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At least 235 records · Page 13

Effect of polycyclosilane microstructure on thermal properties

Thermal characterization of polysilanes has focused on the influence of organic side chains, whereas little is understood about the influence of silane backbone microstructure on thermal stability, phase properties, and pyrolysis. To address this knowledge gap, we prepared three distinct polycyclosilanes: linear polymers synthesized from the cyclosilane building blocks 1,4Si 6 and 1,3Si 6 , as well as a cyclic polymer of 1,3Si 6 . Thermal properties across the temperature range 25 to 600 °C were investigated using differential scanning calromietry (DSC) and thermogravimetric analysis (TGA). We found differences between linear and cyclic materials, including a phase transition unique to the cyclic polymer and lower rates of mass loss during pyrolysis. Density functional theory (DFT) calculations provided insight into microstructure-dependent pyrolysis.

36 MATERIALS SCIENCE↗

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

A process optimization framework for laser direct energy deposition: Densification, microstructure, and mechanical properties of an Fe-Cr alloy

Laser Direct Energy Deposition (DED) is a metal additive manufacturing technique with the ability to fabricate large and complex parts through deposition of metal powders. However, achieving high-density parts and targeted build heights using DED can be challenging due to the large number of highly sensitive process variables. This work proposes a robust fabrication parameter optimization framework to generate process maps for primary parameters in DED, including laser power, scan speed, mass flow rate, hatch spacing, and layer height. Simple single-track experiments were utilized to map out the parameter space, and a combination of geometric criteria for hatch spacing and layer height were proposed to determine parameter sets that achieve both targeted build heights and mitigate porosity formation. Using this framework, specimens with >99 % density and consistent mechanical properties were successfully fabricated over a wide range of process parameters for an Fe-9wt.%Cr (Fe9Cr) alloy, a surrogate for radiation damage-resistant reduced activation ferritic/martensitic (RAFM) steels. Processing these materials using DED is of particular interest in the development of plasma facing components for nuclear fusion applications. The microstructure and mechanical properties of as-printed Fe9Cr were characterized using optical and electron microscopy, X-ray diffraction, and uniaxial tensile tests. As-printed Fe9Cr displayed ~25 % elongation and ultimate tensile strengths of up to 475 MPa which is comparable to similar wrought alloys. Finally, the proposed framework will allow for accelerated DED parameter optimization for novel alloy systems, as well as open the possibility for local microstructure control while simultaneously mitigating defect formation.

42 ENGINEERING↗

Uranium-Titanium Alloys: The Effect of Ti Content on Phase Transformations, Microstructures, and Mechanical Properties

This report documents the findings of collaborative research done at Sandia National Laboratory and the Y-12 Development Division during the 1980s. Ongoing progress reports were presented at various U. S. Department of Energy (DOE) meetings throughout the 1980s, but the findings were never integrated into an inclusive final report. This report provides a summary of the key findings and implications of this research. This work was supported by the DOE National Nuclear Security Administration. The effect of titanium content on phase transformations, microstructures, and mechanical properties of uranium-titanium alloys has been investigated in alloys containing 0.3 wt.% to 2.0 wt.% Ti.

36 MATERIALS SCIENCE↗

Effect of Hot Isostatic Pressing on the Microstructure and Mechanical Properties of Additively Manufactured Ti Alloys

A previous SAND report, SAND2020-11353 described the basic metallurgical and surface roughness properties of additively manufactured Ti-64 material made using a powder bed fusion process. As part of that work, material was post-processed using a hot isostatic press (HIP) to densify and heat treat the material. This report is meant as an addendum to the original report and to provide specific data on material processed with HIP. The main focus of this report is to show the effects of HIP on the microstructure and mechanical properties of AM Ti-64 and Ti-5553.

36 MATERIALS SCIENCE↗

Microstructural Characteristics, Mechanical Properties, and Corrosion Behavior of Field-Assisted Diffusion Welded Alloy 617

This study investigated the microstructural characteristics, mechanical response, and corrosion resistance of Alloy 617 diffusion welded by electric field-assisted sintering (EFAS). The microstructure exhibited good grain boundary (GB) migration across the interface and flat interface in the samples bonded at different conditions. Graded grain size was observed, with grain coarsening being more significant near sample surface due to EFAS-induced temperature gradient. Tensile testing revealed that the specimens fractured in the matrix away from the interface. The peak strength of 807 MPa was obtained in the samples welded at 1000°C. The materials obtained at 1100°C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed the flat interfaces were less ductile compared to the matrix. The hardness reduced near sample surfaces due to enlarged grains induced by temperature gradient. The interfaces with GB migration exhibited improved corrosion resistance in molten salt compared to the flat interfaces.

