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Recent Advancements in the PATO Material Response Code

Introduction: Predicting the complicated multiphysics phenomena during atmospheric entry requires high-fidelity modeling tools to refine estimates of mission risks during entry. To this end, new capabilities are being added to the Porous-material Analysis Toolbox based on OpenFOAM (PATO) [1,2,3]. PATO is an open-source software for Computational Material Response (CMR) of reactive porous materials submitted to high-temperature environments. The objective of this work is to highlight current efforts to add to and improve upon the modeling capabilities of PATO. These include efforts to loosely couple PATO with other discipline specialized codes including hypersonic Computational Fluid Dynamics (CFD), to assess the interaction effects between pyrolysis gas blowing and the boundary layer, and Computational Solid Mechanics (CSM), to address modeling of mechanical erosion. Other refinements include surface phenomena modeling capabilities to address the effects of silicone-based coatings applied to the TPS during flight preparation, and a unified multiphase solver for a mixed porous-material and plain-fluid domain. Coupling CMR with CFD (CMR/CFD): A loose coupling between PATO and the Data Parallel Line Relaxation (DPLR) [4] CFD code has been achieved by making use of a blowing boundary condition at the heatshield surface available in DPLR. Starting with heat flux estimates with no pyrolysis gas blowing at the surface, blowing gases are computed by the CMR and passed to the CFD such that aerothermal properties of the environment can be recomputed for a new CMR computation. This leads to an iterative process which is supplemented with an estimate of the radiative heat flux using the Nonequilibrium air radiation (NEQAIR) [5] program. The entire iterative process is illustrated in Figure 1. This coupling strategy has been utilized in computing the MSL material response. The goal is to compare the coupled CMR/CFD results with material response results obtained using traditional blowing corrections. Coupling CMS with CMR: A mechanical erosion model is currently being implemented in PATO to account for the additional mass removal induced by high shear conditions. The modeling process at each timestep consists of updating the mechanical properties as a function of temperature and computing the stress tensor and displacement fields of the material. Then, a failure criteria model determines the regions in which the stress exceeds the ultimate strength values resulting in mesh movement to account for mass removal. This model allows the material response simulation to compute the recession due to both oxidation and shear-induced erosion. The model is demonstrated by computing material response of sphere-cone arc jet samples. Surface Modeling Capabilities: NuSil, a silicone-based coating, was sprayed onto the MSL and Mars 2020 heatshields to mitigate shedding of phenolic dust. To better understand the effects of the NuSil coating on the material response, a novel model has been implemented in PATO. In this model, the equilibrium of the charred NuSil surface is modeled as pure silica, and a constant offset, inspired by the classical spallation model, is added to the the char blowing rate and wall enthalpy to reproduce HyMETS experimental results. The model has also been used to estimate the 3D material response of the MSL heatshield [6]. Unified Solver: In addition to the iterative loose coupling approach mentioned above, a multiphase unified solver is being developed to couple the environment (plain-fluid phase) and the porous-material phase. The solver is based on the volume averaged conservation of mass, momentum, and energy for the macroscale with closure models which include microscale effects through effective physicochemical properties. The unified solver has been used to compute flow through a porous plug and solve the Beavers and Joseph problem [7]. Since the strong coupling between phases is inherent to this solver, modeling assumptions present in other coupling methods of material response are mitigated. This strategy also makes it feasible to capture the competition between surface and volume ablation in the same computational domain, which is usually not possible with other coupling approaches.

