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At least 19 records

Nanometer-scale resolution in an ultra-high pressure environmental TEM holder

Environmental Transmission Electron Microscopy gas holders are vital for studying catalyst nanostructures in reactive gases. Although there are existing methods to understand the behavior of catalysts during reaction, a “pressure gap” exists. Pressures of up to 4.5 bar have been demonstrated, but many industrial catalysts operate at 10–100 bar. This work introduces an ultra-high-pressure TEM gas holder designed to bridge this gap. Experiments demonstrate it can safely operate and achieve nanometer-scale resolution (~ 1.5 nm) in an Environmental TEM at pressures up to 27.5 bar. Practical resolution limitations are attributed to contamination and vibration rather than increased gas scatter.

36 MATERIALS SCIENCE

Development of a Target Rod Rabbit Holder Facility in the Large Removable Beryllium Position

A new facility, the removable beryllium-target rod rabbit holder facility (RB*-TRRH), was designed and fielded in the large removable beryllium (RB*) position in the High Flux Isotope Reactor (HFIR). This facility supports three shortened target rod rabbit holders (sTRRHs), which allow for the irradiation of six axially stacked rabbit capsules per sTRRH. This will allow for the simultaneous irradiation of 18 rabbit capsules in the RB* position and will provide an alternative location for low-cost rabbit capsules to be irradiated in HFIR. The first capsules inserted into this facility are 18 perforated capsules that contain representative steel specimens of interest to the calandria of Canada deuterium uranium (CANDU) reactors as part of a lifetime extension program with Canadian Nuclear Laboratories (CNL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

A fully contained sample holder capable of electron-yield detection at soft X-ray energies

A holder has been developed that enables electron yield-detected soft X-ray spectroscopy of fully contained samples at low temperature. Crucially, this design uses elements of the sample containment to collect ejected electrons, removing the need to expose samples directly to the vacuum environment of the spectrometer. The design is modular and should be adaptable to a number of different endstation configurations, enabling spectroscopy of air-sensitive, radioactive and vacuum-sensitive (biological) samples.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS

Z Machine Detonator Holder Testing

Current packaging for the detonators used on the Z Machine is dirty, not well suited for reusability, and labor intensive to use. A new packaging design is developed, explosively tested, and approved by the numerous stakeholders resulting in more efficient operations and lowered costs.

42 ENGINEERING

High Yield nTOF Spec A and NP Filter Holders Static and Seismic Analysis

The Neutron Time-of-Flight (nTOF) detectors located in the Alcove and at the North Pole (Spec A and Spec NP respectively) need filtering in the beam path to enable them to take data at NIF yields above 5MJ. The filtering consists of 12cm of filter material divided into four, 3cm thick “pucks.” The pucks are 7cm in diameter. Each puck is mounted into a rotatable stage, also called a Filter Flipper, that can bring it into and out of the beam path, see Figure 1-1. These stages are bolted onto a plate that connects the filter stages to the mounting hardware used to position them in the NIF Target Bay. The top-level filter mount assemblies will be permanently mounted in the facility; removal is possible if needed for NIF maintenance, but the design intent is for the assemblies to remain in their locations after alignment is completed.

