Coarse-grained Specimens Research Articles

Achieving an excellent combination of strength and ductility in metastable β titanium alloys via coupling isothermal ω phase and TRIP/TWIP effects

TRIP/TWIP metastable β titanium alloys demonstrate high strain hardening rates and excellent tensile ductility. However, the precipitation of nanometer-sized ω phase through microstructural control significantly improves strength but often results in a significant decrease in ductility. This research proposes a novel strategy by precipitating isothermal ω phase (ωiso) and integrating mechanical twinning/martensitic transformation to address these challenges. The single-phase β coarse-grained (CG) specimens of metastable Ti25Nb (at.%) alloy were subjected to solution treatment in the β phase region, followed by aging at 300 °C for 60 min to obtain CG60. The ωiso-reinforced CG60 specimen exhibited a 12 % uniform elongation (1 % higher than CG specimen) and a yield strength of 857 MPa (approximately 67 % higher than CG specimens). In the CG60 specimen, deformation mechanisms were mainly attributed to the TRIP, TWIP and dislocation slip, with TWIP being predominant. As aging time increased, ω phase (localized barriers) and improved β matrix stability progressively suppressed TRIP and TWIP effects, with TWIP being completely inhibited first. Transmission electron microscopy and computational findings suggest that a denser distribution of ωiso contributes more significantly to the strengthening of the alloy.

Grain size dependent deformation microstructure evolution and work-hardening in CoCrNi medium entropy alloy

This study clarified the grain size dependence of the deformation microstructure evolution and work-hardening behavior in CoCrNi medium entropy alloy. We fabricated fully recrystallized specimens with coarse-grained (CG) and ultrafine-grained (UFG) specimens by severe plastic deformation and subsequent annealing processes. Tensile deformation was applied to the specimens at room temperature. The UFG specimen exhibited both high strength and high ductility compared to conventional UFG metals due to the high work-hardening ability. In the CG specimen, three distinct types of deformation microstructures consisting of dislocations and deformation twins developed depending on grain orientations, similar to the single-crystalline specimens. In the UFG specimen, widely extended stacking faults and randomly-tangled dislocations were found to coexist in most grains. Deformation twins were found to nucleate without evidence of dislocation reactions regardless of grain orientations, implying abnormal nucleation mechanisms of deformation twins in the UFG specimen. Dislocation densities quantified by in-situ synchrotron XRD measurements during tensile deformation were higher in the UFG specimen than those in the CG specimen and conventional UFG metals. Our analysis showed that the work-hardening behavior of the specimens was primarily controlled by increases in dislocation density as well as the introduction of planar defects during deformation. Through comparisons with the CG specimen and conventional UFG metals, we concluded that the excellent work-hardening ability of the UFG specimen was mainly due to the evolution of unique deformation microstructures and rapid increase in dislocation density, which could be due to inhibited dynamic recovery in the MEA.

A strategy for simultaneously enhancing the strength and ductility of metastable β titanium alloys: Coupling heterogeneous structure and TRIP effects

The applicability of metastable β titanium alloys is frequently constrained by their relatively low yield strength. This study has successfully designed a metastable β titanium alloy with heterogeneous microstructures (HS) comprising both deformed and recrystallized grains, achieved through simple cold rolling followed by short-term annealing. Compared to traditionally coarse-grained (CG) specimen that is entirely crystallized and equiaxed, the HS specimen exhibit not only a postponed initiation of double yielding but also superior yield strength (enhanced by 27.8 %) and ductility (enhanced by 7 %). The delayed double yielding and enhanced strength in the HS specimen are ascribed to the restriction of dislocation motion by α" martensite and the heterogeneous deformation induced (HDI) strengthening mechanisms. The ductility of the HS specimen exceeds that of the CG specimen, owing to the combined effect of HDI hardening and the transformation-induced plasticity (TRIP) effects. The more pronounced TRIP effect in the HS specimens results from the synergistic effect of the elevated HDI stress and the applied external stress, which promotes the occurrence of stress-induced martensitic phase transformation. This study offers a novel strategy for the development of high-performance metastable β titanium alloys.

