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At least 37 records · Page 2

Deep-Learning-Enabled Crack Detection and Analysis in Commercial Lithium-Ion Battery Cathodes

We report in Li-ion batteries, the mechanical degradation initiated by micro cracks is one of the bottlenecks for enhancing the performance. Quantifying the crack formation and evolution in complex composite electrodes can provide important insights into electrochemical behaviors under prolonged and/or aggressive cycling. However, observation and interpretation of the complicated crack patterns in battery electrodes through imaging experiments are often time-consuming, labor intensive, and subjective. Herein, a deep learning-based approach is developed to extract the crack patterns from nanoscale hard X-ray holo-tomography data of a commercial 18650-type battery cathode. Efficient and effective quantification of the damage heterogeneity with automation and statistical significance is demonstrated. The crack characteristics are further associated with the active particles’ packing densities and a potentially viable architectural design is discussed for suppressing the structural degradation in an industry-relevant battery configuration.

25 ENERGY STORAGE↗

Fatigue Crack and Porosity Measurement in Composite Materials by Thermographic and Ultrasonic Methods

Many nondestructive methods exist for the detection of localized material anomalies in an otherwise good composite structure. The problem arises when the material system as a whole has degraded during service or was improperly manufactured. Porosity and intra-ply microcracking are two such conditions that in unlined composite pressure vessels can be very troublesome to detect and when linked through the thickness can be critical to mission success. These leak paths may lead to loss of pressure/propellant, increased risk of explosion and possible cryo-pumping. Research sought nondestructive methods for quantifying porosity and microcracking in composite tankage. Both thermographic and resonance ultrasound methods have been utilized with artificial neural network and statistical approaches to analyze the data. Resonant ultrasound spectroscopy provides measurements, which are sensitive to fine details in the materials character, such as micro-cracking and porosity. Here, the higher frequency (shorter wavelength) components of the signal train provide more significant interaction with the defects causing the spectral characteristics to shift toward lower amplitudes at the higher frequencies. As the density of the defects increases more interactions occur and more drastic amplitude changes are observed. From a thermal perspective, the higher the defect density the lower the through thickness thermal diffusivity will be. Utilizing a point heat source, and thermographically recording the heat profile with time, diffusivity calculations can be made which in turn can be related to the relative quality of the material. Preliminary experiments to verify the measurable effect on the resonance spectrum of the ultrasonic data to detect microcracking and for porosity detection thermographically are presented. Methods involving supervised and unsupervised artificial neural networks as well as other clustering algorithms are developed for signal identification.

Walker, James L.↗

Influence of supplementary cementitious materials on microstructure and transport properties of spacer-concrete interface

Reinforcement spacers are a critical component of concrete structures. Their presence affects microstructure and transport properties of concrete cover though this is not widely appreciated. This paper presents the first study to determine whether the negative effects of spacers can be mitigated through the use of supplementary cementitious materials such as silica fume, fly ash and blast-furnace slag. Concrete samples (>200) with different spacers, binders, curing and drying regimes were prepared and tested for diffusion, permeation, absorption, electrical conductivity, carbonation and microstructure. It was found that spacers increase all transport properties, the extent depending on type of spacer, drying regime and transport mechanism. The spacer-concrete interface is weak, porous and micro-cracked, and this lowers the resistance of concrete to ingress of aggressive agents. The beneficial effects of SCMs (strength enhancement and densification) and prolonged curing (120-day) are insufficient to overcome the negative effects of spacers. Implications for durability are discussed.

36 MATERIALS SCIENCE↗

An innovative digital image correlation technique for in-situ process monitoring of composite structures in large scale additive manufacturing

As additive manufacturing (AM) continues to develop and become a standardized manufacturing method, there will be a continued need to provide in-situ monitoring during the manufacturing of polymer composite printed components. Thermal residual stress is a primary cause of failures such as interlayer disbonds or delamination, micro cracking, and dimensional instability, which can occur during or after the build. Here, we report a novel digital image correlation (DIC) adaptation to monitor thermal residual stresses during the entire print process for large-scale AM. In this work, DIC has been investigated (a) by the natural speckle produced by the polymer surface for correlation, (b) to monitor AM build, and (c) to evaluate the effect of thermal residual stress on warpage of the printed component. The natural speckle pattern of the AM material resulted in a respectable 3.57% error compared to the traditional painted speckle pattern of 3.05% error. DIC measured a 190% increase in vertical displacement at the edge of the wall compared to the center, indicating warpage during AM. This work is a step towards a non-intrusive residual stress measuring technique using DIC for large-scale AM.