Thermal Protection Systems↗
DOE OSTI2016

Effect of a gas on the ejection of particles from the free surface of a sample subjected to a shock wave with various intensities

In view of the possible effect of contamination of a plasma by metal particles on the operation of a number of facilities or on the detection of the motion of liners by Doppler methods, a particular attention has been recently focused on the problem of the ejection of particles from the shock-loaded free surface of a sample or on the “dusting” problem. Most information concerns the dusting source associated with the roughness of the surface, manufacturing technology, and the defectiveness and aging of a material. Factors affecting this process such as the profile and amplitude of the pressure on the front of the shock wave arriving at the free surface of the sample, the presence of the gas in front of the free surface, and the pressure in this gas are less studied.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Fracture‐Resistant and Thermally Insulating Ultrahigh‐Temperature Carbide Foams

Dense ultrahigh‐temperature ceramics (UHTCs) carbides are recognized as potential materials for thermal protection systems (TPS) owing to properties beyond existing structural materials’ capabilities. Recent advances in UHTCs have enabled the development of multiscale porous microstructures. Herein, it is highlighted that the porosity in UHTCs are no longer treated as a defect but as a functional property specifically tailored for thermal insulation. It is a promising solution to design and fabricate bulk UHTC foams via a freeze‐drying (FD) approach followed by calibrated pressureless spark plasma sintering. Herein, monolithic TaC and HfC UHTC foams and their composite show the partial solid–solution formation of (Ta, Hf)C with porosity ≥50%. TaC–HfC foam (≈80–92 N) shows an intermediate load‐bearing capability compared to monolithic TaC (≈120–135 N) and HfC (≈28–35 N) foams, with no evident cracking on the sample surface. The thermal conductivity of partial solid‐solution TaC–HfC foam increases up to fivefold compared to parent UHTC foams. In the results, solid solutions’ efficacy and pores’ unidirectionality in providing thermal insulation to TaC–HfC while maintaining its high‐load bearing capability are illustrated. In conclusion, the developed technique establishes a new paradigm shift in UHTCs, expanding their potential for TPS in extreme environments.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanoscale Antiferromagnetic Domain Imaging using Full-Field Resonant X-ray Magnetic Diffraction Microscopy

The physical properties of magnetic materials frequently depend not only on the microscopic spin and electronic structures, but also on the structures of mesoscopic length scales that emerge, for instance, from domain formations, or chemical and/or electronic phase separations. However, experimental access to such mesoscopic structures is currently limited, especially for antiferromagnets with net zero magnetization. Here, full-field microscopy and resonant magnetic X-ray diffraction are combined to visualize antiferromagnetic (AF) domains of the spin–orbit Mott insulator Sr 2 IrO 4 with area over ≈0.1 mm 2 and with spatial resolution as high as ≈150 nm. With the unprecedented wide field of views and high spatial resolution, an intertwining of two AF domains on a length comparable to the measured average AF domain wall width of 545 nm is revealed. This mesoscopic structure comprises a substantial portion of the sample surface, and thus can result in a macroscopic response unexpected from its microscopic magnetic structure. In particular, the symmetry analysis presented in this work shows that the inversion symmetry, which is preserved by the microscopic AF order, becomes ill-defined at the mesoscopic length scale. We report this result underscores the importance of this novel technique for a thorough understanding of the physical properties of antiferromagnets.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Top-Down Fabrication of Atomic Patterns in Twisted Bilayer Graphene

Atomic-scale engineering typically involves bottom-up approaches, leveraging parameters such as temperature, partial pressures, and chemical affinity to promote spontaneous arrangement of atoms. These parameters are applied globally, resulting in atomic-scale features scattered probabilistically throughout the material. In a top-down approach, different regions of the material are exposed to different parameters, resulting in structural changes varying on the scale of the resolution. In this work, the application of global and local parameters is combined in an aberration-corrected scanning transmission electron microscope (STEM) to demonstrate atomic-scale precision patterning of atoms in twisted bilayer graphene. The focused electron beam is used to define attachment points for foreign atoms through the controlled ejection of carbon atoms from the graphene lattice. The sample environment is staged with nearby source materials such that the sample temperature can induce migration of the source atoms across the sample surface. Under these conditions, the electron-beam (top-down) enables carbon atoms in the graphene to be replaced spontaneously by diffusing adatoms (bottom-up). Using image-based feedback control, arbitrary patterns of atoms and atom clusters are attached to the twisted bilayer graphene with limited human interaction. Finally, the role of substrate temperature on adatom and vacancy diffusion is explored by first-principles simulations.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Spatially Distributed Ramp Reversal Memory in VO 2

