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At least 253 records · Page 14

High Temperature Anode Recycle Blower for Solid Oxide Fuel Cell, Phase II (Final Report)

Broad commercialization of solid oxide fuel cells (SOFCs) requires anode offgas recycle blowers (ARCB) that are specifically designed for handling the challenging operating conditions presented by the SOFC process gases. Otherwise, they can be susceptible to frequent maintenance, low reliability, and short life. This report presents details of a DOE-funded Phase II effort conducted by Mohawk Innovative Technology, Inc. (MiTi®) for the development and testing of an oil-free, low cost, high-temperature centrifugal ARCB based on compliant foil bearing (CFB) technology for support of a 100 kW solid oxide fuel cell power plant. This Phase II builds on the results of a successful Phase I development project that resulted in the demonstration of a low TRL-6 prototype, shown in Figure 1. This Phase II final report presents design improvements over the Phase I prototype, presents the assembled test ARCBs, and discusses the advantages of this novel technology, particularly its long life and maintenance-free operation, which are derived from the use of CFBs. Also included are preliminary techno-economic analysis considerations for cost-effective deployment of the technology. The specific objectives of this project, as stated in the statement of program objectives (SOPO) were 1) to follow the methodology of design for manufacturing (or manufacturability) and assembly for implementing improvements identified as part of the Phase I effort with the purpose of reducing cost, enabling mass production, and facilitating the commercialization of a revised ARCB design, and 2) to fabricate four complete ARCB units based on the revised design and demonstrating their performance in both a laboratory setting and in an actual SOFC power plant. Execution of this SOPO would be supported by a number of technical tasks resulting in the fabrication and testing of the prototypes. To this end, MiTi continued the teaming relationship started during Phase I of the program with subcontracting partner FuelCell Energy, Inc. (FCE), which integrated (under a parallel effort funded by DOE Award DE-FE0026199) a modular 200 kWe SOFC power plant. MiTi and FCE coordinated to ultimately incorporate one of MiTi’s ARCB prototypes into one of the 100 kWe SOFC Modular Power Blocks (MPB) that constitute the core of FCE’s SOFC power plant for in-situ long-duration testing. Additionally, MiTi would explore the scalability and extendibility of the technology to other applications, as well as conduct a basic techno-economic analysis.

03 NATURAL GAS↗

Evidence for a High Temperature Whisker Growth Mechanism Active in Tungsten during In Situ Nanopillar Compression

A series of nanopillar compression tests were performed on tungsten as a function of temperature using in situ transmission electron microscopy with localized laser heating. Surface oxidation was observed to form on the pillars and grow in thickness with increasing temperature. Deformation between 850 °C and 1120 °C is facilitated by long-range diffusional transport from the tungsten pillar onto adjacent regions of the Y2O3-stabilized ZrO2 indenter. The constraint imposed by the surface oxidation is hypothesized to underly this mechanism for localized plasticity, which is generally the so-called whisker growth mechanism. The results are discussed in context of the tungsten fuzz growth mechanism in He plasma-facing environments. The two processes exhibit similar morphological features and the conditions under which fuzz evolves appear to satisfy the conditions necessary to induce whisker growth.

36 MATERIALS SCIENCE↗

Detection of voids in hydrogen embrittled iron using transmission X-ray microscopy

Hydrogen embrittlement remains a barrier to widespread adoption of hydrogen as a carbon-neutral energy source. Here, hydrogen embrittlement mechanisms are investigated across length scales in iron using transmission X-ray microscopy (TXM), digital image correlation (DIC), and notched tensile testing during in-situ electrochemical hydrogen charging. TXM reveals void size and spatial distribution ahead of a propagating crack. We find hydrogen charging leads to voids within ~10 μm of the crack tip and suppression of voids beyond this distance. Near the crack tip, voids are elongated in the direction of the crack and are smaller than voids in an uncharged sample. In the presence of hydrogen, these voids lead to quasi-cleavage fracture and a sharper crack tip. DIC shows localization and reduction of plastic strain with hydrogen charging, and tensile testing reveals a reduction in fracture energy and elongation at failure. Finally, these results are discussed in the context of hydrogen embrittlement mechanisms.

