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At least 271 records · Page 15

Spatially resolved phase transformation mapping in 410 stainless steel during additive manufacturing visualized via real-time infrared data

Here, in this study, we demonstrate that spatially resolved cooling curves derived from real-time infrared (IR) thermography during additive manufacturing (AM) can capture spatial variations in phase transformation temperatures through cooling curve analysis (CCA). Using this approach, we show that during laser hot-wire deposition of 410 stainless steel (410SS), the martensite start temperature (M s ) evolves dynamically throughout the build. The M s temperature is spatially nonuniform, ranging from 185 °C to 348 °C, with the lowest values toward the build center and higher values toward the upper region of the deposit. In the lower portion of the build, no M s inflection is detected via CCA, consistent with transformation occurring earlier during thermal cycling followed by tempering during subsequent thermal cycles. These trends in M s are corroborated by characterizing the microstructure by electron backscatter diffraction (EBSD). Traditionally, M s is assumed to be constant, and a single interpass temperature is applied during both deposition and residual stress modeling. Our results demonstrate that IR-derived cooling curves provide a route to spatially and temporally resolved transformation temperature tracking for dynamic interpass control and improved residual-stress modeling.

Additive manufacturing↗

Deformation behavior of a Co-Cr-Fe-Ni-Mo medium-entropy alloy at extremely low temperatures

In this work, we report the mechanical and microstructural characteristics of a medium-entropy alloy, Co 17.5 Cr 12.5 Fe 55 Ni 10 Mo 5 (atomic percent, at%) at cryogenic temperatures, down to a record low temperature of 0.5 K. The alloy exhibits excellent strength and ductility combined with a high strain-hardening rate in the entire temperature range investigated. Its property profile, including the yield strength, ultimate tensile strength, strain hardening capability, and absorbed mechanical energy, is better than those of most alloys and HEAs used in cryogenics. Within the interval of extremely low temperatures considered (0.5–4.2 K), the alloy exhibits several unusual features, including anomalies of the temperature dependence of the yield strength and tensile ductility, discontinuous plastic deformation (DPF), and a change in the propensity for the deformation-induced martensitic transformation. While the occurrence of these effects in the same temperature interval may be fortuitous, we hypothesize that they are interrelated and provide a tentative explanation of the observed phenomena on this basis.

36 MATERIALS SCIENCE↗

Orientation dependence of the effect of short-range ordering on the plastic deformation of a medium entropy alloy

Multi-principal-element alloys (also known as medium and high entropy alloys) offer a much larger and richer design space than conventional alloys, providing opportunities for discovering new functionalities and their governing physics. Some of these alloys exhibit an outstanding combination of high strength and ductility, linked to the activation of various deformation modes triggered by low-energy stacking faults. However, a pressing question remains: Is the plasticity of medium- and high-entropy alloys governed only by stacking fault energy, or does atomic short-range order (SRO) play a role? Here, to answer this, we investigated how SRO affects the deformation in single-crystalline NiCoCr, with previous contradictory findings. First, we established unique experimental evidence for SRO formation in bulk single crystals using high-energy synchrotron transmission X-Ray Diffraction. By tuning the degree of SRO by aging at high temperatures, twinning density and strain-induced martensitic phase transformation can be significantly increased in the [110] and [111] orientations under tension, increasing the tensile ductility; yet, no increase was observed along the [001] orientation due to lack of TWinning-Induced Plasticity (TWIP) or TRansformation-Induced Plasticity (TRIP), indicating a strong crystallographic orientation dependence. Our first-principles thermodynamic calculations unequivocally show SRO exists and governs the observed microstructural evolution and deformation hardening behavior. Here we find direct proof that SRO triggers a simultaneous TWIP and TRIP in NiCoCr, a rare microstructural evolution path. Our findings establish that the interplay of SRO and plasticity could be exploited to alter deformation modes and yield unprecedented mechanical response in medium- and high-entropy alloys.