Ramp‐reversal memory has recently been discovered in several insulator‐to‐metal transition materials where a non‐volatile resistance change can be set by repeatedly driving the material partway through the transition. This study uses optical microscopy to track the location and internal structure of accumulated memory as a thin film of VO 2 is temperature cycled through multiple training subloops. These measurements reveal that the gain of insulator phase fraction between consecutive subloops occurs primarily through front propagation at the insulator‐metal boundaries. By analyzing transition temperature maps, it is found, surprisingly, that the memory is also stored deep inside both insulating and metallic clusters throughout the entire sample, making the metal‐insulator coexistence landscape more rugged. This non‐volatile memory is reset after heating the sample to higher temperatures, as expected. Diffusion of point defects is proposed to account for the observed memory writing and subsequent erasing over the entire sample surface. By spatially mapping the location and character of non‐volatile memory encoding in VO 2 , this study results enable the targeting of specific local regions in the film where the full insulator‐to‐metal resistivity change can be harnessed in order to maximize the working range of memory elements for conventional and neuromorphic computing applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Geochemical assessment of mineral sequestration of carbon dioxide in the midcontinent rift

Abstract This study examines the potential of Midcontinent Rift rocks to facilitate long‐term CO 2 sequestration by providing the necessary Ca and Mg for carbonate mineralization. Surface samples were collected from the Oronto and Bayfield‐Jacobsville Groups around Lake Superior and used for petrography and X‐ray diffraction to determine their mineral composition. Also, X‐ray fluorescence was also used to assess their bulk chemical composition. The samples were then exposed to CO 2 and deionized water in Teflon‐lined vessels at 90°C, and the resulting leachate fluids were analyzed for the cation released during the testing. SEM microscopy was used to examine the samples for potential mineralization of carbonate minerals. The Oronto Group sediments consist primarily of feldspathic to feldspathic lithic arenites with a chlorite‐dominated matrix, and the primary porosity is blocked by calcite and hematite cement. The Bayfield–Jacobsville sequences are porous quartz arenites to feldspathic quartz arenites that do not contain significant accumulation of Ca‐, Mg‐, and Fe‐bearing minerals. The leachate fluids obtained from Oronto Group samples exhibit a maximum Ca release rate (5.2 × 10 −4 mole/cm 2 .day), indicating rapid calcite cement dissolution and increased porosity and permeability. SEM/EDS microanalysis revealed areas where pore‐filling calcite was preferentially dissolved. Longer‐term rock‐water reactions resulted in induced carbonate mineralization, as evidenced by calcite crystals observed in a sample reacted for 102 days. © 2024 Society of Chemical Industry and John Wiley & Sons, Ltd.

Energy & Fuels↗
DOE OSTI2024

Utilization of Ultrasonication as a Method of Reducing Organic and Inorganic Contamination in Post‐Consumer Plastic Film Waste

Post-consumer plastic film waste often carries organic and inorganic contaminants that challenge recycling processes and affect the quality of recycled products. An effective contaminant removal procedure through washing such single-used plastic films (SUPFs) can address environmental and waste management concerns. This study compares the efficiency of different washing techniques in reducing SUPF contamination. To evaluate the efficacy of each washing technique, film samples collected from material recovery facilities are individually exposed to friction, ultrasonic-assisted, and a combination of both washes. Thermal analysis indicates that the polymers' melting temperature, crystallization temperature, and crystallinity remain unaffected by the washing methods, demonstrating method aptness. Confocal laser scanning microscope images show that washing results in a cleaner sample surface. 91% ash reduction during the combined wash treatment indicates a high method efficiency compared to the individual friction and ultrasonic wash procedures. This is further validated by reducing characteristic contaminant IR bands (3600–3000, 1750–1600, and 1100–1000 cm −1 ). Elements of concern such as Cd, Cr, Hg, and Pb in SUPFs after each washing technique applied conform with regulations (<100 ppm) for packaging products. This research shows the novel ultrasonic washing reduces more contamination than friction with shorter wash times and no surfactants.