08 HYDROGEN↗

Experimental evaluation of localized creep deformation in grade 91 steel weldments

Spatially resolved measurement of localized creep deformation in heterogeneous creep resistant steel weldments is crucial but challenging for lifetime assessments of critical steam components in power plants. Here, experimental approaches were established to quantitatively evaluate commonly observed localized creep deformation in multi-pass Grade 91 steel weldments. An in-situ digital image correlation (DIC) system was utilized with a creep testing frame to monitor and measure both full-field strain and localized strain accumulation across the weldments during long-term creep testing at elevated temperatures. The in situ DIC method measured not only the creep deformation behavior of the weld metal, heat affected zone (HAZ), and base metal, but also creep strain evolution for each sub-region within the HAZ itself, including coarse-grained HAZ, fine-grained HAZ (FGHAZ), and intercritical HAZ (ICHAZ). The DIC results revealed that local creep strain in the ICHAZ reached up to 90% strain before final rupture, whereas nominal creep strain measured by the standard extensometer of the tested cross-weld specimen was below 10%, indicative of Type IV cracking of the Grade 91 weld. Microstructural analyses revealed that the faster creep degradation/deformation in the HAZ was caused mainly by accelerated matrix grain recrystallization/growth and a reduced pinning effect from the segregated and coarsened precipitates in the FGHAZ and ICHAZ. The ultimate creep rupture occurred in the ICHAZ owing to its lowest creep resistance induced by the largest recrystallized grain size, the lowest fraction of coincidence site lattice, and the lowest local strain energies/dislocation densities.

36 MATERIALS SCIENCE↗

Fracture resistance of hierarchical Cu–Mo nanocomposite thin films

We report the fracture behavior of high-temperature co-sputtered Cu/Mo nanocomposite thin films was investigated through in situ 3-point bend testing of pre-notched microbeams in SEM. The as-synthesized nanocomposites present hierarchical nano/microstructures composed of a matrix of phase-separated Cu–Mo with nanoscale ligaments dispersed with sub-micron scale Cu-rich islands containing Mo nano-precipitates. Results show a significant crack growth resistance in the hierarchical nanocomposite, several times higher than that measured in Cu/Mo nanoscale multilayers. Based on electron microscopy characterization, three mechanisms of crack growth resistance in the hierarchical structures are proposed: crack bridging by the Cu-rich layer, crack deflection via shear along the Cu/Mo interface, and multiple cracking. This work demonstrates an approach to increase toughness in high strength nanocomposites through interface micro-structure design.

36 MATERIALS SCIENCE↗

Ligand enhanced activity of in situ formed nanoparticles for photocatalytic hydrogen evolution

One consistent challenge of both computational and empirical catalyst screening is ensuring that the variables chosen for the screen are driving the performance analyzed. Furthermore, we compare photocatalytic hydrogen evolution from in situ formed Au and Au/Cu nanoparticles to nanoparticles of the same composition synthesized prior to being used as catalysts, as well as compare them to in situ formed Au and Au/Cu nanoparticles in the presence of exogeneous ligand. For all experiments, we observed that ligand-terminated nanoparticles performed better than un-stabilized in situ formed nanoparticles. We tested the generality of this result by studying Co, Ni, and Pd in the same system and also observed that the introduction of nanoparticle ligand leads to enhanced catalytic activity. Taken together, these results suggest 1) nanoparticle ligands can be beneficial, and even necessary, to produce catalysts with sustained activity 2) For computational prediction of these catalysts, factors relating to particle formation and stability need to be considered when both generating predictions as well as interpreting experimental results based on those predictions

08 HYDROGEN↗

Laboratory-Based Micro-X-ray Computed Tomography of Energy Materials at Idaho National Laboratory

Abstract The Idaho National Laboratory (INL) has implemented laboratory-based micro-X-ray computed tomography in a laboratory equipped for the examination of highly radioactive samples. This capability provides nondestructive three-dimensional volumetric information on samples to inform subsequent traditional destructive examinations as well as real-world inputs for high-fidelity scientific modeling. Samples can be imaged with spatial resolutions ranging from several hundred nm/voxel up to ~ 100 µm/voxel. The best usable spatial resolution achieved to date is 384 nm/voxel with this instrument, while the highest radiological dose rate of a sample imaged is ~ 60 R/h β/γ on contact. Advanced data analysis, including custom tomographic reconstruction and segmentation methods, have also been developed to support this capability. In addition to traditional digital X-ray radiography and tomography, this instrument is also able to visualize in situ tensile and compression testing as well as perform diffraction contrast tomography. This work describes the X-ray computed tomography post-irradiation examination capabilities at INL, as well as detailing a variety of applications this instrument has examined.

