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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Characterization and Speciation of Marine Materials Using Synchrotron Probes: Guidelines for New Users

Synchrotron instruments are useful for marine studies because they make nondestructive measurements of chemical composition and speciation on small sample volumes and at low concentrations. Synchrotron beamtime is available without cost using a peer-reviewed proposal system. New users do not have to be synchrotron radiation experts to design a good experiment, but some guidance is needed to design and propose appropriate experiments. Here we present some of that guidance to encourage and increase access to synchrotron facilities for marine science. We provide advice and examples from experts on how to access these instruments, choose the optimal sample preparation, and avoid common pitfalls. We then present some examples of successful marine studies that use these techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Swift heavy ion irradiation effects in zirconium and hafnium carbides

The behavior of microcrystalline zirconium carbide (ZrC) and hafnium carbide (HfC) was studied under highly ionizing irradiation conditions at room temperature. The induced structural modifications were characterized via synchrotron-based X-ray diffraction experiments. Unit-cell expansion and buildup of microstrain were determined across a wide fluence range and linked to chemical compositions of the target material. The observed swelling resulting from irradiation with 198 MeV Xe ions in both carbide materials is characterized by two distinct mechanisms that operate within different fluence regimes. Unit-cell expansion initially proceeds by a direct-impact behavior that reaches saturation, followed at higher fluences by a second, linear swelling regime. The overall behavior, particularly the direct-impact regime, is similar for ZrC and HfC, with a more pronounced second defect accumulation process in HfC. Swelling in ZrC shows the same two distinct mechanisms upon irradiation with 198 MeV Xe ions and 946 MeV Au ions, but swelling induced by the lower-energy ions is greater across the entire fluence series. Accounting for the difference in energy deposition density between the two irradiation conditions reveals that the first swelling mechanism (direct-impact behavior) is likely related to the formation of more simple defects. In contrast, the second damaging mechanism at higher fluences (linear increase) cannot be fully explained by the induced energy density, and swelling remains somewhat higher for the low-velocity Xe irradiation. This may suggest that more complex defects and defect clusters are responsible for this swelling regime, with either their size and/or morphology modified at different energy densities.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Response of ZrC to swift heavy ion irradiation

Zirconium carbide (ZrC) is commonly used for energy sector research, as well as a surrogate for the proposed advanced nuclear fuel candidate uranium carbide. Here this study investigates structural modifications to nanocrystalline and microcrystalline ZrC resulting from dense electronic excitations induced by swift heavy ion exposure. Samples were irradiated with 946 MeV Au ions to various fluences up to 6 × 10 13 ions cm –2 and characterized using synchrotron-based x-ray diffraction. The evolution of the unit-cell parameter and heterogeneous microstrain were evaluated as a function of fluence and compared with those of nanocrystalline and microcrystalline CeO 2 (a surrogate for UO 2 fuel) irradiated under identical conditions. Distinct differences were observed in the radiation responses of the carbide and oxide across both grain sizes. Most notably, microcrystalline ZrC exhibits swelling characterized by two distinct regimes, which does not result in saturation at the ion fluences achieved. This contrasts with CeO 2 , which exhibits the well-documented direct-impact defect accumulation mechanism, reaching a steady-state saturation of swelling at higher fluences. Nanocrystalline CeO 2 undergoes more pronounced swelling compared with microcrystalline CeO 2 , in contrast to nanocrystalline ZrC, which exhibits only minimal unit-cell changes. These results demonstrate that swift heavy ion-induced structural changes can be quite different in carbides and oxides, which must be considered when extrapolating fission-fragment type damage in current fuels to advanced fuels.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2024

Oil-Pressure Based Apparatus for In-Situ High-Energy Synchrotron X-Ray Diffraction Studies During Biaxial Deformation

