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At least 217 records · Page 12

Cluster defects in gibbsite nanoplates grown at acidic to neutral pH

Gibbsite [α-Al(OH) 3 ] is the solubility limiting phase for aluminum across a wide pH range, and it is a common mineral phase with many industrial applications. The growth mechanism of this layered-structure material, however, remains incompletely understood. Synthesis of gibbsite at low to circumneutral pH yields nanoplates with substantial interlayer disorder. Here we examine defects in this material in detail, and the effects of recrystallization in highly alkaline sodium hydroxide solution at 80 °C. We employed a multimodal approach, including scanning electron microscopy, magic-angle spinning nuclear magnetic resonance (MAS-NMR), Raman and infrared spectroscopies, X-ray diffraction (XRD), and X-ray total scattering pair distribution function (XPDF) analysis to characterize the ageing of the nanoplates over several days. Additionally, XRD and XPDF indicate that gibbsite nanoplates precipitated at circumneutral pH contain dense, truncated sheets imparting a local difference in interlayer distance. These interlayer defects appear well described by flat Al 13 aluminum hydroxide nanoclusters nearly isostructural with gibbsite sheets present under synthesis conditions and trapped as interlayer inclusions during growth. Ageing at elevated temperature in alkaline solutions gradually improves crystallinity, showing a gradual increase in H-bonding between interlayer OH groups. Between 7 to 8 vol% of the initial gibbsite nanoparticles exhibit this defect, with the majority of differences disappearing after 2–4 hours of recrystallization in alkaline solution. The results not only identify the source of disorder in gibbsite formed under acidic/neutral conditions but also point to a possible cluster-mediated growth mechanism evident through inclusion of relict oligomers with gibbsite-like topology trapped in the interlayer spaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of Properties of Laser Powder Bed Fusion 3D-Printed Inconel 718 for Centrifugal Turbomachinery Applications

Here, this paper presents the results of a comprehensive effort to characterize the properties of Inconel 718 produced by a form of laser powder bed fusion (LPBF) additive manufacturing (AM) or 3D-printing, subsequently subjected to hot isostatic pressing (HIP) and heat treatment according to standards F3055-14a and AMS 5663, respectively. Material property data, while broadly available for traditional Inconel 718 presentations (e.g. forgings or castings), is currently lacking for the 3D-printed material. It is expected that while limited in size, the experimental data sets presented provide sufficient information to glean the capability of LPBF Inconel 718. These include: 1) Chemical composition, electron backscatter diffraction (EBSD), and x-ray energy dispersive spectroscopy (XEDS) characterization of 3D-printed material structure; 2) Tensile properties — 0.2% yield stress, ultimate stress, modulus of elasticity, and elongation to failure — based on 108 samples, as functions of temperature and sample print orientation; 3) Creep rupture data including the Larson-Miller parameter, based on 21 samples; and 4) High cycle fatigue data based on 21 samples as a function of temperature. Results are compared to available standards and/or data for forged, cast, and other AM Inconel 718. A key observation of this study, based on the EBSD results, is that while the material appears to approach full recrystallization following heat treatment, there is a detectable fraction of the material that does not fully recrystallize, resulting in a material with mechanical properties (e.g. yield stress, creep rupture) measurably lower than those of forgings, but higher than those of castings.

30 DIRECT ENERGY CONVERSION↗

Understanding Microstructural Effects on Dynamic Performance Towards the Development of Shock Metamaterials

With the recent advances in additive manufacturing (AM), long-range periodic lattice assemblies are being developed for vibration and shock mitigation components in aerospace and military applications with unique geometric and topological structures. There has been extensive work in understanding the static properties associated with varying topology of these lattice architectures, but there is almost no understanding of microstructural affects in such structures under high-strain rate dynamic loading conditions. Here we report the shock behavior of lattices with varying intrinsic grain structures achieved by post process annealing. High resolution 316L stainless steel lattices were 3D printed by a laser-powder bed fusion machine and characterized by computed tomography. Subsequent annealing resulted in stress-relieved and recrystallized lattices. Overall the lattices had strong cubic texture aligning with the x-, y- and z-directions of the build with a preference outside the build direction (z). The recrystallized sample had more equiaxed polygonal grains and a layer of BCC ferrite at the surface of the structure approximately 1 grain thick. Upon dynamic compression the as-deposited lattice showed steady compaction behavior while the heat-treated lattices exhibit negative velocity behavior indicative of failure. We attribute this to the stiffer BCC ferrite in the annealed lattices becoming damaged and fragmenting during compression.

