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At least 217 records · Page 12

Microstructure Evolution and Mechanical Response of Nanolaminate Composites Irradiated with Helium at Elevated Temperatures

In this paper, we summarize recent work on helium (He) interaction with various heterophase boundaries under high temperature irradiation. We categorize the ion-affected material beneath the He-implanted surface into three regions of depth, based on the He/vacancy ratio. The differing defect structures in these three regions lead to the distinct temperature sensitivity of He-induced microstructure evolution. The effect of He bubbles or voids on material mechanical performance is explored. Finally, overall design guidelines for developing materials where He-induced damage can be mitigated in materials are discussed.

36 MATERIALS SCIENCE↗

Hot Deformation Behavior and Microstructural Evolution of Antibacterial Austenitic Stainless Steel Containing 3.60% Cu

Hot deformation behavior of as-cast antibacterial austenitic stainless steel containing 3.60% copper was investigated in a temperature range of 900-1150 °C and strain rate range of 0.01-20 s{sup −1}. At strain rates higher than 1 s {sup −1}, the flow stress curves were corrected considering adiabatic heating. Kinetic analysis indicated that the hot deformation activation energy of steel was 376.02 kJ mol{sup −1}. The microstructural evolution under different temperatures was observed by optical microscopy. The nucleation sites for recrystallization and different orientations and twin ratios under different strain rates were analyzed by electron backscatter diffraction. The results showed that hot deformation was dominated by continuous dynamic recrystallization in the high-temperature and high-strain-rate region (1050-1150 °C, 1-20 s{sup −1}). On increasing the temperature and strain rate, the degree of recrystallization and twinning increased simultaneously. These phenomena promoted one another. Thus, the volume fraction of the recrystallized and twinned grains increased with the addition of Cu.

36 MATERIALS SCIENCE↗

Mechanical response and microstructure evolution from multiaxial stress relaxation in textured zircaloy nuclear cladding

Modern energy markets provide motivation for nuclear reactors to increase operational flexibility and load following capacity of existing reactor designs. The operational power changes result in fuel pellet expansion and contraction resulting in pellet-cladding mechanical interaction (PCMI) and high cladding stresses that are strongly related to stressed corrosion cracking (SCC) which can lead to fuel rod failure. This work aims to quantify the stress fields in cladding with a focus on multiaxial stress relaxation response from an imposed strain and the resulting microstructure changes in textured zircaloy claddings. Stress relaxation tests resulting in multiaxial stress fields are performed to measure the material response of Zircaloy-4 nuclear cladding. Multiple experiments using samples from the same piece of cladding are performed so samples with the same processing history may be removed at strategic points throughout mechanical testing for microstructure characterization. The microstructure evolution is analyzed with mechanical response to evaluate the static recovery impact on crystallographic texture and grain morphology. Experiments are performed at Idaho National Laboratory using an experimental device capable of applying internal pressure and independent axial load to commercial nuclear cladding at elevated temperatures with stress- or strain-controlled experimental capability. X-ray diffraction and electron backscatter diffraction are used for microstructure analysis. Rheological models are used to visualize the multiaxial stress-strain relationships and isolate elastic, plastic, and viscoplastic material properties for analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructure evolution and mechanical performance of nickel based superalloy C1023 at elevated temperatures

Highlights: • Growth and strengthening mechanisms of carbide in superalloy C1023 were investigated. • Carbide dendrite primary arm grows selectively based on the vertex of blocky carbonitride. • Monolayer or multilayer carbide dendrite arm has certain crystal relationship with γ′ and γ. • Plastic deformation of γ hinders interior crack propagating from MC to matrix at 650 °C. • Oxidation of GBs significantly weakens the tensile strength of the superalloy at 850 °C. - Abstract: Microstructure evolution of polycrystalline nickel based superalloy C1023 casting was investigated by comparing as cast superalloy and heat treated superalloy in the paper. Influences of strengtheners and carbides on the tensile behaviors of heat treated superalloy at different temperatures (20 °C, 650 °C, and 850 °C) were studied. Resulting data from deep corrosion suggested that growth mode of scripted carbide included nucleation on the vertex of blocky carbonitride, expansion of dendrite arm in C-rich area, and enlargement of dendrite cap. Decomposition of MC carbide generated numerous octahedral M{sub 23}C{sub 6} carbide as well as nanoscale Cr-Mo-rich nuclei. Diffusion of Mo from γ to precipitates such as γ', MC, and M{sub 23}C{sub 6}, occurred during the heat treatment while irregular γ' (4 nm–500 nm) transformed into cuboidal particles. At 650 °C, no significant deterioration of tensile strength was found while plastic deformation ability of γ base was improved. Oxidation of grain boundaries (GBs) dominated the crack behavior of the superalloy at 850 °C.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Analysis of contact conditions and microstructure evolution in shear assisted processing and extrusion using smoothed particle hydrodynamics method

