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At least 145 records · Page 8

Flexible cryogenic air separation unit—An application for low-carbon fossil-fuel plants

In this study, the rapid integration of intermittent renewable sources into the electricity grid is driving the need for a flexible cryogenic air separation unit (ASU) coupled with a low-carbon fossil-fuel plant. However, the state-of-the-art ASU process is highly integrated and nonlinear, which can significantly restrict its ramping rate. In this work, we study the fundamental dynamics of a state-of-the-art double-column ASU, focusing on the dynamic characteristics of the highly integrated and nonlinear heat and mass transfers, and we propose basic control methods for achieving high process ramping rates. We found that the vapor–liquid countercurrent flows in the low-pressure column are critical to the cryogenic rectification of air, which governs the ramp rate of the ASU. This countercurrent flow structure is created through a complex heat integration process in the ASU. Here, this process is simplified as a countercurrent heat transfer to reduce the complexity of studying the ASU dynamics. To preserve this flow structure, the heat integration is maintained so that its heat duty follows the ASU load, using several basic controllers on the critical stream flowrates. A flow-driven dynamic ASU model is built in Aspen Plus Dynamics to capture the basic ramping dynamics. This model revealed a fundamental mismatch in the dynamics in the ASU column that causes a significant loss of O 2 product purity when ramping down the ASU and slightly increases the purity when ramping up. Based on these findings, we propose a basic control method for rapidly ramping down/up the ASU while maintaining O 2 product purity. Simulation results show the ASU basic dynamic process successfully ramps at a rate up to 10 %/min (40–100 % load) while maintaining the O 2 product purity at 95.2–95.6 mol%.

42 ENGINEERING↗

Minimizing Crinkling of Soft Specimens Using Holey Gold Films on Molybdenum Grids for Cryogenic Electron Microscopy

We introduce a novel composite holey gold support that prevents cryo-crinkling and reduces beam-induced motion of soft specimens, building on the previously introduced all-gold support. The composite holey gold support for high-resolution cryogenic electron microscopy of soft crystalline membranes was fabricated in two steps. In the first step, a holey gold film was transferred on top of a molybdenum grid. In the second step, a continuous thin carbon film was transferred onto the holey gold film. This support (Au/Mo grid) was used to image crystalline synthetic polymer membranes. The low thermal expansion of Mo is not only expected to avoid cryo-crinkling of the membrane when the grids are cooled to cryogenic temperatures, but it may also act to reduce whatever crinkling existed even before cooling. Here, the Au/Mo grid exhibits excellent performance with specimens tilted to 45°. This is demonstrated by quantifying beam-induced motion and differences in local defocus values. In addition, images of specimens on the Au/Mo grids that are tilted at 45° show high-resolution information of the crystalline membranes that, after lattice-unbending, extends beyond 1.5 Å in the direction perpendicular to the tilt axis.

36 MATERIALS SCIENCE↗

Cryogenic Reduction of Surface-Bound HKUST-1Crystallites

HKUST-1 is a canonical Cu-based metal-organic framework (MOF) with potential roles in catalysis. A convenient hydroxy double salt templating synthesis was used to produce a thin layer of HKUST-1 crystallites amenable to surface science spec-troscopies under controlled conditions. To study the nature of the Cu sites, N2 and CO2 were adsorbed at cryogenic tempera-tures as passive probe molecules for Cu2+ sites. CO, which is commonly used as a probe molecule of both Cu2+ and Cu1+ sites in porous materials, was found to be a non-innocent probe molecule that reduces the Cu2+ and forms CO2. Isotopically labeled 13CO confirmed the Cu2+ reduction and CO oxidation. The results offer a way to tune Cu oxidation states in HKUST-1, even in the cryogenic temperature regime.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cryogenic “Iodide-Tagging” Photoelectron Spectroscopy: A Sensitive Probe for Specific Binding Sites of Amino Acids