36 MATERIALS SCIENCE↗

STEP Report on Advanced ODS FeCrAl Alloys for Fission Applications

Oak Ridge National Laboratory is developing advanced low-Cr oxide dispersion strengthened (ODS) FeCrAl alloys for accident tolerant fuel (ATF) cladding. This report presents the characterization of two new ODS FeCrAl tubes by using powder commercially mechanically alloyed by Zoz GmbH, which underwent high-precision tube rolling with two different annealing schedules. This work shows that the ODS FeCrAl tube without recrystallization exhibits consistent mechanical behavior in comparison with a previously produced tube. The second tube, which underwent a full recrystallization step before the final tube rolling step, showed some circumferential cracking and exhibited limited ductility in the axial tube tensile tests. Based on current and prior work on the ODS FeCrAl alloy system, this report compares the current state of the scientific literature on the alloy class with that of wrought FeCrAl without oxide additions. Then, this report makes recommendations for future research directions that should be undertaken to increase the technology readiness level for ODS FeCrAl as a viable ATF candidate material. This report has been submitted as fulfillment of milestone M3FT-20OR020202064 titled, “STEP Report on Advanced ODS FeCrAl Alloys for Fission Applications” for the US Department of Energy Office of Nuclear Energy’s Advanced Fuel Campaign of the Fuel Cycle R&D program.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterization of Disconnection Content Associated with Grain Boundary Motion in Tungsten

The objective of this study is to develop a new computational methodology to predict the motion of grain boundaries in tungsten associated with recrystallization. This approach accounts recently discovered high-temperature grain boundary phases in tungsten and other metals and alloys. This paper reports the initial work in the project that developed a novel technique for molecular dynamics to characterize disconnections, dislocation-like defects in grain boundaries that mediate grain boundary motion. Grain boundary properties are needed for a thermomechanical model of recrystallization of tungsten for magnetic fusion applications.

36 MATERIALS SCIENCE↗

The 650 °C Tensile Deformation of Graded IN718-René41 Superalloy Fabricated by Laser Blown-Powder Directed Energy Deposition

The microstructure and 650 °C tensile properties of a compositionally graded IN718-René41 (718-R41) superalloy fabricated by laser blown-powder directed energy deposition (DED-LB/M) are investigated to understand structure–property relationships and baseline tensile properties. Digital Image Correlation (DIC), in situ neutron diffraction, and conventional characterization techniques are performed to study the as-built and heat-treated states. The applied heat treatment generates static recrystallization and equiaxed grains in 718-rich compositions, while R41-rich compositions remain partially or un-recrystallized possibly influenced by a higher MC carbide fraction (>0.5%). The yield strengths of the 718 and R41 sections in the heat-treated state are comparable to wrought forms but the graded compositions show weakness due to unoptimized heat treatment. Diffraction elastic constants first decrease and then increase along the 718-R41 composition gradient, while a small difference is observed between the as-built and heat-treated states and γ, γ′ phases. Overall, the compositionally graded region shows a smooth transition in the elastic properties. Grain-level load transfer from the (220) to (200) grains shows compositional dependence, and qualitatively agrees with DIC-measured macroscopic yield strength. Within the (200) grains, the γ/γ′ phases deform elastically until the γ phase yields and afterwards, the γ′ phase takes load from the γ phase.

Huang, Shenyan (ORCID:0000000196528114)↗

The effect of solute additions on the steady-state creep behavior of dispersion-strengthened aluminum.

The effect of solute additions on the steady-state creep behavior of coarse-grained dispersion-strengthened aluminum alloys was studied. Recrystallized dispersion-strengthened solid solutions were found to have stress and temperature sensitivities quite unlike those observed in single-phase solid solutions having the same composition and grain size. The addition of magnesium or copper to the matrix of a recrystallized dispersion-strengthened aluminum causes a decrease in the steady-state creep rate which is much smaller than that caused by similar amounts of solute in single-phase solid solutions. All alloys exhibited essentially a 4.0 power stress exponent in agreement with the model of Ansell and Weertman. The activation energy for steady-state creep in dispersion-strengthened Al-Mg alloys, as well as the stress dependence, was in agreement with the physical model of dislocation climb over the dispersed particles.

Reynolds, G. H.↗

Resistance spot welding of dispersion-strengthened nickel alloys

To develop easily-applied production method for resistance spot welding use unrecrystallized sheet material, develop welding schedule that will produce a solid-state spot weld without recrystallizing sheet, and postheat to produce grain growth across weld line during recrystallization of sheet material.

