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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Physical properties of 𝑅⁢ Co 2 ⁢Al 8 single crystals (𝑅 = La, Ce, Pr, Nd, and Sm) : An emerging structure-type for anisotropic Kondo-lattice studies

Systematic investigations of rare-earth (𝑅)-based intermetallic materials are a leading strategy to reveal the underlying mechanisms governing a range of physical phenomena, such as the formation of a Kondo lattice and competing electronic and magnetic anisotropies. Here, in this work, the magnetic, thermal, and transport properties of 𝑅⁢Co 2 ⁢Al 8 (𝑅 = La, Ce, Pr, Nd, and Sm) single crystals are presented. LaCo 2 ⁢Al 8 is characterized as a Pauli paramagnet, and transport measurements, with the current along and perpendicular to the orthorhombic 𝑐-axis (𝜌 𝑐 and 𝜌 𝑎⁢𝑏 , respectively), reveal a clear electronic anisotropy, with 𝜌 𝑎⁢𝑏 ⁢≈ (4 –7)⁢𝜌 𝑐 at 300K . We show that CeCo 2 ⁢Al 8 is a Kondo lattice for which the Kondo coherence temperature 𝑇$^*_K$, deduced from broad maximums in 𝜌 𝑐 and 𝜌 𝑎⁢𝑏 at ≈ 68 and 46 K, respectively, is also anisotropic. This finding is related to a possible underlying anisotropy of the Kondo coupling in CeCo 2⁢ Al 8 . The Pr- and Nd-based materials present strong easy-axis anisotropy (𝑐-axis) and antiferromagnetic (AFM) orders below 𝑇 = 4.84 and 8.1K , respectively. Metamagnetic transitions from this AFM to a spin-polarized paramagnetic phase state are investigated by isothermal magnetization measurements. The Sm-based compound is also an easy-axis AFM with a transition at 𝑇 = 21.6K .

Garcia, Fernando A. [Ames Laboratory (AMES), Ames,↗
DOE OSTI2024

Optimization of Structurally Enhanced Solder Transient Liquid Phase Bonding

High temperature packaging technologies are a necessity for high temperature capable devices. SAC305 solder has an operational limit of 174°C imposed by creep effects which aligns well with current junction temperature limits of 175°C. Wide band gap semiconductor materials have the potential to reach junction temperatures of up to 800°C that are not currently attainable with significant reliability. Capitalizing on this potential will requires substrates and attachments that can operate well beyond the current 175°C standard. Silver sintering pastes have received widespread interest as a high temperature attachment alternative. However, the process requires high pressure bonding in an inert environment to achieve acceptable bond quality. Transient liquid phase (TLP) sintering is capable of good bond quality without pressure requirements but suffers from low thermal conductivity and only slightly reduced cost compared to silver sintering. SAC305 solder contains the same constituent materials for TLP as available copper-tin TLP sintering paste. By introducing engineered surface structures into the bond, intermetallic formation can be accelerated producing a bond similar to TLP sintering but in an ambient environment and for reduced cost. While this process has been demonstrated, it has not yet been optimized. Currently bonds are formed using a 75 μm stencil on substrate surface structures 24 μm tall, covering 19% of the bonding area. The process takes about 4 hours not including the formation of surface structures. Here, this study will center on the effects of stencil thickness and coating methods. Samples will be analyzed by scanning acoustic microscopy, die shear testing and cross sectional scanning acoustic microscopy.

