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At least 163 records · Page 9

Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)

An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.

20 FOSSIL-FUELED POWER PLANTS↗

Development of interatomic potential and effect of ordering on defect properties in CrMnV

Developing materials that can withstand extreme environments, such as high radiation doses and elevated temperatures, is crucial for next-generation particle accelerators, including the 2.4 MW Long-Baseline Neutrino Facility. High-Entropy Alloys have emerged as promising candidates for beam window materials due to their superior mechanical strength, corrosion resistance, and radiation tolerance. In this study, we focus on the Cr–Mn–V alloy system, developing and employing machine-learning interatomic potentials (MLIPs) to investigate the formation of an ordered phase and its influence on defect properties. Using hybrid Monte Carlo-Molecular Dynamics simulations, we observe the formation of a B2-ordered phase at lower temperatures, consistent with Density Functional Theory (DFT) predictions. Ordered structures display a bimodal distribution of migration energies and reduced mean square displacement values, indicating suppressed vacancy diffusion. Our results also show that the migration energy barrier varies based on the atomic species, with Mn and V exhibiting the highest and lowest average barriers, respectively. These findings suggest that atomic ordering inhibits defect mobility, potentially enhancing the radiation resistance of CrMnV alloys. The validated MLIP provides a reliable framework for simulations that are faster than traditional DFT while maintaining the accuracy required to study defect and ordering properties.

36 MATERIALS SCIENCE↗

High Power Targetry R&D and support for future generation accelerator

A high-power target system is a key beam element to complete future High Energy Physics (HEP) experiments. The target endures high power pulsed beam, leading to high cycle thermal stresses/pressures and thermal shocks. The increased beam power will also create significant challenges such as corrosion and radiation damage that can cause harmful effects on the material and degrade their mechanical and thermal properties during irradiation. This can eventually lead to the failure of the material and drastically reduce the lifetime of targets and beam intercepting devices. Designing a reliable target is already a challenge for MW class facilities today and has led several major accelerator facilities to operate at lower power due to target concerns. With present plans to increase beam power for next generation accelerator facilities in the next decade and the multi-year time-scale to acquire the knowledge on material behavior under such extreme environment, timely R&D of robust high-power targets is critical to fully secure the physics benefits of ambitious accelerator power upgrades. The next generation of high-power targets for future accelerators will use more complex geometries, novel materials, and new concepts allowing better high heat flux cooling methods. Advanced numerical simulations need to be developed to satisfy the physical design requirements of reliable beam-intercepting devices. In parallel, radiation hardened beam instrumentation irradiation methods for high-power targets must be further developed. Additional irradiation facilities are needed since only a few facilities worldwide offer beams for target testing, and the beam provided may not be appropriate for the specific facility or project. Thus, a comprehensive research and development program must be implemented to address the challenges that multi-MW targets face.

Pellemoine, F.↗

Possibility of an integrated transmission electron microscope: enabling complex in-situ experiments

Abstract Multimodal in-situ experiments are the wave of the future, as this approach will permit multispectral data collection and analysis during real-time nanoscale observation. In contrast, the evolution of technique development in the electron microscopy field has generally trended toward specialization and subsequent bifurcation into more and more niche instruments, creating a challenge for reintegration and backward compatibility for in-situ experiments on state-of-the-art microscopes. We do not believe this to be a requirement in the field; therefore, we propose an adaptive instrument that is designed to allow nearly simultaneous collection of data from aberration-corrected transmission electron microscopy (TEM), probe-corrected scanning transmission electron microscopy, ultrafast TEM, and dynamic TEM with a flexible in-situ testing chamber, where the entire instrument can be modified as future technologies are developed. The value would be to obtain a holistic understanding of the underlying physics and chemistry of the process-structure–property relationships in materials exposed to controlled extreme environments. Such a tool would permit the ability to explore, in-situ, the active reaction mechanisms in a controlled manner emulating those of real-world applications with nanometer and nanosecond resolution. If such a powerful tool is developed, it has the potential to revolutionize our materials understanding of nanoscale mechanisms and transients. Graphical Abstract

36 MATERIALS SCIENCE↗

Thermal shielding by subliming volume reflectors in convective and intense radiative environments.

The behavior of dielectric materials having densely packed internal scattering centers subject to extreme convective and radiative environments is analyzed. Experiments have shown that these materials act as volume reflectors of incident radiation even when the exposed surface is being eroded by thermochemical ablation. The analysis was applied to interpret experiments of subliming Teflon models exposed to combined radiative and convective fluxes up to 1.7 kW/sq cm for several seconds. Results show that, although the exposed surface receded at an apparently steady rate, the internal temperature climbed continually, due to internal absorption of radiation and would have caused failure internally if the test duration were extended a few seconds. Thus, performance is time-limited by the internal absorption coefficient. Results were obtained for larger configurations and other materials. Typically, Teflon shells may withstand radiant fluxes up to 20 kW/sq cm for about 5 sec and fritted quartz up to 50 kW/sq cm for about 8 sec (corresponding to the Jupiter entry).

