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DOE OSTI2022

Digestion processes and elemental analysis of oxide and sulfide solid electrolytes

Detailed elemental analysis is essential for a successful development and optimization of material systems and synthesis methods. This is especially relevant for Li- and Na-containing compounds, found in state-of-the-art and next-generation battery systems. Their materials’ properties and thus the final device performance strongly depend on the crystal structure, the stoichiometry, and defect chemistry, e.g., influencing charge carrier concentration and activation energies for vacancy transport. However, a detailed quantitative analysis of light elements in a heavy matrix, featuring a broad range of solubilities and vapor pressures, is often difficult and associated with large uncertainties and thus neglected in favor of just reporting the stoichiometry as “weighed in.” Here, in this work, we report several approaches to digest and dissolve various oxide and sulfide-based materials, used in next-generation Li batteries, for elemental analysis via optical emission spectroscopy. These include the most common solid electrolytes Li-La-Ti–O, a perovskite material (LLTO), and Li-La-Zr-O which has garnet structure (LLZO). Additionally, a facile thermal digestion process is reported for a surrogate sulfide solid electrolyte (Na 2 S). The digestion procedures reported here are suitable for almost any laboratory environment and, when applied, will improve understanding of the synthesis-structure–property correlations needed to advanced batteries with all solid-state configurations.

Malkowski, Thomas F.↗

DOE OSTI2017

Solvent Extraction of Rare Earth Elements from a Nitric Acid Leach Solution of Apatite by Mixtures of Tributyl Phosphate and Di-(2-ethylhexyl) Phosphoric Acid

Solvent extraction of rare earths from nitrate leach liquor of apatite using mixtures of tributyl phosphate (TBP) and di-(2-ethylhexyl) phosphoric acid (D2EHPA) was studied. The effects of nitrate and hydrogen ion concentration of the aqueous phase as well as the composition and concentration of extractants in the organic phase on the extraction behavior of lanthanum, cerium, neodymium, and yttrium were investigated. The distribution ratio of REEs increases by increasing the nitrate concentration in aqueous phase and concentration of extractants in organic phase, but the hydrogen ion concentration in aqueous phase has a decreasing effect. Yttrium as a heavy rare earth is more sensitive to these parameters than light rare earth elements. Although the composition of organic phase has a minor effect on the extraction of light rare earths, the percent of extraction of yttrium decreases dramatically by increasing the TBP content of organic phase. Mixtures of TBP and D2EHPA can show either synergism or antagonism extraction depending on the concentration and composition of extractants in organic phase. The best condition for separating rare earth elements in groups of heavy and light REEs can be achieved at high nitrate concentration, low H{sup +} concentration, and high concentration of D2EHPA in organic phase. Separation of Ce and La by TBP and D2EHPA is practically impossible in the studied conditions; however, low nitrate concentration and high hydrogen ion concentration in aqueous phase and low concentration of extractants in organic phase favor the separation of Nd from other light rare earth elements.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Kinetic Study on Alloying Element Transfer During an Electroslag Remelting Process

Experimental and theoretical studies have been carried out to investigate the effects of slag on the alloying elements in ingots during the electroslag remelting (ESR) process with a focus on developing a mass-transfer model to understand the mechanism of slag-metal reaction. Stainless steel 1Cr21Ni5Ti was used as the electrode and remelted with two different kinds of slags using a 50-kg ESR furnace. The contents of sulfur, aluminum, titanium and silicon along the axial direction of the produced ingots were analyzed. On the basis of the penetration and film theories, the theoretical model developed in this work elucidates the kinetics of the slag-metal reaction revealing the mechanism of alloying element transfer during the ESR process. The calculation results obtained from the model agree well with the experimental results. The model indicates that the resultant [O] coming from the desulfurization reaction of (O{sup 2−}) + [S] = (S{sup 2−}) + [O] causes the oxidation of alloying elements in steel by [M] + [O] = (MO). The distribution ratio of sulfur L{sub S} decreases with the increase of slag temperature in the first slag-temperature-rising period, and the concentration of sulfur in the ingot at the beginning of the ESR process is lower than in the rest of the process because of the combination of the large distribution ratio of sulfur L{sub S} and excellent kinetic conditions. The concentration of aluminum along the height of the ingot has an increasing trend in the first slag-temperature-rising period, while it has a decreasing trend in the rest of the process. Two methods can solve this problem: one is starting up the ESR furnace by high temperature molten slag technology and the other is continually adding extra titania into the molten slag in the first slag-temperature-rising period.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Design, Processing, and Properties of WTaCrV-Hf Multi-principal Element Alloys

