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DOE OSTI2021

The mechanism driving a solid–solid phase transition in a biomacromolecular crystal

A solid-solid phase transition (SSPT) occurs between distinguishable crystalline forms. Because of its importance in application and theory in material science and condensed matter physics, SSPT has been studied most extensively in metallic alloys, inorganic salt or small organic molecular crystals, but much less so in biomacromolecular crystals. In general, the mechanism of SSPT at atomic and molecular levels is not well understood. Here, we describe the ordered molecular rearrangements in biomacromolecular crystals of the adenine riboswitch (riboA) aptamer using real-time serial crystallography and solution atomic force microscopy (AFM). The large, ligand-induced conformational changes drive the initial phase transition from the apo unit cell (AUC) to the trans unit cell 1 (TUC1). During this transition, coaxial stacking of P1 duplexes becomes the dominant packing interface, whereas P2-P2 interactions are almost completely disrupted, resulting in “floating” layers of molecules. The coupling points in TUC1 and their local conformational flexibility allow the molecules to reorganize to achieve the more densely packed and energetically favorable bound unit cell (BUC). Our study thus reveals the interplay between the conformational changes and the crystal phases—the underlying mechanism that drives the phase transition. Using polarized video microscopy (PVM) to monitor the SSPT in small crystals at high ligand concentration, we have identified the time window during which the major conformational changes take place, and simulated the in crystallo kinetics. Together, these results provide the spatiotemporal information necessary for informing time-resolved crystallography (TRX) experiments. Moreover, this study illustrates a practical approach to characterize SSPT in transparent crystals.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Hydrolysis of methylphosphonic anhydride solid to methylphosphonic acid probed by Raman and infrared reflectance spectroscopies

Much is still unknown about the mechanisms and rates of environmental degradation of organophosphorous pesticides and agents. In this study we focus on the degradation of one organophosphorous compound, namely solid methyl phosphonic acid anhydride [CH3P(O)OHOP(O)OHCH3, MPAN] and its rate of conversion to methyl phosphonic acid (MPA) via heterogeneous hydrolysis. Pure MPAN was synthesized and loaded in open sample cups placed inside exposure chambers containing saturated salt solutions to control the relative humidity (RH). The reaction was monitored in the sample cup at various times using both infrared hemispherical reflectance (HRF) spectroscopy and Raman spectroscopy. Calibrated HRF and Raman spectra of both pure reagents as well as gravimetrically prepared mixtures were used to quantify the concentrations of MPAN and MPA throughout the reaction. Results show that both HRF and Raman spectroscopies are convenient non-invasive methods for detection of solid chemicals. The MPAN degradation rate displayed a very strong dependence on relative humidity: At room temperature the reaction showed 50% conversion of the MPAN in 761 ± 54 hours at 33% RH, 33 ± 4 hours at 43% RH, 17 ± 2 hours at 54% RH and just 7 ± 1 hours at 75% RH. Although MPAN hydrolysis is a second-order reaction, the 33 and 43% RH data, at early reaction times, could be fit with a zeroth order reaction, indicating water vapor and MPAN concentrations were not initially rate controlling. The 54 and 75% RH experiments showed significant deliquescence and decay data could only be fit assuming multiple reactions, implying chemical and/or physical processes partially controlled the hydrolysis rate, in contrast to a single process at low relative humidity.

methyl phosphonic acid, methyl phosphonic anhydrid↗

DOE OSTI2021

Unveiling enhanced oxidation resistance and mechanical integrity of multicomponent ultra–high temperature carbides