This work showcases cryogenic and temperature-dependent “iodide-tagging” photoelectron spectroscopy to probe specific binding sites of amino acids using the glycine-iodide complex (Gly?I-) as a case study. Multiple Gly?I- isomers were generated from ambient electrospray ionization and kinetically isolated in a cryogenic ion trap. These structures were characterized with temperature-dependent “iodide-tagging” negative ion photoelectron spectroscopy (NIPES) where iodide was used as the “messenger” to interpret electronic energetics and structural information of various Gly?I- isomers. Accompanied by theoretical computations and Franck-Condon simulations, a total of five cluster structures have been identified along with their various binding motifs. This work demonstrates that “iodide-tagging” NIPES is a powerful general means for probing specific binding interactions in biological molecules of interest.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

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↗

Extracellular filaments revealed by affinity capture cryogenic-electron tomography

Cryogenic-electron tomography (cryo-ET) has provided an unprecedented glimpse into the nanoscale architecture of cells by combining cryogenic preservation of biological structures with electron tomography. Micropatterning of extracellular matrix proteins is increasingly used as a method to prepare adherent cell types for cryo-ET as it promotes optimal positioning of cells and subcellular regions of interest for vitrification, cryo-focused ion beam (cryo-FIB) milling, and data acquisition. Here we demonstrate a micropatterning workflow for capturing minimally adherent cell types, human T cells and Jurkat cells, for cryo-FIB and cryo-ET. Our affinity capture system facilitated the nanoscale imaging of Jurkat cells, revealing extracellular filamentous structures. It improved workflow efficiency by consistently producing grids with a sufficient number of well-positioned cells for an entire cryo-FIB session. Affinity capture can be extended to facilitate high-resolution imaging of other adherent and non-adherent cell types with cryo-ET.

Biochemistry↗

A classical equation that accounts for observations of non-Arrhenius and cryogenic grain boundary migration

Observations of microstructural coarsening at cryogenic temperatures, as well as numerous simulations of grain boundary motion that show faster migration at low temperature than at high temperature, have been troubling because they do not follow the expected Arrhenius behavior. This work demonstrates that classical equations, that are not simplified, account for all these oddities and demonstrate that non-Arrhenius behavior can emerge from thermally activated processes. According to this classical model, this occurs when the intrinsic barrier energies of the processes become small, allowing activation at cryogenic temperatures. Additional thermal energy then allows the low energy process to proceed in reverse, so increasing temperature only serves to frustrate the forward motion. This classical form is shown to reconcile and describe a variety of diverse grain boundary migration observations.

36 MATERIALS SCIENCE↗

A cryogenic near-field thermal diode leveraging superconducting phase transitions

Control of charge and heat transport is essential for computing and thermal management technologies. Recent work with superconducting materials has shown rectified electrical supercurrents near liquid helium temperatures. However, despite large theoretical interest and expected impact on quantum technologies, no experiments have demonstrated control of nanoscale radiative heat currents at cryogenic temperatures. Here we study photon-mediated thermal transport in nanogaps between niobium and gold. Using novel scanning calorimetric probes and nanofabricated devices, we reveal a ~20-fold suppression of radiative heat transport, when niobium transitions from the metallic to the superconducting state. Taking advantage of this effect, we also demonstrate a niobium-based cryogenic thermal diode with a heat rectification ratio of 70%. As a result, the experimental techniques and advances presented here will enable studying nanoscale thermal transport in quantum materials and advancing thermal management of superconducting devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Investigating the hydrolysis of cryogenically layered molybdenum hexafluoride through a disordered hydrogen-bonded network