36 MATERIALS SCIENCE↗

Experimental study of fracture slip due to stress perturbation in fractured geo-resources

Anthropogenic activities such as underground fluid injection/extraction, well stimulation, and dam impoundment will perturb the state-of-stress in the subsurface, which could activate critically stressed pre-existing fractures and faults. Fault and fracture activation can induce seismicity, change flow behavior, and damage asperities on the fracture surface to alter reservoir permeability. Here, in this study, triaxial shear tests were conducted on saw cut and rough fracture Barre granite specimens to better characterize how a decrease in normal stress and increase in shear stress will influence crystalline rock fracture hydromechanical properties. In a triaxial set up, confining pressure (CP) and differential stress (DS) were used to induce normal and shear stress on a 45° oriented fracture. Fracture slip and the corresponding stress relaxation was observed when the confining stress decreased. Fracture permeability increased when the fracture slipped. Moreover, new micro-cracks observed by x-ray images indicated the creation of new flow paths for fluid movement. The experimental outcomes of this study indicate that decrease in normal stress due to stress perturbations along the faults/fractures in the extensional stress regime can induce the slip along the fracture. This could have a significant influence on slope stability in quarries, stimulation and injection strategy in deep geo-resources, and potentially minimize the risk of induced seismicity. The observed stress dependency of hydraulic aperture in rough fracture during pre- and post-slip stages could provide key inputs for field-scale simulation of geo-resources.

58 GEOSCIENCES↗

Modeling low cycle fatigue (LCF) of additively manufactured Hastelloy X using An accelerated crystal plasticity fatigue damage model

This paper presents a microstructure-based model for low cycle fatigue (LCF) behavior and life of Nickel-based alloy Hastelloy X manufactured using laser-powder bed fusion (L-PBF) additive manufacturing (AM). AM Hastelloy X, a solution-strengthened alloy, is tested at elevated temperature under fully reversed LCF conditions at different strain levels. A generalized plane strain finite element model is generated from electron backscatter diffraction (EBSD) characterization. The constitutive behavior of the material under fatigue is modeled using crystal plasticity and calibrated with both monotonic tensile and cyclic stress–strain data. The fatigue micro-crack initiation and propagation in the microstructure is modeled using a modified Chaboche fatigue damage model. An embedded boundary condition with a homogenous medium is used to apply the cyclic deformation and prevent numerically introduced over-constraints during fatigue simulation. A ‘cycle-jump’ method is used to accelerate the fatigue simulation and reduce the computational cost. The simulation results are compared to LCF experiments, showing satisfactory matches in cyclic stress behavior and number of cycles to macro-crack initiation for all applied strain ranges. In addition, the model illustrates the potential for quantifying microscale fatigue life impacting factors such as microstructure and surface roughness, which is needed to accurately quantify the reliability of AM components in service.

36 MATERIALS SCIENCE↗

Investigation of the structure and chemical nature of Pd fission product agglomerations in irradiated TRISO particle SiC

Tristructural-isotropic (TRISO)-coated fuel particles are used in high-temperature gas-cooled nuclear reactors. Although the polycrystalline 3C-SiC layer acts as the main barrier to fission product release, post-irradiation examinations have shown that certain metallic fission products are found outside of the TRISO coated particle, with no observable micro-cracks or other mechanical failure feature. In this study, an atomic resolution transmission electron microscopy investigation of a SiC layer of a neutron irradiated (19.38% fissions per initial metal atom average burnup; 1072°C time-averaged temperature) TRISO-coated particle from the first advanced gas reactor experiment at Idaho National Laboratory containing mainly Pd and U was conducted. The fission product Pd was found to be present at dislocation cores associated with twins, stacking faults, and their intersections. The Pd present at the dislocation cores were bonded to Si, suggesting that the diffusion of Pd along the SiC dislocation cores involves the formation of Pd-Si bonds. Evidence of single atom grain boundary migration was also found. Fission product agglomerations at grain boundaries most likely consist of a random solid solution containing Si-FP, Si-C, and C-C type bonding arrangements. No difference in the Si- or C-bonding environment is found for the unoccupied grain boundary adjacent to a fission product agglomeration compared to the bulk SiC.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Investigation of ion irradiation effects on mineral analogues of concrete aggregates