36 MATERIALS SCIENCE↗

Understanding the asymmetric orientations and stress states in polycrystalline NiTi SMA by in-situ synchrotron-based high-energy X-ray diffraction

The stress-induced martensite transformations (SIMTs) dramatically affect the recoverable strain and mechanical response of polycrystalline NiTi. An in-depth understanding of the propagation manner and orientation preference of SIMTs is therefore crucial. Here, in this work, we present a unique asymmetric anisotropy of SIMTs and lattice strains induced by Lüders-type deformation in polycrystalline NiTi, achieved through a combination of in-situ synchrotron X-ray diffraction and uniaxial tensile loading and unloading experiments. Our experimental findings reveal that in polycrystalline NiTi under uniaxial deformation, the asymmetry of SIMTs is attributed to the inhomogeneous strain field caused by the Lüders-type mechanism. The asymmetrical SIMT starts with the forward Lüder band and disappears along with the backward Lüder band. The austenite with the favored orientation of $\langle$110$\rangle$ A //loading direction (LD) transformed and recovered back at a higher rate compared to other orientations during both loading and unloading.

36 MATERIALS SCIENCE↗

Influence of fatigue precracking and specimen size on Master Curve fracture toughness measurements of EUROFER97 and F82H steels

EUROFER97 and F82H steels are two leading reduced-activation ferritic-martensitic (RAFM) steels for fusion first wall and blanket applications. Exposure to the harsh environment of fusion reactors can result in severe degradation of fracture toughness. Thus, the post-irradiation evaluation of fracture toughness is critical for understanding the material behavior. Due to the space constraints of irradiation facilities and challenges in controlling a uniform irradiation condition for large size specimens, the development of small specimen test techniques (SSTT) is indispensable to evaluate the performance of irradiated materials. In this study, we evaluated specimen size effects on the Master Curve fracture toughness of EUROFER97 and F82H steels. A wide variety of specimens, including 0.5 T compact tension (C(T)) specimens, 0.16 T mini-compact tension (miniC(T)) specimens, and 1.65 mm miniature bend bar specimens, were tested. The testing methodology was based on the Master Curve method in the ASTM E1921 standard. No specimen size effect was observed in 0.5 T C(T) and 0.16 T miniC(T) specimens on the Master Curve reference temperature T0, while 1.65 mm miniature bend bar specimens yielded a higher T 0Q . A strong effect of fatigue precracking on T 0 for 0.5 T C(T) and 0.16 T miniC(T) specimens was observed, such that testing on specimens with skewed fatigue precrack fronts resulted in lower T 0 than for specimens with ASTM standard qualified straight fatigue precrack fronts. The results highlight the importance of experimental quality control in developing SSTT for Master Curve fracture toughness testing. Lastly, we also evaluated and provided recommendations on the minimum number of specimens needed for each specimen type for yielding reliable T 0Q values.

36 MATERIALS SCIENCE↗

Rapid tempering to enhance dynamic performance of high and ultra-high strength steels

This study employed rapid, short-time duration (1 s) tempering to improve the dynamic performance of high-strength steel (HSS) and ultra-high-strength steel (UHSS), compared to quenched and conventionally (1800 s) tempered microstructures. Rapid tempering significantly improved the Charpy toughness of both steels compared to the conventionally tempered condition at an equivalent tempering parameter (TP) or hardness level. For conventionally tempered conditions, tempered martensite embrittlement was observed within the tempering temperature range of 200–400 °C, whereas rapid tempering exhibited increased Charpy toughness with increasing tempering temperature across all tempering conditions. Dynamic compression experiments indicated that rapid tempering led to improved ductility compared to the conventionally tempered condition at an equivalent TP. This work shows that the same rapid tempering strategy used for HSS is directly transferable to a higher-carbon UHSS and provides the first systematic evidence of improved strength-ductility combinations and cracking resistance under dynamic compression, supported by Kolsky bar experiments.