42 ENGINEERING

AGR-5/6/7 Thermal Model with Non-uniform Gas Gaps

Fuel compact temperatures are a crucial factor in assessing the irradiation performance of tri-structural isotropic fuel particles. In the absence of direct measurement, fuel compact temperatures were calculated using a three-dimensional finite element thermal model, which is subject to simulation uncertainty. The most dominant factor in the uncertainty of calculated fuel temperatures is the gas gap uncertainty due to the nub-to-shell clearance caused by a design error of AGR-5/6/7 capsules. The thermal model was revised to examine the most probable graphite offset position for six different days during the irradiation for Capsules 1 and 2. The analysis varied the offset distance and azimuthal direction at both the top and bottom of the holder. The best-fit offset was estimated based on the minimum root mean square error of the residuals (measured minus calculated) for the operational thermocouples (TCs). From these results, the following conclusions were made: (1) The holder offsets led to slightly lower average temperatures but wider temperature variations (lower minimum and higher peak fuel temperatures) for both Capsule 1 and Capsule 2. (2) During earlier cycles (162A–164B), when numerous TCs were still operational, the best-fit offset distance varied over a specific range for both the top and bottom ([0.002–0.0035 in.] for Capsule 1 and [0.003-0.004 in] for Capsule 2). In contrast, the offset azimuthal direction varied widely, especially for the offset at the bottom of the Capsule 1 holder. This is because holder movement was somewhat constrained at the top of Capsule 1 by the TC leads running through the capsule head and into the holder and by the through tubes in Capsule 2, but the Capsule 1 bottom did not have this type of constraint. (3) During later cycles, when all TCs failed, applying the maximum possible offset of 0.006 in. to the northwest direction for both the top and bottom resulted in a calculated peak fuel temperature of 1557? in Capsule 1 (i.e., a 135? increase from 1422? with zero offset on September 20, 2019 (166A)); the maximum offset of 0.0068 in. to the south for both top and bottom resulted in a calculated peak fuel temperature of 1110°C in Capsule 2 on April 20, 2020 (i.e., a 116? increase from 994? with zero offset (168A)). High peak fuel temperatures in Capsule 1 during Cycle 166A could be the cause of massive particle failure near the end of this cycle. (4) Even though the highest temperature at the tip of Type-N TCs, such as TC-1-7, slightly exceeded 1000?, the temperature along the TC wire reached as high as 1335? assuming an offset of 0.006 in. in the northwest of Capsule 1 holder near the end of Cycle 166A. This temperature significantly exceeds the temperature threshold at which TC degradation is expected to occur, ultimately contributing to considerable particle failures in Capsule 1. For eight Type-N TCs in Capsule 2, the peak TC line temperature was much lower (i.e., 1029°C for TC-2-5), assuming maximum offset of 00068 in. to the south during cycle 168A.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Bias-Modulated ALD of ZnO: Insights into Precursor-Surface Interactions for ZnO Films

Atomic layer deposition (ALD) is widely used to deposit conformal thin films but is often limited in the tunability of the resulting material’s properties. Substrate bias and electric fields alter precursor-surface interactions and provide means to tune material properties. To explore this, we performed zinc oxide (ZnO) ALD using diethylzinc (DEZ) and water on silicon native oxide substrates at 150 °C in a sample holder designed to create a static electrical field by biasing one plate of a parallel plate capacitor-style sample holder during deposition. ZnO films prepared in an electric field/on a biased sample holder were thinner, changed relative crystalline composition, and contained more carbon compared to samples grown in identical sample holders without bias. The thickness was independent of the magnitude of the eletric field between plates, indicating that the primary driver for the change was substrate biasing not the electric field between plates of the parallel plate capacitor-style sample holder. Density functional theory calculations showed enhanced electron migration between dissociatively adsorbed DEZ molecules and the ZnO (002) facet with increasing force from an electric field at the substrate surface, which strengthens the electronic interactions between the surface and the adsorbate. These models offer a compelling explanation for the inhibited growth, changes in the crystallinity, and increase in carbon content of films grown in an electric field/on biased plates.

Jones, Jessica C. (ORCID:0000000174754620)

Fission Product Quantification and Burnup Analysis via Gamma Spectrometry of the AGR-5/6/7 TRISO Fuel Experiment