The development of a new class of multicomponent ultra-high temperature ceramics (MC-UHTCs), often referred to as high-entropy UHTCs, has gained increased interest due to the possibility of improved thermomechanical and oxidation properties. In this study, a systematic approach by gradual addition in the UHTC components ranging from a binary to a dense quaternary (Ta,Nb,Hf,Ti)C is synthesized using spark plasma sintering (SPS). The solid solutioning was the critical factor in homogenizing the composition in the multicomponent system. The segregation of NbC and HfC was seen in binary and ternary UHTC systems, while a single-phase homogeneity was observed in the quaternary UHTC improving its hardness up to 34.8 GPa. The presence of closely spaced slip lines in the MC-UHTCs enhances resistance to indentation damage up to 72% at an applied load of 200 N. The formation of complex mixed oxide phase of Hf6Ta2O17 ensued in the lower to negligible oxidation even up to 3 min of plasma exposure with temperature exceeding 2800°C. In sum, though the entropy remains medium (0.96R) for the selected system, the quaternary UHTC system undoubtedly has significantly better thermomechanical performance when compared to established baseline UHTCs. Furthermore, this raises the debate on the justification for calling a multicomponent system a “high entropy” to be seen in a new light. The developed MC-UHTCs elicits the paradigm of this new class of UHTCs expanding their potential in thermal protection systems for hypersonic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Phase-field modeling of rate-dependent fluid-driven fracture initiation and propagation

The rate-dependent behavior associated with deformation and fracturing of materials, such as natural rocks, poses significant challenges for modeling. In addition to the complications of the viscoelastic response, the speed of fracture propagation reflects micromechanical mechanisms in the fracture process zone(FPZ). In order to represent these complicated behaviors, a thermodynamically consistent, rate-dependent fracture model is required. Based on rigorous thermodynamic principles, we derive a rate-dependent phase-field mechanical model coupled with single-phase fluid flow in both the matrix and the fracture. The model is guaranteed to satisfy energy conservation during fracture propagation. Here, the system of equations is solved using the introduced solution procedure and a novel preconditioner that accounts for the complex fluid-structure interaction. The proposed phase-field model is tested against several benchmark problems on solid-fluid coupling, fluid-driven fracture propagation and rate-dependent viscoelastic deformation. The model serves as a strong basis for investigating rate-dependent fracturing experiments and for making predictions of material behaviors under new conditions.

42 ENGINEERING↗

NASA NTRS2016

Low Temperature Regolith Bricks for In-Situ Structural Material

Current technology for producing in-situ structural materials on future missions to Mars or the moon relies heavily on energy-intensive sintering processes to produce solid bricks from regolith. This process requires heating the material up to temperatures in excess of 1000 C and results in solid regolith pieces with compressive strengths in the range of 14000 to 28000 psi, but are heavily dependent on the porosity of the final material and are brittle. This method is currently preferred over a low temperature cementation process to prevent consumption of precious water and other non-renewable materials. A high strength structural material with low energy requirements is still needed for future colonization of other planets. To fulfill these requirements, a nano-functionalization process has been developed to produce structural bricks from regolith simulant and shows promising mechanical strength results. Functionalization of granular silicate particles into alkoxides using a simple low temperature chemical process produces a high surface area zeolite particles that are held together via inter-particle oxygen bonding. Addition of water in the resulting zeolite particles produces a sol-gel reaction called "inorganic polymerization" which gives a strong solid material after a curing process at 60 C. The aqueous solution by-product of the reaction is currently being investigated for its reusability; an essential component of any ISRU technology. For this study, two batches of regolith bricks are synthesized from JSC-1A; the first batch from fresh solvents and chemicals, the second batch made from the water solution by-product of the first batch. This is done to determine the feasibility of recycling necessary components of the synthesis process, mainly water. Characterization including BET surface area, SEM, and EDS has been done on the regolith bricks as well as the constituent particles,. The specific surface area of 17.53 sq m/g (average) of the granular regolith material was obtained from nitrogen adsorption isotherm measurement. The size, shape and textures of regolith from SEM shows that the particles are 25-50 micrometers in size and mostly irregular in shape (Figure 1a). The elemental composition of regolith was identified from EDS analysis showed the presence of Si, Al, Fe, Na, Mg, Ca, Ti, O and C (see figure 1b). Each set of cylindrical brick samples were prepared by low energy process, and cured for 21 and 28 days, respectively to compare their compressive strength. Figure 1c, and d shows the JSC-1A brick and the compressive strength measurements. The results from the 21 day cured bricks (2 bricks) have been done and yielded an aver-age strength of 3050 psi, considerably higher than Portland cement mortars (Type IV and V). This promising technology provides the benefits of construction material similar to concrete, with a low complexity, low energy synthesis process and the likelihood of complete reusability of precious resources. Compressive strength using this method can be improved by increasing the surface area of the particles, using bi-modal particle size distribution, and adding certain additives to increase inter-particle forces.

