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DOE OSTI2018

ToF-SIMS characterization of glyoxal surface oxidation products by hydrogen peroxide: A comparison between dry and liquid samples

As one of the simplest volatile organic compounds (VOCs), glyoxal and its oxidation products were considered to be important precursors to aqueous secondary organic aerosol (aqSOA) formation. Herein, we analyzed products from glyoxal oxidation by hydrogen peroxide in dry and liquid samples using time-of-flight secondary ion mass spectrometry (ToF-SIMS). ToF-SIMS spectra and spectral principal component analysis (PCA) were used to investigate surface oxidation products. Dry samples were prepared on clean silicon wafers. Liquid samples consisting of glyoxal and hydrogen peroxide (H2O2) were introduced to a vacuum compatible microfluidic reactor prior to UV illumination or dark aging followed by in situ liquid SIMS analysis. A number of reaction products were observed in both dry and liquid samples; different oligomers and carboxylic acids could be formed depending on reaction conditions. In addition, hydrolyzed products were observed in the liquid samples, but not in the dry samples. Although dry samples reveal some products of the aqueous process, they are not fully representative as results from those of the aqueous samples. Our findings suggest that the ability to characterize the liquid surface reaction products provides more realistic information of the reaction products associated with aqSOA formation in the atmosphere. Meanwhile, the high mass resolution spectra from the dry sample SIMS measurement are helpful to identify oxidation products in the liquid samples.

, Aqueous Secondary Organic Aerosol, Sample Prepar↗

NASA NTRS1980

Mars sample return: Site selection and sample acquisition study

Various vehicle and mission options were investigated for the continued exploration of Mars; the cost of a minimum sample return mission was estimated; options and concepts were synthesized into program possibilities; and recommendations for the next Mars mission were made to the Planetary Program office. Specific sites and all relevant spacecraft and ground-based data were studied in order to determine: (1) the adequacy of presently available data for identifying landing sities for a sample return mission that would assure the acquisition of material from the most important geologic provinces of Mars; (2) the degree of surface mobility required to assure sample acquisition for these sites; (3) techniques to be used in the selection and drilling of rock a samples; and (4) the degree of mobility required at the two Viking sites to acquire these samples.

Nickle, N.↗

NASA NTRS2012

Space X1 First Entry Sample

One mini-grab sample container (m-GSC) was returned aboard Space X1 because of the importance of quickly knowing first-entry conditions in this new commercial module. This sample was analyzed alongside samples of the portable clean room (PCR) used in the Space X complex at KSC. The recoveries of C-13-acetone, fluorobenzene, and chlorobenzene from the GSCs averaged 130, 129, and 132 %, respectively.

James, John T.↗

DOE OSTI2019

Waste Characterization Methods Based on Gamma-ray Imaging Spectrometers - 19454

Characterization of LLW, ILW, U, NORM and TENORM is critical to the nuclear industry's bottom line. Accurate measurements enable the disposal of waste at the lowest possible cost. In the past the most accurate technology available involved using HPGe detectors and extensive system modeling to estimate the total source term given what the user knows about the geometry of the source and any shielding between the source and the detectors. Now there are a variety of imaging detectors that are available commercially, including CZT and HPGe detectors that achieve energy resolution ≤1% FWHM at 662 keV. These devices couple the traditional high resolution spectroscopic analysis with next generation gamma-ray imaging information to more accurately characterize the radiation source term. Uncertainties in the source location will result in significant error in the characterization of an object's radioactivity. It is helpful if the object can be spun, such as a barrel, so that any asymmetry in the source distribution is averaged out from the detector's point of view. Even in the case of a spinning barrel it is important to determine if the radiation is concentrated near the center of the barrel or distributed near the edge. The closer one measures to a barrel, which usually dictates the time required to acquire data, the more these spatial variations in the source distribution will affect the calculated activity of each isotope. This paper will focus on showing the use of CZT imaging spectrometers to characterize complicated radiation source terms. The radiation images are used to determine where the source term should be defined in a radiation transport model that calculates the expected number of photopeak counts for each isotope detected. This is used to calculate the activity of the source. The transport model is used to determine the attenuation of the radiation source term through distance and shielding material, but the detection efficiency is based solely on radiation measurement data. These measurements are taken with a robotic source positioning device that allows for detailed directional efficiency calibration. It is a fully automated system where a detector is loaded into the device and all of the efficiency curves are captured as a function of direction by creating new measurements for each location the robot positions the source. These measurements are tagged with the true source location and the efficiency curve is calculated for each measurement. This is used to create a response function matrix as a function of energy and incident direction which is used to convert the direction dependent flux on the detector head determined from the simulation model to the expected number of counts per unit activity of each isotope of interest. The results of these source term reconstructions in both the spatial and spectral domain will be shown. The impact of improper specification of the source term will be shown for a few standard waste characterization scenarios to demonstrate the importance of proper source location determination. Finally, the underlying calibration method and some sample efficiency curves as a function of direction will be shown to demonstrate the importance of calibrating out directional response functions in imaging devices (which often have a strong forward sensitivity bias). (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