Background: Understanding biaxial loading response at the microstructural level is crucial in helping better design sheet manufacturing processes and calibrate/validate material deformation models. Objective: The objective of this work was to develop a low-cost testing apparatus to probe, with sufficient spatial resolution, the micro-mechanical response of a sheet material in-situ under biaxial loading conditions. Methods: The testing apparatus fabricated as a part of this study operates in a similar fashion to a standard bulge test and uses oil pressure to generate biaxial loading conditions. This biaxial testing apparatus was operated within a synchrotron beamline to characterize the mechanical response of a flash-processed steel sheet using in-situ high-energy X-ray diffraction (XRD) measurements. Further, the GSAS-II package was utilized to develop a workflow for the analysis of the large volume of diffraction data acquired. The workflow was then used to extract the peak position, width, and integrated intensity of the XRD peaks corresponding to the major body-centered cubic phase. Results: The equi-biaxial nature of the loading in the measured area was independently corroborated using experimental (XRD) and simulation (finite element analysis) methods. Furthermore, we discuss the evolution of elastic strain in the major body-centered cubic phase as a function of applied oil pressure and location on the steel sheet. Conclusions: A key advantage of the biaxial apparatus fabricated in this synchrotron study is demonstrated using the results obtained for the flash-processed steel sheet – i.e., mapping the lattice plane-dependent response to biaxial loading for a relatively large sample area in a spatially resolved manner.

36 MATERIALS SCIENCE↗
DOE OSTI2023

High‐Nickel Heterostructured Cathodes with Local Stoichiometry Control for High‐Voltage Operation

The growing demand for lithium‐ion batteries to power electric vehicles and other energy‐dense devices continues to fuel the need for cathodes of increasingly higher nickel in cathodes. The relentless pursuit of high Ni content, however, raises concerns on compromising cell lifetime and safety, especially under high‐voltage operation. Alternative to the traditional design of uniform or core–shell composition, we report a rational control of local stoichiometry in high‐Ni cathodes, enabling their high thermal and cycling stabilities—up to 258 °C at the fully charged state and 91.4% capacity retention for 100 cycles between 2.7 and 4.4 V. Multimodal synchrotron X‐ray characterization unveils the heterostructure of secondary particles, featuring a high‐Ni core (LiNi 0.90 Mn 0.05 Co 0.05 O 2 ) covered by a thin Ni‐gradient layer that remains stable over prolonged cycling due to suppressed oxygen release and structural deterioration. This work underlines, the intricate interplay between local stoichiometry and redox reactions in stabilizing high‐Ni cathodes for high‐voltage operation while ensuring safety.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Influence of thermal treatment on structure and catalytic performance of ceria-zirconia supported copper oxide (CuO x /Ce y Zr 1-y O 2 ) catalysts for CO oxidation

Copper oxide (CuO x ) supported on ceria-zirconia (Ce y Zr 1-y O 2 , y = 1.0, 0.5, 0.0) catalysts were investigated to elucidate the effects of thermal treatment on their physicochemical properties and catalytic performance in carbon monoxide (CO) oxidation. Here, the catalysts were synthesized via a one-pot chemical vapor deposition (OP-CVD) method at 700˚C and 900˚C with controlled Cu loading. Characterization techniques, including synchrotron X-ray diffraction (S-XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma spectroscopy (ICP), and N 2 adsorption-desorption, were implemented to probe the crystalline structure, molecular and electronic structure, oxygen vacancies, specific surface area (SSA) and metal loading. CO oxidation was chosen as a model reaction to explore the structure-catalytic performance relationship. A ∼100% CO conversion was achieved at < 150˚C, particularly with the CuO x /CeO 2 catalyst calcined at 700˚C. In contrast, calcination at 900˚C caused a ∼90% decrease in SSA and a ∼24% increase in T 50 . Activity tests revealed that increasing ZrO 2 content lowered CO oxidation activity despite generating more defect sites. In-situ measurement of the 700 °C calcined samples revealed the presence of stable and unstable defects in CuO x /Ce 0.5 Zr 0.5 O 2 and CeO 2 respectively, which play a key role in the activity of the catalysts. The results highlight that catalytic performance is closely related to the SSA. Furthermore, an optimum calcination temperature favor significant oxygen vacancy formation with required CuO x -support interactions, enhancing redox properties and catalytic performance.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Mechanistic transition of stainless steel 304L corrosion in MgCl 2 phase change material under thermal cycling

