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At least 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Controlling Preferred Grain Orientation in Vapor-Deposited Metal-Halide Perovskite Thin Films

Metal-halide perovskites are promising semiconductor materials for light-absorber layers in solar cells due to their optimized band gap, defect tolerance, and relative ease of synthesis. In this work, we demonstrate the viability of vapor transport deposition (VTD), a solvent-free processing method, to realize polycrystalline films of both lead iodide (PbI 2 ) and methylammonium lead iodide (MAPbI 3 ) perovskites showing preferential crystallographic orientation. Notable is the difference in perovskite film texturing observed for sequentially and co-deposited VTD films of MAPbI 3 , as well as the lack of strong preferential orientation in solution-processed MAPbI 3 films. While sequential deposition of the perovskite precursors PbI 2 and methylammonium iodide (MAI) leads to a MAPbI 3 film with a limited preferential grain orientation, co-deposited MAPbI 3 films mirror the orientation of excess PbI 2 present in the film. The latter is confirmed by the similar dependence of preferential orientation for PbI 2 and co-deposited MAPbI 3 on underlayer roughness, as well as the emergence of preferential orientation in MAPbI 3 only when excess PbI 2 is present. Both MAPbI 3 and PbI 2 films show a strong preferred lattice orientation on smooth substrates, while on rougher substrates, this orientation is disrupted. Furthermore, these results are interpreted as excess PbI 2 frustrating the diffusion of MAI in the film, which would otherwise disrupt the preferred orientation, pointing to a notable difference in lattice orientation arising from processing technique and conditions.

Deposition↗
DOE OSTI2025

An engineering perspective on evaluating mechanisms governing ductility in pure molybdenum

The United States lacks a stable domestic supply of 99 mTc, a critical medical imaging isotope generated from 99 Mo. Accelerator-based production using 100 Mo targets (aMo) introduces mechanical concerns due to the ductile-to-brittle transition temperature inherent to refractory metals like Mo. This study evaluates the tensile behavior of aMo targets from 25 to 1000 °C, compared to powder-metallurgy-processed natural Mo (PMo) and cast-and-rolled Mo (RMo), both as-received and after 5 ppm O 2 exposure in flowing He. RMo showed superior ductility (7.3% at 25 °C, 48% at 1000 °C) and strength, attributed to its fine, elongated grains and high geometrically necessary dislocation density. PMo exhibited variable ductility (up to 33%), while aMo remained brittle, with a maximum elongation of 10.4% at 600 °C. EBSD analysis revealed weak texture in PMo and aMo, but high defect density in aMo limited dislocation mobility. This work links processing, microstructure, and deformation mechanisms to guide fabrication of ductile refractory targets.

Hyer, Holden C. [Oak Ridge National Laboratory (OR↗
DOE OSTI2021

Surface and subsurface characterization of laser-interference structured Ti6Al4V

Ti6Al4V specimens were exposed to high-energy laser pulses of 1.24 J/cm 2 fluences per pulse using a two-beam optical configuration to attain laser-interference. In addition to the formation of periodic surface textures by laser-interference, scanning electron microscope (SEM) images demonstrated several microstructural changes on the surface processed. Moreover, the surface and subsurface of Ti6Al4V specimens were characterized for the as-received and laser-interference processed conditions using x-ray photoelectron spectroscopy (XPS) and electron energy dispersive spectroscopy (EDS). The XPS data showed that this laser technique is effective at removal of surface contaminants for Ti6Al4V. The XPS analysis also revealed the formation of an oxy-nitride layer on the laser treated material. Finally, the microstructure analysis indicates that grain refinement, dendrite and twin structures were found near the surface due to laser processing.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructural Evolution of Steel During Magnetic Field-Assisted Processing

Advancing magnetic field-assisted processing, as an energy-efficient method for tailoring steel microstructures, requires a thorough understanding of how the high magnetic field impacts microstructural evolution, particularly its effect on prior austenite grain structures. The current investigation of a near-eutectoid composition, Fe-C alloy, uses electron backscatter diffraction to examine the morphology and orientation of martensite and pearlite microstructures, and to reconstruct the parent austenite microstructures present during equivalent heating under varied magnetic field strengths (0-T, 2-T, 5-T, and 9-T). It was observed that the magnetic field has a negligible effect on martensite lath/block width, slightly decreases prior austenite grain size, and increases the fraction of austenite grains with annealing twins. Additionally, the magnetic field increases the phase fraction of proeutectoid ferrite but has a negligible effect on pearlite block size and the distribution of boundary misorientation angles. No preferred texture was induced by the magnetic field, regardless of the applied field direction, in the proeutectoid ferrite phase or the martensite and prior austenite microstructures. Furthermore, the observed results contradict previous literature, and the differences are discussed.

