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At least 1,063 records · Page 59

Microstructural characteristics of adiabatic shear localization in a metastable beta titanium alloy deformed at high strain rate and elevated temperatures

The microstructural evolution and grain refinement within adiabatic shear bands in the Ti6554 alloy deformed at high strain rates and elevated temperatures have been characterized using transmission electron microscopy. No stress drops were observed in the corresponding stress–strain curve, indicating that the initiation of adiabatic shear bands does not lead to the loss of load capacity for the Ti6554 alloy. The outer region of the shear bands mainly consists of cell structures bounded by dislocation clusters. Equiaxed subgrains in the core area of the shear band can be evolved from the subdivision of cell structures or reconstruction and transverse segmentation of dislocation clusters. It is proposed that dislocation activity dominates the grain refinement process. The rotational recrystallization mechanism may operate as the kinetic requirements for it are fulfilled. The coexistence of different substructures across the shear bands implies that the microstructural evolution inside the shear bands is not homogeneous and different grain refinement mechanisms may operate simultaneously to refine the structure. - Graphical abstract: Display Omitted - Highlights: • The microstructure within the adiabatic shear band was characterized by TEM. • No stress drops were observed in the corresponding stress–strain curve. • Dislocation activity dominated the grain refinement process. • The kinetic requirements for rotational recrystallization mechanism were fulfilled. • Different grain refinement mechanisms operated simultaneously to refine the structure.

36 MATERIALS SCIENCE↗

Study of tempering behavior of lath martensite using in situ neutron diffraction

To elucidate changes in the density and substructure of dislocations during tempering of lath martensite steel, a convolutional multiple whole-profile fitting method was applied to in situ neutron diffraction profiles. With increasing tempering temperature, the dislocation density scarcely changed in the beginning and then decreased at temperatures above 473 K, whereas the dislocation arrangement drastically changed at temperatures above 673 K. The strength of the steel is speculated to depend on the density and arrangement of dislocations. - Highlights: • A convolutional multiple whole-profile fitting method was applied. • Dislocation density and dislocation arrangement changing with tempering were discussed. • Dislocation density scarcely changed in the beginning. • And then dislocation density decreased at temperatures above 473 K. • The dislocation arrangement drastically changed at temperatures above 673 K.

36 MATERIALS SCIENCE↗

Quantitative analysis of microstructure and deformation mechanisms during isothermal compression of Ti–5Al–5Mo–5V–1Cr–1Fe alloy

The effects of the processing parameters on the grain size and volume fraction of equiaxed α for Ti–5Al–5Mo–5V–1Cr–1Fe are quantitatively investigated using isothermal compression tests. The microstructure features, such as the morphology of equiaxed and acicular α phase, the dislocation distribution, the formation of substructure are in depth discussed with the help of transmission electron microscopy (TEM) and scanning electron microscopy (SEM) experiments so as to clarify the deformation mechanisms. The results show that few DRX α grains appear in the α + β phase region. In the β phase region, selective DRX occurs and the amount of DRX increases with increasing strain rate. DRV is main softening mechanism in the tested deformation temperature range. The elongated β grains are observed at medium deformation temperatures and lower strain rates. This phenomenon demonstrates that β phase is mainly involved in the deformation. At higher deformation temperatures and lower strain rates, acicular α is not observed for this alloy. Possible reason is that acicular α dissolves into the β matrix. - Highlights: • Few DRX α grains appear in the α + β phase region. • DRX occurs in the β phase region and raises with increasing strain rate. • α phase deforms less than β matrix at medium temperatures and lower strain rates. • Acicular α is not observed at higher temperatures and lower strain rates.