Refractory multi-principal element alloys are candidates for high-temperature structural components due, in part, to their high strength and high melting points. Single-phase materials are initially preferred for isotropic material properties as a function of time and temperature in service conditions. This work outlines a computational rank-ordering and experimental validation methodology for single-phase body-centered-cubic phase stability in WTaCrV-Hf alloys using order–disorder transition temperature. Eight compositions were fabricated by arc-melting and heat-treated at 1400 °C for 24 hrs. X-ray diffraction, energy-dispersive x-ray spectroscopy, and Vickers hardness testing showed alloys with order–disorder transition temperatures below 600 °C formed a single-phase body-centered-cubic structure during solidification and remained single-phase after heat-treatment. The sample possessing the lowest order–disorder transition temperature exhibited slip traces suggestive of room-temperature plastic deformation under Vickers indentation, with both heat-treated single-phase samples exhibiting hardnesses over 800 HV with little cracking compared to tungsten. These results establish order–disorder transition temperature as a viable predictive parameter for multi-principal element alloy phase stability. The methodology outlined in this work provides a framework for future design, fabrication, and characterization of high-temperature structural multi-principal element alloys.

CALPHAD↗

DOE OSTI2026

MoNbTi-based Refractory Multi-principal Element Alloy System: A Review of the Thermodynamic Phase Predictions, Formed Microstructures, and Mechanical Properties as a Function of the Fabrication Methods (AM versus SPS versus VAM)

Abstract Multi-principal element alloys, particularly of refractory compositions, are an increasingly popular candidate for extreme-environment applications, including for next-generation nuclear reactors and in other industries, such as biomedical and aerospace, due to their high strength. The ability to achieve solid-solution microstructures provides these alloys with improved mechanical properties; however, these microstructures are heavily composition- and processing-dependent. In this review, the multi-principal element alloy MoNbTi-based system (with Zr, V, and Cr additions) was selected to compare the effects of elemental composition and processing route on the resulting microstructures and mechanical properties. The review provides insight into identifying the optimal alloy composition and processing route for a balance of desired microstructure and mechanical properties.

Krogh, Kara↗

DOE OSTI2017

Clusters of Monoisotopic Elements for Calibration in (TOF) Mass Spectrometry

Precise calibration in TOF MS requires suitable and reliable standards, which are not always available for high masses. We evaluated inorganic clusters of the monoisotopic elements gold and phosphorus (Au{sub n}{sup +}/Au{sub n}{sup -} and P{sub n}{sup +}/P{sub n}{sup -}) as an alternative to peptides or proteins for the external and internal calibration of mass spectra in various experimental and instrumental scenarios. Monoisotopic gold or phosphorus clusters can be easily generated in situ from suitable precursors by laser desorption/ionization (LDI) or matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Their use offers numerous advantages, including simplicity of preparation, biological inertness, and exact mass determination even at lower mass resolution. We used citrate-stabilized gold nanoparticles to generate gold calibration clusters, and red phosphorus powder to generate phosphorus clusters. Both elements can be added to samples to perform internal calibration up to mass-to-charge (m/z) 10–15,000 without significantly interfering with the analyte. We demonstrated the use of the gold and phosphorous clusters in the MS analysis of complex biological samples, including microbial standards and total extracts of mouse embryonic fibroblasts. We believe that clusters of monoisotopic elements could be used as generally applicable calibrants for complex biological samples. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2018

A thermal-mechanical finite element workflow for directed energy deposition additive manufacturing process modeling

