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At least 127 records · Page 7

Microstructural Evolution During a Solid State Tube Pinch Weld of Type 304l Stainless Steel

Microstructure development is examined for a specialized spot weld that is used as a solid-state closure process for austenitic stainless steel tubing, referred to as pinch welding. In order to elucidate the microstructural evolution of the weld, a series of test welds were made at nominal conditions using tubing and production like components. These pinch welds normally terminate after twelve cycles of a 60 Hz AC weld process. In this study, production tubes were welded from one to twelve cycles and the microstructure and weld variables after each individual weld cycle number were characterized using radiography and optical metallography. Two electrochemical etchants were used to highlight different microstructural features. The study revealed that: (1) this type pinch weld is largely complete after about six cycles of 60 Hz AC current, half the weld time utilized; (2) the resistance, deformation, and closure length approach “steady-state” conditions after six cycles; and (3) both oxalic and nitric acid electrolytic etchants are useful for highlighting specific microstructural attributes of type 304 L stainless steel. Finally, two distinct microstructural regions can be identified for these welds: the edge of the weld, which is driven by concentrated deformation, recrystallization, and grain growth, and the center region, which is more typical of forge welding and micro-asperity breakdown followed by diffusion and grain-growth.

36 MATERIALS SCIENCE↗

Microstructure evolution and magnetic properties of FeB/Pt multilayers and FeBPt composite films

Comparisons of microstructural evolution and magnetic properties were made of a FeB12/Pt10/[FeB1.2/Pt1]{sub 15}/Ta5 nm multilayered structure with a FeB12/Pt10/FeBPt33/Ta5 nm co-deposited structure. The Ta capping layer was used to protect the films from oxidation. Both these samples were sputtered in the same planetary deposition system onto thermally oxidized silicon substrates. They both represent layer-by-layer deposition, with the second type of deposition having atomically fine layers, more than an order of magnitude finer than the first type. The samples were annealed at a range of times, temperatures, and vacuum conditions. X-ray diffraction (XRD), transmission electron microscopy, and alternating gradient magnetometry were employed to characterize the structural and magnetic properties, respectively. Significant differences were observed between the two types of structures. A maximum coercivity of 8.9 kOe was seen for the atomically fine multilayer, about 10% more than that for the coarse multilayer. XRD analysis confirmed that both the coarse and fine multilayers were in the L1{sub 0} phase after annealing. Our results indicate that the co-deposited film, which is really composed of atomically fine multilayers, is superior to the coarse multilayered FeB/Pt for the formation of L1{sub 0}-phase FePt.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Microstructure Evolution and Effect on Resistivity for Cu Nanointerconnects and Beyond

In this paper, we investigate the microstructure evolution in Cu, Co and Ru nanointerconnects and the scaling effect on resistivity. The scaling effect on microstructure of Cu interconnects was analyzed to the 24 nm linewidth for the 14 nm node using a high-resolution TEM precession microdiffraction technique. The TEM study was supplemented by a Monte Carlo simulation to investigate grain growth in nanointerconnects based on local energy minimization. The scaling effect on electrical resistivity was analyzed for Cu, Ru and Co nanointerconnects, taking into account the contributions from surface and grain boundary scatterings. The results for Cu and Co are consistent with recent experiments.

36 MATERIALS SCIENCE↗

Application of morphological synthesis for understanding electrode microstructure evolution as a function of applied charge/discharge cycles

Morphological analysis and synthesis operations were employed for analysis of electrode microstructure transformations and evolution accompanying the application of charge/discharge cycles to electrochemical storage systems (batteries). Using state-of-the-art morphological algorithms, it was possible to predict microstructure evolution in porous Si electrodes for Li-ion batteries with sufficient accuracy. Algorithms for image analyses (segmentation, feature extraction, and 3D-reconstructions using 2D-images) were also developed. Altogether, these techniques could be considered supplementary to phase-field mesoscopic approach to microstructure evolution that is based upon clear and definitive changes in the appearance of microstructure. However, unlike in phase-field, the governing equations for morphological approach are geometry-, not physics-based. Similar non-physics based approach to understanding different phenomena was attempted with the introduction of cellular automata. It is anticipated that morphological synthesis and analysis will represent a useful supplementary tool to phase-field and will render assistance to unraveling the underlying microstructure-property relationships. The paper contains data on electrochemical characterization of different electrode materials that was conducted in parallel to morphological study.