Magnesium chloride (MgCl 2 )-based molten salt phase change materials (PCMs) are promising candidates for thermal energy storage (TES) owing to their advantageous thermophysical properties, however, their high corrosivity in the molten state limits material compatibility. In this study, the corrosion behavior of 304?L stainless steel (SS304L) exposed to MgCl2 PCM was investigated as a function of thermal cycling (up to 9000 cycles) relevant to PCM-based TES systems. Microstructural changes and elemental redistribution at the alloy-salt interface under thermal cycling conditions were characterized using synchrotron-based X-ray fluorescence (XRF) and scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDS). Results show that corrosion is governed by selective Cr-dissolution and elemental diffusion near the interface and grain boundaries. A clear transition in the dominant corrosion mechanism is observed with increasing thermal cycles. Surface corrosion is the dominant mechanism up to 1000 cycles, whereas intergranular corrosion becomes the primary degradation mode beyond 2000 cycles. These mechanistic changes are interpreted in terms of evolving interfacial chemistry, microstructure and the diffusion-driven redistribution of alloying elements.

36 MATERIALS SCIENCE↗
DOE OSTI2024

High-entropy Li-rich layered oxide cathode for Li-ion batteries

High-entropy oxides (HEOs) are emerging as promising cathode materials for Li-ion batteries (LIBs) due to their stable solid-state phase and compositional flexibility. Herein, we investigate the structural and electrochemical properties of a novel non-equimolar high-entropy cathode material, termed high-entropy Li-rich layered oxide (HE-LLO, Li 1.15 Na 0.05 Ni 0.19 Mn 0.56 Fe 0.02 Mg 0.02 Al 0.02 O 1.97 F 0.03 ), in comparison to a pristine Li-rich layered oxide (PR-LLO, Li1.2Ni0.2Mn0.6O2). The incorporation of multiple cations (Na + , Al 3+ , Mg 2+ , Fe 3+ ) and anion (F - ) into HE-LLO introduces compositional diversity, enhancing structural stability through the entropy stabilization effect. Theoretical calculations confirm a significantly higher configurational entropy in HE-LLO compared to PRLLO, supporting its high-entropy nature. Electrochemical evaluations demonstrate that HE-LLO exhibits considerable capacity retention, preserving 76.8 % of its discharge capacity at 0.5C after 200 cycles, compared to only 36.2 % for PR-LLO. Even under high-temperature conditions, HE-LLO outperformed PR-LLO, maintaining 76.1 % of its discharge capacity after 100 cycles at 5C, while PR-LLO retained only 12.4 %. These enhancements are attributed to the improved phase reversibility and higher Li + ion diffusion coefficients of HE-LLO, validated by ex-situ characterizations using a synchrotron X-ray technique, along with density functional theory (DFT) calculations. In conclusion, these findings highlight the promise of non-equimolar HEOs as a novel design strategy for highperformance cathode materials.

25 ENERGY STORAGE↗
DOE OSTI2023

Role of Fe in long-range ordered Ni 2 Cr precipitates in Ni-Cr-Fe model alloys during isothermal aging