This work proposes a finite element (FE) analysis workflow to simulate directed energy deposition (DED) additive manufacturing at a macroscopic length scale (i.e. part length scale) and to predict thermal conditions during manufacturing, as well as distortions, strength and residual stresses at the completion of manufacturing. The proposed analysis method incorporates a multi-step FE workflow to elucidate the thermal and mechanical responses in laser engineered net shaping (LENS) manufacturing. For each time step, a thermal element activation scheme captures the material deposition process. Then, activated elements and their associated geometry are analyzed first thermally for heat flow due to radiation, convection, and conduction, and then mechanically for the resulting stresses, displacements, and material property evolution. Finally, simulations agree with experimentally measured in situ thermal measurements for simple cylindrical build geometries, as well as general trends of local hardness distribution and plastic strain accumulation (represented by relative distribution of geometrically necessary dislocations).

42 ENGINEERING↗

DOE OSTI2014

X-ray relative intensities at incident photon energies across the L{sub i} (i=1–3) absorption edges of elements with 35≤Z≤92

The intensity ratios, I{sub Lk}/I{sub Lα1} (k=l,η,α{sub 2},β{sub 1},β{sub 2,15},β{sub 3},β{sub 4},β{sub 5,7},β{sub 6},β{sub 9,10},γ{sub 1,5},γ{sub 6,8},γ{sub 2,3},γ{sub 4}) and I{sub Lj}/I{sub Lα} (j=β,γ), have been evaluated at incident photon energies across the L{sub i} (i=1–3) absorption edge energies of all the elements with 35≤Z≤92. Use is made of what are currently considered to be more reliable theoretical data sets of different physical parameters, namely, the L{sub i} (i=1–3) sub-shell photoionization cross sections based on the relativistic Hartree–Fock–Slater (RHFS) model, the X-ray emission rates based on the Dirac–Fock model, and the fluorescence and Coster–Kronig yields based on the Dirac–Hartree–Slater model. In addition, the Lα{sub 1} X-ray production cross sections for different elements at various incident photon energies have been tabulated so as to facilitate the evaluation of production cross sections for different resolved L X-ray components from the tabulated intensity ratios. Further, to assist evaluation of the prominent (L{sub i}−S{sub j}) (S{sub j}=M{sub j}, N{sub j} and i=1–3, j=1–7) resonant Raman scattered (RRS) peak energies for an element at a given incident photon energy (below the L{sub i} sub-shell absorption edge), the neutral-atom electron binding energies based on the relaxed orbital RHFS calculations are also listed so as to enable identification of the RRS peaks, which can overlap with the fluorescent X-ray lines. -- Highlights: •The L X-ray relative intensities and Lα{sub 1} XRP cross sections are evaluated using physical parameters based on the IPA models. •Comparison of the intensity ratios evaluated using the DHS and DF models based photoionization cross sections is presented. •Importance of many body effects including electron exchange effects is highlighted.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2022

Extreme hardness at high temperature with a lightweight additively manufactured multi-principal element superalloy

Materials are needed that can tolerate increasingly harsh environments, especially ones that retain high strength at extreme temperatures. Higher melting temperature alloys, like those consisting primarily of refractory elements, can greatly increase the efficiency of turbomachinery used in grid electricity production worldwide. Existing alloys, including Ni- and Co-based superalloys, used in components like turbine blades, bearings, and seals, remain a performance limiting factor due to their propensity, despite extensive optimization efforts, for softening and diffusion-driven elongation at temperatures often well above half their melting point. To address this critical materials challenge, we present results from integrating additive manufacturing and alloy design to guide significant improvements in performance via traditionally difficult-to-manufacture refractory alloys. We present an example of a multi-principal element alloy (MPEA), consisting of five refractory elements and aluminum, that exhibited high hardness and specific strength surpassing other known alloys, including superalloys. The alloy shows negligible softening up to 800°C and consists of four compositionally distinct phases, in distinction to previous work on MPEAs. Density functional theory calculations reveal a thermodynamic explanation for the observed temperature-independent hardness and favorability for the formation of this multiplicity of phases.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Cross-kingdom expression of synthetic genetic elements promotes discovery of metabolites in the human microbiome