36 MATERIALS SCIENCE↗

Atomistic modeling of interface strengthening in Al-Si eutectic alloys

Al-Si cast alloys are usually composed of α-Al and Al-Si eutectic. Si flakes and Al matrix generally hold cube-on-cube orientation relationship with the primary interface (111) Al ∥(111) Si . Extensive experimental studies demonstrated that Si flakes cannot significantly improve mechanical properties of Al-Si cast alloys. We hypothesize that the weak strengthening effect associated with Si flakes might be attributed to thermomechanical properties of Al-Si interfaces besides their morphologies. To characterize Al-Si interfaces with a large lattice mismatch (> 30%), we proposed the quasi-coincident site lattice (Q-CSL) as reference lattice, and demonstrated that the Q-CSL Al-Si coherent interface has three characteristic coherent structures, one stable and low energy structure and two metastable and high energy structures. The translation vectors for the same type of coherent Q-CSL structures are consistent with three displacement shift complete (DSC) vectors. The two metastable structures can be obtained by shifting the low energy structure with three partial DSC vectors. Semi-coherent interface is composed of the low energy Q-CSL patches and three sets of interface misfit dislocations with Burgers vectors same as the DSC vectors. Atomistic simulations revealed that Al-Si interface exhibits low shear resistance. Ideal shear strength of the Q-CSL coherent interface is 110 MPa and semi-coherent interface is 20 MPa. The low shear resistance is attributed to the glide of interface misfit dislocations. Al-Si interface also exhibits low formation and migration energies of point defects. Owing to low shear strength and low formation and migration energies of point defects, interface sliding or shear readily happen under mechanical loading or during dislocation-interface interactions. Lattice dislocations can cross slip onto or climb along Al-Si interfaces. These reactions decrease the number of accumulated dislocation loops around Si flakes and promote nucleation and emission of lattice dislocations from Al-Si interfaces to matrix, consequently reduce the repulsive force on approaching dislocations and weaken Si flakes strengthening effect. In situ tension and compression tests in a scanning electron microscope reveal relatively weak strengthening effect due to Si flakes, consistent with the computed dislocation interaction with interfaces and shear behavior of interfaces.

36 MATERIALS SCIENCE↗

Elucidating the temperature dependence of TRIP in Q&P steels using synchrotron X-Ray diffraction, constituent phase properties, and strain-based kinetics models

Understanding the deformation-induced martensitic transformation (DIMT) is critical for interpreting the structure-property relationships that govern the performance of transformation-induced plasticity (TRIP) assisted steels. However, modern TRIP-assisted steels often exhibit DIMT kinetics that are not easily captured by existing empirical models based on bulk tensile strain. We address this challenge by combined bulk uniaxial tensile tests and in-situ high energy synchrotron X-ray diffraction, which resolved the phase volume fractions, stress-strain response, and microstructure evolution of each constituent phase. A modification of the Olson-Cohen model is implemented, which describes the martensitic transformation kinetics as a function of the estimated partitioned strain in austenite, rather than the bulk tensile strain. This DIMT kinetic model is used as a framework to clarify the root cause of an insufficiently understood toughness trough reported for TRIP-assisted steels during deformation at elevated temperatures. Here, the importance of the temperature-dependent toughness is discussed, based on the opportunity to modify deformation processes to tailor the DIMT kinetics and mechanical properties during forming and in service.

36 MATERIALS SCIENCE↗

In-situ x-ray computed tomography analysis of fracture mechanisms in ultrasonic additively manufactured Al-6061 alloy

The deformation and failure mechanisms in an ultrasonic additively manufactured Al-6061 alloy are studied using in-situ x-ray computed tomography during tensile deformation as well as ex-situ characterization with scanning electron microscopy. The role of pre-existing voids between the build layers on the failure mechanism is discussed with a focus on individual foil failures and void coalescence.

36 MATERIALS SCIENCE↗

Liquid-free covalent reinforcement of carbon nanotube dry-spun yarns and free-standing sheets

Carbon nanotubes (CNTs) possess exceptional mechanical properties, surpassing stiffness and strength metrics of common materials such as steel alloys by 100× at the nanoscale. However, when myriads of individual CNTs are bundled together into macroscopic ensembles like fibers or sheets, the result is a 100-fold drop in strength compared to its individual components. Here we present a general strategy aimed to close this gap in property scaling. By using vapor-phase polymerization of a crosslinkable polymer, we reinforced the weak interlinkages among individual CNTs within both yarns and sheets to promote a better transference of mechanical load across the structure. Furthermore, after the treatment, dry-spun, low-density 2.3 μm thin yarns increased their elastic moduli by at least 300%, and free-standing CNT sheets exhibited a 10× boost. In-situ synchrotron small-angle X-ray scattering revealed that polymer-reinforced yarns undergo limited CNT bundle rearrangement when subjected to tensile loads compared to pristine yarns. This evidence supports the hypothesis that the polymer hinders CNTs slippage, the root cause of the poor scaling of mechanical properties in these materials. While we demonstrated this reinforcement method for CNT structures, it is not specific to CNTs and could be used in a wide variety of other hierarchical nanostructured ensembles.

