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At least 91 records · Page 5

Effect of processing parameters and strut dimensions on the microstructures and hardness of stainless steel 316L lattice-emulating structures made by powder bed fusion

In this study, we present the effects of input processing parameters and strut thickness (in square struts) on microstructure and properties in laser powder bed fusion additively manufactured stainless steel 316L lattice-emulating structures. Lattice-emulating X-structures with square cross-sections of 1.5, 1.0, and 0.5 mm were fabricated using three different parameter sets with varying power, speed, and therefore, linear energy density. Grain size and morphology were shown to be dictated by epitaxial growth, which was dependent on weld pool morphology. Additionally, grain size and morphology were shown to change across the thickness direction of the struts (from the bottom inclined surface to the top inclined surface). The spatial variation in grain size was reflected by changes in hardness through the thickness of each strut. The 0.5 mm struts exhibited more significant grain elongation in the strut direction and larger sub-grain solidification cell diameters than their thicker counterparts. The larger sub-grain solidification cell diameters in the 0.5 mm samples resulted in correspondingly lower hardness values when compared to samples of higher thicknesses.

36 MATERIALS SCIENCE↗

Thermoelectric Properties of TiNiSn Half Heusler Alloy Obtained by Rapid Solidification and Sintering

Thermoelectric TiNiSn-based half Heusler compound reveals high Seebeck coefficient and electrical conductivity, leading to high power factor. As a consequence of the solidification path, TiNiSn single phase cannot be obtained directly from the liquid phase. Thus, a long annealing step is needed to homogenize the alloy. In this work, we present a new processing route for half Heusler compound formation, combining arc melting of pure elements, rapid solidification of the molten alloy and sintering. Rapid solidification of the molten alloy allows to obtain almost single TiNiSn phase, limiting the formation of the primary TiNi{sub 2}Sn phase as a consequence of the deep undercooling of the liquid. The rapidly solidified alloy was ground to powder and sintered by open die pressing. As-sintered samples show a density around 95% of the theoretical value. Thermal cycling of the sintered samples shows evolution of the phases, suggesting that after sintering the sample is not in equilibrium yet. After the second thermal cycle thermoelectric properties become reproducible, indicating the attainment of the equilibrium. In conclusion, the proposed processing route allows to obtain dense TiNiSn in bulk form avoiding the time-consuming annealing step, typically used to homogenize this alloy after solidification.

36 MATERIALS SCIENCE↗

Layer-by-Layer Freezing of Nanoconfined Water

Abstract Nanoconfined water plays a pivotal role in a vast number of fields ranging from biological and materials sciences to catalysis, nanofluidics and geochemistry. Here, we report the freezing and melting behavior of water (D 2 O) nanoconfined in architected silica-based matrices including Vycor glass and mesoporous silica SBA-15 and SBA-16 with pore diameters ranging between 4–15 nm, which are investigated using differential scanning calorimetry and 2 H nuclear magnetic resonance spectroscopy. The results provide compelling evidence that the extreme dynamical heterogeneity of water molecules is preserved over distances as small as a few angstroms. Solidification progresses in a layer-by-layer fashion with a coexistence of liquid-like and solid-like dynamical fraction at all temperatures during the transition process. The previously reported fragile-to-strong dynamic transition in nanoconfined water is argued to be a direct consequence of the layer-by-layer solidification.

42 ENGINEERING↗

Assessment of Directionally Solidified Eutectic Sm–Fe(Co)–Ti Alloys as Permanent Magnet Materials

Sm–Fe–Ti and Sm–Fe0.8Co0.2–Ti alloys were prepared via arc-melting and directionally solidified on a water-cooled copper hearth. The as-solidified alloys featured cells of the Sm(Fe,Co,Ti)12–Ti(Fe,Co) 2+δ –(α-Fe) lamellar eutectic. The lamellae of Sm(Fe,Co,Ti)12 phase with a crystal structure of the ThMn12 type were less than 0.2 μm thick, and had their [001] easy-magnetization directions oriented along the temperature gradient of the solidification. The eutectic microstructure led to an increased coercivity, especially in the Co-added alloys. Below 250 °C, this coercivity was found not to vary much with temperature with a temperature coefficient of -0.18 %/°C. However, the modest absolute values, reaching only 0.7 kOe, are insufficient for utilization of the directionally solidified alloys as anisotropic permanent magnets.

