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At least 55 records · Page 3

A near-field study of VO2/(100)TiO2 film and its crack-induced strain relief

Temperature-induced metal–insulator transition (MIT) in vanadium dioxide (VO2) has been under intense research interest for decades both theoretically and experimentally. Due to the complex nature of electron correlations, the underlying physics behind the MIT in VO2 has yet to be fully grasped. In this work, we utilize the fine resolution of the scattering-type scanning near-field optical microscope to investigate the MIT in an epitaxial VO2 thin film on the (100)R TiO2 substrate with mid-infrared light. Bidirectional tweed-like metal–insulator phase coexistence patterns are observed and understood under the Landau free energy paradigm. More interestingly, delayed metallic nucleation is observed near the surface cracks due to local strain relief. This research proposes ideas in investigating the temperature–pressure phase diagram and tuning the interplay between local strain and MIT in oxide thin films.

Chen, Xinzhong (ORCID:0000000261033848)↗

Comparative analysis of temperature dependent properties of commercial nuclear fuel pellet and surrogates undergoing cracking: A review

A variety of normal and accident scenarios can generate thermal stresses enough to cause cracking in light water reactor (LWR) fuel. To better understand this behavior, cracking experiments have been carried out to induce thermal gradients in fuel pellets via induction heating and direct resistance heating. In this study, Ceria (CeO 2 ) and yttria stabilized zirconia (YSZ) pellets were chosen as a surrogate fuel material for uranium dioxide (UO 2 ). Induction heating was done using copper coils and molybdenum susceptors which heated the surrogates to a threshold temperature that is sufficiently high for the fuel material to conduct current. Thereafter, direct resistance heating was achieved by passing current through the specimen using a DC power supply to introduce volumetric heating to replicate reactor operating conditions. Simultaneous real-time dual imaging of the ceria pellet surface has been designed using optical and infra-red camera system to capture images of cracks and full-field temperature gradients on pellet. It was observed that YSZ pellets need a much higher voltage-current for volumetric heating and do not exhibit the cracking pattern as ceria and UO 2 , hence YSZ was ruled out for further consideration. Ceria was found to be an appropriate surrogate for UO 2 . Furthermore, the experimental set up and test conditions demand the need to primarily understand the thermo-physical, mechanical and optical properties of UO 2 and the surrogates. Thus, it is essential to have an in-depth knowledge about the various temperature dependent properties of UO 2 and CeO 2 for establishing a comparative analysis between the surrogate and UO 2 for conducting experiments.

36 MATERIALS SCIENCE↗

Chloride-Induced Stress Corrosion Cracking of Friction Stir-Welded 304L Stainless Steel: Effect of Microstructure and Temperature

Dry storage canisters of used nuclear fuels are fabricated using SUS 304L stainless steel. Chloride-induced stress corrosion cracking (CISCC) is one of the major failure modes of dry storage canisters. The cracked canisters can be repaired by friction stir welding (FSW), a low-heat input ‘solid-phase’ welding process. It is important to evaluate the ClSCC resistance of the friction stir welded material. Stress corrosion cracking (SCC) studies were carried out on mill-annealed base materials and friction stir welded 304L stainless U-bend specimens in 3.5% NaCl + 5 N H2SO4 solution at room temperature and boiling MgCl2 solution at 155 °C. The engineering stress on the outer fiber of the FSW U-bend specimen was ~60% higher than that of the base metal (BM). In spite of the higher stress level of the FSW, both materials (FSW and BM) showed almost similar SCC failure times in the two different test solutions. The SCC occurred in the thermo-mechanically affected zone (TMAZ) of the FSW specimens in the 3.5% NaCl + 5 N H2SO4 solution at room temperature, while the stirred zone (SZ) was relatively crack-free. The failure occurred at the stirred zone when tested in the boiling MgCl2 solution. Hydrogen reduction was the cathodic reaction in the boiling MgCl2 solution, which promoted hydrogen-assisted cracking of the heavily deformed stirred zone. The emergence of the slip step followed by passive film rupture and dissolution of the slip step could be the SCC events in the 3.5% NaCl + 5 N H2SO4 solution at room temperature. However, the slip step height was not sufficient to cause passivity breakdown in the fine-grained SZ. Therefore, the SCC occurred in the partially recrystallized softer TMAZ. Overall, the friction-stirred 304L showed higher tolerance to ClSCC than the 304L base metal.

