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Influence of High Pulsed Magnetic Field on the Dislocations and Mechanical Properties of Al{sub 2}O{sub 3}/Al Composites

At T6 state, Al–Zn–Mg–Cu aluminum matrix composites reinforced with Al{sub 2}O{sub 3} particles generated in situ were subjected to high pulsed magnetic fields at different magnetic induction intensities (B = 2, 3 and 4 T). The results show that the dislocation densities in the treated samples increased with increasing B, and the magnetoplastic effect was determined to be the primary cause. The effect of the magnetic field is believed to alter the spin state of free electrons between dislocations and obstacles from the singlet state (associated with high bonding energy) to the triplet state (low bonding energy). The maximum ultimate tensile strength of 532 MPa was obtained at B = 4 T with 30 pulses, which was 20.7% higher than that of the initial sample, primarily because of dislocation strengthening. At B = 2 T, the elongation was at its maximum of 9.3%, representing an increase of 12% compared with the initial sample, while the associated ultimate tensile strength (447 MPa) was still higher than that of the untreated sample (440 MPa). The relationship between mechanical properties and microstructure was analyzed, and the improved properties observed in this work are explained by the transition of the electron spin state and the piling up of dislocations.

36 MATERIALS SCIENCE↗

A microstructure-based modeling approach to predict the mechanical properties of Zr alloy with hydride precipitates

In nuclear reactors, hydrides can form in fuel cladding due to hydrogen absorption in ZIrcaloy and cause embrittlement. This work presents a microstructure-based finite element model to predict the stress-strain response of Zircaloy containing hydrides. Quantitative microstructural details extracted from scanning electron microscopy (SEM) images were used to generate heterogeneous microstructures including the morphology and spatial distribution of hydrides. The constitutive material model for zircaloy in this study is based on crystal plasticity theory which considers the hexagonal close-packed (HCP) atomic structure of Zircaloy material. The hydrides were modeled as brittle material along with a damage model. Hydride formation inside the zircoloy matrix results in residual stress. This phenomenon is also captured in this model. A parametric study has been conducted to understand the effect of volume fraction, orientation, and lamellae thickness of the hydride phase on the mechanical properties of the overall material.

Kulkarni, Shank S.↗

Assessment of Process Modeling Tools for Determining Variability in Additively Manufactured Parts

The Advanced Materials and Manufacturing Technologies (AMMT) program aims to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy However, the unique aspects of additive manufacturing (AM) materials in terms of their processing history, microstructure, and properties, are a major barrier for qualification and certification of nuclear components. Much of this challenge may be attributed to component scale variations in microstructure and properties that are driven by local influences of process conditions and geometry on thermal history, melt pool dynamics, and corresponding microstructure evolution. Computational modeling tools may be helpful in this regard to aid in predicting and controlling this level of variability. The purpose of this report is to review the current state-of-the-art for process modeling with regards to metal AM. For this purpose, we consider specifically the case study of laser powder bed fusion (LPBF) processing of SS316, a family of alloys that are both commonly used in nuclear energy applications and suitable for AM processing. The report first introduces the necessary components of a process modeling workflow, followed by a review of the current status of each. At the end, application of these modeling tools to understanding variability in AM process given their current state are considered, and recommendations for future development are proposed

36 MATERIALS SCIENCE↗

Microstructural Development and Mechanical Properties of Friction Stir Welded Ferritic Stainless Steel AISI 409

This work investigates the effect of friction stir welding process parameters (rotation rate and traverse speed) on the microstructural evolution of friction stir welded (FSWed) ferritic stainless steel (FSS) AISI 409. Optical microscope, scanning electron microscope and electron backscattering diffraction are used to quantitatively assess the development in grain structure and texture. The microstructural development suggested that thermo-mechanical deformation occurs in the stir zone within the austenite/ferrite phase region, ultimately transforming upon cooling into bainitic/ferritic microstructure. The fraction and size of the bainitic/ferritic grains are found to vary through the thickness of the joints. High fractions of coarse ferritic grains are found near the top of the stir zone, and low fraction of fine ferritic grains is found near the bottom of the stir zone. This bainitic/ferritic grain structure resulted in an increase in the hardness of the stir zone by about 74% relative to the base material. The tensile strength of the FSWed FSS joints is almost at the same level of the base material with reduction in the ductility as a result of the increased hardness of the weld zone.