Shear assisted processing and extrusion (ShAPE) is a solid-phase processing technique that adds an additional shear force as compared with a conventional extrusion approach. Recently, ShAPE has demonstrated the capability of extruding high-performance aluminum alloy 7075 (AA7075) tubes at speeds up to 12.2 m/min without surface tearing. However, the relationship among the ShAPE processing parameters, thermomechanical conditions, contact conditions, heat generation, and microstructure evolution remains primarily empirical because an insightful understanding of the associated physics is still lacking. To help elucidate these relationships, this work proposes a thermomechanical meshfree model for the first time for ShAPE processing of AA7075 using the smoothed particle hydrodynamics (SPH) method. The meshfree model is first validated thoroughly by experimental data in terms of material flow, die face temperature, and extrusion force with various processing parameters. The validated model is then used to analyze the steady-state contact conditions and heat generation rates during ShAPE processing. Distributions of the average grain size of AA7075 being extruded are calculated using the SPH model output. The meshfree model results reveal that extrusions conducted at lower temperatures and higher strain rates yield more refined grains and possibly higher material strength, which is also consistent with the experimental observations.

36 MATERIALS SCIENCE↗

Microstructural evolution of ω assisted α precipitates in β-CEZ alloy during ageing process

Highlights: • Ultrafine Athermal ω precipitates were formed in β-CEZ alloy by quenching from above the β transus temperature. • In the ageing process, these ω precipitates coarsen, accompanied by the form of needle-like α phase. • ω precipitates were formed by {111}β planes shift 0.5d222 along the direction. • The superfine α particles are formed in close proximity of the ω/β interface. - Abstract: The microstructural evolution in β-CEZ (Ti-5Al-2Sn-4Zr-4Mo-2Cr-1Fe wt%) alloy, after quenching and ageing, has been investigated by combining results from orientation imaging microscopy, transmission electron microscopy, high-resolution TEM (HRTEM). Ultrafine Athermal ω precipitates (about 1 nm) are formed in this alloy by quenching from above the β transus temperature. In the ageing process, these ω precipitates coarsen, accompanied by the form of needle-like α phase. The scale of ω assisted α increased from 5 to 10 nm in width and about 50 nm in length to 10 nm in width and 100–300 nm in length while extending ageing time from 2 h to 5 h at 350 °C. However, when going on extending the ageing time from 5 h to 20 h at 350 °C, the scale of α didn't grow dramatically but the density of α increased clearly. When increasing the ageing temperature from 350 °C to 450 °C, the scale of ω assisted α grow dramatically. Furthermore, the structural relationship of ω and α is observed by HRTEM images. It can be found that ω precipitates were formed by {111}β planes shift 0.5d222 along the <111> direction, and the superfine α particles are formed in close proximity of the ω/β interface.