Mechanical behavior of unsaturated soils from suction controlled ring shear tests

The shear strength behavior associated with a large shear deformation of both the fine- and coarse-grained unsaturated soils is important in interpreting and forecasting the initiation and movement of landslides. For this reason, a suction-controlled ring shear apparatus was designed by introducing modifications to the conventional Bromhead ring apparatus extending the axis translation technique. A series of suction-controlled ring shear tests were performed on fine- and coarse-grained unsaturated soil specimens subjecting to large shear deformation. The experimental results are presented and interpreted for highlighting: (i) the shear stress/void ratio-shear displacement relationships; (ii) the envelopes of the residual shear strength; (iii) the void ratio, water ratio and degree of saturation of the fine-grained soil specimens sheared to the residual state under different net normal stresses and matric suctions. These results provide valuable information toward understanding and interpreting the behaviors of landslides in unsaturated soils that experience the first failure and the reactivation along a pre-sheared slip surface.

Grain-refined metastable β titanium alloy with suppressed ω-assisted nucleation and enhanced mechanical properties

The mechanical characteristics of metastable β titanium alloys are related to the α precipitates that form during aging. Although precipitation behavior can be modulated by ω-assisted nucleation, the influence of grain size (GS) on this process has not been fully considered. In this study, the effects of grain refinement on mechanical properties and ω-assisted nucleation were investigated by aging the Ti-5.3Cr-4.9Mo-4.9 V-4.3Al-0.9 Nb-0.3Fe (TB18) alloy with coarse grains (87 μm) or fine grains (25 μm) at different heating rates (RH). It was found that ω-assisted nucleation depends on the RH, with a lower RH promoting the processes of ω-assisted nucleation and the precipitation of finer secondary α (αs) plates. The vacancy concentration after annealing reduced with decreasing GS, indicating that ω-assisted nucleation is suppressed by grain refinement. Additionally, grain refinement significantly improved the ductility of the TB18 alloy. This effect was attributed to enhanced homogeneous plastic deformation and an increase in slip systems, such as pyramidal <c+a> slip on αs plates. At ultimate tensile strengths of 1300–1550 MPa, the elongation of the fine-grained specimens was typically 2–3 times greater than that of the coarse-grained specimens. Furthermore, the corresponding mixed fracture mode involved a greater extent of ductile fracture. Therefore, the mechanical properties of metastable β titanium alloys are primarily limited by coarse β grains.

Effect of prior austenite grain size on austenite reversion, bainite transformation and mechanical properties of Fe-2Mn-0.2C steel

To elucidate the response of austenite reversion and subsequent bainite transformation behavior to the prior austenite grain (PAG) size, the transformation kinetics and amount of reverted austenite in the intercritical region, the subsequent bainite transformation kinetics, and the tensile properties were investigated by dilatometers, scanning electron microscopy, electron backscatter diffraction, transmission electron microscopy, and the mechanical tests. The results show that, when annealed at 730 °C, fine-grained specimens exhibit faster reverted austenite transformation rate than coarse-grained specimens due to the presence of more PAG boundaries. As the intercritical temperature rises to 760 °C, more intragranular globular austenite forms in the coarse-grained specimen, which accelerates the reverted austenite transformation rate. Compared to fine-grained specimens, coarse-grained specimens exhibit faster bainite transformation and higher amount of bainitic ferrite. The microstructure after austempering consists of intercritical ferrite, bainitic ferrite, RA and fresh martensite. With increasing the austempering time, more bainitic ferrite is formed and the amount of RA and fresh martensite decreases. With increasing the austempering time, the increase in the amount of bainitic ferrite leads to an increase in the yield strength, while the decrease in the amount of RA leads to a decrease in the elongation. Moreover, compared with coarse-grained specimens, the finer microstructure in fine-grained specimens improves yield and tensile strengths, while higher amount of RA contributes to larger uniform and total elongations.