36 MATERIALS SCIENCE↗

Isothermal solidification for high-entropy alloy synthesis

Kinetically trapping the high-temperature states through rapid cooling solidification is widely used for the synthesis of high-entropy alloys (HEAs), especially those with intrinsically immiscible elemental combinations. However, strategies need to be developed to overcome the fundamental limitations of rapid cooling solidification in controlling the crystallinity, structure and morphology of HEAs. Here, in this study, we introduce an isothermal solidification strategy for the synthesis of HEAs by rapidly altering the metal alloy composition through liquid–liquid interface reactions at low temperatures, for example, from 25 °C to 80 °C. We use gallium (Ga)-based metal as the sacrificial reagent and mixing medium. By directing the reactions to the interfaces between the Ga-based liquid metal and an aqueous metal ion solution, the foreign metal ions can be reduced at the interfaces and incorporated into the liquid metal quickly. HEAs with various crystallinity (single crystal, mesocrystal, polycrystal and amorphous), morphology (zero, two and three dimensions) and compositions can be achieved through the isothermal solidification. Ga can be completely consumed, resulting in Ga-free HEAs. If desired, Ga can be one of the metal elements in the final products. In situ liquid phase transmission electron microscopy (TEM) studies and theoretical analysis show the isothermal solidification mechanisms. Our direct observations show the enhanced mixing of liquid metal elements and the solidification process with fluctuating nucleation dynamics. The isothermal solidification marks a powerful strategy for HEA synthesis through an unexplored pathway of kinetically trapping the high-entropy states.

Zhang, Qiubo [Lawrence Berkeley National Laborator↗

Mechanical Behavior of Additively Manufactured Molybdenum and Fabrication of Microtextured Composites

Refractory metals are a class of high-melting-temperature materials suitable for use in extreme environment applications. Interestingly, during additive manufacturing many pure refractory metals exhibit a switch from (001) to (111) build direction fiber preference with increasing surface energy density. Here we exploit this solidification physics to fabricate material with “mesoscale composite” engineered structures consisting of features with contrasting (001) and (111) build direction microtextures. Separately, elevated temperature tensile testing of EBM fabricated material with a randomized distribution of mixed (001)/(111)-fiber grains is shown to exhibit excellent properties. These results are utilized to build a crystal plasticity model for evaluating the local inelastic response of the composite mesoscale structures. Analysis of printed microstructures and microstructure-scale simulations indicate that both macro-scale and localized material behavior may be tailored. This strategy can be potentially used to synthesize materials with optimized performance for high-temperature applications.

36 MATERIALS SCIENCE↗

Localized Strain Analysis of Ce- and Mg-Treated Cast Iron under Uniaxial Compression

Cast iron exhibits a wide range of mechanical properties, depending on its microstructural features. The microstructure of cast iron consists of several microconstituents with different elastic-plastic behavior, making the strain non-uniform across the bulk material. To understand the individual effects of these microconstituents on the overall mechanical behavior, local strain analysis using digital image correlation analysis was carried out. Samples with two different compositions (varying cerium, magnesium and silicon) were processed at different solidification velocities in a Bridgman furnace. Sections of the directionally solidified samples were loaded under uniaxial compression to measure global and local strain behavior. Despite the variability of the microstructure, the stress–strain curves obtained by digital image correlation (DIC) were found to react in a well-controlled way to changes in solidification velocity. It was observed that high-strain failure (greater than 15%) was accompanied by local straining of the softer ferritic phase, but during low-strain failure, local straining was not prominent. Higher nodularities, due to higher solidification velocities, raised the compressive strength without affecting the toughness significantly. Higher percentages of carbides led to higher compressive strengths with corresponding losses in ductility. The continuity of the matrix was also found to play an important role in the behavior during compression.

