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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Microstructural characterisation of friction stir welding joints of mild steel to Ni-based alloy 625

In this study, 6-mm-thick mild steel and Ni-based alloy 625 plates were friction stir welded using a tool rotational speed of 300 rpm and a travel speed of 100 mm·min{sup −1}. A microstructural characterisation of the dissimilar butt joint was performed using optical microscopy, scanning and transmission electron microscopy, and energy dispersive X-ray spectroscopy (XEDS). Six different weld zones were found. In the steel, the heat-affected zone (HAZ) was divided into three zones and was composed of ferrite, pearlite colonies with different morphologies, degenerated regions of pearlite and allotriomorphic and Widmanstätten ferrite. The stir zone (SZ) of the steel showed a coarse microstructure consisting of allotriomorphic and Widmanstätten ferrite, degenerate pearlite and MA constituents. In the Ni-based alloy 625, the thermo-mechanically affected zone (TMAZ) showed deformed grains and redistribution of precipitates. In the SZ, the high deformation and temperature produced a recrystallised microstructure, as well as fracture and redistribution of MC precipitates. The M{sub 23}C{sub 6} precipitates, present in the base material, were also redistributed in the stir zone of the Ni-based alloy. TMAZ in the steel and HAZ in the Ni-based alloy could not be identified. The main restorative mechanisms were discontinuous dynamic recrystallisation in the steel, and discontinuous and continuous dynamic recrystallisation in the Ni-based alloy. The interface region between the steel and the Ni-based alloy showed a fcc microstructure with NbC carbides and an average length of 2.0 μm. - Highlights: • Comprehensive microstructural characterisation of dissimilar joints of mild steel to Ni-based alloy • Friction stir welding of joints of mild steel to Ni-based alloy 625 produces sound welds. • The interface region showed deformed and recrystallised fcc grains with NbC carbides and a length of 2.0 μm.

36 MATERIALS SCIENCE↗
DOE OSTI2016

The microstructure of the surface layer of magnesium laser alloyed with aluminum and silicon

The surface layer under analysis was formed as a result of diffusion bonding of a thin AlSi20 plate to a magnesium substrate followed by laser melting. Depending on the process parameters, the laser beam melted the AlSi20 plate only or the AlSi20 plate and a layer of the magnesium surface adjacent to it. Two types of microstructure of the remelted layer were thus analyzed. If the melting zone was limited to the AlSi20 plate, the microstructure of the surface layer was typical of a rapidly solidified hypereutectic Al–Si alloy. Since, however, the liquid AlSi20 reacted with the magnesium substrate, the following intermetallic phases formed: Al{sub 3}Mg{sub 2}, Mg{sub 17}Al{sub 12} and Mg{sub 2}Si. The microstructure of the modified surface layer of magnesium was examined using optical, scanning electron and transmission electron microscopy. The analysis of the surface properties of the laser modified magnesium revealed that the thin layer has a microstructure of a rapidly solidified Al–Si alloy offering good protection against corrosion. By contrast, the surface layer containing particles of intermetallic phases was more resistant to abrasion but had lower corrosion resistance than the silumin type layer. - Highlights: •A CO{sub 2} laser was used for surface alloying of Mg with AlSi20. •Before alloying, an AlSi20 plate was diffusion bonded with the Mg substrate. •The process parameters affected the alloyed layer microstructure and properties. •With melting limited to AlSi20, the layer had a structure of rapidly solidified AlSi20. •Mg–Al and Mg–Si phases were present when both the substrate and the plate were melted.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructural characteristics of σ phase and P phase in Ru-containing single crystal superalloys