25 ENERGY STORAGE↗

High temperature oxidation and microstructural evolution of cold spray chromium coatings on Zircaloy-4 in steam environments

Oxidation kinetics and microstructural evolution of cold sprayed Cr coatings on Zircaloy-4 at 1130–1310 °C in flowing steam at atmospheric pressure have been studied. The study is aimed at understanding of the response of Cr coated Zr-alloy under a steam environment and high temperatures pertinent to design basis accidents (DBAs) and beyond design basis accidents (BDBAs) in light water reactors (LWRs). Surface morphology, microstructure, and phases of post-oxidation test samples were characterized using Scanning Electron Microscopy (SEM), x-ray diffraction (XRD), and Scanning Transmission Electron Microscopy (STEM). Growth kinetics of the Cr-oxide scale and interdiffusion layers between the Cr coating and the Zr-alloy substrate were quantified from cross-sectional SEM images. Cross-sectional analysis showed that the Cr coatings offered a 50 times reduction in oxidation rate over bare Zircaloy-4 in a 1310 °C steam environment. Oxidation kinetics at 1130 °C followed parabolic law (i.e., n ~ 0.5 in power law kinetics) but at 1230 °C and 1310 °C the value of n was suppressed to below 0.5 possibly due to the volatilization of Cr species at the two highest temperatures. Interdiffusion at coating/substrate interface resulted in formation of a brittle Cr 2 Zr or Zr(Fe, Cr) 2 intermetallic compound layer on the order of micrometer in thickness and scattered Cr-rich precipitates were observed well below the interface within the Zr-alloy substrate after cooling. These experimental results could provide data to LWR system simulation codes for better estimation of coping time in the event of accidents.

36 MATERIALS SCIENCE↗

Coupled cluster and dislocation dynamics modeling of microstructure evolution in irradiated materials

We develop here a coupled cluster and dislocation dynamics framework to study the microstructure evolution of irradiated materials. The framework not only accounts for the three dimensional diffusion of radiation-generated clusters, but also their interaction with dislocation networks and the resultant climb motion of discrete dislocations within finite crystals. The framework is solved with a superposition solution scheme, and is applied to investigate the evolution of the irradiation-induced dislocation loops in zirconium (Zr), considering the effects of various bias factors including the diffusion anisotropy difference (DAD) of interstitials and interstitial clusters, the dislocation bias of defects to discrete dislocation segments, and the production bias of defects from the radiation cascade. We find that the DAD is the most critical factor influencing the kinetics of the loop evolution in Zr, while the recombination/interaction of mobile defects can induce a strong spatial dependence of the loop evolution together with the DAD. Here, the method is also adopted to study the evolution of interstitial $\langle$a$\rangle$ and vacancy $\langle$c$\rangle$ dislocation loop ensembles consistent with the microstructure observed during irradiation-induced growth of Zr. Our findings not only reveal the spatial dependence of the size and ellipticity of the dislocation loops, but also suggest a limit on the anisotropy factor of interstitials to reproduce the co-growth of $\langle$a$\rangle$ and $\langle$c$\rangle$ loops in zirconium, in good agreement with experimental observations and other simulation results.

Bias factors↗

Phase transformation and microstructure evolution of the deformed Ti-30Zr-5Nb shape memory alloy

The phase transformation and microstructures of the deformed Ti-30Zr-5Nb shape memory alloy were investigated. The X-ray diffraction measurements indicated that the Ti-30Zr-5Nb alloy was composed of a single orthorhombic α″-martensite phase. The alloy exhibited one yielding behavior in the tensile test, with a critical stress of ~ 600 MPa and a tensile strain of approximately 15%. A shape memory recovery accompanied by a permanent strain was exhibited in the deformed alloys when heated at 873 K. The permanent strain increased with increasing pre-strain. The microstructure evolution of the deformed alloy was investigated by transmission electron microscopy. The results showed that the martensite reorientation occurred and the dislocations were generated during deformation. The alloy displayed a reversible martensite transformation start temperature as high as 763 K. However, no strain-induced martensite stabilization was found in the deformed alloy with different pre-strain levels, potentially because the large chemical energy of the Ti-30Zr-5Nb alloy depressed the effects of the elastic energy and the dissipative energy. - Highlights: • Ti-30Zr-5Nb alloy is composed of single orthorhombic α″-martensite phase with M{sub s} of 721 K. • No martensite stabilization has been found in Ti-30Zr-5Nb alloy with different pre-strain. • Ti-30Zr-5Nb shows the maximum shape memory effect of 2.75% with a pre-strain of 8%.