The precipitation of new phases during long-term service at elevated temperatures is a concern for the thermal stability of engineering alloys. In Ni-Cr-based alloys, e.g., Alloy 690, the formation of long-range ordered Ni 2 Cr causes embrittlement and may impact the lifetime of nuclear power plant components. In this work, we quantify the formation and evolution of Ni 2 Cr precipitation in eleven Ni-Cr-Fe model alloys with 0, 5, 7, and 10wt % Fe contents, and with Ni/Cr atomic ratios of 1.8, 2.0, 2.2, 2.4. These alloys were isothermally aged up to 10,000h at temperatures between 330 and 475°C. The alloys were characterized by synchrotron-based x-ray diffraction and Vickers hardness testing to quantify Ni 2 Cr precipitate size, and the impact of precipitate size on the mechanical properties as a function of Fe content. After 10,000 h of aging at 475°C and 418°C, the formation of Ni 2 Cr was observed in all alloys with 0 and 5wt % Fe. After 10,000h of aging at 418°C, Ni 2 Cr precipitates were also observed in the 7wt % Fe containing Ni/Cr=2.0 sample. Further, no clear evidence of Ni 2 Cr was observed in any of the 10wt % Fe samples at any time and temperature combination. We find that the face-centered cubic matrix lattice contraction and Vickers hardness are correlated with the Ni 2 Cr formation. The greatest change in hardness and lattice contraction occurs in stoichiometric alloys (Ni/Cr=2.0) with 0wt % Fe at 475°C. The rate of change in the material properties for the 5wt % Fe alloys is reduced, however the magnitude of changes is similar to 0wt % Fe alloys. A precipitation hardening model developed for Ni-Cr alloys based on critical resolved shear stress with weakly coupled dislocations shows a clear link between Ni 2 Cr precipitate size and hardness. This trend held across all alloys with Ni 2 Cr formation regardless of Fe concentration. This important structure-property relationship can potentially help define Ni-Cr-Fe-based component lifetimes directly through an understanding of how Ni 2 Cr formation impacts mechanical properties as a function of Fe content.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Inhibit the strain accumulation for 5V spinel cathode by mitigating the phase separation during high voltage stage

LiNi 0.5 Mn 1.5 O 4 (LNMO) spinel cathode is a potential cathode material for high-power, low-cost lithium-ion batteries (LIBs) due to its low raw material cost, high operating voltage and efficient lithium-ion transport channel. However, LNMO suffers from structural stability due to the two-phase-transformation during charge/discharge process, leading to poor cycling performance. Here, to address the issues, we have constructed a homogeneous aggregated LNMO cathode with a multifaceted primary particle, namely the LNMO with single-crystal secondary particles (SSP LNMO). Ex situ and in situ characterizations including the synchrotron X-ray diffraction, the neutron diffraction and full pouch cell validated that the SSP LNMO exhibit a single solid-solution reactions with a restrained lattice evolution during the delithiation/lithiation process. This is in contrast to the normal LNMO cathode, which demonstrates a significant two-phase transition from spinel Li 1-x Ni 0.5 Mn 1.5 O 4 to rock-salt MnO 2 at high voltage. Therefore, the SSP LNMO has greatly improved cycle life compared to the normal LNMO cathode. Overall, this study demonstrates the possibility of constructing LNMO based on primary-grain morphology modulation to improve the intrinsic stability of LIBs.

25 ENERGY STORAGE↗
DOE OSTI2025

Structure of Novel Phosphonium-Based Ionic Liquids with S and O Substitutions from Experiments and a Mixed Quantum-Classical Approach

This article presents experimental characterization information and synchrotron X-ray scattering measurements on a set of novel O- and S-substituted phosphonium-based ionic liquids (ILs) all coupled with the bis(fluorosulfonyl)imide (FSI-) anion. The ILs include the ethoxyethyltriethylphosphonium (P 222(2O2) + ) and triethyl[2-(ethylthio)ethyl]phosphonium (P 222(2S2) + ) cations, and we contrast results on these with those for unsubstituted triethylpentylphosphonium (P 2225 + ). The article also introduces a physics-based protocol that combines classical force field studies on larger simulation boxes with classical and first-principles studies on smaller boxes. The method produces significantly improved S(q) functions in the regime which in prior publications we have associated with inter- and intraionic adjacency correlations. By understanding which shorter-range structural changes improve S(q) in the q-regime of interest, we are also able to pinpoint specific deficiencies in the classical force field model. The approach we take should be quite general and could help study other complex liquids on different length scales.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Composition, Activity, and Stability of IrO x Oxygen Evolution Reaction Electrocatalysts

