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At least 109 records · Page 6

Microstructural evolution and electrical resistivity of nanocrystalline W thin films grown by sputtering

Highlights: • W thin films with thicknesses of 5–40 nm were deposited by sputtering and annealed up to 400°C. • Grain size of the beta (β)-W was about 5 nm, whereas that of the alpha (α)-W was about 130 nm. • Thickness dependent electrical resistivity variations as a function of annealing temperature were presented. - Abstract: Tungsten (W) thin films and nanostructures, particularly those having a beta (β)-phase, have attracted a large amount of attention lately because an ultrathin β-phase W film attached to a ferromagnetic layer can reverse the direction of magnetization upon current injection. However, in-depth microstructural studies including the phase transformation in W films as a function of thickness and post-deposition heat treatment temperature are rare. Here, we report the microstructural evolution and the change in the electrical resistivity of W films with thicknesses of 5–40 nm. Microstructural analyses indicate that the β-W is nanocrystalline with a small grain size of about 5 nm, while the alpha (α)-W has a grain size larger than 130 nm with random crystal orientation. We present a state diagram showing the phase of the W film as functions of film thickness and annealing temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Study on the Hot Deformation Behavior and Microstructure Evolution of Cu-Cr-In Alloy

Based on the hot compressive tests in the temperature range of 700-900 °C and strain rate range of 0.01-10 s{sup −1}, the hot deformation behavior of a Cu-Cr-In alloy was investigated. The true stress–strain curves of the alloy were obtained, and a constitutive equation for the alloy was established by the method of equivalent stress. The processing maps were constructed based on the constitutive equation, and the microstructural evolutions were analyzed and correlated with the processing maps. The results show that the true stress of the alloy increased with decreasing strain rate and decreased with increasing temperature. The microstructures of the alloy deformed under different conditions were in good accordance with the processing maps results. According to the processing maps and the microstructures of the alloy with true strains of 0.4 and 0.8, the optimal hot deformation conditions lie in the range of 850-900 °C and strain rate range of 0.01-0.1 s{sup −1}.

36 MATERIALS SCIENCE↗

Annealing-induced microstructural evolution and mechanical anisotropy improvement of the Mg-Gd-Y-Zr alloy processed by hot ring rolling

Highlights: • Growth of SRX grains in GBR is random, while that of TBR is anisotropic. • The new texture component in annealed MR weakens the anisotropy obviously. • T6 treatment leads to an excellent comprehensive mechanical property. - Abstract: Hot ring rolling (HRR) is widely used to fabricate large-size seamless ring-shape components. However, this process produces a severe mechanical anisotropy, which is not acceptable in practical industrial application and should be avoided. This paper reports the annealing-induced microstructural evolution and mechanical anisotropy improvement of HRRed Mg-8.12Gd-1.82Y-0.35Zr alloy ring. Results show that annealing treatment could improve the microstructural homogeneity of the ring owing to the occurrence of static recrystallization (SRX). SRX grains are preferentially formed at twin boundaries and initial grain boundaries due to high dislocation density, high level of stored energy, and stress concentration. Twin boundaries, to some extent, can suppress the migration of SRX grain boundaries. In addition, occurrence of SRX weakens the texture intensity and basal pole inclination, leading to a decrease in the mechanical anisotropy of the ring. Considering the weakened anisotropy, comparable strength, and improved ductility, annealing + aging (T6), compared with direct aging (T5), is a more suitable heat treatment schedule for the HRRed Mg-8.12Gd-1.82Y-0.35Zr alloy ring.

36 MATERIALS SCIENCE↗

A Gaussian process autoregressive model capturing microstructure evolution paths in a Ni–Mo–Nb alloy