36 MATERIALS SCIENCE↗

Microstructure evolution and mechanical properties of the compressively deformed AgInCd alloy during annealing treatment

Highlights: • The microstructure of AgInCd alloy during annealing treatment is investigated. • Nanoscale deformation twins are formed in the deformed AgInCd alloy. • Deformation twins are transformed into stacking faults by detwinning mechanism. • Annealing twins show higher thermal stability than deformation twins. - Abstract: The microstructure evolution and mechanical properties of the compressively deformed AgInCd alloy during annealing treatment have been investigated in the present study. In the deformed AgInCd alloy, many deformation markings are formed and these deformation markings are mainly composed of nanoscale deformation twins. The AgInCd alloy exhibits a significant work hardening capability because of the formation of deformation twins. The recrystallization temperature of the deformed AgInCd alloy is between 300 °C and 350 °C. In the AgInCd alloy annealed at 300 °C, the deformation twins are eliminated and a large number of dark strips consisting of stacking faults are presented in the un-recrystallized regions, indicating that the deformation twins are transformed into stacking faults by the detwinning mechanism. The annealing twins show higher thermal stability than the deformation twins. The strength and microhardness of the deformed AgInCd alloy gradually decrease with the increase of annealing temperature.

36 MATERIALS SCIENCE↗

Microstructural evolution and phase stability in Nb-containing interstitial Fe-Mn-Co-Cr-C high-entropy alloys: An in-situ synchrotron X-ray diffraction study during laser melting

The influence of Nb on phase stability and microstructural evolution in an interstitial Fe-Mn-Co-Cr-C high-entropy alloy was investigated using in-situ synchrotron X-ray diffraction (SXRD) during laser melting. Scheil-Gulliver simulations predict the formation of σ and γ-f.c.c. phases in all three alloys, along with NbC in Nb-containing compositions. SXRD confirmed the presence of most predicted phases, but the σ phase was absent. Nb promotes crystallite refinement and increases dislocation density, though excessive additions reduce refinement efficiency due to solubility limits and secondary phase formation. Furthermore, Nb addition also enhances ε-h.c.p. phase formation by reducing stacking fault energy through NbC-induced carbon depletion. Analysis of intensity peak evolution reveals that Nb alters preferred grain orientations, reducing {111} γ intensity while enhancing {220} γ , leading to a more isotropic grain distribution. Overall, Nb plays a key role in phase selection, microstructure refinement, and preferred orientation evolution, allowing the tailored microstructure of high-entropy alloys via rapid solidification.

Interstitial high entropy alloys↗

Creep property and microstructure evolution of a nickel-base single crystal superalloy in [011] orientation

The creep property and microstructure evolution of a single crystal superalloy with [011] orientation were investigated at the temperatures of 700 °C, 900 °C and 1040 °C. It is shown that there exist stages of primary, steady-state, and tertiary creep under the lower temperature 700 °C. As the temperature increases to high temperatures of 900 °C and 1040 °C, steady-state creep stage is reduced or disappears and the shape of creep curves is dominated by an extensive tertiary stage. The minimum creep strain rate exhibits power law dependence on the applied stress; the stress exponents at 700 °C, 900 °C and 1040 °C are 28, 13 and 6.5, respectively. Microstructure observation shows that the morphologies of γ′ phase almost keep original shape at the lower temperature 700 °C and high applied stress. With the increasing creep temperature, γ′ precipitates tend to link together and form lamellar structure at an angle of 45° inclined to the applied stress. Transmission electron microscopy (TEM) investigations reveal that multiple < 110 > (111) slip systems gliding in the matrix channels and shearing γ′ precipitates by stacking faults or bending dislocation pairs are the main deformation mechanism at the lower temperature of 700 °C. At the high temperatures of 900 °C and 1040 °C, dislocation networks are formed at γ/γ′ interfaces and the γ′ rafts are sheared by dislocation pairs. - Highlights: • Creep properties of < 011 >-oriented single crystal superalloys were investigated. • γ′ phases become rafting at an angle of 45° inclined to the applied stress. • Creep deformation mechanisms depend on temperature and stress.