Howe, J. T.↗

Uranus Probe Entry and Descent Mission Concept

Introduction: Uranus was identified as the third highest priority flagship mission in the 2012-2022 Planetary Science Decadal Survey. This latest concept study was requested by the Decadal Survey panel to determine NASA’s planetary science priorities from 2022-2032. This study focused on the probe’s entry and descent aspects and associated trades for viable trajectory options. Uranus Mission and Descent Probe: The proposed Uranus Orbiter and Probe (UOP) Flagship mission will investigate Uranus and its surrounding moons using an orbiting spacecraft with a Uranus descent probe. Unlike previous studies the probe release will occur after orbit insertion allowing sufficient separation of critical events during the orbit insertion burn. The probe will be released at an altitude that allows one hour of in situ atmospheric readings that will be relayed to the orbiter. Afterwards the orbiter will transition to the moon tour phase of the mission. The configuration chosen for the entry aeroshell was a 45° sphere-cone. This shape has been used in the past in the Pioneer Venus Galileo missions. However, the nose radius considered in the present study differed from the values used in either of the previous configurations, primarily to reduce the heat flux at the stagnation point. A two-step approach was used in the development of flight trajectories for the chosen configuration. In the first step, the trajectory code POST2 was used to screen the thousands of entry states provided by interplanetary trajectory simulations, which were terminated at an altitude of 2000 km from the reference surface (1 bar) of Uranus. The screening criteria were: (i) optimization of the communication geometry between the entry probe and orbiter to ensure at least 1 hour of science measurements, (ii) peak stagnation point pressures to be less than six bar, (iii) peak heat fluxes to be less than 5 kW/cm2; the latter two constraints being the limits of ground-test capabilities of the arc jets at NASA Ames Research Center. The entry team investigated two trajectories that met the criteria above, a shallow entry (high heat load ~44 kJ/cm2) and a steeper entry (high heat rate ~1950 W/cm2). In the second step, the two bounding candidate entry states from the POST2 screening process were used in developing flight trajectories using TRAJ coupled with FIAT (a materials thermal response and sizing code) and a margins policy to determine a margined uniform thickness (hence mass) of the forward heatshield material based on the aerothermal environments at the stagnation point. Since the combination of TRAJ and FIAT size the TPS based on stagnation point environments only, flow field computations using DPLR were necessary to determine turbulent aerothermal environments on the conical flank, and the augmentation of these environments due to surface roughness. The environments at select locations on the forward heatshield were then used to size the thermal protection material, with the largest thickness value then used to estimate the mass. The newly developed woven thermal protection material –HEEET (Heatshield for Extreme Entry Environments Technology) –was considered for the forward heatshield and PICA (Phenolic-Impregnated Carbon Ablator) was considered for the backshell. These NASA-developed materials are at TRL 6 and TRL 9, respectively. Furthermore, two options were considered for the HEEET material: (i) a dual-layer option with a denser recession layer on top and an insulative layer underneath it, and (ii) a single layer option consisting of the insulative layer alone. Results: It is clear that probe entry states are feasible and the selected TPS options are able to perform in the predicted aerothermal environments thus enabling the mission to meet of the descent probe portion of this flagship mission

Entry Descent and Landing↗

Simulation, Structural, Thermal and Mechanical Properties of the FeTiTaVW High Entropy Alloy

Developing new materials to be applied in extreme environments is an opportunity and a challenge for the future. High entropy alloys are new materials that seem promising approaches to work in nuclear fusion reactors. In this work, FeTaTiVW high entropy alloys were developed and characterized with Molecular Dynamic and Hybrid Molecular Dynamic Monte Carlo simulations. The simulation results show that phase separation originates a lower potential energy per atom and a high level of segregation compared to those of a uniform solid solution. Moreover, the experimental diffractogram of the milled powder shows the formation of a body-centred cubic-type structure and the presence of TiO2. In addition, the microstructure of the consolidated material evidenced three phases: W-rich, Ti-rich, and a phase with all the elements. This phase separation observed in the microstructure agrees with the Hybrid Molecular Dynamic Monte Carlo simulation. Moreover, the consolidated material’s thermal conductivity and specific heat are almost constant from 25 °C to 1000 °C, and linear expansion increases with increasing temperature. On the other hand, specific heat and thermal expansion values are in between CuCrZr and W values (materials chosen for the reactor walls). The FeTaTiVW high entropy alloy evidences a ductile behaviour at 1000 °C. Therefore, the promising thermal properties of this system can be attributed to the multiple phases and systems with different compositions of the same elements, which is exciting for future developments.