ISRU↗

NASA NTRS1999

Dynamics of the Molten Contact Line

The purpose of this program is to develop a basic understanding of how a molten material front spreads over a solid that is below its melting point, arrests, and freezes. Our hope is that the work will contribute toward a scientific knowledge base for certain new applications involving molten droplet deposition, including the "printing" of arbitrary three-dimensional objects by precise deposition of individual molten microdrops that solidify after impact. Little information is available at this time on the capillarity-driven motion and arrest of molten contact line regions. Schiaffino and Sonin investigated the arrest of the contact line of a molten microcrystalline wax spreading over a subcooled solid "target" of the same material. They found that contact line arrest takes place at an apparent liquid contact angle that depends primarily on the Stefan number S=c(T(sub f) -T(sub t)/L based on the temperature difference between the fusion point and the target temperature, and proposed that contact line arrest occurs when the liquid's dynamic contact angle approaches the angle of attack of the solidification front just behind the contact line. They also showed, however, that the conventional continuum equations and boundary conditions have no meaningful solution for this angle. The solidification front angle is determined by the heat flux just behind the contact line, and the heat flux is singular at that point. By comparing experiments with numerical computations, Schiaffino and Sonin estimated that the conventional solidification model must break down within a distance of order 0.1 - 1 microns of the contact line. The physical mechanism for this breakdown is as yet undetermined, and no first-principles theory exists for the contact angle at arrest. Schiaffino and Sonin also presented a framework for understanding how to moderate Weber number molten droplet deposition in terms of similarity laws and experimentation. The study is based on experiments with three molten materials- molten wax on solid wax, water on ice, and mercury on frozen mercury- which between them span a considerable range of the deposition/solidification similarity parameters. Correlations are obtained for the spreading velocity, spreading time scales, the spreading factor (i.e. ratio of deposited drop's final footprint radius and the drop's initial radius), post-spreading liquid oscillation amplitudes and time scales, and bulk solidification time scales. Duthaler carried out an experimental and theoretical investigation of the relationship between the liquid's apparent contact angle and the Capillary number Ca=mu U/sigma based on contact line speed, for molten materials spreading over subcooled solids. This relationship is required for modeling of melt spreading. We have adapted Voinov's methodology to the molten contact line and formulated a theoretical model for the Ca vs. contact angle relationship, based Schiaffino and Sonin#s (1997a,b) wedge-like solidification front model. With the solidification front angle taken from Schiaffino and Sonin, the model is in good agreement with the experimental results for Ca vs. contact angle. Duthaler also extended the experimental investigation of droplet deposition and contact line freezing to more materials, including solder on glass, solder on solder, water on ice, and molten microcrystalline wax on wax. The latter also included tests on inclined targets. Deposition tests have also been done with molten octacosane (C28H58) on various targets. An important objective of our program has been the development of micron-scale sensors for measuring the transient temperature at a point on the substrate surface as a molten contact line moves over it. The expectation is that this temperature history will yield a better understanding of the thermal process in the contact line region. The sensors are of the thermistor type, either 2.5 microns or 1.5 microns square, microfabricated with silicon-based technology on either pure silicon or amorphous silicon dioxide chips. Each chip has 32 sensors distributed on its surface in arrays. The time response is better than 10 ms. At the time of writing, sensor calibration is in progress. Results on thermal transients during contact line passage will be discussed at the conference. While we expect that the data will provide information on the near-contact-line heat transfer process, we also foresee possible problems. First, the spatial resolution of the sensors may be insufficient to resolve the near-contact-line region. Second, the sensors protrude about 0.5 microns above the substrate surface, and may affect the contact line motion. Third, a sensor's temperature history depends on both the heat flux distribution into it from the fusion front and the thermal properties of the substrate below it and the solidified melt between it and the fusion front. The heat flux distribution in the contact line region must therefore be unfolded from computations of the overall system's transient thermal response.

