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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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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Coregistered positron emission particle tracking (PEPT) and X-ray computed tomography (CT) for engineering flow measurements

Increasingly, fully 3D experimental measurements of flow in complex engineering geometries are required to validate computational fluid dynamics models that support and inform reactor design and licensing. One barrier to such measurements is the complexity of typical reactor components and subsequent lack of optical access in these systems. To overcome this, the deployment of coregistered positron emission particle tracking (PEPT) and X-ray computed tomography (CT) is explored for flow measurement in reactor thermal hydraulic components and model (scaled) systems. Through this methodology, fully 3D flow information (via PEPT) and detailed internal geometry (via CT) are captured in opaque systems such as pipes, rod bundles, packed beds, etc. The reconstructed flow field and geometry can then be overlain to reveal detailed flow features around internal structures within a given test section. This is enabled through the use of a combined preclinical PET/CT scanner with overlapping PET and CT fields of view. Such measurements are useful for characterizing flow inside such intricate nuclear thermal hydraulic components as core geometries and heat exchangers, among others, and providing valuable 3D validation data for CFD models. In this work, basic tests of this 3D flow/geometry mapping are presented, and the implications of such measurements are discussed. Further, preliminary measurements are made with both point sources and flow in a simple pipe flow geometry to evaluate the capabilities of this technique. PEPT and CT features are coregistered with up to 0.1 mm precision, and pipe flow mean velocity and Reynolds stresses are reconstructed with similar accuracy to previous PEPT demonstrations. The utility of PEPT/CT is shown herein, and suggestions for future measurements are made.

3D flow measurement↗
DOE OSTI2022

The formation and evolution of Ni 2 Cr precipitates in Ni–Cr model alloys as a function of stoichiometry characterized by synchrotron x-ray diffraction

Ni-based alloys containing significant amounts of Cr, may precipitate new phases during long-term service at elevated temperatures. In Ni–Cr model alloys, the formation of Ni 2 Cr has been found to impact the material properties, including the strength and ductility after isothermal aging below the critical temperature of 590°C. In this work, we quantify the formation and evolution of long-range ordering in four Ni–Cr binary model alloys (Ni/Cr = 1.8, 2.0, 2.2, 2.4) after isothermal aging up to 10,000h at temperatures between 373 and 475°C. The alloys were characterized by hardness testing and synchrotron-based x-ray diffraction to quantify the impact of Ni 2 Cr phase fraction and precipitate size on mechanical properties. After 500h of isothermal aging, the formation of Ni 2 Cr was detected in all four alloys at 475°C. In the stochiometric alloy samples (Ni/Cr = 2.0), the formation of Ni 2 Cr was found after 500 and 3000h aging at 418 and 373°C, respectively. We found that the matrix lattice contraction and Ni 2 Cr phase fraction both saturate after early aging times. This is in stark contrast to the hardness and Ni 2 Cr precipitate size that both continue to increase with increasing aging time. Our results highlight that changes in hardness correlate linearly with Ni 2 Cr precipitate size rather than phase fraction. This important structure-property relationship can potentially help define Ni–Cr-based component lifetimes directly through an understanding of how Ni 2 Cr formation impacts strength and ductility. Here, we find that a precipitation hardening model for critical resolved shear stress with weakly coupled dislocations shows good agreement with the material property changes quantified from experimental measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2022

The XMM Cluster Survey analysis of the SDSS DR8 redMaPPer catalogue: implications for scatter, selection bias, and isotropy in cluster scaling relations

