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At least 505 records · Page 28

Effects of Proton Irradiation on GaN Vacuum Electron Nanodiodes

Gallium nitride (GaN)-based nanoscale vacuum electron devices, which offer advantages of both traditional vacuum tube operation and modern solid-state technology, are attractive for radiation-hard applications due to the inherent radiation hardness of vacuum electron devices and the high radiation tolerance of GaN. Here, we investigate the radiation hardness of top-down fabricated n-GaN nanoscale vacuum electron diodes (NVEDs) irradiated with 2.5-MeV protons (p) at various doses. We observe a slight decrease in forward current and a slight increase in reverse leakage current as a function of cumulative protons fluence due to a dopant compensation effect. The NVEDs overall show excellent radiation hardness with no major change in electrical characteristics up to a cumulative fluence of 5E14 p/cm 2 , which is significantly higher than the existing state-of-the-art radiation-hardened devices to our knowledge. In conclusion, the results show promise for a new class of GaN-based nanoscale vacuum electron devices for use in harsh radiation environments and space applications.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Imaging of the electronic bonding of diamond at pressures up to 2 million atmospheres

Diamond shows unprecedented hardness. Because hardness is a measure of resistance of chemical bonds in a material to external indentation, the electronic bonding nature of diamond beyond several million atmospheres is key to understanding the origin of hardness. However, probing the electronic structures of diamond at such extreme pressure has not been experimentally possible. The measurements on the inelastic x-ray scattering spectra for diamond up to 2 million atmospheres provide data on the evolution of its electronic structures under compression. The mapping of the observed electronic density of states allows us to obtain a two-dimensional image of the bonding transitions of diamond undergoing deformation. The spectral change near edge onset is minor beyond a million atmospheres, while its electronic structure displays marked pressure-induced electron delocalization. Such electronic responses indicate that diamond’s external rigidity is supported by its ability to reconcile internal stress, providing insights into the origins of hardness in materials.

36 MATERIALS SCIENCE↗

Annual LDRD Report (FY2019)

The performance of Nuclear Deterrence (ND) systems could be improved by adopting advanced commercial CMOS technologies. However, the radiation hardness of these ND systems must be assured. This project quantified dose rate upset thresholds, allowing us to evaluate whether advanced commercial technologies can be used in rad hard applications. This project also evaluated the susceptibility of advanced commercial technologies to neutron displacement damage and single event effects, and developed hardness assurance methods. As a result of this work, Sandia is now collaborating more closely with DoD agencies and their contractors to understand and improve the radiation hardness of advanced commercial technologies. Sandia Capabilities (SPHINX, lon Beam Lab, FPGA test capabilities) were developed and are being utilized by other programs. Staff were trained to do radiation survivability testing and developed proposals that were funded. Internal and external collaborations and partnerships were developed, including with Georgia Tech. This project received the Best Paper award at the 2019 Hardened Electronics And Radiation Technology (HEART) Conference.

36 MATERIALS SCIENCE↗

Radiation Hardened Electronics for Reactor Environments

Radiation-hardened (rad-hard) electronics have been the shortcoming in nuclear sensing and instrumentation. Placing advanced sensors and associated electronics closer to a nuclear reactor core will improve reactor control and operation through increased signal accuracy, precision, and fidelity, resulting in safer, more efficient energy production. However, the extreme temperature and bombarding radiation environment of nuclear applications make research and development into electronics and electronic materials technologies essential to enabling improved safety, monitoring, and control of the existing nuclear reactor fleet and the next generation of reactors, including microreactors. To help the US Department of Energy (DOE) define a course for the Office of Nuclear Energy (NE)-funded rad-hard electronics research, Oak Ridge National Laboratory staff present this summary of the state-of-the-art (SOA) technology for the design and implementation of rad-hard electronics and systems, including research efforts and commercial offerings. A collection of technological gaps associated with reactor applications are compiled herein. Based on the radiation degradation mechanisms discussed in this report, along with the state-of-the-art summary survey and a compiled list of gaps, a high-level research plan of future NE funding direction was developed and is provided. This report outlines these activities and provides a summary of SOA electronics technology for rad-hard instrumentation in reactors, a list of the major technology gaps observed, and a draft plan for addressing the present and future needs of reactor instrumentation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Qualification of Digitized Legacy Fast Reactor Data