ductile failure↗

Selective laser melting of Co-29Cr-6Mo alloy with laser power 180–360 W: Cellular growth, intercellular spacing and the related thermal condition

Highlights: • Increasing laser power increases the track size but not the track shape significantly. • Solidification mode and texture are similar over the range of laser power used. • Intercellular spacing is not affected by laser power but decreases slightly with growth angle. • Thermal gradient and cooling rate have been estimated to be ~ 2 × 10{sup 7} K/m and ~ 2 × 10{sup 6} K/s, respectively. - Abstract: A feature of solidification during selective laser melting (SLM) is cellular growth. Thus, how growth direction and cell size may be affected and possibly be controlled by SLM parameters are important to be understood. Furthermore, intercellular spacing (λ{sub 1}) is suggestive of the thermal condition during solidification which needs to be known for advancing the understanding of SLM. In this work, grain solidification orientation and λ{sub 1} of a Co-Cr-Mo alloy produced by SLM over a range of laser power (P = 180–360 W) with other parameters kept unchanged have been evaluated. It has been found that the overall preferred growth of cellular solidification is not significantly affected by P. This is because, over the range of P values used, the shape of track did not change sufficiently to result in a significant variation of growth direction during epitaxial growth. It has also been found that P does not affect λ{sub 1}. This suggests, since growth rate (R) relates to scan speed (v) which is unchanged, P does not significantly affect the temperature gradient of the solidification front (G). From the measured λ{sub 1} and estimated R, G and thus cooling rate ( T-dot ) can be estimated following the commonly used primary arm spacing model. The estimated G and T-dot which could not be directly measured will be compared with those predicted by simulation and the estimated T-dot will also be compared with those determined by using an emperical relationship from literature.

36 MATERIALS SCIENCE↗

Interaction between laser radiation and metallic powder of 316L austenitic steel during selective laser melting

Highlights: • Single and multiple tracks on a loose bulk powder substrate were generated. • Understanding of the microstructure development during SLM was achieved. • Single tracks reveal a nearly symmetrical crystallography with elongated grains. • Multiple tracks show elongated grains perpendicular to the build direction. - Abstract: During selective laser melting (SLM), a complex heat state develops that leads to a characteristic crystallography and microstructure of the processed materials. Depending on the geometry of the processed part, most scan tracks of a new layer, so-called hatches, are located above a dense substrate or already solidified structures whereas others are located above loose powder. This is, inter alia, the case for overhanging structures. Attributable to the lower thermal conductivity of loose powder, temperature gradients and cooling rates of the melt pool differentiate in these areas, resulting in a different microstructural build-up. In this work, the microstructure and the crystallographic orientation of grade 316L austenitic stainless steel processed by SLM was investigated to understand the interaction between the laser radiation and the metallic powder during SLM-processing and to investigate the remelting of a track on a previous SLM-densified track. Single and multiple tracks on a loose bulk powder substrate, as well as single tracks on a dense substrate plate, were generated. A parameter study revealed that high energy densities are necessary to build continuous tracks on a loose bulk powder substrate. In addition, the amount of adhered particles, which are sintered on the fully melted and solidified tracks, is determined in comparison to the melted powder because the sintered particles strongly influence the surface roughness. To understand the microstructure development and, particularly, the influence of adjacent hatches during SLM-processing, investigations on the resulting microstructure and crystallographic orientation of a single track and two connected multiple tracks were carried out. During SLM processing of the tracks, the substrate plate and the solidified structures influence the temperature gradient and cooling rate of the melt pool, thus directionally solidified and elongated grains occur. Furthermore, the solidification is characterized by an epitaxial growth due to a distinct thermal gradient between the melt pool and the surrounding elements.