36 MATERIALS SCIENCE↗

An investigation on microstructure evolution and mechanical properties during liquid state diffusion bonding of Al2024 to Ti–6Al–4V

Joining mechanism of Ti/Al dissimilar alloys was studied during liquid state diffusion bonding process using Cu/Sn/Cu interlayer at 510 °C under vacuum of 7.5 × 10{sup −5} Torr for various bonding times. The microstructure and compositional changes in the joint zone were analyzed by scanning electron microscopy equipped with energy dispersive spectroscopy and X-ray diffraction. Microhardness and shear strength tests were also applied to study the mechanical properties of the joints. It was found that with an increase in bonding time, the elements of interlayer diffused into the parent metals and formed various intermetallic compounds at the interface. Diffusion process led to the isothermal solidification and the bonding evolution in the joint zone. The results from mechanical tests showed that microhardness and shear strength values have a straight relation with bonding time so that the maximum shear strength of joint was obtained for a bond made with 60 min bonding time. - Highlights: • Liquid state diffusion bonding of Al2024 to Ti–6Al–4V was performed successfully. • Diffusion of the elements caused the formation of various intermetallics at the interface. • Microhardness and shear strength values have a straight relation with bonding time. • The maximum shear strength reached to 36 MPa in 60 min bonding time.

36 MATERIALS SCIENCE↗

Explicit Backscattering Coefficient for Ultrasonic Wave Propagating in Hexagonal Polycrystals with Fiber Texture

Hexagonal polycrystalline materials such as titanium, zirconium and magnesium are common in engineering structures like car bodies and airplane engines. These components are usually specially designed in microstructure level to guarantee desired mechanical properties, so microstructure characterization is of great importance to the optimization of manufacturing processes. Compared with traditional destructive characterization methods like scanning electron microscopy (SEM), the ultrasonic approach is nondestructive and cost-effective. Although some progress has been made in ultrasonic microstructure characterization of polycrystal aggregates of hexagonal grains, some factors like macro texture and grain size distribution associated with realistic microstructures were not accounted for yet. Targeting one common texture component for hexagonal polycrystalline materials, {0001} basal fiber texture, this paper derived the explicit backscattering coefficient for aggregates of ellipsoidal grains through one texture parameter and obtained an analytical backscattering coefficient for microstructures with various grain size distributions. In this study, the basal fiber texture was quantified by the 1D Gaussian orientation distribution function (ODF), which merely includes one texture parameter, and its relationship with generalized spherical harmonics ODF was also addressed. Moreover, explicit expressions for effective elastic moduli and elastic constant covariances were derived. Furthermore, some computational examples were given to demonstrate the impacts of texture, frequency, grain geometry and grain size distribution on backscattering behavior. The theoretical results in this study will greatly benefit the later ultrasonic microstructure characterization of hexagonal polycrystalline materials.

42 ENGINEERING↗

Microstructure, microstructural stability and mechanical properties of sand-cast Mg–4Al–4RE alloy

This paper presents a methodology for assessing the phase composition and the results of structural stability tests of the sand-cast Mg–4Al–4RE alloy after annealing it at 175 and 250 °C for 3000 h. The microstructure was analyzed with optical, scanning electron, and transmission electron microscopy. The phase composition was determined with X-ray diffraction. The structure of the Mg–4Al–4RE (AE44) alloy is composed of large grains of α-Mg solid solution, needle-shaped precipitates of the Al{sub 11}RE{sub 3}phase, polyhedral precipitates of the Al{sub 2}RE phase and Al{sub 10}RE{sub 2}Mn{sub 7} phase. After annealing at 175 °C for 3000 h, no changes in the alloy structure are observed, whereas after annealing at 250 °C the precipitates of the Al{sub 11}RE{sub 3} phase are found to be in the initial stages of spheroidization. The coarse-grained structure and unfavorable morphology of the intermetallic phases in the sand-cast AE44 alloy, which are caused by low solidification rates, result in low creep resistance up to 200 °C and low mechanical properties at ambient temperature and at 175 °C. - Highlights: • Complement the knowledge about the microstructure of Mg-Al-RE alloys. • Clarify the mechanism of formation of Mg17Al12 phase above 180 °C. • Applying a chemical dissolution of the α-Mg in order to phase identification. • Applying a statistical test to assess the spheroidization of precipitates. • Quantitative description of microstructure of Mg-Al-RE alloys.