304L austenitic stainless steel↗

Design Methods, Tools, and Data for Ceramic Solar Receivers

This report presents the development of tools and methods for evaluating the reliability and performance of ceramic materials in high temperature solar receivers. As Concentrating Solar Power (CSP) technologies aim for higher operating temperatures to enhance efficiency and meet industrial process heat requirements, current high temperature metallic materials face challenges in maintaining structural integrity. This report explores advanced ceramics as a promising alternative, given their superior high temperature strength and lower thermal expansion, compared to metals. To address the need for effective ceramic receiver design tools, this report integrates statistical failure models of ceramics into the existing srlife tool: an open-source software package designed to estimate the life of high temperature CSP components. These failure models account for the inherent variability and flaw distribution in ceramics, as well as the impact of subcritical crack growth under high temperature cyclic loads. The report also presents experimental data collected for a commercially available ceramic material, SiC, and details the process of estimating reliability model parameters from these data. A comparative design analysis is then performed between ceramic (SiC) and metallic (current nickel-based superalloys A740H and A282) receiver. This comparison demonstrates that SiC receivers can achieve service life exceeding 30 years under high incident heat flux conditions, compared to just a few years for metallic receivers.

14 SOLAR ENERGY↗

Microstructure and fracture toughness characterization of three 9Cr ODS EUROFER steels with different thermo-mechanical treatments

Ferritic martensitic ODS steels are one of the candidate structural materials for future Gen-IV nuclear fission and fusion reactors. Here, the dependence of fracture toughness on microstructure was investigated by comparing three 9Cr ODS EUROFER steels manufactured through different thermo-mechanical processing routes. Quasi-static fracture toughness testing was performed with sub-sized C(T) specimens and microstructural characterization was carried out using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy. It was found that at lower test temperatures (-100 – 22 °C), the fracture toughness was primarily controlled by crack initiation at sub-micron particles and by production of secondary cracks during fracture. At higher temperatures (above 100 °C), fracture toughness was predominantly controlled by the matrix ductility and the grain boundary strength with a relatively ductile coarse-grained alloy demonstrating higher fracture toughness compared to high-strength fine-grained alloys. These results and discussion show that variations in thermomechanical treatments can produce significant differences in microstructure and fracture toughness behavior of ferritic martensitic ODS steels.

36 MATERIALS SCIENCE↗

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗

Robustness and printed sensor qualification

A limiting factor of additive manufactured (AM) sensors for in-pile applications is the development of appropriate interconnection and packaging strategies that can maintain reliable performance in extreme environments. Failure mechanisms in these harsh conditions could include, but not limited to, materials interaction (i.e., intermetallic formation) and coefficient of thermal expansion (CTE) mismatch between the individual components of the sensors. To mitigate premature failure and enable the successful sustained operation of AM sensors, non-destructive qualification tests are used as an intermediate process control step used for verifying robustness and reliability of the sensor before they are deployed. A materials system of interest is the use of barium strontium titanium oxide (BST) films on stainless steel 316L (SS316L) substrate. Due to BST’s high dielectric constant and tunable dielectric properties, there is an interest for its application as an insulation/encapsulation layer for capacitive strain gauges when printed on structural materials. Previous work on the BST/SS316L material system, however, showed that the BST cracks when exposed to temperatures up to 600 °C due to CTE mismatch between the printed BST film and the metallic substrate. When comparing different fabrication techniques, less surface cracking was observed in the samples that deposited thinner (i.e., 2-20 μm) than samples that were thicker (i.e., 135 µm – 300 µm). The objective of this report is to establish a qualification process that will determine and address any challenges (i.e., mechanical failure of thick prints) of the AM sensor prior to its application in experimental tests. To demonstrate the qualification process in this report, laser spallation and uniaxial tensile tests using dynamic and quasi-static loading, respectively, will be discussed.

