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At least 847 records · Page 47
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

A crystal plasticity finite element model embedding strain-rate sensitivities inherent to deformation mechanisms: Application to alloy AZ31

We report the fundamental power-law relationship representing the flow rule in crystal visco-plasticity ensures uniqueness in the selection of slip systems accommodating imposed plastic strain-rates. The power-law relationship also introduces an artificially high strain-rate sensitivity in crystal plasticity simulations, unless a high value of the power-law exponent is used. However, the use of high values for the exponent is limited by numerical tractability. This paper presents a numerical method implemented in a crystal plasticity finite element (CPFE) model for embedding any value of the power-law exponent reflecting the true material strain-rate sensitivity. Importantly, the method does not increase computation time involved in the simulations. The enhanced CPFE model is used to interpret and predict a complex strain-rate sensitive response and microstructural evolution of AZ31 Mg alloy. Measured values of strain-rate sensitivity for slip and twinning modes are used in the simulations. Calculations show that the model successfully captures the phenomena pertaining to the effect of changing applied strain-rate on the mechanical response including flow stress and evolution of texture and twinning for a broad range of strain-rates ranging from 10 -3 s -1 to 10 3 s -1 and loading orientations in tension and compression. It is shown that such predictions are a consequence of not only relative amounts of slip and twinning activities driven by a set of accurately characterized hardening law parameters but also values of the strain-rate sensitivities inherent to individual deformation mechanisms. Besides, the model validates the measured strain-rate dependency of deformation mechanisms while accurately reproducing the mechanical data. Hence, the model can be used to verify and further refine or infer measured strain-rate sensitivity per deformation mechanism by reproducing experimental data.

36 MATERIALS SCIENCE↗
DOE OSTI2018

High- and Low-Temperature Deformation Behavior of Different Orientation Hot-Rolled Annealed Zircaloy-4

In this paper, the hot-rolled annealed Zircaloy-4 samples with different orientation were subjected to uniaxial compression with a strain rate of 0.001 s{sup −1} to obtain the stress-strain curves of different initial orientation samples at different temperatures. Electron backscatter diffraction (EBSD) technique and transmission electron microscope (TEM) technique were used to analyze the microstructures and textures of compressed samples. The mechanical properties and microstructural evolution of rolling directions (RD), transverse directions (TD) and normal directions (ND) were investigated under the conditions of – 150 °C low temperature, room temperature and 200 °C high temperature (simulated lunar temperature environment). The results show that the strength of Zircaloy-4 decreases with the increase in deformation temperature, and the strength in three orientations is ND > TD > RD. The deformation mechanism of hot-rolled annealed Zircaloy-4 with different orientation is different. In RD, {101̄0}〈a〉 prismatic slip has the highest Schmid factor (SF), so it is most easy to activate the slip, followed by TD orientation, and ND orientation is the most difficult to activate. The deformed grains abide slip→twinning→slip rule, and the different orientation Zircaloy-4 deformation mechanisms mainly are the twinning coordinated with the slip.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure and Deformation Mechanism of AZ31 Magnesium Alloy Under Dynamic Strain Rate

A hot-rolled AZ31Mg alloy sheet was subjected to dynamic plastic deformation parallel to the rolling direction, and microstructural evolutions and mechanical properties of the deformed samples were examined. It has been found that dynamic strain rate could facilitate {10-12} twin nucleation and growth and leads to a lower yield stress of about 20 MPa and an early end to twinning characteristic (happening at a strain point of about 6%) shown in the stress–strain curve. {10-12} twinning mechanism dominates the early plastic deformation; but when plastic strain exceeds ~ 9%, dislocation–slip mechanism instead of {10-12} twinning dominates the later plastic deformation. And this premature transformation of the dominant deformation mechanisms from {10-12} twinning to dislocation slip is caused by dynamic strain rate. The effect of dynamic strain rate on the number of twin nucleations remains unclear, and the more systematic researches are needed in the future.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of short-range order on microstructure, texture and strain hardening of cold drawn Cu-10 at.%Mn alloy