42 ENGINEERING↗
DOE OSTI2020

Activation Energy for Solder Bond Degradation: Thermal Cycling of Field-aged Modules at Multiple Upper Temperatures

The reliability of solder joints in the solar cell metallization-interconnect system influences the lifetime of photovoltaic modules. Two field-aged modules-one with Sn 62 Pb 36 Ag 2 solder at the solder joints (Solarex MSX 60), and the other with the standard Sn 60 Pb 40 solder (Siemens M55)-were subjected to a modified thermal cycling (TC) test of IEC 61215. Three sections in each module were maintained at 85 degrees C, 95 degrees C, and 105 degrees C during the 15-minute high temperature dwell time. Current equivalent to the module short-circuit current was injected through the module when the chamber temperature was above 25 degrees C to simulate regular field operation. This novel approach aims to induce thermomechanical fatigue (TMF) at the solder joints and intermetallic compound (IMC) formation at the metal/solder interfaces. The activation energy (E a ) for solder bond degradation was calculated based on the series resistance (R s ) increase in TC testing rather than power drop to avoid the effect of confounding variables. Module-level R s increase in MSX 60 module after TC800 cycles and in M55 module after TC400 cycles was 1.22% and 183.7%, respectively. The E a determined for the module with 2wt% Ag is 0.24 eV and for that with the standard solder is 0.27 eV. The solder bond degradation seems to have been driven by TMF rather than IMC formation for both modules.

14 SOLAR ENERGY↗
DOE OSTI2020

Control of polymorphism during epitaxial growth of hyperferroelectric candidate LiZnSb on GaSb (111)B

A major challenge for ferroelectric devices is the depolarization field, which competes with and often destroys long-range polar order in the limit of ultrathin films. Recent theoretical predictions suggest a new class of materials, termed hyperferroelectics, that should be robust against the depolarization field and enable ferroelectricity down to the monolayer limit. Here, the authors demonstrate the epitaxial growth of hexagonal LiZnSb, one of the hyperferroelectric candidate materials, by molecular-beam epitaxy on GaSb (111)B substrates. Due to the high volatility of all three atomic species, they find that LiZnSb can be grown in an adsorption-controlled window, using an excess zinc flux. Within this window, the desired polar hexagonal phase is stabilized with respect to a competing cubic polymorph, as revealed by x-ray diffraction and transmission electron microscopy measurements. First-principles calculations show that for moderate amounts of epitaxial strain and moderate concentrations of Li vacancies, the cubic LiZnSb phase is lower in formation energy than the hexagonal phase, but only by a few millielectronvolts per formula unit. Therefore, they suggest that kinetics plays a role in stabilizing the desired hexagonal phase at low temperatures. Their results provide a path toward experimentally demonstrating ferroelectricity and hyperferroelectricity in a new class of ternary intermetallic compounds.

42 ENGINEERING↗
DOE OSTI2022

Preface for the special collection commemorating the career of Pat Thiel

This Special Collection in the Journal of Vacuum Science and Technology A (JVST A) has been compiled to commemorate the career of Professor Patricia (Pat) Thiel as a scientific leader in the international surface science community. Pat passed away in September 2020 due to breast cancer. This Collection includes 26 articles from colleagues, collaborators, and former Thiel group members. The topics overlap Pat’s scientific interests and advances in areas that include chemisorption, reconstruction, and complex formation on metal surfaces; submonolayer nucleation and growth and kinetic roughening of epitaxial thin films; coarsening of surface nanostructures; intercalation; surface phenomena for intermetallics including quasicrystals; and atomic-scale friction. We wish to thank the authors for their contributions towards producing this impressive Special Collection.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2020

A fivefold UO$_2^{2+}$ node is a path to dodecagonal quasicrystal approximants in coordination polymers [plus supplemental information]

Aperiodic formations continue to focus interest in areas ranging from advanced scientific theories to practical everyday applications. Starting from diverse and tightly bonded intermetallic compounds, this world showed an important breakthrough toward the so-called soft systems of meso/macroscale: liquid crystals, thin films, polymers, proteins, etc. This work opens a route for making bulk quasicrystals (QC) in an unprecedented but very common area, with molecular ligands. Since these systems are, to a large extent, transparent, they extend the possible areas of QC application to previously unreachable corners, e.g., photonics. We combined efficient bridging ligands with uranyl pentagonal bonding centers and, unexpectedly, brought the unique attributes of f-element coordination chemistry to an interdisciplinary area of aperiodic formations. Taking advantage of the planar coordination of uranyl ions, we were able to direct the structure expansion solely in two directions with a characteristic snub square tiling, a predicted but previously unobtainable dodecagonal approximant.