ABSTRACT In this paper, we present the X-ray analysis of Sloan Digital Sky Survey DR8 redMaPPer (SDSSRM) clusters using data products from the XMM Cluster Survey (XCS). In total, 1189 SDSSRM clusters fall within the XMM–Newton footprint. This has yielded 456 confirmed detections accompanied by X-ray luminosity (LX) measurements. Of these clusters, 381 have an associated X-ray temperature measurement (TX). This represents one of the largest samples of coherently derived cluster TX values to date. Our analysis of the X-ray observable to richness scaling relations has demonstrated that scatter in the TX–λ relation is roughly a third of that in the LX–λ relation, and that the LX–λ scatter is intrinsic, i.e. will not be significantly reduced with larger sample sizes. Analysis of the scaling relation between LX and TX has shown that the fits are sensitive to the selection method of the sample, i.e. whether the sample is made up of clusters detected ‘serendipitously’ compared to those deliberately targeted by XMM. These differences are also seen in the LX–λ relation and, to a lesser extent, in the TX–λ relation. Exclusion of the emission from the cluster core does not make a significant impact on the findings. A combination of selection biases is a likely, but yet unproven, reason for these differences. Finally, we have also used our data to probe recent claims of anisotropy in the LX–TX relation across the sky. We find no evidence of anistropy, but stress this may be masked in our analysis by the incomplete declination coverage of the SDSS.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2024

Phase Transformations Driving Biaxial Stress Reduction During Wake-Up of Ferroelectric Hafnium Zirconium Oxide Thin Films

Biaxial stress is identified to play an important role in the polar orthorhombic phase stability in hafnium oxide-based ferroelectric thin films. However, the stress state during various stages of wake-up has not yet been quantified. In this work, the stress evolution with field cycling in hafnium zirconium oxide capacitors is evaluated. The remanent polarization of a 20 nm thick hafnium zirconium oxide thin film increases from 9.80 to 15.0 µC cm –2 following 10 6 field cycles. This increase in remanent polarization is accompanied by a decrease in relative permittivity that indicates that a phase transformation has occurred. The presence of a phase transformation is supported by nano-Fourier transform infrared spectroscopy measurements and scanning transmission electron microscopy that show an increase in ferroelectric phase content following wake-up. The stress of individual devices field cycled between pristine and 10 6 cycles is quantified using the sin 2 (ψ) technique, and the biaxial stress is observed to decrease from 4.3 ± 0.2 to 3.2 ± 0.3 GPa. The decrease in stress is attributed, in part, to a phase transformation from the antipolar Pbca phase to the ferroelectric Pca2 1 phase. This work provides new insight into the mechanisms controlling and/or accompanying polarization wake-up in hafnium oxide-based ferroelectrics.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Multimodal Defect Imaging of Pure Tungsten Components Fabricated via Electron Beam Powder Bed Fusion

The utilization of additive manufacturing (AM) techniques for refractory materials in high-temperature environments has significantly expanded because of the ability to fabricate geometrically complex components. Electron beam powder bed fusion (EB-PBF), which provides lower residual stress, a cleaner vacuum environment, and better efficiency for high melting point, is one of the best-suited AM methods to produce advanced refractory components. However, the property variation attributed to the heterogeneous microstructure and process-induced defects has hindered the widespread adoption of EB-PBF-produced material like tungsten. While numerous in-situ monitoring and defect detection methods have been demonstrated for EB-PBF, a workflow that compares and evaluates process-induced abnormalities from different imaging perspectives is still limited. This study examines a feature-embedded tungsten component manufactured via the EB-PBF process to demonstrate the defect detection capabilities of a multimodal defect imaging workflow. The predefined and process-induced defects are evaluated by harnessing various imaging techniques, including in-situ electron imaging, layerwise near-infrared (NIR) imaging, post-build high-energy x-ray computed tomography (CT), and conventional destructive metallography. The results highlight the strengths and limitations of distinctive defect imaging techniques concerning specific defect types, sizes, and conditions. It was found that electron imaging can provide more abnormal detection capabilities while maintaining a higher measuring accuracy, against the conventional metallography in this case study, compared with NIR and CT imaging techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Male Runners With Lower Energy Availability Have Impaired Skeletal Integrity Compared to Nonathletes

