Interstitial alloying is an effective strategy for enhancing the mechanical properties of high-entropy alloys (HEAs). However, in carbon-containing HEAs, the coexistence of interstitial carbon and carbides complicates the investigation of interstitial carbon's individual effects on strength and ductility. To address this, a carbide-free interstitial-strengthened HEA, FeMnCoNiCx, was designed by incorporating elements with low carbon affinity, enabling a clear assessment of the role of interstitial carbon. The results demonstrate that interstitial carbon solution simultaneously improves strength, ductility, and work hardening capability. Synchrotron radiation experiments reveal that the interstitial carbon containing alloy sustains higher lattice elastic strain, dislocation density, and stacking fault probability during tensile deformation, with the increased dislocation density being the primary contributor to enhanced work hardening. First-principles calculations further elucidate the lattice distortion, chemical inhomogeneity and electronic localization effects induced by interstitial carbon, as well as their potential influence on strength and ductility. This study highlights the importance of carbide-free interstitial carbon-strengthened HEAs for a fundamental understanding of carbon's influence on mechanical properties.
In this study, pulsed neutron Bragg-edge transmission (BET) imaging was employed to characterize plastic deformation of high-manganese (Mn) austenitic steel during cryogenic impact fracture. Electron backscatter diffraction (EBSD) was used to examine the microstructural evolution. The results reveal that the Bragg-edge width of the (200) lattice plane, σ200 = 100 µs, was identified as the critical value for large plastic deformation. Accordingly, the characteristic regions were classified by σ200 value. Regions with σ200 > 100 µs correspond to crack initiation and stable crack growth, while those with σ200 < 100 µs correspond to unstable crack growth. Both crack initiation and stable crack growth regions exhibited higher levels of plastic deformation, twin density, and dislocation density compared to unstable crack growth regions. Moreover, σ200 showed strong positive correlations with the dislocation density, twin density and hardness. As the test temperature decreased from 273 to 77 K, the transition point from stable to unstable crack growth occurred earlier. This is responsible for the reduction in impact absorbed energy. These findings provide new insights into the cryogenic toughening mechanism of high-Mn austenitic steel.
The cryogenic fracture mechanism of high-Mn austenitic steels was investigated using a quasi-in situ experiment of interrupted Charpy impact test, together with electron backscatter diffraction (EBSD) and neutron Bragg-edge transmission (BET) imaging. The results show that voids coalesce through void sheeting at 77 K, a fracture mechanism associated with superior cryogenic toughness. The widely and ring-like distributed deformation twins ahead of the crack tip contribute limitedly to alleviating strain localization at 77 K. However, by suppressing the increase in stress triaxiality, deformation twins play a key role in promoting void sheeting and preventing the transition to quasi-cleavage fracture. This work lays the foundation for subsequent investigations into cryogenic toughening.
The surface induction-hardened S38C medium carbon steel shows a good balance of strength and toughness, but complicates the evaluation of fatigue resistance, mainly because of gradient residual stress (RS) and grains. An integrated fatigue resistance assessment (AIFA) framework was proposed to consider the residual stress relief under stochastic loads. To this end, quasi-in situ neutron diffraction and Bragg-edge imaging were combined to probe the evolution of residual stress during crack propagation. Firstly, a rigid-flexible coupled vehicle dynamics model was adopted to obtain the time-domain variable amplitude loading spectrum. Then, Fortran subroutines were developed to assign these data into full-scale S38C axle model, and the remaining life was predicted using the damage tolerance approach. The results demonstrate that crack propagation would accelerate when residual stress is considered in the case of the crack depth exceeding 3.0 mm. It is, for the first time, found that 15 mmand 5 mm-thickness fan-shaped specimens can retain the axial and hoop residual strain in terms of diffraction angle variation, respectively, for full-scale structural S38C steel axles. In the absence of RS, the remaining life of the axle decreases sharply from 624,800 to 51,300 km as the crack depth increases from 3.0 to 16 mm. Compared with the standard method under constant amplitude loading without residual stress relief, the present AIFA method provides the more accurate but conservative fatigue life prediction.