Molybdenum hexafluoride (MoF6) is used as a non-radioactive substitute for uranium to study the hydrolysis of metal hexafluorides. Molybdenum hexafluoride gas and water vapor, from the air, were sequentially layered onto a diamond substrate kept at liquid nitrogen temperature using a custom designed cryogenic cell with a copper cold finger. Reaction progress was monitored by transmission Fourier Transform Infrared Spectroscopy (FTIR) through the layers and diamond substrate over several hours while allowing the substrate to warm. Changes in the modes in the 500–1000 cm -1 region are tracked as the reaction progresses in order to identify intermediate species. Strong absorption features are also observed in the 1000–3000 cm -1 range, suggesting the presence of ionic dissociation intermediates trapped in a disordered H-bonded network of cryogenic hydrofluoric acid. Here, a possible reaction pathway is proposed and the final hydrolysis product is characterized by FTIR, UV-vis, and scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Near-cryogenic direct air capture using adsorbents

Direct air capture (DAC) of CO 2 is a key component in the portfolio of negative emissions technologies for mitigating global warming. However, even with the most potent amine sorbents, large-scale DAC deployment remains limited by high energy and capital costs. Recently, adsorbents relying on weak interactions with CO 2 have emerged as a potential alternative, thanks to their rapid adsorption kinetics and superior long-term stability, particularly under sub-ambient conditions (∼253 K). Despite these advantages, their use is hindered by the need for a water-removal process, location-specific constraints, and insufficient working capacity even in cold climates. In this study, we hypothesized that further reducing the adsorption temperature to a near-cryogenic range (160–220 K) could enable cost-effective DAC by utilizing the full potential of physisorbents. We primarily consider integrating DAC with a relatively untapped source of cold energy—liquified natural gas (LNG) regasification—to perform near-cryogenic DAC. From large-scale molecular simulations, Zeolite 13X and CALF-20 were identified as promising candidates. These materials were subsequently examined through experiments, including breakthrough analyses at 195 K. Their high CO 2 sorption capacity (4.5–5.5 mmol g −1 ), combined with a low desorption enthalpy and robust long-term stability, led to a threefold reduction in the levelized cost of capture (down to 68.2 USD per tonne CO 2 ). Estimates of the global LNG regasification resource suggest that LNG–DAC coupling could potentially enable the capture of 103–142 megatonnes of CO 2 annually as of 2050.

Kim, Seo-Yul [Georgia Institute of Technology, Atl↗

Cryogenic goniometer for measurements in pulsed magnetic fields fabricated via additive manufacturing technique

Complex high-precision mechanical devices can be fabricated using 3-dimensional printing technology with the help of computer-aided design. Using 3D stereolithography, we have constructed a cryogenic goniometer for measurements in pulsed magnetic fields of up to 100 T, at temperatures as low as 0.5 K. We review the properties of several materials tested in developing the goniometer and report on its design and performance. The goniometer allows samples to be rotated in situ to a precision of 0.2 deg, so that the field can be applied at many different angles to the samples’ symmetry directions. Following its success, we establish that 3D printing is now a viable technology for pulsed-field and other cryogenic probes.

3D printing↗

A multi-channel x-ray temporal diagnostic for measurement of time-resolved electron temperature in cryogenic deuterium–tritium implosions at OMEGA

Electron-temperature (T e ) measurements in implosions provide valuable diagnostic information, as Te is unaffected by residual flows and other non-thermal effects unlike ion temperature inferred from a fusion product spectrum. In OMEGA cryogenic implosions, measurement of T e (t) can be used to investigate effects related to time-resolved hot-spot energy balance. The proposed diagnostic utilizes five fast-rise (~15 ps) scintillator channels with distinct x-ray filtering. Furthermore, titanium and stepped aluminum filtering were chosen to maximize detector sensitivity in the 10 keV–20 keV range, as it has been shown that these x rays have similar density and temperature weighting to the emitted deuterium–tritium fusion neutrons. Initial data collected using a prototype nosecone on the existing neutron temporal diagnostic demonstrate the validity of this diagnostic technique. The proposed system will be capable of measuring spatially integrated T e (t) with 20 ps time resolution and <10% uncertainty at peak emission in cryogenic DT implosions.

