Work hardening behavior of hot-rolled metastable Fe50Co25Ni10Al5Ti5Mo5 medium-entropy alloy: in situ neutron diffraction analysis.

Metastability engineering is a strategy to enhance the strength and ductility of alloys via deliberately lowering phase stability and prompting deformation-induced martensitic transformation. The advantages of the strategy are widely exploited by ferrous medium-entropy alloys (MEAs) that exhibit phase transformation from metastable face-centered cubic (FCC) to hexagonal close-packed (HCP) or body-centered cubic (BCC) martensite and a significant increase in work hardening. Fe50Co25Ni10Al5Ti5Mo5 (at%) MEA is an example of such materials, which shows ~1.5 GPa of tensile strength assisted by exceptional work hardening from the deformation-induced BCC martensitic transformation. In this work, the martensitic transformation and its effect on the mechanical response of the MEA were studied by in situ neutron diffraction under tensile loading. Strain-induced BCC martensite started forming rapidly from the beginning of plastic deformation, reaching a phase fraction of ~100% when deformed to ~10% of true strain. Lattice strain and phase stress evolution indicate that stress was dynamically partitioned onto the newly formed BCC martensite, which is responsible for the work hardening response and high flow stress of the MEA. This work shows how great a role FCC to BCC martensitic transformation can play in enhancing the mechanical properties of ferrous MEAs.

Non-Hookean large elastic deformation in bulk crystalline metals.

Crystalline metals can have large theoretical elastic strain limits. However, a macroscopic block of conventional crystalline metals practically suffers a very limited elastic deformation of <0.5% with a linear stress-strain relationship obeying Hooke's law. Here, we report on the experimental observation of a large tensile elastic deformation with an elastic strain of >4.3% in a Cu-based single crystalline alloy at its bulk scale at room temperature. The large macroscopic elastic strain that originates from the reversible lattice strain of a single phase is demonstrated by in situ microstructure and neutron diffraction observations. Furthermore, the elastic reversible deformation, which is nonhysteretic and quasilinear, is associated with a pronounced elastic softening phenomenon. The increase in the stress gives rise to a reduced Young's modulus, unlike the traditional Hooke's law behaviour. The experimental discovery of a non-Hookean large elastic deformation offers the potential for the development of bulk crystalline metals as high-performance mechanical springs or for new applications via "elastic strain engineering."

Flexible and Tough Superelastic Co-Cr Alloys for Biomedical Applications.

The demand for biomaterials has been increasing along with the increase in the population of elderly people worldwide. The mechanical properties and high wear resistance of metallic biomaterials make them well-suited for use as substitutes or as support for damaged hard tissues. However, unless these biomaterials also have a low Young's modulus similar to that of human bones, bone atrophy inevitably occurs. Because a low Young's modulus is typically associated with poor wear resistance, it is difficult to realize a low Young's modulus and high wear resistance simultaneously. Also, the superelastic property of shape-memory alloys makes them suitable for biomedical applications, like vascular stents and guide wires. However, due to the low recoverable strain of conventional biocompatible shape-memory alloys, the demand for a new alloy system is high. The novel body-centered-cubic cobalt-chromium-based alloys in this work provide a solution to both of these problems. The Young's modulus of <001>-oriented single-crystal cobalt-chromium-based alloys is 10-30 GPa, which is similar to that of human bone, and they also demonstrate high wear and corrosion resistance. They also exhibit superelasticity with a huge recoverable strain up to 17.0%. For these reasons, the novel cobalt-chromium-based alloys can be promising candidates for biomedical applications.

In-situ neutron diffraction study of lattice deformation behaviour of commercially pure titanium at cryogenic temperature.

Titanium has a significant potential for the cryogenic industrial fields such as aerospace and liquefied gas storage and transportation due to its excellent low temperature properties. To develop and advance the technologies in cryogenic industries, it is required to fully understand the underlying deformation mechanisms of Ti under the extreme cryogenic environment. Here, we report a study of the lattice behaviour in grain families of Grade 2 CP-Ti during in-situ neutron diffraction test in tension at temperatures of 15-298 K. Combined with the neutron diffraction intensity analysis, EBSD measurements revealed that the twinning activity was more active at lower temperature, and the behaviour was complicated with decreasing temperature. The deviation of linearity in the lattice strains was caused by the load-redistribution between plastically soft and hard grain families, resulting in the three-stage hardening behaviour. The lattice strain behaviour further deviated from linearity with decreasing temperature, leading to the transition of plastically soft-to-hard or hard-to-soft characteristic of particular grain families at cryogenic temperature. The improvement of ductility can be attributed to the increased twinning activity and a significant change of lattice deformation behaviour at cryogenic temperature.

