Behavior in Al-Li Alloy 2195

Transmission electron microscopy was used to study time-temperature-precipitation (TTP) behavior in aluminum-lithium (Al-Li) 2195 alloy. Al-Li 2195 (nominally Al + 4 percent Cu + 1 percent Li + 0.3 percent Ag + 0.3 percent Mg + 0.1 percent Zr) was initially solutionized for 1 hr at 950 F and then stretched 3 percent. Heat treatments were conducted for up to 100 hr at temperatures ranging from 200 to 1,000 F. TTP diagrams were determined for both matrix and subgrain boundaries. Depending upon heat treatment conditions, precipitate phases (such as GP zone, theta'', theta', theta, delta', T1, TB, and T2) were found in the alloy. The TTP diagrams were applied as a guide to avoid T1 precipitation at subgrain boundaries, as part of an effort to improve the alloy's cryogenic fracture toughness (CFT). New understanding of TTP behavior was instrumental in the development of a two-step artificial aging treatment that significantly enhanced CFT in Al-Li 2195.

Chen, P. S.↗
DOE OSTI2026

Optical interference for the guidance of cryogenic focused ion beam milling beyond the axial diffraction limit

Cryogenic focused ion beam (Cryo-FIB) milling has become a standard step in the cryogenic electron tomography (Cryo-ET) workflow and is required to thin cells to electron-semitransparency. However, this destructive process removes the vast majority of the cellular material and raises a critical question: what thin section should be preserved for Cryo-ET analysis? Using a tri-coincident cryogenic FIB-SEM-LM system, we identify an interferometric optical response that can be used for targeting lamella production to fluorescently labeled structures with accuracy beyond the diffraction limit. Here we demonstrate this approach using synthetic samples of fluorescent beads embedded in micron-scale droplets of amorphous ice. We then apply the approach to capture virions inside host cells. Successful targeting is confirmed by Cryo-ET revealing clusters of virions in intracellular vesicles. The method does not require any fluorescent fiducials or axial registration and can be performed on any fluorescently labeled structure that is visible in widefield fluorescence microscopy.

Cryoelectron microscopy↗
DOE OSTI2024

Conjugate Multimode Heat Transfer Analysis of Cryogenic EXLO Manipulation

Abstract In this study, a conjugate radiation/conduction multimode heat transfer analysis of cryogenic focused ion beam (FIB) milling steps necessary for producing ex situ lift out specimens under cryogenic conditions (cryo-EXLO) is performed. Using finite volume for transient heat conduction and enclosure theory for radiation heat transfer, the analysis shows that as long as the specimen is attached or touching the FIB side wall trenches, the specimen will remain vitreous indefinitely, while actively cooled at liquid nitrogen (LN2) temperatures. To simulate the time needed to perform a transfer step to move the bulk sample containing the FIB-thinned specimen from the cryo-FIB to the cryo-EXLO cryostat, the LN2 temperature active cooling is turned off after steady-state conditions are reached and the specimen is monitored over time until the critical devitrification temperature is reached. Under these conditions, the sample will remain vitreous for >3 min, which is more than enough time needed to perform the cryo-transfer step from the FIB to the cryostat, which takes only ∼10 s. Cryo-transmission electron microscopy images of a manipulated cryo-EXLO yeast specimen prepared with cryo-FIB corroborates the heat transfer analysis.

Materials Science↗
DOE OSTI2024

Deterministic fabrication of graphene hexagonal boron nitride moiré superlattices

The electronic properties of moiré heterostructures depend sensitively on the relative orientation between layers of the stack. For example, near-magic-angle twisted bilayer graphene (TBG) commonly shows superconductivity, yet a TBG sample with one of the graphene layers rotationally aligned to a hexagonal Boron Nitride (hBN) cladding layer provided experimental observation of orbital ferromagnetism. To create samples with aligned graphene/hBN, researchers often align edges of exfoliated flakes that appear straight in optical micrographs. However, graphene or hBN can cleave along either zig-zag or armchair lattice directions, introducing a 30° ambiguity in the relative orientation of two flakes. By characterizing the crystal lattice orientation of exfoliated flakes prior to stacking using Raman and second-harmonic generation for graphene and hBN, respectively, we unambiguously align monolayer graphene to hBN at a near-0°, not 30°, relative twist angle. We confirm this alignment by torsional force microscopy of the graphene/hBN moiré on an open-face stack, and then by cryogenic transport measurements, after full encapsulation with a second, nonaligned hBN layer. This work demonstrates a key step toward systematically exploring the effects of the relative twist angle between dissimilar materials within moiré heterostructures.

boron nitride↗
NASA NTRS1983

Development of tough, strong, iron-base alloy for cryogenic applications

The development of an iron-base alloy that combines the normally divergent properties of high toughness and high strength at cryogenic temperatures is discussed. Specifically, alloy properties were sought which at -196 C would exhibit a fracture toughness of 220 MPa-m(1/2) with a corresponding yield strength of 1.4 GPa (200 ksi). Early work showed that high toughness could be achieved in Fe-12Ni alloys containing reactive metal additions such as Al, Nb, Ti, and V. Further research emphasized strengthening of these tough alloys by thermomechanical processing and the addition of Cu. Results showed that high strength and high toughness could be achieved in a single alloy at temperatures as low as -196 C. An alloy with composition Fe-12Ni-9.5Al-2Cu exhibited a yield strength of 1.65 GPa with a corresponding fracture toughness of 220 MPa-m(1/2) at -196 C. Strengthening due to Cu additions to the Fe-12Ni base alloys results primarily from precipitation of Cu-rich epsilon particles approximately 20 nm in diameter. Strengthening mechanisms are discussed in terms of an elastic modulus hardening model and are supported by transimission electron microscopy examinations of selected test specimens.