36 MATERIALS SCIENCE↗

Continuous microstructure evolution of ball rolled TWIP Ti15Mo alloy and its effect on phase precipitation behavior

Highlights: • Gradient microstructure was induced by ball rolling method in a Ti15Mo alloy. • Twin density increased and then decreased as increasing distance from surface. • Ultrafine (α + β) duplex structure was formed in the heavily deformed region. • α-phase in plate was precipitated in twined region in slightly deformed region. • Strengthening by formation of sub/nano-grains was notable than that by twins. - Abstract: A β-type Ti15Mo alloy with {332}<113> twinning-induced plasticity (TWIP) effect was utilized to investigate the continuous microstructure evolution of β-matrix by ball rolling method. Precipitation behavior of α-phase and strengthening mechanism were examined in regions with different strain. Amounts of intersected twins were present in the slightly deformed region of β-matrix, and their area fraction decreased with an increase of distance from rolled surface. The β-matrix close to surface was heavily deformed to result in the formation of abundant subgrains and nanograins, which was caused by cooperative occurrence of twinning refinement, intragranular dislocation activities and subgrain rotation. Mechanical twins provided the preferential nucleation sites for plate-like α-phase with strong variant selection. Equiaxed α-phase preferentially nucleated at the boundaries of subgrains and nanograins with weak variant selection to form the ultrafine (α + β) duplex structure. Due to the formation of subgrains and nanograins as well as the strain hardening, strengthening became more significant than that by twinning refinement solely. Similarly, the ultrafine (α + β) duplex structure exhibited a better strengthening effect than that by precipitation of plate-like α-phase. The diversities of deformation microstructure combined with different precipitation behaviors of α-phase are desirable for controlling the mechanical properties of β-type TWIP titanium alloys.

36 MATERIALS SCIENCE↗

Mechanical Properties and Microstructural Evolution of Yb-Modified Al-20%Si Alloy

In the study, the mechanical properties and microstructural evolution of hypereutectic Al-20%Si-xYb alloys (x = 0, 0.1, 0.3, 0.5 and 0.7 wt.%) were studied. The as-prepared samples were characterized by scanning electron microscopy, optical microscope, x-ray diffraction (XRD) and electron probe microanalysis. The characterization results showed with the addition amount of Yb increasing to 0.5%, the eutectic Si structure was gradually modified from coarse needle-like/platelet-like structure into fine coral-like fibrous structure and the primary Si phases were gradually converted from coarse platelet-like/star-like/polygonal shape into fine blocky shape. In particular, according to the results of WDS and XRD analyses, the Yb-rich intermetallic phase in the Al-20%Si alloy is Al{sub 3}Yb. Tensile test was carried out to study the mechanical properties of Al-20%Si-x%Yb alloys, and results showed that the elongation and ultimate tensile strength increased by 73.6% and 64.5%, respectively.

36 MATERIALS SCIENCE↗

Microstructural Evolution of Al-1Fe (Weight Percent) Alloy During Accumulative Continuous Extrusion Forming

As a new microstructure refining method, accumulative continuous extrusion forming (ACEF) cannot only refine metal matrix but also refine the phases that exist in it. In order to detect the refinements of grain and second phase during the process, Al-1Fe (wt pct) alloy was processed by ACEF, and the microstructural evolution was analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results revealed that the average grain size of Al-1Fe (wt pct) alloy decreased from 13 to 1.2 μm, and blocky Al{sub 3}Fe phase with an average length of 300 nm was granulated to Al{sub 3}Fe particle with an average diameter of 200 nm, after one pass of ACEF. Refinement of grain was attributed to continuous dynamic recrystallization (CDRX), and the granulation of Al{sub 3}Fe phase included the spheroidization resulting from deformation heat and the fragmentation caused by the coupling effects of strain and thermal effect. The spheroidization worked in almost the entire deformation process, while the fragmentation required strain accumulation. However, fragmentation contributed more than spheroidization. Al{sub 3}Fe particle stimulated the formation of substructure and retarded the migration of recrystallized grain boundary, but the effect of Al{sub 3}Fe phase on refinement of grain could only be determined by the contrastive investigation of Al-1Fe (wt pct) alloy and pure Al.

36 MATERIALS SCIENCE↗

Microstructure Evolution of U–Zr System in A Thermal Cycling Neutron Diffraction Experiment: Extruded U–10Zr (wt. %)

Microstructure evolution of 1073 K extruded U–10Zr (wt. %) fuel during thermal cycling (303–1073 K with a ~9 hour hold at 873 K during cooling) was investigated using in situ neutron diffraction. Analysis was performed using Rietveld texture and crystal structure refinements from time–of–flight neutron diffraction data, with a focus on the evolution of textures and lattice parameters as a function of temperature. The α–U phase exhibits lattice contraction with increasing temperature along the b lattice direction and lattice expansion in the other directions while the other phases exhibit lattice expansion with temperature in all directions. Contrary to the established phase diagram, the β–U phase is absent at the temperatures of the thermal cycling. (001) α and (110) γ plane normals are observed with a strong preferred orientation along the extrusion direction. Finally, the variant selection of (001) α ||(110) γ is observed for the first time.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of Nickel Content on Microstructural Evolution in Austempered Solution-Strengthened Ferritic Ductile Cast Iron