The Integral Fast Reactor (IFR) fuel compatibility test program (1984-1994) included a variety of fuel pin examinations conducted at the Hot Fuel Examination Facility (HFEF) and the Alpha-Gamma Hot Cell Facility (AGHCF). Hard copy data records of these examinations have been recovered, scanned, and preserved in PDF format. Many hard copy records are now qualified in accordance with an NRC-approved Quality Assurance Program Plan (QAPP), and there is an ongoing effort to qualify additional legacy records. This legacy fuel performance data is vital to support design and licensing of fast reactors with validation of state-of-the-art codes and advanced methods for design and analysis. Stakeholders can most easily utilize this data when the PDF scans have been converted into digital data tables. However, qualification of the scanned hard copy data does not qualify the digital data file resulting from the digitization of the data contained in the record; the subject matter expert (SME) must make a review of the digitized data table as well before it can be designated as qualified. This report outlines a peer review process to qualify the digital data file(s), typically in CSV format, corresponding to hard copy records in accordance with the existing QAPP.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

RePED 250: A Revolutionary, High Drilling Rate, High-T Geothermal Drilling System and Companion Power Electronics

Geothermal drilling in the United States is drastically slower and more costly than Oil and Gas (O&G) drilling, primarily due to the additional challenges in geothermal wells: hard rock types and high temperatures. The Repetitive Pulsed Electric Drill (250°C) (RePED-250), developed by Tetra Corporation has the potential to change this with a novel electro-crushing technology. RePED-250 releases pulses of electricity through the rock, which causes it to break in tension, instead of compression like conventional rotary drilling. The tensile strength of hard rocks like granite is only ~5% of their compressive strength, requiring less energy, time, and wear on the bit compared to conventional drilling. The RePED drill bit has no moving parts, uses drilling mud to remove rock fragments, and uses standard drill pipe, enabling a direct transition from conventional drilling systems. The objective of this project is to move RePED technology towards commercial readiness for high-temperature geothermal applications. This involves: 1) Creating high-temperature, high power electronic components for the RePED drill capable of operating at the high temperatures of a geothermal well. The target is a 250°C ambient environment. Specifically, capacitors, high voltage switches, and a downhole generator capable of generating the necessary power. 2) Demonstrating RePED’s effectiveness drilling through hard rock (granite) and examining its pathway to commercialization and effect on the US geothermal market. Work on this project has led to significant improvement over the state-of-the-art for all the examined electronics, through design, modeling, and testing of these novel components, though some additional development is still needed to deploy these high-temperature parts in a geothermal well. Besides their use in RePED-250, each component has applications in other industries where the stability of electronics at high-temperature is needed. To address the second barrier to commercialization, a 9” hole was drilled through a sample block of granite, demonstrating the tool’s effectiveness in hard rock. The team investigated RePED-250’s effect on well cost and the geothermal industry, through various techno-economic models described in the report.

15 GEOTHERMAL ENERGY↗

RePED 250: A Revolutionary, High Drilling Rate, High-T Geothermal Drilling System and Companion Power Electronics (Final Report)

Geothermal drilling in the United States is drastically slower and more costly than Oil and Gas drilling, primarily due to the additional challenges in geothermal wells: hard rock types and high temperatures. The Repetitive Pulsed Electric Drill (250 degrees C) (RePED-250), developed by Tetra Corporation has the potential to change this with a novel electro-crushing technology. RePED-250 releases pulses of electricity through the rock, which causes it to break in tension, instead of compression like conventional rotary drilling. The tensile strength of hard rocks like granite is only ~5% of their compressive strength, requiring less energy, time, and wear on the bit than conventional drilling. The RePED drill bit has no moving parts, uses drilling mud to remove rock fragments, and standard drill pipe, enabling a direct transition from conventional drilling systems. The objective of this project is to move RePED technology towards commercial readiness for high-temperature geothermal applications. This involves: 1) Creating high-temperature, high power electronic components for the RePED drill capable of operating at the high temperatures of a geothermal well. The target is a 250 degrees C ambient environment. Specifically, capacitors, high voltage switches, and a downhole generator capable of generating the necessary power. 2) Demonstrating RePED's effectiveness drilling through hard rock (granite) and examining its pathway to commercialization and effect on the US geothermal market. Work on this project has led to significant improvement over the state-of-the-art for all the examined electronics, through design, modeling, and testing of these novel components, though some additional development is still needed to deploy these high-temperature parts in a geothermal well. Besides their use in RePED-250, each component has applications in other industries where the stability of electronics at high-temperature is needed. To address the second barrier to commercialization, a 9" hole was drilled through a sample block of granite, demonstrating the tool's effectiveness in hard rock. The team investigated RePED-250's effect on well cost, and the geothermal industry, through various models described in the report.