36 MATERIALS SCIENCE↗

Correlative characterization of primary particles formed in as-cast Al-Mg alloy containing a high level of Sc

Primary particles formed in as-cast Al-5Mg-0.6Sc alloy and their role in microstructure and mechanical properties of the alloy were investigated using optical microscopy (OM), scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and tensile testing. It was found that primary particles due to a close orientation to matrix could serve as the potent heterogeneous nucleation sites for α-Al during solidification and thus impose a remarkable grain refinement effect. Eutectic structure consisted of layer by layer of ‘Al{sub 3}Sc + α-Al + Al{sub 3}Sc + ⋯’ and cellular-dendritic substructure were simultaneously observed at the particles inside, indicating that these particles could be identified as the eutectics rather than individual Al{sub 3}Sc phase. A calculating method, based on EBSD results, was introduced for the spatial distribution of these particles in matrix. The results showed that these eutectic particles randomly distributed in matrix. In addition, the formation of primary eutectic particles significant improved the strength of the Al-Mg alloy in as-cast condition, which is ascribed to the structural evolution from coarse dendrites to prefect fine equiaxed grains. On the other hand, these large-sized particles due to the tendency to act as the microcrack sources could cause a harmful effect in the ductility of Al-Mg-Sc alloy. - Highlights: •Primary particles exhibit an ‘Al{sub 3}Sc + α-Al + Al{sub 3}Sc + ⋯’ multilayer feature with a cellular-dendritic mode of growth. •EBSD analyses the mechanism of grain refinement and the distribution of primary particles in α-Al matrix. •A computational method was presented to calculate the habit planes of primary particles.

36 MATERIALS SCIENCE↗

Microstructural analysis on cleavage fracture in pearlitic steels

Microstructural features controlling cleavage fracture in pearlitic structures were investigated by means of scanning electron microscopy and electron backscattered diffraction. It was found that pearlite block size corresponds well to the cleavage facet size, and a single cleavage facet usually contains multiple pearlite colonies. Pearlite block size and cleavage facet size decrease with the refinement of prior austenite grain size, while pearlite colony size only changes slightly. The cleavage crack can largely deflect at block boundaries rather than at colony boundaries. Pearlite block can act as the dominant substructure on cleavage crack propagation in pearlitic steels. - Highlights: •The cleavage crack propagation path in pearlitic structures was analyzed by EBSD. •Pearlite block boundaries can effectively hinder the crack propagation. •Pearlite block size corresponds well to the cleavage facet size. •A single cleavage facet usually contains multiple pearlite colonies.

36 MATERIALS SCIENCE↗

Defect features, texture and mechanical properties of friction stir welded lap joints of 2A97 Al-Li alloy thin sheets

1.4 mm 2A97 Al-Li alloy thin sheets were welded by friction stir lap welding using the stirring tools with different pin length at different rotational speeds. The influence of pin length and rotational speed on the defect features and mechanical properties of lap joints were investigated in detail. Microstructure observation shows that the hook defect geometry and size mainly varies with the pin length instead of the rotational speed. The size of hook defects on both the advancing side (AS) and the retreating side (RS) increased with increasing the pin length, leading to the effective sheet thickness decreased accordingly. Electron backscatter diffraction analysis reveals that the weld zones, especially the nugget zone (NZ), have the much lower texture intensity than the base metal. Some new texture components are formed in the thermo-mechanical affected zone (TMAZ) and the NZ of joint. Lap shear test results show that the failure load of joints generally decreases with increasing the pin length and the rotational speed. The joints failed during the lap shear tests at three locations: the lap interface, the RS of the top sheet and the AS of the bottom sheet. The fracture locations are mainly determined by the hook defects. - Highlights: • Hook defect size mainly varies with the pin length of stirring tool. • The proportion of LAGBs and substructured grains increases from NZ to TMAZ. • Weld zones, especially the NZ, have the much lower texture intensity than the BM. • Lap shear failure load and fracture location of joints is relative to the hook defects.

36 MATERIALS SCIENCE↗

Characterizing dislocation configurations and their evolution during creep of a new 12% Cr steel

Highlights: • Applicability of different techniques to characterize particular dislocation configuration. • XRD models in combination with TEM and EBSD to measure the dislocation density. • Substructure evolution during creep of a new 12% Cr steel is discussed. - Abstract: In this research, different types of dislocations are characterized and quantified in a newly developed 12% Cr steel in as-received as well as in crept conditions. X-ray diffraction (XRD) patterns are analyzed using three different models. The dislocation densities are determined employing the Convolution Multiple Whole Profile (CMWP) fitting, the analysis of the asymptotic part of the X-ray line profile (Groma's method), and the Rietveld refinement coupling Popa's and Williamson-Smallman approaches. CMWP method is used to measure the internal dislocation density inside the subgrains consisting of mobile and dipole dislocations, and the results show good agreement with Transmission Electron Microscopy (TEM) measurements. Groma's method is used to evaluate the total dislocation density, with results comparable to those obtained from the combination of Electron Backscatter Diffraction (EBSD) and TEM. Rietveld method gives the internal dislocation density or mobile dislocation density depending on the model chosen. The experimentally determined results such as creep strain, dislocation densities and subgrain size are compared with theoretical predictions and they are found in good agreement.