36 MATERIALS SCIENCE↗

Microstructure Evolution and Mechanical Properties of Keyhole Repair Welds in AA 2219-T851 Using Refill Friction Stir Spot Welding

The search for a suitable friction-based keyhole repair technique that fulfills the requirements for high-quality repair welds has become an important research topic, especially for aerospace applications. In order to provide and analyze an universal keyhole repair method for lightweight metals, refill friction stir spot welding is applied to through-hole repairs in 3- and 6-mm-thick sheets of precipitate hardening AA 2219-T851. Keyholes with a diameter of 7.5 mm were repair welded achieving a defect-free microstructure. The correlation between the microstructural evolution imposed by the repair process and the resulting mechanical properties is shown. A comprehensive analysis of the precipitate evolution in peak-aged AA 2219 during RFSSW is presented. Thermal cycle measurements revealed high heating rates and peak temperatures of up to 520 °C in the weld center. The thermal cycle caused mainly dissolution and minor equilibrium phase formation in the stirred zone. In the HAZ, overaging of the strengthening precipitates dominates with minor dissolution and equilibrium phase formation only in the direct proximity of the SZ. Microstructural analysis revealed typical weld zone formation with inhomogeneous grain size distribution in the SZ. The resulting mechanical properties are dominated by an inhomogeneous hardness distribution with lowest hardness in the TMAZ at 5 mm from the center of the weld. During tensile loading main yielding and the final fracture occur in the area of lowest strength. Tensile testing showed yield strength of 40 to 46% and UTS of 28 to 25% below BM values in 3- and 6-mm-thick sheets, respectively. The sheet thickness and post-weld natural aging were found to influence the mechanical properties of the weld significantly.

36 MATERIALS SCIENCE↗

Microstructure evolution and properties of graphene nanoplatelets reinforced aluminum matrix composites

Highlights: • Lamellar structure of GNPs fibers and Al matrix was obtained in the rolling direction. • Stacking faults were observed in Al grains due to greatly increased GNPs/Al interfaces. • Strength of Al-0.2 wt% GNPs increased 36.8% with negligible electrical conductivity loss. - Abstract: Aluminum matrix composites reinforced with graphene nanoplatelets (GNPs) were prepared by continuous casting and subsequent rolling. Al-GNPs master alloy, prepared by ball milling and cold pressing, was added into Al melts to fabricate the composites. Microstructure evolution of the composites were observed using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron back scattered diffraction (EBSD). GNPs distributed uniformly in the as-cast specimen and then transformed into fibers in the rolling direction after deformation and finally a lamellar structure formed in the composites. Raman spectra showed that the structural damage of GNPs mainly came from ball milling. The interface between GNPs and Al was well combined in general while a few microcracks were observed, which reduced the ductility of the composites and no adverse aluminum carbide (Al{sub 4}C{sub 3}) was detected at the interface. Stacking faults were observed interior of the aluminum grain, which may due to the existence of plentiful interface introduced by GNPs. Fracture observation revealed that the load transferred from Al matrix to GNPs. The ultimate tensile strength of Al-0.2 wt% GNPs composites was about 36.8% higher than that of pure Al with the same casting and rolling process, which should result from the lamellar structure and load transfer, while the conductivity of the composites decreased slightly, indicating that interface scattering between Al and GNPs is very limited. The investigation results show that Al-GNPs composite is potential for high strength and high conductivity application.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effect of Gold on the Microstructural Evolution and Integrity of a Sintered Silver Joint

There is a need for next-generation, high-performance power electronic packages and systems employing wide band gap devices to operate at high temperatures in automotive and electric grid applications. Sintered silver joints are currently being evaluated as an alternative to Pb-free solder joints. Of particular interest is the development of joints based on silver paste consisting of nanoscale or micron scale particles that can be processed without the application of an external pressure. Microstructural evolution at the interface of a pressureless sintered silver joint formed between a SiC die with a Ti/Ni/Au metallization and an Active Metal Brazed substrate with Ag metallization at 250 °C was evaluated using Scanning Electron Microscopy, X-ray microanalysis, and X-ray Photo Electron Spectroscopy. Results from Focused Ion Beam cross-sections show that during sintering, the pores in the sintered region close to the Au layer tend to be smaller and are oriented predominantly with their longer dimension oriented parallel to the interface. With further densification, this results in the alignment of small pores parallel to the interface, creating a path for easy crack propagation. Lastly, X-ray microchemical analyses results confirm interdiffusion between Au and Ag and that a region with poor mechanical strength is formed at the edge of this region of interdiffusion.