36 MATERIALS SCIENCE↗

Enabling 6.5% Silicon Electric Steel for Motor Application

Compared to the most widely used 3.2% Si steel, 6.5% Si steel exhibits superior magnetic and electric properties and promises an improvement to the efficiency and power density of electrical machines and transformers. However, due to the heterogeneous formation of B2 and D03 ordered phases, 6.5% Si steel is too brittle to be produced using the traditional cold roll process. And the thin sheet obtained via Si vapor deposition followed by diffusion process is difficult to stamp and assemble. At Iowa State University and Ames Laboratory, a novel process was developed to enable the cost-effective deployment of this brittle materials. The process is developed based on the observation that the deleterious ordered phases can be fully or partially suppressed by rapid cooling. The innovation lies in the production of small ductile flakes using rapid solidification and the consolidation of the obtained flakes directly into a fully dense part with near-net-shape.

36 MATERIALS SCIENCE↗

Interaction of Strain Refined Precipitates and Recrystallized Grains in Nb-Ti Microalloyed Steel during Continuous Casting, Hot-Core Heavy Reduction Rolling, and Reheating Process

Hot-core heavy reduction rolling (HHR{sup 2}) is an energy-saving process that directly rolls continuously cast slabs at the end of solidification that have a large temperature gradient. Here, we elucidated the interaction of strain refined precipitates and recrystallized grains in Nb-Ti microalloyed steel during continuous casting, hot-core heavy reduction rolling, and reheating process. Furthermore, theoretical models were established to calculate recrystallization driving force and pinning force at temperatures in the range of 850-1300 °C by a two-stage interrupted compression test using a Gleeble-3800 thermomechanical simulator. The study indicated that a random dispersion of strain refined precipitates with a size range of ~ 6-10 nm was obtained in the hot-core heavy reduction rolled slab, which was different from the coarse and uneven distribution of precipitates in a conventional slab. Upon reheating, the austenite grains in the hot-core heavy reduction rolled slab were significantly refined and evenly distributed along the thickness direction. This is attributed to the random dispersion of strain refined precipitates formed in the HHR{sup 2} process.

36 MATERIALS SCIENCE↗

Experimental Investigation of a Phase Change Material Charged Finned-Tube Heat Exchanger

Understanding different thermal performance aspects of phase change material heat exchangers (PCM-HX) is critical for designing future energy-efficient thermal energy storage systems. This paper presents an experimental performance analysis of a vertically oriented annular finned-tube PCM-HX in a cylindrical container tested under six different melting and solidification test conditions, varied by heat transfer fluid’s (HTF) inlet temperatures and flow directions. The PCM-HX structure with 20 evenly spaced fins was 3D printed in aluminum, and the PCM-HX container was 285 mm in height. The PCM-HX average porosity was 89.7%, where the PCM mass was 246.4 g. Water served as the HTF, and a PCM with a nominal phase change temperature of 35 °C was selected. Instead of opaque conventional insulation sheets, a combination of air-and-argon-filled see-through insulation cylinders was assembled with the PCM-HX to visualize the phase-change phenomena, while minimizing the uncertainties due to heat loss. In total, there were 78 T-type thermocouples installed in the test section which allows a more precise assessment of thermal mass and heat loss, which are often neglected in similar studies found in the literature. We validated the reliability of the test facility as the repeated test results had negligible deviations under the same test conditions. The energy balances between the estimated theoretical and experimentally calculated PCM storage, considering heat loss and thermal mass, were within ±9% deviation for all test conditions. From the experimental investigations, we made several following observations. It was found that the melting pattern of the finned-tube PCM-HX with small gaps between the container wall and the fins was largely affected by the HTF flow directions, unlike the typical straight annular tube PCM-HX. For effective charging and discharging processes, a combination of upward melting and downward solidification is recommended to shorten the test duration. However, an upward solidification should be considered to minimize the cavity formation between the fins caused by the PCM volume contraction during the solidification process.