15 GEOTHERMAL ENERGY↗

Using Machine Learning for Quantum Annealing Accuracy Prediction

Quantum annealers, such as the device built by D-Wave Systems, Inc., offer a way to compute solutions of NP-hard problems that can be expressed in Ising or quadratic unconstrained binary optimization (QUBO) form. Although such solutions are typically of very high quality, problem instances are usually not solved to optimality due to imperfections of the current generations quantum annealers. In this contribution, we aim to understand some of the factors contributing to the hardness of a problem instance, and to use machine learning models to predict the accuracy of the D-Wave 2000Q annealer for solving specific problems. We focus on the maximum clique problem, a classic NP-hard problem with important applications in network analysis, bioinformatics, and computational chemistry. By training a machine learning classification model on basic problem characteristics such as the number of edges in the graph, or annealing parameters, such as the D-Wave’s chain strength, we are able to rank certain features in the order of their contribution to the solution hardness, and present a simple decision tree which allows to predict whether a problem will be solvable to optimality with the D-Wave 2000Q. We extend these results by training a machine learning regression model that predicts the clique size found by D-Wave.

97 MATHEMATICS AND COMPUTING↗

Kinetic Simulations of Radiative Magnetic Reconnection in the Coronae of Accreting Black Holes

We perform 2D and 3D particle-in-cell simulations of reconnection in magnetically dominated e ± plasmas subject to strong Compton cooling. Magnetic reconnection under such conditions can operate in accretion disk coronae around black holes, which produce hard X-rays through Comptonization. Our simulations show that most of the plasma in the reconnection layer is kept cold by Compton losses and locked in magnetically dominated plasmoids with a small thermal pressure. Compton drag clears cavities inside plasmoids and also affects their bulk motions. These effects, however, weakly change the reconnection rate and the plasmoid size distribution from those in nonradiative reconnection. This demonstrates that the reconnection dynamics is governed by similar magnetic stresses in both cases and weakly affected by thermal pressure. We examine the energy distribution of particles energized by radiative reconnection and observe two distinct components: (1) A mildly relativistic peak, which results from bulk motions of cooled plasmoids. This component receives most of the dissipated reconnection power and dominates the output X-ray emission. The peak has a quasi-Maxwellian shape with an effective temperature of ~100 keV. Thus, it mimics thermal Comptonization used previously to fit hard-state spectra of accreting black holes. (2) A high-energy tail, which receives ~20% of the dissipated reconnection power. It is populated by particles accelerated impulsively at X-points or "picked up" by fast outflows from X-points. The high-energy particles immediately cool, and their inverse Compton emission explains the MeV spectral tail detected in the hard state of Cyg X-1. Our first-principle simulations support magnetic reconnection as a mechanism powering hard X-ray emission from magnetically dominated regions of accreting black holes.

79 ASTRONOMY AND ASTROPHYSICS↗

Complexity-theoretic foundations of BosonSampling with a linear number of modes

BosonSampling is the leading candidate for demonstrating quantum computational advantage in photonic systems. While we have recently seen many impressive experimental demonstrations, there is still a formidable distance between the complexity-theoretic hardness arguments and current experiments. One of the largest gaps involves the ratio of {particles} to modes -- all current hardness evidence assumes a dilute regime in which the number of linear optical modes scales at least quadratically in the number of particles. By contrast, current experiments operate in a saturated regime with a linear number of modes. In this paper we bridge this gap, bringing the hardness evidence for experiments in the saturated regime to the same level as had been previously established for the dilute regime. This involves proving a new worst-to-average-case reduction for computing the Permanent which is robust to both large numbers of row repetitions and also to distributions over matrices with correlated entries. We also apply similar arguments to give evidence for hardness of Gaussian BosonSampling in the saturated regime.