36 - MATERIALS SCIENCE↗

Fracture toughness and crack propagation in LX-17 and PBX 9502 insensitive high explosives

High explosive materials, and in particular insensitive high explosive (IHE) materials, are of significant interest. TATB-based LX-17 and PBX 9502 are two IHE’s and mechanical properties are an important metric of performance. In this work we present, for the first time, a study of fracture as a function of temperature and displacement rate and starter crack length on billet pressed IHE materials using a standard three point bend technique. We demonstrated that the technique can yield consistent results over time by measuring samples from the same lots 4 years later and observed that the fracture toughness of LX-17 and PBX 9502 are similar. We also determined the temperature dependence for different starter crack lengths and found that the fracture toughness generally decreases with larger starter crack sizes and temperatures. For the LX-17, where a wide temperature range of -60 C to 50 C was investigated, the impact of temperature on fracture toughness between -20 C and 23 C was less than expected. For the PBX 9502 we observed the difference in fracture toughness values between -20 C and 23 C did depend on the particular lot, and also there was a tendency of the fracture toughness to scale with the tensile strength. We also investigated the effect of a lower displacement rate and observed that while the impact on the fracture toughness was relatively small, the samples surprisingly did not break (fail) after exceeding the peak load. We took advantage of this to perform x-ray computed tomography (CT) of the samples to image crack propagation in the intact samples. We observed that cracks were generally straight and unaffected by the microstructure in the LX-17, in contrast to the PBX 9502 where the direction of the cracks would frequently change and were likely influenced by the underlying microstructure.

36 MATERIALS SCIENCE↗

Identifying the microstructural features associated with void nucleation during elevated–temperature deformation of copper

The microstructural-scale mechanisms that produce cracks in metals during deformation at elevated temperatures are relevant to applications that involve thermal exposure. Prior studies of cavitation during high-temperature deformation, for example, creep, suffered from an inability to directly observe the microstructural evolution that occurs during deformation and leads to void nucleation. Here the current study takes advantage of modern high-speed electron backscatter diffraction (EBSD) detectors to observe cavitation in oxygen-free, high-conductivity copper in situ during deformation at 300°C. Most voids formed at the triple junction between a twin boundary and a high-angle grain boundary (HAGB). This finding does not contradict previous studies that suggested that twins are resistant to cracking—it reveals that cracks in HAGBs originate at twin/HAGB triple junctions and that cracks preferentially grow along HAGBs rather than the accompanying twins. Atomistic simulations explored the origins of this observation and suggest that twin/HAGB triple junctions are microstructural weak points.

36 MATERIALS SCIENCE↗

Self-Healing Cements with Improved Toughness at Casing and Formation Interfaces for Subsurface Applications (CRADA 530)

Over the three-year CRADA, Pacific Northwest National Laboratory (PNNL) advanced a new class of Molecular Velcro™ self-healing wellbore cements designed to improve the long-term integrity of wells used for geothermal energy production and carbon storage. Conventional wellbore cement can crack due to repeated mechanical loading, temperature swings, and exposure to aggressive subsurface fluids. Once cracks form, they can create leakage pathways, drive expensive remediation (“workovers”), and in extreme cases shorten well life. This project addressed that problem by developing polymer-modified cement systems that can autonomously re-seal cracks and better tolerate the extreme conditions experienced in subsurface wells, while remaining compatible with practical cementing operations.

15 GEOTHERMAL ENERGY↗

AOI [1]: Passive Wireless Sensor Systems Fabricated by Direct-Writing for Temperature and Health Monitoring of Energy Systems in Harsh-Environments (Final Report)