36 - MATERIALS SCIENCE↗

Interfacial microstructure and mechanical properties of rotary inertia friction welded dissimilar 422 martensitic stainless steel to 4140 low alloy steel joints

In this work, dissimilar rotary inertia friction welds between 422 martensitic stainless steel and 4140 martensitic low-alloy steel were made to fabricate prototype heavy-duty diesel engine pistons. The influence of the inertia friction welding process and post weld heat treatment (PWHT) temperature on the interfacial microstructure evolutions and corresponding effects on mechanical properties of the 422/4140 welds were evaluated in detail. Carbon diffused from the 4140 side to the 422 side during PWHT at 650 °C for 1.5 h, causing the formation of a hard carbide-rich layer on the 422 side, and a softer but discontinuous C-depleted layer the 4140 side. PWHT at 700 °C for 1.5 h greatly accelerated C diffusion across the interface relative to 650 °C, resulting in a thicker hard carbide-rich layer and a relatively thick and continuous layer of coarse C-depleted grains (ferrite) on the 4140 side. In addition, the PWHT temperature greatly influenced the tensile properties and fracture behavior of the welds, with the 650 °C PWHT-ed samples failing predominately in a ductile manner in the 4140 heat affected zone during tensile testing. Conversely, the 700 °C PWHT specimens exhibited a strength reduction compared with the 650 °C PWHT specimens because of additional coarsening of the interfacial ferrite layer and softening of the base materials during PWHT, with brittle fracture between the hard and soft layers the predominate failure mechanism. Based on the findings, a reduced PWHT temperature and/or time, minimizing the hardness differential of the base metals, and pre-heating the 422 steel prior to welding are the potential pathways to achieve a more optimal balance between desirable tempering and stress relief of the weld microstructure and undesirable C migration across the weld interface, and to reduce the strength mismatch across the weld.

36 MATERIALS SCIENCE↗

Influence of Rare Earth Ce Additions on Microstructure and Mechanical Properties of Experimental Pipeline Steels

Herein, the effect of Ce additions ranging from 57 to 263 ppm is evaluated for an experimental pipeline steel. Compared to the Ce-free steel, progressive Ce additions result in a slightly refined microstructure, significantly improve transverse impact properties, and slightly increase strength. All these observations can be attributed to the gradual transformation of Mn sulfide and Mn–Si–Al oxide inclusions to Ce-containing oxide/sulfides. In particular, the inclusions consist exclusively of sub-5 μm spherical Ce 2 O 2 S particles upon near-stoichiometric additions of Ce, considering the oxygen and sulfur impurity level of the steel. In conclusion, the results suggest that Ce is a potentially promising alloying addition for next-generation pipeline steels by replacing overtly deleterious inclusions with potentially beneficial ones.

36 MATERIALS SCIENCE↗

The Trajectory of Additively Manufactured Titanium Alloys with Superior Mechanical Properties and Engineered Microstructures

Additive manufacturing (AM) plays a crucial role in the manufacturing and development of advanced materials including titanium alloys for engineering applications. During the last two decades, a great deal of effort has been devoted to print titanium parts with desired properties. However, due to presence of non-equilibrium/metastable phases, anisotropic microstructure, and various porosities in the printed titanium alloys, achieving an excellent combination of mechanical properties has been challenging. Here this review paper aims to provide a comprehensive overview of multiple post-process and in-process approaches to achieve enhanced strength-ductility combinations by microstructure engineering. Approaches such as addition of alloying elements/nucleants, multi-step post heat treatment, in-situ heat treatment, forced inter-pass cooling, in situ peening/rolling, hybridizing microstructure, high-intensity acoustic vibration, thermo-hydrogen refinement of microstructure, deliberately introducing lack of fusion defects with subsequent hot isostatic pressing are discussed in detail. Finally, we conclude by highlighting the challenges associated with each method and potential areas of improvement that can pave the way to develop reliable components with enhanced performance.

