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At least 289 records · Page 16

Effects of doping, hydrostatic pressure, and thermal quenching on the phase transitions and magnetocaloric properties in Mn 1– x Co x NiGe

The effects of doping, hydrostatic pressure, and thermal quenching on the phase transitions and magnetocaloric properties of the Mn 1–x Co x NiGe system have been investigated. Cobalt doping on the Mn site shifted the martensitic structural transition toward lower temperature until it was ultimately absent, leaving only a magnetic transition from a ferromagnetic (FM) to a paramagnetic (PM) state in the high-temperature hexagonal phase. Co-occurrence of the magnetic and structural transitions to form a first-order magnetostructural transition (MST) from the FM orthorhombic to the PM hexagonal phase was observed in samples with 0.05 < x < 0.20. An additional antiferromagnetic–ferromagnetic-like transition was observed in the martensite phase for 0.05 < x < 0.10, which gradually vanished with increasing Co concentration (x > 0.10) or magnetic field (H > 0.5 T). The application of external hydrostatic pressure shifted the structural transition to lower temperature until an MST was formed in samples with x = 0.03 and 0.05, inducing large magnetic entropy changes up to –80.3 J kg –1 K –1 (x = 0.03) for a 7-T field change under 10.6-kbar pressure. Similar to the effects of the application of hydrostatic pressure, an MST was formed near room temperature in the sample with x = 0.03 by annealing at high temperature (1200 °C) followed by quenching, resulting in a large magnetic entropy change of –56.2 J kg –1 K –1 . Furthermore, these experimental results show that the application of pressure and thermal quenching, in addition to compositional variations, are effective methods to create magnetostructural transitions in the MnNiGe system, resulting in large magnetocaloric effects.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Assessment of minnealloy fabrication via three routes

Transformer cores exhibiting higher operating power and improved efficiency are of great interest to electrical utilities, industry, and the de-carbonization effort. Minnealloy, α″-Fe16(C,N)2, a martensite made only of iron, nitrogen, and carbon, has shown the largest saturation magnetization of any soft ferromagnet, 250 emu/g, and tunable magnetocrystalline anisotropy. Given this represents a significant increase in power transferred per cycle compared to legacy transformer core materials, we investigate three novel, industrially scalable routes for fabricating Minnealloy. The martensite phase content is investigated for each route. Vibrating sample magnetometry is used to investigate the change in saturation magnetization and coercivity with respect to the relative content of the desired phase and other iron, iron-nitride, and iron oxide phase impurities. The relationship between structure and magnetic properties of bulk α″-Fe16(C,N)2 is investigated using LDA, PBE, and PBEsol exchange-correlation functionals within the frameworks of Hubbard-corrected density functional theory (DFT+U).

36 MATERIALS SCIENCE↗

Large magnetocaloric effect in rapidly quenched Mn 50- x Co x Ni 40 In 10 nanomaterials

The effect of Co addition on magnetic hysteresis, martensitic transformation temperature, and magnetic entropy change of rapidly-quenched Mn 50- x Co x Ni 40 In 10 alloy nanomaterials has been investigated. The melt-spun Mn 50 Ni 40 In 10 sample exhibits a small magnetic hysteresis which is further reduced by Co doping as measured between 0 and 2 T. The martensitic transformation temperature increases linearly with the electron concentration in the alloy from 195 K for Mn 50 Ni 40 In 10 to 378 K for Mn 45 Co 5 Ni 40 In 10 . The Mn 47 Co 3 Ni 40 In 10 alloy, which has phase-transition temperature close to room temperature, exhibits a substantial peak entropy change of 29.7 J kg -1 K -1 at magnetic field change of 2 T. Our results demonstrate that Mn 47 Co 3 Ni 40 In 10 nanomaterial exhibits promising magnetocaloric properties for near-room-temperature magnetic refrigeration.