Moore, T. J.↗

Development of advanced high strength tantalum base alloys. Phase 3: Influence of metallurgical condition on the mechanical properties of ASTAR-811C sheet

Metallurgical condition was shown to have a significant effect on the creep properties of ASTAR-811C (Ta-8W-1Re-0.7Hf-0.025C) sheet. Cold worked material exhibited creep rates 30 times higher than solution annealed material and 10 times greater than for recrystallized material. Both grain size and the carbide morphology changes as the final annealing temperature was raised from 3000 F to 3600 F. However, the lowest creep rates were achieved for material which retained the high temperature form of the Ta2C precipitate. Samples with GTA weldments had essentially identical properties as recrystallized base metal. Cooling rates from 3600 F of 5, 50, and 800 F deg/min. had little effect on the 2000 and 2400 F creep behavior of ASTAR-811C.

Ammon, R. L.↗

Development of forming and joining technology for TD-NiCr sheet

Forming joining techniques and properties data were developed for thin-gage TD-NiCr sheet in the recrystallized and unrecrystallized conditions. Theoretical and actual forming limit data are presented for several gages of each type of material for five forming processes: brake forming, corrugation forming, joggling, dimpling and beading. Recrystallized sheet can be best formed at room temperature, but unrecrystallized sheet requires forming at elevated temperature. Formability is satisfactory with most processes for the longitudinal orientation but poor for the transverse orientation. Dimpling techniques require further development for both material conditions. Data on joining techniques and joint properties are presented for four joining processes: resistance seam welding (solid-state), resistance spot welding (solid-state), resistance spot welding (fusion) and brazing. Resistance seam welded (solid-state) joints with 5t overlap were stronger than parent material for both material conditions when tested in tensile-shear and stress-rupture. Brazing studies resulted in development of NASA 18 braze alloy (Ni-16Cr-15Mo-8Al-4Si) with several properties superior to baseline TD-6 braze alloy, including lower brazing temperture, reduced reaction with Td-Ni-Cr, and higher stress-rupture properties.

Torgerson, R. T.↗

The age and petrography of two Luna 20 fragments and inferences for widespread lunar metamorphism.

Ages were determined by the Ar-40/Ar-39 method on two metaclastic rocks returned from the lunar highlands north of Mare Fecunditatis by the Luna 20 probe. Both samples gave very well-defined argon retention ages of 3.90 plus or minus 0.04 AE which are indistinguishable from each other within a resolution of 0.02 AE. Both fragments, 22006 and 22007, are highly recrystallized polymict breccias; there is no evidence of radiogenic Ar-40, and the age almost surely dates the time of recrystallization. The cosmic ray exposure ages of these fragments are similar and high: 900 million years for 22006, 1300 million years for 22007. 22007 also contains substantial trapped argon with a high Ar-40/Ar-36. The Luna 20 results greatly extend the area of the moon's surface exhibiting a well-defined record of metamorphism at 3.9 AE. So far, lunar history in the interval from 4.6 to 3.9 AE is not preserved in the ages of surface rocks. This obliteration suggests lunar-wide metamorphic conditions occurring or terminating at this time as a result of major impacts.

Podosek, F. A.↗

Deformation and annealing response of TD-nickel chromium sheet

The deformation and annealing response of TD-nickel chromium (TD-NiCr) 0.1 inch thick sheet was examined using various cold-rolling and annealing treatments. Upon annealing (above 816 C (1500 F), the as-received material was converted from an initially ultra-fine grain size (average grain dimension 0.51 micron) to a large grain structure. Increases in grain size by a factor of 100 to 200 were observed for this transformation. However, in those material states where the large grain transformation was absent, a fine grain recrystallized structure formed upon annealing (above 732 C (1350 F)). The deformation and annealing response of TD-NiCr sheet was evaluated with respect to the processing related variables as mode and severity of deformation and annealing temperature. Results indicate that the large grain transformation, classical primary recrystallization occurs. Using selected materials produced during the deformation and annealing study, the elevated temperature tensile properties of TD-NiCr sheet were examined in the temperature range 593 C (1100 F) to 1093 C (2000 F). It was observed that the elevated temperature tensile properties of TD-NiCr sheet could be optimized by the stabilization of a large grain size in this material using the cold working and/or annealing treatments developed during the present investigation.