36 MATERIALS SCIENCE↗

Investigations of γ′, γ″ and δ precipitates in heat-treated Inconel 718 alloy fabricated by selective laser melting

Highlights: • The γ austenite matrix shows a fine cellular substructure. • γ′ and three variants of γ″ precipitates around 10–50 nm develop within cellular γ. • Coarser acicular γ″ and plate-like δ occur at grain boundaries and intragranular γ. • The orientation relationships of γ″ with γ, and of δ with γ are observed. - Abstract: Inconel 718 alloy samples were fabricated by selective laser melting (SLM). Microstructure and precipitation in solution-heat-treated- and double-aging-SLM-made Inconel 718 were studied by scanning and transmission electron microscopy. Electron microscope observations showed that disc-shaped and cuboidal γ″, and circular γ′ precipitates with an average size of 10–50 nm developed within cellular γ austenite matrix. The simulated, experimentally observed electron diffraction patterns, and dark-field imaging further revealed that the precipitation of three variants of γ″ in the γ matrix occurred. The coarser acicular γ″, and globular as well as plate-like δ phases precipitated at grain boundaries and also within the interior of austenite matrix. The morphology, distribution and crystallography of these precipitates and their formation mechanisms were analyzed and discussed.

36 MATERIALS SCIENCE↗

The effect of a prior short-term ageing on mechanical and creep properties of P92 steel

Highlights: • The results of simulated ageing at 650°C allows to estimate degradation of P92 steam pipes due to accidental overheating. • Simulated ageing has only a slight effect on ambient tensile properties and hardness. • A sudden decrease in impact properties occurred after ageing for 2000h. The FATT of about 25°C was determined. • The creep results show a clear detrimental influence of tempering ageing on the creep strength. • No Z-phase precipitation occurred due to the ageing process. - Abstract: We have investigated the effect of prior short-term ageing on the mechanical and creep properties of tungsten and boron modified 9%Cr ferritic steel (ASTM Grade P92 steel), to provide material data base for the estimation of material degradation due to occurrence of accidental overheating in the early stage of service loading. The steel was aged at 650 °C for up to 100, 200, 500, 1000, 2000 and 5000 h prior to mechanical and creep testing. Changes in the microstructure during ageing had a slight effect on the reduction of room temperature tensile properties. A sudden decrease on impact properties occurred after ageing for 2000 h, but the occurred impact energy of about 70 J is in accordance with the specified minimum value of 68 J at room temperature for the virgin condition. The creep behaviour of P92 steel in the as-received condition and after different isothermal ageing exposures prior to creep was investigated at 600 and 650 °C in the power-law creep regime. The initial applied tensile stress ranged from 90 to 200 MPa. The results clearly show a detrimental influence of isothermal ageing on creep properties even after a few hundred hours. Based on microstructure analysis, which was done mostly in a qualitative way, a significant decrease in the creep life after ageing resulted from changes of the dislocation substructure and instability of Laves phase and M{sub 23}C{sub 6} particles.

36 MATERIALS SCIENCE↗

Ultrafine gradient microstructure induced by severe plastic deformation under sliding contact conditions in copper

Highlights: • Sliding contact produces a gradient microstructure by severe plastic deformation. • Nanohardness is increased strongly by grain size and dislocation hardening. • The texture components in the deformed layer correspond to pure shear. • Grain size distribution, boundary misorientation and KAM were analysed. • Strain induced effects compete with crystallisation to determine the microstructure. - Abstract: Sliding contact induces severe plastic deformation (SPD) at the surface of ductile materials and induces a microstructural gradient associated to a significant increase of hardness toward the surface. This gradient allows observing all stages of grain refinement in SPD, as illustrated here by the analysis of polycrystalline electrolytic copper tested in a coaxial tribometer. Materials tested in the cold-rolled state and after annealing were characterised by high-resolution electron backscattering diffraction and nano-indentation. The incremental plastic strain produces an ultrafine microstructure in the top layers, which gradually changes to the original size in unaffected material. In cold-rolled material, an intermediate recrystallised layer is observed. The separation of the Misorientation Angle Distribution (MAD) in a low-angle portion and a high angle portion allows characterising the accumulation of strain induced misorientation, while the Kernel Average Misorientation (KAM) provides information on the evolution of substructure at the finest levels. The results point toward a process where strain-induced effects compete continuously with recrystallisation, except for the surface layer in the cold-rolled material, where dynamic recrystallisation is dominant. Combining the information from KAM and subgrain size distribution, the measured hardness can be explained as a combination of grain size and dislocation hardening.