Small molecules encoded by biosynthetic pathways mediate cross-species interactions and harbor untapped potential, which has provided valuable compounds for medicine and biotechnology. Since studying biosynthetic gene clusters in their native context is often difficult, alternative efforts rely on heterologous expression, which is limited by host-specific metabolic capacity and regulation. Here, in this work, we describe a computational-experimental technology to redesign genes and their regulatory regions with hybrid elements for cross-species expression in Gram-negative and -positive bacteria and eukaryotes, decoupling biosynthetic capacity from host-range constraints to activate silenced pathways. These synthetic genetic elements enabled the discovery of a class of microbiome-derived nucleotide metabolites—tyrocitabines—from Lactobacillus iners. Tyrocitabines feature a remarkable orthoester-phosphate, inhibit translational activity, and invoke unexpected biosynthetic machinery, including a class of “Amadori synthases” and “abortive” tRNA synthetases. Our approach establishes a general strategy for the redesign, expression, mobilization, and characterization of genetic elements in diverse organisms and communities.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2021

Modelling the development of capillary pressure in freshly 3D-printed concrete elements

3D concrete printing is a promising technology recently developed to automate construction. Since no formwork is used in this technology to support and protect fresh concrete, there are two aspects which considerably accelerate the development of capillary pressure in 3D-printed concrete in comparison to conventionally placed concrete: i) high stiffness of 3D-printed needed to provide sufficient buildability, and ii) very early and fast evaporation of pore water. Accelerated development of capillary pressure may lead to severe plastic shrinkage cracking in 3D-printed elements and, hence, need to be mitigated. This investigation aims at providing a poromechanical model for capillary pressure development in 3D-printed elements. To simulate the development of capillary pressure and plastic shrinkage, environmental factors, material properties, and element geometry need to be considered as a whole. The model inputs – coefficient of permeability, static bulk modulus, air entry pressure and chemical shrinkage rate – were determined experimentally. The model was validated for two fine-grained concretes. Both 3D-printed materials yielded faster capillary pressure increase in comparison to cast concrete, while partial substitution of cement with silica fume further accelerated the capillary pressure development. Furthermore, due to the lower permeability of the mixture containing silica fume, the gradient of capillary pressure between 3D-printed layers increased, as did the gradient of plastic shrinkage.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Trace elements, oxidative status and antioxidant capacity as biomarkers in very low birth weight infants

Reference data on trace elements, oxidative status and antioxidants in very low birth weight infants (VLBW) are limited and need to be updated for use in clinical settings. Serum and urine of 30 VLBW infants (mean weight, 1167 g) at mean age of 23.8 (t0) and 37.8 (t1) days were analyzed. Cadmium (Cd), copper (Cu), iron (Fe), mercury (Hg), manganese (Mn), selenium (Se) and zinc (Zn), nitrate/nitrite (NOx), catalase (CAT), CuZnFeMn-superoxide dismutases (CuZnFeMn-SODs), total antioxidant capacity (SAC: sum of thiols, proteins, bilirubin, uric acid, β-beta-carotene, ascorbic acid, vitamin E) and total oxidative status (SOS: sum of lipo- and hydroperoxides) were determined. A higher urinary excretion of Cu and Zn was observed at t0 than at t1; while an increase in urine Cd was found at t1 respect to t0. A deficiency in serum levels of Cu and Zn was also found. A lower CAT activity, a higher total oxidants level (SOS) and a reduction of total antioxidant barriers (SAC) were observed in some infants. No Fe and Mn deficiency or Hg overload was found; also CuZnFeMn-SODs and NOx levels did not change. The findings showed that losses of trace elements and incomplete mineral body stores were more pronounced in the earlier life stage (at 23.8th day) than later on; moreover, antioxidant defenses were poor and lipo- and hydroperoxides were higher still at 5 weeks of infants’ life. - Highlights: • Trace elements, oxidants, antioxidants in very low birth weight infants are assessed. • Serum deficiency and urinary loss of Cu and Zn are observed soon after birth. • Oxidative stress and poor antioxidant capacity are found in the first weeks of life.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2018

Toxics (Pb, Cd) and trace elements (Zn, Cu, Mn) in women during pregnancy and at delivery, South Benin, 2014–2015