42 ENGINEERING↗
DOE OSTI2021

Generalized Ellipsometry Measurements of Crystalline Thin Film and Bulk Tin Oxide

Here, several bulk and thin-film crystals of SnO2 are grown and examined using generalized ellipsometry techniques. The bulk samples are grown using the chemical vapor transport technique and thin films of SnO2 are grown using the pulsed laser deposition technique. The bulk samples are examined using the two-modulator generalized ellipsometry microscope (2-MGEM) at normal incidence and the spectroscopic two-modulator generalized ellipsometer (2-MGE). The spectroscopic optical functions of tin oxide are then obtained using the 2-MGE from 1.46 to 6.2 eV. The material is highly birefringent, and the ordinary bandgap is less than the extraordinary band edge. 2-MGE measurements are also made on thin-film samples of crystalline tin oxide grown on sapphire and rutile, showing no cross polarization. Because of the complicated morphology of the tin oxide films grown on sapphire, the ellipsometry data are simulated using the Tauc–Lorentz model. Films grown on rutile had the optic axis perpendicular to the sample surface, but the film is strained, resulting in a more complicated ellipsometric spectrum. These films are modeled using the air/surface roughness/tin oxide/interface/rutile model, where the roughness and interface are modeled using the incomplete Beta function.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Laser Microdissection and Atmospheric Pressure Chemical Ionization Mass Spectrometry Coupled for Multimodal Imaging

This paper describes the coupling of ambient laser ablation surface sampling, accomplished using a laser capture microdissection system, with atmospheric pressure chemical ionization mass spectrometry for high spatial resolution multimodal imaging. A commercial laser capture microdissection system was placed in close proximity to a modified ion source of a mass spectrometer designed to allow for sampling of laser ablated material via a transfer tube directly into the ionization region. Rhodamine 6G dye of red sharpie ink in a laser etched pattern as well as cholesterol and phosphatidylcholine in a cerebellum mouse brain thin tissue section were identified and imaged from full scan mass spectra. A minimal spot diameter of 8 m was achieved using the 10X microscope cutting objective with a lateral oversampling pixel resolution of about 3.7 m. Distinguishing between features approximately 13 m apart in a cerebellum mouse brain thin tissue section was demonstrated in a multimodal fashion including co-registered optical and mass spectral chemical images.

atmospheric pressure chemical ionization (APCI)↗
DOE OSTI2018

Integration of paper spray ionization high‐field asymmetric waveform ion mobility spectrometry for forensic applications

Rationale Paper spray ionization (PSI) is an attractive ambient ionization source for mass spectrometry (MS) since it allows the combination of surface sampling and ionization. The minimal sample preparation inherent in this approach greatly reduces the time needed for analysis. However, the ions generated from interfering compounds in the sample and the paper substrate may interfere with the analyte ions. Therefore, the integration of PSI with high‐field asymmetric ion mobility spectrometry (FAIMS) is of significant interest since it should reduce the background ions entering the mass analyzer without complicating the analysis or increasing analysis time. Here we demonstrate the integration of PSI with FAIMS/MS and its potential for analysis of samples of forensic interest. Methods In this work, the parameters that can influence the integration, including sampling and ionization by paper spray, the FAIMS separation of analytes from each other and background interferences, and the length of time that a usable signal can be observed for explosives on paper, were evaluated with the integrated system. Results In the negative ion analysis of 2,4,6‐trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN), octahydro‐1,3,5,7‐tetranitro‐1,3,5,7‐tetrazocine (HMX), and 1,3,5‐trinitroperhydro‐1,3,5‐triazine (RDX), amounts as low as 1 ng on paper were readily observed. The successful positive ion separation of a set of illicit drugs including heroin, methamphetamine, and cocaine was also achieved. In addition, the positive ion analysis of the chemical warfare agent simulants dimethyl methylphosphonate (DMMP) and diisopropyl methylphosphonate (DIMP) was evaluated. Conclusions The integration of PSI‐FAIMS/MS was demonstrated for the analyses of explosives in negative ion mode and for illicit drugs and CW simulants in positive mode. Paper background ions that could interfere with these analyses were separated by FAIMS. The compensation voltage of an ion obtained by FAIMS provided an additional identification parameter to be combined with the mass spectrum for each analyte.