An assessment of total depletion uncertainties for a GBC-32 dry storage cask with PLUS7 fuels using Monte Carlo sampling and two-way ANOVA F-test

It is important to accurately evaluate depletion uncertainties that exist due to the limitations of a computer code on accuracy in a nuclear depletion calculation for criticality safety analysis. In this work, the bias and bias uncertainty in the effective neutron multiplication factor (k{sub eff}) for the generic 32 PWR-assembly burnup credit (GBC-32) cask system were assessed using the Monte Carlo uncertainty sampling method for three different burnups and the isotopic biases and uncertainties obtained with the calculated and measured isotopic concentrations. The PLUS7 used nuclear fuel assemblies discharged from the Hanbit Nuclear Power Plant Unit 3 were assumed to be loaded into the GBC-32 cask. In addition, the statistical F-test in the two-way analysis of variance (ANOVA) was suggested to efficiently estimate the statistically converged total depletion uncertainty in k{sub eff}, with a significant reduction of computing efforts in the Monte Carlo criticality calculations, and it was applied to the GBC-32 cask system after a sensitivity analysis was performed to select the important nuclides having significant contributions to the total depletion uncertainty. With the statistical F-tests in the two-way ANOVA, 100 criticality calculations were needed to get a statistically converged total depletion uncertainty for 10 and 30 GWD/MTU, while 120 criticality calculations were needed for 50 GWD/MTU. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

Hints for Small Disks around Very Low Mass Stars and Brown Dwarfs

The properties of disks around brown dwarfs and very low mass stars (hereafter VLMOs) provide important boundary conditions on the process of planet formation and inform us about the numbers and masses of planets than can form in this regime. We use the Herschel Space Observatory PACS spectrometer to measure the continuum and [O i] 63 μ m line emission toward 11 VLMOs with known disks in the Taurus and Chamaeleon I star-forming regions. We fit radiative transfer models to the spectral energy distributions of these sources. Additionally, we carry out a grid of radiative transfer models run in a regime that connects the luminosity of our sources with brighter T Tauri stars. We find that VLMO disks with sizes 1.3–78 au, smaller than typical T Tauri disks, fit well the spectral energy distributions assuming that disk geometry and dust properties are stellar mass independent. Reducing the disk size increases the disk temperature, and we show that VLMOs do not follow previously derived disk temperature–stellar luminosity relationships if the disk outer radius scales with stellar mass. Only 2 out of 11 sources are detected in [O i] despite a better sensitivity than was achieved for T Tauri stars, suggesting that VLMO disks are underluminous. Using thermochemical models, we show that smaller disks can lead to the unexpected [O i] 63 μ m nondetections in our sample. The disk outer radius is an important factor in determining the gas and dust observables. Hence, spatially resolved observations with ALMA—to establish if and how disk radii scale with stellar mass—should be pursued further.