47 OTHER INSTRUMENTATION↗

Application of an energy-dependent instrument response function to analysis of nTOF data from cryogenic DT experiments

Neutron time-of-flight (nTOF) detectors are used to diagnose the conditions present in inertial confinement fusion (ICF) experiments and basic laboratory physics experiments performed on an ICF platform. The instrument response function (IRF) of these detectors is constructed by convolution of two components: an x-ray IRF and a neutron interaction response. The shape of the neutron interaction response varies with incident neutron energy, changing the shape of the total IRF. Analyses of nTOF data that span a broad range of energies must account for this energy-dependence in order to accurately infer plasma parameters and nuclear properties in ICF experiments. This work briefly reviews a matrix multiplication approach to convolution which allows for an energy-dependent change in the shape of the IRF. This method is applied to synthetic data resembling symmetric cryogenic DT implosions to examine the effect of the energy-dependent IRF on the inferred areal density. Here, results of forward fits that infer ion temperatures and areal densities from nTOF data collected during cryogenic DT experiments on OMEGA are also discussed.

47 OTHER INSTRUMENTATION↗

Causes of fuel–ablator mix inferred from modeling of monochromatic time-gated radiography of OMEGA cryogenic implosions

Here, we present evidence, in the context of OMEGA cryogenic target implosions, that laser imprint, known to be capable of degrading laser-direct-drive target performance, plays a major role in generating fuel–ablator mix. OMEGA cryogenic target implosions show a performance boundary correlated with acceleration-phase shell stability; for sufficiently low adiabats (where the adiabat is the ratio of the pressure to the Fermi pressure) and high in-flight aspect ratios (IFAR's), the neutron-weighted shell areal density and neutron yield relative to the clean simulated values sharply decline. Direct evidence of Rayleigh–Taylor fuel–ablator mixing was previously obtained using a Si Heα backlighter driven by an ~20-ps short pulse generated by OMEGA EP. The shadow cast by the shell shortly prior to stagnation, as diagnosed using backlit radiographs, shows a softening near the limb, which is evidence of an ablator–fuel mix region for a low-adiabat implosion (α ~ 1.9, IFAR = 14) but not for a moderate adiabat implosion (α ~ 2.5, IFAR = 10). We find good agreement between experimental and synthetic radiographs in simulations that model laser imprint and account for uncertainty in the initial ablator thickness. Furthermore, we further explore the role of other mechanisms such as classical instability growth at the fuel–ablator interface, species concentration diffusion, and long-wavelength drive and target asymmetries.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Enhanced laser-energy coupling with small-spot distributed phase plates (SG5-650) in OMEGA DT cryogenic target implosions

Cryogenic deuterium–tritium ice target implosions on OMEGA with new small-spot (SG5-650) distributed phase plates (DPPs) achieved an (11 ± 4)% increase in energy coupling compared to implosions with larger-spot SG5-850 DPPs by decreasing the ratio of the laser spot diameter to the target diameter from 0.93 to 0.75. The SG5-650 DPPs provide a focus spot size of 674 μm, which is defined as the diameter that encircles 95% of the measured beam energy compared to 834 μm for the SG5-850, which are the standard DPPs in cryogenic target implosions on OMEGA. The hydrodynamic efficiency, defined as the ratio of the kinetic energy in the imploding shell to the laser energy, increased from 4.5% to 5.0% based on radiation-hydrodynamic calculations benchmarked to shell trajectory and bang-time measurements. Furthermore, the higher coupling came with a trade-off of an increased hot-electron production as well as increased hydrodynamic instabilities seeded by a larger mode-10 amplitude from the beam port geometry, both of which may have reduced the fusion neutron production and areal density.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Diagnosing low-mode (ℓ < 6) and mid-mode (6 ≤ ℓ ≤ 60) asymmetries in the post-stagnation phase of laser-direct-drive deuterium–tritium cryogenic implosions on OMEGA