36 MATERIALS SCIENCE↗

Microstructural evolution in doped high entropy alloys NiCoFeCr-3X (X=Pd/Al/Cu) under irradiation

Commonly studied equatomic single-phase FCC high entropy alloys based on 3d transition metals like NiCoFeCr do not provide adequate strength and radiation resistance at high doses for nuclear structural applications. In the current study, the major alloying effects like lattice distortion, ordering and clustering tendencies were investigated by adding low concentration of Pd, Al, or Cu respectively to study the doping effects on the ion irradiation response of NiCoFeCr alloy. The alloys were irradiated with 3 MeV Ni 2+ ions at 500 °C to a fluence of 1 × 10 17 /cm 2 at a beam flux of approximately 2.8 × 10 12 ions/cm 2 /s. The microstructural evolution upon irradiation i.e., formation of dislocation networks, radiation induced segregation and precipitation, and void formation were studied in detail. Further, post-irradiation characterization results showed that a Pd addition leads to a high void nucleation rate but controlled void growth, which may be attributed to increased lattice distortion. In Al added HEA, our microstructural analysis indicates that radiation induced ordered L1 2 precipitates do not affect void swelling significantly. Cu addition led to Cu precipitation that drastically suppressed dislocation density and void swelling of the alloy. Additionally, a model was developed to qualitatively describe the trend in void swelling of typical FCC alloys under ion irradiation. This model was able to qualitatively explain the suppression and reappearance of void swelling in ion irradiated alloys that generally occurs near the region with peak implanted ion concentration.

36 MATERIALS SCIENCE↗

Unveiling the microstructural evolution of carbon fibers derived from polyamide-6

Polyacrylonitrile-based carbon fibers have dominated the industry for decades, but the high cost of polyacrylonitrile has prevented the widespread adoption of carbon fiber in high-volume structural applications. As such, a significant amount of research has been dedicated to finding an alternative, low-cost carbon fiber precursor. In this work, carbon fibers were produced from polyamide-6 using metal salt impregnation and a thermo-oxidative stabilization step. To gain further insight into the carbonization process and microstructural transformation, the morphologies, crystallinities, elemental compositions, and thermal stabilities of the fibers were characterized at various stages of processing. The stabilization step resulted in a significant increase in carbon yield, indicating a dramatic increase in thermal stability. This is due to the crosslinking of polyamide-6 chains, which was confirmed by functional group analysis. The crystallinity of the fibers was also significantly altered during processing, as the produced carbon fibers consisted of pseudo-amorphous carbon with two distinct regions of metal salt impregnation. Finally, the findings and microstructural evolution mechanisms provide guidelines for further research into carbon fiber produced from polyamide-6.

36 MATERIALS SCIENCE↗

Influence of post deposition annealing on the microstructural evolution and tensile behavior of austenitic stainless-steel alloy 709 made by laser powder bed fusion

Structural materials used in the next generation nuclear reactors or other advanced energy systems are often required to withstand higher operating temperatures for a longer service life. Alloy 709 (A709), a Nb-containing and N-stabilized Fe-25Ni-20Cr austenitic stainless steel, has been recommended for high-temperature reactor constructions due to the better performance over the baseline Type 316H stainless steel. Here, in the current manuscript, for the first time, the microstructure evolution and tensile behavior of an A709 made by laser powder bed fusion (LPBF) is discussed. The as deposited and heat treated LPBF alloys are compared with a reference wrought alloy. Owing to the chemical segregation and a higher number of dislocations, the LPBF materials show a significantly higher density of precipitates formed during high temperature treatments when compared to the wrought samples. This is reflected when looking at the tensile properties, both at room and elevated temperatures, where LPBF samples show higher strengths compared to wrought materials.

36 MATERIALS SCIENCE↗

Microstructure evolution during binder jet additive manufacturing of H13 tool steel

H13 is one of the most used tool steels for both hot and cold work tooling applications. Binder jet additive manufacturing offers the potential to deposit complex tools at scale due to larger powder bed sizes and faster deposition rates. However, to date there is no published literature on the sintering of H13 to full densification. Here, we discuss the pressureless sintering of binder jet AM H13 steel to full densification via supersolidus liquid phase sintering (SLPS) while presenting appropriate process windows (1360 °C – 1380 °C) for densification without distortion. The process windows have been rationalized based on thermodynamic calculations of liquid volume fractions with temperature. We show that higher binder saturation results in higher carbon retention and subsequently early liquid formation that can initiate the sintering process at lower temperatures. We report abnormal grain growth during sintering and found that the solidification phase transformations play a critical role on microstructural evolution and must be considered to accurately model the kinetics of SLPS.