Highlights: • Excluding the effect of stacking fault energy, short-range order effect is discussed solely. • Short-range order is beneficial for twinning and slip planarity. • Short-range order promotes the formation of <111> fiber texture. • Strain hardening improving by short-range order. - Abstract: The aim of the present study is to investigate the effect of short-range order (SRO) on the microstructural evolution and mechanical property of Cu-10 at.%Mn alloy during cold drawing deformation. Characterization of the cold drawn Cu-10 at.%Mn alloy samples were performed using transmission electron microscope (TEM) and electron back scattering diffraction (EBSD), and their hardness were also tested. The results show that SRO is beneficial for both twinning and the transition of dislocation glide from wavy slip to planar slip at the low strains. At the high strains, the wavy slip generates due to the destruction of SRO. SRO increases the volume fraction of <111> texture component and the critical strain threshold. Moreover, the presence of SRO significantly improves strain hardening by combining the effects of dislocation, deformation twinning and texture hardening, which results in a significant increase of hardness.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Interfacial microstructure and mechanical properties of rotary inertia friction welded dissimilar 422 martensitic stainless steel to 4140 low alloy steel joints

In this work, dissimilar rotary inertia friction welds between 422 martensitic stainless steel and 4140 martensitic low-alloy steel were made to fabricate prototype heavy-duty diesel engine pistons. The influence of the inertia friction welding process and post weld heat treatment (PWHT) temperature on the interfacial microstructure evolutions and corresponding effects on mechanical properties of the 422/4140 welds were evaluated in detail. Carbon diffused from the 4140 side to the 422 side during PWHT at 650 °C for 1.5 h, causing the formation of a hard carbide-rich layer on the 422 side, and a softer but discontinuous C-depleted layer the 4140 side. PWHT at 700 °C for 1.5 h greatly accelerated C diffusion across the interface relative to 650 °C, resulting in a thicker hard carbide-rich layer and a relatively thick and continuous layer of coarse C-depleted grains (ferrite) on the 4140 side. In addition, the PWHT temperature greatly influenced the tensile properties and fracture behavior of the welds, with the 650 °C PWHT-ed samples failing predominately in a ductile manner in the 4140 heat affected zone during tensile testing. Conversely, the 700 °C PWHT specimens exhibited a strength reduction compared with the 650 °C PWHT specimens because of additional coarsening of the interfacial ferrite layer and softening of the base materials during PWHT, with brittle fracture between the hard and soft layers the predominate failure mechanism. Based on the findings, a reduced PWHT temperature and/or time, minimizing the hardness differential of the base metals, and pre-heating the 422 steel prior to welding are the potential pathways to achieve a more optimal balance between desirable tempering and stress relief of the weld microstructure and undesirable C migration across the weld interface, and to reduce the strength mismatch across the weld.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Interface-correlated bonding properties for a roll-bonded Ti/Al 2-ply sheet

Highlights: • The feasible post roll-bonding annealing condition of Ti/Al clad was deduced. • The optimum thickness of the TiAl{sub 3} IMC diffusive layer is about 200 nm. • A ‘zipper-like’ failure mode at the interface yields the maximum bonding strength. - Abstract: We investigated the influence of annealing conditions on the interface-correlated microstructural evolution and subsequent bonding properties of a warm roll-bonded Ti/Al clad sheet. A TiAl{sub 3} intermetallic compound layer with a thickness of 160 nm was initially generated at the joint interface between the Ti and Al alloys by warm rolling. When the annealing time and temperature were increased to a maximum of 6 h and 650 °C, respectively, the thickness of the TiAl{sub 3} layer increased to 320 nm. The feasible annealing conditions for the optimum bonding strength were within 550 °C-6 h and 600 °C-3 h. An improvement in the bonding strength between Ti and Al is strongly correlated with the generation of considerable metallurgical bonding. This is manifested in the zipper-like failure mode that occurs at the TiAl{sub 3} joint interface for a layer thickness of less than 300 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Decarburization and Carburization Behavior of Grade 91 Steel in Sodium Environments

