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ACTA Vol. 199，15 Oct. 2020, P19-33

In this experiment, the origin of dislocation structures in AM stainless steels was systematically investigated by controlling the effect of thermal stress through geometric constraints for the first time. Stainless steel 316L parts were produced in the form of “1D” rods, “2D” walls, and "3D" rectangular prisms to evaluate the effect of constraints to thermal expansion/shrinkage on the development of defect microstructures and to elucidate the origin of additively manufactured (AM) dislocation microstructures. Dislocation density, organization, chemical micro-segregation, precipitate structures, and misorientations were analyzed as a function of increasing constraints around solidifying material in 1D, 2D, and 3D components built using both directed energy deposition (DED) and powder-bed selective laser melting (SLM). In DED parts, the dislocation density was not dependent on local misorientations or micro-segregation patterns, but evolved from approximately ρ⊥=10¹²m⁻² in 1D parts to ρ⊥=10¹⁴m⁻² in 3D parts, indicating that it is primarily thermal distortions that produce AM dislocation structures. In DED 3D parts and SLM parts, dislocation densities were highest (ρ⊥≈1014m-2) and corresponded to the formation of dislocation cells approximately 300-450 nm in diameter. Dislocation cells overlapped with dendrite micro-segregation in some but not all cases. The results illustrate that dendritic micro-segregation, precipitates, or local misorientations influence how the dislocations organize during processing, but are not responsible for producing the organized cell structures. This work shows that AM dislocation structures originate due to thermal distortions during printing, which are primarily dictated by constraints surrounding the melt pool and thermal cycling.

ACTA Vol. 199, 15 Oct. 2020, P42-52

Grain boundary (GB) migration associated with grain growth and recrystallization encounters lattice defects frequently, while the atomistic mechanisms of GB-defect interactions during these dynamic processes remain largely unclear. Here, we systematically investigate the atomistic mechanism of the interactions between migrating Σ11(113) symmetrical tilt GBs and different lattice defects, including full dislocation, stacking fault and nanotwin in Au, via the integrated in situ nanomechanical testing and molecular dynamics simulations. Experimental evidence demonstrated a conservative defect accommodation mechanism of Σ11(113) GB and a coupled GB-twin evolution, where localized atom displacement dominated the GB-defect interactions. Moreover, the shear-coupled GB migration was unperturbed by the interaction, due to the glissile residual disconnections left on the GB. These findings provide a comprehensive experimental understanding on the atomistic mechanism of GB migration under the influence of different lattice defects, which significantly advances the theoretical development of GB-dominated plasticity under more realistic circumstances.

ACTA Vol. 199, 15 Oct. 2020, P53-62

英文摘要

ACTA Vol. 199, 15 Oct. 2020, P63-72

Solute segregation at grain boundaries (GBs) is known to have a profound impact on material properties, and as such is becoming routinely used as an element in alloy design. Beyond the dilute limit, the extent of solute GB segregation is known to be concentration dependent. Using hybrid Monte Carlo/Molecular Statics simulations of Mg segregation in Al, we decouple the two contributions to this composition dependence: (i) spectrality of atomic environments at the boundary and (ii) solute-solute interactions. Although only contribution (ii) is typically considered in the literature, we argue that both contributions are equally important to understand concentration dependence and correctly quantify GB solute segregation in a binary alloy. Finally, a thermodynamic segregation isotherm is outlined that accounts for both the spectrality of grain boundary sites and solute-solute interactions. Unlike classical isotherms like those of McLean or Fowler-Guggenheim, which can be successfully fitted to GB segregation data only over a limited range of composition and temperature, our proposed model is shown to be accurate across the composition-temperature space.

ACTA Vol. 199, 15 Oct. 2020, P73-84

This work probes the effect of ultrasonic melt treatment (UST) on primary intermetallic particles and α-Al using pure Al and Al–Zr alloys (Al–0.3Zr–0.1Ti, Al–0.5Zr, Al–0.5Zr–0.5Mg–0.9Si) solidified at various cooling rates of 0.2–70 K s−1. The application of UST is shown to decrease the size and increase the number density and volume fraction of D023-structured primary Al3Zr and Al3(Zr,Ti) particles with a high nucleation potency for α-Al formation. High-resolution transmission electron microscopy analysis reveals that the cavitation-induced wetting and dispersion of γ-Al2O3 inoculant particles contribute to the refinement of primary intermetallic particles. The grain size of Al–Zr alloys increases with increasing cooling rate because of the concomitantly reduced formation of primary intermetallic inoculant particles. The UST-induced refinement of primary Al3Zr particles and the increased number density lead to grain refinement in Ti-free Al–Zr alloys. For the Ti-containing Al–Zr alloy, UST-induced grain refinement is achieved only at a very low cooling rate of 0.2 K s−1, possibly because of the side effects of UST on the growth-restricting influence of Ti. The fast cooling–induced solidification enables significant age-hardening by L12-Al3Zr nanoprecipitation (~5 nm) and is not affected by UST. Thus, this study shows that UST can be used to reduce the degree of grain coarsening of age-hardenable Al–Zr alloys at high cooling rates.