Microstructural instability caused by topologically close-packed (TCP) phase precipitation restricts the useful compositional range of advanced Ni-base single crystal superalloys in industrial applications. Limited systematic investigations of TCP formers (Cr and Mo) additions on microstructural evolution of both the σ phase and the P phase in Ru-containing single crystal superalloys have been reported. In this study, the microstructural characteristics of σ phase and P phase were investigated in three Ru-containing superalloys with different levels of Cr and Mo additions at 950 °C and 1100 °C by using phase extraction, X-ray diffraction, scanning electron microscope and high resolution transmission electron microscopy. The experimental results indicated that the high level additions of Cr and Mo promoted the formation of σ phase and P phase, respectively. The amount of σ phase was much higher than that of P phase after long term exposure at 950 °C and 1100 °C. The sheet-like σ phase existed in the alloy with higher Cr addition after thermal exposure at 950 °C and 1100 °C for 1000 h, while the needle-like P phase precipitated in high Mo content alloy after thermal exposure at 1100 °C for 1000 h and the intergrowth of σ phase and P phase was observed after thermal exposure at 950 °C for 500 h. Both the σ phase and P phase were enriched in Re, W, Cr and Mo, but the σ phase contained more Re and Cr while the P phase contained more Mo and Ni, and Ru was found in both phases. The nucleation of σ phase was much easier than P phase due to the more ledge steps in the interfacial structure between σ phase and matrix, as well as the higher partitioning ratios of Re, Cr and Mo. This study is helpful to understand the microstructural evolution of σ phase and P phase, and to optimize the alloy design in Ru-containing superalloys. - Highlights: •Microstructures of σ phase and P phase were characterized in detail. •Cr and Mo influenced the precipitation of σ phase and P phase, respectively. •Partitioning ratios and interfacial relationship decided precipitation behaviors.

36 MATERIALS SCIENCE↗
DOE OSTI2017

A microstructural analysis of aluminum buildup during thermomechanical processing

Highlights: • Microstructure of roll coating developed on a ground steel work roll was examined. • Roll coating was formed during the 20 pass hot rolling schedule of an Al-Mg alloy. • The roll coating had a complex layered nanocrystalline and amorphous structure. • The roll coating layers were composed of metallic Al, porous MgO and C. • Work roll debris, Fe and Cr, were observed embedded within the roll coating. - Abstract: The microstructure and composition of a roll coating built-up on an AISI M2 steel work roll during a 20 pass hot rolling schedule using a laboratory rolling tribo-simulator with a roll-on-block configuration was examined. The AISI M2 steel work roll was characterized by grinding grooves and possessed a surface roughness (R{sub a}) of 0.17 μm. The roll coating developed under these lubricated conditions was discontinuous, patchy and streaked out in the rolling direction. The microstructure and chemical composition of the material transfer that made up the roll coating was analysed and revealed to possess a complex composite microstructure consisting of nanocrystalline aluminum, nanocrystalline/amorphous MgO and amorphous carbon layers. The nanocrystalline MgO layers were porous structures lying between the solid metallic aluminum layers. Debris particles from the wear of the work roll were detected embedded within the carbon layer and at the base of the roll coating. The microstructure of the roll coating appear to be determined by the deformation conditions experienced during the rolling process, while its composition is dependent on the composition of the rolled alloy, the work roll and the lubrication conditions employed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

The partial substitution of Y with Gd on microstructures and mechanical properties of as-cast and as-extruded Mg-10Zn-6Y-0.5Zr alloy

