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At least 109 records · Page 6

Intermediate-phase engineering via dimethylammonium cation additive for stable perovskite solar cells

Achieving the long-term stability of perovskite solar cells is arguably the most important challenge required to enable widespread commercialization. Understanding the perovskite crystallization process and its direct impact on device stability is critical to achieving this goal. The commonly employed dimethyl-formamide/dimethyl-sulfoxide solvent preparation method results in a poor crystal quality and microstructure of the polycrystalline perovskite films. In this work, we introduce a high-temperature dimethyl-sulfoxide-free processing method that utilizes dimethylammonium chloride as an additive to control the perovskite intermediate precursor phases. By controlling the crystallization sequence, we tune the grain size, texturing, orientation (corner-up versus face-up) and crystallinity of the formamidinium (FA)/caesium (FA) y Cs 1-y Pb(I x Br 1-x )3 perovskite system. A population of encapsulated devices showed improved operational stability, with a median T80 lifetime (the time over which the device power conversion efficiency decreases to 80% of its initial value) for the steady-state power conversion efficiency of 1,190 hours, and a champion device showed a T80 of 1,410 hours, under simulated sunlight at 65 degrees C in air, under open-circuit conditions. In conclusion, this work highlights the importance of material quality in achieving the long-term operational stability of perovskite optoelectronic devices.

14 SOLAR ENERGY↗

Shear Assisted Processing and Extrusion of Magnesium Alloy Machining Chips

The Pacific Northwest National Laboratory (PNNL) utilized Shear Assisted Processing and Extrusion (ShAPE) to convert magnesium alloy machining chips directly into wrought material. PNNL fabricated 0.25” and 0.50” round rod from cold compacted briquettes pressed from dry-machined chips by Loukus Technologies. The alloy composition is proprietary and protected by a Materials Transfer Agreement (MTA) between PNNL and Loukus. Extrusions were fabricated using the ShAPE 2.0 machine, tooling, and process. PNNL is evaluating tensile properties per ASTM E8 and microstructure for grain size, texture, and porosity using Scanning Electron Microscopy (SEM) and Electron Backscatter Diffraction (EBSD). Tensile properties and microstructure results were not available at the time of writing this document. Extruded rods have also been sent to Loukus for evaluation.

36 MATERIALS SCIENCE↗

Wire-Based Additive Manufacturing of Stainless Steel Components

In this work three different wire-fed additive manufacturing (AM) processes were employed to evaluate differences between laser, arc, and electron beam heat sources used for high-deposition-rate AM on the order of 1 kg/h. Optimum weld and build parameters were developed independently to match the characteristics of each heat source using 308L stainless steel welding wire as the feedstock. Laser-wire AM was made with the lowest energy per unit length of weld and had the best control of the melt pool and surface finish. Wire arc-based AM had an intermediate energy per unit length of weld of approximately 5× that of the laser process, while electron beam wire AM had the highest energy per unit length of weld at approximately 10× that of the laser process. Analysis of the parts that were built included evaluation of mechanical properties and microstructures, and these properties are discussed with respect to the difference in input energy and cooling rates. Results show that all three processes build parts with properties that exceed those of annealed 304L wrought stainless steel. However, significant differences exist between the processes, and the results presented here can be used to help select the best wire-fed process for a given high-deposition-rate application.

36 MATERIALS SCIENCE↗

The relative density of lunar soil

The specific gravity and minimum and maximum bulk densities were determined for three one-gram lunar soil samples containing particles less than 1 mm in diameter: 14163,148; 14259,3; and 15601,82. The specific gravity varied from 2.90 to 2.93 for the Apollo 14 samples to 3.24 for the Apollo 15 sample. The difference is attributed to the higher proportion of agglutinates and breccias and fewer mineral fragments and basalts in the Apollo 14 soils. The minimum bulk densities varied from 0.87 to 1.10 g/cu cm, while the maximum densities varied from 1.51 to 1.89 g/cu cm. The ranges in values were due to differences in the specific gravity, re-entrant intragranular voids, particle shape, surface texture, and grain arrangements. The in situ lunar soil in the plains areas of the moon can have a low to medium relative density at the surface, increasing rapidly to a very high relative density at depths greater than 10 to 20 cm.