Complementary layer thickness effects on strength and plasticity in Q235 and SUS304 steels provide a novel strategy to realize high strength and high plasticity of heterogeneous Q235/SUS304 multilayered steel. In this work, the tensile deformation behaviors and fracture characteristics of vacuum hot-rolled Q235/SUS304 multilayered steel with various layer thicknesses ranging from 223 mu m to 5 mu m were deeply investigated. The tensile strength improved with the reduction of layer thickness, and the uniform elongation was first increased and then decreased with decreasing layer thickness, and the peak value appeared at the layer thickness of 20 mu m. Interestingly, the fracture elongation forms a high plateau value within the 10 similar to 20 mu m range. Further analysis reveals that the severe strain localization in the brittle SUS304 thin layers is delayed by the ductile Q235 layers, which is mainly attributed to the different texture evolution and dislocation configuration characteristics during tensile deformation.
The lattice parameters of both the product phase and the matrix phase have determined using in situ X-ray and neutron diffraction measurements during forward and reverse transformations in steels. The lattice parameters are well known to be influenced by various factors, including temperature, internal stresses induced by transformation strains, partitioning of alloying elements, crystal defects, and magnetic strains. Therefore, it is crucial to accurately disentangle the contributions of these factors to the observed changes in lattice parameters. This review examines the evaluation of internal strain (stress) associated with ferrite, pearlite, bainite, martensite, and reverse austenite transformations, with a particular emphasis on the distinction between diffusional and displacive transformations. Additionally, the effects of plastic deformation of austenite on the bainite or martensite transformation are discussed. In this context, the roles of dislocations and vacancies are highlighted as key areas for further investigation.
The magnesium alloy AZ31, which has undergone high-pressure torsion processing, was subjected to in situ annealing microbeam synchrotron high-energy X-ray diffraction and compared to the as-received rolled sheet material that was investigated through in situ neutron diffraction. While the latter only exhibits thermal expansion and minor recovery, the nanostructured specimen displays a complex evolution, including recovery, strong recrystallization, phase transformations, and various regimes of grain growth. Nanometer-scale grain sizes, determined using Williamson–Hall analysis, exhibit seamless growth, aligning with the transition to larger grains, as assessed through the occupancy of single-grain reflections on the diffraction rings. The study uncovers strain anomalies resulting from thermal expansion, segregation of Al atoms, and the kinetics of vacancy creation and annihilation. Notably, a substantial number of excess vacancies were generated through high-pressure torsion and maintained for driving the recrystallization and forming highly activated volumes for diffusion and phase precipitation during heating. The unsystematic scatter observed in the Williamson–Hall plot indicates high dislocation densities following severe plastic deformation, which significantly decrease during recrystallization. Subsequently, dislocations reappear during grain growth, likely in response to torque gradients in larger grains. It is worth noting that the characteristics of unsystematic scatter differ for dislocations created at high and low temperatures, underscoring the strong temperature dependence of slip system activation. Graphical Abstract
The quasi-static superelastic responses and hierarchical martensite transformation from body-centered cubic (BCC) to face-centered cubic (FCC) under dynamic impact in Fe42Mn34Al15Ni7.5Ti1.5 alloys were investigated. Polycrystalline and oligocrystalline alloys were produced through solution heat treatment and cyclic heat treatment processes, respectively. The results show the volume fraction of residual martensite for oligocrystalline alloys is lower, which exhibits better superelastic responses compared with polycrystalline alloys. Dynamic impact tests indicate that, despite the weakening of the grain boundary strengthening effect, the ultimate strength of the oligocrystalline alloys closely matches that of the polycrystalline alloys under dynamic impact. The martensite transformation of the FeMnAlNiTi alloy is characterized as hierarchical under dynamic impact, and increasing strain rates and grain sizes can enhance the BCC→FCC martensite transformation, resulting in higher martensite phase fractions for oligocrystalline alloys. The increase in ultimate strength is attributed to the dynamic Hall-Petch effect introduced by more martensite phase interfaces under dynamic impact.