Computational Complexity (cs.CC)↗

FEMTOSECOND LASER DRILLING OF SILICON NITRIDE

Ceramics are employed in various engineering applications including electronics, semiconductors, automotive and aerospace industry, among others. Ceramics are desirable materials due to their high hardness, thermal resistance, chemical, thermal, and mechanical properties. A drawback of engineering ceramics is the manufacturing process. Ceramics are hard and brittle and conventional drilling or cutting methods can damage the material. These challenges in manufacturing have limited the application of ceramics in certain engineering applications. The non-contact machining of ceramics through ultrashort pulsed laser drilling offers a possible solution to the manufacturing issues. The advantage of laser drilling is the ability to machine hard and brittle materials. A laser, pulsed in the time regime of femtoseconds (fs), drills/machines sharp and well-defined holes and cuts. Additionally, the short pulse width results in limited melting, cracking, or heat transfer to the surrounding material, as well as no residual stresses. This non-contact process can greatly aid in the machining of hard materials. This study focuses on drilling into silicon nitride to produce zero-taper through holes. With this, other thicknesses can be explored, to achieve zero-taper holes.

Femtosecond laser ablation, Ceramics, Silicon Nitr↗

Determining the Effects of Neutron Irradiation on the Structural Integrity of Additively Manufactured Heat Exchangers for Very Small Modular Reactor Applications, DOE Final Report (Project # 19-16980)

Auburn University (AU) teamed with the University of Missouri Research Reactor (MURR) and Kansas State University (KSU) to determine how to best use laser-powder bed fusion (L-PBF) additive manufacturing (AM) methods for generating radiation resistant nickel-based superalloys, Inconel alloy 625 and 718, for special purpose reactor (SPR) or very small modular reactor (vSMR) heat-exchangers (HeXs). Compact, conformal, and durable HeXs that are tolerant of extreme environments are needed for supporting the technical maturity of next-generation, portable compact reactors. AM is an enabler for realizing this new wave of HeXs – providing a means to make customizable hot and cold stream architectures with novel flow path geometries (e.g., tortuous channels with non-uniform, asymmetric cross-sections) and reduced layer-to-layer contact resistance (i.e., no separate bonding procedure required). AM further enables a more time/cost efficient means for fabricating SPRs by reducing the number of suppliers required for HeX assembly and allowing for on-site HeX fabrication. The project aim has been to better understand how neutron irradiation affects the microstructure and properties of additively manufactured nickel-based superalloys, to accelerate their safe, reliable use in the modular reactor industry. The major objective was to qualify/quantify the microstructure and microhardness of nickel-based superalloys (including Inconel 718 and 625) additively manufactured via the L-PBF process in the neutron-dosed (irradiated) and non-irradiated states over a course of 3 years. Effects of build orientation during L-PBF and post-AM heat treatments on neutron resistance, microstructure and mechanical properties were also investigated. Neutron damage mechanisms via hardening were characterized. This project combined subject-matter experts in AM, mechanical/microstructure metallic part characterization, and neutron irradiation, as well as unique assets and capabilities at AU and MURR at MU, to ensure project results translated to effectively addressing known gaps in nuclear science and engineering. Parts were fabricated using L-PBF systems readily available at AU. Specimens were then irradiated using MURR facilities; a manipulator equipped hot cell was also used to measure material hardness after dosing. MURR, a 10 MW, light-water nuclear reactor, is the largest, highest powered, highest-flux university owned research reactor in the U.S. The major findings in this project provide evidence that AM can serve as an alternative way to build structural components for future advanced small modular reactors using advanced materials like Inconel 625 (IN625) or Inconel 718 (IN718). After full spectrum neutron irradiation, vertically as-built AM IN625 samples were observed to display better resistance towards radiation-induced-hardening defects relative to traditionally machined metals. A Vickers microhardness tester, using settings of 1 kgf and dwell time of 15 seconds per indentation, was used to measure hardness in this study. The as-built, vertically printed samples experienced 1.2% of radiation hardening vs. 5.25% radiation hardening observed in wrought IN625. Another set of IN625 and IN718 samples were exposed to fast neutron irradiation. It was observed that IN718 showed more resistance towards radiation hardening compared to IN625 samples indicating IN718 had a better performance. Results showed that the IN718 samples experienced less change (-2.5 to 3.24 %) in microhardness. On the other hand, IN625 samples underwent more (0.9 to 7.21%) change in microhardness after fast neutron irradiation. AM IN625 samples were irradiated using an ion (proton) beam in cyclotron. The mechanical properties of AM samples post irradiation were compared with wrought samples. The irradiated region on the samples were tested using nano-hardness indention. It was observed that the beam current and time used in this study generated an annealing effect and thus reduced the hardness of the samples. The sum of the project results provide precious insight into how one may minimize radiation hardening in AM materials while maintaining material property constraints. Results should assist engineers in selecting an appropriate heat treatment for AM nickel-based superalloys for increased radiation resistance. Results should increase confidence levels for adopting AM for building nuclear reactor components which perform the same or better than conventionally manufactured components. Fast neutron irradiation testing provided an accelerated means of obtaining radiation effects without making materials radioactive and difficult to handle.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗

Correlation between microstructure and residual stress formation in friction stir welded armor steels characterized by neutron diffraction

Friction stir welding (FSW) is a solid-state joining process that minimizes the heat-affected zone (HAZ) compared with fusion-based arc welding, making it well suited for joining martensitic armor steels where hardness and ballistic resistance are critical. This study investigates residual stress formation in three defect-free FSW butt-joint configurations relevant to armored-vehicle fabrication: similar rolled homogeneous armor (RHA–RHA, Case 1), similar high-hardness armor (HHA–HHA, Case 2), and dissimilar HHA–RHA (Case 3) joints produced under temperature-controlled conditions (770 °C). Neutron diffraction was employed to quantify the magnitude and spatial distribution of residual stresses in the longitudinal, transverse, and normal directions and to correlate them with weld microstructure and hardness. Tensile residual stresses were concentrated in the softened HAZ, reaching approximately 300 MPa for Case 2 and 400 MPa for Case 1 (≈50–70 % of the base-metal yield strength; ∼581 MPa for RHA and ∼566 MPa for HHA), while compressive residual stresses dominated the stir zone. The spatial extent of tensile stresses scaled with the width of the softened HAZ, which was largest in the dissimilar HHA–RHA joint and smallest in the HHA–HHA joint. Full-width-at-half-maximum (FWHM) analysis revealed low microstrain in overtempered HAZ regions and high microstrain in the stir zone associated with severe plastic deformation and fresh martensite formation. This work demonstrates that residual stress evolution in FSW of martensitic armor steels is governed not primarily by peak temperature or thermal contraction, as inferred from fusion-welding analogies, but by the competition between transformation-induced volumetric expansion and tempering-induced stress relaxation. The relative dominance of these mechanisms is shown to depend on alloy hardenability and local thermal history, leading to more extensive HAZ softening and broader tensile stress regions in the lower-hardenability RHA steel. These findings establish a transferable mechanistic framework for optimizing solid-state joining strategies in high-strength steels and other transformation-hardening alloys beyond armor applications.

Friction stir welding↗

Electrolyte-driven interphase stabilization in high-voltage sodium-ion full cells

Sodium-ion batteries with a high-voltage O3-type layered oxide cathode paired with a hard carbon anode can offer high energy density; however, significant interfacial instabilities driven by electrode/electrolyte reactions limit a broader industrial adoption. Localized high concentration electrolytes (LHCEs) are a rational choice as they promote salt decomposition over solvent, forming stable, inorganic-rich electrode-electrolyte interphases (EEIs). We present here a comparison of high-voltage (4.2 V) hard carbon | NaNi 1/3 Fe 1/3 Mn 1/3 O 2 pouch cells in LHCEs and in a standard carbonate-based electrolyte by (i) examining the influence of diluent choice on the electrochemical performance of LHCEs and (ii) investigating how the electrolyte chemistry affects the composition and structure of EEIs formed. Importantly, LHCEs demonstrate superior electrochemical performance, achieving 37% higher capacity after 200 cycles (119 vs. 87 mA h g -1 ) compared to the carbonate-based electrolyte. The enhanced stabilization provided by LHCEs at the interface with high-voltage sodium layered oxide cathode is revealed by gas evolution measurements obtained through online electrochemical mass spectrometry (OEMS). Time-of-flight secondary ion mass spectrometry paired with focused ion beam and advanced statistical analyses reveal that the superior performance of LHCE stems from a robust, thin cathode electrolyte interphase formed on the sodium layered oxide cathode and a homogeneous solid electrolyte interphase formation on the hard carbon anode. Furthermore, this study highlights the critical importance of electrolyte design in interphase stabilization, which plays a key role in advancing sodium-ion batteries toward commercial viability.