Physics↗

Controlling phase transitions in MnNiGe using thermal quenching and hydrostatic pressure

Here, the phase transitions in MnNiGe compounds were explored by manipulating the heat treatment conditions and through hydrostatic pressure application. As the quenching temperature increased, both the first-order martensitic structural transition temperatures and magnetic transition temperatures decreased relative to those in the slowly-cooled samples. When the samples were quenched from 1200 °C, the first-order martensitic structural transition temperature lowered by more than 200 K. The structural transitions also shifted to lower temperature with the application of hydrostatic pressure during measurement. Temperature-dependent x-ray diffraction results reveal that the changes of the cell parameters resulting from the structural transitions are nearly identical for all samples regardless of the extensive variation in their structural transition temperatures. In addition, neutron scattering measurements confirm the magnetic structure transition between simple and cycloidal spiral magnetic structures.

36 MATERIALS SCIENCE↗

In situ measurement of phase transformations and residual stress evolution during welding using spatially distributed fiber-optic strain sensors

Welding of high-strength steels can result in large tensile strains as the base metal and filler material cool from their molten state. To combat these large tensile strains, low-transformation-temperature (LTT) metal fillers have been proposed. These fillers undergo a martensitic phase transformation at a lower temperature which can ultimately reduce the tensile strain or can even introduce compressive strain adjacent to the weld metal. However, the process for optimizing the composition of the LTT material, as well as various weld parameters for each unique weld geometry, can be quite expensive, especially if the acceptance criterion requires using neutrons, x-ray beams, or destructive techniques to characterize residual stresses. This work describes a simple, low-cost method for quantifying residual stresses and phase transformations in situ during welding. Spatially distributed fiber-optic sensors were bonded to a cast iron plate, along with tack-welded thermocouples, to measure temperature and strain during multiple passes with LTT filler metals. Results show that the fiber-optic sensors can successfully resolve compressive strain adjacent to the weld region caused by the martensitic phase transformations in the LTT filler material.

47 OTHER INSTRUMENTATION↗

Fermi surface studies of the low-temperature structure of sodium

Sodium is the most abundant alkali-metal element and has one of the simplest electronic structures of any metal. At ambient conditions, sodium forms a body-centered-cubic lattice. However, during cooling, it undergoes a partial martensitic phase transition to a complex mixture of rhombohedral polytypes commencing from 36 K. Although the Fermi surface (FS) of bcc sodium has been extensively studied, not much attention has been given to the FS of the martensite structure. Here we report results for the Fermi surface and quantum oscillation (QO) frequencies of several energetically favorable crystal structures of Na at low temperature from first-principles calculations. Interestingly we find that despite drastic differences in the crystal structures of the candidate low-temperature phases of sodium, for all these phases the strongest quantum oscillation peak is centered at 28 kT. Our theoretical results are accompanied by experimental data of QO on a multigrain sodium sample at T = 0.3 K and B max = 18 T exhibiting a sharp peak at 28 kT, independent of the sample orientation. The persistence of this peak even in the presence of the structural transitions has an implication for using the quantum oscillations of polycrystalline sodium for high magnetic field calibration.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A novel physics-based and data-supported microstructure model for part-scale simulation of laser powder bed fusion of Ti-6Al-4V