ACTA Vol. 199, 15 Oct. 2020, P107-115

This study reports a thermodynamic route for self-forming an ultrathin V-Nb-Mo-Ta-W high-entropy alloy layer for potential use as a promising diffusion barrier. In Cu alloy films minor-doped with 1.2 at.% of one-to-five metallic elements (V, Nb, Mo, Ta and W), the alloying elements spontaneously segregated. Under the competition of enthalpy and mixing entropy that determines the delta Gibbs free energy, one and, in particular, five alloying element(s) formed an alloy solution layer at the Cu/Si interface, whereas three alloying elements differently formed intermetallic compound clusters at the grain boundaries of Cu. Dominant factors for the final states of the alloying elements include the large positive enthalpy between Cu and the alloying elements, the negative enthalpy among the alloying elements, and the low-to-high mixing entropy among the alloying elements. The self-forming quinary alloy layer of only 1.5 nm thick provided excellent resistance to the interdiffusion of Cu and Si up to 700°C, better than practical and other newly developed barrier materials.

ACTA Vol. 199, 15 Oct. 2020, P116-128

In this paper, we develop a mean-field model for simulating the microstructure evolution of crystalline materials during static recrystallization. The model considers a population of individual cells (i.e. grains and subgrains) growing in a homogeneous medium representing the average microstructure properties. The average boundary properties of the individual cells and of the medium, required to compute growth rates, are estimated statistically as a function of the microstructure topology and of the distribution of crystallographic orientations. Recrystallized grains arise from the competitive growth between cells. After a presentation of the algorithm, the model is compared to full-field simulations of recrystallization performed with a 2D Vertex model. It is shown that the mean-field model predicts accurately the evolution of boundary properties with time, as well as several recrystallization parameters including kinetics and grain orientations. The results allow one to investigate the role of orientation spreads on the determination of boundary properties, the formation of recrystallized grains and recrystallization kinetics. The model can be used with experimentally obtained inputs to investigate the relationship between deformation and recrystallization microstructures.

ACTA Vol. 199, 15 Oct. 2020, P129-140

Ti-Nb based alloys exhibit superelastic and shape memory properties over a wide range of temperatures, making them attractive for industrial applications. However, within the literature there are significant variations in the reported transformation behaviour for a given composition that remain unexplained. These variations are problematic to engineering design and limit the industrial uptake of these alloys. To investigate the source of these discrepancies, the transformation behaviour of Ti-24Nb (at.%) in two significantly different microstructural conditions, following cold rolling (CR) and following a subsequent solution heat treatment (ST), has been studied using in situ synchrotron diffraction data whilst undergoing a three step thermal cycle. When cooling from 350 to -196?C, the CR condition material underwent both the β to α? and β to ω transformations, whilst only the β to ω transformation was observed in the ST condition material. These results show that the transformation behaviour of Ti-Nb alloys, in particular the β to α? transformation, is significantly influenced by prior processing and that theories of mutual exclusivity between α? and ω phase formation need revisiting. In addition, several features within the datasets were inconsistent with a solely thermally driven martensite formation mechanism and an alternative description that includes other factors is discussed.

ACTA Vol. 199, 15 Oct. 2020, P141-154

Nanocrystalline (NC) materials possess excellent room temperature properties, such as high strength, wear resistance, and toughness as compared to their coarse-grained counterparts. However, due to the excess free energy, NC microstructures are unstable at higher temperatures. Significant grain growth is observed already at moderately low temperatures, limiting the broader applicability of NC materials. Here, we present a design approach that leads to a significant improvement in the high temperature tensile creep resistance (up to 0.64 of the melting temperature) of a NC Cu-Ta alloy. The design approach involves alloying of pure elements to create a distribution of nanometer sized solute clusters within the grains and along the grain boundaries. We demonstrate that the addition of Ta nanoclusters inhibits the migration of grain boundaries at high temperatures and reduces the dislocation motion. This leads to a highly unusual tensile creep behavior, including the absence of any appreciable steady-state creep deformation normally observed in almost all materials. This design strategy can be readily scaled-up for bulk manufacturing of creep-resistant NC parts and transferred to other multicomponent systems such as Ni-based alloys.