Magnetic Materials↗
DOE OSTI2020

Chemo‐mechanical Alterations Induced From CO 2 Injection in Carbonate‐Cemented Sandstone: An Experimental Study at 71 °C and 29 MPa

Abstract Carbon capture, utilization, and storage may lead to mechanical degradation of the subsurface reservoir from fluid‐rock interaction, which could lead to wellbore instability or reservoir compaction. To better understand potential relationship between mechanical degradation with various carbonate cement textures and compositions in sandstone reservoirs, six flow‐through experiments were conducted. Formation water (TDS = 5,390 mg/L) enriched with CO 2 flowed through two types of Pennsylvanian Morrow B Sandstone: an ankerite‐siderite‐cemented sandstone (disseminated cement texture) and a calcite‐cemented sandstone (poikilotopic cement texture). The experiments produced little change in permeability in the ankerite‐siderite‐cemented sandstone, but permeability increased up to more than 1 order of magnitude in the calcite‐cemented sandstone. Ultrasonic measurements and cylinder‐splitting tests (also known as Brazilian tests) suggested negligible mechanical degradation of the ankerite‐siderite‐cemented sandstone. Variable changes, with significant mechanical degradation in the static moduli, were observed in the calcite‐cemented sandstone. Thus, dissolution of the disseminated ankerite‐siderite cement (0.28–0.30%) had minimal impact on modifying the flow network and the mechanical integrity of the sandstone, whereas dissolution of the poikilotopic calcite cement (0.89–1.13%, quantified with fluid chemistry and visualized with X‐ray microcomputed tomography) impacted the mechanical strength of the sandstone by disconnecting framework grains. With the high water‐to‐rock mass ratios (7.3–8.2) and number of pore volumes (147–675) employed in these experiments, potential risks are most relevant to regions near injection wells. Ultimately, the chemo‐mechanical effects induced by CO 2 injection are strongly influenced by the cement texture and composition and the burial history of the reservoir rock.

Wu, Z.↗
DOE OSTI2021

Shear assisted processing and extrusion of enhanced strength aluminum alloy tubing

Hollow extrusions are used in many industries to make strong, lightweight, and affordable structures. Shear Assisted Processing and Extrusion (ShAPE) enables the extrusion of many alloys, often with noteworthy properties. In this investigation, ShAPE was used to extrude 1 and 2 mm wall tubes of aluminum alloy 6063 measuring 12 mm in diameter at extrusion speeds up to 3.8 m/min. This speed is 10 and 15 times faster than has been reported for any alloy using ShAPE and friction stir back extrusion, respectively. Increasing the extrusion speed from 0.7 to 3.8 m/s resulted in using 68% less process energy at steady state. Microstructural analysis and tensile testing were performed on as-extruded tubes and tubes with a direct T5 heat treatment. Grain refinement from 65 µm to below 20 µm was observed. Growth of macroscale Mg 2 Si strengthening precipitates was not observed. ShAPE processing resulted in recrystallization, and extrusion speed was shown to influence final extrudate texture. Here, transmission electron microscopy analysis revealed that the as-extruded microstructure was free of nanoscale ß" strengthening precipitates. Nanoscale ß" was prominent in direct-aged (T5) ShAPE tubes, similar to a slightly over-aged conventional T6 microstructure. As-extruded tubes had ultimate tensile strengths on par with conventional T5 extrusions and approximately double the total elongation. Tubes that underwent a T5 heat treatment had yield and ultimate strengths averaging 198 and 234 MPa, respectively, with an average total elongation of 11%. The tensile test results are comparable to a conventional T6 heat treatment, but without the solutionization heat treatment step. Mechanical properties either remained flat or improved with increased extrusion speed, which suggests that ShAPE can be scaled up to an industrial process to create energy- and economically efficient high-strength extrusions.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Selective laser melting of 304L stainless steel: Role of volumetric energy density on the microstructure, texture and mechanical properties