The elasto-plastic material behavior, material strength and failure modes of metals fabricated by additive manufacturing technologies are significantly determined by the underlying process-specific microstructure evolution. In this work a novel physics-based and data-supported phenomenological microstructure model for Ti-6Al-4V is proposed that is suitable for the part-scale simulation of laser powder bed fusion processes. The model predicts spatially homogenized phase fractions of the most relevant microstructural species, namely the stable β-phase, the stable α s -phase as well as the metastable Martensite α m -phase, in a physically consistent manner. In particular, the modeled microstructure evolution, in form of diffusion-based and non-diffusional transformations, is a pure consequence of energy and mobility competitions among the different species, without the need for heuristic transformation criteria as often applied in existing models. The mathematically consistent formulation of the evolution equations in rate form renders the model suitable for the practically relevant scenario of temperature- or time-dependent diffusion coefficients, arbitrary temperature profiles, and multiple coexisting phases. Due to its physically motivated foundation, the proposed model requires only a minimal number of free parameters, which are determined in an inverse identification process considering a broad experimental data basis in form of time-temperature transformation diagrams. Subsequently, the predictive ability of the model is demonstrated by means of continuous cooling transformation diagrams, showing that experimentally observed characteristics such as critical cooling rates emerge naturally from the proposed microstructure model, instead of being enforced as heuristic transformation criteria. Eventually, the proposed model is exploited to predict the microstructure evolution for a realistic selective laser melting application scenario and for the cooling/quenching process of a Ti-6Al-4V cube of practically relevant size. Numerical results confirm experimental observations that Martensite is the dominating microstructure species in regimes of high cooling rates, e.g., due to highly localized heat sources or in near-surface domains, while a proper manipulation of the temperature field, e.g., by preheating the base-plate in selective laser melting, can suppress the formation of this metastable phase.

Inverse parameter identification↗

Multitask graph neural networks for elastoplastic response prediction in dual-phase polycrystals

Microstructure-sensitive prediction of elastoplastic response remains a recurring bottleneck in multiscale damage and fatigue modeling, where large ensembles of statistically distinct polycrystals are required to quantify variability and extreme-value behavior. In this work, we develop a multitask graph neural network (GNN) surrogate that maps dual-phase ferrite–martensite polycrystal microstructures to Statistical Volume Element (SVE)-level elastoplastic Quantities of Interest (QoIs). Each SVE is represented as a grain-adjacency graph, with node features encoding phase, geometry, and crystallographic orientation, and edge features encoding relative misorientation. A message-passing graph convolution generates node embeddings, which are pooled into a graph representation and passed to a multitask regression head that jointly predicts 10 scalar QoIs and vector-valued stress–strain responses in orthogonal loading directions across multiple martensite volume fractions and SVE sizes. Results show high accuracy for scalar QoIs and strong agreement for full stress–strain trajectories, with population envelopes reproducing both median behavior and finite-SVE variability across compositions and partition scales. A unified model trained on pooled volume-fraction data preserves most within-regime accuracy relative to regime-specific models while also capturing the broader cross-regime variation reflected in the pooled test set. Distributional comparisons further demonstrate that the surrogate preserves heterogeneity under SVE partitioning, enabling statistically consistent block-wise random-field construction for mesoscale analyses. Overall, the proposed grain-graph surrogate provides a practical pathway to accelerate ensemble-based studies of SVE-level constitutive variability in dual-phase polycrystals.