Highlights: • The as-extruded Mg-10Zn-6Y-0.5Zr and Mg-10Zn-3Y-3Gd-0.5Zr alloys show bimodal microstructure and DRXed microstructure. • In addition to W phase, Icosahedral quasicrystal phase layer is observed at the surface of some W phase particles in as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt. %) alloy. • The as-extruded Mg-10Zn-6Y-0.5Zr (wt. %) alloy exhibits TYS of 341 MPa, UTS of 368 MPa and elongation to failure of 6.8%. While the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt. %) alloy shows lower TYS of 247 MPa, UTS of 330 MPa and higher elongation to failure of 19.8%. - Abstract: Mg-10Zn-6Y-0.5Zr (wt%) alloy and Mg-10Zn-3Y-3Gd-0.5Zr (wt%) alloy with medium RE content have been fabricated by conventional casting and indirect extrusion. The as-extruded Mg-10Zn-6Y-0.5Zr (wt%) alloy shows a bimodal microstructure containing dynamic recrystallized (DRXed) grains with average grain size of 2 μm and deformed regions. In addition to the fragmented W phase particle bands distributing along the extrusion direction, large amount of nano W phase and small amount of nano β{sub 2}′ phase are precipitated in the matrix. While the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt%) alloy exhibits completely dynamic recrystallized microstructure with average grain size of 3 μm. The broken W phase particles are distributed homogeneously in the matrix. Icosahedral quasicrystal phase layer is observed at the surface of some W phase particles in the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr alloy. The as-extruded Mg-10Zn-6Y-0.5Zr (wt%) alloy exhibits yield strength of 341 MPa, ultimate tensile strength of 368 MPa and elongation to failure of 6.8%. While the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr (wt%) alloy shows lower yield strength of 247 MPa, ultimate tensile strength of 330 MPa and higher elongation to failure of 19.8%. The higher strength in the as-extruded Mg-10Zn-6Y-0.5Zr (wt%) alloy is mainly attributed to higher area fraction of unDRXed regions with strong texture and the precipitation of nano W and β{sub 2}′ phase. The fully recrystallized microstructure with weak texture and the formation of icosahedral quasicrystal phases with good coherent bond with α-Mg contribute to the good ductility of the as-extruded Mg-10Zn-3Y-3Gd-0.5Zr alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural evolution and mechanical properties of maraging steel produced by wire + arc additive manufacture process

Highlights: • Wire + arc additive manufacture (WAAM) was applied to produce maraging steel structures. • Microstructure evolution of WAAM alloy was characterized and correlated with the layer-by-layer building manner. • Mechanical properties of WAAM alloy were tested and correlated with the aging response of WAAM microstructure. • Retained austenite content was measured and correlated with the tensile strength loss. - Abstract: Wire + arc additive manufacture is developed for producing large-scale metallic components. In this paper, maraging steel parts were produced, and the microstructure and mechanical properties were investigated. The microhardness and tensile strength of the as deposited alloy reduced from the bottom to the top due to the transient thermal cycling, which resulted in partial aging and non-uniform formation of intermetallic compounds along the building direction. Solutionizing, followed by 3 h aging, significantly reduced the microstructural heterogeneity and increased the mechanical properties by 24.7% through the formation of large amounts of finely distributed precipitates. The as deposited alloy possessed superior strength to the wrought alloy in solutionized condition but inferior to the later in aged condition, which was attributed to the less pronounced aging response of the low-angle columnar grains characterized microstructure and the presence of retained and reverted austenite.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure and functionality of a uniquely graded super duplex stainless steel designed by a novel arc heat treatment method

Highlights: • A uniquely graded duplex stainless steel microstructure was fully characterized. • Nitrogen depletion occurred by solid state diffusion next to the fusion boundary. • Phase fractions and stability were compared to thermodynamic calculations. • Orientation relationships and morphology of sigma, chi, nitrides and R were studied. • A diagram summarizing functionality of aged duplex microstructures is introduced. - Abstract: A novel arc heat treatment technique was applied to design a uniquely graded super duplex stainless steel (SDSS), by subjecting a single sample to a steady state temperature gradient for 10 h. A new experimental approach was used to map precipitation in microstructure, covering aging temperatures of up to 1430 °C. The microstructure was characterized and functionality was evaluated via hardness mapping. Nitrogen depletion adjacent to the fusion boundary depressed the upper temperature limit for austenite formation and influenced the phase balance above 980 °C. Austenite/ferrite boundaries deviating from Kurdjumov–Sachs orientation relationship (OR) were preferred locations for precipitation of σ at 630–1000 °C, χ at 560–1000 °C, Cr{sub 2}N at 600–900 °C and R between 550 °C and 700 °C. Precipitate morphology changed with decreasing temperature; from blocky to coral-shaped for σ, from discrete blocky to elongated particles for χ, and from polygonal to disc-shaped for R. Thermodynamic calculations of phase equilibria largely agreed with observations above 750 °C when considering nitrogen loss. Formation of intermetallic phases and 475 °C-embrittlement resulted in increased hardness. A schematic diagram, correlating information about phase contents, morphologies and hardness, as a function of exposure temperature, is introduced for evaluation of functionality of microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2018

On the formation mechanism of the ring-like microstructure of high-pressure die-cast A390 alloy