Martins, Ricardo (ORCID:0000000177685704)↗

White Papers for the Next Decadal Survey: Thermal Protection Systems and Instrumentation

NASA is anticipated to commission the next Planetary Science Decadal Survey (PSDS) with preparation expected in early calendar year 2020. The new PSDS will outline the priorities of science missions for the decade spanning 2023-2032. For the previous PSDS, the science and technology communities have been invited to submit white papers to the PSDS sub-panels as background information to guide the PSDS recommendations. The National Research Council has previously stated that white papers that represent the opinion of many authors from different institutions carried more significant and weight, and the recommendations from the previous PSDS attempted to reflect more of a consensus opinion.In 2009, a total of 4 white papers were submitted to the PSDS panels regarding thermal protection system (TPS) readiness for missions, as well as one on TPS instrumentation. The TPS readiness papers were co-authored by 90 individuals from many institutions. These white papers surveyed the TPS materials for both forebody and afterbody of a probe and analyzed the suitability of materials for missions to each destination. In addition, each paper outlined the ground testing required and ongoing technology development. Recommendations were provided for further technology development and ground test capability in order to fulfill future missions. Planning for the next PSDS: Many improvements and changes have occurred in the past 10 years with regard to TPS materials and instrumentation. New materials have been developed and tested, such as the high density material Heatshield for Extreme Entry Environment Technology (HEEET), and new capabilities for ground testing for high heating and high pressures have been added such as the 3” nozzle at the Ames arc jet. NASA has also flown several TPS instrumentation suites, such as MEDLI and EFT-1.In order to provide the PSDS sub-panels with the most current information about the state-of-the-art suit-ability for TPS materials for entry missions, we are be-ginning to update and draft new white papers. We will present the outline for material to be covered in the white papers, and we invite all IPPW attendees to parti-ciate in co-authoring these papers.

Hwang, H. H.↗

A Comparative Study of Thermal Oxidization Resistance of a High-Entropy Metal Boride and a High-Entropy Metal Carbide

We present a systematic study of thermal oxidation resistance of transition metal borides and carbides up to 1300 °C in a dry air environment. A High-Entropy Metal Boride (HEMB), of composition (Hf 0.2 , Mo 0.2 , Nb 0.2 , Ta 0.2 , Zr 0.2 )B 2 , and a similar High-Entropy Metal Carbide (HEMC) (Hf, Mo, Nb, Ta, Zr)C 5 were synthesized from precursor mixtures, under 30 MPa of pressure at a temperature of 1800 °C using a Spark Plasma Sintering Device. The synthesized phases were confirmed via X-ray Diffraction analysis, which showed a pure hexagonal AlB 2 -type structure for HEMB and a face-centered cubic (FCC) structure for HEMC, with lattice parameters, a = 3.10 Å and c = 3.37 Å for HEMB and a = 4.524 Å for HEMC. Oxidation resistance was evaluated using a simultaneous thermogravimetric analysis and differential scanning calorimetry (TGA/DSC) stage in which HEMB and HEMC were heated up to 1300 °C at a rate of 2 °C/min in a dry air environment. Scanning electron microscopy (SEM) was used to analyze the resulting oxidized material. Our study demonstrates that HEMB shows better thermal oxidation resistance as compared to a similar metal composition HEMC at high temperatures.

36 MATERIALS SCIENCE↗

Nonmetallic-materials development for spacecraft applications

The development, characteristics, and applications of nonmetallic materials used for spacecraft structures are discussed. The effects of extremes in environment as a factor in material selection are considered. Material design parameters are especially complex because of the requirements imposed for additional fire safety and resistance to the free space and lunar surface environment.