Crystal plasticity↗

Report on partially complete post-irradiation-examination of the INL samples

Ferritic-martensitic steels (NF616 and T91), and austenitic stainless steel 800H and its Grain Boundary Engineering (GBE)-treated version 800H-TMP (ThermoMechanical Processing) were irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and their microstructures and mechanical properties were characterized. Ferritic-martensitic steels were irradiated up to 8.16 dpa in the irradiation temperatures ranging from 241 °C to 447.5 °C. Selected 800H and 800H-TMP samples were also irradiated up to 9.12 dpa at 359°C to 431°C. Vickers hardness measurement, fractography, and microstructural characterization were performed on the selected samples in the LAMDA lab. Radiation-induced hardening of NF616 and T91 was observed in the hardness measurements which show ~37% to ~65% increases, depending on irradiation dose and irradiation temperature. Within the irradiation conditions studied in this work, samples with a higher dose had a higher hardness. All the tested alloy 800H and 800H-TMP in this work showed irradiation-hardening by ~96±7% to ~152±10%. Alloy 800HTMP tended to have slightly smaller irradiation-hardening than alloy 800H. The fractography of NF616 samples D2 (2.96 dpa at 291.5°C), D4 (5.91 dpa at 359°C), and D6 (8.16 dpa at 431°C) indicated loss of ductility with negligible necking for the sample D2, yet obvious ductile failure for samples D4 and D6. Fractography of alloy 800H samples N4 (7.27 dpa at 359°C), N5 (3.9 dpa at 451.5°C), and N6 (9.01 dpa at 431°C), and alloy 800H-TMP samples P4 (7.36 dpa at 359°C), P5 (3.95 dpa at 451.5°C), and P6 (9.12 dpa at 431°C) indicated that all samples failed in a ductile mode, with obvious necking. Dimples were observed where large Ti-containing particles were observed for the samples. TEM characterization was performed on alloy 800H (N4, N5, N6) and 800H-TMP (P4, P5 and P6). Accumulation of M23C6 precipitates at grain boundaries was observed in all samples, and the presence of Ti(C,N) precipitates at grain boundaries and in the matrix was observed in alloy 800H-TMP. M23C6 precipitates were found to have the cube-on-cube orientation relationship with the matrix. In addition, nanoscale Si-rich clusters were observed in the matrix of all samples. Atom probe tomography was conducted on the same samples, and their results are being analyzed to be integrated with the TEM results for a confident description of the clustering behavior. Due to the low irradiation temperature (up to 451.5°C), dislocation loops formed in all samples, with the density and the average size of dislocation loops in the order of 1022 – 1023 m-3 and 11.7 – 15.9 nm, respectively. The loop densities in alloy 800H were higher than that in alloy 800H-TMP under the same irradiation conditions. Further systematic data analyses, together with some complementary experiments, will be pursued for these samples to foster peer-reviewed journal article publications.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Investigating the Role of Defects in α-Pu Phase Transitions using Density Functional Theory

Before reaching its relatively low melting point of 913 K, plutonium undergoes six solid state phases: simple monoclinic alpha, body-centered monoclinic beta, face-centered orthorhombic gamma, face centered cubic delta, body-centered tetragonal delta-prime, and body-centered cubic epsilon phases. Due to their low symmetry, the monoclinic alpha and beta phases have not been studied extensively, however it has been previously hypothesized that the transition between alpha and beta is caused by defects in the lattices due to the incommensurate number of atoms. Additionally, the martensitic delta to alpha phase transformation in plutonium-gallium alloys induces an expanded alpha lattice known as alpha prime, most likely due to the insoluble gallium impurity atom. This work explores how defects such as plutonium interstitials and gallium interstitials and substitutionals may affect the alpha plutonium lattice, providing a better understanding of the mechanisms for the alpha-beta and martensitic phase transformations through density functional theory (DFT). Results indicate that plutonium interstitials within the alpha lattice induce beta features structurally and electronically, such as volume expansion and bonding changes, and gallium interstitials and substitutionals within the alpha lattice induce volume changes as observed experimentally in alpha prime.

36 MATERIALS SCIENCE↗

The Toughness of High-Strength Steel Weld Metals

Low-temperature phase transformation (LTPT) welding consumables are a new class of welding wires developed to mitigate hydrogen-induced cracking in the welding of high-strength steels without preheating or postweld heat treatment. LTPT weld metals have a high strength, but their toughness needs further investigation. LTPT weld metals predominately contain a martensite microstructure, which is necessary to achieve high strength; however, martensitic weld metals containing oxide inclusions have relatively poor toughness. For this study, three welding processes — gas metal arc welding (GMAW), gas tungsten arc welding (GTAW), and hot wire GTAW — were investigated. Optical microscopy, scanning electron microscopes, and transmission electron microscopes were employed for characterization. The role of the shielding gas in the formation of oxide inclusions in LTPT weld metals was investigated. The formation of oxide inclusions in the weld metals was related to the CO 2 in the shielding gas. When 100% Ar or a pure inert shielding gas mixture was used for all three welding processes, oxide inclusions were greatly reduced, and the weld metal toughness improved considerably, matching the base metal toughness. The mechanism by which inclusions promote fracture propagation in the weld metal was proposed.