Sonin, Ain A.↗

DOE OSTI2025

Comparison of Nuclear Thermal Propulsion Reactor Cores Using Different Fuel Forms, Neutron Spectra, and Uranium Enrichments

A comparison of 300 MWt HEU and HALEU NTP cores using different fuel forms is presented to demonstrate trends and potentially inform fuel development. Compared to HEU, HALEU cores require additional in-core moderation. Beryllium was chosen as the reference in-core moderator material; metal hydrides may also be considered. Typical NTP fuel forms such as carbide and carbonitride solid solutions, carbide-graphite composites, CERMETs and CERCERs were considered together with less typical fuel forms such as UC and U metal. Be-moderated HALEU cores are heavier than HEU cores (1.9-2.7 and 0.9-2.0 metric tons, respectively). Furthermore, HALEU loading is very sensitive to the amount of in-core moderation which translates into tight fabrication tolerances. HALEU cores requires more reactivity control mechanisms than HEU cores to compensate for temperature feed-back. Using enrichments only slightly above HALEU (e.g., 25%) may provide a compromise between the administrative preference for using HALEU and the engineering preference for simplifying the reactor systems by, for example, not using in-core moderators.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Pore-Scale Modeling of Mineral Growth and Nucleation in Reactive Flow

A fundamental understanding of mineral precipitation kinetics relies largely on microscopic observations of the dynamics of mineral surfaces exposed to supersaturated solutions. Deconvolution of tightly bound transport, surface reaction, and crystal nucleation phenomena still remains one of the main challenges. Particularly, the influence of these processes on texture and morphology of mineral precipitate remains unclear. This study presents a coupling of pore-scale reactive transport modeling with the Arbitrary Lagrangian-Eulerian approach for tracking evolution of explicit solid interface during mineral precipitation. It incorporates a heterogeneous nucleation mechanism according to Classical Nucleation Theory which can be turned “on” or “off.” This approach allows us to demonstrate the role of nucleation on precipitate texture with a focus at micrometer scale. In this work precipitate formation is modeled on a 10 micrometer radius particle in reactive flow. The evolution of explicit interface accounts for the surface curvature which is crucial at this scale in the regime of emerging instabilities. The results illustrate how the surface reaction and reactive fluid flow affect the shape of precipitate on a solid particle. It is shown that nucleation promotes the formation of irregularly shaped precipitate and diminishes the effect of the flow on the asymmetry of precipitation around the particle. The observed differences in precipitate structure are expected to be an important benchmark for reaction-driven precipitation in natural environments.

58 GEOSCIENCES↗

NASA NTRS1999

Reducing and Inducing Convection in Ge-Si Melts with Static Magnetic Field

Results of a study of the effectiveness of using static magnetic fields to reduce convection in Ge-Si melts will be presented. Lenz's law causes a retardation of convection when a static magnetic field is applied to an electrically conducting liquid. However, during the solidification of a solid-solution system such as Ge-Si, the interface is neither isothermal nor isoconcentrational. The variation of temperature and chemical composition along the interface causes thermoelectric currents to be generated within the solidifying material (and the container if it is electrically conductive). These currents, in the presence of a magnetic field, can cause movement (stirring, convection) in the melt which can exceed convection induced by normal thermosolutal mechanisms. Crystals have been grown by both the Bridgman and floating-zone methods. Clear evidence for the existence of this thermoelectromagnetic convection, especially in the case of Si floating-zone growth, will be presented.