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

Review—Meeting Fuel Cell Catalyst Requirements for Heavy-Duty Vehicle Applications

Catalyst requirements for proton exchange membrane (PEM) fuel cells differ by applications. Commercial heavy-duty vehicle (HDV) applications consume more H 2 fuel and demand higher durability than many others and the total cost of ownership (TCO) of the vehicle is largely related to the performance and durability of catalysts. This article is written to bridge the gap between the industrial requirements and academic activity for advanced cathode catalysts with an emphasis on durability. From a materials perspective, the underlying nature of the carbon support, Pt-alloy crystal structure, stability of the alloying element, cathode ionomer volume fraction, and catalyst-ionomer interface play a critical role in improving performance and durability. We provide our perspective on four major approaches, namely, mesoporous carbon supports, ordered PtCo intermetallic alloys, thrifting ionomer volume fraction, and shell-protection strategies that are currently being pursued. While each approach has its merits and demerits, their key developmental needs for future are highlighted.

Ramaswamy, Nagappan (ORCID:0000000234302758)↗
DOE OSTI2022

Improving the damage tolerance of Si 3 N 4 by forming laminate composites with refractory metals

The objective of this research was to demonstrate that the damage tolerance of Si 3 N 4 could be significantly improved by forming laminate composites with refractory metals, providing materials that undergo graceful failure, rather than the fast-fracture mechanism exhibited by monolithic Si 3 N 4 . A damage tolerant Si 3 N 4 could be used as a ring material in an all-ceramic bearing, decreasing the chance for catastrophic failure if the ring is stressed in tension during operation. The technical approach formed a laminate composite material using alternating Si 3 N 4 -metallic layers, with both outer layers being Si 3 N 4 to take advantage of its greater wear resistance, chemical stability, and thermal stability. The metallic layers are designed to arrest any cracks in the outer layers, thus producing a toughened Si 3 N 4 and avoiding the catastrophic failure behavior exhibited by monolithic ceramics. The laminate composites were fabricated using a combination of tape-casting Si 3 N 4 and metals from slurries, as well as metal foils, followed by hot pressing at 1500°C. The metallic materials employed were chromium, titanium, and tantalum. Analysis confirmed that the interfaces were well formed, and the laminates with chromium and titanium formed intermetallic compounds more readily than the composites with tantalum. The Si 3 N 4 -Ta laminates demonstrated crack deflection and bridging behavior during failure and flexural strength of 800–900 MPa. The hardness and elastic modulus of Si 3 N 4 -Ta laminates measured by nanoindentation were similar to those reported in literature. The hardness across the interface of the Si 3 N 4 -Ta composite varied according to the composition of the interface, which displayed a profile indicative of a diffusion bond.