Fracture Toughness Investigations of an Ion‐Irradiated Nanocrystalline TiZrNbHfTa Refractory High‐Entropy Alloy

Refractory high‐entropy alloys (RHEAs) show potential for use in extreme environments, such as advanced nuclear reactors, owing to their high melting temperature, and often outstanding combinations of mechanical properties, corrosion resistance, and irradiation‐damage tolerance. This study evaluates the fracture toughness of a TiZrNbHfTa RHEA across different scales and microstructures, with a focus on the impact of He2+‐ion irradiation. Micro‐ and millimeter‐scale specimens with nanocrystalline (NC) microstructures are compared to existing ASTM standard sized coarse‐grained (CG) specimen data, with critical dimensions spanning over three orders of magnitude, from 10 μm to 12 mm. The ASTM standard sized CG specimens exhibit a fracture toughness 41‐fold greater than their NC microscale counterparts (210–5.1 MPa m1/2), while NC millimeter‐scale specimens show a 7.5‐fold higher fracture toughness than NC microscale specimens (38.1–5.1 MPa m1/2). He2+‐ion irradiation leads to a 27% decrease in fracture toughness in the NC microscale specimens. The results highlight the impact of sample dimensional scale, microstructure, and ion irradiation on the fracture toughness of the RHEA, indicating a need for thorough examination of such factors when investigating the mechanical properties of these materials.

Assessing the tribo-corrosion resistance of surface nanostructured stainless-steel

In this work, surface mechanical rolling treatment (SMRT) was applied as a post-process nanostructuring technique to improve the tribo-corrosion degradation resistance of coarse grain (CG) 316L stainless steel (SS). The experimental findings reveal that when tribo-corrosion wear took place, the CG specimen experienced severe surface de-passivation, which increased wear-corrosion synergy and the rate of material loss. On the other hand, the SMRT specimen experienced enhanced re-passivation kinetics, which reduced wear-corrosion synergy and the rate of material loss. The wear mechanism for both the CG and SMRT specimens was abrasion-dominant, with the CG specimen having the presence of micro-pits within the wear track. In addition to these findings, the reduced surface roughness, improved hardness, formed compressive stresses, microstructural refinement, and martensite phase transformation induced by the SMRT process contributed to the enhanced tribo-corrosion resistance of the SMRT specimen. In total, SMRT was found to be a feasible technique to improve the tribo-corrosion resistance of CG 316L SS.

Failure behaviors and acoustic emission characteristics of flawed granite of different grain sizes: Insights from true triaxial experiments with a free face

In this study, a group of experiments using true triaxial stress conditions with free face loading are performed on granite specimens with non-penetrating double flaws. The crack development and failure characteristics of these specimens are explored by integrating video of the free face and acoustic emission technology, with the combination of the four different intermediate principal stresses and three different grain sizes of the granite chosen as variables. First, surface flaws with a depth of 50 mm are found to have limited influence on the specimen’s failure mode. The intermediate principal stress has a greater effect as it inhibits the development of surface cracks; however, surface cracks develop much more readily in coarse-grained specimens than in other specimens. Second, when the intermediate principal stress exceeds 10 MPa, the rock burst failure phenomenon occurs in the specimen. Third, irrespective of changes in the intermediate principal stress and granite specimen grain size, the specimens primarily fail by tensile-shear failure and shear failure. Extending inward from the free face in the σ3 direction, according to the failure types, the failure types can be classified into tensile failure, shear failure, and tensile-shear failure. Finally, using the stress state synthesis method, the specimen’s stress state and crack distribution mechanism on the σ2 loading plane are analyzed.

Probing the impact of grain size distribution on the deformation behavior in fine-grained austenitic stainless steel: A critical analysis of unimodal structure versus bimodal structure

This study investigated the effect of grain size distribution on the deformation behavior in fine-grained (FG) austenitic stainless steels (γ-SSs). Commercial Cr–Mn–N γ-SS was selected as the coarse-grained (CG) specimen, which was cold rolled and then annealed at 1000 °C for 60 s and 700 °C for 3600 s to obtain FG specimens with similar grain sizes but different grain size distributions. The CG specimens annealed at 1000 °C for 60 s and 700 °C for 3600 s were referred to as unimodal-FG and bimodal-FG specimens, respectively. The tensile properties revealed that the yield strength was enhanced from 383 MPa to 685 MPa when the grain size was refined from CG (10.7 μm) to FG (∼1.8 μm). Moreover, the bimodal-FG specimen exhibited a higher total elongation of 48% than 36.5% for the unimodal-FG specimen. Transmission electron microscopy, electron backscatter diffraction and X-ray diffraction were used to identify the microstructural characteristics during tension. The results indicated that the main deformation mechanisms of γ-SSs specimens during tension were dislocation generation and accumulation at the initial stage, deformation twinning at the intermediate stage, and deformation-induced martensite (DIM) at the final stage. Compared with the unimodal-CG counterpart, grain refinement in the unimodal-FG specimens restricted the formation of DIM due to the increased austenite stability. A newly discovered phenomenon was that the bimodal-FG specimens promoted the formation of geometrically necessary dislocation (GND) and DIM compared to the unimodal-FG, which was due to the uneven deformation in grains located on hetero-boundaries (HBs). Moreover, the bimodal-FG specimen was preferentially formed DIM on HBs, especially in the smaller grains side rather than inside larger grains due to the higher stress concentration in smaller grains.