Szofran, Frank R.↗

NASA NTRS1998

Interaction between Convection and Heat Transfer in Crystal Growth

Crystals are integral components in some of our most sophisticated and rapidly developing industries. Single crystals are solids with the most uniform structures that can be obtained on an atomic scale. Because of their structural uniformity, crystals can transmit acoustic and electromagnetic waves and charged particles with essentially no scattering or interferences. This transparency, which can be selectively modified by controlled additions of impurities known as dopants, is the foundation of modern electronic industry. It has brought about widespread application of crystals in transistors, lasers, microwave devices, infrared detectors, magnetic memory devices, and many other magnets and electro-optic components. The performance of a crystal depends strongly on its compositional homogeneity. For instance, in modern microcircuitry, compositional variations of a few percent (down to a submicron length scale) can seriously jeopardize predicted yields. Since crystals are grown by carefully controlled phase transformations, the compositional adjustment in the solid is often made during growth from the nutrient. Hence, a detailed understanding of mass transfer in the nutrient is essential. Moreover, since mass transfer is often the slowest process during growth, it is usually the rate limiting mechanism. Crystal growth processes are usually classified according to the nature of the parent phase. Nevertheless, whether the growth occurs by solidification from a melt (melt growth), nucleation from a solution (solution growth), condensation from a vapor (physical vapor transport) or chemical reaction of gases (chemical vapor deposition), the parent phase is a fluid. As is with most non-equilibrium processes involving fluids, liquid or vapor, fluid motion plays an important role, affecting both the concentration and temperature gradients at the soli-liquid interface.

Source record↗

DOE OSTI2023

Synthesis and Structural Study of Substituted Ternary Nitrides for Ammonia Production

Over the past few decades, inorganic nitride materials have grown in importance in part due to their potential as catalysts for the synthesis of NH 3 , a key ingredient in fertilizer and precursor to industrial chemicals. Of particular interest are the ternary (ABN) or higher-order nitrides with high metal-to-nitrogen ratios that show promise in enhancing NH 3 synthesis reaction rates and yields via heterogeneous catalysis or chemical looping. Although metal nitrides are predicted to be numerous, the stability of nitrogen triple bonds found in N 2 , especially in comparison to the metal–nitrogen bonds, has considerably hindered synthetic efforts to produce complex nitride compounds. In this study, we present an exhaustive down-selection process to identify ternary nitrides for a promising chemical looping NH 3 production mechanism. We also report on a facile and efficient two-step synthesis method that can produce well-characterized η-carbide Co 3 Mo 3 N/Fe 3 Mo 3 N or filled β-manganese Ni 2 Mo 3 N ternaries, as well as their associated quaternary, (Co,Fe) 3 Mo 3 N, (Fe,Ni) 2 Mo 3 N, and (Co,Ni) 2 Mo 3 N, solid solutions. To further explore the quaternary space, syntheses of (Co,Ni) 3 Mo 3 N (Ni ≤ 10 mol %) and Co 3 (Mo,W) 3 N (W ≤ 10 mol %) were also investigated. The structures of the nitrides were characterized via X-ray powder diffraction. The morphology and compositions were characterized with scanning electron microscopy. In conclusion, the multitude of chemically unique, but structurally related, nitrides suggests that properties such as nitrogen activity may be tunable, making the materials of great interest for NH 3 synthesis schemes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Confinement-controlled selective CO 2 insertion into a dicopper dihydride core: A multiscale mechanistic study