The oxygen evolution reaction (OER) is integral to several electrochemical energy conversion and storage technologies, including carbon dioxide reduction to value added fuels, nitrogen reduction to ammonia, reversible fuel cells, rechargeable metal−air batteries, and water electrolysis to produce hydrogen. Iridium oxide (IrO x ) is widely recognized as the benchmark OER catalyst for acidic environments. Despite widespread use of IrO x catalysts, most notably in proton-exchange membrane water electrolyzers (PEMWEs), a comprehensive understanding of the physicochemical properties of commercial catalysts and the impact of these properties on both the activity and stability of these catalysts is lacking. Here, we study commercial IrO x catalysts with different physicochemical properties, three nominally considered amorphous and three rutile, to elucidate how structural and compositional variations affect OER activity and stability. Utilizing standardized aqueous electrochemical protocols, time-resolved dissolution quantification using inductively-coupled plasma mass spectrometry, and physicochemical characterization, including multiple synchrotron X-ray techniques, we systematically correlate catalyst properties with OER performance and degradation behavior aided by principal component analysis (PCA). Our results demonstrate the general trend of amorphous IrO x having higher intrinsic activity but limited stability and crystalline rutile IrO 2 having lower activity but enhanced stability against dissolution. The trends within the amorphous and rutile catalyst groups correlate with inherent material properties, including phase composition and structure, crystallinity, particle size, surface area, and surface structure/chemistry. Notably, we identify a rutile catalyst with the largest crystallite/ domain sizes, moderate surface area, a small fraction of hydrous phase, and a favorable pore structure (trimodal distributions of pore sizes ranging from 2−5 nm) that exhibits the best balance between activity and stability among the six catalysts studied here. These findings illustrate a fundamental structure-governed trade-off between activity and stability and highlight the critical role of surface chemistry modification and structure engineering in IrO x catalyst optimization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Effect of Lithium Doping on MgO Hydroxylation and Carbonation

Recovery of magnesium from brines can potentially be used to source MgO (periclase) as a CO 2 sorbent or for Mg-based cements. However, it is not clear how common impurities in brines, such as lithium, affect the resulting MgO reactivity. Here, to test the effect of lithium incorporation on MgO reactivity for hydration and carbonation, we combined computational simulations with experiments. Experimentally altered (Mg,Li)O with a low dopant concentration (0.012 ± 0.002% w/w Li) was characterized using synchrotron-based X-ray scattering and high-resolution electron microscopy to measure reaction layer formation on (Mg,Li)O. Single-crystal X-ray diffraction analysis of (Mg,Li)O demonstrates that the incorporation of lithium leads to the formation of oxygen vacancies. The presence of vacancies is likely causing faster hydroxylation rates as predicted by ab initio molecular dynamics simulations. However, the faster hydroxylation rates likely lead to faster passivation of the surface because we observe thinner reaction layers on (Mg,Li)O samples both over short time periods (30 days) and over long time periods (28 years). After 28 years, the reaction layer on the (Mg,Li)O sample was less than one-third of the thickness of that of the pure MgO sample. In addition, over 30 days, reaction layers on (Mg,Li)O samples primarily formed at steps rather than on terraces, in contrast to our previous observations on MgO. Based on our results, naturally occurring impurities in MgO modify its reactivity even at very low concentrations and need to be considered for accurate reaction rate prediction for application of MgO as a CO 2 sorbent or in cements.

MgO↗
DOE OSTI2023

High-entropy electrolytes for practical lithium metal batteries

Electrolyte engineering is crucial for improving battery performance, particularly for lithium metal batteries. Recent advances in electrolytes have greatly improved cyclability by enhancing electrochemical stability at the electrode interfaces, but concurrently achieving high ionic conductivity has remained challenging. Here we report an electrolyte design strategy for enhanced lithium metal batteries by increasing the molecular diversity in electrolytes, which essentially leads to high entropy electrolytes (HEEs). We find that in weakly solvating electrolytes, the entropy effect reduces ion clustering while preserving the characteristic anion-rich solvation structures, which is characterized by synchrotron-based X-ray scattering and molecular dynamics simulations. Electrolytes with smaller- sized clusters exhibit a 2-fold improvement in ionic conductivity compared to conventional weakly- solvating electrolytes, enabling stable cycling at high current densities up to 2C (6.2 mA cm -2 ) in anode- free LiNi 0.6 Mn 0.2 Co 0.2 (NMC622)||Cu pouch cells. In conclusion, the efficacy of the design strategy is verified by performance improvements in three disparate weakly solvating electrolyte systems.