Development of triaxial compressive apparatus for neutron experiments with rocks.

Underground engineering for processes such as geological disposal of high-level nuclear waste, CO2 capture and storage, and mining and drilling for resources requires an understanding of the mechanical behavior of rocks at subsurface stress states, i.e., triaxial compressive stress. Strain measurement using neutron diffraction can be applied to rocks to analyze strain accumulation mechanisms at the microscopic scale. This study reports the development of triaxial compressive apparatus for strain measurement using neutron diffraction. The apparatus can analyze rock specimens (diameter, 25 mm; length, 50 mm) and apply a maximum confining pressure of 50 MPa. Materials for the components of the apparatus were investigated theoretically based on neutron beam transmission and experimentally using neutron diffraction experiments. The feasibility of the apparatus was verified by measuring strain at hydrostatic pressure under the application of confining pressure and triaxial compression. The theoretical and experimental results show that the apparatus could obtain sufficient neutron statistics from a rock specimen. It was confirmed experimentally that the measured strain values are correlated with the applied confining pressure and stress. The lattice strains of quartz minerals measured by neutron diffraction showed linear deformation behavior, indicating that elastic strain accumulated in the minerals. This apparatus will enable the finding of new insights into the deformation mechanisms of rocks.

Microstructural Evolution and Mechanical Properties of Non-Equiatomic (CoNi)74.66Cr17Fe8C0.34 High-Entropy Alloy.

In this study, we manufactured a non-equiatomic (CoNi)74.66Cr17Fe8C0.34 high-entropy alloy (HEA) consisting of a single-phase face-centered-cubic structure. We applied in situ neutron diffraction coupled with electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) to investigate its tensile properties, microstructural evolution, lattice strains and texture development, and the stacking fault energy. The non-equiatomic (CoNi)74.66Cr17Fe8C0.34 HEA revealed a good combination of strength and ductility in mechanical properties compared to the equiatomic CoNiCrFe HEA, due to both stable solid solution and precipitation-strengthened effects. The non-equiatomic stoichiometry resulted in not only a lower electronegativity mismatch, indicating a more stable state of solid solution, but also a higher stacking fault energy (SFE, ~50 mJ/m2) due to the higher amount of Ni and the lower amount of Cr. This higher SFE led to a more active motion of dislocations relative to mechanical twinning, resulting in severe lattice distortion near the grain boundaries and dislocation entanglement near the twin boundaries. The abrupt increase in the strain hardening rate (SHR) at the 1~3% strain during tensile deformation might be attributed to the unusual stress triaxiality in the {200} grain family. The current findings provide new perspectives for designing non-equiatomic HEAs.

Stacking Fault Driven Phase Transformation in CrCoNi Medium Entropy Alloy.

Phase transformation is an effective means to increase the ductility of a material. However, even for a commonly observed face-centered-cubic to hexagonal-close-packed (fcc-to-hcp) phase transformation, the underlying mechanisms are far from being settled. In fact, different transformation pathways have been proposed, especially with regard to nucleation of the hcp phase at the nanoscale. In CrCoNi, a so-called medium-entropy alloy, an fcc-to-hcp phase transformation has long been anticipated. Here, we report an in situ loading study with neutron diffraction, which revealed a bulk fcc-to-hcp phase transformation in CrCoNi at 15 K under tensile loading. By correlating deformation characteristics of the fcc phase with the development of the hcp phase, it is shown that the nucleation of the hcp phase was triggered by intrinsic stacking faults. The confirmation of a bulk phase transformation adds to the myriads of deformation mechanisms available in CrCoNi, which together underpin the unusually large ductility at low temperatures.

Cooperative deformation in high-entropy alloys at ultralow temperatures.

High-entropy alloys exhibit exceptional mechanical properties at cryogenic temperatures, due to the activation of twinning in addition to dislocation slip. The coexistence of multiple deformation pathways raises an important question regarding how individual deformation mechanisms compete or synergize during plastic deformation. Using in situ neutron diffraction, we demonstrate the interaction of a rich variety of deformation mechanisms in high-entropy alloys at 15 K, which began with dislocation slip, followed by stacking faults and twinning, before transitioning to inhomogeneous deformation by serrations. Quantitative analysis showed that the cooperation of these different deformation mechanisms led to extreme work hardening. The low stacking fault energy plus the stable face-centered cubic structure at ultralow temperatures, enabled by the high-entropy alloying, played a pivotal role bridging dislocation slip and serration. Insights from the in situ experiments point to the role of entropy in the design of structural materials with superior properties.

Synergetic strengthening of layered steel sheet investigated using an in situ neutron diffraction tensile test.