36 MATERIALS SCIENCE↗

Tempering and Austempering of Double Soaked Medium Manganese Steels

The addition of a tempering or austempering step to the double soaking of a 0.14C–7.17Mn (wt pct) steel was investigated in the present contribution. The double soaking heat treatment is a two-step intercritical annealing heat treatment, which generates microstructures of athermal martensite, retained austenite and ferrite when applied to medium manganese steels. Microstructures following double soaking and (aus)tempering contained a combination of retained austenite, athermal or tempered martensite, and blocky or bainitic ferrite. X-ray diffraction, dilatometry and transmission Kikuchi diffraction were utilized to investigate microstructural changes which occurred during tempering or austempering. The resulting mechanical properties were measured using uniaxial tensile testing. The double soaking plus tempering heat treatment was shown to generate an ultimate tensile strength of 1,340 MPa in combination with 28 pct total elongation while the double soaking plus austempering heat treatment resulted in an ultimate tensile strength of 1,675 MPa and total elongation of 22 pct. Overall, both novel heat treatments produced a combination of strength and ductility desired for the third generation of advanced high strength steels.

36 MATERIALS SCIENCE↗

Microstructure and Mechanical Properties of Intercritically Treated Grade 91 Steel

Premature creep failures at the intercritical heat affected zone (ICHAZ) of creep-resistant steel weldments have been frequently reported. However, the creep degradation mechanism of different microstructure constituents in ICHAZ is complicated and needs further clarification. In this work, Grade 91 steel was intercritically heat-treated at a temperature (860 °C) between the critical temperatures AC1 and AC3, and a correlation between microstructure and mechanical properties of the heat-treated specimen was built. The effects of austenitization and tempering resulting from the intercritical treatment (IT) differentiated the local strain energies between the two microstructure constituents: newly transformed martensite (NTM) and over-tempered martensite (OTM). The formation of NTM grains led to a hardness increase from 247 HV0.5 in the base metal to 332 HV0.5 in the IT specimen. The ultimate tensile strength (UTS) increased from 739 MPa in the base metal to 1054 MPa in the IT specimen. Extensive growth of the OTM grains and rapid recovery of NTM grains took place simultaneously in the IT specimen during a typical tempering at 760 °C. These microstructure degradations led to a lowered hardness of 178 HV0.5, a reduced UTS of 596 MPa, and a poor creep resistance with a minimum creep strain rate of 0.49 %/h at 650 °C in an IT + tempering (ITT) specimen.

36 MATERIALS SCIENCE↗

Transient Microstructure Evolutions and Local Properties of Dual-Phase 980 MPa Grade Steel Via Friction Stir Spot Processing

Friction stir processing is a novel solid-state process to modify microstructures and their properties by intense, localized plastic deformation. However, little research has been reported for microstructure evolutions of advanced high-strength steels during the process. The present work focuses on the study of transient microstructure changes and local mechanical properties for friction stir spot processed dual-phase (DP) 980 MPa grade steel (DP980) under different peak temperatures. A pinless silicon nitride ceramic tool was used to produce relatively simple material deformation and flow near the tool. Friction stir spot processed steel samples were characterized by optical and electron microscopies. Furthermore, Vickers microhardness and nano-indentation measurements were used to study local mechanical properties for correlation with microstructures. A swallow layer of refined grains (<0.6 µm) was obtained with a low peak temperature (under 400 °C), whereas higher peak temperatures (>Ac 1 ) led to a change in grain size with different microstructures (fine-grained DP or martensite). Electron back-scattered diffraction characterizations revealed a large deformation in the as-received microstructures (mixture of ferrite and tempered martensite) induced by friction stir spot processing, leading to recrystallization and grain refinement around the stirred zone. Also, nano-indentation measurements showed a higher hardness than the hardness of the as-received DP980. Friction stir processing with different process conditions effectively changed microstructures and local mechanical properties.