Stephens, J. R.↗
DOE OSTI2021

Preparing Lamellae from Vitreous Biological Samples using a Dual-Beam Scanning Electron Microscope for Cryo-Electron Tomography

Presented here is a protocol for preparing cryo-lamellae from plunge-frozen grids of Plasmodium falciparum-infected human erythrocytes, which could easily be adapted for other biological samples. The basic principles for preparing samples, milling, and viewing lamellae are common to all instruments and the protocol can be followed as a general guide to on-grid cryo-lamella preparation for cryo-electron microscopy (cryoEM) and cryo-electron tomography (cryoET). Electron microscopy grids supporting the cells are plunge-frozen into liquid nitrogen-cooled liquid ethane using a manual or automated plunge freezer, then screened on a light microscope equipped with a cryo-stage. Frozen grids are transferred into a cryo-scanning electron microscope equipped with a focused ion beam (cryoFIB-SEM). Grids are routinely sputter coated prior to milling, which aids dispersal of charge build-up during milling. Alternatively, an e-beam rotary coater can be used to apply a layer of carbon-platinum to the grids, the exact thickness of which can be more precisely controlled. Once inside the cryoFIB-SEM an additional coating of an organoplatinum compound is applied to the surface of the grid via a gas injection system (GIS). This layer protects the front edge of the lamella as it is milled, the integrity of which is critical for achieving uniformly thin lamellae. Regions of interest are identified via SEM and milling is carried out in a step-wise fashion, reducing the current of the ion beam as the lamella reaches electron transparency, in order to avoid excessive heat generation. A grid with multiple lamellae is then transferred to a transmission electron microscope (TEM) under cryogenic conditions for tilt-series acquisition. A robust and contamination-free workflow for lamella preparation is an essential step for downstream techniques, including cellular cryoEM, cryoET, and sub-tomogram averaging. Development of these techniques, especially for lift-out and milling of high-pressure frozen samples, is of high-priority in the field.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Synthesizing intermetallic thermoelectric materials using metal flux growth method

With zero energy poverty by 2050 goals, exploring innovative energy technologies is essential. Thermoelectric materials (TEMs) have the potential to harness waste heat and convert it to electricity (e.g., for spacecraft power, sensors, and cryogenic cooling). Two limitations of thermoelectric compounds are their low efficiency and limited pool of materials. Optimizing the efficiency of TEMs is challenging due to the interdependent relationship between electrical and thermal conductivity. A deeper understanding of electronic properties and lattice thermal conductivity is necessary to “understand, predict and ultimately control” the thermoelectric properties of TEMs. Understanding the influence of light-atom-doping and intrinsic defects on the electronic properties of the f-element containing TEMs are important questions that need to be answered to design and synthesize TEMs with optimal parameters. The purpose of this work is to understand how doping f-element based TEMs with light elements, such as carbon and boron, would impact the crystal structure, bond lengths, band gaps, and thermoelectric characteristics. High-quality f¬-element containing intermetallic single crystals are grown in metal flux media. In molten metal flux growth method, one or more low-melting metals such as aluminum, gallium, tin, and bismuth are used in excess as the reaction medium. As these are solution-state reactions, we can use lower temperatures than solid-state reactions and isolate the kinetic products instead of the thermodynamically stable compound. Then these are characterized using X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, magnetization, electrical and thermal conductivities, and thermoelectric power.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗
DOE OSTI2021

Preparation of Ultrathin Gold Films with Subatomic Surface Roughness

Nanoscale device fabrication requires control over film growth at the atomic scale. Growth conditions must be tuned in consideration of interface parameters like chemical bonding, surface free energy, and lattice matching. In metals, electronic properties may also be utilized for control of physical parameters. Quantum size effects can induce metals to spontaneously form specific shapes and sizes according to their electronic structure. Unfortunately, such electronic growth is generally known only for a few systems and is typically only stable under cryogenic conditions. In this work, we explore a recently discovered class of electronic growth systems in which metal films are grown upon the relatively inert surfaces of van der Waals crystals. In this class of materials, the electronic growth is highly stable at room temperature and actually requires higher temperature annealing to achieve proper equilibrium. We work with the Au/MoS 2 system, which shows excellent stability and can readily form discrete and atomically flat nanostructures. Here, we show how the electronic growth modes facilitate the formation of atomically flat films with nanometer scale thickness. Here, the surface roughness of these films was found to be less than a single atom over several square microns, creating nearly perfect surfaces for studies of self-assembled monolayers or other applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Spontaneous Polarization in an Ultrathin Improper-Ferroelectric/Dielectric Bilayer in a Capacitor Structure at Cryogenic Temperatures

To determine the effect of depolarization and the critical thickness in improper-ferroelectric hexagonal-ferrite thin films, we investigate the polarization switching of a ferroelectric/dielectric bilayer in capacitor structures at 20 K. Experimentally, we show that the spontaneous polarization persists throughout the studied thickness range (3 to 80 unit cell), even with a thick (10-nm) dielectric layer, suggesting no practical thickness limit for applications. By fitting the effect of depolarization using the phenomenological theory, we show that the spontaneous polarization remains finite when the thickness of the ferroelectric layer approaches zero, providing a hint for the absence of critical thickness. We also find that the interfacial effects limit the multidomain formation and govern the polarization switching mechanisms.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