25 ENERGY STORAGE↗

Indentation investigation of 304L stainless steel friction stir weld simulated crack repair

Simulated cracks were repaired in 304L stainless steel using low temperature friction stir welding. Indentation studies were carried out to understand the effect of microstructural features on the mechanical property variation across the weld and to measure the size of the weld zones with a quantitative technique. Microhardness and nanoindentation hardness profiles were constructed on a transverse section across the weld. The data obtained were correlated by extrapolating the nanoindentation hardness to greater depths which showed that the nanoindentation hardness closely reflects the microhardness values throughout the weld. Finally, grain size in the stir zone (SZ) was found to vary with the tool temperature which, in turn, alters the nanoindentation modulus variability and higher tool temperature resulted in widening of the SZ.

36 MATERIALS SCIENCE↗

The formation and evolution of Ni 2 Cr precipitates in Ni–Cr model alloys as a function of stoichiometry characterized by synchrotron x-ray diffraction

Ni-based alloys containing significant amounts of Cr, may precipitate new phases during long-term service at elevated temperatures. In Ni–Cr model alloys, the formation of Ni 2 Cr has been found to impact the material properties, including the strength and ductility after isothermal aging below the critical temperature of 590°C. In this work, we quantify the formation and evolution of long-range ordering in four Ni–Cr binary model alloys (Ni/Cr = 1.8, 2.0, 2.2, 2.4) after isothermal aging up to 10,000h at temperatures between 373 and 475°C. The alloys were characterized by hardness testing and synchrotron-based x-ray diffraction to quantify the impact of Ni 2 Cr phase fraction and precipitate size on mechanical properties. After 500h of isothermal aging, the formation of Ni 2 Cr was detected in all four alloys at 475°C. In the stochiometric alloy samples (Ni/Cr = 2.0), the formation of Ni 2 Cr was found after 500 and 3000h aging at 418 and 373°C, respectively. We found that the matrix lattice contraction and Ni 2 Cr phase fraction both saturate after early aging times. This is in stark contrast to the hardness and Ni 2 Cr precipitate size that both continue to increase with increasing aging time. Our results highlight that changes in hardness correlate linearly with Ni 2 Cr precipitate size rather than phase fraction. This important structure-property relationship can potentially help define Ni–Cr-based component lifetimes directly through an understanding of how Ni 2 Cr formation impacts strength and ductility. Here, we find that a precipitation hardening model for critical resolved shear stress with weakly coupled dislocations shows good agreement with the material property changes quantified from experimental measurements.

36 MATERIALS SCIENCE↗

Tribological behavior of spark plasma sintered Ti 3 SiC 2 MAX phase composites

Ti₃SiC₂ MAX phases are considered promising candidates for tribological applications; but, their low hardness (5-6 GPa) can lead to increased abrasive wear and higher wear rates. This study investigates the effect of incorporating hard SiC particles on microstructure, mechanical, and tribological behavior of Ti₃SiC₂-SiC-based MAX phase composites prepared using spark plasma sintering at 1400 °C, 40 MPa, 15-minute holding time. Phase and microstructural characterization of composites confirmed the formation of Ti₃SiC₂ MAX phase (90%) along with TiC as a minor phase (10%). For Ti₃SiC₂-SiC, homogeneous distribution of SiC grains within Ti₃SiC₂ matrix resulted in increased hardness from ~11.6 GPa to ~14.8 GPa; however, the flexural strength decreased from ~615 MPa to ~597 MPa due to coefficient of thermal expansion mismatch. Tribological behavior of Ti₃SiC₂-SiC MAX phase composites was assessed using unidirectional sliding ball-on-flat tests with a 52100 steel ball at different loads and a constant speed of 0.05 m/s. SiC reinforced composites exhibited a decreased friction coefficient from 0.39 to 0.29 and wear rates comparable to Ti₃SiC₂ (7-10×10⁻³ mm³/N·m). SEM and EDS analysis of the worn surfaces indicated material transfer from the steel ball counter body and its oxidation due to frictional heating, at lower loads (2N and 5N), whereas at higher load (10N), fracture of the transfer layer dominated, with the presence of microcracks, delamination, grain pull-outs, and wear debris. Improved mechanical properties and good adhesion of SiC with Ti₃SiC₂ matrix resulted in reduced microcracks and grain pull-outs, making Ti₃SiC₂-SiC/Steel tribo-pair more suitable for tribological applications.

36 MATERIALS SCIENCE↗