The hot-rolled microstructure of medium Mn steel has coarse grains and severe elemental segregation, resulting in low strength and plasticity. Constructing a multiphase structure, refining the microstructure, and regulating elemental segregation enhance the mechanical properties. In this study, liquid nitrogen treatment created a layered distribution of austenite and martensite. Warm rolling was then used to reduce layer thickness and refine grain structure. After liquid nitrogen and warm rolling treatments, the strength and plasticity of medium Mn steel increased to 1270 MPa and 23.3%, respectively, far exceeding the hot-rolled state (724 MPa, 12.8%). Warm rolling also triggers austenite reverted transformation (ART) and introduces high-density dislocations, further improving austenite stability. This strengthening effect is higher than that from intercritical annealing alone. Improved austenite stability delays the transformation induced plasticity (TRIP) effect, preventing brittle fracture and enhancing deformation coordination between layers, significantly increasing the plastic deformation capacity of medium Mn steel.
Gradient distribution of triaxial residual stresses to a depth of several millimeters is retained in middle carbon steel S38C axles after high-frequency induction hardening, which has become a critical concern for fatigue structural integrity. To address this, the axial, hoop, and radial gradient residual strains inside the axles were measured for the first time by advanced neutron diffraction. The SIGINI Fortran subroutine was then adopted to reconstruct the global initial residual stress field from the measured data. Experimental and simulation results show that residual stresses of about -520 MPa (axial), -710 MPa (hoop), and -40 MPa (radial) residual stress were retained below the axle surface. Subsequently, the fatigue crack propagation behavior of S38C axles was numerically investigated in the framework of fracture mechanics. The calculated results clearly show that the compressive residual stresses at a depth of 0-3 mm from the axle surface lead to a low crack growth driving force, and that fatigue cracks do not propagate as long as the crack depth is less than 3.7 mm for hollow S38C axles. These results further indicate that the maximum defect size allowed in routine inspections is acceptable from a safety and economic point of view. Accurate measurement and characterization of the global gradient residual stress field through experiments and simulations can provide an important reference for optimizing the mileage intervals of nondestructive testing (NDT) of surface defects in these surface-strengthened railway axles.
The influence of interstitial carbon on the texture evolution of high-entropy alloys during cold rolling was investigated. To prevent carbide formation, elements with weak carbon affinity were carefully selected in the (FeMnCoNi)96.5C3.5 alloy. Neutron diffraction, electron channeling contrast imaging, and electron backscatter diffraction were used to analyze the texture and microstructure evolution in alloys with and without carbon addition. Though their texture components are similar at the early stage of deformation, the Brass and Goss textures in the carbon-containing alloy at 50 % cold rolling reduction are obviously higher than those in the carbon-free alloy, while Copper and S textures are lower. A large number of deformation twins induced in the carbon-containing alloy is attributed as the significant reason for the texture differences. This work helps to understand the impact of interstitial carbon on the texture evolution of high-entropy alloys, providing valuable insights for microstructure and performance optimization.