Additive manufacturing is increasingly being employed to produce components of complex geometries in structural alloys because of the expected energy savings associated with the near-net-shape capability and the ability to build in novel internal features that are not possible with many conventional manufacturing approaches. However, because of the extreme thermal conditions encountered, the non-equilibrium microstructures produced during powder bed-based additive manufacturing processes must be subjected to custom post-heat treatment processes to recover the target mechanical properties. Phase-field models and simulation techniques have matured to a state where the microstructure evolution paths, and the morphologies of the resulting precipitate phases can be predicted reasonably accurately, considering alloy-specific thermodynamic and kinetic aspects of the nucleation and growth processes. However, phase-field simulations are computationally intensive, which precludes the ability to apply the simulations directly to the length scale of the entire component. Therefore, it is highly desirable to develop low-computational-cost surrogate models that effectively capture the physics at the microstructural length scale, while facilitating the design of optimized processing conditions resulting in location-specific targeted microstructures at the component scale. The work presented here demonstrates the application of the materials knowledge system framework to develop a surrogate model that effectively captures the microstructural path during annealing of a Ni–Mo–Nb alloy containing different Mo and Nb compositions known to segregate during solidification under additive manufacturing conditions. Specifically, the surrogate model built in this work is based on a Gaussian process autoregressive model informed by statistical representation of simulated microstructures using two-point correlations and dimensionality reduction through principal component analysis. In conclusion, this surrogate model is shown to capture the bifurcation of the microstructural path during precipitation, which yields a microstructure dominated by the $\gamma^{\prime\prime}$ phase at high Nb concentrations and the $\delta$ phase at low Nb concentrations.

36 MATERIALS SCIENCE↗

Evaluating microstructure evolution in an SOFC electrode using digital volume correlation

Degradation mechanisms within solid oxide fuel cells (SOFC) during thermal cycling limit operational start-up times and cell lifetime, and must therefore be better understood and mitigated. This work explores such mechanisms using digital volume correlation (DVC) techniques applied to lab-based X-ray tomograms where the microstructural evolution is evaluated during the operational cycling of a Ni–YSZ/YSZ cell. To emulate reduced start-up times, five tomograms were collected over four operational thermal cycles to 750 °C at various ramp-rates: 3, 10, 20 and 30 °C min –1 . Two key features are observed in the 3D strain profiles. Firstly, during low ramp-rates the material produces microscopic channels towards cluster-points. This is thought to be caused by the ceramic skeleton inhibiting the effects of sintering. Secondly, previously unseen macroscopic ‘waves’ developed after high-rate cycling, consisting of linear regions of compression and tension throughout the sample. These wave features decay away from a heterogeneous defect which is thought to be responsible for the non-uniform strain profile. This work demonstrates the first use of sub-micron DVC computations applied to an SOFC exposed to operationally relevant temperatures. Lastly, these findings will assist in the development of new electrode materials from their fabrication to operation, ultimately supporting commercial viability of SOFCs.

30 DIRECT ENERGY CONVERSION↗

Effect of Ni content in Cu 1-x Ni x coating on microstructure evolution and mechanical properties of W/Mo joint via low-temperature diffusion bonding

The 93W and Mo1 refractory metals were bonded with different Cu 1- x Ni x coating interlayers of various Ni content using plasma-activated sintering at 700 °C. The effects of the Ni content in the Cu 1- x Ni x coating interlayer on the interfacial microstructure evolution and mechanical properties of the W/Mo joints were studied. The maximum average shear strength of the W/Mo joint was 316.5 MPa when the Ni content of the Cu 1- x Ni x coating interlayer was 25 %. When the Ni content of the Cu 1- x Ni x coating interlayer was below 50 %, the atomic diffusion at the W/Mo joint interface was adequate without the formation of intermetallic compounds, as demonstrated by the High Resolution Transmission Electron Microscope analyses of the joints. The presence of Ni in Cu 1- x Ni x promoted diffusion bonding at the interface, which contributed to the high mechanical properties of the W/Mo joint. With an increase in the Ni content of the Cu 1- x Ni x coating interlayer, the MoNi intermetallic compound (IMC) nucleated and grew at the Cu 1- x Ni x coating/Mo1 interface. When the Ni content of the Cu 1- x Ni x coating interlayer was above 50 %, the generation of a brittle MoNi IMC weakened the shear strength of the W/Mo joint dramatically.

36 MATERIALS SCIENCE↗

Decoupling of strain and temperature effects on microstructural evolution during high shear strain deformation

The interplay between defect generation by shear strain and defect annihilation by local heating is difficult to predict in shear-assisted processing techniques. In this study, we decoupled the effects of high shear strain and external heating in an immiscible Cu-Nb alloy using a pin-on-disk tribometer to mimic the microstructural evolution of material during solid-phase processing. The change in sub-surface deformation, strain distribution, and redistribution of the second phase as a function of temperature were examined using transmission electron microscopy and atom probe tomography. Zener-Hollomon parameter is used to semi-quantify the deformation of Cu-Nb alloys as a function of strain and temperature.