36 MATERIALS SCIENCE↗

Effect of aging temperature on phase decomposition and mechanical properties in cast duplex stainless steels

The microstructure and mechanical properties in unaged and thermally aged (at 280 oC, 320 oC, 360 oC, and 400 oC to 4300 h) CF–3 and CF–8 cast duplex stainless steels (CDSS) are investigated. The unaged CF–8 steel has Cr-rich M23C6 carbides located at the δ–ferrite/γ– austenite heterophase interfaces that were not observed in the CF–3 steel and this corresponds to a difference in mechanical properties. Both unaged steels exhibit incipient spinodal decomposition into Fe-rich α–domains and Cr-rich α’–domains. During aging, spinodal decomposition progresses and the mean wavelength (MW) and mean amplitude (MA) of the compositional fluctuations increase as a function of aging temperature. Additionally, G–phase precipitates form between the spinodal decomposition domains in CF–3 at 360 oC and 400 oC and in CF–8 at 400 oC. The microstructural evolution is correlated to changes in mechanical properties.

atom probe tomography↗

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↗

Quantifying Grain Level Stress-Strain Behavior for AM40 via Instrumented Microindentation

ABSTRACT Microindentation is performed on hot isostatic pressed (HIP) Mg-Al (AM40) alloy samples produced by high-pressure die cast (HPDC) process for the purpose of quantifying the mechanical properties of the α-Mg grains. The process of obtaining elastic modulus and hardness from indentation load-depth curves is well established in the literature. A new inverse method is developed to extract plastic properties in this study. The method utilizes empirical yield strength-hardness relationship reported in the literature together with finite element modeling of the individual indentation. Due to the shallow depth of the indentation, indentation size effect (ISE) is taken into account when determining plastic properties. The stress versus strain behavior is determined for a series of indents. The resulting average values and standard deviations are obtained for future use as input distributions for microstructure-based property prediction of AM40.

AM40↗

TEM Approaches for Microstructure-Informed Prediction of Mechanical Properties in Structural Alloys

Predicting the mechanical performance of structural alloys from their evolving microstructure remains a major challenge in materials science, particularly for nuclear structural materials, where irradiation-induced defects span multiple types and length scales and interact through complex mechanisms. The dispersed barrier hardening (DBH) [1] and Friedel–Kroupa–Hirsch (FKH) [2,3] models have been widely used to evaluate the hardening contributions of individual obstacles and to estimate tensile strength from quantified microstructures; however, when multiple size-dependent obstacles coexist and evolve, predicting temperature-dependent tensile strength becomes significantly more complex, and a fully consistent hardening model is still lacking. Transmission electron microscopy (TEM) plays a central role in refining hardening models and enabling predictive assessments of tensile strength evolution by providing quantitative characterization of dislocations, irradiation-induced defects (e.g., dislocation loops and cavities), precipitates, and grain structure (Fig. 1.). These experimentally measured defect densities are incorporated into physically based hardening models with size- and shape- dependent obstacle strengths [4], using root-sum-square superposition for obstacles of comparable strength and linear superposition for dissimilar ones [5]. In addition, recent advances in TEM [6-8], including high-resolution imaging, 4D-STEM strain mapping, EDS/EELS elemental analysis, and flash-polishing-based TEM specimen preparation and extraction-replica methods (Fig. 2), further improve the accuracy of microstructural quantification. By comparison with prior studies as well as our own results, we show that when TEM-derived microstructural information is carefully integrated with physically grounded hardening models, yield strength (or irradiation-induced hardening) measured at room temperature can be predicted with good quantitative agreement across multiple alloy classes. In-situ TEM combined with high-temperature mechanical testing represents an important next step for refining hardening models by directly probing dislocation–obstacle interactions across varying irradiation doses and temperatures [9]. Because the barrier strength factor (α) depends on both temperature and obstacle size, it should not be treated as a constant fitting parameter; rather, it must be explicitly evaluated to achieve physically meaningful predictions of mechanical behaviour at operating temperatures. This presentation therefore discusses why all strengthening contributions (e.g., Peierls stress, solid-solution strengthening, voids, bubbles, dislocation loops, dislocation lines, and grain boundaries) must be considered collectively, why appropriate superposition methods are essential when obstacles possess different barrier strength factors, how hardness measurements can be meaningfully related to tensile properties, and how TEM-derived microstructural information can be systematically incorporated into hardening models. More broadly, it outlines a pathway toward microstructure-informed prediction of mechanical properties and supports the goal of establishing science-based tools for evaluating structural materials in extreme environments [10].