36 MATERIALS SCIENCE↗

In situ observation of the deformation and fracture of an alumina-alumina ceramic-matrix composite at elevated temperature using x-ray computed tomography

The deformation and fracture of a 0/90° Nextel 720 mullite fibre / alumina matrix ceramic-matrix composite material has been observed by in situ synchrotron x-ray computed micro-tomography at ambient temperature and at 1100 °C. A three-point loading configuration was used and samples were loaded monotonically until final fracture. Here, the flexural strength was found to be unaffected by temperature. 3D visualisation of the microstructure showed fracture occurred by propagation of internal cracks at stresses close to the flexural strength. Shear fractures propagated across fibre bundles that were oriented perpendicular to the flexural stress at both room temperature and 1100 °C. At the higher temperature, an additional failure mode of delamination was observed, that may arise from relaxation of thermal residual stresses and creep.

36 MATERIALS SCIENCE↗

Evaluating the bond strength and fracture mechanisms of cold-sprayed zinc coating on AZ91 magnesium substrate via a combined experimental and computational approach

Magnesium (Mg) alloys are ideal candidates for automotive applications due to their high strength to weight ratio, castability, recyclability etc., however, they lack corrosion and oxidation resistance. Solid-state deposition techniques, such as cold spray, have been demonstrated to enhance their corrosion resistance as it relies on the severe plastic deformation of powder particles upon impact with the substrate to form a metallurgical bond with the substrate and within the coating. At cold sprayed interfaces, a heterogeneous microstructure is formed that includes some porosity, oxides and intermetallics which can significantly affect coating performance. Thus, establishing a direct correlation between the interface microstructure and its properties can aid in designing optimal cold spray parameters. In this study, we investigated the microstructure and mechanical properties of a zinc (Zn) coating deposited on a high pressure die cast (HPDC) AZ91 Mg substrate via high resolution scanning transmission electron microscopy, in situ micro-tensile testing, and finite element method (FEM) modeling. Micro-tensile pillars fabricated using the plasma focused ion beam (PFIB) successfully isolates the coating-substrate interface within the gauge length. The average bond strength of Zn-Mg interface was determined to be ∼140 MPa with failure occurring partially at the interface and mostly into the coatings. A detailed microstructural characterization revealed evidence of a strong metallurgical bonding at the Zn-Mg interface and formation of the C14 MgZn 2 laves phase interlayer resulting in a mixed mode of fracture during the micro-tensile experiments. FEM modeling reveals the stress distribution along the interfaces and suggests that a MgZn 2 layer thickness between 200–400 nm is optimum to increase the bond strength and minimize the triaxiality. Such a site-specific interfacial analysis with correlative computational modeling provides crucial insight into the overall performance of cold spray interfaces.

Bond strength↗

Investigation of hardening mechanisms and size effects in proton-irradiated HT-9 steels

Ferritic/martensitic steels, such as HT-9, are known for their complex microstructural features and mechanical properties. Here in this paper, in-situ micro-tensile tests and traditional fractography methods were utilized to study the fracture behavior of proton-irradiated HT-9 steels. First, to evaluate the viability of micro-tensile tests for nuclear material qualification process, meso-tensile tests on as-received HT-9 steels were performed. Fracture mechanisms of unirradiated HT-9 steels at both length scales were compared and underlying mechanisms discussed. The direct comparison of micro- and meso-scale data shows a distinctive size effect demonstrated by the increase in yield stress (YS). Upon completion of initial assessment, specimens were irradiated with 4 MeV + protons to three fluences, all of which were lower than 0.01 displacements per atom (dpa). As expected, the YS increases with irradiation. However, at 7 × 10 -3 dpa, the reversal of the trend was observed, and the YS exhibited sharp decline. We demonstrate that at lower length scales, grain structure has a more profound impact on the mechanical properties of irradiated materials, which provides information needed to fill in the gap in current understanding of the HT-9 fracture at different length scales.