36 MATERIALS SCIENCE↗

Multi-scale modeling of fuel fragmentation and microstructural evolution

An overview of NEAMS program activities to model fuel fragmentation and microstructual evolution to a group of industry attendees at a meeting hosted by EPRI. Topics include atomistic methods to determine grain boundary strength, phase-field fracture modeling to determine critical pressure at grain boundaries, and coupled phase-field-cluster dynamics to model microstructural evolution.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of Zinc Interlayer in Microstructure Evolution and Mechanical Properties in Dissimilar Friction Stir Welding of Aluminum to Titanium

The welding of aluminum (Al) and titanium (Ti) is difficult and challenging due to the differences in their chemical and physical properties, and the formation of brittle intermetallic phases. In the present experiment, a zinc (Zn) interlayer was used during friction stir welding of Al to Ti. The weld was characterized in detail to understand the mechanisms associated with microstructural evolution and improvement in mechanical properties of the weld. X-ray computed tomography results reveal three-dimensional distribution of particles and flakes of titanium in the weld nugget. It was also observed that Ti particles are inhomogeneously distributed in the weld and the distribution depends on their morphology. Such a distribution of Ti was informative in understanding material flow. In addition, the consolidation of Zn in the Al matrix reveals the nature of material flow in the weld nugget as well. The importance of the Zn interlayer and mechanism of phase formation was explored in this study. It was characterized that the mechanical mixing of Zn with Al and Ti alters phase evolution and restricts the formation of conventional Al{sub 3}Ti intermetallic phase. The presence of zinc homogenizes elemental distribution and inhibits the formation of brittle intermetallic phases, which leads to a substantial improvement in mechanical properties of the weld.

36 MATERIALS SCIENCE↗

Effect of microalloying additions on microstructural evolution and thermal stability in cast Al-Ni alloys

Enhancement of thermal stability in Al-Ni alloys through microalloying with slow-diffusing elements, specifically Zr, has been previously reported which is attributed to Zr segregation at the Al/Al 3 Ni interface. In this study, we explore the influence of microalloying Al-Ni alloys with Zr, Ti, V, and Fe on microstructural evolution, hardness, and electrical and thermal conductivity across a range of heat-treatment temperatures from 300 to 450 °C. The distribution of microalloying elements and precipitates after heat treatment is characterized using atom probe tomography (APT). Our investigation confirms Zr segregation to the Al/Al 3 Ni interface, while similar interfacial segregation is absent with the addition of Ti, V, and Fe. Additionally, our analysis of the Al 3 Ni microfiber morphology reveals that their coarsening and spheroidization rates are similar with and without interfacial segregation; thus, retaining the fiber reinforcement through interfacial segregation of slow diffusing elements may not be an effective strategy. Precipitation of L1 2 nanoparticles was found to be the dominant mechanism affecting enhanced hardness and electrical conductivity in Al-Ni-Zr alloys, attributed to precipitation strengthening and solute depletion, respectively. Similar precipitation was not observed for additions of Ti, V, and Fe following heat treatment. We provide a thermodynamic explanation for this limitation. Furthermore, the findings of this study suggest that an effective approach for designing Al-Ni alloys should involve prioritizing microalloying elements to maximize L1 2 precipitation and minimize solute content in the FCC-Al matrix post heat treatment, rather than focusing on Al/Al3Ni interfacial segregation.

36 MATERIALS SCIENCE↗

On the mobility of defect clusters and their effect on microstructure evolution in fcc Ni under irradiation

Here, µs-scale molecular dynamics studies of vacancy and interstitial clusters in fcc Ni revealed three- and one- dimensional (3-D and 1-D) modes of the cluster motion. The 1-D mobility of interstitial defects is known to enhance swelling rate. The theoretical analysis performed here suggests two novel mechanism by which the 3-D mobile clusters affect microstructure evolution under irradiation. First, the mobility of vacancy clusters hinders nucleation of stable voids due to recombination with interstitial-type loops and edge dislocations. Second, the capture efficiency of dislocations is higher for 3-D mobile vacancy and interstitial clusters than single defects, with the combined effect depending on relative fractions of clustered vacancies and interstitials produced in cascades. The observed differences in radiation damage of most fcc and bcc metals is attributed to the difference in cascade-produced vacancy defects: immobile SFTs and loops in fcc metals and mobile clusters in bcc metals. In this context, fcc Ni is similar to bcc metals due to its high stacking fault energy.