Lin, Yan-Ru [ORNL] (ORCID:0000000339991473)↗

Microstructural characterization and mechanical property of active soldering anodized 6061 Al alloy using Sn-3.5Ag-xTi active solders

Active solders Sn-3.5Ag-xTi varied from x = 0 to 6 wt.% Ti addition were prepared by vacuum arc re-melting and the resultant phase formation and variation of microstructure with titanium concentration were analyzed using X-ray diffraction, optical microscopy and scanning electron microscopy. The Sn-3.5Ag-xTi active solders are used as metallic filler to join with anodized 6061 Al alloy for potential applications of providing a higher heat conduction path. Their joints and mechanical properties were characterized and evaluated in terms of titanium content. The mechanical property of joints was measured by shear testing. The joint strength was very dependent on the titanium content. Solder with a 0.5 wt.% Ti addition can successfully wet and bond to the anodized aluminum oxide layers of Al alloy and posses a shear strength of 16.28 {+-} 0.64 MPa. The maximum bonding strength reached 22.24 {+-} 0.70 MPa at a 3 wt.% Ti addition. Interfacial reaction phase and chemical composition were identified by a transmission electron microscope with energy dispersive spectrometer. Results showed that the Ti element reacts with anodized aluminum oxide to form Al{sub 3}Ti-rich and Al{sub 3}Ti phases at the joint interfaces. - Highlights: Black-Right-Pointing-Pointer Active solder joining of anodized Al alloy needs 0.5 wt.% Ti addition for Sn-3.5Ag. Black-Right-Pointing-Pointer The maximum bonding strength occurs at 3 wt.% Ti addition. Black-Right-Pointing-Pointer The Ti reacts with anodized Al oxide to form Al{sub 3}Ti-rich and Al{sub 3}Ti at joint interface.

36 MATERIALS SCIENCE↗

Microstructures and phase transformations of Ti-30Zr-xNb (x = 5, 7, 9, 13 at.%) shape memory alloys

The microstructures, phase transformations and shape memory properties of Ti-30Zr-xNb (x = 5, 7, 9, 13 at.%) alloys were investigated. The X-ray diffraction and transmission electron microscopy observations showed that the Ti-30Zr-5Nb, Ti-30Zr-7/9Nb and Ti-30Zr-13Nb alloys were composed of the hcp α′-martensite, orthorhombic α″-martensite and β phases, respectively. The results indicated the enhanced β-stabilizing effect of Nb in Ti-30Zr-xNb alloys than that in Ti-Nb alloys due to the high content of Zr. The differential scanning calorimetry test indicated that the Ti-30Zr-5Nb alloy displayed a reversible transformation with a high martensitic transformation start temperature of 776 K and a reverse martensitic transformation start temperature (A{sub s}) of 790 K. For the Ti-30Zr-7Nb and Ti-30Zr-9Nb alloys, the martensitic transformation temperatures decreased with the increasing Nb content. Moreover, an ω phase transformation occurred in the both alloys upon heating at a temperature lower than the corresponding A{sub s}, which is prompted by more addition of Nb. Although the critical stress in tension of the three martensitic alloys decreased with increasing Nb content, the Ti-30Zr-9Nb alloy showed a critical stress of as high as 300 MPa. Among all the alloys, the Ti-30Zr-9Nb alloy exhibited the maximum shape memory effect of 1.61%, due to the lowest critical stress for the martensite reorientation. - Highlights: •Ti-30Zr-5Nb alloy is composed of hcp α′-martensite with the M{sub s} of 776 K. •Ti-30Zr-7Nb and Ti-30Zr-9Nb alloys are predominated by orthorhombic α″-martensite. •Ti-30Zr-13Nb alloy consists of a single β phase due to the β-stabilizing effect of Nb. •The martensitic transformation temperatures decrease with increasing Nb content. •Ti-30Zr-9Nb alloy shows the maximum shape memory effect of 1.61%.

36 MATERIALS SCIENCE↗

Thermodynamic modeling and experimental validation of the Fe-Al-Ni-Cr-Mo alloy system

NiAl-type precipitate-strengthened ferritic steels have been known as potential materials for the steam turbine applications. In this study, thermodynamic descriptions of the B2-NiAl type nano-scaled precipitates and body-centered-cubic (BCC) Fe matrix phase for four alloys based on the Fe-Al-Ni-Cr-Mo system were developed as a function of the alloy composition at the aging temperature. The calculated phase structure, composition, and volume fraction were validated by the experimental investigations using synchrotron X-ray diffraction and atom probe tomography. With the ability to accurately predict the key microstructural features related to the mechanical properties in a given alloy system, the established thermodynamic model in the current study may significantly accelerate the alloy design process of the NiAl-strengthened ferritic steels.