Researchers at West Virginia University (WVU) propose to demonstrate a wireless, high-temperature sensor system for monitoring the temperature and health of energy-system components. The active sensor and electronics for wireless communication will be composed entirely of an electroceramic materials (conductive ceramics) which are capable of withstanding the harsh-environments required for fossil energy-based technologies. This work will focus primarily on the fabrication and testing of temperature (thermocouples and thermistors) and health (strain/stress and crack propagation sensors) that function at extreme temperatures (up to 700-1700ºC). The electronics will accompany the high-temperature sensor, which will include a passive wireless communication circuit that allows the transmission of the data based on the LCR resonance principle to a near-by reader antenna. This passive transmission of data will reduce the need for interconnect wires near the active, and possibly rotating, energy-system component. The research will include process development to permit the 2D/3D direct-writing of the entire sensor and communication circuit onto the energy-system component. The direct-writing will be facilitated by using silicon-based polymer-derived precursors to form the high-temperature, stable electroceramic compositions. In addition, methods for direct-writing the circuit onto a fugitive carrier substrate will be completed, which will permit a “peel-and-stick”-like transfer of the sensor circuit to the energy-system component. This feature will allow the economical and precise placement of the sensor circuit onto components of various shapes and locations, without altering the geometry and active features of the manufactured component, or the removal (or decommissioning) of the component for installation. The proposed work will be directed at the following areas: 1) Investigation of phase formation, sintering/grain growth, and electrical properties of polymer-derived electroceramic composites; 2) Definition of processes to direct-write through ink-jet and robo-casting the polymer-derived electroceramic composites onto oxide and polymer surfaces; 3) Development of methods to form monolithic "peel-and-stick" preforms that will efficiently transfer the sensor circuit to ceramic surfaces after thermal treatment; 4) Design of passive wireless LCR circuits and receiver (reader) antennas for communication and testing at high temperatures; 5) Investigation of the passive wireless sensor system developed (and method of transferring sensor system) for temperature and stress/strain measurements on a SOFC repeat unit and a singular gas turbine blade prototype as example applications.

01 COAL, LIGNITE, AND PEAT↗

srlife : A software tool for estimating the life of high temperature concentrating solar receivers. Part II – Ceramic receivers

As Concentrating Solar Power (CSP) technologies aim for higher operating temperatures to enhance efficiency and meet industrial process heat demands, high-temperature metallic materials, including nickel-based superalloys, face challenges in maintaining structural integrity. Advanced ceramics offer a promising alternative due to their superior high-temperature strength. However, accurately assessing the performance of ceramic components requires a fundamentally different approach from that used for metallic components. This Part II of a two-part paper describes the integration of ceramic statistical failure models within srlife – an open-source tool for predicting the life of high-temperature CSP receivers. These models account for the inherent variability in ceramic strength, as well as the effects of subcritical crack growth (SCG) under high temperature cyclic loads. Here, the paper includes an example problem that demonstrate the process of evaluating ceramic receivers using srlife. Part I details the life estimation process for metallic receivers (i.e. creep-fatigue life) along with input and output data structure, thermohydraulic analysis, and structural analysis. The complete tool is available as open-source software at https://github.com/srlife-project/srlife and can be installed via the PyPi package manager (https://pypi.org). By supporting both ceramic and metallic receiver analyses, srlife facilitates fair comparisons between competing metallic and ceramic designs, enabling accurate evaluations of plant efficiency and the economic benefits of ceramic solar receivers and other components.

High temperature ceramic receivers↗

Multiscale modeling of hydrogenolysis of ethane and propane on Ru(0001): Implications for plastics recycling

Plastic waste presents an environmental threat. Chemical recycling via hydrogenolysis can convert plastic waste into waxes, lubricants, and fuels. Among catalysts, Ru stands out for its superior activity and selectivity. The chemistry of light alkane hydrogenolysis can help understanding plastics deconstruction. Here, we perform first-principles calculations, develop descriptor-based relations, and conduct microkinetic modeling and analysis on ethane and propane. Predictions are in excellent agreement with experimental data. We identify a similar cracking pattern for both hydrocarbons entailing a deeply dehydrogenated species with the removal of four hydrogen atoms: CHCH*+* → 2CH* for ethane and CH 3 CCH*+2* → CH 3 C* + CH* for propane. We find that the rate-determining step is the C-C cracking for ethane and the first dehydrogenation from the terminal carbon (CH 3 CH 2 CH 3 *+* → CH 3 CH 2 CH 2 *+H*) for propane. The vinyl species CH 2 CH* produced from propane cracking is responsible for whether a single or multiple cracking events occur and effectively controls the selectivity. Specifically, ethane formation in propane hydrogenolysis is suppressed at elevated temperatures due to over-cracking via multiple (two here) cracking events being preferred over hydrogenation and desorption of ethane from the catalyst. Our workflow and models provide a baseline for future studies on heavier hydrocarbons. Insights into recent experimental studies of polyethylene over Ru-based catalysts are discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Evaluation of ceria as a surrogate material for UO 2 in experiments on fuel cracking driven by resistive heating

