Twin Fault Probability Research Articles

Nanostructuring of an additively manufactured CoCrFeNi multi-principal element alloy using severe plastic deformation: Comparison of two materials processed by different laser scan speeds

Experiments were conducted to reveal the refinement of the microstructure and the evolution of the hardness of an additively manufactured (AM) CoCrFeNi multi-principal element alloy (MPEA) processed by severe plastic deformation (SPD) using high pressure torsion (HPT) technique. AM was carried out by laser powder bed fusion (L-PBF) technique at two different laser scan speeds. The as-built alloys for both laser scan speeds have a single-phase face-centered cubic (fcc) structure with <110> fiber texture parallel to the building direction. X-ray line profile analysis (XLPA) revealed that the dislocation density was considerably high even in the AM-processed state before HPT (3 × 1014 m−2) which increased by two orders of magnitude during HPT. The saturation of the lattice defects (dislocation density and twin fault probability) as well as the crystallite size occurred at a shear strain of about 10 during HPT. In both AM-processed alloys, <111> fiber texture developed parallel to the normal of the HPT-processed disks. For both laser scan speeds, the initial grain size in the AM-processed samples was refined from 70 to 90 μm to the nanocrystalline regime after 10 turns of HPT. Additionally, nanotwins formed with a probability of about 3 %. The initial hardness of the AM-processed MPEA samples for both laser scan speeds was 2700–2800 MPa, which is superior to that of CoCrFeNi produced by casting (about 1380 MPa). This can be explained by the high dislocation density in the AM-processed specimens. The formation of nanostructure with high lattice defect density during HPT resulted in a very high hardness value of about 5500 MPa in the AM-processed CoCrFeNi MPEA samples for both laser scan speeds.

Nanostructuring of Additively Manufactured 316L Stainless Steel Using High-Pressure Torsion Technique: An X-ray Line Profile Analysis Study.

Experiments were conducted to reveal the nanostructure evolution in additively manufactured (AMed) 316L stainless steel due to severe plastic deformation (SPD). SPD-processing was carried out using the high-pressure torsion (HPT) technique. HPT was performed on four different states of 316L: the as-built material and specimens heat-treated at 400, 800 and 1100 °C after AM-processing. The motivation for the extension of this research to the annealed states is that heat treatment is a usual step after 3D printing in order to reduce the internal stresses formed during AM-processing. The nanostructure was studied by X-ray line profile analysis (XLPA), which was completed by crystallographic texture measurements. It was found that the as-built 316L sample contained a considerable density of dislocations (1015 m-2), which decreased to about half the original density due to the heat treatments at 800 and 1100 °C. The hardness varied accordingly during annealing. Despite this difference caused by annealing, HPT processing led to a similar evolution of the microstructure by increasing the strain for the samples with and without annealing. The saturation values of the crystallite size, dislocation density and twin fault probability were about 20 nm, 3 × 1016 m-2 and 3%, respectively, while the maximum achievable hardness was ~6000 MPa. The initial <100> and <110> textures for the as-built and the annealed samples were changed to <111> due to HPT processing.

Evading the strength-ductility compromise in medium manganese steel by a novel low temperature warm rolling treatment

Strength-ductility trade-off is an enduring problem in a wide range of metals and alloys including the advanced high-strength steels. In this work, we propose a novel non-isothermal low-temperature warm rolling (WR) treatment which was applied after the conventional intercritical annealing (IA) in order to overcome the strength-ductility compromise in a medium manganese steel, Fe-5.1Mn-0.22C-0.85Si-0.42Al (composition in wt%). IA + WR treatment yielded a simultaneous improvement in tensile properties, wherein yield strength (YS), ultimate tensile strength (UTS), and ductility improved by 32%, 12%, and 6% respectively, compared to the conventional IA treatment. Despite an increase in the yield point elongation (2%) and Lüders strain (3%) in the IA + WR specimen, the ductility of the same improved as compared to the IA specimen. Microstructure of the IA + WR specimen was tailored by introducing a significantly higher dislocation density in the constituent ferrite and retained austenite (RA) phases along with a relatively higher density of planar defects (stacking faults and nano-twins) in the RA phase. X-ray line profile analysis quantified the increased dislocation density (order ∼1015 vs 1014 m−2) and twin fault probability (∼1.35% vs ∼0.12%) in the RA phase of the IA + WR compared to the IA specimen. The improvement in YS was primarily due to the increase in the dislocation density of the constituent phases in the IA + WR specimen. Introduction of a high density of lattice defects in the RA phase during the WR treatment above the Md30 temperature enhanced the mechanical stability of the RA phase, leading to a decreased rate of TRIP effect and formation of hierarchical twins during tensile deformation. The near-ubiquitous strength-ductility trade-off was overcome via a tailored microstructure consisting of regulated austenite stability leading to discontinuous TRIP effect, hierarchical twinning in RA phase, and favorable texture in the constituent phases. The present study provides a pathway to tailor the microstructure for escaping the strength-ductility paradox in different metastable FCC alloys such as stainless steel, HEAs, TWIP steels etc.