The effects of Ni content and austempering temperature on microstructural evolution during austempering in solution-strengthened ferritic ductile cast iron with Ni contents between 0 and 1.1 mass% were investigated. The microstructure observation for the samples austempered at temperatures between 375 and 325 °C using an infrared gold image furnace was carried out with optical microscopy, x-ray diffraction measurements, and electron back-scattered diffraction pattern (EBSP) analysis. In addition, the Vickers hardness of both the austempered and as-quenched samples was measured under a load of 0.9807 N. According to the microstructure observations, the matrix of the samples austempered at temperatures between 375 and 325 °C exhibited finer acicular ferrite microstructure with increasing Ni content. Optical microscopy and EBSP analysis revealed that the amount of high-carbon austenite phase for the austempered samples increased with increasing Ni content and austempering temperature. Although samples with higher Ni content were found to contain more high-carbon austenite phase in the matrix, the Vickers hardness of the samples tended to increase with increasing Ni content at the same austempering temperature. The reason for this may be the higher carbon content in the matrix of the samples with higher Ni contents.

36 MATERIALS SCIENCE↗

Effect of Microstructural Evolution on Sagging Behavior of Cold-Rolled Aluminum Foil During the Brazing Thermal Cycle

Effect of microstructural evolution on sagging behavior of aluminum foil was investigated during the brazing thermal cycle. During the brazing thermal cycle, the sagging behavior consists of three stages: slight sagging stage, accelerative sagging stage and slow sagging stage. The sagging of cold-rolled aluminum foil mainly occurs in the accelerative sagging stage, which is governed by recovery under external stress in the sagging test. The coarse recrystallized grain is responsible for the slow sagging stage by reducing grain boundary sliding. Increasing cold-rolled reduction and addition of final annealing heat treatment can improve sagging resistance by shortening recovery process during the brazing thermal cycle. Dissolution of dispersoids has few effects on sagging deformation.

36 MATERIALS SCIENCE↗

Microstructure Evolution and Failure Analysis of an Aluminum–Copper Cathode Conductive Head Produced by Explosive Welding

In this paper, microstructure evolution and failure analysis of the aluminum-copper interface of cathode conductive heads during their use were studied. The interface morphologies, compositions, conductivity and mechanical properties were investigated and analyzed. Obvious corrosion was found on the surface of the contact interface, which was more prevalent on an Al matrix. The crack increased sharply in the local metallurgical bonding areas on the interface, with the compound volume having no significant change. The phase transformation occurred on the interface during use, which was investigated using the elemental composition and x-ray diffraction pattern. The microhardness near the interface increased accordingly. An obvious electrical conductivity decrease appeared on the Al/Cu interface of the cathode conductive head after use over a specific time interval. Therefore, the deterioration of the microstructures and corrosion are the primary factors that affect the electrical conductivity and effective bonding, which will lead to eventual failure.

36 MATERIALS SCIENCE↗

Effect of borides on hot deformation behavior and microstructure evolution of powder metallurgy high borated stainless steel

To investigate borides effect on the hot deformation behavior and microstructure evolution of powder metallurgy high borated stainless steel, hot compression tests at the temperatures of 950– 1150 °C and the strain rates of 0.01– 10 s{sup −1} were performed. Flow stress curves indicated that borides increased the material's stress level at low temperature but the strength was sacrificed at temperatures above 1100 °C. A hyperbolic-sine equation was used to characterize the dependence of the flow stress on the deformation temperature and strain rate. The hot deformation activation energy and stress exponent were determined to be 355 kJ/mol and 3.2, respectively. The main factors leading to activation energy and stress exponent of studied steel lower than those of commercial 304 stainless steel were discussed. Processing maps at the strains of 0.1, 0.3, 0.5, and 0.7 showed that flow instability mainly concentrated at 950– 1150 °C and strain rate higher than 0.6 s{sup −1}. Results of microstructure illustrated that dynamic recrystallization was fully completed at both high temperature-low strain rate and low temperature-high strain rate. In the instability region cracks were generated in addition to cavities. Interestingly, borides maintained a preferential orientation resulting from particle rotation during compression. - Highlights: •The decrement of activation energy was affected by boride and boron solution. •The decrease of stress exponent was influenced by composition and Cottrell atmosphere. •Boride represented a preferential orientation caused by particle rotation.

36 MATERIALS SCIENCE↗