The role of volumetric energy density on the microstructural evolution, texture and mechanical properties of 304L stainless steel parts additively manufactured via selective laser melting process is investigated. 304L is chosen because it is a potential candidate to be used as a matrix in a metal matrix composite with nanoparticles dispersion for energy and high temperature applications. The highest relative density of 99 %±0.5 was achieved using a volumetric energy density of 1400 J/mm 3 . Both XRD analysis and Scheil simulation revealed the presence of a small trace of the delta ferrite phase, due to rapid solidification within the austenitic matrix of 304L. Here, a fine cellular substructure ranged between 0.4–1.8 μm, was detected across different energy density values. At the highest energy density value, a strong texture in the direction of [100] was identified. At lower energy density values, multicomponent texture was found due to high nucleation rate and the existing defects. Yield strength, ultimate tensile strength, and microhardness of samples with a relative density of 99 % were measured to be 540 ± 15 MPa, 660 ± 20 MPa and 254 ± 7 HV, respectively and higher than mechanical properties of conventionally manufactured 304L stainless steel. Heat treatment of the laser melted 304L at 1200 °C for 2 h, resulted in the nucleation of recrystallized equiaxed grains followed by a decrease in microhardness value from 233 ± 3 HV to 208 ± 8 HV due to disappearance of cellular substructure.

304L stainless steel↗
DOE OSTI2021

Microstructure and Mechanical Properties of the AA7075 Tube Fabricated using Shear Assisted Processing and Extrusion (ShAPE)

Shear Assisted Processing and Extrusion (ShAPE) experimental setup and tooling were adopted for extruding thin-walled AA7075 aluminum tube from as-cast non-homogenized billet material in a single run. The mechanical and microstructural characterizations were performed on the extrudate in the as-extruded condition without subsequent heat treating. It was shown that the ShAPE process developed a significantly refined microstructure with uniform and almost equiaxed grain structure on both hoop and axial cross-sections of the extrudate as well as through the thickness of the material. The pole figures and inverse pole figures of the EBSD data showed an strong shear texture development, and it was found out that axial shear is the dominant deformation mechanism in the regions near the inner surface of the tube, while combined axial and torsional shears are the two dominant modes of deformation near the outer surface of the extrudate. As for the mechanical properties, there was an increase of 150% and 73% in the yield and ultimate strengths of the tube produced using ShAPE process, respectively, and a 18% decrease in maximum uniform plastic elongation compared to the conventionally extruded AA7075-O tube.

Shear Assisted Processing and Extrusion, Friction ↗
DOE OSTI2020

Deformation heterogeneity and intragrain lattice misorientation in high strength contrast, dual-phase bridgmanite/periclase

A bridgmanite/periclase aggregate is investigated due to its prevalence in the Earth’s lower mantle and its importance for understanding geodynamic processes. In dual-phase polycrystalline aggregates, both strength contrast between phases and single crystal elastic and plastic anisotropy are known to influence the development of intragrain misorientation, and the evolution of crystallographic texture. In this study, full-field crystal plasticity simulations are performed with a finite element solution method, and applied to an aggregate of a mechanically strong orthorhombic phase with perovskite structure (bridgmanite, MgSiO 3 ), and a relatively weaker cubic phase (periclase, MgO). The relative strengths of the phases are parameterized to elucidate the effect that strength contrast has on texture evolution and single-phase simulations are performed for comparison. Altogether, results indicate that the relative strength between the two phases influences the development of plasticity, and the overall texture evolution. Results are discussed in light of trends related to the evolution of plasticity and misorientation in the aggregate, and their dependence on both the strength contrast between phases as well as the spatial distribution of grains and phases.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Strength, deformation, and equation of state of tungsten carbide to 66 GPa

Here, strength, texture, and equation of state of hexagonal tungsten monocarbide (WC) have been determined under quasi-hydrostatic and non-hydrostatic compression to 66 GPa using angle-dispersive X-ray diffraction in the diamond anvil cell. Quasi-hydrostatic compression in a Ne pressure medium demonstrates that nanocrystalline WC is slightly less incompressible than bulk-scale WC, with respective bulk moduli of K 0 = 377 ± 7 and 397 ± 7 GPa and pressure derivatives K 0 ’ = 3.8 ± 0.3 and 3.7 ±0.3. This decrease in incompressibility with grain size is similar to behavior observed in other ceramics. Under nonhydrostatic compression, WC supports a mean differential stress of ~12-15 GPa at plastic yielding, which occurs at ~30 GPa. Strength in WC is anisotropic, with the (001) plane supporting 29-42% higher stress than stresses calculated from mean strain. Simulations using an Elasto-ViscoPlastic Self-Consistent model indicate that strength inferred from lattice strain theory may be overestimated due to effects of plastic deformation. Plastic deformation generates a texture maximum near $\langle\bar{2}110\rangle$ in the compression orientation, initially through prismatic slip on the {$10\bar{1}0$}$\langle\bar{1}2\bar{1}0\rangle$ and {$10\bar{1}0$}$\langle0001\rangle$ slip systems, followed by activation of pyramidal slip on {$10\bar{1}1$}$\langle\bar{2}113\rangle$ at ~40-50 GPa.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanoscale trace-element zoning in pyrite framboids and implications for paleoproxy applications