Unraveling the friction and wear mechanisms of surface nanostructured stainless-steel

In an effort to improve the friction and wear resistance of coarse grain (CG) 316L stainless steel (SS), the influence of surface nanostructuring formed by a novel surface mechanical rolling treatment (SMRT) technology was investigated. The tribological tests performed in this work consisted of dry reciprocating ball-on-flat tests using Al2O3 as the counter substrate. Results indicate that the SMRT process improved the abrasion resistance of the CG specimen at 15 N, 30 N, and 45 N loads. This finding was due to the combination of surface strengthening, surface smoothening, and the martensite phase transformation induced by SMRT treatment. Aside from the observed change in abrasion resistance, the frictional response of the SMRT specimen was lower than the CG specimen across all loads. Interestingly, the coefficient of friction (COF) for both the CG and SMRT specimens was observed to decrease as the load increased. The formation of surface oxidation contributed to this decrease, as a protective oxide layer was formed. As the load increased, a greater amount of frictional energy was converted into surface oxidation, which reduced the frictional response. Scanning electron microscope (SEM) and energy dispersive X-ray spectroscopy (EDS) investigations of the worn surfaces confirmed these findings, indicating that a combination of oxidative and abrasive wear took place. Collectively, these findings indicate that SMRT treatment is a viable technique to improve the tribological resistance of CG 316L SS.

Grain size independence of cryogenic strain recovery behavior in high-Zr β-Ti alloy

A significant increase in the recovery strain of a high-Zr β-Ti alloy from 2.25 % to 5.5 % when decreasing the deformation temperature from 300 K to 77 K is reported in this study. It is found that the super-elasticity of this alloy is independent of the β-grain size at 77 K. The results reveal that a coarse-grained specimen exhibited approximately the same super-elasticity as its ultra-fine grain counterpart at 77 K. The relative easiness of deformation-induced martensitic transformation and dislocation slip was substantially changed at 77 K, with a strong suppression of dislocation slip, which overshadowed the effect of grain refinement on the super-elasticity.

Microstructure relevant fatigue short crack propagation behavior of Al0.3CoCrFeNi high entropy alloy: in-situ SEM study

The microstructure effects on fatigue short crack propagation behavior of Al0.3CoCrFeNi high entropy alloys (HEAs) were studied by in-situ fatigue testing under scanning electron microscope (SEM). The experimental results indicated that fine grain (FG) specimens had better fatigue crack propagation resistance and higher fatigue life compared with coarse-grain (CG) specimens. Fatigue short crack propagation followed transgranular mode, associated with octahedral slip. The fatigue small crack growth is primarily microstructurally sensitive, showing evident fluctuations related to the blocking effects of grain boundaries and twin boundaries. Furthermore, a modified fatigue crack growth model has been proposed, which can successfully evaluate the crack growth rates of HEAs with different grain microstructures under different fatigue stresses.

Corrosion Resistance of the Welded Joints from the Ultrafine-Grained Near-α Titanium Alloys Ti-5Al-2V Obtained by Spark Plasma Sintering

A solid-phase diffusion welding of coarse-grained and ultrafine-grained (UFG) specimens of titanium near-α alloy Ti-5Al-2V used in nuclear power engineering was made by Spark Plasma Sintering. The failure of the welded specimens in the conditions of hot salt corrosion and electrochemical corrosion was shown to have a preferentially intercrystalline character. In the case of the presence of macrodefects, crevice corrosion of the welded joints was observed. The resistance of the alloys against the intercrystalline corrosion was found to be determined by the concentration of vanadium at the titanium grain boundaries, by the size and volume fraction of the β-phase particles, and by the presence of micro- and macropores in the welded joints. The specimens of the welded joints of the UFG alloy are harder and have a higher resistance to hot salt corrosion and electrochemical corrosion.