Kane, R. D.↗

Pyroxene poikiloblastic rocks from the lunar highlands

The results of detailed petrographic, X-ray, electron microprobe, ion probe, and Ar-40/Ar-39 age studies of pyroxene poikiloblastic breccias, an important lunar highlands lithology, are interpreted to indicate that high grade metamorphic recrystallization occurred over wide regions of the moon at about 4.0 G.y. This metamorphism was probably related to a period of high meteorite influx at that time. The temperatures achieved were highly variable but in some cases were sufficiently intense to cause varying degrees of partial melting of the precursor highlands breccias. A complete spectrum of metamorphic grades from only slight recrystallization to virtually complete melting would be expected in such a model. Such a spectrum is observed in the Apollo 16 rocks.

Bence, A. E.↗

Meteor ablation spheres from deep-sea sediments

Spheres from mid-Pacific abyssal clays (0 to 500,000 yrs old), formed from particles that completely melted and subsequently recrystallized as they separated from their meteoroid bodies, or containing relict grains of parent meteoroids that did not experience any melting were analyzed. The spheres were readily divided into three groups using their dominant mineralogy. The Fe-rich spheres were produced during ablation of Fe and metal-rich silicate meteoroids. The glassy spheres are considerably more Fe-rich than the silicate spheres. They consist of magnetite and an Fe glass which is relatively low in Si. Bulk compositions and relict grains are useful for determining the parent meteoroid types for the silicate spheres. Bulk analyses of recrystallized spheres show that nonvolatile elemental abundances are similar to chondrite abundances. Analysis of relict grains identified high temperature minerals associated with a fine-grained, low temperature, volatile-rich matrix. The obvious candidates for parent meteoroids of this type of silicate sphere is a carbonaceous chondrite.

Blanchard, M. B.↗

Structure of deformed silicon and implications for low-cost solar cells

The paper reports on an investigation of the microstructure and minority carrier lifetime of silicon in uniaxially compressed silicon samples, the objective of which was to determine if it is feasible to produce silicon solar cells from sheet formed by high temperature deformation. It is reported that recrystallization was found to be incomplete in both fine and large grained materials, and that the major mode of recrystallization appears to be migration of existing boundaries into the deformed regions. Also, minority carrier diffusion length was found to be drastically reduced after deformation, perhaps due to contamination or cooling rate, and recovered only slightly with annealing. It is concluded that these results suggest that high temperature deformation of silicon for direct production of sheet for high efficiency solar cells is not practical. It is noted that potential may exist for its use as a coarse grained substrate.

Mardesich, N.↗

Petrography and olivine mineral chemistry of chondrules and inclusions in the Allende meteorite

The examination of 19 polished-thin sections from a sample of the Allende meteorite reveals that anhedral olivine chondrules (OCs) are the most abundant chondrule type (19.7% of total chondrules + inclusions), followed by recrystallized OCs (7.5%), euhedral OCs (2.9%), glassy/skeletal OCs (2.7%), and barred OCs (2.3%). The most abundant inclusions are those comprised of many small olivine crystals with varying amounts of opaque minerals and glass (31.5%), followed by fine grained inclusions (16.1%) and single olivine crystals (15.7%). Microprobe analyses of olivines show that recrystallized and barred chondrules are the most forsteritic and exhibit relatively narrow compositional ranges, whereas single crystals have the widest range, from Fa sub 0.3 to Fa sub 49.

Simon, S. B.↗

EBIC and HVTEM studies of RTR silicon ribbon

The defect structure of RTR ribbon #6-731, run 803 was studied. Prior to laser recrystallization the defect structure consists of closely spaced twin and grain boundaries. Precipitation of impurities occurs after laser recrystallization. The observation of electrically active defects in EBIC was correlated with HVTEM studies. Pairs of electrically active defects in twin boundaries are due to stacking faults connecting the twin boundaries.

Cunningham, B.↗

Epitaxial and polycrystalline GaAs solar cells using OM-CVD techniques

GaAs epitaxial films were grown by chemical vapor deposition using organo-metallic sources (OM-CVD) on single crystal and polycrystalline bulk GaAs, as well as on bulk polycrystalline and recrystallized thin-film Ge substrates. Details of Antireflecting Metal-Oxide-Semiconductor (AMOS) solar cells fabricated on GaAs films grown on bulk polycrystalline Ge and recrystallized Ge thin-film substrates will be discussed, as well as preliminary photovoltaic results obtained for n(+)/p homojunction structures.

Yeh, Y. C. M.↗