79 ASTRONOMY AND ASTROPHYSICS↗

NASA NTRS1990

Carbon in comet dust

The association of Halley particle results with data from existing meteoritic materials that can be analyzed in the laboratory is discussed. Comet samples must exist in present collections of meteoritic materials and the Halley results provide clues for identifying them. Although it is not presently possible to positively identify cometary meteorites or cometary interplanetary dust (IDP) samples, it is possible to determine which materials are similar to Halley dust and which ones are distinctly unlike Halley. The properties of these existing Halley-compatible samples provide insight into the possible properties of cometary material. Positive identification of meteoritic comet samples or direct samples returned from a comet nucleus would of course revolutionize our ability to study carbonaceous matter in comets. Modern analytical techniques are very powerful and it is possible to perform elemental, chemical, mineralogical and even limited isotopic analysis on micron-size particles. There is an important synergism between the laboratory studies of collected samples and astronomical data from comets and interstellar grains. To fully interpret results there must be convincing methods for associating a particular class or classes of meteoritic material with comets. Ultimately this will be done by direct comet sample return such as the Rosetta mission under development by ESA. At the present time the only links that can be made involve comparison with sample properties and measurable properties of comets. Unfortunately there is at present no known unique property of cometary dust that allows its absolute identification in the laboratory. The results from Halley encounters and observation do provide much new information on cometary grains. The Halley grain compositions, density, size distribution and scattering properties all provide a basis for future investigations. Other Halley properties such as the presence of polyoxymethylene and the 3.4um emission feature could play key roles for making convincing links in the future.

Brownlee, D. E.↗

NASA NTRS2011

Space Weathering of Ordinary Chondrite Parent Bodies, Its Impact on the Method of Distinguishing H, L, and LL Types and Implications for Itokawa Samples Returned by the Hayabusa Mission

As the most abundance meteorites in our collections, ordinary chondrites potentially have very important implications on the origin and formation of our Solar System. In order to map the distribution of ordinary chondrite-like asteroids through remote sensing, the space weathering effects of ordinary chondrite parent bodies must be addressed through experiments and modeling. Of particular importance is the impact on distinguishing different types (H/L/LL) of ordinary chondrites. In addition, samples of asteroid Itokawa returned by the Hayabusa spacecraft may re~ veal the mechanism of space weathering on an LLchondrite parent body. Results of space weathering simulations on ordinary chondrites and implications for Itokawa samples are presented here.

Hiroi, T.↗

DOE OSTI2019

Biomonitoring Organochlorine Pesticides in Didelphis virginiana from Yucatan, Mexico by GC-ECD

The aim of the present work was to apply a validated methodology for the detection of organochlorine pesticides in Didelphis virginiana (Virginia opossum) serum samples collected in Yucatan, Mexico. Recent studies performed to investigate the presence of Organochlorines (OCLs) in water, human blood and milk, and animal tissues from Yucatan have shown that the OCLs concentrations are high and can be associated with potential human health risk. Since opossum is considered an important synanthropic species in Yucatan, 40 opossum serum samples were analyzed by gas chromatography with electron capture detector. The most common OCLs found in opossum sera were lindanes, chlordanes, drines, and endosulfan. Heptachlor, heptachlor epoxide, and lindanes were found at the highest concentrations, while dichlorodiphenyl trichloroethane and its metabolites were found at the lowest concentrations in the samples. The good linearity, precision, and accuracy obtained in the evaluated parameters in the extraction and chromatographic methods support its application for the monitoring of OCLs pesticides in populations of opossums and other wild species in Yucatan.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

Separation of Lanthanide Isotopes from Mixed Fission Product Samples

The measurement of radioactive fission products from nuclear events has important implications for nuclear data production, environmental monitoring, and nuclear forensics. In a previous paper, the authors reported the optimization of an intra-group lanthanide separation using LN extraction resin from Eichrom Technologies®, Inc. and a nitric acid gradient. In this work, the method was demonstrated for the separation and quantification of multiple short-lived fission product lanthanide isotopes from a fission product sample produced from the thermal irradiation of highly enriched uranium. The separations were performed in parallel in quadruplicate with reproducible results and high decontamination factors for 153 Sm, 156 Eu, and 161 Tb. Based on the results obtained here, the fission yields for 144 Ce, 153 Sm, 156 Eu, and 161 Tb are consistent with published fission yields. This work demonstrates the effectiveness of the separations for the intended application of short-lived lanthanide fission product analysis requiring high decontamination factors.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRSDate not supplied