36 MATERIALS SCIENCE↗

NMR study of Ni 50+x ⁢Ti 50-x strain glasses

Here, we studied Ni 50+x ⁢Ti 50-x with compositions up to x = 2, performing 47 Ti and 49 Ti nuclear magnetic resonance (NMR) measurements from 4 to 400 K. For large x in this system, a strain glass appears in which frozen ferroelastic nanodomains replace the displacive martensite structural transition. Here, we demonstrate that NMR can provide an extremely effective probe of the strain-glass freezing process, with large changes in NMR line shape due to the effects of random strains which become motionally narrowed at high temperatures. At the same time with high-resolution x-ray diffraction we confirm the lack of structural changes in x ≥ 1.2 samples, while we show that there is little change in the electronic behavior across the strain-glass freezing temperature. NMR spin-lattice relaxation time (T 1 ) measurements provide a further measure of the dynamics of the freezing process, and indicate a predominantly thermally activated behavior both above and below the strain-glass freezing temperature. We show that the strain-glass results are consistent with a very small density of critically divergent domains undergoing a Vogel-Fulcher-type freezing process, coexisting with domains exhibiting faster dynamics and stronger pinning.

36 MATERIALS SCIENCE↗

Crystallographic map: A general lattice and basis formalism enabling efficient and discretized exploration of crystallographic phase space

Three-dimensional lattices are fundamental to solid-state physics. The description of a lattice with an atomic basis constitutes the necessary information to predict solid phase properties and evolution. Here, we present an algorithm for systematically exploring crystallographic phase space. Further, coupled with ab initio techniques, such as density functional theory, this algorithm offers an approach for exploring and tuning materials behavior, with a broad range of potential applications: particularly martensitic phase transformations and materials stability.

36 MATERIALS SCIENCE↗

Machine-Learning Microstructure for Inverse Material Design

Metallurgy and material design have thousands of years’ history and have played a critical role in the civilization process of humankind. The traditional trial-and-error method has been unprecedentedly challenged in the modern era when the number of components and phases in novel alloys keeps increasing, with high-entropy alloys as the representative. New opportunities emerge for alloy design in the artificial intelligence era. Here a successful machine-learning (ML) method is developed to identify the microstructure images with eye-challenging morphology for a number of martensitic and ferritic steels. Assisted by it, a new neural-network method is proposed for the inverse design of alloys with 20 components, which can accelerate the design process based on microstructure. The method is also readily applied to other material systems given sufficient microstructure images. This work lays the foundation for inverse alloy design based on microstructure images with extremely similar features.

36 MATERIALS SCIENCE↗

Rapid Phase Transitions of Thermotropic Glycolipid Quasicrystal and Frank‐Kasper Mesophases: A Mechanistic Rosetta Stone

Abstract Experimental results are presented that serve to lower the barrier for developing the science and technology of non‐classical thermotropic glycolipid mesophases, which now include dodecagonal quasicrystal (DDQC) and Frank–Kasper (FK) A15 and σ mesophases that can be produced under mild conditions from a versatile class of sugar‐polyolefin conjugates. By employing “alloys” comprised of mono‐ and disaccharide‐polyolefin conjugates, and optionally with vitamin E as a small molecule phase modulator, we report the spontaneous formation of stable A15 mesophases at ambient temperature. We further document a rich thermotropic phase map that includes DDQC, A15, and σ mesophases of tunable periodicity that are connected through rapid thermotropic phase transitions as a function of increasing temperature in the order: liquid‐like packing (LLP)→DDQC → A15→σ→ disorder. This first direct observation of a rapid thermotropic A15→σ phase transition provides support for a diffusionless martensitic process proceeding through strain‐induced introduction of planar defects into the A15 lattice.