X-ray line profile analysis study on the evolution of the microstructure in additively manufactured 316L steel during severe plastic deformation

316L stainless steel was manufactured by additive manufacturing (AM), and then, the samples were severely deformed by the high-pressure torsion (HPT) technique. The evolution of the microstructure was monitored by X-ray line profile analysis. This method gives the crystallite size and the density of lattice defects, such as dislocations and twin faults. The AM-processing of the HPT disks was performed in two different modes: the laser beam was parallel or orthogonal to the normal direction of the disks. The subsequent HPT deformation was carried out for ½, 1, 5 and 10 turns. The microstructure and hardness evolution during HPT were similar regardless of the laser beam direction. For both sample series, the minimum achievable crystallite size was about 30 nm, while the dislocation density and the twin fault probability got saturated at the values of 300–350 × 1014 m−2 and 3.5–4%, respectively. The microstructure evolution during HPT of the AM-prepared 316L steel was compared with the HPT-induced changes in an as-cast counterpart. It was found that while the AM-prepared 316L steel remained a single-phase face-centered cubic γ-structure during HPT, in the as-cast samples a body-centered cubic (bcc) martensitic α-phase became the main phase with increasing the imposed strain of HPT due to the lower Ni content. In the saturation state achieved by HPT the initially as-cast 316L steel had a considerably higher hardness (about 6000 MPa) than that for the AM-prepared samples (~ 5000 MPa) due to the large fraction of the hard bcc phase formed during HPT.

Effect of Si on the evolution of plasticity mechanisms, grain refinement and hardness during high-pressure torsion of a non-equiatomic CoCrMnNi multi-principal element alloy

The present study unraveled the defining role of small silicon (Si) addition (5 atomic %) in dramatically altering the plasticity mechanisms, grain refinement and hardening response of a non-equiatomic CoCrMnNi multi-principal element alloy (MPEA) during high-pressure torsion (HPT) processing. Both the Si-free and the Si-added MPEAs had a face-centered cubic (FCC) structure and were subjected to a quasi-constrained HPT processing at 6 GPa pressure to different number of turns (0.5 and 5). Microstructure evolution was studied at the center and edge of the HPT-processed discs using X-ray diffraction line profile analysis (XLPA) and transmission electron microscopy (TEM). Si addition altered the predominant plasticity mechanism from micro-band formation to extensive occurrence of nano-twinning at the early stage of HPT processing. At later stages of HPT processing, both alloys exhibited deformation twinning but its propensity was considerably higher for the Si-added MPEA, as revealed by ∼50% higher twin fault probability. Additionally, the Si-added MPEA showed ∼30% higher dislocation density at any given stage of HPT processing compared to the Si-free MPEA. A significantly accelerated nano-structuring coupled with a finer saturation grain size was observed in the Si-added MPEA (34 nm for Si-free versus 23 nm for Si-added). These effects can be explained by the influence of Si addition on lowering the stacking fault energy (SFE) (from ∼40 mJ/m2 in Si-free to ∼20 mJ/m2 in Si-added MPEA) and increasing the solute pinning effect of Si on lattice defects. The plasticity mechanisms at nano-scale were also influenced by the presence of Si as confirmed by the formation of nano-twins and stacking faults inside the nano-grains for the Si-added and Si-free MPEAs, respectively. The differences in plasticity mechanisms and microstructure evolution resulted in enhanced hardness in the early stages of HPT processing for the Si-added MPEA, but the difference in hardness between the two alloys tended to be reduced at higher strains.