Two heats of G91 steel have been investigated in sodium at 550-650°C to understand its corrosion behaviour, microstructural evolution, and tensile properties. Sodium exposure tests of subsized tensile and coupon specimens of G91 base metal and weldment were conducted in Argonne’s forced convection sodium materials testing loops. Maximum exposure times of ~39,000 h at 550°C, ~37,000 h at 600°C, and ~20,000 h at 650°C have been achieved, respectively. Thermal aging experiments of G91 steel were conducted in parallel, and the data of the sodium-exposed specimens were compared with the thermal aging data of the same heat to isolate the thermal aging effect from the effect of sodium exposure. It was found that the tensile strength of G91 steel can be reduced by more than 50% after sodium exposures at 650°C. The effect of a sodium environment on tensile properties is largely dependent on the carburization/decarburization behavior of G91 steel exposed to sodium. The carbon concentrations in sodium in Argonne’s SMT-1 and SMT-2 loops were determined by the equilibration method. The carbon activity in sodium was established by equilibrating high-purity nickel in sodium, analyzing the material for carbon, and using the reported data on the carbon solubility for this material. The carbon activity results were combined with the carbon solubility data in sodium to establish the carbon concentration in sodium. The carbon concentrations in the SMT-1 and SMT-2 loop were estimated to be 1.23 and 0.25 ppm, respectively. With this initial success, we will continue to monitor the carbon contents in the two loops to correlate the microstructural and mechanical property changes with the sodium purity. Future experiments will also consider sodium exposure tests in controlled carbon activities. Online monitoring and control of carbon contents in sodium in nuclear reactors would also be of interest. Thermodynamic analysis was conducted to understand the carburization-decarburization behavior of G91 steel exposed to sodium in the SMT-1 and SMT-2 loops. The equilibrium carbon activity in the alloy was evaluated by the thermodynamics of M 23 C 6 carbides. The calculated carburization-decarburization boundary showed that G91 would undergo decarburization at 650°C in the SMT-1 loop and carburization at 600°C in the SMT-2 loop, which is consistent with our findings from the sodium exposure tests. Future work will include thermodynamic analysis of the carbon concentration – activity relationship including the effect of carbide-forming elements, vanadium and niobium in G91 steel. Kinetics of carbon diffusion and the effect on microstructure and mechanical performance under various service conditions will also be investigated. The ultimate goal is to understand the mechanisms and the kinetics of carbon transfer in the sodium-steel system and to provide a basis for predicting the effect of long-term decarburization-carburization process on the integrity of reactor components.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2018

Quantitative Comparison of Ternary Eutectic Phase-Field Simulations with Analytical 3D Jackson–Hunt Approaches

For the analytical description of the relationship between undercoolings, lamellar spacings and growth velocities during the directional solidification of ternary eutectics in 2D and 3D, different extensions based on the theory of Jackson and Hunt are reported in the literature. Besides analytical approaches, the phase-field method has been established to study the spatially complex microstructure evolution during the solidification of eutectic alloys. The understanding of the fundamental mechanisms controlling the morphology development in multiphase, multicomponent systems is of high interest. For this purpose, a comparison is made between the analytical extensions and three-dimensional phase-field simulations of directional solidification in an ideal ternary eutectic system. Based on the observed accordance in two-dimensional validation cases, the experimentally reported, inherently three-dimensional chain-like pattern is investigated in extensive simulation studies. The results are quantitatively compared with the analytical results reported in the literature, and with a newly derived approach which uses equal undercoolings. A good accordance of the undercooling–spacing characteristics between simulations and the analytical Jackson–Hunt apporaches are found. The results show that the applied phase-field model, which is based on the Grand potential approach, is able to describe the analytically predicted relationship between the undercooling and the lamellar arrangements during the directional solidification of a ternary eutectic system in 3D.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Characterization of the microstructure of yttrium hydride under proton irradiation

High moderation per unit volume solid moderator materials like yttrium hydride (YH x ) are necessary for compact nuclear microreactors. However, the phase stability and hydrogen transport processes of YH x under high-temperature irradiation are largely unknown. Proton irradiation was conducted on YH x at 300 °C and 580 °C to 0.2 dpa using 1 MeV or 2 MeV protons in a high-vacuum environment. The hydrogen concentration was determined before and after irradiation using elastic recoil detection analysis, and microstructural evolution was examined via post-irradiation scanning transmission electron microscopy and Raman spectroscopy. Dislocation loops and cavities were observed in all conditions; their distribution was correlated with the bombarding proton energy and ion irradiation temperature. This work revealed that hydrogen retention is proportional to the formation of traps for hydrogen gas atoms and identified pathways for hydrogen release. The relative contributions of bulk or fast diffusion paths, such as grain boundaries, delamination boundaries, and stacking faults are discussed; the primary mechanisms of hydrogen loss are likely based on diffusion, ruling out artefacts of the experimental design. In conclusion, the study suggests proton irradiation may be a strong surrogate to study hydrogen transport in hydride moderator materials under irradiation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Microstructure modeling of nuclear structural materials: Recent progress and future directions