Abstract Context Female athletes, particularly runners, with insufficient caloric intake for their energy expenditure [low energy availability (EA) or relative energy deficiency] are at risk for impaired skeletal integrity. Data are lacking in male runners. Objective To determine whether male runners at risk for energy deficit have impaired bone mineral density (BMD), microarchitecture, and estimated strength. Design Cross-sectional. Setting Clinical research center. Participants 39 men (20 runners, 19 controls), ages 16–30 years. Main Outcome Measures Areal BMD (dual-energy x-ray absorptiometry); tibia and radius volumetric BMD and microarchitecture (high-resolution peripheral quantitative computed tomography); failure load (microfinite element analysis); serum testosterone, estradiol, leptin; energy availability. Results Mean age (24.5 ± 3.8 y), lean mass, testosterone, and estradiol levels were similar; body mass index, percent fat mass, leptin, and lumbar spine BMD Z-score (−1.4 ± 0.8 vs −0.8 ± 0.8) lower (P < .05); and calcium intake and running mileage higher (P ≤ .01) in runners vs controls. Runners with EA <median had lower lumbar spine (−1.5 ± 0.7, P = .028), while runners with EA ≥median had higher hip (0.3 ± 0.7 vs −0.4 ± 0.5, P = .002), BMD Z-scores vs controls. After adjusting for calcium intake and running mileage, runners with EA <median had lower mean tibial total and trabecular volumetric BMD, trabecular bone volume fraction, cortical porosity, and apparent modulus vs controls (P < .05). Appendicular lean mass and serum estradiol (R ≥ 0.45, P ≤ .046), but not testosterone, were positively associated with tibial failure load among runners. Conclusions Despite weight-bearing activity, skeletal integrity is impaired in male runners with lower caloric intake relative to exercise energy expenditure, which may increase bone stress injury risk. Lower estradiol and lean mass are associated with lower tibial strength in runners.

Haines, Melanie S. (ORCID:0000000310024754)↗
DOE OSTI2021

Temperature dependence of field-response mechanisms in 0.4Ba(Zr 0.2 Ti 0.8 )O 3 &#x2013;0.6(Ba 0.7 Ca 0.3 )TiO 3

Understanding the temperature dependence of how ferroelectric materials respond to electric fields is critical for determining how best to use these materials in applications. In this study, temperature dependent in situ x-ray diffraction is used to study how field-response mechanism Ba ( Zr 0.2 Ti 0.8 ) O 3 – x ( Ba 0.7 Ca 0.3 ) TiO 3 evolves with temperature. Increasing the measurement temperature was found to slightly reduce the extent of domain reversal and the magnitude of the 111 lattice strain. Instead, these results indicate that temperature predominantly impacted the angular dependence of the 002/200 lattice strain. We attribute the observed differences in 002/200 lattice strain to the flattening of the free-energy near the tetragonal-orthorhombic phase boundary, where the flattening of the energy landscape promotes a polarization rotation response during the application of electric fields at room temperature.

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

Probing Fundamental Mechanisms of Plastic Deformation with High Energy X-rays (Final Progress Report)

Overall, substantial progress was made on developing BCDI techniques in the direction of imaging defects in multi-crystal samples. Section 2.1 describes a new method to reconstruct the 3D atomic displacement field within a grain from multiple coherently resolved diffraction peaks. The key development is the ability to recover a best fit to the grain shape at the same time as the internal displacement (strain) variation with no prior knowledge of the microstructure. This is complemented by the development of a method, Sec. 2.2, to separate out sets of Laue reflections that belong to a single grain (and thus be able to index its orientation) in the commonly encountered situation in which the beam illuminates several grains in a given location. This is essential for enabling collection of coherent diffraction data (at APS 34-ID-C) from neighboring grains. All experiments depend on the quality of samples used. Although good progress has been made with thin film samples, we are working with a broader range of geometries. A new sample design uses a high-Z metal (e.g., Pt) deposited in a sub-micron trench in a low-Z metal (e.g., Al) so that the grain size is prevented from exceeding the current limit for BCDI. We also report in section 3.1 on successfully applying NF-HEDM to a fine-grain Mg sample that would normally be considered out of scope for the method. This represents progress towards being able to map out polycrystalline samples in 3D before performing BCDI on individual grains. We further report in section 3.2 on preliminary NF-HEDM characterization of a sample of UO2 that has sub-micron grains; the data imply the capability of mapping fine-grain polycrystals at 1-ID-E, again for the purposes of BCDI in the bulk. Lastly, our plan is to load grains in polycrystalline samples by inducing thermal stress. We also report the experimental measurements of the Ti- 6Al-4V alloy obtained at the European Synchrotron Radiation Facility (ESRF), which had been indexed and mapped via HEDM at APS in section 9. As discussed below, however, technique development pre-occupied the team throughout the project which meant that we did not make any significant progress towards answering the original hypotheses as stated in the proposal. In summary, we assert that we have made good progress in methods and samples and future work taking advantage of this progress is likely to obtain and analyze BCDI data from multiple adjacent grains in 3D polycrystals. Obtaining such data depends on re-gaining access to the Advanced Photon Source, which is anticipated in late summer or the Fall. In all cases, work has involved close collaboration with faculty, staff, postdocs and students from Brigham Young University (BYU), the Los Alamos National Laboratory and APS beamlines 1-ID and 34-ID.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Refined room-temperature equation of state of Bi up to 260 GPa