25 ENERGY STORAGE↗
DOE OSTI2020

Fluorination and reduction of CaCrO 3 by topochemical methods

Topochemical reactions between CaCrO 3 and polyvinylidene difluoride yield the new fluorinated phase CaCrO 2.5 F 0.5 , which was characterized by powder synchrotron X-ray diffraction, X-ray photoemission spectroscopy, and magnetic susceptibility measurements. The reaction proceeds via reduced oxide intermediates, CaCrO 2.67 and CaCrO 2.5 , in which CrO 6 octahedral and CrO 4 tetrahedral layers are stacked in a different manner along the c axis of CaCrO 3 . These two intermediate phases can be selectively synthesized by the carbothermal reduction with g-C 3 N 4. Both CaCrO 3 and CaCrO 2.5 F 0.5 adopt the same orthorhombic space group, Pbnm ; however, the fluorinated phase has decreased Cr–O–Cr bond angles as compared to the parent compound in both the ab plane and along the c -direction, which indicates an increased orthorhombic distortion due to the fluorination. Overall, while the oxygen vacancies are ordered in both intermediate phases, CaCrO 2.67 and CaCrO 2.5 , a site preference for fluorine in the oxyfluoride phase cannot be confirmed. CaCrO 3 and CaCrO 2.5 F 0.5 undergo antiferromagnetic phase transitions involving spin canting, where the fluorination causes the transition temperature to increase from 90 K to 110 K, as a result of the competition between the increased octahedral tilting and the enhancement of superexchange interactions involving Cr 3+ ions in the CaCrO 2.5 F 0.5 structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Halide segregation to boost all-solid-state lithium-chalcogen batteries

Mixing electroactive materials, solid-state electrolytes, and conductive carbon to fabricate composite electrodes is the most practiced but least understood process in all-solid-state batteries, which strongly dictates interfacial stability and charge transport. Here, we report on universal halide segregation at interfaces across various halogen-containing solid-state electrolytes and a family of high-energy chalcogen cathodes enabled by mechanochemical reaction during ultrahigh-speed mixing. Bulk and interface characterizations by multimodal synchrotron x-ray probes and cryo–transmission electron microscopy show that the in situ segregated lithium halide interfacial layers substantially boost effective ion transport and suppress the volume change of bulk chalcogen cathodes. Various all-solid-state lithium-chalcogen cells demonstrate utilization close to 100% and extraordinary cycling stability at commercial-level areal capacities.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Effect of thermal aging and irradiation on microstructure and crack growth response of Alloy 690

Nickel-base Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs reactors are expected to operate for 40-80 years. Likewise, advanced water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is a potential concern for the long-term performance of both existing and advanced nuclear plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 690 during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni 2 Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 690 under accelerated thermal aging and irradiation conditions. The materials studied involved Alloy 690 from two sources: (i) Alloy 690 plate from an Alloy 152 dissimilar metal weld (DMW) joining the Alloy 690 plate to Alloy 533 LAS, aged at three different temperatures (370°C, 400°C and 450°C) for up to 75,000h (equivalent to 60 years of service), and (ii) specimens neutron-irradiated in the BOR-60 reactor up to 40 dpa. For aged Alloy 690 specimens, hardness was found to increase with aging time, however, the microstructural characterization by means of synchrotron X-ray did not find evidence of LRO. The microstructural characterization of neutron-irradiated specimens by TEM found no evidence of LRO either. Testing in a primary water environment of Alloy 690 specimens aged to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloy. The SCC CGR response was also low. Overall, the two Alloy 690 heats investigated in this work, aged up to 60-year service equivalents or exposed to neutron irradiation up to 40 dpa, did not exhibit a deterioration in microstructure or performance.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