Modeling and simulation of microstructures are essential to understand the complex responses and behaviors of nuclear materials in extreme environments. The needs to assess the extended life operation as well as the growing interest in accelerating nuclear materials development and qualification have stimulated the use of high-fidelity multiscale models aided by empirical and ab initio data. This paper reviews the role of various models across different length and time scales in investigating irradiation effects on microstructure evolution and degradation, in particular the embrittlement caused by radiation induced or enhanced formation of nanoscale chemical heterogeneities. The strength and limitations of these models, including classical rate theories, cluster dynamics, phase-field methods, and atomistic models informed by ab initio energies, are discussed with seminal examples. Challenges regarding the lack of thermo-kinetic data and theoretical treatments considering chemical complexities and magnetic excitations, as well as the stabilizing effect by excess point defects in nuclear structural materials are presented, along with potential solutions based on ab initio informed surrogate energy models and statistical sampling by Monte Carlo simulations. Further, the review then highlights the opportunities to leverage the advantages of different methods by establishing hybrid models by shared variables or coupled codes and applications. Finally, the review concludes with forward-looking remarks on how the use of physics-based models can aid the improvement of machine-learning models of property degradation and vice versa.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effects of Bi-Sb Addition and Solution Treatment on Microstructures and Mechanical Properties of Al-20 wt.% Mg{sub 2}Si Composites

In this study, the effects of compound modification with Bi and Sb and solution treatment on the microstructures evolution and the mechanical properties of Al-20 wt.% Mg{sub 2}Si composites were investigated. The specimens were observed by optical microscope, scanning electron microscope equipped with an energy-dispersive spectrometer and x-ray diffraction. The characterization results showed that 2.0 wt.% Sb and 0.2 wt.% Bi addition refined the primary Mg{sub 2}Si from 95 to 10 μm, accompanied by a change in morphology from coarse dendrites to dispersive fine polygons. After solution treatment at 540 °C for 15 h, the sharp polygonal primary Mg{sub 2}Si particles were blunted and the flake-like eutectic Mg{sub 2}Si phases were changed to small spherical particles, resulting in the increase in the Brinell hardness of the composites from HB 94.53 to 134.67. Mechanical tests revealed that both tensile strength and hardness of the composite were improved by compound modification with Bi and Sb, and the ultimate tensile strength (UTS) was increased from 216 MPa unmodified to 257 MPa with optimum modification of 2 wt.% Sb and 0.2 wt.% Bi. A propounded change in hardness from HB 94.53 to 130.67 was also investigated.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Bismuth borate zinc glass braze for bonding sapphire in air

Highlights: • Sapphire was brazed with a novel 50Bi{sub 2}O{sub 3}–40B{sub 2}O{sub 3}–10ZnO (mol.%) glass at temperatures of 600–700 °C for 20 min in air. • Bi{sub 4}B{sub 2}O{sub 9} and Bi{sub 24}B{sub 2}O{sub 39} were formed in the joints brazed at 600 and 625 °C, respectively. • ZnAl{sub 2}O{sub 4} particles were formed in the joints when the brazing temperature was 635 °C. • The maximum shear strength of 85 MPa was obtained for the joints brazed at 650 °C for 20 min. - Abstract: Reliable brazing of sapphire was successfully achieved by using a novel 50Bi{sub 2}O{sub 3}–40B{sub 2}O{sub 3}–10ZnO (mol%) glass braze and joining cycles that peak at temperatures of 600 − 700 °C for 20 min in air. The effect of the brazing temperature on microstructure evolution as well as mechanical properties of the sapphire/sapphire joints was investigated. The results showed that Bi{sub 4}B{sub 2}O{sub 9} and Bi{sub 24}B{sub 2}O{sub 39} were formed in the joints brazed at 600 and 625 °C, respectively. ZnAl{sub 2}O{sub 4} particles were formed in the joints when the brazing temperature was 635 °C due to a reaction between the glass and the sapphire substrate. With the brazing temperature increasing, ZnAl{sub 2}O{sub 4} particles exhibited steady growth, from ~ 160 nm at 635 °C to ~ 455 nm at 700 °C. Besides, ZnAl{sub 2}O{sub 4} particles began to aggregate when the temperature was 675 °C. The strength increased sharply when the brazing temperature increased to 635 °C, which was mainly attributed to the formation of ZnAl{sub 2}O{sub 4} particles in the joint domain. The maximum shear strength of 85 MPa was obtained for the joints brazed at 650 °C for 20 min. The joint shear strength decreased due to the aggregation of ZnAl{sub 2}O{sub 4} particles in the joint.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Vibro-acoustic Testing for Microstructure Characterization and Metrology: Technology Commercialization Fund—Fiscal Year 2017