36 MATERIALS SCIENCE↗

Impact of Hydrogen Combustion on the Oxidation-induced Degradation of Heavy-duty Diesel Engine Piston Materials

High temperature ferritic-martensitic steels are candidate materials for heavy-duty diesel engine pistons. The envisioned transition to hydrogen blended fuels is expected to alter the post-combustion atmosphere in the engines, primarily resulting in a higher water vapor content (> 20 vol%) and potentially higher exhaust gas temperatures. The oxidation resistance of existing and newly developed alloys will be a critical life-limiting mechanism under these conditions. In the present work, the oxidation behavior of candidate piston alloys was evaluated in air+10 vol.% H2O and air+30 vol.% H2O at 700°C. Thermal cyclic (1h cycle) exposures were conducted for two variants of commercial UNSS42200 ferritic-martensitic steel and two developmental alloy steels for up to 300h. The developmental alloys each have similar compositions but with one containing elevated Cu levels of 3 wt.%, A significant reduction in resistance to breakaway oxidation was observed for the commercial alloys in the higher water vapor atmosphere. Microstructural characterization (optical metallography, scanning electron microscopy and electron microprobe analysis) revealed the formation of thick Fe-rich oxides even for the high Cr (~12 wt.%) steels after an initial stage of protective oxidation with MnCr-rich spinels. The impact of the evaporation-induced loss of Cr on the time and temperature dependent compositional changes in the alloys was correlated with experimental findings. For the developmental alloys, Cu additions appear to play a role in significantly reducing oxidation kinetics in air+30 vol.% H2O at 700°C.

Pillai, Rishi [ORNL] (ORCID:0000000243688197)↗

The role of nickel content and the magnetic remanence in iron-nickel alloys of lunar composition

Lunar samples are magnetic primarily due to the body centered cubic (BCC) iron and iron-nickel alloys they contain. Presented for the first time are results which demonstrate that the magnitude of the martensitic thermal remanence (MTRM) induced on quenching iron-nickel alloy in the geomagnetic field depends on the nickel content of the alloy. High magnetic stability is due to the increasing dislocation density and increasingly complex microstructures associated with increasing nickel content in the alloys. The results agree with the mechanical and structural properties of the alloys. The characteristic quench martensite microstructure observed on metallographic examination provides a recognition criterion for the MTRM mechanism. These results are important for lunar and meteoritic research intending to ascertain the paleofield responsible for the observed remanent magnetization.-

Wasilewski, P.↗

Phase transformation and stabilization of a high strength austenite

An investigation of the phase transformation and the austenite stabilization in a high strength austenite has been made. An Fe-29Ni-4.3Ti austenite age-hardened by gamma-prime (Ni3Ti) precipitates showed a further increase of strength after martensitic and reverse martensitic phase transformations. The stability of ausaged austenite as well as ausaged and transformation-strengthened austenite was improved significantly through an isothermal treatment at 500 C. The Ms temperature of the strengthened austenite was restored to nearly that of annealed austenite while the austenite was hardened to R(C) 41 through precipitation and phase transformations. The observed austenite stabilization is attributed to the formation of GP zones or short-range order of less than about 10A in size.

Jin, S.↗

Fractographic analysis of gaseous hydrogen induced cracking in 18Ni maraging steel

Electron microscope fractographic analysis supplemented an extensive study of the kinetics of gaseous hydrogen assisted cracking in 18Ni maraging steel. Temperature determined the crack path morphology in each steel which, in turn, was directly related to the temperature dependence of the crack growth rate. Crack growth in the low temperature regime proceeded along prior austenite grain boundaries. Increasing the temperature above a critical value produced a continuously increasing proportion of transgranular quasi-cleavage associated with lath martensite boundaries. The amount of transgranular cracking was qualitatively correlated with the degree of temperature-induced deviation from Arrhenius behavior. Fractographic observations are interpreted in terms of hypothesized mechanisms for gaseous hydrogen embrittlement. It is concluded that hydrogen segregation to prior austenite and lath martensite boundaries must be considered as a significant factor in developing mechanisms for gaseous embrittlement of high strength steels.

Gangloff, R. P.↗