Highlights: • Lack of data on maternal exposure to toxic and trace elements in Africa. • Longitudinal blood measurements of Pb, Cd, Zn, Cu and Mn during pregnancy in Benin. • Evidence of maternal exposure to Pb and Cd. • Identification of potential sources for Pb exposure during pregnancy. During pregnancy, fetal development can be hindered by maternal exposure to toxic elements and abnormal concentrations of trace elements. Few data are available in African countries. Our goal was to assess the body burden of lead (Pb), cadmium (Cd), manganese (Mn), zinc (Zn) and copper (Cu) in pregnant women in Benin. The study was carried out in Sô-Ava district, from November 2015 to April 2016. Sixty women were recruited from the RECIPAL pre-conceptional cohort study. In all women, blood samples were collected during the first trimester of pregnancy. Thirty-two women had additional maternal and cord blood samples collected at delivery. Blood samples were analyzed by inductively coupled plasma mass spectrometry. At delivery, Cd median (IQR) concentration in maternal blood was 0.34 µg/L (0.24–0.46) in this non-smoking population. Pb median (IQR) concentration in maternal blood at delivery was 37.4 µg/L (30.5–52.0), with 31.3% of blood Pb levels above the 50 μg/L threshold. These pregnant women lived in semi-rural lakeside villages. Potential sources of Pb exposure identified during pregnancy were having water supply by drill pump and activities such as smoking fish by the woman and fishing by the household head. At delivery, Zn, Cu, and Mn median (IQR) concentrations in maternal blood were, respectively, 5415 μg/L (4894–5822), 1609 μg/L (1295–1771) and 16.0 μg/L (12.5–20.8). Pb, Cd, Mn and Cu blood concentrations were significantly higher at delivery than during the first trimester of pregnancy. Pb, Cd, Zn and Cu concentrations were significantly lower in cord blood than in maternal blood, contrary to Mn concentration, which was significantly higher in cord blood than in maternal blood at delivery. This exploratory study is the first one performed in Benin, and warns us about exposition of women from Sô-Ava district to Pb and Cd during pregnancy.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

Prototyping phase of the high heat flux scraper element of Wendelstein 7-X

The water-cooled high heat flux scraper element aims to reduce excessive heat loads on the target element ends of the actively cooled divertor of Wendelstein 7-X. Its purpose is to intercept some of the plasma fluxes both upstream and downstream before they reach the divertor surface. The scraper element has 24 identical plasma facing components (PFCs) divided into 6 modules. One module has 4 PFCs hydraulically connected in series by 2 water boxes. A PFC, 247 mm long and 28 mm wide, has 13 monoblocks made of CFC NB31 bonded by hot isostatic pressing onto a CuCrZr cooling tube equipped with a copper twisted tape. 4 full-scale prototypes of PFCs have been successfully tested in the GLADIS facility up to 20 MW/m 2 . The difference observed between measured and calculated surface temperatures is probably due to the inhomogeneity of CFC properties. The design of the water box prototypes has been detailed to allow the junction between the cooling pipe of the PFCs and the water boxes by internal orbital welding. In conclusion, the prototypes are presently under fabrication.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2017

Thermal-hydraulics modeling for prototype testing of the W7-X high heat flux scraper element

The long-pulse operation of the Wendelstein 7-X (W7-X) stellarator experiment is scheduled to begin in 2020. This operational phase will be equipped with water-cooled plasma facing components to allow for longer pulse durations. Certain simulated plasma scenarios have been shown to produce heat fluxes that surpass the technological limits on the edges of the divertor target elements during steady-state operation. In order to reduce the heat load on the target elements, the addition of a “scraper element” (SE) is under investigation. The SE is composed of 24 water-cooled carbon fiber reinforced carbon composite monoblock units. Multiple full-scale prototypes have been tested in the GLADIS high heat flux test facility. Previous computational studies revealed discrepancies between the simulations and experimental measurements. In this work, single-phase thermal-hydraulics modeling was performed in ANSYS CFX to identify potential causes for such discrepancies. Possible explanations investigated were the effects of a non-uniform thermal contact resistance and a potential misalignment of the monoblock fibers. And while the difference between the experimental and computational results was not resolved by a non-uniform thermal contact resistance, the computational results provided insight into the potential performance of a W7-X monoblock unit. Circumferential temperature distributions highlighted the expected boiling regions of such a unit. Finally, simulations revealed that modest angles of fiber misalignment in the monoblocks result in asymmetries at the unit edges and provide temperature differences similar to the experimental results.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2015