Low- and mid-mode perturbations are possible candidates for performance limitations in cryogenic direct-drive implosions on the OMEGA laser at the Laboratory of Laser Energetics. Simulations with a 3D hydrocode demonstrated that hotspot imagers do not show evidence of the shell breakup in the dense fuel. However, these same simulations revealed that the low- and mid-mode perturbations in the dense fuel could be diagnosed more easily in the post-stagnation phase of the implosion by analyzing the peak in the x-ray emission limb at the coronal–fuel interface than before or at the stagnation phase. In experiments, the asymmetries are inferred from gated images of the x-ray emission of the implosion by using a 16-pinhole array imager filtered to record x-ray energies >800 eV and an x-ray framing camera with 40-ps time integration and 20-μm spatial resolution. Furthermore, a modal analysis is applied to the spatial distribution of the x-ray emission from deuterium and tritium cryogenic implosions on OMEGA recorded after the bang time to diagnose the low- and mid-mode asymmetries, and to study the effect that the beam-to-target ratio (Rb/Rt) has on the shell integrity.

47 OTHER INSTRUMENTATION↗

The Simons Observatory: Cryogenic half wave plate rotation mechanism for the small aperture telescopes

We present the requirements, design, and evaluation of the cryogenic continuously rotating half-wave plate (CHWP) for the Simons Observatory (SO). SO is a cosmic microwave background polarization experiment at Parque Astronómico de Atacama in northern Chile that covers a wide range of angular scales using both small (Ø0.42 m) and large (Ø6 m) aperture telescopes. In particular, the small aperture telescopes (SATs) focus on large angular scales for primordial B-mode polarization. To this end, the SATs employ a CHWP to modulate the polarization of the incident light at 8 Hz, suppressing atmospheric 1/f noise and mitigating systematic uncertainties that would otherwise arise due to the differential response of detectors sensitive to orthogonal polarizations. The CHWP consists of a 505 mm diameter achromatic sapphire HWP and a cryogenic rotation mechanism, both of which are cooled down to ~50 K to reduce detector thermal loading. Under normal operation, the HWP is suspended by a superconducting magnetic bearing and rotates with a constant 2 Hz frequency, controlled by an electromagnetic synchronous motor. We find that the number of superconductors and the number of magnets that make up the superconducting magnetic bearing are important design parameters, especially for the rotation mechanism’s vibration performance. The rotation angle is detected through an angular encoder with a noise level of 0.07 μrad √ $\overline{s}$. During a cooldown process, the rotor is held in place by a grip-and-release mechanism that serves as both an alignment device and a thermal path. In this paper, we provide an overview of the SO SAT CHWP: its requirements, hardware design, and laboratory performance.

47 OTHER INSTRUMENTATION↗

Cryogen-free modular scanning tunneling microscope operating at 4-K in high magnetic field on a compact ultra-high vacuum platform

One of the daunting challenges in modern low temperature scanning tunneling microscopy (STM) is the difficulty of combining atomic resolution with cryogen-free cooling. Further functionality needs, such as ultra-high vacuum (UHV), high magnetic field (HF), and compatibility with μm-sized samples, pose additional challenges to an already ambitious build. We present the design, construction, and performance of a cryogen-free, UHV, low temperature, and high magnetic field system for modular STM operation. An internal vibration isolator reduces vibrations in this system, allowing for atomic resolution STM imaging while maintaining a low base temperature of ∼4 K and magnetic fields up to 9 T. Samples and tips can be conditioned in situ utilizing a heating stage, an ion sputtering gun, an e-beam evaporator, a tip treater, and sample exfoliation. In situ sample and tip exchange and alignment are performed in a connected UHV room temperature stage with optical access. Multisite operation without breaking vacuum is enabled by a unique quick-connect STM head design. A novel low-profile vertical transfer mechanism permits transferring the STM between room temperature and the low temperature cryostat.

Instruments & Instrumentation↗