ACTA Vol. 199, 15 Oct. 2020, P169-180

英文摘要

ACTA Vol. 199, 15 Oct. 2020, P181-192

After pre-charging at the gaseous phase with a concentration of ~7,000 at. ppm, solute hydrogen was discovered to have an abnormal effect on both the strength and ductility enhancement of a commercially-available, Fe-24Cr-19Ni-based, stable austenitic stainless steel that had been subjected to tensile testing at various strain-rates. Specifically, the impact of hydrogen on material strength was accompanied by amplified yield and flow stresses, as well as tensile strength, while the improvement in ductility featured extended uniform elongation and strain-to-fracture, both of which became more pronounced as hydrogen concentration intensified. The product between tensile strength and uniform elongation served as indicators of the strength-ductility balance, at which hydrogen maximally optimized the indicator at the particular intermediate strain-rate. The yield/flow stress augmentations were interpreted in terms of solid-solution strengthening, whereas the enhanced ductility was primarily ascribed to the facilitation of mechanical twinning, whereby dynamic hydrogen-dislocation interaction exerted a critical influence as was indirectly revealed by supplemental stress-relaxation experiments.

ACTA Vol. 199, 15 Oct. 2020, P193-208

Key mechanisms and elementary diffusion processes that control the growth kinetics of σ precipitates in high-entropy alloys were investigated in the present study. For this purpose, an off-equiatomic Cr26Mn20Fe20Co20Ni14 alloy with an initially single-phase FCC structure was subjected to isothermal heat treatments, which are known to promote the formation of σ phase, i.e., aging between 600 °C and 1000 °C for times ranging from 0.1 h to 1000 h. The growth kinetics of σ precipitates at grain boundaries of the FCC matrix and those located within the interior of the grains were analyzed separately. The latter precipitates are found to grow through direct substitutional diffusion of Cr-solutes towards and Mn, Fe, Co, and Ni away from them and the growth rate of the allotriomorphs can be rationalized by the collector plate mechanism of interfacial diffusion-aided growth. From the growth-kinetics data obtained in the present study, lattice interdiffusion coefficients as well as diffusivities along crystalline defects were obtained. Above 800 °C, the growth kinetics are dominated by lattice interdiffusion of Cr in the FCC matrix described by DL = 9.8×10-4exp[(-300 kJ/mol)/(RT)] m2/s. At lower temperatures, the growth kinetics are enhanced by fast interdiffusion along dislocation pipes, which temperature dependence is given by DD = 5.0×10-3exp[(-205 kJ/mol)/(RT)] m2/s. The Cr-diffusivity along σ/FCC interphase boundaries deduced from the thickening kinetics of grain boundary precipitates can be represented by the Arrhenius relationship DI = 0.5×10-4exp[(-145 kJ/mol)/(RT)] m2/s, which is similar to that found for grain boundary interdiffusion in metals and alloys.

ACTA Vol. 199, 15 Oct. 2020, P209-224

Superlattice stacking fault propagation dominates the creep deformation behaviour of nickel-based superalloys at intermediate temperatures. These planar defects may appear under many different configurations depending on the dislocation arrangements and their interactions with the precipitates. Whilst these have been spotted and described before, no systematic way to explain their configurations has been provided. The current study quantifies the types of faults in multiple grains within a tensile crept polycrystalline alloy via a combination of scanning transmission electron microscopy and electron backscatter diffraction. A new defect consisting of a superlattice intrinsic stacking fault in the precipitates and an extrinsic stacking fault in the matrix is observed and a mechanism for its formation is proposed. In combination with data from the literature on single crystals, the results are incorporated into a robust framework to discern the orientation dependencies of these faults. A comprehensive analytical model based on a series of one-dimensional force balances on different dislocation configurations is developed first for the case of athermal stacking fault propagation for the cases of cuboidal and spherical precipitates. The model is then extended to include six configurations of superlattice faults and microtwinning. This results in novel mechanistic maps that account for stress, orientation and microstructure, with excellent qualitative agreement with experiments.

ACTA Vol. 199, 15 Oct. 2020, P225-239

The microstructures and mechanical properties of the 316L austenitic stainless steel fabricated using binder jet printing (BJP) and selective laser melting (SLM) were investigated and compared with those of the conventionally manufactured (CM) alloy, with particular emphasis on the unnotched fatigue resistance. Results show that the work hardening behavior, ductility, and fatigue strength (σf) of the BJP specimens, which contain significant amounts of pores, are surprisingly comparable to those of the CM alloy. In contrast, the SLM specimens are considerably stronger, especially in terms of the yield strength, less ductile, and far inferior in terms of σf although the porosity in them is relatively smaller as compared to the BJP specimens. These results are rationalized by recourse to the distinct microstructures in the two additively manufactured alloys, which stem from the different processing conditions experienced by them. The planar slip regime that prevails in the early stages of plastic deformation of the BJP alloys and a combination of other microstructural factors lead to the arrest of small cracks that nucleate at the corners of the pores, both under quasi-static and cyclic loads; as a result, neither ductility nor fatigue strength are adversely affected by the porosity in the BJP alloys. In the SLM alloy, the cellular structure, which enhances the yield strength considerably, is too fine whereas the columnar grains are minimally misoriented and coarse enough to induce any crack deflection or arrest. Implications of these results in terms of possible directions for designing AM alloys with high mechanical performance are discussed.