Surface hardening of TiZrNbHfTa high entropy alloy via oxidation

We investigate the oxidation of TiZrNbHfTa high entropy alloy between 550 °C and 650 °C as a surface hardening method. Coarse-grained specimens with grain boundaries perpendicular to the surface exhibit catastrophic oxidation, while ultrafine-grained, cold-rolled specimens show a continuous mass gain and the formation of an adherent, µm-sized, vitreous oxide layer. Underneath, TiZrNbHfTa decomposes into a bcc- and an hcp-phase, while selective internal oxidation of hafnium and zirconium occurs upon oxygen inward diffusion. Oxygen concentration- and microhardness-depth profiles confirm an increase in oxygen concentration and hardness at the surface, raising the initial hardness by four times to 1522 ± 64 HV0.5.

Dependence of Charpy Impact Properties of Fe-30Mn-0.05C Steel on Microstructure

Fe-30Mn-0.05C steel specimens with cold-rolled, partially recrystallized, fine-grained, and coarse-grained microstructures were fabricated by means of 80% cold rolling followed by annealing at 550–1000 °C. The initial and deformed microstructures were characterized, and the Charpy impact properties were tested at room temperature (RT) and liquid nitrogen temperature (LNT). It was found that the Charpy absorbed energy increased with the annealing temperature, while the specimens showed different trends: parabolic increase at RT and exponential increase at LNT, respectively. Compared with the fully recrystallized specimens, those with a partially recrystallized microstructure exhibited lower impact energy, especially at LNT. This was because cracks tended to nucleate and propagate along the recovery microstructure where stress concentration existed. The grain size played an important role in the twinning behavior and impact properties. High Charpy impact energy (~320 J) was obtained in the coarse-grained specimen having the grain size of 42.1 μm at both RT and LNT, which was attributed to the activation of high-density deformation twinning. However, deformation twinning was inhibited in the specimen with the average grain size of 3.1 μm, resulting in limited work hardening and lower impact energy.

Phase Equilibrium of Methane Hydrate in Sediments: Experimental and Theoretical Characterization

A series of phase equilibrium tests were performed to explore the influence of various experimental conditions, including initial water content, dry density, and salt content, on the phase equilibrium behavior of methane hydrate in fine- and coarse-grained sediments. The results indicate that the phase equilibrium condition of pore hydrate is significantly influenced by the adopted experimental conditions and the sediment types. It is shown that in equilibrium, a unique relationship (the soil hydration characteristic curve (SHCC)) exists among the temperature shift, the unhydrated water, and the amount of dissolved salt. Under salt-free conditions, the SHCC is independent of dry density for coarse-grained specimens, whereas it is slightly influenced by the dry density for fine-grained specimens. A recently developed phase equilibrium model of pore hydrate, which can account for osmotic, capillary, and adsorptive effects, is introduced to interpret the experimental results. It is shown that the SHCC of the coarse-grained specimens can be very well described by the model; for fine-grained specimens, however, the effect of salt content on matric suction has to be taken into account in the model prediction.

Effects of Grain Size, Thickness and Tensile Direction on Yield Behavior of Pure Titanium Sheet

Yield phenomena during the tensile testing of pure titanium sheets of 0.2 mm and 0.4 mm in thickness were investigated in detail focusing on the effects of grain size (d), thickness (t), t/d ratio and tensile direction. With decreasing grain size, the yielding behavior changed from continuous yielding to one accompanied with yield point drop. Upper and lower yield stresses and 0.2%-proof stress followed the Hall–Petch relationship; however, coarse-grained specimens (d ≧ 20 µm) showed larger scatter in 0.2%-proof stress than the others. Consequently, the Hall–Petch coefficient (k) and friction stress (σ0) derived from 0.2%-proof stress are not accurate enough. The values of k and σ0 derived from various yield stresses and tensile directions were in the range of 250–600 MPa·µm0.5 and 30–180 MPa, respectively. Therefore, the validity of stress for yield stress was a concern, and the combination of the lower yield stress in the fine-grain range (d ≦ 20 µm) and 0.2%-proof stress excluding work-hardening in the coarse-grain range (d > 20 µm) was suggested to obtain reliable values of k and σ0, resulting in values of 370–460 MPa·µm0.5 and σ0 65–140 MPa, respectively. Moreover, it was revealed that k decreased and σ0 increased with the increasing angle of tensile direction to the rolling direction, regardless of thickness. The anisotropy of k is presumed to be affected by the grain boundary character rather than the Schmid factor, and neither rigidity nor the length of the Burgers vector are responsible. Meanwhile, the anisotropy of σ0 is verified to be affected by Schmid factors. Furthermore, it was clarified that the t/d ratio hardly affects upper and lower yield stresses (t/d > 14) nor 0.2%-proof stress (1.5 ≦ t/d ≦ 14).