36 MATERIALS SCIENCE↗
DOE OSTI2026

MnRhBi3: A Cleavable Antiferromagnetic Metal

This dataset contains DFT input and output files supporting the theoretical modeling in the associated publication (Chem. Mater. 2024, 36, 11306-11316). The calculations characterize MnRhBi3, an orthorhombic (Cmmm) van der Waals-layered intermetallic compound that cleaves easily between neighboring Bi layers. The dataset is organized into three calculation types: (i) Bulk: Structural relaxations of the periodic MnRhBi3 crystal in antiferromagnetic (AFM) and ferromagnetic (FM) configurations, using the vdW-DF-optB86b functional. These provide the equilibrium lattice constants, magnetic energy differences (AFM is 0.5 meV/f.u. lower than FM), and magnetic moments (4.4 µB/Mn, 0.17 µB/Rh, 0.18 µB/Bi) reported in Table 1 of the main text. (ii) Slab: Same magnetic configurations computed with an 18 Ang vacuum layer introduced between Bi layers, used to calculate the cleavage energy Ec = 0.56 J/m2 (AFM) and 0.57 J/m2 (FM), establishing MnRhBi3 as a van der Waals-layered material comparable to graphite, MoS2, and CrI3. (iii) ELF: Single-point calculation on the relaxed bulk AFM geometry with LELF=.TRUE., producing the ELFCAR file used to generate electron localization function isosurfaces and contour maps (Fig. 2, main text) showing Bi lone pairs directed into the van der Waals gaps. All folders contain CONTCAR, INCAR, KPOINTS, OUTCAR, and POSCAR. The ELF/ folder additionally contains ELFCAR. Calculations were performed using VASP 6.3.2 with PBE + vdW-DF-optB86b, PAW potentials, and an energy cutoff of 800 eV.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Additive manufacturing of high-strength multiphase nanostructures in the binary Ni–Nb system for the discovery of new types of superalloys

Abstract Ni-based superalloys have been studied extensively due to their impressive mechanical properties, including strength and creep resistance at high temperatures. Growing interest surrounding additive manufacturing (AM) methods has led to recent investigations of alloys that are traditionally difficult to process, including Ni-based superalloys. Recent work has shown that AM methods enable high-throughput materials discovery and optimization of difficult- or impractical-to-process alloys, including those with high or even majority refractory element compositions. This work focuses on AM-enabled investigations of composition-dependent mechanical and microstructural properties for Ni–Nb binary alloys. Specifically, we report on the mechanical behavior of compositionally-graded Ni x Nb 1− x and uniform composition Ni 59.5 Nb 40.5 specimens made with AM. The AM fabrication process resulted in extraordinarily high strength, attributed to the formation of a dual-phase microstructure consisting of δ-Ni 3 Nb and µ-Ni 6 Nb 7 intermetallic compounds with nanostructured and multimodal grain size and eutectic lamellar spacing. Graphic Abstract

Jones, M. R.↗
DOE OSTI2025

CALPHAD-based Bayesian optimization to accelerate alloy discovery for high-temperature applications

Two crucial properties influencing the performance of high-temperature alloys are coefficient of thermal expansion (CTE) and phase constitution. It is desirable to have alloys with low CTE, which reduces CTE mismatch with the surface oxide and the likelihood of oxide spallation. Reducing the amount of brittle intermetallic phases such as Sigma (σ) enhances alloy ductility and processability. Here, we propose a multi-objective Bayesian Optimization (BO) model to simultaneously minimize CTE (at an operational temperature of 1150 °C) and T σ (temperature when the Sigma phase completely dissolves in the metal matrix), properties which are obtained from high-throughput CALculation of PHAse Diagrams (CALPHAD). The model successfully identifies several alloys with CTE ≤ 2 × 10 –5 /K and T σ ≤ 500 °C by exploring just 7% of the nickel–chromium–cobalt–aluminum–iron (Ni–Cr–Co–Al–Fe) composition space. Such multi-objective alloy design frameworks can be used to inform additive manufacturing experiments and accelerate alloy discovery for high-temperature energy applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Diffusion bonding of tungsten-vanadium-zirconium using vacuum hot pressing for the development of a low decay heat cladding solution for tungsten spallation targets