Synergetic strengthening induced by plastic strain incompatibility at the interface, and the resulting extra geometrically necessary dislocations (GNDs) generated during plastic deformation, were investigated to understand the origin of extra strength in heterogeneous structured (HS) materials. The mechanism of extra GND generation in twinning-induced plasticity (TWIP)-interstitial free (IF) steel layered sheet was quantitatively analyzed by conducting in situ neutron scattering tensile test. Load partitioning due to the different mechanical properties between the TWIP-steel core and IF-steel sheath at the TWIP/IF interface was observed during the in situ tensile testing. Because of the plastic strain incompatibility from load partitioning, extra GNDs are generated and saturate during tensile deformation. The extra GNDs can be correlated with the back-stress evolution of the HS materials, which contributes to the strength of layered materials. Because of the back-stress evolution caused by load partitioning, the strength of TWIP-IF layered steel is higher than the strength estimated by the rule-of-mixtures. This finding offers a mechanism by which extra GNDs are generated during load partitioning and shows how they contribute to the mechanical properties of HS materials.

High stereographic resolution texture and residual stress evaluation using time-of-flight neutron diffraction.

Neutron diffraction texture measurements provide bulk averaged textures with excellent grain orientation statistics, even for large-grained materials, owing to the probed volume being of the order of 1 cm3. Furthermore, crystallographic parameters and other valuable microstructure information such as phase fraction, coherent crystallite size, root-mean-square microstrain, macroscopic or intergranular strain and stress, etc. can be derived from neutron diffractograms. A procedure for combined high stereographic resolution texture and residual stress evaluation was established on the pulsed-neutron-source-based engineering materials diffractometer TAKUMI at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Research Center, through division of the neutron detector panel regions. Pole figure evaluation of a limestone standard sample with a well known texture suggested that the precision obtained for texture measurement is comparable to that of the established neutron beamlines utilized for texture measurement, such as the HIPPO diffractometer at the Los Alamos Neutron Science Center (New Mexico, USA) and the D20 angle-dispersive neutron diffractometer at the Institut Laue-Langevin (Grenoble, France). A high-strength martensite-austenite multilayered steel was employed for further verification of the reliability of simultaneous Rietveld analysis of multiphase textures and macro stress tensors. By using a texture-weighted geometric mean micromechanical (BulkPathGEO) model, a macro stress tensor analysis with a plane stress assumption showed a rolling direction-transverse direction (RD-TD) in-plane compressive stress (about -330 MPa) in the martensite layers and an RD-TD in-plane tensile stress (about 320 MPa) in the austenite layers. The phase stress partitioning was ascribed mainly to the additive effect of the volume expansion during martensite transformation and the linear contraction misfit between austenite layers and newly transformed martensite layers during the water quenching process.

Martensite phase stress and the strengthening mechanism in TRIP steel by neutron diffraction.

Two TRIP-aided multiphase steels with different carbon contents (0.2 and 0.4 mass%) were analyzed in situ during tensile deformation by time-of-flight neutron diffraction to clarify the deformation induced martensitic transformation behavior and its role on the strengthening mechanism. The difference in the carbon content affected mainly the difference in the phase fractions before deformation, where the higher carbon content increased the phase fraction of retained austenite (γ). However, the changes in the relative fraction of martensitic transformation with respect to the applied strain were found to be similar in both steels since the carbon concentrations in γ were similar regardless of different carbon contents. The phase stress of martensite was found much larger than that of γ or bainitic ferrite since the martensite was generated at the beginning of plastic deformation. Stress contributions to the flow stress were evaluated by multiplying the phase stresses and their phase fractions. The stress contribution from martensite was observed increasing during plastic deformation while that from bainitic ferrite hardly changing and that from γ decreasing.

Development of a cryogenic load frame for the neutron diffractometer at Takumi in Japan Proton Accelerator Research Complex.

To prepare for projects such as the Large Hadron Collider upgrade, International Thermonuclear Experimental Reactor and Demonstration reactor, it is important to form a clear understanding of stress-strain properties of the materials that make up superconducting magnets. Thus, we have been studying the mechanical properties of superconducting wires using neutron diffraction measurements. To simulate operational conditions such as temperature, stress, and strain, we developed a cryogenic load frame for stress-strain measurements of materials using a neutron diffractometer at Japan Proton Accelerator Research Complex (J-PARC) Takumi beam line. The maximum load that can be applied to a sample using an external driving machine is 50 kN. Using a Gifford-MacMahon cryocooler, samples can be measured down to temperatures below 10 K when loaded. In the present paper, we describe the details of the cryogenic load frame with its test results by using type-304 stainless steel wire.