Competitive strengthening between dislocation slip and twinning in cast-wrought and additively manufactured CrCoNi medium entropy alloys

In situ neutron diffraction experiments have been performed under loading in cast-wrought (CW) and additively manufactured (AM) equiatomic CoCrNi medium-entropy alloys. The diffraction line profile analysis correlated the faulting-embedded crystal structure to the dislocation density, stacking/twin fault probability, and stacking fault energy as a function of strain. The results showed the initial dislocation density of 1.8 × 1013m−2 in CW and 1.3 × 1014m−2 in AM. It significantly increased up to 1.3 × 1015m−2 in CW and 1.7 × 1015m−2 in AM near fracture. The dislocation density contributed to the flow stress of 470 MPa in CW and 600 MPa in AM, respectively. Meanwhile, the twin fault probability of CW (2.7%) was about two times higher than AM (1.3%) and the stacking fault probability showed the similar tendency. The twinning provided strengthening of 360 MPa in CW and 180 MPa in AM. Such a favorable strengthening via deformation twinning in CW and dislocation slip in AM was attributed to the stacking fault energy. It was estimated as 18.6 mJ/m2 in CW and 37.5 mJ/m2 in AM by the strain field of dislocations incorporated model. Dense dislocations, deformation twinning, and atomic-scale stacking structure were examined by using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM).

On the enhanced hardening ability and plasticity mechanisms in a novel Mn-added CoCrNi medium entropy alloy during high-pressure torsion

Microstructure and texture evolution during high-pressure torsion (HPT) of a novel Mn-added CoCrNi medium entropy alloy (Co33Ni33Cr19Mn15) is investigated for the first time. The alloy exhibited a rapid rise in hardness at relatively low shear strains (γ≤20). It is attributed to an extensive dislocation activity to achieve saturation in dislocation density of ~1016 m−2, combined TWIP and TRIP effects and microstructural refinement. At higher shear strain, hardness increased at much reduced rates owing to saturation of dislocation density, twin fault probability and the TRIP effect, besides continued grain refinement for severe nano-structuring led to subsequent strengthening. The FCC phase showed remarkable stability except a small degree of initial deformation-induced HCP martensitic transformation in an early stage of HPT. The ideal shear texture components were observed at low shear strain, and these continued to evolve up to 5 turns of HPT processing. For similar HPT processing conditions, the studied alloy showed superior hardness (~650 Hv) compared to a wide spectrum of FCC materials, which is ascribed to a combination of the strengthening mechanisms of Taylor hardening, the TRIP and TWIP effects and Hall-Petch strengthening resulting from the nano-structured grains having an average size of ~35 nm.

Temperature-dependent hardening contributions in CrFeCoNi high-entropy alloy

We studied the deformation behavior of CrFeCoNi high-entropy alloy by in situ neutron diffraction at room temperature, intermediate low temperature of 140 K, low temperatures of 40 K (no serrated deformation) and 25 K (with massive serrations). The evolution of lattice strain and texture along different grain orientations provided distinct insights into deformation behavior at low temperatures. The in situ data showed an early activation of stacking faults and a higher stacking fault probability with decreasing test temperature. The stacking fault probability reached ∼4.7% at low temperatures. The dislocation density at 40 and 25 K evolved similarly and had a very high value of ∼9.2 × 1015 m−2. However, twin fault probability at 25 K (∼6%) was higher than that at 40 K (∼5%). The samples at 40 and 25 K deformed uniformly and lacked any necking region, thus imparting an excellent ductility of ∼58%. The contributions from different deformation mechanisms to the yield strength and strain hardening have been estimated. The athermal contributions to the yield strength were ∼183 MPa at all temperatures, while the Peierls stress increased significantly at low temperatures (from 148 MPa at room temperature to 493 MPa at 25 K). Dislocations contributed to ∼94% strain hardening at room temperature. Although the dislocation strengthening remained the major hardening mechanism at very low temperatures, the planar faults contribution increased steadily from 6% at room temperature to 28% at 25 K.