Highlights: • High-pressure die casting A390 alloy exhibited ring-like microstructure consisted of PSPs-free and PSPs-rich zones. • With 3D data, the size and morphology distribution of PSPs showed similar tendency regardless of the location. • The latent heat released from the PSPs led to the formation of ring-like band. • Widely observed defect band was inhibited because of the precipitation and growth of PSPs during solidification. - Abstract: The microstructure of the A390 alloy during high pressure die casting (HPDC), including pores, primary silicon particles (PSPs) and Cu-rich phases was characterized using synchrotron X-ray tomography. On the cross section of the sample exhibited ring-like or band microstructure, which comprised multiple PSPs-free and PSPs-rich zones. The PSPs distributed evenly in both size and morphology regardless of the ring-like microstructure. The size of aluminum dendrites changed according to the location of the ring-like microstructure, and was highly dependent on the local latent heat released from the PSPs as well as the distribution of the ‘net’ Cu-rich phases. Along the radial direction of the sample exhibited an abrupt increase of pores, indicating a tendency for forming a defect band in but such tendency was inhibited because of the huge amount of latent heat released by the PSPs during solidification, which was quite different from that of either magnesium alloys or hypoeutectic aluminum alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Meso-scale microstructural agglomerate quantification in boron carbide using X-ray microcomputed tomography

Highlights: • First known quantification of agglomerate defect distributions comprising of carbonaceous and aluminum nitride phases B{sub 4}C. • In-depth statistical analyses of the size, orientation, and morphology of the defects. • The determination of directional dependence of the hot-pressing direction on the agglomerate distributions. - Abstract: Failure in brittle materials is governed, in part, by the specific microstructure of that material, with heterogeneous microstructures generally leading to reduced mechanical properties and performance. In ceramics used for armor, an increase in compressive strength can be an indicator of improved ballistic performance. In hot-pressed boron carbide (B{sub 4}C) ceramic plates, failure has been attributed to carbonaceous flakes observed on the fracture surfaces of failed specimens. However, this current work shows agglomerates, in addition to the carbonaceous flakes, are present in this boron carbide. The density and distribution of these agglomerates are believed to influence the ballistic performance. Therefore, it is of interest to improve the quantification of meso-scale microstructural agglomerates so that strategies can be developed to mitigate them. This work is focused on the microstructural characterization of dumbbell-shaped compression specimens that were machined from a single tile of pressure-aided densification (PAD) B{sub 4}C, using high-resolution micro-computed tomography (microCT). Large clusters of non-B{sub 4}C agglomerates, up to 125 μm in diameter, were observed in addition to the typical smaller carbonaceous flakes and aluminum-based phases. Agglomerate size distribution, orientation, morphology, and spacing were quantified both parallel and perpendicular to the pressing direction. This defect quantification provides valuable information for a better understanding of the material microstructure which is a critical step in improving armor materials for the future.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure and microhardness of wire-based laser metal deposited AA5087 using an Ytterbium fibre laser

Highlights: • Heat conduction strongly affects the microstructural development. • Heat conduction conditions changes with increasing part height. • Anisotropic microstructural development affects the microhardness of the part. • Anisotropic mechanical properties along the structure are assumed. - Abstract: Wire-based additive manufacturing has been increasingly investigated in recent years. Although it is possible nowadays to manufacture structures that are free from inner defects such as porosity and cracks using wire and arc additive manufacturing, there is still a lack of knowledge regarding wire-based laser metal deposition of aluminium and its alloys. In order to be able to produce locally tailored part properties, it is necessary to understand the process parameter to material property relationships. Using laser energy sources, it becomes possible to analyse in detail the heat input and to observe occurring microstructural evolutions. This work includes a microstructural and mechanical characterization of an AA5087 wall structure. Detailed analyses of the chemical composition, texture, and microhardness of the structure have been performed. The microstructure contains different grain orientations as well as grain shapes and sizes along the structure, resulting in locally different material properties. The results have been analysed and discussed in reference to fundamental theories such as the Hall–Petch and Orowan mechanisms.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effects of initial microstructures on serrated flow features and fracture mechanisms of a nickel-based superalloy