36 MATERIALS SCIENCE↗

Interface-engineered (AlMnCoNiZn) 3 O 4 @PPy nanocomposites for superior lithium storage: Mechanism and performance

The practical application of graphite anodes in lithium-ion batteries (LIBs) is constrained by low specific capacity (372 mAh g -1 ) and sluggish kinetics. Here, to address these limitations, our present study focuses on high-entropy oxides (HEOs), which offer high theoretical capacity and structural stability. We synthesized spinel-structured (AlMnCoNiZn) 3 O 4 nanoparticles via a solution combustion method and fabricated an (AlMnCoNiZn) 3 O 4 @polypyrrole (PPy) nanocomposite through in-situ polymerization. Our electrochemical tests demonstrate that the PPy modification significantly enhances performance. While the pristine (AlMnCoNiZn) 3 O 4 delivered 445 mAh g −1 after 100 cycles at 100 mA g −1 and 350 mAh g −1 after 1000 cycles at 1000 mA g −1 , the (AlMnCoNiZn) 3 O 4 @PPy composite achieved 695 mAh g −1 after 100 cycles and maintained 675 mAh g −1 after 1000 cycles. Furthermore, the composite improved rate capacity at 1000 mA g −1 from 211 mAh g −1 to 403 mAh g −1 . This work highlights how conductive and flexible polymer modifications can dramatically improve the electrochemical properties of HEOs. The developed (AlMnCoNiZn) 3 O 4 @PPy composite provides a promising direction for designing advanced anodes to meet next-generation energy storage demands.

Anodes material↗

Amorphous complexions alter the tensile failure of nanocrystalline Cu-Zr alloys

Grain boundary-based mechanisms are known to control the plastic deformation and failure of nanocrystalline metals, with manipulation of the boundary structure a promising path for tuning this response. In this study, the role of interfacial structural disorder on plasticity and failure of nanocrystalline Cu-Zr alloys is investigated with in situ scanning electron microscopy tensile deformation experiments. Two model materials are created, one with only the typical ordered grain boundaries and another with amorphous intergranular films interspersed into the boundary network, while the microstructures are otherwise identical. Hence, the importance of complexion type on plasticity and failure is isolated by only varying complexion structure. Here, the tensile experiments show that failure of the samples containing amorphous films is significantly retarded, as evidenced by an increase in the cross-sectional area reduction, a decrease in the occurrence of shear-dominated failure, a decrease in strain localization, and fracture surfaces with more elongated dimple features. As a whole, this study provides direct evidence that structural disorder at the grain boundaries can be beneficial for improving the ductility of nanocrystalline metals.

36 MATERIALS SCIENCE↗

Experimental and simulated heating in nanocrystalline diamond charge exchange injection films using an electron beam to mimic SNS conditions

Nanocrystalline diamond (NCD) foils have been in use at the Spallation Neutron Source as primary stripper foils for charge exchange injection since the machine’s inception. NCD’s low atomic number leads to reduced beam scattering while still being easy to handle, as opposed to even lighter elements. NCD foils also have the benefit of being free-standing, and rigid when grown under the right conditions to minimize residual stresses. This study overviews a method to mimic the Spallation Neutron Source (SNS) beam and characterize thermally driven failure of NCD foils. To do this, a foil test stand was developed with in situ diagnostics that tracks signs of foil sublimation and thinning. The foil test stand’s electron beam is equated to the SNS beamline by comparing peak deposited energy densities for both beams. Post-mortem testing is also conducted to help elucidate changes the NCD foils undergo during exposure to the beam. Further, a COMSOL simulation was also developed as a method to assess potential future changes to the NCD film and predict how changes to beam conditions will effect foil temperatures. This method allows for examination of the NCD foil’s thermal limits and can be used to assess future changes to SNS stripper foils.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Multi-modal tomographic imaging system for poolside characterization of nuclear test fuels: Design considerations and studies

Testing and qualification of advanced nuclear fuels involves an iterative process of prototyping, in-pile irradiation testing, and in-situ or ex-situ examination. Fuel restructuring and fission product migration during burnup are among the most important aspects of fuel evolution that affect several important performance characteristics such as heat removal, accident tolerance, and fission product retention. Pool-side non-destructive characterization techniques provide fuel developers with tools to understand fuel evolution at different points of burnup. A design for a compact, submersible, and multi-modal gamma-ray tomography system for imaging irradiated nuclear fuel is presented here. Detector selection, collimator geometry and fabrication, mechanical design, imaging protocol and acquisition speed are discussed. Modeling calculations show that sub-millimeter resolution can be achieved in both transmission computed tomography images as well as in emission computed tomography images in a matter of hours. Several design compromises and fabrication challenges are discussed which should be taken into consideration for future submersible gamma-ray tomography instruments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