There is a need in nuclear reactors to inspect irradiated materials and structures. A portable scanning infrastructure for a material characterization technique called vibro acoustography (VA) is being developed by the Idaho National laboratory for nuclear applications to characterize fuel, cladding materials, and structures. The proposed VA technology is based on ultrasound and acoustic waves; however, it provides information beyond what is available from the traditional ultrasound techniques and can expand the knowledge on nuclear material characterization and microstructure evolution. VA technique has several advantages over traditional characterization techniques. VA is a non-contact submersion technique that is inherently wireless transmission and reception (from the ultrasonic transmitter to the acoustic receiver). The transmission medium can be most liquids used for reactor cooling such as water and sodium. For nuclear in-pile applications, the Ultrasonic Transducer (UT) will need to have a line of sight location that is within lower radiation flux zones. Multiple UT sources can be frequency multiplexed to allow a single hydrophone receiver to monitor several locations. The reactor structure can also be an integral part of the transmission system acting as waveguides to deliver the acoustic signal to an acoustic receiver. Because of the long wavelength of the acoustic signal, the acoustic receiver does not have to be line of sight with respect to the component under test. The focusing and generation of the acoustic beat frequency from two ultrasonic waves allows for the potential to ultrasonically image complex shapes. These features will significantly reduce experiment complexity, installation times and cost while being safe and easy to use.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Research on Resistance Heating Behavior of High-Strength Steel and its Hot-Stamping Forming

A hot-stamping process of high-strength steel sheet using resistance heating (RH) was developed to improve springback and formability. The RH curves of S355J2W steel and the microstructure and mechanical properties after RH were explored to control and guide the RH time and the selected current density for the subsequent RH hot-stamping forming. Moreover, scanning electron microscopy observations revealed the microstructure evolution in RH and the improvement of mechanical properties at a current density of 0-6.67 A mm{sup −2}, showing the advantage of the application of RH to these materials. The results showed that steel strength can be increased by up to 3.2% and the elongation can be improved by up to 33% after RH. In addition, the forming height increased and the forming angle is closer to the desired angle with the increased current density in cap-shaped RH hot-stamping forming experiment, which means that the forming accuracy is improved. A comparison of the forming accuracy of cap-shaped parts formed by RH under different current densities with those heated to the same temperature by furnace heating (FH) shows that there is no obvious difference between them. The heating time of RH is much shorter than that of the FH, and the surface quality of the parts formed by RH hot-stamping is better than that of the parts formed by FH hot-stamping. These results demonstrate that the RH method has the advantages of efficiency, safety, energy saving and the improvement of surface quality as well as a clear understanding of the benefits of RH hot-stamping forming for materials properties and forming accuracy; this work also develops and applies fundamental theory to practical engineering of bogie cover plate manufacturing.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Selective laser melting of 304L stainless steel: Role of volumetric energy density on the microstructure, texture and mechanical properties