36 MATERIALS SCIENCE↗

Martensite crystallography and chemistry in dual phase and fully martensitic steels

Highlights: • Lath martensite islands and bands were indexed in variations of dual-phase steels. • Detail insight was obtained by combined EBSD, APT, TEM, nano-indentation analysis. • The islands predominantly consist of one main packet with all six variants. • The bands are composed of connected domains, each largely made of one main packet. • Tempering at ~450 °C causes carbon partition to lath boundaries and dislocation cores. - Abstract: Lath martensite is important in industry because it is the key strengthening component in many advanced high strength steels. The study of crystallography and chemistry of lath martensite is extensive in the literature, however, mostly based on fully martensitic steels. In this work, lath martensite in dual phase steels is investigated with a focus on the substructure identification of the martensite islands and microstructural bands using electron backscattered diffraction, and on the influence of the accompanied tempering process during industrial coating process on the distribution of alloying elements using atom probe tomography. Unlike findings for the fully martensitic steels, no martensite islands with all 24 Kurdjumov-Sachs variants have been observed. Almost all martensite islands contain only one main packet with all six variants and minor variants from the remaining three packets of the same prior austenite grain. Similarly, the martensite bands are typically composed of connected domains originating from prior austenite grains, each containing one main packets (mostly with all variants) and few separate variants. The effect of tempering at ~450 °C (due to the industrial zinc coating process) has also been investigated. The results show a strong carbon partitioning to lath boundaries and Cottrell atmospheres at dislocation core regions due to the thermal process of coating. In contrast, auto-tempering contributes to the carbon redistribution only in a limited manner. The substitutional elements are all homogenously distributed. The phase transformation process has two effects on the material: mechanically, the earlier-formed laths are larger and softer and therefore more ductile (as revealed by nanoindentation); chemically, due to the higher dislocation density inside the later-formed laths, which are generally smaller, carbon Cottrell atmospheres are predominantly observed.

36 MATERIALS SCIENCE↗

Effect of austenite grain size on acicular ferrite transformation in a HSLA steel

Highlights: • The fraction of acicular ferrite increases with reduced austenite grain sizes. • The reduction of austenite grain size refines and homogenises the microstructure. • There is a limit to increase the acicular ferrite fraction by reducing austenite size. • An equation relating effective grain sizes with processing parameters was proposed. - Abstract: Austenite grain size is well known to have a significant influence on various phase transformations in steels. Although the effects of many thermomechanical processing parameters on acicular ferrite (AF) transformation in HSLA steels have been investigated, little attention has been paid to the influence of austenite grain size. Therefore, in this research, different parameters of solid-solution heat treatment and rough deformation were adopted to generate austenite with different grain sizes and the effects of austenite grain size before deformation on the AF transformation and grain refinement were investigated. It was found that the reduction of prior-austenite grain size (PAGS) from 62.8 μm to 37.0 μm before austenite deformation promotes the AF transformation and simultaneously refines and homogenises the transformed microstructures. A reciprocally increased density of deformation induced dislocations with the reduction of PAGS was proposed to account for these results, which not only increase the nucleation sites of AF but also suppress the lengthening of BF laths. Further reducing PAGS from 37.0 μm to 22.3 μm, the fraction of AF is not increased and the transformed microstructure is not refined. Possible differences in the type, distribution, and density of austenite deformation substructures between austenite with PAGSs of 37.0 μm and 22.3 μm were argued to be responsible for the cease of grain refinement. The relationship between effective grain sizes and the S{sub v} parameter was investigated and an equation relating effective grain sizes with processing parameters was also proposed.