Five capsules containing varying configurations of TRISO fuel compacts were irradiated in the most recent Advanced Gas Reactor (AGR) TRISO test campaign, AGR-5/6/7. As part of the post-irradiation examination (PIE) of this work all the fuel compacts and capsule graphite holders were measured with the Precision Gamma Scanner (PGS) to determine isotopic activities and locations using gamma spectrometry. Measuring the compacts allowed for the comparison of physics model depletion calculations with the measured compact activity to validate models. These measurements also are used to find compacts of interest with low fission product retention that may be tested in subsequent PIE. Measurements of the holders can confirm fission product distribution and migration. Of the isotopes measured, Cs-137 and Cs-134 were used to estimate location of failed particles as well as determine a measured burnup estimation. Results from Capsule 1 compacts and the holder indicate many fuel particle failures occurred. There are high amounts of cesium in the holder near Stack 9 of Capsule 1 that corresponds to low fractions?measured-to-calculated (M/C) ratio?of cesium remaining in those compacts. All other capsules had cesium retention ratios near 1. The isotope 110mAg had less consistent results. Capsule 2 compacts exhibited a M/C of 0.20, much lower than anticipated for the temperatures these compacts underwent. Capsule 3 experienced much higher temperatures, >1300C and had an average M/C of 0.75. These are the opposite results than what was predicted by past AGR experiments for the relationship between temperature and isotope retention. Capsule 4 and 5 showed good fission product retention and agreement with the physics model predictions. The burnup results from the PGS measurements showed strong agreement between the physics models and the measured values. Using a ratio of Cs-134/Cs-137 to calculate the burnup match closely with the physics models. Additionally, the Cs-137 burnup results were less accurate but extremely close to the model results.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Facile Tensile Testing Platform for In Situ Transmission Electron Microscopy of Nanomaterials

In situ tensile testing using transmission electron microscopy (TEM) is a powerful technique to probe structure-property relationships of materials at the atomic scale. In this work, a facile tensile testing platform for in situ characterization of materials inside a transmission electron microscope is demonstrated. The platform consists of: 1) a commercially available, flexible, electron-transparent substrate (e.g., TEM grid) integrated with a conventional tensile testing holder, and 2) a finite element simulation providing quantification of specimen-applied strain. The flexible substrate (carbon support film of the TEM grid) mitigates strain concentrations usually found in free-standing films and enables in situ straining experiments to be performed on materials that cannot undergo localized thinning or focused ion beam lift-out. The finite element simulation enables direct correlation of holder displacement with sample strain, providing upper and lower bounds of expected strain across the substrate. The tensile testing platform is validated for three disparate material systems: sputtered gold-palladium, few-layer transferred tungsten disulfide, and electrodeposited lithium, by measuring lattice strain from experimentally recorded electron diffraction data. The results show good agreement between experiment and simulation, providing confidence in the ability to transfer strain from holder to sample and relate TEM crystal structural observations with material mechanical properties.

2D materials

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Ultracold cryogenic TEM with liquid helium and high stability

Cryogenic transmission electron microscopy has revolutionized structural biology and materials science. To image below liquid nitrogen temperatures, various liquid helium stages have been constructed but have proven to be complex and unstable, making high-resolution imaging challenging. This problem is even more pronounced in side-entry specimen holders common on modern transmission electron microscopes. Here, we introduce an ultracold liquid helium transmission electron microscope side-entry specimen holder, featuring continuous cryogen flow and vibration decoupling. This instrument is compatible with modern aberration-corrected microscopes and achieves sub-25 K base temperature, ±2 mK thermal stability over many hours, and atomic resolution—setting the stage for a new era of cryogenic electron microscopy.

42 ENGINEERING

High-Rate Sputter Deposition of Ultrathick Boron Carbide Coatings on Rolling Spherical Substrates

Amorphous boron carbide (B 4 C) is a promising next-generation ablator material for inertial confinement fusion. However, the deposition of ultrathick B4C coatings with submicron-scale density uniformity on spherical substrates, as required for ablator shell fabrication, remains challenging. Here, in this study, we use direct current magnetron sputtering to deposit B 4 C onto 2-mm-diameter Si spheres rolling in a dish-shaped substrate holder. High deposition rates of ∼3 μm/h are achieved. Ultrathick films have a columnar microstructure, with the column width determined by the density of nodular defects. Nodular defect nucleation is dominated by the pickup of particulates from the holder during substrate rolling. We demonstrate the fabrication of a hollow B 4 C spherical shell with a wall thickness of 80 μm. Also demonstrated is the laser machining of holes in the B 4 C coating, which is necessary for both the chemical removal of the Si template and the attachment of a fusion fuel fill tube.