Dawn, F. S.↗

Micromechanical simulation of damage progression in carbon phenolic composites

Carbon/phenolic composites are used extensively as ablative insulating materials in the nozzle region of solid rocket motors. The current solid rocket motor (RSRM) on the space shuttle is fabricated from woven rayon cloth which is carbonized and then impregnated with the phenolic resin. These plies are layed up in the desired configuration and cured to form the finished part. During firing, the surface of the carbon/phenolic insulation is exposed to 5000 F gases from the rocket exhaust. The resin pyrolizes and the material chars to a depth which progresses with time. The rate of charring and erosion are generally predictable, and the insulation depth is designed to allow adequate safety margins over the firing time of the motor. However, anomalies in the properties and response of the carbon/phenolic materials can lead to severe material damage which may decrease safety margins to unacceptable levels. Three macro damage modes which were observed in fired nozzles are: ply lift, 'wedge out', and pocketing erosion. Ply lift occurs in materials with plies oriented nearly parallel to the surface. The damage occurs in a region below the charred material where material temperatures are relatively low - about 500 F. Wedge out occurs at the intersection of nozzle components whose plies are oriented at about 45 deg. The corner of the block of material breaks off along a ply interface. Pocketing erosion occurs in material with plies oriented normal to the surface. Thermal expansion is restrained in two directions resulting in large tensile strains and material failure normal to the surface. When a large section of material is removed as a result of damage, the insulation thickness is reduced which may lead to failure of the nozzle due to excessive heating of critical components. If these damage events cannot be prevented with certainty, the designer must increase the thickness of the insulator thus adding to both weight and cost. One of the difficulties in developing a full understanding of these macro damage mechanisms is that the loading environment and the material response to that environment are extremely complex. These types of damage are usually only observed in actual motor firings. Therefore, it is difficult and expensive to evaluate the reliability of new materials. Standard material tests which measure mechanical and thermal properties of test specimens can only provide a partial picture of how the material will respond in the service environment. The development of the ANALOG test procedure which can combine high heating rates and mechanical loads on a specimen will improve the understanding of the interactive effects of the various loads on the system. But a mechanistic model of material response which can account for the heterogeneity of the material, the progression of various micromechanical damage mechanisms, and the interaction of mechanical and thermal stresses on the material is required to accurately correlate material tests with response to service environments. A model based on fundamental damage mechanisms which is calibrated and verified under a variety of loading conditions will provide a general tool for predicting the response of rocket nozzles. The development of a micromechanical simulation technique was initiated and demonstrated to be effective for studying across-ply tensile failure of carbon/phenolic composites.

Slattery, Kerry T.↗

Common Probe Design Study and Follow-On Activities

The Common Probe Study was funded by the NASA's Planetary Science Division in the Science Mission Directorate in 2018 to investigate the feasibility of a common aeroshell design for atmospheric probe missions at Venus, Jupiter, Saturn, Uranus, and Neptune. The study involved 4 NASA Centers: Ames Research Center, Goddard Space Flight Center, Langley Research Center, and the Jet Propulsion Laboratory. The common aeroshell design that was studied was a 400 kg, 1.5 m diameter, 45-degree sphere cone shape with a high density heatshield material (Heatshield for Extreme Entry Environments Technology, or HEEET) and a parachute system to extract the descent vehicle. This size of aeroshell could accommodate a descent vehicle of 0.75 m diameter, which could encompass both Tier 1 and Tier 2 science instruments at each of the 5 destinations. Study methodology: First, a notional payload of instruments for each destination was defined based on the top priority measurements indicated by the Planetary Science Decadal Survey. Steep and shallow entry flight path angles (EFPA) were defined for each planet based on qualification and operational g-load limits for current, state-of-the-art instruments. Interplanetary trajectories were then identified that bounded the EFPA range.Next, 3-DoF simulations for entry trajectories were run using the entry state vectors from the interplanetary trajectories. Conical ribbon parachutes were sized based on heatshield separation dynamics. Aero-heating correlations were used to generate stagnation point convective and radiative heat flux profiles. High fidelity thermal response models for various TPS materials were used to size stagnation point thicknesses, with margins based on previous studies. Backshell TPS masses were assumed based on scaled heat fluxes from the heatshield and also from previous mission concepts.Based on these analyses, we have found that the common design is applicable for atmospheric probe missions for 4 out of the 5 destinations. Because of the unique gravity well for Jupiter, the entry environments are more severe resulting in heat loads an order of magnitude higher than for the other destinations.The next step is to determine what follow-on activities NASA should engage in. A questionnaire for the atmospheric probe community has been developed, with a focus on what size of aeroshell should be further analyzed (smaller or same diameter), and what incentives would make using such an aeroshell, if assembled and available, desirable to mission proposers.Preliminary results from this questionnaire will be presented.