36 MATERIALS SCIENCE↗

Temperature and Microstructural Effects on the Superconducting Properties of Niobium Thin Films

Here, superconducting thin films have a wide range of dc and RF applications, from detectors to superconducting radio frequency. Amongst the most used materials, niobium (Nb) has the highest critical temperature (TC) and highest lower critical field (HC1) of the elemental superconductors and can be deposited on a variety of substrates, making Nb thin films very appealing for such applications. Here, we present temperature-dependent dc studies on the critical temperature and critical fields of Nb thin films grown on copper and r-plane sapphire surfaces. Additionally, we correlate the dc superconducting properties of these films with their microstructure, which allows for the possibility of tailoring future films for a specific application.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Creep Resistant Martensitic Steels for Operation at High-Temperatures in Power Generation Applications

Increasing the temperature capabilities of ferritic/martensitic 9-12% Cr steels can help in increasing the operating temperature of land-based turbines and minimize the use of expensive high-temperature alloys in the hot section. A creep resistant martensitic steel, JMP, was developed with the potential to operate at or above 650°C. The design of the alloys originated from computational modeling for phase stability and precipitate strengthening using fifteen constituent elements. Cobalt was used for increased solid solution strengthening, Si for oxidation resistance and different W and Mo concentrations for matrix strength and stability. The JMP steels showed increases in creep life compared to MARBN/SAVE12AD at 650°C for testing at various stresses between 138 MPa and 207 MPa. On a Larson-Miller plot, the performance of the JMP steels surpasses that of state-of-the-art MARBN steel. Approximately 21 years of cumulative creep data are reported for the JMP steels which encompasses various compositions. The relationships between composition-microstructure-creep properties are discussed including characterization of microstructures after >20,000 hours in creep.

Detrois, Martin↗

Spark Plasma Extrusion and the Thermal Barrier Concept

Spark plasma sintering (SPS) is currently a major powder consolidation process with many advantages; however, it is still largely limited to the processing of simple shapes such as discs due to its geometric restrictions. Alternatively, spark plasma extrusion (SPE) is a recently developed process that has superiority over SPS in terms of faster consolidation, generating products of extended geometries and potential grain refinement capabilities under applied current. So far, work on SPE has resulted in large temperature gradients within the extruding material with microstructural and properties in-homogeneities. The present paper reports on a novel approach (thermal barrier concept) that allows the SPE of materials with enhanced uniformity in terms of microstructures and properties. Both aluminum and aluminum-carbon nanotube composites have been successfully processed using this new approach.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

The annealing effects on the micro-structure and properties of RuMoC films as seedless barrier for advanced Cu metallization

100 nm thick RuMoC films and 5 nm thick RuMoC films with Cu capping have been deposited on Si(111) by magnetron co-sputtering with Ru and MoC confocal targets. The samples were subsequently annealed at temperatures ranging from 450 to 650 °C in vacuum at a pressure of 3 × 10{sup −4} Pa to study the annealing effects on the microstructures and properties of RuMoC films for advanced seedless Cu metallization applications. The sheet resistances, residual oxygen contents, and microstructures of the RuMoC films have close correlation with the doping contents of Mo and C, which can be easily controlled by the deposition power ratio of MoC versus Ru targets (DPR). When DPR was 0.5, amorphous RuMoC film (marked as RuMoC II) with low sheet resistances and residual oxygen contents was obtained. The fundamental relationship between the annealing temperatures with the microstructures and properties of the RuMoC films was investigated, and a critical temperature point was revealed at about 550 °C where the components and microstructures of the RuMoC II films changed obviously. Results indicated that below 550 °C, the RuMoC II films remained amorphous due to the well-preserved C-Ru and C-Mo bonds. However, above 550 °C, the microstructures of RuMoC II films transformed from amorphous to nano-composite structure due to the breakage of Ru-C bonds, while the supersaturated solid solution MoC segregated out along the grain boundaries of Ru, thus hindering the diffusion of Cu and O atoms. This is the main mechanism of the excellent thermal stability of the RuMoC films after annealing at high temperatures. The results indicated great prospects of amorphous RuMoC films in advanced seedless Cu metallization applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