36 MATERIALS SCIENCE↗

Enhanced mechanical properties of carbon-doped FeNiMnAlCr high entropy alloy via hot-rolling

This work demonstrates an improvement in the mechanical performance of the high entropy alloy Fe 40.4 Ni 11.3 Mn 34.8 Al 7.5 Cr 6 containing 1.1 at. % carbon (CHEA) by hot-rolling followed by annealing at 1323 K. The microstructure was examined using scanning electron microscopy, electron backscatter diffraction, X-ray diffraction, and transmission electron microscopy. Room-temperature tensile tests were used to assess the alloy's mechanical properties. The presence of dense dislocation walls indicate that the alloy has not fully recrystallized and, moreover, the deformation substructure and the large fraction of Σ3 twin boundaries contribute to the high room temperature yield strength (~523 MPa). Despite the presence of substantial dislocation density, the annealed, hot-rolled CHEA displays an improvement in elongation to fracture (~33%) compared to the negligible ductility (< 2%) observed for the alloy after it has been simply annealed. Finally, the present work shows that hot rolling can produce good strength and ductility in the alloy while establishing the processing conditions necessary for the large-scale manufacture and utilization of its remarkable properties.

36 MATERIALS SCIENCE↗

Template-directed preparation of two-layer porous NiO film via hydrothermal synthesis for lithium ion batteries

Graphical abstract: A two-layer porous NiO film is prepared via hydrothermal synthesis method based on monolayer polystyrene sphere template and shows noticeable Li battery performance with good cycle life and high capacity. Highlights: ► Two-layer porous NiO film is prepared via monolayer polystyrene spheres template. ► NiO film with high capacity as anode material for lithium ion batteries. ► Two-layer porous structure is favorable for fast lithium ion and electron transfer. -- Abstract: A two-layer porous NiO film is prepared by hydrothermal synthesis method through self-assembled monolayer polystyrene spheres template. The substructure of the NiO film is composed of ordered close-packed hollow-sphere array and the superstructure is made up of randomly NiO nanoflakes. The electrochemical properties are measured by galvanostatic charge/discharge tests and cyclic voltammetric analysis (CV). As anode material for lithium ion batteries, the two-layer porous NiO film exhibits high initial coulombic efficiency of 75%, high reversible capacity and rather good cycling performance. The discharge capacity of the two-layer porous NiO film is 501 mAh g{sup −1} at 0.5 C after 50 cycles. The two-layer porous architecture is responsible for the enhancement of electrochemical properties.

36 MATERIALS SCIENCE↗

Preparation of defect-free asymmetric gas separation membranes with dihydrolevoglucosenone (Cyrene TM ) as a greener polar aprotic solvent

Nonsolvent-induced phase separation (NIPS) is widely used to prepare asymmetric gas separation membranes. Most industrial NIPS casting solution formulations are limited to a small group of glassy polymers and, importantly, require toxic polar aprotic solvents such as N,N-dimethylacetamide (DMAc), N,N-dimethylformamide (DMF), or N-methyl-2-pyrrolidone (NMP). Growing restrictions on the use of such solvents are spurring the search for more benign casting solution formulations that do not compromise membrane performance. Herein this study reports high-flux, defect-free asymmetric polysulfone (PSf) gas separation membranes prepared using dihydrolevoglucosenone (Cyrene TM ), a polar aprotic solvent that is believed to be safer than DMAc, DMF, and NMP, as the majority casting solution component. Optimized formulations and casting conditions produce membranes with hydrogen permeances exceeding 100 gas permeance units (GPU) and selectivities at or above those of dense PSf films. Dry/wet NIPS membrane performance improved with shorter dry step times and increased Cyrene TM loadings relative to the volatile solvent, tetrahydrofuran (THF), in the casting solution. The high water-Cyrene TM Flory-Huggins interaction parameter, $\mathcal{X}12$ , and high casting solution viscosities help suppress the formation of skin layer defects and sublayer macrovoids. In some cases, membrane selectivities were influenced by substructure resistance, providing insight into the relationship between sublayer morphology and membrane performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Machine learning prediction on the fractional free volume of polymer membranes