Carrier, W. D., III↗

Experiments on water/melt explosions, nature of products, and models of dispersal

Experiments were carried out in a steel pressure device using controlled amounts of water and thermite melt to examine the mechanical energy released on explosive mixing following the initial contact of the two materials. An experimental design was used to allow the direct calculation of the mechanical energy by the dynamic lift of the device as recorded both optically and physically. A large number of experiments were run to accurately determine the optimum mixture of water and melt for the conversion of thermal to mechanical energy. The maximum efficiency observed was about 12% at a water/thermite mass ratio of 0.50. These experiments are the basis for the development of models of hydroexplosions and melt fragmentation. Particles collected from the experimental products are similar in size and shape to pyroclasts produced by much larger hydrovolcanic explosions. Melt rupture at optimum ratios produces very fine particles whereas rupture at high or low water/melt ratios produces large melt fragments. Grain surface textures in the experimental products are also related to the water/melt ratio and the mechanism of explosive mixing. It is thus possible to have qualitative information about the nature of the explosion from the sizes and shapes of the fragments produced.

Sheridan, M. F.↗

Origin of SNC kaersutitic amphibole: Experimental data

The SNC meteorites, a group of cumulus textured, fine grained diabases, pyroxenites, and dunites, appear to have crystallized at relatively shallow depths on the same SNC parent body. Hydrous minerals generally are not present among the cumulus and intercumulus minerals in these meteorites except for some iddingsite alteration of olivine. The presence of hydrous magmatic amphibole in the SNC melt inclusions indicates that crystallization of the melt inclusions had to take place at significant pressure, probably greater than 1 kb based on previous amphibole stability data. If experimental data for kaersutite amphibole were to be obtained, it should be possible to estimate this pressure more precisely then previously, and to estimate the volatile (H2O) content of the parent magma. At this point, the factors controlling the chemistry and stability of high TiO2, kaersutitic amphiboles are not known. In an attempt to determine the factors which control the stability and chemistry of TiO2-rich amphibole, data was refined and extrapolated from four experimental studies of amphibole-melt equilibria recently completed. At the same time, hypothermal experiments were performed on a composition considered to be an early melt in the Shergotty magma liquid line of descent. The latter experiments were an attempt to reproduce crystallization of the amphibole-bearing melt inclusions.

Rutherford, M. J.↗

Chemical differences between small subsamples of Apollo 15 olivine-normative basalts

Results are presented on the chemical and petrological characterization of nine samples of an Apollo 15 mare basalt suite. The results show that all nine samples are low-silica olivine normative basalts (ONBs) similar to those described earlier for low-silica ONBs from Apollo 15 site. The samples were found to vary in texture and grain size, from fine-grained intergranular or subophitic basalts to coarse-grained granular 'microgabbros'. Several displayed macroscopic heterogeneity. Variation diagrams show that the overall trend of the data is consistent with the fractionation of olivine (plus minor Cr-spinel) from a high-MgO parent magma.

Shervais, J. W.↗

Tambo Quemado: Extraordinary concentrations of REE and refractory trace elements caused by artificial heating

Buchwald examined samples of the IIIB iron Tambo Quemado (TAMQ) cut from the 130 kg main mass. He determined it had been artificially heated, at some time prior to being reported, in an attempt to obtain metal from it. Although the Widmanstatten structure appears relatively unaffected under macroscopic examination, microscopic study of etched sections reveals the effect of the heating. Taenite and plessite area boundaries are indistinct due to high temperature diffusion. Schreibersite, once present in significant amounts, has been melted. Schreibersites in the interior have resolidified in fine-grained eutectic textures surrounded by dark-etching metal rims supersaturated with phosphorus. Buchwald states that phosphate minerals were probably present originally, because graftonite, and its polymorph sarcopside (both essentially Fe3(PO4)2), are common in irons of the IIIB groups. Based on his metallographic study Buchwald estimates TAMQ was heated to 1000 C for about one hour. An interior sample from TAMQ was examined in order to determine what effect this unintended heating 'experiment' had upon the phosphate phases.