Pyrite framboids (spherical masses of nanoscale pyrite) are among the earliest textures of pyrite to form in sediments. It has been proposed that their trace-element (TE) contents can be used to track the TE composition of the water column in which they formed. However, it is not clear how these TEs are associated with the framboidal pyrite grains. For instance, it is important to know whether they are incorporated uniformly or are enriched in different regions of the framboid. Here, we used high-resolution scanning transmission electron microscopy to identify chemical zoning within pyrite framboids. We found that initial, nanoscale pyrite euhedral crystals, which make up the volumetric majority of the framboids, are covered/infilled by later pyrite that templates on the earlier pyrite. Further, this later pyrite is enriched in TEs, suggesting that many TEs are incorporated in pyrite relatively late (during early diagenesis; not in the water column). This observation suggests that although chemical analyses of pyrite framboids may provide ocean-water chemistry trends through time, the details are complex. Specifically, the TEs found in pyrite may be linked to adsorption onto organic matter, detrital material, and authigenic minerals such as Fe- and Mn-oxide phases followed by desorption in the sediments or release via dissolution and incorporation into pyrite as overgrowths on the initial nanoscale euhedral crystals that make up framboids. While the use of pyrite chemistry to understand past ocean conditions remains promising, and even diagenetic additions may not preclude the utility of pyrite for reconstructing ancient ocean conditions, care must be taken in interpretations because the end concentration may be influenced by diagenesis.

58 GEOSCIENCES↗
DOE OSTI2020

Constitutive behavior and processing maps of a new wrought magnesium alloy ZE20 (Mg-2Zn-0.2Ce)

ZE20 (Mg-2Zn-0.2Ce) 2 is a new wrought magnesium alloy with improved extrudability and mechanical properties [1]. To understand the constitutive behavior and workability of this new alloy, Gleeble thermomechanical testing has been carried out in this study. The flow stress behavior of ZE20 was investigated between 250 °C–450 °C and 10 –3 s –1 –1.0 s –1 in isothermal compression. Constitutive descriptions of the flow stress are provided. A new general approach at application of the extended Ludwik equation is demonstrated and was found to be more accurate than the hyperbolic sine Arrhenius model while having a similar number of model constants. Processing maps were developed based on the experimental results and are verified with microstructural investigation. A region of safe processing with non-basal texture and high activity of dynamic recrystallization (DRX) was found between 375 °C and 450 °C, from 10 –1 s –1 to 10–2.5 s –1 . A region of potentially safe processing with annealing that is associated with shear band nucleation of non-basal grains was identified for temperatures as low as 300 °C and rates as high as 10 –1 s –1 .

36 MATERIALS SCIENCE↗
DOE OSTI2022

Intense cyclic heating effects on thermo-fracture and thermal shock of solid tungsten and open-cell tungsten foam

Here we investigate here the effects of transient (cyclic) arc-jet plasma and laser heating on fracture behavior of W-foam and solid tungsten. The two key parameters that control the foam thermomechanical response are its density and mean cell size expressed in Pores Per Inch (PPI). Tungsten foam samples were fabricated with Chemical Vapor Deposition (CVD) with variety of PPI and relative density. These were tested under two types of qualitatively different conditions: (1) high-enthalpy arc-jet, and (2) high-power cyclic laser heating. None of the foam samples showed macroscopic through-thickness cracks. However, distributed micro-cracks were observed on ligaments and their triple junctions. Under the same loading conditions, W-foam and solid tungsten showed similar crack network pattern and characteristic length-scale. However, Crack Opening Displacement (COD) was twice as large in solid W as compared to W-foam. Foam samples that have been previously exposed to a low-pressure helium plasma showed significant changes in their surface forming nano-texture fuzz which was removed by subsequent testing in the arc-jet. Extensive fracture and re-crystallization were observed in the thin solid W disk that was fully-constrained from expansion. Thicker and fully-constrained solid W disks did not display recrystallization, grain growth, and extensive cracking. However, thicker disks that were free to expand showed some recrystallization and extensive through-thickness cracks due to less effective cooling and thus higher temperatures. Laser beam testing showed no visible damage formation at 0.19 GW/m 2 and 0.38 GW/m 2 for both low-density (23%) and high-density (43%) foams at low pulses (100-1000). Micro-cracks were observed after 10,000 pulses at 0.19 GW/m 2 in both foams, and in low-density foam after 100,000 at 0.38 GW/m 2 . The nature of thermomechanical damage in W-foam exposed to extreme power (GW/m 2 ) short-duration laser pulses was found to be qualitatively similar to that of high power (MW/m 2 ) long-duration arc-jet.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Alloying effects on deformation induced microstructure evolution in copper