At room temperature, bismuth undergoes several structural transitions with increasing pressure before taking on a body-centered cubic (bcc) phase at approximately 8 GPa. The bcc structure is stable to the highest measured pressure and its simplicity, along with its high compressibility and atomic number, makes it an enticing choice as a pressure calibrant. Here, we present three data sets on the compression of bismuth in a diamond anvil cell in a neon pressure medium, up to a maximum pressure of about 260 GPa. The use of a soft pressure medium reduces deviatoric stress when compared to previous work. With an expanded pressure range, a higher point density, and a decreased uniaxial stress component, we are able to provide more reliable equation of state parameters. We also conduct density functional theory electronic-structure calculations that confirm that the bcc phase is energetically favored at high pressure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Examining polymer‐protein biophysical interactions with small‐angle x‐ray scattering and quartz crystal microbalance with dissipation

Abstract Polymer‐protein hybrids can be deployed to improve protein solubility and stability in denaturing environments. While previous work used robotics and active machine learning to inform new designs, further biophysical information is required to ascertain structure–function behavior. Here, we show the value of tandem small‐angle x‐ray scattering (SAXS) and quartz crystal microbalance with dissipation (QCMD) experiments to reveal detailed polymer‐protein interactions with horseradish peroxidase (HRP) as a test case. Of particular interest was the process of polymer‐protein complex formation under thermal stress whereby SAXS monitors formation in solution while QCMD follows these dynamics at an interface. The radius of gyration ( R g ) of the protein as measured by SAXS does not change significantly in the presence of polymer under denaturing conditions, but thickness and dissipation changes were observed in QCMD data. SAXS data with and without thermal stress were utilized to create bead models of the potential complexes and denatured enzyme, and each model fit provided insight into the degree of interactions. Additionally, QCMD data demonstrated that HRP deforms by spreading upon surface adsorption at low concentration as shown by longer adsorption times and smaller frequency shifts. In contrast, thermally stressed and highly inactive HRP had faster adsorption kinetics. The combination of SAXS and QCMD serves as a framework for biophysical characterization of interactions between proteins and polymers which could be useful in designing polymer‐protein hybrids.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2021

The ultrahigh pressure stability of silver: An experimental and theoretical study

We measured the atomic volume of Ag in a toroidal diamond anvil cell to a maximum pressure of 416 GPa and calculated the atomic volume and elastic constants of Ag up to 750 and 460 GPa, respectively. Our density functional theory calculations at 0 K utilize an all-electron fully relativistic method and agree well with our volume measurements, particularly at pressures above ~75 GPa. In this work, we corrected our experimental results for non-hydrostaticity using a line shift analysis, and the resulting Vinet equation of state (EOS) parameters are reported. We find that the uniaxial stress sustained by Ag increases linearly up to 4.5 GPa at a pressure of 416 GPa. Our experimental results indicate that the fcc structure of Ag remains stable to at least 416 GPa at room temperature. Our theoretical results show that C44 increases as pressure increases and reaches a maximum at ~100 GPa above which it begins to decrease, a sign that the fcc structure of Ag is becoming unstable, and at V/V 0 = 0.30, the bcc structure is lower in energy than fcc.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Applied in-plane strain effects on the polarization response of ferroelectric hafnium zirconium oxide thin films