Effects of strain rate on mechanical properties of heterogeneous nano-structured SUS316LN stainless steel: Revealed by in-situ X-Ray diffraction at synchrotron radiation facility

A SUS316LN austenitic stainless steel was heavily cold rolled to develop heterogeneous nano (HN)-structure. And the effects of strain rate on the tensile deformation behavior of the HN-structured SUS316LN stainless steel were investigated. For this purpose, changes in lattice defect densities, such as dislocation density and stacking fault probability, during the tensile tests were investigated by means of in-situ X-ray diffraction (XRD) measurements at a synchrotron facility. The strength and elongation to failure simultaneously increased with increasing applied strain rate. The analyses of XRD profiles and microstructural observation revealed that twin fault probability as well as dislocation density and stacking fault probability increased with increasing strain rate. The more enhanced formation of ultra-fine twins by the increase in strain rate led to higher work hardening and resulted in more excellent strength/ductility balance.

Influence of the preparation conditions on the microstructure of electrodeposited nanocrystalline Ni–Mo alloys

Structural parameters of electrodeposited Ni–Mo alloys with Mo concentrations up to 6.1 at% were determined by X-ray line profile analysis as a function of various deposition parameters such as pH, Mo(VI) concentration of the bath and deposition current density. In addition to crystallite size, parameters describing the defect structure, such as twin fault probability and dislocation density, were also determined. These microstructural parameters cannot be obtained using classical evaluation methods of X-ray diffractograms. It was found that the crystallite size decreased while the defect density increased with increasing Mo content of the deposits in a sample series where the single variable was the Mo(VI) concentration of the bath. A similar trend was found when the current density was varied for a sample series processed with constant Mo(VI) concentration. However, the comparison of the different sample series revealed that the defect structure is a result of a complex interplay of all deposition conditions and is not solely related to the Mo content of the deposits. The influence of the electrodeposition parameters on the defect structure is discussed in detail.

Improved Hardness and Thermal Stability of Nanocrystalline Nickel Electrodeposited with the Addition of Cysteine.

Experiments were conducted for the study of the effect of cysteine addition on the microstructure of nanocrystalline Ni films electrodeposited from a nickel sulfate-based bath. Furthermore, the thermal stability of the nanostructure of Ni layers processed with cysteine addition was also investigated. It was found that with increasing cysteine content in the bath, the grain size decreased, while the dislocation density and the twin fault probability increased. Simultaneously, the hardness increased due to cysteine addition through various effects. Saturation in the microstructure and hardness was achieved at cysteine contents of 0.3–0.4 g/L. Moreover, the texture changed from (220) to (200) with increasing the concentration of cysteine. The hardness of the Ni films processed with the addition of 0.4 g/L cysteine (∼6800 MPa) was higher than the values obtained for other additives in the literature (<6000 MPa). This hardness was further enhanced to ∼8400 MPa when the Ni film was heated up to 500 K. It was revealed that the hardness remained as high as 6000 MPa even after heating up to 750 K, while for other additives, the hardness decreased below 3000 MPa at the same temperature.

Influence of pack cementation time on the microstructure of Cu nanofoams processed by dealloying

Copper nanofoams were processed by dealloying for a prospective application as a Li-ion battery anode. The precursor material was produced by pack cementation. The effect of length of pack-cementation time on the pore structure and the microstructure of the struts was investigated in this study. It was found that for high pack-cementation times a hierarchical pore structure with nano- and micro-sized pores was formed. In addition, the longer the pack-cementation time, the lower the crystallite size and the dislocation density in the struts. A very high twin fault probability was also detected, irrespective of pack-cementation time.