Olsen, E.↗

Nitrogen and xenon isotopic disequilibrium in Bachmut (L6) chondrule J2689 and matrix

Chondrule J2689, a large (8-mm) RP chondrule from Bachmut (L6) was previously found to be in disequilibrium with its host in a variety of features: (1) It has a fine-grained hornfelsic texture; (2) it contains low amounts of metal with a low-Ni taenite composition not found in the matrix; (3) the Ni/Co ratio of that metal is close to the solar ratio, which is equal to the bulk Ni/Co ratio (23) of the chondrule; (4) the bulk alkali content of the chondrule is high and the Na/K ratio is fractionated with respect to the average L chondrite ratio of 8; (5) Cr is depleted in spite of the high pyroxene content; (6) the siderophile elements are strongly depleted but are fractionated with their abundances increasing with volatility; and (7) the O isotopes of the chondrule and the host are out of equilibrium. However, the (Fe,Mg) silicates, feldspar, and chromite have chemical compositions indistinguishable from that of the host chondrite. We have studied a chip of the chondrite and of adjacent matrix by stepwise heating and by combustion in O for N and Xe isotopic abundances. (1) The chondrule preserved distinct bulk, metal, and O isotopic compositional features. It is therefore unlikely that the 'equilibration' of the major silicates Fe/Mg ratios could have taken place after accretion; (2) the chondrule was well equilibrated before break-up and exposure to cosmic rays; (3) two N signatures in the matrix also indicate that the matrix is not equilibrated; and (4) all data collected so far point toward the presence of unequilibrated Bachmut components. Very few reactions took place after accretion.

Kim, Y.↗

Microstructural and Mechanical Property Characterization of Shear Formed Aerospace Aluminum Alloys

Advanced manufacturing processes such as near-net-shape forming can reduce production costs and increase the reliability of launch vehicle and airframe structural components through the reduction of material scrap and part count and the minimization of joints. The current research is an investigation of the processing-microstructure-property relationships for shear formed cylinders of the Al-Cu-Li-Mg-Ag alloy 2195 for space applications and the Al-Cu-Mg-Ag alloy C415 for airframe applications. Cylinders which had undergone various amounts of shear-forming strain were studied to correlate the grain structure, texture, and mechanical properties developed during and after shear forming.

Troeger, Lillianne P.↗

Deconvoluting the Friction Stir Weld Process for Optimizing Welds

In the friction stir welding process, the rotating surfaces of the pin and shoulder contact the weld metal and force a rotational flow within the weld metal. Heat, generated by the metal deformation as well as frictional slippage with the contact surface, softens the metal and makes it easier to deform. As in any thermo-mechanical processing of metal, the flow conditions are critical to the quality of the weld. For example, extrusion of metal from under the shoulder of an excessively hot weld may relax local pressure and result in wormhole defects. The trace of the weld joint in the wake of the weld may vary geometrically depending upon the flow streamlines around the tool with some geometry more vulnerable to loss of strength from joint contamination than others. The material flow path around the tool cannot be seen in real time during the weld. By using analytical "tools" based upon the principles of mathematics and physics, a weld model can be created to compute features that can be observed. By comparing the computed observations with actual data, the weld model can be validated or adjusted to get better agreement. Inputs to the model to predict weld structures and properties include: hot working properties ofthe metal, pin tool geometry, travel rate, rotation and plunge force. Since metals record their prior hot working history, the hot working conditions imparted during FSW can be quantified by interpreting the final microstructure. Variations in texture and grain size result from variations in the strain accommodated at a given strain rate and temperature. Microstructural data from a variety of FSWs has been correlated with prior marker studies to contribute to our understanding of the FSW process. Once this stage is reached, the weld modeling process can save significant development costs by reducing costly trial-and-error approaches to obtaining quality welds.