36 MATERIALS SCIENCE↗

Electric field enhanced diffusion welding of alloy 617: Microstructural characteristics and mechanical properties

This study investigated the microstructural characteristics and mechanical behavior of diffusion welded nickel-based Alloy 617 obtained by electric field-assisted sintering (EFAS) using various parameters. The interfacial microstructure exhibited different characteristics including good grain boundary (GB) migration across the interface in the samples diffusion-welded at 1100 °C and a flat interface in the samples joined at 1000 °C and 1050 °C. The interface consisted of fine Al 2 O 3 oxides, while precipitation of interfacial M 23 C 6 carbides was not observed. Grain boundaries migrated across the Al 2 O 3 oxides, leaving these oxides within the grains. Graded grain size was observed, with grain coarsening being more significant near the sample surface due to the temperature gradient induced by EFAS. Tensile testing revealed that the specimens fractured in the matrix away from the interface, indicting strong diffusion-welded joints. Further, the peak tensile strength of 807 MPa was obtained in the samples welded at 1000 °C due to minimal grain growth. The materials obtained at 1100 °C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed alternating high and low strain segments in the samples produced at 1000 °C and 1050 °C, indicating that the flat interfaces with no GB migration were less ductile compared to the matrix. A greater strain uniformity was observed along the bond interfaces with improved GB migration. The hardness reduced near the sample surfaces due to enlarged grains induced by temperature gradient. This study demonstrates that GB migration and enhanced mechanical strength can be achieved in diffusion-welded Alloy 617.

36 MATERIALS SCIENCE↗

Effects of Solidification Cooling Rates on Microstructures and Physical Properties of Fe-6.5%Si Alloys

Compared to the widely used Fe-3.2wt%Si steel, Fe-6.5wt%Si has superior electric and magnetic properties, including higher electrical resistivity, lower iron loss, higher permeability, and near zero magnetostriction. However, Fe-6.5wt%Si sheet is difficult to produce using traditional manufacturing processes as the high silicon content favors the formation of ordered phases that embrittle the material. Fortunately, these ordered phases can be suppressed if the alloy is cooled fast enough from a high temperature kinetically trapping the disordered solid solution or amorphous state. Planar flow casting is known for its rapid solidification rate. In order to consider it as a viable method to manufacture ductile Fe-6.5wt%Si sheets, the effect of cooling rate on physical properties of Fe-6.5wt%Si alloy are systematically investigated. In this work, various cooling rates are achieved by changing melt-spin wheel speeds, which significantly affect the solidification temperature profile and have profound effects on ordering, microstructures, textures, hardness, and magnetic properties. High cooling rates result in refined grains, reduced ordering, enhanced <100> out of the plane texture, decreased hardness, and increased coercivity. This study demonstrates a critical cooling rate at ~1.7 × 10 5 K/s, corresponding to a tangential wheel speed of 5-7 m/s, below which the hardness significantly increases in agreement with the sudden increase of the ordered phases that causes the material embrittlement.

36 MATERIALS SCIENCE↗

Microstructure and creep properties of cast near-eutectic Al–Ce–Ni alloys

This study investigates the as-cast and aged microstructures, thermal stability, ambient temperature strengthening, and creep resistance of three ternary Al–Ce–Ni alloys (wt%): near-eutectic Al–10Ce–5Ni (with both eutectic and hypoeutectic regions), hypoeutectic Al-7.5Ce-3.75Ni (with numerous primary Al dendrites), and hypereutectic Al-12.5Ce-6.25Ni (with coarse, blocky primary Al3Ni and Al11Ce3 precipitates and some primary Al dendrites). Depending on the alloy composition and local solidification conditions, the following eutectic morphologies are found: (i) coarse Al–Ce eutectic colonies where Al 11 Ce 3 is in the form of “Chinese script”, (ii) intermingled regions of binary Al–Ce and Al–Ni eutectic colonies, with finer Al 3 Ni and Al 11 Ce 3 fibers, (iii) large ternary eutectic colonies, where the binary Al 3 Ni and Al 11 Ce 3 phases are alternating or intertwining within the individual, fine fibers (diameters of ~60–170 nm, depending on solidification rates), and (iv) ternary eutectic zones (between primary Al dendrites), where fine Al 3 Ni and Al 11 Ce 3 build up a 3D-interconnected network. The high volume fraction of intermetallic phases and extremely fine eutectic spacing/fiber diameter both contribute to high ambient strengthening (higher as-cast microhardness than binary Al–Ce or Al–Ni), and also provide enhanced creep resistance at 300 and 350 °C. Additionally, the alloys are coarsening-resistant up to 425 °C for extended periods, with a gradual decrease in microhardness. The alloys aged at 400 °C to 1050 h show fiber fragmentation and coarsening of the resulting particles, with the faster-diffusing Ni driving more rapid coarsening of the Al 3 Ni particles which engulf finer, more stable Al 11 Ce 3 particles. Severe overaging (performed at 590 °C for 24 h) leads to Al 3 Ni and Al 11 Ce 3 spheroids which remain submicron-sized in eutectic colonies, but micron-sized at colony boundary and at Al dendrite-eutectic interface. Creep resistance at 300 °C of overaged Al–10Ce–5Ni remains substantial, consistent with load-transfer based composite strengthening being an important strengthening mechanism in these alloys, making them excellent candidates for replacement of heavier steel or titanium parts operating under stress up to 300 °C.