Highlights: • Uniaxial tensile tests are performed on a nickel-based superalloy at 473 K–973 K and low strain rates. • Effects of initial microstructures on serrated flow features, and fracture characteristics are analyzed. • The dislocation across slip in the matrix is responsible for the serrated flow. • Nucleation and growth of micro-voids is the main fracture mechanism of ST and HS superalloys. • The better tensile ductility is obtained with raising the deformation temperatures for the SAT superalloy. - Abstract: The uniaxial tensile experiments are performed on a nickel-based superalloy with different initial microstructures at intermediate temperatures (473–973) K and low strain rates (0.0001–0.001) s{sup −1}. Effects of initial microstructures on plastic deformation mechanisms, serrated flow features, and fracture characteristics are analyzed. It is clearly demonstrated that the plastic deformation mechanism of serrated flow is irrelevant to the initial microstructures, and the dislocation across slip in the matrix is responsible for the serrated flow. However, the effects of initial microstructures on fracture mechanisms are obvious, i.e., the main fracture mechanism of the ST (solution treated) and HS (solution plus γ′/γ″ phases aging precipitation) superalloys are the nucleation and growth of micro-voids, which accelerates the break of carbides and interfacial failure of carbides/matrix. While for the SAT (solution plus δ phases aging precipitation) superalloy, δ phases and carbides play a significant role in the nucleation of micro-voids. Furthermore, the increase of the deformation temperature reduces the elongation to fracture of the ST and HS superalloys. However, the better tensile ductility is obtained with raising the deformation temperatures for the SAT superalloy.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Fine grained fully lamellar structure acquisition and microstructure characteristics of Ti-44Al-4Nb-4V-0.3Mo-Y alloy

Highlights: • Cellular structure is the component of the microstructure of hot forging in α + β two-phase-field. • Inhomogeneous lamellar structure could be eliminated by hot forging in β+γ binary phase field. • After hot forging and annealing at β+γ two-phase-region, fine grained fully-lamellar microstructure is obtained. - Abstract: In this paper, the microstructure characteristic of a β solidifying TiAl alloy Ti-44Al-4Nb-4V-0.3Mo-Y (at. %) was investigated systematically. Cylindrical blanks were isothermal forged at 1250 °C within (α + β) two-phase-field and 1200 °C within (β + γ) two-phase-field under the strain rate of 0.02 s{sup −1} and 0.03 s{sup −1}, with a total reduction of 75%. The microstructure of the alloy forged in α + β two-phase-field consists of lamellar colonies (only represents α{sub 2}/γ lamellar colonies), mixture structure of β/B2 phase and γ phase as well as β/γ lamellae resulted from cellular reaction. However, a large amount of equiaxed γ grains appear with no β/γ lamellae available under forging in β + γ two-phase-field, and the average size of γ grain is about 10 μm. By further annealed at 900 °C for about 0.5 h, the structure of hot forging at 1250 °C is composed of β/B2 phase and equiaxed γ grains with the mean size about 5 μm. After heat treated at 1200 °C for 2 h, the microstructure of this annealed samples is characterized by fine grained fully lamellar (FFL) structure with size of 20 μm. A specially designed hot forging process is proposed, which prevents the existence of inhomogeneous lamellar structure.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of microstructures on hot compression behavior of a Ti-43Al-2Si alloy fabricated by cold crucible continuous casting

Highlights: • TiAl alloys with different lamellar colonies were fabricated by cold crucible continuous casting. • EBSD was used to investigate the evolution of lamellae during the hot compression. • Lamellar colony boundaries promote the dynamic recrystallization process. - Abstract: To investigate the influence of lamellar orientation and colony boundary on deformation behavior, fully lamellar Ti-43Al-2Si alloys were prepared by cold crucible continuous casting and isothermal compression tests were conducted at different temperatures in the range 1373–1523 K with a strain rate of 0.01 s{sup −1}. The as-cast microstructures were elongated colony with lamellae oriented at nearly 45° to the compression direction and equiaxed colony with various lamellae orientations, respectively. The results revealed that serious cracking or sliding traces appeared on the surface of deformed specimens with elongated colony original microstructure and that their peak stresses were lower compared to those of specimens with equiaxed colony original microstructure. The relationship between deformation behaviors and as-cast microstructure was analyzed in detail. It was found that the recrystallization/globularization level is significantly lower than that in specimens with equiaxed colony original microstructure during hot deformation owing to the preferred nucleation sites in colony boundaries. Finally, the lamellae conversion process was characterized to reveal the softening mechanisms of full lamellar TiAl-based alloy during hot compression.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Multi-scale and multi-technic microstructure analysis of a linear friction weld of the metastable-β titanium alloy Ti-5Al-2Sn-2Zr-4Mo-4Cr (Ti17) towards a new Post-Weld Heat Treatment