Comparison of dislocation density, twin fault probability, and stacking fault energy between CrCoNi and CrCoNiFe medium entropy alloys deformed at 293 and 140K

To elucidate deformation behavior behind the exceptional mechanical properties of CrCoNi based medium entropy alloys, the deformation related microstructural parameters were determined by using in situ neutron diffraction and peaks profile analysis methods. Superior tensile strength and elongation of the CrCoNi alloy is relevant to higher twin fault probability (Ptw, up to 3.8%) and dislocation density (ρ, up to 9.7 x 1015 m−2) compared to those (1.3% and 3.4 x 1015 m−2, respectively) of the CrCoNiFe at 293K. Meanwhile, at 140K, the Ptw of the CrCoNiFe significantly increased up to 4.4% with the stable ρ of ~5.0 x 1015 m−2 and its mechanical properties overwhelm those of the CrCoNi at 273K. Such twinning dominant deformation mechanism at low temperature is also assured by lower stacking fault energy (SFE) of the CrCoNiFe (7.4 mJ/m2) at 140K compared to those of the CrCoNi (16.1 mJ/m2) and CrCoNiFe (32.1 mJ/m2) alloys at 293K.

Influence of severe plastic deformation on the microstructure and hardness of a CoCrFeNi high-entropy alloy: A comparison with CoCrFeNiMn

The evolution of microstructure and hardness in a CoCrFeNi high-entropy alloy (HEA) processed by severe plastic deformation (SPD) was studied. SPD-processing was carried out using a high-pressure torsion (HPT) technique up to twenty turns at room temperature that introduces a highest nominal shear strain of about 800. It was found that most of grain refinement and an increase of lattice defect (dislocations and twin faults) density occurred up to the shear strain of ~10. The saturation grain size was about 80 nm, while the maximum values of the dislocation density and the twin fault probability were ~150 × 1014 m−2 and ~3%, respectively. In addition, a 111 texture was formed during HPT-processing. The evolution of hardness with strain followed a trend suggested by the changes in the microstructure. The saturation hardness was as high as ~5100 MPa. The microstructure and hardness obtained for the HPT-processed CoCrFeNi were compared with the values determined formerly for CoCrFeNiMn. It was found that, although the saturation grain size in the CoCrFeNi was much higher than that for the CoCrFeNiMn HEA, the hardness was similar for the two alloys due to the close values of the twin fault probability which can be explained by the similar stacking fault energies.

Study of deformation microstructure of nickel samples at very short milling times: effects of addition of \u03b1-Al2O3 particles

Deformation microstructure of pure Ni powder milled for short duration was studied. The microstructure, as obtained on the basis of Rietveld analysis and microstructural modeling, shows inhomogeneity and consists of ‘heavily deformed’ with twin faults probability and ‘slightly deformed’ components with varying dislocation densities. The modified Williamson–Hall analysis was performed for both the subcomponents with the relevant scaling parameter. Attempts were made to elucidate the nature of dislocation present in the milled samples. The correction due to extra broadening from stacking fault was calculated from the refined values of twin fault probability. In-depth microstructural modeling with restrictedly random distribution of dislocation and a lognormal distribution of spherical particles were done for the two subcomponents to explore the inhomogeneous microstructure. The effect of α-Al2O3 addition is found in reduction in the Ni particle size and yielding more uniform size distribution. It is shown that X-ray line profile analysis is capable of modeling such inhomogeneous microstructure.

Stacking Fault Energy, Dislocation Density, and Twin Fault Probability Determined by Neutron Diffraction Peak Profile Analysis in CrCoNi Based Medium Entropy Alloys

Neutron diffraction peak profile analysis was used to determine stacking fault energy (SFE), dislocation density, and twin fault probability (Ptw) in CrCoNi and CrCoNiFe medium entropy alloys at 293K and 140K. The CrCoNi shows higher Ptw (up to 3.8%) and dislocation density (up to 9.7 x 1015 m-2) than CrCoNiFe (1.3% and 3.4 x 1015 m-2, respectively) at 293K. Meanwhile, at 140K, the Ptw in CrCoNiFe increases significantly to 4.4%. The dominant twinning deformation is due to the lower SFEs of CrCoNi (16.1 mJ/m2) at 293K and CrCoNiFe (7.4 mJ/m2) at 140K compared to 32.1 mJ/m2 for CrCoNiFe at 293K.