Initial analysis of “stone” size Ryugu samples: current status

As a part of the initial analysis of the Ryugu samples, we perform a variety of analyses of millimeter-sized "stones". Our goals are to elucidate the entire formation process of C-type asteroid Ryugu from the viewpoint of petrology and mineralogy ande obtain necessary information by sample analysis, and then simulate the formation of Ryugu based on the evidencef obtained rom sample analysis. Eighteen stones (8 from Room A and 10 from Room C) were received from the ISAS curation facility on June 1, 2021, and brought into a fully nitrogen-displaced glove box at Tohoku University. At the same time, we also received the powder samples from Room A and Room C. To completely block the atmosphere from leaking into the container, all samples were put in the sample transport containers prepared by ISAS, transferred from the main chamber to the glovebox at ISAS, and then all containers were completely sealed in plastic bags with moisture and oxygen absorbers. No moisture or oxygen was detected when the bags were opened in the glove box at Tohoku University, so it was confirmed that there was no exposure to the atmosphere during transport. To date, a number of analyses have been carried out successfully and almost on schedule. The analysis started with the measurement of reflectance spectra, which are sensitive to atmospheric oxidation, hydroxylation, and adsorbed water. The visible, near-infrared, and mid-infrared reflectance spectra were measured while the samples were kept airtight. The spectra of powder samples and stone samples (as aggregates and as single stone) were successfully obtained. A major feature of the stone team's analysis is the use of synchrotron radiation facilities around the world. Since this analysis is non-destructive, stone samples whose reflectance spectra were measured were sent to KEK, SPring-8, ESRF (France), SOLEIL (France), DESY (Germany), and APS (USA). Using these synchrotron radiation facilities, high spatial resolution and sensitivity XRD, STXM, XANES, CT [1], IR-CT, FT-IR [2, 3], XRF, and Mössbauer analyses were performed. Most of the analyses were carried out under air-tight conditions on the stone samples and the particulates separated from the stone samples. These analyses allowed us to determine the three-dimensional distribution of minerals and elements, redox state, density and porosity of the stone samples. Furthermore, as a characteristic analysis of the stone team, light elemental analysis using negative Muon was performed at the MLF facility of J-PARC with an exceptionally long allocation of machine time. This is the only non-destructive method to measure the concentration of light elements in the whole (not the surface) of stone samples. Because the characteristic X-rays produced by muon irradiation are much higher in energy than the fluorescent X-rays produced by X-ray irradiation, there is little effect of self-absorption by the sample, and therefore, the concentration of light elements such as carbon, oxygen, and Na in the entire "stone" sample can be determined. Some stone samples are currently being measured for heat and strength physical properties in order to understand the physical properties of asteroid Ryugu. The data obtained from these measurements are useful for interpreting the remote-sensing data data taken from the surface layer of the asteroid Ryugu [4-7]. It is also important for understanding the behavior of the Ryugu material during impact events. The surfaces of many stone samples were observed by electron microscopy and other techniques, especially on natural “flat” surfaces formed on 5 stomes. As a result, characteristric mineral aggregates formed by the reactions with water and characteiristic impact features were observed on some of the samples. Based on the observations of surfaces and the synchrotron measurements of the whole stones, important objects such as characteristic structures and specific crystal aggregates for understanding the formation history of the asteroid were identified, and these parts were separated from the stone samples using an Xe beam (pFIB) and analyzed by various methods including transmission electron microscopy and synchrotron radiation analysis. Many stone samples, from which important objects have been separated, are embedded in epoxy resin and cut to produce many polished sections. Electron microscopy and spectroscopic measurements of the polished surfaces are being carried out to reveal the detailed mineralogical properties and elemental distribution inside the stone samples. In the fall, machine time for synchrotron radiation will begin, and we plan to analyze single crystals and characteristic objects separated from the stone samples.