36 MATERIALS SCIENCE↗

Rapid Phase Transitions of Thermotropic Glycolipid Quasicrystal and Frank‐Kasper Mesophases: A Mechanistic Rosetta Stone

Abstract Experimental results are presented that serve to lower the barrier for developing the science and technology of non‐classical thermotropic glycolipid mesophases, which now include dodecagonal quasicrystal (DDQC) and Frank–Kasper (FK) A15 and σ mesophases that can be produced under mild conditions from a versatile class of sugar‐polyolefin conjugates. By employing “alloys” comprised of mono‐ and disaccharide‐polyolefin conjugates, and optionally with vitamin E as a small molecule phase modulator, we report the spontaneous formation of stable A15 mesophases at ambient temperature. We further document a rich thermotropic phase map that includes DDQC, A15, and σ mesophases of tunable periodicity that are connected through rapid thermotropic phase transitions as a function of increasing temperature in the order: liquid‐like packing (LLP)→DDQC → A15→σ→ disorder. This first direct observation of a rapid thermotropic A15→σ phase transition provides support for a diffusionless martensitic process proceeding through strain‐induced introduction of planar defects into the A15 lattice.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Review and construction of interatomic potentials for molecular dynamics studies of hydrogen embrittlement in Fe─C based steels

Abstract Reducing hydrogen embrittlement in the low‐cost Fe─C based steels have the potential to significantly impact the development of hydrogen energy technologies. Molecular dynamics studies of hydrogen interactions with Fe─C steels provide fundamental information about the behavior of hydrogen at microstructural length scales, although such studies have not been performed due to the lack of an Fe─C─H ternary interatomic potential. In this work, the literature on interatomic potentials related to the Fe─C─H systems are reviewed with the aim of constructing an Fe─C─H potential from the published binary potentials. We found that Fe─C, Fe─H, and C─H bond order potentials exist and can be combined to construct an Fe─C─H ternary potential. Therefore, we constructed two such Fe─C─H potentials and demonstrate that these ternary potentials can reasonably capture hydrogen effects on deformation characteristics and deformation mechanisms for a variety of microstructural variations of the Fe─C steels, including martensite that results from γ to α phase transformation, and pearlite that results from the eutectic formation of the Fe 3 C cementite compound.

Zhou, Xiaowang↗

Quantifying adherence of oxide scales on steels exposed to high temperature and pressure steam

Oxide scale exfoliation is a major concern in fossil fuel power generation because it can cause tube blockages and erode valves and steam turbine components downstream. There is still considerable scientific and commercial interest to improve the mechanistic understanding of oxide failures by developing models to predict exfoliation and the extent of tube blockage as a function of operating conditions and component geometries. Tensile testing inside a scanning electron microscope was conducted on ferritic–martensitic and austenitic steel specimens with the steam side (Fe,Cr)-rich oxides grown after exposures for up to 1000 h in steam with ~100 ppb O 2 at 276 bar and 550°C. Multiple oxide layer cracks and delamination events were observed and analyzed in detail during the tests. Results from the testing agreed well with earlier observations that had identified the failure location at the outer–inner oxide layer for all tested materials. Calculated adhesion energies identified the outer–inner oxide interface of alloy 347HFG as the weakest interface.

36 MATERIALS SCIENCE↗

Evaluation of coated steels in supercritical CO 2

The carburizing supercritical CO 2 (sCO 2 ) environment limits the use of lower cost steels in the lower temperature (450–650°C) portions of the sCO 2 Brayton cycle because of concerns about internal carburization and embrittlement. Results on a ferritic–martensitic steel and conventional and advanced austenitic steels at 450–650°C in 30 MPa sCO 2 with and without 1% O 2 and 0.1% H 2 O additions have indicated that sCO 2 environments will have lower maximum operating temperatures compared to steam plants. Pack Al and Cr coatings were evaluated at 650°C on T91 and 316H substrates and showed some benefit for up to 2000 h at 650°C, especially without impurities. However, characterization indicated Al 2 O 3 was not formed and Cr-rich carbides formed in the Cr coatings. With the addition of impurities in the sCO 2 , the coatings were less protective at 650°C. Subsequent exposures at 600°C in sCO 2 showed similar behavior. Postexposure evaluations included measuring the bulk C content and room temperature tensile properties. Finally, improvements were indicated but the tensile results were complicated by the high temperature pack coating process affecting the substrate properties.