Highlights: • Soft joint showing sharp macro-zones and marked by asymmetrical process effects • Gradient of thermomechanical loads identified through progressive stages of transformation • Highly textured recrystallized β grains at the joint core with distorted β lattice • Lattices, phase fractions, microstructures and hardness homogenized after heat treatment - Abstract: Linear Friction Welding (LFW) is a solid-state joining process producing narrow joints mainly developed for the aircraft industry. The Thermo-Mechanical Processing (TMP) loads imposed on the material cause complex microstructure transformations. This study aimed at characterizing the local microstructures and crystallographic configurations to identify the mechanisms impacting the stability and the mechanical properties of a Ti17 LFW joint with the objective of establishing an innovative homogenizing Post-Weld Heat Treatment (PWHT). The process caused a narrow zone of ±2 mm from the friction interface to reach the isothermal α → β transformation temperature under a heating rate of 500 K/s followed by quenching (−100 K/s). The TMP resulted in the formation a ±3 mm wide soft Process Affected Zone (PAZ) delimited by three characteristic zones: the Welding Line (WL width ≈ 400 μm), The Thermo-Mechanically Affected Zone (TMAZ width ≈ 1 mm) and the Heat Affected Zone (HAZ). β TMP resulted in the total dissolution of the α phase in the joint core (WL + TMAZ) and formed strongly textured {110}<111> β recrystallized grains in the WL by continuous dynamic recrystallization of squeezed prior-β grains in the TMAZ. α + β TMP led to a gradual loss of hardness in the HAZ whose microstructure is similar to the one of the base material (BM) but is subject to gradual α laths dissolution due to the local temperatures experienced during LFW. A PWHT consisting in a β annealing followed by an α + β ageing resulted in a uniformly hardened weld with a homogenized Widmanstätten microstructure in the whole assembly.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A detailed study of the microstructure and thermal stability of typical SiC fibers

Highlights: • The cross-sectional microstructure and thermal stability of typical SiC fibers were characterized via SEM and TEM. • The SiC fiber with gradient microstructure has better properties than that with uniform microstructure. • The graphite exhibits straight planes on the fiber surface while they're turbostratic inside the fiber. Continuous SiC fibers have attracted increasing research interest for their significant application in aerospace and nuclear energy. Control of inhomogeneity and decrement of defects are crucial for improving the mechanical and high-temperature performance of SiC fibers. Thus an understanding of fine and detailed microstructural and microchemical distribution of SiC fibers is urgently needed. In the present work, the cross-sectional phase distributions, morphologies and defects of amorphous, non-stoichiometric and near-stoichiometric SiC fibers were well characterized. From surface to core, the amorphous and non-stoichiometric fibers exhibited uniform microstructures, but a gradient change along the radial direction was observed in the near-stoichiometric fiber. Nanosized SiC and turbostratic carbon (2–4 nm) were randomly distributed inside the amorphous fiber. A large amount of graphite surrounding SiC grains appears in the non-stoichiometric fiber which possess low strength and weak thermal stability. The near-stoichiometric fiber has transgranular fracturing, high strength and favorable thermal stability, and the graphite planes are turbostratic inside the fiber but straight on the surface. The results of both energy-dispersive X-ray spectrometry measurements and first-principles calculations demonstrate that Al atoms can occupy Si sites in the SiC grains. Our findings offer fine understanding for fabricating SiC fibers with superior properties.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

An automated procedure built on MTEX for reconstructing deformation twin hierarchies from electron backscattered diffraction datasets of heavily twinned microstructures