Inertial confinement fusion targets

Window Cooling Studies and Disk Vibration Testing on a Subset of Mo-100 Disks

Production of metastable Technetium-99 (Tc-99m), a radioactive tracer that emits gamma rays, is vital to the medical imaging community. Tc-99m is extracted from the decay of Molybdenum-99 (Mo-99) which has a half-life of about 2-3 days. The work presented in this report is part of the NNSA’s mission to produce Mo-99 commercially, within the US, without the use of highly enriched uranium (HEU) in support of nonproliferation and global security. Los Alamos National Laboratory (LANL) is working with NorthStar Medical Radioisotopes (NMR) on their efforts to produce Mo-99 through the irradiation of Mo-100 targets using an electron beam. The NMR target comprises a stack of approximately 60-70 Mo-100 disks with diameter 24 mm and thickness 0.74 mm held in stainless steel laminations, each separated using 0.25 mm thick stainless-steel spacers. The symmetric target stack is housed in an Inconel vessel with two Inconel windows on either side. Two electron accelerators are used to produce 40 MeV, 3.16 µA electron beams each that penetrate the Inconel windows and irradiate the Mo-100 disks. Approximately 90% of the total 250 kW beam power is deposited in the NMR target during the irradiation process, with a smaller percentage adding up to 2.2 kW of heat deposited on the Inconel window. During irradiation, pressurized helium gas flows through thin gaps between the disks cooling the beam window, target disks, disk laminations and spacers. Both NMR and LANL have found during cold testing of the target system (no heat deposition) that the Mo 100 disks undergo significant mass loss and disk breakage due to vibrations induced by the flowing helium gas. The mass loss is not only undesirable due to monetary loss from reduced final quantities of Mo-99, but also due to the hazards associated with radioactive material trapped in the cooling lines and particle filters. The effect of flow rate and target geometry on the flow induced vibrations need to be quantified, and recommendations provided to minimize this mass loss. LANL has previously also tested NMR’s Inconel beam window by heating the window, while flowing pressurized helium, using the average heat deposited on the window. However, the NMR beam is pulsed with a duty cycle of 12.5%, which introduces oscillation in temperature around the nominal 600 °C steady state value with each pulse. Available fatigue curves for Inconel are few, established for room temperature, and they are based on mechanical strain cycles not thermally induced strain as in the NMR target. The effect of pulsed beam heating on the Inconel window therefore needs to be quantified. This report details the experiments conducted to assess the factors that lead to mass loss in the NMR target disks as well as to understand the effect of a pulsed beam on NMR’s Inconel window. This work describes LANL’s experimental characterization of the flow induced vibrations and disk mass loss in a reduced scale set-up containing 5 to 10 Mo-100 disks. We use high speed imaging, displacement measurements and microphone measurements combined with signal processing to estimate the vibration frequency of each disk. The effect of disk thickness, target fit and duration of testing on the mass loss is described. We find that in the current configuration of NMR targets, the vibrations and mass loss on the first disk are minimized, while those in the adjacent disks are highest. The microphone and high-speed image data show that increased flow rates and increased duration of testing increases vibration frequency and mass loss. The mass loss is due to both disk rotation and back and forth motion. There are visible wear marks on the disks with the highest mass loss. We also note that the current NMR window gap reduces flow induced vibrations compared to the previous smaller gaps. Improved target holders significantly reduce disk mass loss to almost negligible quantities. This work finds that the larger window to first disk gap and improved target holder geometry should allow NMR to successfully conduct irradiations with minimal mass loss. The window tests were conducted to understand the effect of a pulsed beam on both the window longevity and to estimate the window temperature and displacement during pulsing. The experiments presented here were performed at significantly low power, due to the limitations of the induction heating system. The window temperature rose to approximately 73 °C with a significantly reduced power of 45 W without beam pulsing. With a 5 Hz pulse rate, 12.5% duty cycle, the window temperature remained constant at 26 °C. These experiments will be repeated with improved coil geometry and reported in upcoming journal papers.