The influence of biaxial stress on the maximum and remanent polarizations of 10 nm thick hafnium zirconium oxide thin films in metal–ferroelectric–metal capacitor structures has been quantified. In the as-prepared state with a nominal biaxial tensile strain of 0.20% and no applied extrinsic stress, remanent and maximum polarizations of 7.6 and 13.1 μC/cm 2 , respectively, were measured using a 2 MV/cm applied electric field. Reducing the intrinsic strain by 0.111% through the application of a compressive uniaxial stress results in a decrease in the remanent and maximum polarizations to 6.8 and 12.2 μC/cm 2 , respectively. Here, the polarization dependence on strain is nearly linear between these values. The observed variation in polarization with strain is consistent with strain impacting ferroelastic switching whereby in-plane tension increases the fraction of the short polar axis orienting out-of-plane, hence increasing out-of-plane polarization. In contrast, reducing the in-plane strain through compression results in an increase in the fraction of the long non-polar axis orienting out-of-plane, thereby decreasing out-of-plane polarization.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Multiscale operando X-ray investigations provide insights into electro-chemo-mechanical behavior of lithium intercalation cathodes

The electrochemical performance and cycle life of lithium-ion batteries (LIBs) depend on the electrochemical, chemical, and mechanical behavior of electrodes and electrolytes. Despite extensive studies conducted previously, challenges exist to decouple these behaviors, capture the evolution of electro-chemo-mechanical behavior in realistic conditions, and correlate atomic-scale stress evolution to micro-scale bulk mechanical degradation. Here, we report multiscale operando techniques to investigate polydisperse battery electrodes by integrating volume-averaged quantitative synchrotron X-ray scattering with high-resolution transmission X-ray microscopy (TXM). The former provides us information spanning a wide spatial range, from Angstrom-level atomic structures to micrometer-level particle scales, while the latter provides time-resolved 2D images of the particles during cycling. The complementarity of the two operando techniques is demonstrated by an over-lithiation test of LiCoO 2 electrodes, where particles crack and eventually pulverize. Additionally, the techniques are applied to study LiCoO 2 cycling stability from 3.0 V to 4.5 V. Operando X-ray scattering result shows nanometer-scale features keep forming in LiCoO 2 electrodes during cycling, resulting in an increased projected area observed by the TXM experiment. The formation of such features is inhibited by a polymer coating on the electrode, leading to vastly improved cycling stability. The polymer coating alleviates LiCoO 2 surface deterioration, reduces side product generation, and inhibits LiCoO 2 particles volume expansion during the cycling test. These operando multimodal X-ray techniques presented herein thus offer a novel, multiscale diagnostic modality for studying existing and emerging battery materials, aiding the development of next-generation LIBs.

25 ENERGY STORAGE↗
DOE OSTI2022

Effect of thermal aging on microstructure and crack growth response of Alloy 152 weld

Nickel-based 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 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 power 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 152 weldments 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 Ni2Cr 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 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for up to 75,000h (equivalent to 60 years of service). The microstructural characterization by means of synchrotron X-ray did not find evidence of LRO in any of the three heats aged to an equivalent of 60 years of service. Testing in a primary water environment of a heat of Alloy 152 aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloy. However, the SCC CGR response of the aged sample appears to show a deterioration in performance.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Strain-induced topological transitions in epitaxial films of cadmium arsenide