The role of volumetric energy density on the microstructural evolution, texture and mechanical properties of 304L stainless steel parts additively manufactured via selective laser melting process is investigated. 304L is chosen because it is a potential candidate to be used as a matrix in a metal matrix composite with nanoparticles dispersion for energy and high temperature applications. The highest relative density of 99 %±0.5 was achieved using a volumetric energy density of 1400 J/mm 3 . Both XRD analysis and Scheil simulation revealed the presence of a small trace of the delta ferrite phase, due to rapid solidification within the austenitic matrix of 304L. Here, a fine cellular substructure ranged between 0.4–1.8 μm, was detected across different energy density values. At the highest energy density value, a strong texture in the direction of [100] was identified. At lower energy density values, multicomponent texture was found due to high nucleation rate and the existing defects. Yield strength, ultimate tensile strength, and microhardness of samples with a relative density of 99 % were measured to be 540 ± 15 MPa, 660 ± 20 MPa and 254 ± 7 HV, respectively and higher than mechanical properties of conventionally manufactured 304L stainless steel. Heat treatment of the laser melted 304L at 1200 °C for 2 h, resulted in the nucleation of recrystallized equiaxed grains followed by a decrease in microhardness value from 233 ± 3 HV to 208 ± 8 HV due to disappearance of cellular substructure.

304L stainless steel↗
DOE OSTI2018

Effect of Cooling Rate on Microsegregation During Solidification of Superalloy INCONEL 718 Under Slow-Cooled Conditions

The solidification sequence, microstructural evolution, solid-liquid interface variation, interdendritic segregation, and elemental distribution of as-cast IN718 alloy at three slow-cooling rates (5, 10, and 20 °C/min) were investigated by differential scanning calorimetry (DSC), confocal laser scanning microscopy (CLSM), optical microscopy (OM), field-emission scanning electron microscopy (FESEM), and electron-probe microanalysis (EPMA) techniques. The results indicate that as the cooling rate decreases, the constitutional supercooling at the solidification front affects the solid-liquid interface more significantly, and the size and quantity of the Laves phase increase. However, the composition of the Laves phase is insensitive to the cooling rate in the range of conditions studied here. In dendrite core, the contents of Ni, Cr, Fe, and Al follow a slight downward trend with an increasing cooling rate, whereas the Nb, Mo, and Ti contents show an upward trend. Additionally, Mo shows a stronger propensity to segregate under slow-cooling conditions because its effective partition coefficient almost linearly decreased with decreasing cooling rate, which is same as Nb. Using the parameters experimentally determined in this study and the Clyne–Kurz equation, we achieved reasonable agreement between the calculated and measured liquid composition change during the solidification process at different cooling rates. All experimental and theoretical programs in this research were undertaken with the aim of gaining further understanding of the microsegregation behaviors in large-scale IN718 ingots, whose cooling rates are within a lower range.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Chromium Tolerant, Highly Active and Stable Electrocatalytic Internal Surface Coating for Cathode of Commercial SOFCs (Final Report)