Tomoki Nakamura↗

NASA NTRS2006

Pyroxenes in Martian meteorites as petrogenetic indicators

Pyroxenes in Martian meteorites are important recorders of petrogenetic processes. Understanding the details of pyroxene major and minor element compositional variations can provide important insights into those processes. A combination of careful petrographic analysis of natural samples and experimental crystallization studies can lead to better understanding of the processes that gave rise to these samples on Mars. In addition, experimentally determined major, minor and trace element partition coefficients are important for using natural pyroxenes to estimate the compositions of the melts from which they crystallized and the oxidation conditions that prevailed during crystallization. We will report on minor element (Al, Ti, Cr) zoning in nakhlite pyroxenes and in synthetic pyroxenes that we have grown for the purposes of determining pyroxene/melt partition coefficients for Sr and REE. The natural pyroxenes have patchy Al zoning that, by analogy with our experimental pyroxenes, we interpret as sector zoning. The irregular patchy nature of the zoning is probably the result of the vagaries of growth kinetics and local environment during crystal growth. More slowly cooled nakhlites have the most distinct bimodal zoning, with one mode having Al2O3 around 0.5-0.6 wt%, and the other around 0.9 %. Average Al content increases with increasing cooling rate. This feature is puzzling, since the cumulus pyroxenes were almost certainly present at the time of eruption. Al and Ti are strongly correlated, but Cr is completely decoupled from those elements. The synthetic pyroxenes are distinctly sector zoned in Al and Ti, and the sector-to-sector variation in Al within a single crystal has important effects on trace element partition coefficients. Trivalent REE are strongly correlated with Al, while divalent elements (Sr, Eu+2) show a significantly weaker correlation. For example, as the Al2O3 content varies from 0.3 to 0.6 wt % from one sector to another, D(Gd) increases by approx.80% while D(Sr) and D(Eu) only increase by 20-30% at oxygen fugacities near IW. The different Al dependency of D for trivalent REE vs. divalent Eu and Sr considerably complicates the calibration of the Eu oxybarometer.

McKay, Gordon↗

DOE OSTI2016

MPLEx: a Robust and Universal Protocol for Single-Sample Integrative Proteomic, Metabolomic, and Lipidomic Analyses

In systems biology studies, the integration of multiple omics measurements (i.e., genomics, transcriptomics, proteomics, metabolomics, and lipidomics) has been shown to provide a more complete and informative view of biological pathways. Thus, the prospect of extracting different types of molecules (e.g., DNAs, RNAs, proteins, and metabolites) and performing multiple omics measurements on single samples is very attractive, but such studies are challenging due to the fact that the extraction conditions differ according to the molecule type. Here, we adapted an organic solvent-based extraction method that demonstrated broad applicability and robustness, which enabled comprehensive proteomics, metabolomics, and lipidomics analyses from the same sample.

Nakayasu, Ernesto S.↗

NASA NTRS2002

PCS: The First Fluid Physics Payload on ISS

The Physics of Colloids in Space (PCS) experiment was accommodated within International Space Station (ISS) EXpedite the PRocessing of Experiments to Space Station (EXPRESS) Rack 2 and was remotely operated from early June 2001 until February 2002 from NASA Glenn Research Center's Telescience Support Center in Cleveland, Ohio and from a remote site at Harvard University in Cambridge, Massachusetts. PCS is an experiment conceived by Professor David A. Weitz of Harvard University (the Principal Investigator), focusing on the behavior of three different classes of colloid mixtures. The sophisticated light scattering instrumentation comprising PCS is capable of color imaging, and dynamic and static light scattering from 11 to 169 degrees, Bragg scattering over the range from 10 to 60 degrees, and laser light scattering at low angles from 0.3 to 6.0 degrees. The PCS instrumentation performed remarkably well, demonstrating a flexibility that enabled experiments to be performed that had not been envisioned prior to launch. While on-orbit, PCS accomplished 2400 hours of science operations, and was declared a resounding success. Each of the eight sample cells worked well and produced interesting and important results. Crystal nucleation and growth and the resulting structures of two binary colloidal crystal alloys were studied, with the long duration microgravity environment of the ISS facilitating extended studies on the growth and coarsening characteristics of the crystals. In another experiment run, the de-mixing of the colloid-polymer critical-point sample was studied as it phase-separates into two phases, one that resembles a gas and one that resembles a liquid. This process was studied over four decades of length scale, from 1 micron to 1 centimeter, behavior that cannot be observed in this sample on Earth because sedimentation would cause the colloids to fall to the bottom of the cell faster than the de-mixing process could occur. Similarly, the study of gelation and aging of another colloid-polymer sample, the colloid-polymer gel, also provided valuable information on gelation mechanisms, as did investigations on the extremely the low concentration silica and polystyrene fractal gel samples.