25 ENERGY STORAGE↗

Enabling On-Demand Aerospace Component Manufacturing: Topology Optimization of GE Engine Bracket and Fabrication Using Metal FFF

Additive Manufacturing (AM) offers advantages over conventional manufacturing processes, particularly by reducing the number of parts produced through multistage combined technologies, but these often result in low manufacturing yields or require post-processing. AM facilitates the production of complex geometries with fine features, overhangs, and lattice structures. For instance, Laser Powder Bed Fusion (LPBF) technology enables the fabrication of intricate parts that can be easily post-processed by removing residual powder. Laser powder bed AM technologies are widely discussed in the literature due to their design freedom in creating complex geometries, with and without the need for support generation. However, rapid solidification due to a thermal gradient in the build direction, which leads to the formation of columnar grains and warpage, is one of the challenges. To address this challenge, we propose layer-by-layer metal FFF technology, followed by the debinding and sintering process, as an alternative to powder- and laser-based approaches. Furthermore, design for additive manufacturing (DfAM) principles are discussed to minimize the need for support generation and enable easy post-processing, thereby improving surface finish to meet high tolerances in fabricating components for aerospace and healthcare applications.

Singh, Abhishek [University of Michigan, Ann Arbor↗

Unraveling compacted graphite evolution during solidification of cast iron using in-situ synchrotron X-ray tomography

In spite of many years of research, the physical phenomena leading to the evolution of compacted graphite (CG) during solidification is still not fully understood. In particular, it is unknown how highly branched CG aggregates form and evolve in the semi-solid, and how local microstructural variations at micrometer length scale affect this growth process. We present here the first time-resolved synchrotron tomography combined with a bespoke high-temperature environmental cell that allows direct observation of the evolution of CG and relates this dynamic process to the local surrounding microstructures in a cast iron sample during repeated melting and solidification. Distinct processes are identified for the formation of CG involving the nucleation, growth, development of branches and interconnection of graphite particles, ultimately evolving into highly branched graphite aggregates with large sizes and low sphericities. CG is found to nucleate with a spheroidal or a plate-like shape, developing branches induced by high carbon concentration, e.g. thin melt channels. Additionally, CG grows much faster than spheroidal graphite during subsequent cooling in solid state. The direct visualization of the dynamic solidification process provides unprecedented new insights into formation mechanisms of CG and correlating factors such as local microstructural variations, and guides the development of CG iron solidification models.

36 MATERIALS SCIENCE↗

Microstructural and Mechanical Characterization of Directionally Solidified Conventional and Nb-Modified Mar-M247 Superalloy

This study analyzes the effects of replacing Ta by Nb (at.% basis) in the phase transformation temperatures, Scheil solidification behavior, and microstructural mechanical features of a Nb-modified as well as conventional Mar-M247 superalloys. Both alloys were directionally solidified at a withdrawal rate of 18 cm/h under a thermal gradient of about 80 °C/cm. DSC results were compared to thermodynamic simulations of phase transformation temperatures and showed a good correlation. The replacement of Ta by Nb has not altered the solidification path of Mar-M247, keeping the sequence L → L + γ → L + γ + MC → L + γ + MC + γ/γ′ eutectic. Due to the segregation of Hf and Zr to the very last liquid to solidify, a low melting point γ/Ni{sub 5}(Hf,Zr) constituent was observed. The as-solidified microstructures of both Mar-M247(Nb) and Mar-M247 were constituted of columnar dendrites of gamma matrix (γ) phase with cuboidal gamma-prime (γ′) precipitates. In addition, γ/γ′-eutectic was observed in the interdendritic region along with MC carbides in blocky, script (blocky dendritic), needle-like and fine nodular morphologies. Both alloys contained about 1.5 vol.% of MC carbides. The MC carbides in Mar-M247(Nb) and Mar-M247 are, respectively, Nb-rich and Ta-rich, with only a limited amount of Hf being detected in the MC phase. The yield stress of Nb-modified Mar-M247 showed higher values up to 750 °C. For higher temperatures, above 800 °C, a conventional Mar-M247 presented a higher value of yield stress.