Schneider, Judy↗

Mineralogy of Pyroxene and Olivine in the Almahata Sitta Ureilite

The Almahata Sitta meteorite (hereafter "Alma") is the first example of a recovered asteroidal sample that fell to earth after detection still in the orbit (2008TC3 asteroid), and thus is critical to understand the relationship between meteorites and their asteroidal parent bodies [1]. Alma is a polymict ureilite showing a fine-grained brecciated texture with variable lithologies from black, porous to denser, white stones [1]. It is an anomalous ureilite because of wide compositional ranges of silicates with abundant pores often coated by vapor-deposit crystals [1]. Nevertheless, Alma has general similarities to all ureilites because of reduction textures of silicates suggestive of rapid cooling from high temperature as well as heterogeneous oxygen isotope compositions [e.g., 1-5]. Alma is especially unique because it spans the compositional range of known ureilites [1]. In this abstract we report detailed mineralogical and crystallographic investigations of two different fragments to further constrain its thermal history with regards to the nature of the ureilite parent body.

Mikouchi, T.↗

Curiosity's Mars Hand Lens Imager (MAHLI): Inital Observations and Activities

MAHLI (Mars Hand Lens Imager) is a 2-megapixel focusable macro lens color camera on the turret on Curiosity's robotic arm. The investigation centers on stratigraphy, grain-scale texture, structure, mineralogy, and morphology of geologic materials at Curiosity's Gale robotic field site. MAHLI acquires focused images at working distances of 2.1 cm to infinity; for reference, at 2.1 cm the scale is 14 microns/pixel; at 6.9 cm it is 31 microns/pixel, like the Spirit and Opportunity Microscopic Imager (MI) cameras.

Mars Science Laboratory (MSL)↗

Evolution of the Oxidation State of the Earth's Mantle: Challenges of High Pressure Quenching

The oxidation state of the Earth's mantle during formation remains an unresolved question, whether it was constant throughout planetary accretion, transitioned from reduced to oxidized, or from oxidized to reduced. We investigate the stability of Fe3+ at depth, in order to constrain processes (water, late accretion, dissociation of FeO) which may reduce or oxidize the Earth's mantle. Experiments of more mafic compositions and at higher pressures commonly form a polyphase quench intergrowth composed primarily of pyroxenes, with interstitial glass which hosts nearly all of the more volatile minor elements. In our previous experiments on shergottite compositions, variable fO2, T, and P is less than 4 GPa, Fe3+/TotFe decreased slightly with increasing P, similar to terrestrial basalt. For oxidizing experiments less than 7GPa, Fe3+/TotFe decreased as well, but it's unclear from previous modelling whether the deeper mantle could retain significant Fe3+. Our current experiments expand our pressure range deeper into the Earth's mantle and focus on compositions and conditions relevant to the early Earth. Experiments with Knippa basalt as the starting composition were conducted at 1-8 GPa and 1800 C, using a molybdenum capsule to set the fO2 near IW, by buffering with Mo-MoO3. TEM and EELS analyses revealed the run products from 7-8 GPa quenched to polycrystalline phases, with the major phase pyroxene containing approximately equal Fe3+/2+. A number of different approaches have been employed to produce glassy samples that can be measured by EELS and XANES. A more intermediate andesite was used in one experiment, and decompression during quenching was attempted after, but both resulted in a finer grained polyphase texture. Experiments are currently underway to test different capsule materials may affect quench texture. A preliminary experiment using liquid nitrogen to greatly enhance the rate of cooling of the assembly has also been attempted and this technique will be refined in further experiments.

Danielson, L. R.↗

Oxygen, Magnesium, and Aluminum Isotopes in the Ivuna CAI: Re-Examining High-Temperature Fractionations in CI Chondrites