Doherty, M.↗

DOE OSTI2017

Cryo-STEM Tomography with Inpainting

Traditionally, microscopists have worked with the Nyquist-Shannon theory of sampling, which states that to be able to reconstruct the image fully it needs to be sampled at a rate of at least twice the highest spatial frequency in the image. This sampling rate assumes that the image is sampled at regular intervals and that every pixel contains information that is crucial for the image (it even assumes that noise is important). Images in general, and especially low dose S/TEM images, contain significantly less information than can be encoded by a grid of pixels (which is why image compression works). Mathematically speaking, the image data has a low dimensional or sparse representation. Through the application of compressive sensing methods [1,2,3] this representation can be found using pre-designed measurements that are usually random for implementation simplicity. These measurements and the compressive sensing reconstruction algorithms have the added benefit of reducing noise. This reconstruction approach can be extended into higher dimensions, whereby the random sampling in each 2-D image can be extended into: a sequence of tomographic projections (i.e. tilt images); a sequence of video frames (i.e. incorporating temporal resolution and dynamics); spectral resolution (i.e. energy filtering an image to see the distribution of elements); and ptychography (i.e. sampling a full diffraction image at each location in a 2-D grid across the sample). This approach has been employed experimentally for materials science samples requiring low-dose imaging [2], and can be readily applied to biological samples. Figure 1 shows the resolution possible in a complex biological system, mouse pancreatic islet beta cells [4], when tomogram slices are reconstructed using subsampling. Reducing the number of pixels (1/6 pix and 1/3*1/3) shows minimal degradation compared to the reconstructions using all pixels (all data and 1/3 tilt). Although subsampling 1/6 of the tilts (1/6 of overall dose) degrades the reconstruction to the point that the cellular structures cannot be identified. Using 1/3 of both the pixels and the tilts provides a high quality image at 1/9 the overall dose even for this most basic and rapid demonstration of the CS methods. Figure 2 demonstrates the theoretical tomogram reconstruction quality (vertical axis) as undersampling (horizontal axis) is increased; we examined subsampling pixels and tilt-angles individually and a combined approach in which both pixels and tilts are sub-sampled. Note that subsampling pixels maintains high quality reconstructions (solid lines). Using the inpainting algorithm to obtain tomograms can automatically reduce the dose applied to the system by an order of magnitude. Perhaps the best way to understand the impact is to consider that by using inpainting (and with minimal hardware changes), a sample that can normally withstand a dose of ~10 e/Å2 can potentially be imaged with an “equivalent quality” to a dose level of 103 e/Å2. To put this in perspective, this is approaching the dose level used for the most advanced images, in terms of spatial resolution, for inorganic systems. While there are issues for biological specimens beyond dose (structural complexity being the most important one), this sampling approach allows the methods that are traditionally used for materials science to be applied to biological systems [5]. References: [1] A Stevens, H Yang, L Carin et al. Microscopy 63(1), (2014), pp. 41. [2] L Kovarik, A Stevens, A Liyu et al. Appl. Phys. Lett. 109, 164102 (2016) [3] A Stevens, L Kovarik, P Abellan et al. Adv. Structural and Chemical Imaging 1(10), (2015), pp. 1. [4] MD Guay, W Czaja, MA Aronova et al. Scientific Reports 6, 27614 (2016) [5] Supported by the Chemical Imaging, Signature Discovery, and Analytics in Motion Initiatives at PNNL. PNNL is operated by Battelle Memorial Inst. for the US DOE; contract DE-AC05-76RL01830.