Comprehensive information on in situ microstructural and crystallographic changes during the preparation/manufacturing processes of various materials is highly necessary to precisely control the microstructural morphology and the preferred orientation (or texture) characteristics for achieving an excellent strength–ductility–toughness balance in advanced engineering materials. In this study, in situ isothermal annealing experiments with cold-rolled 17Ni-0.2C (mass%) martensitic steel sheets were carried out by using the TAKUMI and ENGIN-X time-of-flight neutron diffractometers. The inverse pole figures based on full-profile refinement were extracted to roughly evaluate the preferred orientation features along three principal sample directions of the investigated steel sheets, using the General Structure Analysis System (GSAS) software with built-in generalized spherical harmonic functions. The consistent rolling direction (RD) inverse pole figures from TAKUMI and ENGIN-X confirmed that the time-of-flight neutron diffraction has high repeatability and statistical reliability, revealing that the principal preferred orientation evaluation of steel materials can be realized through 90° TD ➜ ND (transverse direction ➜ normal direction) rotation of the investigated specimen on the sample stage during two neutron diffraction experiments. Moreover, these RD, TD, and ND inverse pole figures before and after the in situ experiments were compared with the corresponding inverse pole figures recalculated from the MUSASI-L complete pole figure measurement and the HIPPO in situ microstructure evaluation, respectively. The similar orientation distribution characteristics suggested that the principal preferred orientation evaluation method can be applied to the in situ microstructural evolution of bulk orthorhombic materials and spatially resolved principal preferred orientation mappings of large engineering structure parts.
Unconventional white‐beam Laue synchrotron X‐ray diffraction is used on fine‐grained, as‐rolled magnesium alloy during an in situ heating experiment. At high temperatures, reflections of single grains are superimposed on the halo stemming from matrix grains. Some unique grain reflections spontaneously move, indicating grain rotations in response to torque expedited at grain boundaries. When a grain boundary spontaneously activates, it can begin to rotate, allowing diffusive mass transport and activating the boundaries of its other neighbors. Now the given grain can freely rotate toward coalescence; however, the multitude of grain boundaries compete in torque orientation and magnitude, resulting in zigzag rotations. After coalescence, the larger grain is still active and continues this scenario of growth, while the majority of the matrix grains remain inactive. The first‐time experimental observation of such erratic grain behavior supplies the missing puzzlestone leading to anomalous grain growth, long postulated in literature. The method of white beam Laue diffraction on fine‐grained polycrystalline materials delivers a novel experimental method to study the erratic behavior of grain reorientation, as requested long ago by the scientific community. Such findings apply to wide ranges of materials undergoing grain growth, creep, and superplasticity, including those in metal engineering, ceramics, and geophysical disciplines.
Non-destructive and quantitative mapping of gradient residual strain distribution in surface-hardened railway S38C axles could provide a positive reference for determining service lifetime and maintenance strategy. To tackle this concern, time-of-flight neutron Bragg-edge transmission imaging was employed by real axle samples with and without impacted crater. A novel and simple procedure to formulate the residual strain field was also developed in this work, with the transmission batch code in Appendix A. By mapping the global two-dimensional residual strains, it can be verified that the residual strains into the axle are uniformly distributed in the hoop direction. Subsequently, it was revealed that the axial and hoop residual strains, respectively in the cylinder and the long strip samples prepared from a real S38C hollow axle, indicated a gradient evolution distribution with a depth of similar to 8 mm, covering a range of -5500 similar to 1000 mu epsilon for axial strains and -6500 similar to 1000 mu epsilon for hoop strains. More importantly, the maximum compressive lattice strain of the cylinder sample was increased by 15.61 %, and 22.35 % at the impacting speeds of 100, and 125 m/s, respectively; and that of the long strip sample increased by 29.17 %, and 43.70 %, respectively. It can thus be concluded that lattice strains have redistributed around the impact crater, demonstrating the local alteration of the residual strain field. These new findings suggest the localized variation in residual strains should be taken into account while evaluating the service damage evolution of railway axles, especially those affected by high-speed impacts during operation.
High-speed railway S38C axles undergo surface induction hardening for durability, but are susceptible to fatigue cracks from foreign object impact. The neutron diffraction method was employed to measure the residual strain in S38C axles, obtaining microscopic lattice distortion data, for the gradient layer at a depth of 8 mm under the surface. The results showed that after induction-hardening, the microscopic lattice distortion had a gradient distribution, decreasing with the distance from the surface. However, in the case of impacting speed of 600 km/m, the average microscopic lattice distortion increased with the distance from the surface, reaching a maximum augmentation of 55 pct. These findings indicate a strong experimental basis, and improve our understanding of the relationship between macroscopic residual stress and decision-making, in regard to operation and maintenance.