Finite element modeling of rock cutting and its fragmentation process

Rock cutting is a challenging problem from a modeling perspective. The challenges come from the complexity of the physics from the tool-rock interaction to the fracture process and propagation of the quasibrittle rocks. This study was aimed at developing a finite element procedure that was capable of providing reasonable estimates of cutting forces and, at the same time, capturing the essential characteristics of the fragmentation process. Published laboratory rock scratch tests were used as modeling targets since these tests encompass all essential characteristics of rock. Both shallow cuts and deep cuts from a rectangular cutter were analyzed first, and followed by modeling of shallow cuts from a disc cutter. It was concluded that rock cutting could be reasonably modeled by using a plasticity model, an element erosion scheme that remove an element when its energy release equals fracture energy, together with a proper selection of modeling parameters.

02 PETROLEUM↗

DOE OSTI2023

Gas nitriding behavior of refractory metals and implications for multi-principal element alloy design

Multi-principal element alloys (MPEAs) comprise a large, flexible compositional space that enables tuning of their chemistry, structure, and properties. Here, to facilitate the development of nitriding-based surface-enhancement strategies that harness a broad compositional space, this study examined the gas nitriding behavior of Hf, Mo, Nb, Ta, Ti, and Zr as a function of time, temperature (750 and 1000 °C), and nitriding potential (i.e. ammonia-to-hydrogen ratio). These metals were selected because they have a strong driving force to form nitrides, and appear in many promising refractory MPEA compositions. The nitriding temperatures were selected based on the phase transformation temperature of Ti and Zr, and the nitriding potentials were chosen such that all elements are expected to form nitrides. Mass gain measurements indicate that all six elements follow parabolic kinetics. The microstructure observations and quantitative microchemical analysis show formation of dense and well-adhered compound layers for Mo, Nb, and Ta. Thick diffusion zones appear in Hf, Ta, Ti, and Zr, and diffusion coefficients were fit to the composition profiles. Partial delamination of the compound layer occurred for Ti and Zr. Peak hardness values above 30 GPa are obtained in the dense compound layers, and the solute hardening of the underlying alloy is correlated with the nitrogen content. The results provide insight into the dynamics of nitride compound formation relative to interstitial dissolution of nitrogen, and are discussed in the context of MPEA composition and processing design.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Multi-element stochastic spectral projection for high quantile estimation

We investigate quantile estimation by multi-element generalized Polynomial Chaos (gPC) metamodel where the exact numerical model is approximated by complementary metamodels in overlapping domains that mimic the model’s exact response. The gPC metamodel is constructed by the non-intrusive stochastic spectral projection approach and function evaluation on the gPC metamodel can be considered as essentially free. Thus, large number of Monte Carlo samples from the metamodel can be used to estimate α-quantile, for moderate values of α. As the gPC metamodel is an expansion about the means of the inputs, its accuracy may worsen away from these mean values where the extreme events may occur. By increasing the approximation accuracy of the metamodel, we may eventually improve accuracy of quantile estimation but it is very expensive. A multi-element approach is therefore proposed by combining a global metamodel in the standard normal space with supplementary local metamodels constructed in bounded domains about the design points corresponding to the extreme events. To improve the accuracy and to minimize the sampling cost, sparse-tensor and anisotropic-tensor quadratures are tested in addition to the full-tensor Gauss quadrature in the construction of local metamodels; different bounds of the gPC expansion are also examined. The global and local metamodels are combined in the multi-element gPC (MEgPC) approach and it is shown that MEgPC can be more accurate than Monte Carlo or importance sampling methods for high quantile estimations for input dimensions roughly below N=8, a limit that is very much case- and α-dependent.

97 MATHEMATICS AND COMPUTING↗