Tantalum has been used as cladding material for water-cooled solid tungsten targets at many leading spallation neutron production facilities thanks to its high neutron yield, manageable radiation damage behavior, and excellent corrosion/erosion resistance in radiation environments. However, from a safety hazard perspective, thermal neutron capture of tantalum in spallation environments causes a high specific decay heat in the target volume, which often becomes a limiting factor in increasing the beam power on the target. In this paper, we studied vacuum hot pressing (VHP) parameters to diffusion bond zirconium to tungsten to explore the feasibility of using zirconium alloys as an alternative cladding material to tantalum. Zirconium alloys have long been used as cladding material for early generation solid spallation targets, and nuclear fuel rods. In spallation environments zirconium has significantly lower decay heat with shorter decay time compared to tantalum. The hot isostatic pressing (HIP) of zirconium and tungsten is known to produce limited bonding quality due to the formation of the brittle ZrW2 intermetallic layer. To overcome this problem, placing a vanadium interlayer between tungsten and zirconium has been proposed by exploring parameter space in binary alloy phase diagrams. Under the VHP conditions, 860 ◦C at 70 MPa for 4 hours, Zr-V and V-W showed good diffusion bonding, which demonstrates the feasibility of a single step HIP process to make the zirconium alloy clad tungsten spallation volumes.

Lee, Yong Joong↗
DOE OSTI2020

Tribological Behavior of Structural Materials in High Temperature Helium Gas-Cooled Reactor Environments

The High-Temperature Gas-cooled Reactor (HTGR) is a Generation IV concept designed to produce electricity and hydrogen at high efficiencies via high operating temperatures (700 °C or higher). Helium, the primary coolant for HTGRs, contains impurities (e.g., CO, H2O and CH4) that can induce corrosion reactions at high temperatures such as oxidation and (de)carburization, which in turn can affect the tribological behavior of components. Incoloy® 800HT (Ni-Fe-Cr austenitic solid-solution alloy) and Inconel® 617 (Ni-Cr-Co-Mo solid-solution alloy) are two high-temperature superalloys currently selected as candidate structural materials for the HTGR. The objective of this study is to evaluate the high-temperature tribological performance of these two candidate alloys after conditioning them in HTGR environments. Four regimes of corrosion were considered: a non-conditioned regime (Regime I), an oxidizing regime (Regime II), a carburizing and oxidizing regime (Regime III), and a carburizing regime (Regime IV). To simulate oxidation in HTGR, samples were conditioned for 22 days at elevated temperatures in a once-through helium loop with 4 ppmv H2O. Carburization of the samples was achieved by the commercial process, Kolsterising®. In addition, two surface treatments – shot peening and aluminization – were considered as potential routes of improving the alloys’ wear resistance. Surface-treated samples were tested both before and after conditioning in Regime II. Tribological testing of the samples was performed via a pin-on-disk tribometer at elevated temperatures in ambient environment – 650 and 750°C for 800HT; 850 and 900°C for 617 – with applied loads of 1N, 2N and 5N. The wear behavior of the alloys was assessed via wear volume and friction coefficient measurements, supported by morphological, structural and compositional analyses of the wear tracks. Conditioning the samples in Regime II led to the formation of a chromium oxide on both alloys. This protective scale increased the wear resistance compared to that of as-received samples (Regime I) due to the formation of a compacted ‘glaze’ oxide layer during sliding, rendering the wear track nearly undistinguishable from the unworn background and resulting in wear volumes below the detection limits of the measurement technique. The variability of the friction coefficients of the conditioned samples was also considerably reduced compared to that of the as-received samples due to the glaze layer. Additionally, the initial friction coefficients of the samples conditioned in Regime II were reduced by 45% and 54% compared to those of as-received samples for alloys 800HT and 617, respectively. Carburizing the samples (Regime IV) hardened the surfaces of both alloys and promoted the formation of an iron oxide on 800HT during tribological testing, thereby increasing the wear resistance and decreasing the initial friction coefficient by a factor of two compared to those of as-received 800HT. Alloy 617 exhibited an enhanced wear resistance but similar initial friction coefficient compared to those of as-received samples due to the increased surface hardness. The Mn-Cr oxide developed during Regime III conditioning of 800HT did not develop a glaze layer during tribotesting, even at lower loads. Thus, it was not as protective as the oxide produced during conditioning of Regime II samples, leading to lower wear resistance of 800HT in Regime III compared to that measured in the Regime II condition. 800HT benefited from the aluminization surface treatment, particularly before conditioning in Regime II, due to the promotion of a wear-resistant aluminum oxide layer during testing and the increase in surface hardness due to the presence of a FeAl intermetallic phase. The presence of this phase caused an order-of-magnitude reduction in wear volumes compared to those of as-received 800HT. Aluminization of 617 decreased its wear resistance, particularly after conditioning in Regime II, due to significant wear of the aluminum oxide via a ceramic wear mechanism. This aluminum oxide was removed during sliding, causing the wear volumes to increase by a factor of five compared to those of 617 conditioned in Regime II. Shot-peened 800HT exhibited a tribological behavior similar to that of as-received 800HT, despite an enhancement in the rate of chromium oxide formation. Shot-peened 800HT conditioned in Regime II showed lower wear resistance compared to that of 800HT conditioned in Regime II due to the poor adhesion between the oxide and the underlying metal, preventing the formation of the glaze layer during sliding. Shot peening of 617 increased its wear resistance at higher load, reducing worn volumes by 60% compared to that measured with as-received 617. Tribotesting of shot-peened 617 in Regime II revealed that the glaze-oxide layer was formed at every load, resulting in negligible wear, similar to what was observed from testing 617 after conditioning in Regime II. Overall, alloy 617 exhibited tribologically superior behavior compared to that of alloy 800HT, as demonstrated by its lower friction coefficients and its order-of-magnitude lower wear volumes when measurable.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Highly-Accessible Catalysts for Durable High-Power Performance (Final Technical Report)