36 MATERIALS SCIENCE↗

Atomistic simulations of nanoindentation on nanoglasses: Effects of grain size and gradient microstructure on the mechanical properties

The use of nanoglass (NG) microstructures has been shown as an effective strategy to improve the ductility of rather brittle metallic glass alloys. To evaluate the effects of grain size and gradient design on the mechanical properties of NGs, we perform molecular dynamics simulations of nanoindentation on Cu 64 Zr 36 NGs. We consider samples with uniform 3 and 7 nm grain sizes as well as gradient microstructures with gradient grain sizes varying from 3 to 7 nm. Here, the results show that the deformation mechanism in NGs with small grain sizes is dominated by the activation and evolution of multiple shear transformation zones. Increasing grain sizes enhances the elastic modulus and hardness at the cost of reduced abrasion resistance. Though the average grain size at the indentation surface plays a crucial role in the deformation behavior of gradient NG models, their strain localization and plastic deformation states are affected by the grain sizes far from the indenter. Desired combinations of mechanical properties can be realized by different NG microstructure designs.

36 MATERIALS SCIENCE↗

Effect of post-weld heat treatment on microstructure and mechanical properties of rotary inertia friction welded dissimilar 422-4140 martensitic steel piston joints

The study investigated how post‐weld heat treatment (PWHT) temperature affects the microstructure and localized deformation/fracture during bend testing of rotary inertia friction welds (RIFW) between AISI 422 stainless steel and AISI 4140 steel. RIFW produced a fully martensitic interface with approximately 550 HV hardness in both the thermo-mechanically affected (TMAZ) and heat‐affected zones (HAZ). Due to differences in temper resistance, the 4140 TMAZ/HAZ softened progressively under PWHT temperatures from 525 °C to 700 °C, while the 422 TMAZ unexpectedly maintained about 550 HV up to 600 °C before significantly softening at temperatures ≥625 °C. This asymmetric softening generated steep hardness gradients across the interface at temperatures ≤600 °C. Furthermore, carbon migration across the interface was minimal up to 600 °C, moderate at 625 °C, and by 700 °C produced a carbide‐rich eutectoid layer in the 422 TMAZ alongside a carbon‐depleted soft ferrite layer in the 4140 TMAZ. Strain during bending was PWHT‐dependent, concentrating on the 4140 side; in as-welded joints, the high hardness led to deformation and crack initiation in the base metals, whereas in PWHT samples, cracking initiated in the softened 4140 TMAZ near the interface. The intermediate PWHT temperature of 625 °C offered the best balance of limited carbon diffusion across the interface, relatively low peak weld hardness and minimized hardness gradients across the interface, more homogenous deformation, and good bend test performance.