The effect of hydrogen charging on the evolution of lattice defects and phase composition during tension in 316L stainless steel

The effects of hydrogen charging on the evolution of strain-induced lattice defects and phase transformation were investigated in 316L stainless steel. The initial material was obtained by cold rolling to a thickness reduction of 20%. The surfaces of some of the initial samples were cathodically charged with hydrogen. Afterward, both the charged and uncharged samples were subjected to tension until failure. The dislocation density and twin-fault probability in the charged and uncharged specimens during tension were compared. We found that hydrogen charging reduced the degree of increase in the dislocation density and twin-fault probability during the application of tension to the same strain level. Significant martensitic phase transformation was observed in the uncharged samples tested to the strain of 10% or higher. In the hydrogen-charged samples, only a slight increase in the martensite phase fraction was detected. A correlation between the α′-martensite fraction and the dislocation density was found for the studied samples, suggesting that the lower degree of martensitic phase transformation in the charged 316L steel was caused by the smaller amount of stress developed due to the lower dislocation density. In accordance with the differences observed in the phase composition and defect densities, the hydrogen-charged material exhibited lower surface hardness.

The influence of Mo addition on the microstructure and its thermal stability for electrodeposited Ni films

An investigation was conducted to study the effect of molybdenum (Mo) alloying on the grain size and lattice defect structure in nanocrystalline nickel (Ni) films processed by electrodeposition. Moreover, the influence of saccharin addition to the electrolyte bath on the microstructure of Ni-Mo layers with low and high Mo contents was studied. It was found that the higher Mo content resulted in a larger dislocation density and twin fault probability as well as a smaller grain size. The addition of saccharin to the bath resulted in a further increase in the density of both dislocations and twin faults. It was also revealed that Mo alloying improved the thermal stability of the nanostructure in Ni films while saccharin addition yielded a reduction of stability. The reasons for these opposite behaviors were discussed in detail. In addition, the defect structure and its stability in Ni-Mo layers were compared with that for fine-grained bulk samples with the same composition but processed by severe plastic deformation.

Effect of bath additives on the microstructure, lattice defect density and hardness of electrodeposited nanocrystalline Ni films

Experiments were performed for the study of the influence of impurities on the microstructure and hardness of nanocrystalline Ni films. The samples were prepared by electrodeposition using two basic electrolyte solutions (a sulfate-type bath and a Watts-type bath). The effect of saccharin as organic additive on the microstructure, texture and hardness was studied. It was found that the Watts bath without saccharin yielded a larger grain size compared to its sulfate-type counterpart. For both electrolyte solutions, (220) out-of-plane texture was formed in the saccharin-free films. The additive saccharin eliminated the texture and yielded very fine microstructures with high dislocation densities and twin fault probabilities for both solution types. The influence of saccharin on the defect density was higher for the film prepared from the sulfate-type bath. It was revealed that there is a correlation between the defect density and the grain size. When saccharin was added to the Watts bath, the combined effect of nickel-chloride and saccharin led to a bimodal grain size distribution. An additional sample was deposited from an electrolyte containing trisodium citrate to investigate the sodium incorporation in the Ni layers. The correlation between the microstructure and the hardness of the films was discussed in detail.

Investigation of the Microstructure Evolution in a Fe-17Mn-1.5Al-0.3C Steel via In Situ Synchrotron X-ray Diffraction during a Tensile Test.

The quantitative characterization of the microstructure evolution in high-Mn steel during deformation is of great importance to understanding its strain-hardening behavior. In the current study, in situ high-energy synchrotron X-ray diffraction was employed to characterize the microstructure evolution in a Fe-17Mn-1.5Al-0.3C steel during a tensile test. The microstructure at different engineering strain levels—in terms of ε-martensite and α’-martensite volume fractions, the stacking fault probability, and the twin fault probability—was analyzed by the Rietveld refinement method. The Fe-17Mn-1.5Al-0.3C steel exhibits a high ultimate tensile strength with a superior uniform elongation and a high strain-hardening rate. The remaining high strain-hardening rate at the strain level about 0.025 to 0.35 results from ε-martensite dominant transformation-induced-plasticity (TRIP) effect. The increase in the strain-hardening rate at the strain level around 0.35 to 0.43 is attributed to the synergetic α’-martensite dominant TRIP and twinning-induced-plasticity (TWIP) effects. An evaluation of the stacking fault energy (SFE) of the Fe-17Mn-1.5Al-0.3C steel by the synchrotron measurements shows good agreement with the thermodynamic calculation of the SFE.