Tsai, Chia‐Wei↗
DOE OSTI2021

Integrated laser ablation-dropletProbe-mass spectrometry for absolute drug quantitation, metabolite detection, and distribution in tissue

Rationale: Spatially resolved and accurate quantitation of drug-related compounds in tissue is a much-needed capability in drug discovery research. In this work, application of an integrated laser ablation-dropletProbe-mass spectrometry surface sampling system (LADP-MS) is reported, which achieved absolute quantitation of propranolol measured from <500 × 500 μm thin tissue samples. Methods: Mouse liver and kidney thin tissue sections were coated with parylene C and analyzed for propranolol by a laser ablation/liquid extraction workflow. Non-coated adjacent sections were microdissected for validation and processed using standard bulk tissue extraction protocols. High-performance liquid chromatography with positive ion mode electrospray ionization tandem mass spectrometry was applied to detect the drug and its metabolites. Results: Absolute propranolol concentration in ~500 × 500 μm tissue regions measured by the two methods agreed within ±8% and had a relative standard deviation within ±17%. Quantitation down to ~400 × 400 μm tissue regions was shown, and this resolution was also used for automated mapping of propranolol and phase II hydroxypropranolol glucuronide metabolites in kidney tissue. Conclusions: This study exemplifies the capabilities of integrated laser ablation-dropletProbe-mass spectrometry (LADP-MS) for high resolution absolute drug quantitation analysis of thin tissue sections. This capability will be valuable for applications needing to quantitatively understand the spatial distribution of small molecules in tissue.

47 OTHER INSTRUMENTATION↗
DOE OSTI2015

Subcellular-level resolution MALDI-MS imaging of maize leaf metabolites by MALDI-linear ion trap-Orbitrap mass spectrometer

A significant limiting factor in achieving high spatial resolution for matrix-assisted laser desorption ionization-mass spectrometry (MALDI-MS) imaging is the size of the laser spot at the sample surface. We present modifications to the beam-delivery optics of a commercial MALDI-linear ion trap-Orbitrap instrument, incorporating an external Nd:YAG laser, beam-shaping optics, and an aspheric focusing lens, to reduce the minimum laser spot size from ~50 μm for the commercial configuration down to ~9 μm for the modified configuration. This improved system was applied for MALDI-MS imaging of cross sections of juvenile maize leaves at 5-μm spatial resolution using an oversampling method. There are a variety of different metabolites including amino acids, glycerolipids, and defense-related compounds were imaged at a spatial resolution well below the size of a single cell. Such images provide unprecedented insights into the metabolism associated with the different tissue types of the maize leaf, which is known to asymmetrically distribute the reactions of C4 photosynthesis among the mesophyll and bundle sheath cell types. The metabolite ion images correlate with the optical images that reveal the structures of the different tissues, and previously known and newly revealed asymmetric metabolic features are observed.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

Calibration curves for commercial copper and aluminum alloys using handheld laser-induced breakdown spectroscopy