Achieving superior strength and ductility in 7075 aluminum alloy through the design of multi-gradient nanostructure by ultrasonic surface rolling and aging

Aluminum alloys were used in various fields due to their high specific strength and low density. However, the disadvantage of low strength limits its wider application. In this work, the effect of ultrasonic surface rolling process (USRP) and artificial aging on microstructure and mechanical properties of 7075 aluminum alloy were investigated in detail. The results indicated that a multi-gradient nanostructure (MGNS) layer, i.e., grain gradient and precipitation gradient, was generated on the surface of the alloy. The tensile strength of the aged-USRP sample (692 MPa) was about 63 % higher than that of the coarse-grained sample (425 MPa), and the plasticity was comparable to that of the coarse-grained specimen. The underlying mechanisms of grain refinements, precipitation behavior and their effects on tensile properties were quantitatively analyzed. The high strength of the aged-USRP sample originated from grain boundary strengthening, precipitation strengthening, dislocation strengthening and synergistic strengthening. The activation of geometrically necessary dislocations (GNDs) during tensile deformation improved the plastic coordination ability of different microstructures. Thus, excellent strength-ductility synergy of 7075 aluminum alloy was obtained. • Multi-gradient nanostructure was formed on the surface of 7075 Aluminum Alloy. • Gradient nanostructure of type and number density of precipitates formed. • The multi-gradient nanostructure enhanced strength-ductility synergy of the alloy.

Grain size dependant high-temperature hot corrosion (HTHC) degradation behavior in Alloy 617 during exposure in Na2SO4 + NaCl + V2O5 salt mixture

In the present investigation, the implication of grain size on the high-temperature hot corrosion (HTHC) response in Alloy 617 is studied. Towards this, specific thermal and thermo-mechanical processing schedules were employed to attain a wide range of grain sizes (7–70 µm), while maintaining other microstructural features like Σ3 n (n ≤ 3) boundary fraction, retained strain, and precipitate fraction nearly at constant. Subsequently, these specimens were exposed to Na 2 SO 4 + NaCl + V 2 O 5 (75 wt% + 20 wt% + 5 wt%) salt mixture at 1273 K for 24 h. Post-corrosion analyses reveal the formation of a highly porous and thick oxide scale on the as-received (AR) specimen (~32 µm), a relatively less porous and non-uniform oxide scale on the very coarse-grained specimen (~70 µm), and a homogeneous and dense Cr-rich scale on the very fine-grained microstructure (~7 µm). Such a protective scale on the very fine-grained specimen, developed due to the enhanced diffusivity of Cr, obstructs the entry of corrodents and thereby minimizes the percolation depth (~60 µm). The percolation depth is relatively higher (~130 µm) in the very coarse-grained specimen due to the development of a porous and non-uniform oxide scale. However, its percolation depth is still lower than the AR specimen (~ 305 µm), because of the reduced grain boundary area available for the diffusion of the corrosive species into the substrate. The AR specimen has exhibited the maximum percolation depth due to the simultaneous presence of fine and coarse grains, leading to the failure of both the aforementioned resistive mechanisms i.e., the accelerated formation of a protective Cr-rich scale and lesser availability of diffusion paths for the ingression of the corrosive species. • Very fine and very coarse-grained microstructures are resistant to HTHC damage. • AR specimen with inhomogeneous grain size distribution underwent maximum damage. • Grain refinement accelerates Cr-oxide formation that blocks entry of corrodants. • Grain coarsening decreases the channels for ingression of corrodants into the alloy. • Inhomogeneous grain size distribution in AR fails to activate resistive mechanisms.