Here we present a set of algorithms built on the MTEX and MATLAB graph toolboxes for automatic reconstruction of deformation twin hierarchies from Electron Backscatter Diffraction (EBSD) datasets with a focus on developing methods for heavily twinned microstructures (twin fractions >0.5). The algorithms address key issues arising at large strains, mainly: missing twin relationships, grouping of heavily deformed grain fragments into families of similar orientation originating from a single initial grain, identification of parent fragments for large twin volume fractions, and classification of families having twin relationships with multiple families. To facilitate the development of these algorithms, large-grained ultra-high purity α-Ti deformed in compression along two directions is investigated. Graphs are utilized to handle non-local geometric merging and to represent relationships throughout the reconstruction process. When determining if a grain fragment is from the undeformed microstructure, the combined metrics of the fragment's orientation volume fraction in the initial texture and the directed graph centrality measure of out-closeness (the number of nodes reached in a graph from a given node) are essential. To address automation in reconstructing the sequence of twinning and relating fragments originating from a single grain in the initial microstructure, the twin family tree is formulated as a minimum spanning tree emanating from the initial grain family. A scheme constructing the distances associated with twin relationship comprising the spanning tree is developed, and a novel quasi-directional Prim spanning tree algorithm is used to determine the twin family tree. The procedure is demonstrated to significantly improve the level of automation in reconstructing twin hierarchies in heavily twinned microstructure compared to other methodologies in literature. The procedure can readily be applied to analyses of twinning in metals, as well as provide an approach for routinely extracting twin statistics at larger deformation levels than previously possible. Significantly, the procedure is demonstrated to be capable of identifying third generation twinning in α-Ti microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Scan strategies in EBM-printed IN718 and the physics of bulk 3D microstructure development

Three-dimensional (3D) characterization provides opportunities for understanding processing-structure relationships in additively manufactured (AM) materials. Bulk samples of Inconel 718 were fabricated via electron beam melting (EBM) in order to study microstructural development as a function of energy input and beam scan strategy. TriBeam tomography of bulk Inconel 718 microstructures built under steady-state growth conditions reveals the sensitivity of microstructure formation and evolution to machine process parameters. Here, samples manufactured using a narrow range of energy input per unit build area result in varied grain morphologies and crystallographic textures. Using TRUCHAS, a thermal simulation software, the thermal history of bulk scan strategies was predicted, and combined with a calibrated microstructure-processing map to accurately predict bulk grain morphologies. The solidification parameters and the 3D measured nucleation density are used to predict the transition between columnar and equiaxed grain morphologies, providing a process map to guide AM parameter choices to locally control as-printed microstructure. A two-dimensional metric for characterizing bulk grain morphology was also found to agree well with predictions from the process map calibrated by 3D data. Combined with 3D tomography and thermal modelling, the physics of structure development were understood at a new level of detail with respect to the competing processes of grain nucleation and epitaxial growth.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Additive friction stir deposition of SS316: Effect of process parameters on microstructure evolution

Solid state nature of additive friction stir deposition (AFSD) additive manufacturing process is very advantageous in terms of defect formation and microstructural refinement in the material. Current study presents the process optimization, microstructural evolution and kinetics of recrystallization for AFSD deposited low stacking fault energy material - SS316. As deposited microstructure shows equiaxed ultra fine grains with an average grain size of ~5.0 ± 0.5 μm. Shear deformation at high temperature during processing leads to the operation of restoration mechanisms. Observation of necklace type microstructure in the as deposited SS316 is attributed to discontinuous dynamic recrystallization during processing. Recrystallization kinetics of the AFSD SS316 is characterized using Johnson-Mehl-Avarami-Kolmogorov (JMAK) model. Deformation – thermal cycling during AFSD process resulted in inconsistent recrystallization kinetics. Variation in strain, strain rate and temperature during processing with processing parameters result in varying microstructure and tool wear. Further, high strength-ductility combination and sustained work hardening in as deposited SS316 appear to arise from transformation and twinning during deformation, leading to the formation of hierarchical twins and martensitic phase after deformation.

36 MATERIALS SCIENCE↗