36 MATERIALS SCIENCE↗

Investigating microstructural evolution in SolidStir™ extruded oxide dispersion strengthened 14YWT alloy fuel cladding tube

Structural components for extreme environments require advanced materials and manufacturing processes. One such advanced material is oxide dispersion strengthened (ODS) Fe–14 wt.%Cr–3W–0.4Ti–0.3Y 2 O 3 (14YWT), which is developed for components to be used in Gen IV and fusion nuclear reactors. However, the conventional manufacturing processes to produce components, such as fuel cladding tubes, either do not retain the desired microstructural attributes or are costly and less efficient. As a result, a more attractive option is a novel manufacturing process developed on the principle of friction stir welding or processing (FSW/P) and commercially referred to as SolidStir™ Extrusion (SSE). Here this study used the SSE technique to study the manufacturing and microstructural evolution of a fuel cladding tube made of ODS 14YWT alloy. The cladding extrusion by the SSE technique involved the use of ball-milled 14YWT powders with Y, Ti, and O in the solid solution and the use of a specially designed W-25Re-Hf tool for consolidation and extrusion of the powders. A scanning electron microscope (SEM), electron backscattered diffraction (EBSD), and transmission electron microscope (TEM) were utilized for microstructural characterization. A Keyence microscope captured macrostructural photographs of the extruded tube. EBSD examination of the extruded tube on both transverse and longitudinal cross-sections showed the presence of dynamically recrystallized grains and revealed that the average grain size of the transverse cross-section was smaller than that of the longitudinal cross-section. The texture was weak and consisted of some amount of shear texture. The presence of nano-oxide clusters or precipitates of Y, Ti, and O (pyrochlores) in the extruded tube was determined by TEM. Aging heat treatment caused the average precipitate size to decrease and the density to increase compared to the as-processed condition. The results indicated that SSE is a viable tool for manufacturing fuel cladding tubes with the desired microstructural attributes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructure Evolution and Implications for Cu Nanointerconnects and Beyond

The continued scaling of Cu low k technology is facing serious challenges imposed by basic limits from materials, processing and reliability. This has generated great interests recently to further develop Cu nanointerconnects and alternates, particularly Co and Ru nanointerconnects beyond the 10nm node. The performance and reliability are important considerations for the development of nanointerconnects in addition to challenges from processing complexity and manufacturing cost. In this paper, we investigate the microstructure evolution in Cu, Co and Ru nanointerconnects and the effects on resistivity and electromigration (EM), two key factors contributing to the RC delay and reliability of the nanointerconnects.

36 MATERIALS SCIENCE↗

In-situ TEM observation of shear induced microstructure evolution in Cu-Nb alloy

Phase boundaries in multiphase alloys govern defect interaction and chemical intermixing across different phases during plastic deformation. Dynamic interaction of defects with phase boundaries in multiphase alloys, especially for immiscible alloys, has been topic of significant research interest in recent years. In this work, we describe a novel approach for carrying out in-situ TEM shear deformation to directly observe interfacial microstructural evolution of a Cu-Nb alloy. A unique double shear specimen geometry is microfabricated by a focused ion beam technique to apply shear deformation upon push loading inside the TEM. From the real-time observation, we discover that the phase boundary with a zigzag morphology effectively blocks stacking faults nucleated in a Cu grain from slipping into a Nb grain. Meanwhile, the Cu phase bears the most plastic deformation through slip or twinning mechanisms. This work sheds light on understanding the shear deformation and the behavior of phase boundaries in multiphase alloys during shear deformation.

36 MATERIALS SCIENCE↗

Understanding Weld Formation and Microstructure Evolution in Laser Welded Stainless Steels and Ti-6Al-4V

High energy density welding processes are used for many industrial applications, such as aerospace and defense, and certain joint configurations and welding situations render post-weld inspection techniques difficult. Due to the inability to confirm penetration, there is a continual industrial need to improve prediction capabilities to aid in parameter selection. It is also necessary to understand the microstructural evolution to modify phase fractions and mitigate weldability related concerns such as solidification cracking or reduced corrosion performance.

42 ENGINEERING↗

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↗

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↗

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↗