CO 2 is an abundant C 1 feedstock for fuel and chemical synthesis. We have previously demonstrated experimentally a stepwise insertion of CO 2 into a [Cu 2 H 2 ] core via a solid–gas in crystallo reaction, forming formate species that are unstable and inaccessible under solution-phase conditions. This work elucidates how structural confinement within the crystal lattice enables such selective reactivity. In particular, co-crystallized tetrahydrofuran molecules induce site asymmetry around the [Cu 2 H 2 ] unit, modulating both the local electronic environment and CO 2 diffusion pathways. Using a multiscale computational approach that combines classical molecular mechanics, hybrid quantum mechanics/molecular mechanics molecular dynamics, and enhanced-sampling free energy calculations, we demonstrate how site asymmetry affects CO 2 binding affinities and reaction pathways. These results provide detailed mechanistic insight into CO 2 insertion and hydride transfer, highlighting key differences between crystal- and solution-phase pathways and offering a general framework for understanding how lattice confinement shapes chemical reactivity.

Chemical bonding↗

DOE OSTI2022

A deformation-dependent coupled Lagrangian/semi-Lagrangian meshfree hydromechanical formulation for landslide modeling

Abstract The numerical modelling of natural disasters such as landslides presents several challenges for conventional mesh-based methods such as the finite element method (FEM) due to the presence of numerically challenging phenomena such as severe material deformation and fragmentation. In contrast, meshfree methods such as the reproducing kernel particle method (RKPM) possess unique features conducive to modelling extreme events such as the absence of a structured mesh and the ease of adaptive refinement, among others. While the semi-Lagrangian reproducing kernel (SL-RK) shape functions of RKPM defined in the current configuration have proven to be effective in extreme event modelling, the computational cost for the re-evaluation of the shape functions at every time step is costly. In this work, a deformation-dependent coupling of the Lagrangian reproducing kernel (L-RK) and SL-RK approximations is proposed for the solution of a hydro-mechanical formulation for effective simulations of landslides. The ramp function is constructed based on an equivalent plastic strain as a deformation-dependent transition from L-RK shape functions to SL-RK ones as the deformation progresses. The particular focus of the paper will be on modelling seepage-induced landslides with a mixed $$u$$ u – $$p$$ p formulation to couple the solid and fluid phases. Examples are presented to examine the effectiveness of this coupled Lagrangian/semi-Lagrangian reproducing kernel (L–SL RK) formulation and to highlight its performance in landslide modelling.

Baek, Jonghyuk↗

DOE OSTI2025

A Multiscale Approach to Simulate Non‐Isothermal Multiphase Flow in Deformable Porous Materials

Coupled thermal, hydraulic, and mechanical processes in porous materials play important roles in several energy and environmental technologies. The Darcy-Brinkman-Biot (DBB) framework has proven effective in modeling multiphase fluid flow in deformable porous solids across both pore and Darcy scales, including in systems where fractures coexist with a porous matrix. In this study, we extend the DBB framework, originally designed for isothermal conditions, to address non-isothermal problems by incorporating an energy conservation equation. The resulting solver, hybridBiotThermalInterFoam, enables simulations of coupled multiphase fluid flow, heat transfer, and solid deformation in hybrid-scale systems containing both solid-free regions and ductile porous domains. The new solver is validated through comparisons with analytical solutions and, also, against established heat transfer solvers chtMultiRegionFoam and compressibleInterFoam. Further, a series of 2D and 3D case studies, including two-phase heat transfer in solid-free, static, or deformable porous media, highlights the solver's capacity to simulate complex flow dynamics and heat transport in systems involving high mobility ratios, viscous fingering, and fracture propagation. Our results establish the feasibility of incorporating thermal effects in simulations of a wide variety of energy geotechnics and environmental applications, including enhanced hydrocarbon recovery, soil remediation, and enhanced geothermal energy systems.