36 MATERIALS SCIENCE↗

Microstructural evolution and hardness response in the laser beam welded joints of pure titanium during recrystallization and grain growth

Highlights: • The LABs and high local misorientations indicate the existence of plastic strains in the as-welded HAZ and FZ. • During heat treatment the recrystallization occurs in the HAZs, decreasing plastic strains, but it doesn't appear in the FZs. • The coarse and unstrained grains gradually replace the fine and strained ones in the HAZs during recrystallization. • The decrease of plastic strains in the HAZs during recrystallization causes the descent of average hardness values based on the strain strengthening. - Abstract: Microstructural evolution and hardness response in the laser beam welded joints of pure titanium during recrystallization and grain growth were investigated by means of electron backscatter diffraction and hardness measurement. The low-angle boundaries (LABs) and high local misorientations, in the as-welded heat affected zone (HAZ) and fusion zone (FZ), indicate the existence of plastic strains caused by the plastic strains due to the thermal stress and the non-equilibrium phase transformations. The recrystallization occurs in the HAZs during heat treatment, but the grain growth after recrystallization does not appear under the heat treatment conditions. Moreover as a result of the slightly high impurity contents in the as-welded FZ, no distinct recrystallization is found in the FZs in this work. During recrystallization in the HAZs, the coarse and unstrained grains with equiaxed shape and smooth boundary gradually consume the fine and strained ones with irregular shape and serrate boundary. Meanwhile, the LABs disappear and the low local misorientations replace the high ones in the modified grains. The recrystallization during heat treatment causes the decrease of plastic strains in the HAZs, which reflects on the descent of average hardness values based on the strain strengthening.

36 MATERIALS SCIENCE↗

Microstructure evolution and mechanical properties of Cu/Sn/Ag TLP-bonded joint during thermal aging

Highlights: • The thermal reliability of the Cu/Sn/Ag TLP-bonded joint was investigated through high-temperature storage. • A diffusion reaction occurred at the interface between Cu{sub 3}Sn and Ag{sub 3}Sn during thermal aging. • The mechanism of the Cu{sub 3}Sn/Ag{sub 3}Sn interfacial reaction was investigated from thermodynamics and kinetics. - Abstract: Low-temperature transient liquid phase (TLP) bonding is a promising joining technology for high-temperature electronic devices packaging. However, the effect of thermal aging on the joint microstructure and performance has been rarely studied so far. In this paper, the relationship between microstructural evolution and mechanical property was developed for the Cu/Sn/Ag TLP-bonded joint during 350 °C aging. Experimental results show that an interfacial reaction occurs between the intermetallic compounds (IMCs) of Cu{sub 3}Sn and Ag{sub 3}Sn, which induces that a great amount of Cu{sub 3}Sn particles or wedges embed into the Ag-Sn phase layer. The reaction process is controlled by a volume diffusion of Cu elements from the Cu substrate, and capable of promoting the transformation from Ag{sub 3}Sn into Ag(Sn) solid solution. Cu{sub 41}Sn{sub 11} phase can be formed at the expense of Cu{sub 3}Sn and Cu, of which transformation process is completely achieved after aging for 480 h, and the Cu(Sn) solid solution intimately contacts with the opposite Ag(Sn) solid solution in many areas after aging for 960 h. The joint mechanical property initially declines due to the formation of Cu{sub 41}Sn{sub 11} phase and Cu-Sn IMCs grain coarsening, and then increases because of the complete depletion of Cu{sub 3}Sn and substantial precipitation of Cu(Sn) solid solution. After aging for nearly 1000 h, the joint still maintains a high shear strength of >40 MPa, indicating an excellent thermal reliability.