36 MATERIALS SCIENCE↗

Austenite Formation and Manganese Partitioning during Double Soaking of an Ultralow Carbon Medium‐Manganese Steel

Double soaking (DS) is a thermal processing route intended to produce austenite–martensite microstructures in steels containing austenite‐stabilizing additions and consists of intercritical annealing (primary soaking), followed by heating and brief isothermal holding at an increased temperature (secondary soaking), and quenching. Herein, experimental dilatometry during DS of a medium‐manganese (Mn) steel with nominally 7 wt% Mn and an ultralow residual carbon concentration, in combination with phase‐field simulations of austenite formation during secondary soaking, is presented. The feasibility of maintaining heterogeneous Mn distributions during DS is demonstrated and insight is provided on the effects of the secondary soaking temperature and prior Mn distribution on the ferrite‐to‐austenite phase transformation during the secondary soaking portion of the DS treatment.

36 MATERIALS SCIENCE↗

Fatigue behavior of low-cost, non-spherical Ti-6Al-4V powder processed via laser powder bed fusion

Hydride-dehydride Ti-6Al-4V powder with particle size distribution of 75–175 μm were used to manufacture fatigue samples. Optimized processing parameters were used to maintain a relative density of >99.5% in the samples. Fatigue tests were carried out in R = σ min /σ max = -1 condition under stresses ranging from 150 to 500 MPa and the results were compared to samples that were additively manufactured using spherical powders. The fatigue lives were similar between the two types of powder; i.e., powder morphology has no effect on fatigue performance. However, the high surface roughness and martensitic microstructure resulting from the laser powder bed fusion process result in poor performance compared to samples machined from conventionally produced materials. In conclusion, crack initiation occurred consistently from surface defects because of high surface roughness of the additively manufactured parts.

36 MATERIALS SCIENCE↗

Multilayered microstructures with shape memory effects for vertical deployment

This paper presents a fabrication and characterization of multilayered microstructures with shape memory effects enabling large vertical deployment under electro-thermal actuation. Our previous research demonstrated vertical deployment of such microstructures by the effect of thermal mismatch. Development of equiatomic NiTi layers in the multilayered microstructure is investigated further for shape memory effects. Multilayered microstructures are built by sputtered NiTi layers and a lift-off process. Negative photoresist ma-N1420 enables clean lift-off of 500 nm thick NiTi layers by forming a significant undercut profile after development. The parametric study on co-sputter powers for Ti and Ni 50 Ti 50 targets suggests that 100 W RF on Ti target and 200 W DC on Ni 50 Ti 50 target can deposit Ni 49.62 Ti 50.38 layers. X-Ray Diffraction (XRD) and Atomic Force Microscopy (AFM) were used to study the crystal structures and surface topography of NiTi layers. XRD results of post-annealed Ni 49.62 Ti 50.38 layers show coexistence of austenite and martensitic phases at room temperature, suggesting that the transformation temperature of such NiTi layers should be approximate 20 °C. The surface topography of Ni 49.62 Ti 50.38 layers reveals substantial increase of surface roughness at ambient conditions after the annealing. Experimental verification of the multilayered microstructure for vertical deployment was carried out by Signatone Probe Station and Dual Scanning Electron Microscope/Focused Ion Beam (SEM/FIB) system. Finally, a vertical deployment of the two-dimensional (2D) multilayered microstructures for three-dimensional (3D) can be detected by applying a constant voltage of 0.04 V, and the expected 3D deployment displacement is enlarged from 2 μm to 10 μm by introducing the shape memory effect.

42 ENGINEERING↗