04 OIL SHALES AND TAR SANDS↗

DOE OSTI2025

Chromium segregation-induced oxide evolution in Ni-10Cr alloys during high-temperature oxidation

The oxidation behavior of a Ni-10(wt%)Cr alloy under high-temperature O 2 conditions is investigated using transmission electron microscopy and first-principles calculations. Results reveal that chromium segregation plays a central role in driving the evolution of complex oxide phase structures during oxidation. At low Cr concentrations, Cr preferentially segregates to NiO grain boundaries or internal pores, substituting for Ni atoms and forming Ni(Cr)O solid solutions. As Cr content increases, enhanced diffusion promotes Cr penetration into the NiO lattice, leading to the formation of multiphase oxide structures. First-principles modeling corroborates these findings: at low Cr concentrations, Cr atoms favor surface and grain-boundary segregation, while higher concentrations lead to Cr aggregation within the NiO bulk. Furthermore, the integrated experimental-theoretical approach provides atomistic insights into Cr-mediated mass transport mechanisms during alloy oxidation and offers valuable guidance for controlling oxide growth kinetics and phase stability in Ni-Cr alloys, with implications for improving oxidation resistance in high-temperature structural applications.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Stress Corrosion Cracking of NaSICON Membranes in Aqueous Electrolytes for Redox-Flow Batteries

The sodium super-ionic conductor (NaSICON) has versatile applications as a ceramic electrolyte for energy storage, where it can serve as an impermeable separator in solid-state batteries and redox flow systems. In particular, NaSICON systems have been proposed to be relatively stable in contact with water, making them compatible with aqueous battery chemistries. However, owing to their brittle nature and metal oxide constituents, stress-corrosion cracking (SCC) is an important failure mechanism that has not been previously explored. In this study, we assess the fracture toughness of NaSICON membranes in contact with aqueous solutions that are relevant to redox flow systems. Microindentation was performed to generate visible surface cracks and residual stress, which were observed to grow in length after exposure to aqueous solutions. This allows for a quantitative measurement of fracture toughness, which decreases after exposure to water. To contextualize these results, we develop a simplified model of the fracture behavior in aqueous redox-flow batteries that incorporate NaSICON membranes, illustrating the importance of SCC in cell design. This work provides quantitative insights into SCC as a failure mode in NaSICON, enhancing our understanding of the chemo-mechanical behavior of ceramic electrolytes in contact with aqueous solutions.

Zhang, Mengyao↗

NASA NTRS1973

Grain boundary mobility in anion doped MgO

Certain anions OH(-), F(-) and Gl(-) are shown to enhance grain growth in MgO. The magnitude of their effect decreases in the order in which the anions are listed and depends on their location (solid-solution, second phase) in the MgO lattice. As most anions exhibit relatively high vapor pressures at sintering temperatures, they retard densification and invariably promote residual porosity. The role of anions on grain growth rates was studied in relation to their effect on pore mobility and pore removal; the atomic process controlling the actual rates was determined from observed kinetics in conjunction with the microstructural features. With respect to controlling mechanisms, the effects of all anions are not the same. OH(-) and F(-) control behavior through creation of a defect structure and a grain boundary liquid phase while Cl(-) promotes matter transport within pores by evaporation-condensation. Studies on an additional anion, S to the minus 2nd power gave results which were no different from undoped MgO, possibly because of evaporative losses during hot pressing. Hence, the effect of sulphur is negligible or undetermined.

Kapadia, C. M.↗

NASA NTRS1974

Metallographic study of metallic fragment of lunar surface material

A high precision investigation of a metallic fragment from the lunar material returned by the Soviet Luna 16 automatic station revealed three characteristic temperature intervals with different kinetics of solid solution decomposition. The following were found in the structure of the iron-nickel-cobalt alloy: (1) delta-phase and alpha-ferrite of diffusional, displacement origin in the grain boundary and acicular forms; and (2) martensite of isothermal and athermal nature, acicular, lamellar, massive, and dendritic. The diversity of the shapes of structural constituents is associated with the effect on their formation of elastic distortions and various mechanisms of deformation relaxation processes.

Mints, R. I.↗