Handheld laser-induced breakdown spectroscopy (HH LIBS) was used to study the elemental composition of four copper alloys and four aluminum alloys to produce calibration curves. The HH LIBS instrument used is a SciAps Z-500, commercially available, that contains a class-1 solid-state laser with an output wavelength of 1532 nm, a laser energy of 5 mJ/pulse, and a pulse duration of 5 ns. Test samples were solid specimens comprising of copper and aluminum alloys and data were collected from the samples’ surface at three different locations, employing a 12-point-grid pattern for each data set. All three data sets of the spectra were averaged, and the intensity, corrected by subtraction of background, was used to produce the elemental calibration curves. Calibration curves are presented for the matrix elements, copper and aluminum, as well as several minor elements. The surface damage produced by the laser was examined by microscopy. The alloys were tested in air and in a glovebox to evaluate the instrument’s ability to identify the constituents within materials under different environmental conditions. The main objective of using this HH LIBS technology is to determine its capability to fingerprint the presence of certain elements related to subpercent level within materials in real time and in-situ, as a starting point for undertaking future complex material characterization work.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Thermal Evolution of the Proton Irradiated Structure in Tungsten–5 wt% Tantalum

We have monitored the thermal evolution of the proton irradiated structure of W–5 wt% Ta alloy by in-situ annealing in a transmission electron microscope at fusion reactor temperatures of 500–1300 °C. The interstitial-type a/2<111> dislocation loops emit self-interstitial atoms and glide to the free sample surface during the early stages of annealing. The resultant vacancy excess in the matrix originates vacancy-type a/2<111> dislocation loops that grow by loop and vacancy absorption in the temperature range of 600–900 °C. Voids form at 1000 °C, by either vacancy absorption or loop collapse, and grow progressively up to 1300 °C. Tantalum delays void formation by a vacancy-solute trapping mechanism.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Tungsten Blister Formation Kinetic as a Function of Fluence, Ion Energy and Grain Orientation Dependence Under Hydrogen Plasma Environment

This work deals with the formation kinetic of tungsten (W) blisters under smooth plasma conditions, i.e. low hydrogen flux and energy in order to analyze the first stages of their formation. In addition, we focus on determining the W grain orientation where blisters grow preferentially. For this purpose, mirror-polished polycrystalline tungsten samples were exposed to hydrogen plasma under fixed hydrogen flux of 2.2 × 10{sup 20} m{sup −2} s{sup −1}, with a fluence in the range of ~ 10{sup 24} m{sup −2}, ion energy of ~ 20, 120 and 220 eV, and sample surface temperature of ~ 500 K. The formation of blisters at the surface was investigated using SEM, AFM and EBSD to determine the size, the distribution and the orientation of grain where blisters are formed, respectively. The critical fluence for initiating blisters was established around 2.3 × 10{sup 24} m{sup −2}. The evolution of blister size distribution and density is discussed as function of fluence and ion energy. At lower ion energy, i.e. 20 eV, only nanoblisters (less than 150 nm) are observed whatever the fluence value (1.5 and 2.3 × 10{sup 24} m{sup −2}). At higher ion energy i.e. 120 and 220 eV, micrometric (~ few to tens of µm) blisters are observed and their density highly depends on fluence. We show that blisters can also be formed on (001) oriented grains contrarily to previous results from the literature where the (111) orientation seemed more favorable. Such information is of importance for tungsten based fusion tokamak operation and design.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2019

Manufacturing, Structure, Properties of MgB{sub 2}-Based Materials

The composition of MgB{sub 2}-based materials (wires, bulks, and thin films) with high critical current densities, j{sub c}, prepared at different pressure (0.1 MPa–2 GPa)—temperature (600–1050 °C) conditions was analyzed by the X-ray and JAMP−9500F Auger spectrometer (after removing the oxidized layers at the sample surfaces by Ar ion etching performed directly in the vacuum chamber of a microscope). Similar regularly distributed inhomogeneities connected with Mg, B, and admixture O content variation on the nanolevel were observed in all types of the MgB{sub 2}-based materials. The correlations between the character of the material inhomogeneities and the attained superconducting characteristics are discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