A variety of normal operation and accident scenarios can generate thermal stresses large enough to cause cracking in light-water reactor (LWR) fuel pellets. Cracking of fuel pellets can lead to reduced heat removal, larger centerline temperatures, and localized stress in cladding all of which impact fuel performance. Furthermore, pellet cracking also contributes to a temperature reduction in the pellet since the pellet fragments tend to move towards the heat sink (cladding), and the heat flow remains predominantly radial despite the presence of cracks. It is important to understand the temperature profile on the pellet before and after cracking to improve cracking models in fuel performance codes However, in-reactor observation and measurement of cracking is very challenging owing to the harsh environment and design of fuel rods. Recently, an experimental pellet cracking test stand was developed for separate effects testing of normal operations and accident temperature conditions, using thermal imaging to capture the pellet surface temperature for evaluation of thermal stresses and optical imaging to capture the evolution of cracking in real time. Cracking experiments were initially performed using ceria (CeO 2 ) as a surrogate fuel material, which is useful for developing and demonstrating the experimental approaches but is also valuable in its own right for cracking model development and validation. A combination of induction and resistance heating was used for volumetric heat generation in the pellet creating a thermal gradient. The material properties of CeO 2 and UO 2 are reviewed and compared for use in model development. Simulations of the experiment were performed to evaluate the behavior of the surrogate (CeO 2 ) fuel in BISON. The measured temperature profiles from BISON models match reasonably well with the observed experiments for the ceria pellets before cracking. The findings from this work will help improve confidence in fracture models used for fuel pellets under similar in-reactor conditions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Improved damage tolerance of SiC-based nuclear fuel cladding with novel multi-layered SiC coating design at 1200 °C

Continuous SiC fibre reinforced SiC matrix composites (SiC f -SiC m ) with monolithic SiC outer coatings are considered as a damage-tolerant cladding design for loss of coolant accident (LOCA) conditions in light water reactors. However, monolithic SiC coatings are brittle and prone to catastrophic failure. In this study, a SiC f -SiC m cladding with a novel multi-layer SiC outer coating (11 sub-layers, ∼260 µm in total thickness) was investigated under C-ring compression at room temperature and 1200 °C in argon environment. Real-time synchrotron X-ray computed tomography (XCT) was employed to capture crack initiation and propagation processes. Compared to conventional monolithic SiC outer coatings, the multi-layer coating structure facilitated crack deflection and bifurcation enhancing its damage tolerance at both temperatures. Despite pre-existing surface cracks, claddings exhibited stable mechanical-performance at both temperatures. These initial cracks did not critically affect the failure processes as they were not aligned with the maximum stress direction. Furthermore, the microstructure, distribution of residual stresses, and local properties of individual components in the material were thoroughly characterized, and compared with open literature on conventional claddings with monolithic outer coatings. These results provide new insights into the failure mechanisms of multi-layer SiC coatings and offer guidance for the future design of accident-tolerant nuclear fuel claddings.

36 - MATERIALS SCIENCE↗

Thermo-Mechanical Phase-Field Modeling of Fracture in High-Burnup UO2 Fuels Under Transient Conditions

This study presents a novel multiphysics phase-field fracture model to analyze high-burnup uranium dioxide (UO2) fuel behavior under transient reactor conditions. Fracture is treated as a stochastic phase transition, which inherently accounts for the random microstructural effects that lead to variations in the value of fracture strength. Moreover, the model takes into consideration the effects of temperature and burnup on thermal conductivity. Therefore, the model is able to predict crack initiation, propagation, and complex morphologies in response to thermal gradients and stress distributions. Several simulations were conducted to investigate the effects of operational and transient conditions on fracture behavior and the resulting cracking patterns. High-burnup fuels exhibit reduced thermal conductivity, elevating temperature gradients and resulting in extensive radial and circumferential cracks. Transient heating rates and temperatures significantly affect fracture patterns, with higher heating rates generating steeper gradients and more irregular crack trajectories. This approach provides critical insights into fuel integrity during accident scenarios and supports the safety evaluation of extended burnup limits.

Chemistry↗