Fractional free volume (FFV) characterizes the microstructural level features of polymers and affects their properties including thermal, mechanical, and separation performance. Experimental measurements and theoretical analyses have been used to quantify the FFV of polymers, but challenges remain because of their limitations. Experimental measurements are laborious and based on semi empirical equations, while Bondi’s group contribution theory involves ambiguities like the determination of van der Waals volume and the choice of factor values in the theoretical equation. To efficiently evaluate the FFV of polymers, this study utilizes high-throughput molecular dynamics (MD) simulations to build a large dataset regarding polymer’s FFV. Based on this large dataset, we further build machine learning (ML) models to establish the composition-structure relation. Inspired by group contribution theory which correlates polymer’s functional groups to FFV, our ML models correlate polymer’s substructures or physico-chemical indexes to FFV. Here, our study first benchmarks the MD simulation protocol to obtain reliable FFV of polymers and then carries out high-throughput MD simulations for more than 6,500 homopolymers and 1,400 polyamides. Such a large and diverse dataset makes the well-trained ML models more generalizable, compared with the group contribution theory. The efficiency of a feed forward neural network model is further demonstrated by applying it to a hypothetical polyimide dataset of more than 8 million chemical structures. The predicted FFVs of hypothetical polyimides are further validated by MD simulations. The obtained FFVs of the 8 million polymers, plus their previously reported gas separation performances, demonstrate the promising capability of ML virtual screening for the discovery of polymer membranes with exceptional permeability/selectivity.

36 MATERIALS SCIENCE↗

Machine learning-based discovery of molecular descriptors that control polymer gas permeation

While machine learning has found increasing use in predicting the properties of polymeric materials with only a knowledge of chain architecture, determining the molecular factors underpinning properties (“interpretable AI”) has remained less well explored. We show that encoding chain chemistry in commonly employed formats, e.g., binary-valued fingerprints, leads to uniqueness issues during the hashing process to save storage space. This is because the hashing algorithm can map several chemical moieties into the same bit. These issues carry over into the ML algorithms, especially for “inverse” design and interpretable AI, and cannot be avoided by changing the length of the fingerprint. Using MACCS key featurizations of monomer repeats resolves some of these issues, and we show that a few substructures consistently appear in top features for maximizing permeability across several gases and ML models. These are carbon–carbon double bonds (as in polyacetylenes) especially when they are associated with methyl groups (found in branching architectures). Here these results, derived from the limited data set of ~ 500 polymers with experimental gas permeation data, are in agreement with physical insight and thus provide a robust foundation which could further enable study of these material classes through detailed experiments and simulations.

36 MATERIALS SCIENCE↗

Fatigue and Creep-Fatigue Deformation of an Ultra-Fine Precipitate Strengthened Advanced Austenitic Alloy

An advanced austenitic alloy, HT-UPS (high-temperature ultrafine-precipitation-strengthened), has been identified as an ideal candidate material for the structural components of fast reactors and energy-conversion systems. HT-UPS alloys demonstrate improved creep resistance relative to 316 stainless steel (SS) through additions of Ti and Nb, which precipitate to form a widespread dispersion of stable nanoscale metallic carbide (MC) particles in the austenitic matrix. The low-cycle fatigue and creep-fatigue behavior of an HT-UPS alloy have been investigated at 650 °C and a 1.0% total strain, with an R-ratio of -1 and hold times at peak tensile strain as long as 150 min. The cyclic deformation response of HT-UPS is directly compared to that of standard 316 SS. The measured values for total cycles to failure are similar, despite differences in peak stress profiles and in qualitative observations of the deformed microstructures. Crack propagation is primarily transgranular in fatigue and creep-fatigue of both alloys at the investigated conditions. Internal grain boundary damage in the form of fine cracks resulting from the tensile hold is present for hold times of 60 min and longer, and substantially more internal cracks are quantifiable in 316 SS than in HT-UPS. The dislocation substructures observed in the deformed material differ significantly; an equiaxed cellular structure is observed in 316 SS, whereas in HT-UPS the microstructure takes the form of widespread and relatively homogenous tangles of dislocations pinned by the nanoscale MC precipitates. The significant effect of the fine distribution of precipitates on observed fatigue and creep-fatigue response is described in three distinct behavioral regions as it evolves with continued cycling.

36 MATERIALS SCIENCE↗