4140 low-alloy steel↗

Microstructure and mechanical properties of friction stir weld performed on neutron-irradiated 304L steel with helium

As nuclear power plants (NPPs) approach or exceed 40–60 years of service, it may become necessary to repair damaged neutron-irradiated components to prolong longevity. However, fusion welding repair of irradiated steels and metallic materials is challenging because of helium-induced cracking. This study used friction stir welding (FSW) to address helium-related issues, such as helium bubble formation and grain boundary cracking. The microstructure, helium-induced degradation, and mechanical properties of a friction stir weld produced on neutron-irradiated 304L stainless steel with approximately 5.2 appm of helium were characterized. The analysis focused on variations in grain size, texture, and the morphology of helium-induced damage in the friction stir weld. Mechanical properties were characterized on the irradiated base metal (BM) and metallurgical zones of the friction stir weld: the stir zone (SZ), the thermo-mechanically affected zone (TMAZ), and the heat affected zone (HAZ). Only minor scattered porosity in the SZ and TMAZ and a few short microcracks (below 20 μm in length) in the TMAZ were observed, indicating limited helium-induced degradation. Tensile tests revealed good mechanical properties and fractography analysis demonstrated predominantly ductile fracture. In conclusion, the results highlight the immediate and substantial benefits of the FSW approach for repairing or joining helium-containing irradiated materials in NPPs.

36 MATERIALS SCIENCE↗

Microstructure and mechanical properties of hypoeutectic Al–6Ce–3Ni-0.7Fe (wt.%) alloy

Here, a hypoeutectic, Fe-modified Al–Ce–Ni alloy (Al–6Ce–3Ni-0.7Fe, wt.%) is studied in terms of microstructure, thermal stability, ambient temperature strengthening, and creep resistance. The as-cast microstructure consists of primary Al dendrites and interdendritic binary eutectic regions (Al–Al11Ce3 and/or Al–Al9(Fe,Ni)2), with micron/submicron lamellar spacing, depending on the location along the height of the ingot. The cast alloy exhibits excellent coarsening resistance at 400 °C, with mostly unchanged microstructure and microhardness after 6 weeks of aging, indicating good thermal stability of Al11Ce3 and Al9(Fe,Ni)2. Orowan strengthening and load transfer are identified as strengthening mechanisms at ambient and elevated temperature. A high volume fraction of the intermetallic phases (providing load transfer) and relatively coarse eutectic spacing (for modest Orowan strengthening) result in a moderate as-cast microhardness of 566 ± 32 MPa. Creep resistance at 300 and 350 °C is similar to a binary Al-12.5Ce eutectic alloy (with twice the Ce content) because of two countering effects: Al–6Ce–3Ni-0.7Fe shows a higher volume fraction of strengthening intermetallic phases, but it also exhibits a large fraction of primary Al dendrites which weaken the alloy. By contrast, the alloy, when laser-remelted at the surface, has a fully eutectic microstructure without primary aluminum dendrites achieved by high undercooling on solidification, with a refined network of eutectic phases that doubles the microhardness as compared to the cast alloy. Whereas coarsening is faster due to the shorter diffusion distances between the eutectic phases, hardness remains ~30% higher than the as-cast alloy after ~6 weeks aging at 400 °C.

36 MATERIALS SCIENCE↗

Impact of Irradiation on Microstructure and Mechanical Properties of Materials Produced by Advanced Manufacturing

Advanced non-light water reactor designs, known as Generation IV (Gen IV) reactors, typically operate at higher temperatures and under more extreme radiation conditions than conventional light water reactors. A critical aspect of the successful deployment and advancement of Gen IV reactor designs is the selection of appropriate structural materials for specific applications, which necessitates the timely development of new materials and manufacturing processes. Advanced manufacturing (AM) offers numerous opportunities for innovative designs, enabling the production of high-performance components with potentially shorter development cycles compared to traditional manufacturing methods. However, a significant challenge in deploying AM technologies in the nuclear energy sector is the current lack of data on the irradiation performance of AM-produced components. This presentation will discuss neutron and ion irradiation results of AM materials, including stainless steel 316L, Grade 91, SA508, Inconel 718, and Inconel 625 materials. The materials were manufactured by AM, such as Powder Metallurgy Hot Isostatic Pressing (PM HIP), Laser Powder Bed Fusion (LPBF) and Directed Energy Deposition (DED). The effects of neutron irradiation on microstructure (e.g., dislocations, loops, and nanoclusters), tensile properties (e.g., strength and ductility), and ion irradiation on Irradiation-Assisted Stress Corrosion Cracking (IASCC) will be explored. Results are collected from several projects supported by the Nuclear Science User Facilities (NSUF) program.

36 - MATERIALS SCIENCE↗