36 MATERIALS SCIENCE↗

Microstructure evolution of Ag–8Au–3Pd alloy wire during electromigration

As the continuous shrinkage of the interconnect line width in microelectronics devices, there is a growing concern about the electromigration (EM) failure of bonding wire. In addition, an innovative Ag–8Au–3Pd alloy wire has shown promise as an economical substitute for gold wire interconnects due to the cost pressure of gold in the last decade. In present study of the Ag–8Au–3Pd alloy wire, the surface diffusion occupied the dominant position during EM failure, and the activation energy was found to be 0.61 eV. In order to reveal the failure mechanism, the cross-sections of the Ag–8Au–3Pd alloy wire during EM were prepared by focused ion beam (FIB) micro-machining for electron backscatter diffraction (EBSD) analysis. The microstructure evolution of the Ag–8Au–3Pd alloy wire was characterized by the grain size and grain boundary. As a result, the EM failure originates in the atom transportation, which causes grain size increasing and atom diffusion on the wire surface. - Highlights: • The activation energy of Ag–8Au–3Pd alloy wire was obtained as 0.61 eV. • During EM, the silver atoms diffused from negative to the positive terminal on the wire surface. • The microstructure (grain size and grain boundary) was characterized by FIB-EBSD. • During EM, the atom transportation was found to cause grain size growth and atom diffusion on the wire surface.

36 MATERIALS SCIENCE↗

Microstructural evolution and hardness changes in ion irradiated nickel-based Haynes 282 superalloy

This study investigated the crucial aspects of thermal and irradiation stability in precipitation hardened Haynes 282 Ni-based superalloy. The Haynes 282 Ni-based alloy was irradiated by 8 MeV Ni 3+ ions to assess its resistance to phase instabilities and mechanical property alterations. The mid-range doses (at a depth of ∼1 µm) were 1 and 10 displacements per atom (dpa) at temperatures of 600°C and 750°C. Nanoindentation tests provided insights into bulk equivalent hardness of the irradiated and pristine regions, while scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDS) were used to examine the microstructural evolution of irradiation-induced defects and γ′ -Ni 3 (Al, Ti) precipitates and defect structure under irradiation. These precipitates, with an average diameter of 29 nm and a number density of 5 x 10 21 /m 3 , acted as robust dispersion strengthening agents with high radiation point defect sink strength. Remarkably, irradiation did not significantly alter the size or number density of the γ′ precipitates, indicating exceptional thermal stability and radiation resistance of these precipitates at the examined conditions. Radiation-induced dislocation loops were observed at 600°C, albeit without a substantial impact on mechanical properties due to the dominance of γ′ precipitates on the overall alloy strength. The superior stability of γ′ precipitates observed in this study contrasts with several previous research findings on Ni-based alloys that reported poor precipitate stability. Plausible reasons for this difference are discussed. Moreover, this work explicitly outlines a physically grounded approach to ensure accurate microstructure-hardness correlations and clarifies the hardening model by addressing common misapplications of superposition in prior studies.

36 MATERIALS SCIENCE↗

In-Situ Study of Microstructure Evolution of Spinodal Decomposition in an Al-Rich High-Entropy Alloy

High-entropy alloys (HEAs) are materials which leverage the entropy of mixing to motivate the formation of single-phase solid solutions, even of immiscible elements. While these materials are well-recognized for their application to structural engineering, there is increasing interest in the use of HEAs for functional applications such as memory storage and energy devices. The current work investigates the HEA Al 1.3 CoCrCuFeNi, which has been previously shown to be single-phase at high temperatures, but undergoes phase separation at lower temperatures, transforming the structural and the functional properties. This phase separation is investigated at high temperatures with in-situ small angle neutron scattering (SANS) and scanning transmission electron microscopy (EDS). These techniques show that increasing the temperature up to 800°C, the microstructure of the HEA adiabatically disorders and abruptly homogenizes near 700°C, which is consistent with spinodal decomposition. Overall, the microstructural evolution proceeds mainly by the atomistic redistribution of the constituent elements within simple crystal lattices, producing coherent phase mixtures.

36 MATERIALS SCIENCE↗