Hwang, Helen H.↗

Process Intensification for Nanostructure Aluminum Extrusions

A new technology called Shear Assisted Processing and Extrusion (ShAPE™), pioneered at the Pacific Northwest National Laboratory (PNNL), has the potential to revolutionize the US extrusion industry. Maturation of the ShAPE™ process would create a new cross cutting US manufacturing technology that advances three key the objectives within AMO; namely, nanomaterials processing, process intensification, and materials for extreme and harsh environments. PNNL and SCM Metals Products, Inc. (SCM), a division of Kymera International, will collaborate to mature the ShAPE™ extrusion process beyond TRL 3 to increase the likelihood of its adoption by industry. PNNL’s custom (one-of-a-kind in the world) ShAPE™ machine will be used to extrude round rods of high strength aluminum alloy feedstock powder provided by SCM. As proof-of-concept, PNNL has previously extruded 5 mm diameter rods with SCM aluminum alloy powder AL-12.4TM. This project aims to scale up the process to a diameter of 25 mm while retaining the excellent mechanical properties achieved for the 5 mm diameter rods. The degree of process intensification with ShAPE™ will also be estimated. The primary objectives of this project are as follows. 1) Fabricate 25 mm diameter nanostructured extrusions in bulk, directly from AL-12.4TM aluminum alloy powder without the need for canning, degassing, compaction, and other intermediate steps typical of powder metallurgy extrusion. 2) Achieve a microstructure with an ultrafine grained (UFG <1 µm) aluminum matrix having refined and homogenously distributed nanoscale second phases. 3) Show that the ram force can be significantly reduced compared to conventional powder metallurgy extrusion of the same material and estimate the extent of process intensification that may be possible with ShAPE™. 4) Demonstrate improved high-temperature mechanical properties compared to conventional extrusion of the same material. The following tasks will be undertaken to achieve these objectives. PNNL will develop the die set and process parameters necessary to fabricate Al-12.4TM extrusions with a 25 mm diameter. Microstructural analysis will be performed by PNNL while mechanical testing will be conducted by SCM. With information learned from the process development and characterization, PNNL will perform an estimate of the degree of process intensification that may be possible with ShAPE™.

42 ENGINEERING↗

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗

Unravelling the sintering temperature-induced phase transformations in Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics

This work reports on the fundamental details of the crystal structure and phase transformations in Ba(Fe 0.7 Ta 0.3 )O 3-δ , the best known temperature-independent oxygen-sensing ceramic material for applications in extreme environments. Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics were synthesized using conventional solid-state ceramic reaction under variable sintering temperatures (T s = 1200–1350 °C). Combined X-ray diffraction (XRD) and high-resolution transmission electron microscopy (TEM) measurements revealed the T s -induced phase transformations and their origin in Ba(Fe 0.7 Ta 0.3 )O 3-δ . Associated with phase transformations, pseudo-cubic (PC) reflections, such as {200} PC , {211} PC , and {220} PC , exhibited distinct anomalies with increasing T s . At T s = 1200 °C, Ba(Fe 0.7 Ta 0.3 )O 3-δ stabilized in mixed orthorhombic + rhombohedral phases (Amm2 + R3m). With increasing T s (≥1250 °C), Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics stabilized in tetragonal/rhombohedral [P4mm + R3m] mixed phases, while variations in the quantity of the respective phases were observed. Because both structure and crystal chemistry play key roles in achieving enhanced performance in chemical sensing and catalytic converters, detailed understanding of the phase transformations and crystal structure of Ba(Fe 0.7 Ta 0.3 )O 3-δ ceramics, as derived in this work, will be useful to develop chemical sensors with optimum performance for high-temperature and corrosive environments.

36 MATERIALS SCIENCE↗

Interface effect of Fe and Fe 2 O 3 on the distributions of ion induced defects

The stability of structural materials in extreme nuclear reactor environments—with high temperature, high radiation, and corrosive media—directly affects the lifespan of the reactor. In such extreme environments, an oxide layer on the metal surface acts as a passive layer protecting the metal underneath from corrosion. To predict the irradiation effect on the metal layer in these metal/oxide bilayers, nondestructive depth-resolved positron annihilation lifetime spectroscopy (PALS) and complementary transmission electron microscopy (TEM) were used to investigate small-scale defects created by ion irradiation in an epitaxially grown (100) Fe film capped with a 50 nm Fe 2 O 3 oxide layer. In this study, the evolution of induced vacancies was monitored, from individual vacancy formation at low doses—10 –5 dpa—to larger vacancy cluster formation at increasing doses, showing the sensitivity of positron annihilation spectroscopy technique. Furthermore, PALS measurements reveal how the presence of a metal–oxide interface modifies the distribution of point defects induced by irradiation. TEM measurements show that irradiation induced dislocations at the interface is the mechanism behind the redistribution of point defects causing their accumulation close to the interface. Finally, this work demonstrates that the passive oxide layers formed during corrosion impact the distribution and accumulation of radiation induced defects in the metal underneath and emphasizes that the synergistic impact of radiation and corrosion will differ from their individual impacts.

36 MATERIALS SCIENCE↗