Reduction of costly Pt usage in proton exchange membrane fuel cell (PEMFC) electrodes is one of the major challenges towards development and commercialization of fuel cell electric vehicles (FCEV). However, reducing the Pt loading results in increasing local mass transport fluxes, and eventual performance loss, especially at high power. In this project, a team of 4 universities, 2 companies, and a national lab came together to develop fuel cell catalysts and electrodes with high performance and durability. The were several key concepts addressed in this project. The first concept is to develop a carbon support that possess internal porosity which are believed to enhance kinetic activity of the catalysts, and yet the pore morphology allows for good reactant transport. The second concept is to improve the Pt-electrolyte interface in hope to reduce the local transport resistance. This was done by using new ionomers and ionic liquids. The last concept involves improving the catalyst stability by introducing Pt alloy catalyst with ordered intermetallic phase. The collaborative platform provided by DOE funding enabled development of a highly active and durable catalyst with performance that exceeds previous catalysts and meets the DOE targets for light duty vehicle application.

08 HYDROGEN↗
DOE OSTI2020

Production of Radiohalogens: Bromine and Astatine for Imaging and Therapy

Over the course of this two year grant, we have developed and optimized new methods for the production of clinical quality 76 Br, 77 Br, and 80m Br at the University of Wisconsin. This includes the synthesis of a novel isotopically enriched cobalt-selenium intermetallic compound, its fabrication into robust cyclotron targets, and the chemical isolation of the resulting bromine radionuclide. Compared with the previous state-of-the-art, these methods demonstrate a six-times larger 76 Br and three-times larger 77 Br production capacity for a 3-hour cyclotron irradiation. Additionally, the cyclotron targets are exceptionally robust to this process, allowing for their reuse for dozens of radiobromine productions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2021