CI chondrites are thought to approximate the bulk solar system composition since they closely match the composition of the solar photosphere. Thus, chemical differences between a planetary object and the CI composition are interpreted to result from fractionations of a CI starting composition. This interpretation is often made despite the secondary mineralogy of CI chondrites, which resulted from low-T aqueous alteration on the parent asteroid(s). Prevalent alteration and the relatively large uncertainties in the photospheric abundances (approx. +/-5-10%) permit chemical fractionation of CI chondrites from the bulk solar system, if primary chondrules and/or CAIs have been altered beyond recognition. Isolated olivine and pyroxene grains that range from approx. 5 microns to several hundred microns have been reported in CI chondrites, and acid residues of Orgueil were found to contain refractory oxides with oxygen isotopic compositions matching CAIs. However, the only CAI found to be unambiguously preserved in a CI chondrite was identified in Ivuna. The Ivuna CAI's primary mineralogy, small size (approx.170 microns), and fine-grained igneous texture classify it as a compact type A. Aqueous alteration infiltrated large portions of the CAI, but other regions remain pristine. The major primary phases are melilite (Ak 14-36 ), grossmanite (up to 20.8 wt.% TiO 2 ), and spinel. Both melilite and grossmanite have igneous textures and zoning patterns. An accretionary rim consists primarily of olivine (Fa 2-17 ) and low-Ca pyroxene (Fs 2-10 ), which could be either surviving CI2 material or a third lithology.

Frank, D. R.↗

Computational Characterization and Model Verification for 3D Microstructure Reconstruction of Additively-Manufactured Materials

The goal of this study is to characterize and validate the texture and grain topology of additively-manufactured anisotropic three-dimensional (3D) polycrystalline microstructures. The special focus is on developing methodologies to compare the grain shapes and orientations of two-dimensional (2D) and 3D microstructure representations using the same metric. To generate statistical data, synthetic microstructures are reconstructed from experimental data using Markov random field (MRF). The statistical similarity between the experimental and synthetic microstructures is verified by comparing their grain topologies. A universal measure to compare 2D and 3D grains is portrayed through the concept of image moments that are invariant to shape transformations. The graphical plots developed based on moment invariants to compare the 2D and 3D grains are used to verify the synthetic model

Materials Characterization↗

Mechanical response and microstructure evolution from multiaxial stress relaxation in textured zircaloy nuclear cladding

Modern energy markets provide motivation for nuclear reactors to increase operational flexibility and load following capacity of existing reactor designs. The operational power changes result in fuel pellet expansion and contraction resulting in pellet-cladding mechanical interaction (PCMI) and high cladding stresses that are strongly related to stressed corrosion cracking (SCC) which can lead to fuel rod failure. This work aims to quantify the stress fields in cladding with a focus on multiaxial stress relaxation response from an imposed strain and the resulting microstructure changes in textured zircaloy claddings. Stress relaxation tests resulting in multiaxial stress fields are performed to measure the material response of Zircaloy-4 nuclear cladding. Multiple experiments using samples from the same piece of cladding are performed so samples with the same processing history may be removed at strategic points throughout mechanical testing for microstructure characterization. The microstructure evolution is analyzed with mechanical response to evaluate the static recovery impact on crystallographic texture and grain morphology. Experiments are performed at Idaho National Laboratory using an experimental device capable of applying internal pressure and independent axial load to commercial nuclear cladding at elevated temperatures with stress- or strain-controlled experimental capability. X-ray diffraction and electron backscatter diffraction are used for microstructure analysis. Rheological models are used to visualize the multiaxial stress-strain relationships and isolate elastic, plastic, and viscoplastic material properties for analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterization of Additively Manufacture GRCop-42 and GRCop-84

GRCop-42 (Cu-4 at.% Cr-2 at.% Nb) is a copper-based alloy optimized for high temperature, high thermal conductivity applications such as regenerative cooled rocket engine liners. For this application, it is important to minimize contamination such as trace elements and ceramic inclusions. NASA initiated a series of ten builds by eight companies to assess the repeatability of GRCop-42 between vendors and machines. Utilizing inductively coupled plasma – atomic emission spectroscopy (ICP-AES) and energy dispersive spectroscopy (EDS) techniques allowed for identification of contaminants and quantification of their chemistry. In addition, additive manufacturing (AM) creates a unique microstructure that is often highly textured in the build (Z) direction. Electron backscattered diffraction (EBSD) was used to begin quantifying the degree of crystallographic texture in the copper matrix grains. It was also used to identify the crystallographic form of Cr2Nb, the main strengthening phase, present in the samples. Results showed the presence of ceramic inclusions, highly textured grains, and both the low and high temperature phases of Cr2Nb being present.

copper↗