42 ENGINEERING

AGR-5/6/7 Thermal Model with Non-uniform Gas Gaps

The daily as-run thermal analysis for the Advanced Gas Reactor (AGR)-5/6/7 experiment was documented in ECAR-5633 (Hawkes 2021). A finite element model was created for the entire test train, which consisted of five capsules. The fuel compacts, graphite holders, stainless-steel capsule walls, and all other major components were individually modeled, including all thermocouples (TCs). Daily heat rates for each compact and component in the model were input from daily as-run physics analyses. Daily gas compositions for each capsule were also input. The thermal conductivity of the compacts and graphite holders varied with fast neutron fluence. Gas mixture thermal conductivity was implemented using experimentally attained values from the literature. Fluence and temperature-dependent thermal conductivity was used for the graphite components and the fuel compacts. Radiation heat transfer was implemented. The model was tuned in an attempt to match the TC readings during the first cycle by adjusting the Neolube (graphite lubricant) thickness.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Characterizing Hazardous Gases from NMC811 Materials and Coin Cells with TGA and Tube-Furnace FTIR-MS Evolved-Gas-Analysis

Abuse testing is useful for informing the risks of different battery chemistries but has been limited to larger formats. This paper conducted thermal abuse tests at the smaller coin cell level to determine its relevance in specifying vent gas flammability and toxicity. A nitrogen purge carried the evolved gases into a parallel Fourier-transform infrared spectrometer (FTIR) and a mass spectrometer (MS) downstream of the tube furnace. The experimental system was validated by comparing evolved gas data for single components between the tube furnace system and a thermogravimetric analysis (TGA) instrument. Multiple samples were tested during validation, including CaCO3, electrolyte, delithiated NMC 811 cathode, and lithiated graphite anode. Temperature-resolved gas evolution of HF, CO2, CO, H2, and hydrocarbons from isolated components helped to characterize the emission sources. A previously unreported H2 generation mechanism was found. It was shown that the reduced NMC cathode acts as a catalyst to crack polypropylene-decomposed hydrocarbons into H2 at around 450 degrees C. It was also shown, while studying LiPF6 thermal decomposition, that using the tube furnace with a coin cell casing as the sample holder has some advantages for evolved-gas analysis of environmentally sensitive samples relative to testing in TGA instruments. After validation with single components, a fully charged NMC 811 coin cell was failed in the tube furnace. The measured evolved gases were found to be a combination of the species measured from the single component tests. H2 formation related to the reduced cathode was found to have greater abundance than H2 formed from the anode. Hydrogen fluoride emission factors and diethyl carbonate conversion emission factors assist in understanding the gaseous hazards for larger format cells.

25 ENERGY STORAGE

In situ observation of irradiation-induced enhancement to the desorption pressure of zirconium hydride in a nuclear reactor

We quantify the effect of a nuclear-reactor environment on the hydrogen isotope equilibrium vapor pressure over pure zirconium and zirconium hydride. A vacuum-sealed capsule containing a zirconium foil with 6 atom% deuterium was irradiated at a neutron flux of ~10 14 cm -2 s -1 at the University of Missouri Research Reactor (MURR). The internal stainless-steel (SS) sample holder acted as the heat source via gamma absorption. To measure low desorption pressures in a high-flux environment, we developed a method to transduce pressure from the measured sample temperature during irradiation, calibrating with known deuterium pressures in unirradiated capsules at various heating powers using an internal filament-heated system designed to mimic irradiation-induced heating. Our temperature-pressure transduction method operates similarly to a Pirani or thermocouple pressure gauge. The in-reactor measurements revealed a roughly 4-fold enhancement in desorption pressure after only 6 h of irradiation (~2 × 10 18 cm -2 neutron fluence) compared to thermal desorption in control experiments, indicating a nonthermal contribution from neutron irradiation. The slower temperature/pressure stabilization rate in the reactor suggests that desorption pressure enhancement increases with neutron fluence. Further, this enhancement signifies increased solubility of hydrogen isotopes in zirconium during irradiation. We propose that high-energy neutron collisions with hydrogen isotopes in hydrides lead to their decomposition at lower temperatures, supersaturating the surrounding αZr lattice and resulting in higher desorption pressure, which continues to rise as more hydrides dissolve with increasing neutron fluence.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS

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