High Speed Hybrid Reluctance Motor Utilizing Anisotropic Materials

With high cost and volatility driving continued efforts to decrease reliance on the critical heavy rare earth materials used in traction drive applications, General Motors developed three variants of heavy rare earth-free (HRE-free) electric motors. The variants focused on taking advantage of advanced magnet technologies and new rotor topologies to improve mechanical strength and achieve power targets. The three variants were a HRE-free permanent magnet reluctance motor, a synchronous reluctance motor utilizing small HRE-free permanent magnets, and an induction motor with inserted copper bars and cast aluminum end-rings. Motors were designed with the intent of primary or secondary traction applications, depending on the topology. Variant 1 achieved performance comparable to HRE-containing permanent magnet motors through optimized topology and validation of HRE-free magnets, focusing on achieving energy products and demagnetization resistance comparable to those of HRE-containing magnets. Demagnetization testing demonstrated the motor robustness to currents and temperatures exceeding expected vehicle conditions, a key challenge to the use of HRE-free magnets. The Variant 1 motor also showed the best capability of meeting the US Drive technology 2020 targets, due to the high power-density of the permanent magnet motor and the potential cost reductions enabled by the removal of heavy rare earth materials. Variant 2 exhibited high efficiency in high speed regions due to the low high-speed losses, an important consideration for secondary traction applications, and significantly thrifted on magnet mass to reduce cost. Variant 3 contained copper bars within the induction rotor to reduce losses compared to cast aluminum, while using cast aluminum end-rings to reduce the cost and mass of the rotor. Optimization of the Cu-Al interface were focused on, as the interface is prone to forming brittle intermetallic compounds during the casting process. Prototypes of each motor variant were built and tested for performance, mechanical strength, and demagnetization resistance (Variants 1 and 2 only), with torque and power resulting close to the predicted values.

33 ADVANCED PROPULSION SYSTEMS↗
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↗
DOE OSTI2021

Intentional Uranium Tagging for Material Provenance and Pathway Forensics (LA19-Intentional-Forensics-NDD3Bb) (Annual Report for FY21)

This report describes the outcomes of the third and final year of a project to research the feasibility of tagging uranium materials, especially nuclear fuels. The experimental focus remained on metallic uranium forms under prospective surface and bulk tagging scenarios. Overall, the results showed that the tags could be successfully imparted and characterized in both as-built and degraded conditions. This was in line with expectations coming into this project, indicating promise for both surface and bulk tagging of metallic forms of uranium. Multiple surface tagging techniques and detection strategies were explored in FY21, with an emphasis on improving tag quality, readability, and detection in the field. Non-radioactive materials were used as a testbed. Selective deposition via laser beam was determined to be successful in imparting a readable titanium deposit on a stainless steel base plate, and can be read with high resolution characterization techniques (e.g., scanning electron microscopy) and field capable tools (e.g., eddy current testing). Other deposition techniques, such as selective deposition via electron beam and photoluminescent tags, were explored in FY21, and while success for these techniques would be dependent on additional work, these techniques showed potential for surface tagging applications. To survey bulk taggant elements for bulk uranium metal, 16 tagging elements were spread among 18 depleted uranium castings (4 baseline, 3 mix, 1 dilution, and 10 recycle). Most of these were made and characterized in FY21. Taggant acceptability was based upon manufacturability, detectability, and persistence from the standpoint of two detection options: bulk chemical analysis (for “chemical taggants”) and microstructural analysis (for “second phase taggants”). Taggant detection in both up-front manufacturing and in the face of “degradations” such as dilution, mixing, and recycling was generally good. Two independent laboratories carried out chemical analysis on most of the castings, and often at several locations within a casting, and the results are discussed. Scanning electron microscopy+EDS microanalysis revealed the second phases mostly contained the expected tagging elements. The shapes and 2 spatial distributions of these micron-sized carbides, oxides, and intermetallic particles offers opportunities for further science-based investigation and tagging optimization. Overall, V and Co currently appear as the best choices for chemical taggants while Al, Ti, Mn, Co, Pd, and Tb all look good as second phase taggants. The other elements considered here – Sc, Ni, Ge, Nb, Ce, Ta, W, Ir, and Au – while not being ruled out, require more study to become viable options. It is of special note that in the recycling study only one of the 12 elements fell out of detection even after 10 meltings, demonstrating their persistence. An Appendix tabulates all chemical analysis results to enable more quantitative and statistical studies of detection opportunities and limitations, as a part of a related project.

36 MATERIALS SCIENCE↗