Stevens, Andrew↗

DOE OSTI2019

Scaling-Up of Nano-Architected Microstructures: A Mechanical Assessment

Nano– and micro–architected materials generated by ultra–high–resolution 3D printing techniques, such as two–photon polymerization direct laser writing (TPP–DLW) or projection micro–stereolithography (PμSL), have garnered great interest due to their ability to achieve exceptional combinations of material properties. The scalability of these materials, however, remains a crucial challenge as larger high–resolution samples require stitching smaller blocks of the structure of interest together. Herein, scaling techniques and testing methodologies to investigate the effect of stitching on the integrity and mechanical behavior of TPP–DLW parts under tensile load are explored. Specifically, stitched log–pile I–beam specimens with relative densities of 21.5% and 54.7% are tested herein. The micro–tensile tests reveal that the higher–density log–pile samples exhibit brittle behavior with fracture loads at least four times higher than those of lower–density samples. The location of sample failure depends on the type of stitch introduced in the sample, as well as on the relative sample density. Altogether, this study highlights the importance of stitching techniques and relative density for the design of nano– and micro–architected materials.

36 MATERIALS SCIENCE↗

DOE OSTI2019

High Performance Anion Exchange Membrane Fuel Cells Enabled by Fluoropoly(olefin) Membranes

Abstract Although the peak power density of anion exchange membrane fuel cells (AEMFCs) has been raised from ≈0.1 to ≈1.4 W cm −2 over the last decade, a majority of AEMFCs reported in the literature have not been demonstrated to achieve consistently high performance and steady‐state operation. Poly(olefin)‐based AEMs with fluorine substitution on the aromatic comonomer show considerably higher dimensional stability compared to samples that do not contain fluorine. More importantly, fluorinated poly(olefin)‐based AEMs exhibit high hydroxide conductivity without excessive hydration due to a new proposed mechanism where the fluorinated dipolar monomer facilitates increased hydroxide dissociation and transport. Using this new generation of AEMs, a stable, high‐performance AEMFC is operated for 120 h. When the fuel cell configuration is subjected to a constant current density of 600 mA cm −2 under H 2 /O 2 flow, the cell voltage declines only 11% (from 0.75 to 0.67 V) for the first 20 h during break‐in and the cell voltage loss is low (0.2 mV h −1 ) over the subsequent 100 h of cell testing. The ease of synthesis, potential for low‐cost commercialization, and remarkable ex situ properties and in situ performance of fluoropoly(olefin)‐based AEM renders this material a benchmark membrane for practical AEMFC applications.

Zhu, Liang↗

DOE OSTI2022

Enhancement of the Magnetoresistance in the Mobility‐Engineered Compensated Metal Pt 5 P 2

Abstract The magnetoresistance (MR) in nonmagnetic materials continues to be a fertile research area in materials science. The search for giant, positive MR has been limited to a rather small window of materials such as high‐mobility semimetals in single‐crystalline form. Here, the observation of a very large positive MR in metallic Pt 5 P 2 in polycrystalline form is reported. The observations reveal that improvement of the crystallinity results in a significant enhancement of the positive MR, exceeding 10 000% at 9 T, comparable to high‐mobility semimetals. Based on first‐principles calculations combined with magnetotransport and thermoelectric measurements, the Fermi surface of Pt 5 P 2 is found to consist of a collection of multiple electron and hole pockets compensating one another, along with a characteristic pocket continuously connected to the adjacent Brillouin zone, together with possible topologically protected band crossings. This work extends the landscape of high MR candidate materials to polycrystalline metals, which demonstrates the importance of crystallinity and purity of the samples for the optimization of the MR.

36 MATERIALS SCIENCE↗