ACTA Vol. 199, 15 Oct. 2020, P240-252

Much progress has been made over the past few decades in resolving the mechanism for the transformation from ordered body-centered-cubic (B2) austenite to monoclinic martensite (B19′) in NiTi shape memory alloy, as well as the twinning mechanisms in martensite. However, so far no lattice correspondence analyses on the atomic scale have been conducted, as a result, these mechanisms have not been completely understood in terms of the pathways for reversible phase transition and reversible twinning in martensite. In this work, atomistic simulations were performed to investigate how B2 austenite transforms to B19′ martensite and how twins are formed during phase transformation. In particular, lattice correspondence in the structural evolutions was carefully analyzed to reveal the martensitic transformation mechanism and twinning mechanism with much better clarity. The simulation results show that, when martensite grains were nucleated in austenite, they already formed a twin relationship as a natural result of the crystal structure. Thus, self-accommodation is achieved naturally. Coalescence occurred subsequently and some martensite grains grew at the expense of their neighbors, indicating that the interfaces are elastically mobile and their migration is reversible. Eventually twinned martensite variants were created. It is shown that, in the B2 → B19′ transformation, the B19′ monoclinic structure can be treated as a distorted hexagonal close-packed (HCP) structure. With this treatment, it is demonstrated that the martensitic transformation is essentially similar to BCC ↔ HCP transformation which only involves atomic shuffles and is reversible, and twinning in martensite is essentially similar to {101-2} twinning in HCP metals which only involves atomic shuffles and is reversible as well. Another significant discovery is that the B19′ martensite exhibits a very special dual-lattice structure: the relatively weak Ti-Ti bonding of the monoclinic unit cell permits easy reorientation of lattice units. As a result, two differently oriented lattice units co-exist in the same martensite grain which loses long range periodicity, providing an extra degree of freedom for accommodating external and internal strains. These results explain well why B19′ martensite is extremely adaptive to straining and why deformation is reversible.

ACTA Vol. 199, 15 Oct. 2020, P253-263

We investigate the influence of microstructural traps on hydrogen diffusion and embrittlement in the presence of cyclic loads. A mechanistic, multi-trap model for hydrogen transport is developed, implemented into a finite element framework, and used to capture the variation of crack tip lattice and trapped hydrogen concentrations as a function of the loading frequency, the trap binding energies and the trap densities. We show that the maximum value attained by the lattice hydrogen concentration during the cyclic analysis exhibits a notable sensitivity to the ratio between the loading frequency and the effective diffusion coefficient. This is observed for both hydrogen pre-charged samples (closed-systems) and samples exposed to a permanent source of hydrogen (open-systems). Experiments are used to determine the critical concentration for embrittlement, by mapping the range of frequencies where the output is the same as testing in inert environments. We then quantitatively investigate and discuss the implications of developing materials with higher trap densities in mitigating embrittlement in the presence of cyclic loads. It is shown that, unlike the static case, increasing the density of “beneficial traps” is a viable strategy in designing alloys resistant to hydrogen assisted fatigue for both closed- and open-systems.

ACTA Vol. 199, 15 Oct. 2020, P278-287

Investigation on the cyclic response of metallic materials in very high cycle fatigue (VHCF) is a challenging problem, which hinders the development of fatigue theories. To overcome this difficulty, we initially applied several sensible techniques, e.g., High-energy X-ray diffraction (HEXRD), confocal laser scanning microscope (CLSM), nanoindentation and transmission electron microscope (TEM) to investigate the cyclic response of a duplex stainless steel (DSS) in the VHCF regime. In-situ XRD and in-situ digital image correlation (DIC) experiments were subsequently performed at observed changing stages, intending to explore the underlying mechanism of microcrack initiation. The first-hand results obtained revealed that the austenite phase exhibits cyclic softening-hardening-softening behavior during the VHCF process. The in-situ investigations performed at the cyclic softening and hardening stages showed a load partitioning and a load transfer between the two phases, implying the cyclic response can significantly affect the distribution of the applied load. Residual strain obtained by DIC technique after unloading exhibited strong variations at phase boundaries, suggesting micro residual stresses have developed pronouncedly. Based on all the experimental findings, a unified crack initiation mechanism for the investigated DSS during VHCF loading was proposed.