This project is aimed to develop a chromium (Cr) tolerant, highly active, and stable coating layer on the internal surfaces of the porous composite cathode from commercially available SOFCs. Such coating layer was developed using the additive manufacturing process of Atomic Layer Deposition (ALD) and has been applied on the cathode consisting of either an electronic conductor of LaxSr 1-x MnyO 3-δ (LSM) or mixed ionic and electronic conducting La x Sr 1-x Co y Fe 1-y O 3-δ (LSCF). PI's work has demonstrated that the internal surface of cathode from the commercial cells, can be further tailored using ALD coating to dramatically enhance the cell performance. For instance, ALD layer consisting heterostructured nano composite of nano-Pt and nano-(Mn 0.8 Co 0.2 ) 3 O 4 oxide on the internal surface of porous LSM/YSZ cathode from SOFCs, has resulted in the large reduction of the cell polarizations resistance by up to 53%, and enormous increase of power density over 370%. For the cells with LSCF/Sm 2 O 3 doped CeO 2 (SDC) cathode, the conformal layer of nano-composite consisting of superjacent CoOx and subjacent minimum amount of Pt nano-grains has resulted in the power density enhancement by 126% for the large scale industry tubular cells at 750°C, and both the performance enhancement and nanostructure of the ALD layer are stable over ~ 2000 h continuous operation performed at industry test station. In the meanwhile, those ALD coating layer developed by PI's work is also inherently Cr-tolerant, and could act as physical barrier for preventing Cr diffusion into the cathode backbone, so as to mitigate the Cr poisoning effect on the cathode. In this project, the impact of Cr on the performance of those ALD coated commercial cells has been evaluated. Based on evolution of the cell performance, the ALD coating layer chemistry and ALD coating layer thickness has been optimized to maximize the overall Cr tolerance, cell power density and cell longevity. Different ALD coating has been applied onto the internal surface of LSM/YSZ and LSCF/SDC backbone respectively. The architecture/scaffold structures on the internal surface of different cathode, designed by this project, was catalogued and analyzed using High Resolution Transmission Electron Microscopy (HRTEM), and cell power/durability performance are assured via comprehensive electrochemical performance testing in the industry operation relevant conditions. The impact of the electrochemical operation current density, the water humidity, the cell operation temperature, and cell operation duration on the Cr tolerance of ALD coated cells has been systematically investigated. There is completely different nanostructure degradation mechanisms between LSM and LSCF cells induced by Cr contamination. For the LSCF/SDC baseline cell, With the Cr source, there is no apparent Sr surface segregation phase even for the baseline cell operated for 3000 h at 750 °C. With the Cr source, there is significant amorphous (SrCr)Ox phase accumulated in the original pore region. For the commercial baseline cells, Cr contaminants on the LSM electrode severely impacted the entire cell's electrochemical performance and nanostructure degradation. Those degradations include (1). Peak power density loss of 64 % after 109 h of operation. The dramatic increase in Rp (2). They are cracking at LSM/SSZ interface, LSM grains. SSZ remains intact but with (CrMn)Ox. By contrast, ALD coating (MnCo)Ox/Pt dramatically improves the Cr resistance, as follows (1). ALD-coated cell with a power density is 280-380 % of the baseline cell, depending on the ALD layer thickness. (2). For a cell with a 20 nm thick ALD layer, there is a large performance enhancement (> 200 % power density) induced by ALD coating of Cr-tolerant Mn 0.8 Co 0.2 Ox. (3). For a cell with a 20 nm thick ALD layer, after 168 h at 750 °C power density of the ALD-coated cell is ~ 600% of that baseline cell upon operation with Cr contamination for 109 h. The ALD coating on the internal surface of cathode developed by this project integrated multi-functions. Those multi-functions include (1). Dramatically improving the cell power density for the commercial cells; (2). Dramatically improving contamination resistance of the cathode, for being an excellent protection coating layer sealing off Cr contamination. (3). Dramatically increasing the cell longevity by potentially preventing the microstructure evolution and grain coarsening of the cathode. Overall, this project will provide a simple solution to simultaneously enhance power density and increase the reliability, robustness, and endurance of commercial SOFCs, over the entire operating temperature range of 650-800 °C. For the inherently functional SOFC, the ALD coating of LSM based cathode mitigate the Cr-contamination. Power density of ALD-coated cell is ~ 600% of that baseline cell upon operation with Cr contamination. In addition to SOFCs, the novel on-demand design approach and creation of multifunctional heterogeneous architecture on the electrode surface presented in this work opens further research for their application in other types of fuel cells, batteries, and sensors for which electrochemical reactions on the surface are similarly critical.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructural features underpinning the mechanical behavior of powder metallurgy Cr-based alloys

Refractory materials such as Cr-based alloys offer the potential of enhanced elevated temperature performance but have been limited by their poor formability. However, powder metallurgy has been shown to be a viable pathway to fabricate these alloys. Nanophase separation sintering (NPSS) in particular has been used in the literature to accelerate the densification of powder metallurgy Cr- and W-based alloys. Here, we explore microstructure evolution during NPSS in a binary Cr 85 Ni 15 alloy consolidated via (i) cold pressing & pressureless sintering and (ii) hot isostatic pressing followed by hot extrusion & hot upsetting, and the role of these different processing routes on resulting material properties. The alloy lacked room temperature tensile ductility regardless of consolidation process, with multi-length scale characterization, including scanning electron microscopy, transmission electron microscopy, atom probe tomography, X-ray diffraction, and uniaxial tensile testing, revealing that brittleness was due to intrinsically poor Cr grain boundary cohesion. Tensile testing conducted at 760 °C showed marked strength reduction for the extruded & upset (94 %) condition compared to the pressed & sintered (18 %). The formation of orthorhombic CrNi 2 intermetallics functioned as precipitate strengtheners and prevented elevated temperature softening in the pressed and sintered condition. The findings offer foundational insights into aiding the future development of Cr-based alloys.

36 MATERIALS SCIENCE↗