Abnormal damages in railway axles can lead to a significant hazard to running safety and reliability. To this end, a surface treatment was selected to effectively inhibit fatigue crack initiation and growth. In this study, a single-edge notch bending fatigue test campaign with artificial notches was conducted to elucidate the fatigue crack non-propagation behavior in railway S38C axles subjected to an induction hardening process. The fatigue cracking behavior in the gradient structure was revealed by optical microscopy, electron backscatter diffraction, and fractography. The microhardness distribution was measured using a Vickers tester. The obtained results show that the microhardness of the strengthening layer is nearly triple that of the matrix. Owing to the gradient microstructures and hardness, as well as compressive residual stress, the fatigue long crack propagates faster once it passes through the hardened zone (approximately 2.0 mm in the radial depth). Thereafter, local retarding (including deflection, branching, and blunting) of the long crack occurs because of the relatively coarse ferrite and pearlite in the transition region and matrix. Totally, this fatigue cracking resistance is reasonably believed to be due to the gradient microstructure and residual stress. These findings help to tailor a suitable detection strategy for maximum defects or cracks in railway axles.
Considering the complex service environments that high speed railway axles are subjected to, the fatigue crack growth (FCG) behavior of a structurally gradient axle steel with different pre-crack depths both in air and a corrosive medium was investigated at a frequency of 5 Hz. The results indicated that in the high Delta K region, the FCG rate was dramatically accelerated by corrosion but the gap narrows as Delta K decreased. The accelerated corrosion FCG rate was a comprehensive result of the acceleration effect of the anodic dissolution, hydrogen-enhanced localized plasticity and the retardation effect of corrosion-induced crack-tip blunting. Despite the fact that the corrosion resistance gradually decreased as the pre-crack depth increased, the FCG rate in the corrosive medium gradually decreased. This was because fatigue loading played a more important role than corrosion in accelerating the corrosion FCG rate.
A unique impact fracture behavior is found in a high-Mn austenitic steel (24Mn-4Cr-0.4C-0.3Cu) in this work. The steel exhibits concurrent twinning-induced plasticity (TWIP) effect and the transformation-induced plasticity (TRIP) effect. By analyzing the load-deflection curves recorded during Charpy impact testing, the resistance to crack initiation and propagation is quantified from the absorbed energy. The high-Mn steel demonstrates good resistance to crack initiation at 273 K and 77 K. However, as the temperature decreases from 273 K to 77 K, there is an accelerated transition from stable crack growth to unstable crack growth during impact, resulting in the deterioration of resistance to crack propagation. The plastic deformation of the impact-tested samples, especially in the region close to the crack-path profile was quantitatively analyzed using neutron Bragg-edge transmission (BET) imaging. The deformation zones, divided by using the width of the 200 Bragg edge, exhibit good agreement with the impact absorbed energy characteristics obtained from dynamic load-deflection curves. Moreover, the unstable growth transition point was roughly determined on the impact-tested sample. Then, the electron backscatter diffraction (EBSD) technique is employed to examine the deformation microstructure along the crack-path in the impact-tested samples. The results revealed the dual roles of TRIP effect in impact toughness of the high-Mn steel. On one hand, the TRIP effect plays a positive role in improving resistance to crack initiation and propagation. On the other hand, the excessive accumulation of brittle epsilon/alpha ՛-martensite caused by the enhanced TRIP effect at 77 K leads to quasi-cleavage fracture, thereby playing a negative role. Finally, we discussed the prominent toughening mechanisms associated with the TWIP and TRIP effects, which greatly impact the impact fracture behavior.