36 MATERIALS SCIENCE↗

Crack mitigation in additively manufactured AlCrFe 2 Ni 2 high-entropy alloys through engineering phase transformation pathway

The far-from-equilibrium solidification during additive manufacturing often creates large residual stresses that induce solid-state cracking. Here we present a strategy to suppress solid-state cracking in an additively manufactured AlCrFe 2 Ni 2 high-entropy alloy via engineering phase transformation pathway. We investigate the solidification microstructures formed during laser powder-bed fusion and directed energy deposition, encompassing a broad range of cooling rates. At high cooling rates (10 4 –10 6 K/s), we observe a single-phase BCC/B2 microstructure that is susceptible to solid-state cracking. At low cooling rates (10 2 –10 4 K/s), FCC phase precipitates out from the BCC/B2 matrix, resulting in enhanced ductility (~10 %) and resistance to solid-state cracking. Site-specific residual stress/strain analysis reveals that the ductile FCC phase can largely accommodate residual stresses, a feature which helps relieve residual strains within the BCC/B2 phase to prevent cracking. Our work underscores the value of exploiting the toolbox of phase transformation pathway engineering for material design during additive manufacturing.

36 MATERIALS SCIENCE↗

Orientation-controlled crystallization of γ-glycine films with enhanced piezoelectricity

Glycine, the simplest amino acid, is considered a promising functional biomaterial owing to its excellent biocompatibility and strong out-of-plane piezoelectricity. Practical applications require glycine films to be manufactured with their strong piezoelectric polar $\langle$001$\rangle$ direction aligned with the film thickness. Based on the recently-developed solidification approach of a polyvinyl alcohol (PVA) and glycine aqueous solution, in this work, we demonstrate that the crystal orientation of the as-synthesized film is determined by the orientation of glycine crystal nuclei. By controlling the local nucleation kinetics via surface curvature tuning, here we shifted the nucleation site from the edge to the middle of the liquid film, and thereby aligned the $\langle$001$\rangle$ direction vertically. As a result, the PVA–glycine–PVA sandwich film exhibits the highest average piezoelectric coefficient d 33 of 6.13 ± 1.13 pC N –1 . This work demonstrates a promising kinetic approach to achieve crystallization and property control in a scalable biocrystal manufacturing process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Process-microstructure relationship of laser processed thermoelectric material Bi2Te3

Additive manufacturing allows fabrication of custom-shaped thermoelectric materials while minimizing waste, reducing processing steps, and maximizing integration compared to conventional methods. Establishing the process-structure-property relationship of laser additive manufactured thermoelectric materials facilitates enhanced process control and thermoelectric performance. This research focuses on laser processing of bismuth telluride (Bi 2 Te 3 ), a well-established thermoelectric material for low temperature applications. Single melt tracks under various parameters (laser power, scan speed and number of scans) were processed on Bi 2 Te 3 powder compacts. A detailed analysis of the transition in the melting mode, grain growth, balling formation, and elemental composition is provided. Rapid melting and solidification of Bi 2 Te 3 resulted in fine-grained microstructure with preferential grain growth along the direction of the temperature gradient. Experimental results were corroborated with simulations for melt pool dimensions as well as grain morphology transitions resulting from the relationship between temperature gradient and solidification rate. Samples processed at 25 W, 350 mm/s with 5 scans resulted in minimized balling and porosity, along with columnar grains having a high density of dislocations.

Oztan, Cagri↗