In this work, we investigated the effects of alloying elements on plastic deformation and microstructure evolution in polycrystalline copper (Cu) and Cu alloyed with 1 wt. % lead (Cu-1 %Pb). These materials were selected due to the size mismatch between Cu and Pb, with the latter forming precipitates at grain boundaries. Multi-modal characterization techniques, including neutron diffraction, electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM), along with finite element simulations were employed to study the deformation behavior across multiple length scales. While both Cu and Cu-1%Pb exhibited similar macroscale response and final deformation textures, both dislocation line profile analysis and TEM revealed increased dislocation density in deformed Cu-1%Pb specimens. The presence of lead precipitates also significantly affected local plastic deformation during compression, with their influence diminishing with increasing strain. These results demonstrate the complex relationships between alloying elements, plastic deformation, microstructural evolution, and material behavior under load. The insights gained from this multi-scale and multi-technique approach contribute to the fundamental understanding of microstructural evolution in immiscible alloys and are valuable for tailoring the properties of structural materials for specific engineering applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Texture and precipitation behavior of friction stir welded Inconel 825 alloy

The microstructure, texture pattern, and precipitation behavior of friction stir butt welded Inconel 825 alloy are highlighted here. The microstructure of bright regions and black-banded regions in the stir zone (SZ) is characterized by SEM, EBSD, and TEM with EDS. EBSD analysis justifies that the SZ exhibits a dynamic recrystallized structure. Grain boundary mapping corroborates the insignificant difference in the low- and high-angle grain boundaries fraction between the SZ, the thermo-mechanically affected zone, and the base metal. TEM analysis confirms the formation of nano twins and dispersion of nano-size precipitations in the grains, and at the grain boundaries as well. Grain refinement and nano-size precipitation formation in the SZ significantly enhanced both microhardness and tensile strength.

Das, Hrishikesh↗
DOE OSTI2024

Parameter development and characterization of laser powder directed energy deposition of Nb – Alloy C103 for thin wall geometries

This work focuses on the parameter development and microstructural characterization of Nb-based alloy C103 for thin wall structures produced via laser powder – directed energy deposition (LP – DED). Laser power and scanning speeds were varied as part of a design of experiments to identify adequate print parameters. Combinations were evaluated for relative density, porosity, and geometrical accuracy. A combination of a laser power of 1420 W and scanning speed of 14 mm/s resulted in a relative density >99%, exhibited a consistent weld bead profile and was used for further microstructural evaluation. A mix of optical and scanning electron microscopy (SEM) revealed small, slightly elongated grains along the edges and large epitaxial grains in the central region along the Build – Transverse view. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis revealed Hf rich columnar cells in the center that transition into an evenly spaced cellular structure towards the edges of the built sample. Electron backscatter diffraction (EBSD) scans show a sharp [001] texture when looking at the cross section of the sample along the build direction. The Build – Scan view revealed a zig – zag pattern that follows the back – and – forth deposition strategy that was used. Finally, microhardness measurements were taken in the as – built (AB) and stress relieved (SR) conditions to baseline preliminary mechanical properties. The AB condition exhibited a large amount of scatter in the data and averages up to 11% larger than the SR condition. The reduction in scatter upon applying the SR cycle are indicative of a large concertation of dislocations present in the AB condition.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Additively manufactured novel Al-Cu-Sc-Zr alloy: Microstructure and mechanical properties

An in-depth understanding of microstructure and resultant properties is paramount in the design of a novel alloy system, especially for additive manufacturing (AM). The present investigation aims to characterize a prototypical AM Al alloy with great potential for structural applications. An Al-1.5Cu-0.8Sc-0.4Zr alloy designed using integrated computational material engineering was printed using the laser powder bed fusion AM process. This novel alloy shows promising combination of strength and ductility in as-built and peak-aged conditions. This improvement in the tensile properties is attributed to the presence of both coherent L1 2 Al 3 Sc/Al 3 (Sc,Zr) precipitates and Cu-rich regions. The microstructures were studied via extensive microscopy at different length scales using X-ray microscopy, scanning electron microscopy, and transmission electron microscopy. Fractography revealed that the columnar grain boundaries in as-built condition allow easy slip transfer as compared to the equiaxed grains, with the apex of the melt pool acting as the crack nucleation site. Furthermore, the peak aged condition resulted in improved strength while marginally sacrificing ductility due to precipitates decorating dislocations, grain boundaries and melt pool boundaries thus acting as obstacles to slip transfer.

36 MATERIALS SCIENCE↗