Strain in epitaxial thin films can have a profound influence on their electronic bands. Here, we investigate the influence of epitaxial strains on the electronic states of (001)-oriented cadmium arsenide (Cd 3 As 2 ) thin films, which are two-dimensional topological insulators. Cd 3 As 2 films were grown coherently on Al 1−x In x Sb buffer layers with varying degrees of lattice mismatch to Cd 3 As 2 , producing in-plane stresses that ranged from compressive to tensile. Using magneto-transport measurements of the Landau levels of the lowest subbands, we show that films under compression remain in the two-dimensional topological insulator state, while a sufficiently large tensile stress induces a transition to a topologically trivial phase. These results qualitatively agree with expectations from theoretical models for these films. At the topological transition, the gap avoids completely closing, and we discuss possible origins.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Effect of thermal aging on microstructure and stress corrosion cracking behavior of Alloy 152 weldment

Nickel-based 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 are expected to operate for 40-80 years. Likewise, 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 power 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 152 weldments 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 Ni2Cr 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 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for up to 75,000h (equivalent to 60 years of service). The microstructural characterization by means of synchrotron X-ray conducted in small, 0.2 mm - step line scans in the high-deformation regions of the weld root – covering areas spanning from the weld heat affected zone (HAZ) in Alloy 690 to the weld and weld butter on LAS - did not show evidence of LRO in any of the three Alloy 152 heats aged to an equivalent of 60 years of service. Testing in a primary water environment of two heats of Alloy 152 aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloys. However, the SCC CGR response of the aged samples appears to show a deterioration in performance, confirming our previous observation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Molecular Origin of Strain-Induced Chain Alignment in PDPP-Based Semiconducting Polymeric Thin Films

Donor–acceptor (D–A) type semiconducting polymers have shown great potential for the application of deformable and stretchable electronics in recent decades. However, due to their heterogeneous structure with rigid backbones and long solubilizing side chains, the fundamental understanding of their molecular picture upon mechanical deformation still lacks investigation. Here, the molecular orientation of diketopyrrolopyrrole (DPP)-based D–A polymer thin films is probed under tensile deformation via both experimental measurements and molecular modeling. The detailed morphological analysis demonstrates highly aligned polymer crystallites upon deformation, while the degree of backbone alignment is limited within the crystalline domain. Besides, the aromatic ring on polymer backbones rotates parallel to the strain direction despite the relatively low overall chain anisotropy. Additionally, the effect of side-chain length on the DPP chain alignment is observed to be less noticeable. These observations are distinct from traditional linear-chain semicrystalline polymers like polyethylene due to distinct characteristics of backbone/side-chain combination and the crystallographic characteristics in DPP polymers. Furthermore, a stable and isotropic charge carrier mobility is obtained from fabricated organic field-effect transistors. This study deconvolutes the alignment of different components within the thin-film microstructure and highlights that crystallite rotation and chain slippage are the primary deformation mechanisms for semiconducting polymers.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of Thermal Aging on Microstructure and Stress Corrosion Cracking Behavior of an Alloy 152 1st Layer Butter Weldment

Nickel-based 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 are expected to operate for 40- 80 years. Likewise, 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 critical for the long-term performance of both existing and advanced nuclear power 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 152 weldments 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 Ni2Cr 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 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for different durations up to 75,000h (equivalent to 60 years of reactor service). The microstructural characterization by means of synchrotron X-ray conducted in small, 0.2 mm - step line scans in the high-deformation regions of the weld root – covering areas spanning from the weld heat affected zone (HAZ) in Alloy 690 to the weld and weld butter on LAS - did not show evidence of LRO in any of the three Alloy 152 heats aged at 370°C and 450°C to an equivalent of 60 years of service. However, the first weld butter layer has high levels of deformation and is highly susceptible to SCC even in its non-aged condition. Nanohardness testing confirmed the extreme hardening with aging (ΔHV ≅ 100) at two locations within this weldment. In absence of LRO, hardening is suspected to be due to thermally-induced Cr carbide precipitation and coarsening. Testing in a primary water environment of the 1st layer of Alloy 152 weld butter aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloys. Similarly, the SCC CGR response of the aged weld butter does not appear to show a deterioration in performance, however, the difficult-to-test weldment geometry may affect the test results.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