Irradiation can cause prominent damage to reactor concrete aggregates leading to amorphization, strength and modulus decrease, radiation induced volume expansion (RIVE) and micro-cracking, which limits their long-term performance. Here, to develop an improved understanding of irradiation effects in concrete, three mineral analogues of concrete aggregates (limestone, marble and quartzite) were irradiated by 5.5 MeV He ions and 13 MeV Ni ions to surface doses of 0.011 displacements per atom (dpa) and 0.23 dpa, respectively, at room temperature. The two different ion species allow irradiation spectrum effects (ionizing and displacive) to be examined. Irradiation induced cracks were observed in He irradiated limestone and marble, and Ni irradiated quartzite. Full amorphization was observed in Ni irradiated quartzite with 14.3 % RIVE, and ∼25 % hardness and modulus decrease, while almost no change was observed in He irradiated quartzite except 4.35 % RIVE, revealing a possible ionization enhanced diffusion effect for high energy light ions. Furthermore, partial amorphization was observed in Ni irradiated marble and limestone matrix with a 12 % hardness decrease in marble while no amorphization was observed for He irradiation with a 20 % hardness increase in limestone matrix. The role of knock-on damage and irradiation spectrum on amorphization, volumetric expansion and mechanical property changes are discussed. Moreover, the onset and critical doses for amorphization and RIVE in quartz are obtained for ion irradiations at room temperature. The dose dependence of RIVE exhibits a delay compared to the amorphization behavior. The superior irradiation resistance of calcite phase compared to quartz phase implies there could be advantages to using calcareous aggregates and lowering the usage of siliceous aggregates for concrete in nuclear power plants for extended operation beyond 60 years. However, other effects such as corrosion, aging and reactions during severe accidents should also be considered, and further investigations are needed.

Amorphous↗

Fracture behavior of irradiation induced nanocrystalline UO 2 studied by in-situ mechanical testing in transmission electron microscopy

Uranium Dioxide (UO 2 ) is widely used as a fuel in current light water reactors (LWRs). Upon accumulation of radiation damage, LWR UO 2 fuel pellets start to develop a different microstructure at the pellet periphery when fuel burnup exceeds 45–50 GWd/tHM. The resulting porous, nanocrystalline microstructure is one of the most prominent microstructural changes occurring in such fuel. Its fracture mechanisms, which causes fuel fine fragmentation, could impact safety limits when the cladding breaches. Direct measurements of these properties are challenging, therefore a surrogate obtained via ion irradiation can be used. In this study, multiple microcantilevers were fabricated by focused ion beam from both fresh UO 2 and UO 2 irradiated with 84 MeV Xe 26+ ions to a peak dose of 1357 displacements per atom (dpa). Further, the irradiation produced a pseudo high burnup structure approximately 2 µm below the surface. In-situ nano-mechanical bending tests were conducted to investigate the fracture behavior and the effect of the surrogate UO 2 high burnup structure on local fracture properties. Fresh UO 2 fuel was observed to fracture in transgranular mode without nucleation or movement of dislocations. However, the Xe-irradiated nanocrystalline microcantilevers fractured along the grain boundaries, with no influence from the pre-existing micro-cracks in the microcantilever. Fracture toughness for this type of surrogate high burnup UO 2 structure is reported for the first time in literature. Both the fracture stress and toughness show degradation for UO 2 as a result of Xe-irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Analysis of orientation-dependent deformation mechanisms in additively manufactured Zr using in-situ micromechanical testing: Twinning and orientation gradient

Here, orientation-dependent plasticity in zirconium (Zr)-alloy, which is produced through ultrasonic additive manufacturing (UAM) with subsequent hot-isostatic pressing (HIP), was analyzed by recording electron backscattered diffraction (EBSD) data during in-situ micromechanical testing. Three (0001) plane orientations of a hexagonal close-packed (HCP) structure were analyzed parallel to (1) the rolling direction [X||tensile direction (TD)], (2) the build direction [Z], and (3) the transverse direction [Y]. The analysis revealed that the grains with ~<0001>||TD show twin-dominant plasticity with three variants from {10 $\overline{1}$ 2}<$\overline{1}$ 011>; minor slipping with ($10\overline{1}$ 1)[$\overline{2}$ 113], and ($11\overline{2}$ 2)[$\overline{1} \overline{1}$ 23] pyramidal slip has also been observed. However, grains with orientation ~<0001>⊥TD are mainly sensitive to dislocations assisted plasticity-leading to orientation gradients formation. Furthermore, the neck formation was identified as originating from higher populated micro-crack locations and their association with localized plasticity at defect points in the UAM material. These results demonstrate that minimization of impurities to enable grain growth across prior foil interfaces makes HIP an effective methodology for producing Zr plate, with deformation characteristics expected for conventionally manufactured Zr.

36 MATERIALS SCIENCE↗

Characterization of nonlinear ultrasonic waves behavior while interacting with poor interlayer bonds in large-scale additive manufactured materials

Over the past decades, researchers have developed several nonlinear ultrasonic techniques for quality control of materials commonly used in different applications. Owing to the superior sensitivity of nonlinear ultrasound waves to small defects such as micro-cracks, their applicability in different nondestructive testing (NDT) problems has been investigated in numerous studies. These studies utilize frequency domain analysis to detect the generation of higher harmonics because of the formation of defects in the inspected medium. Frequency domain analysis based on the Fourier transform is a significant approach used in linear systems; however, it may not perform adequately on nonlinear systems. Hence, studies on nonlinear dynamics and physics consider analyzing systems' behavior in the phase-space domain. In contrast to the frequency domain analysis, which can result in information loss, analysis in the phase-space domain retains all the information regarding a system's states. Here, we investigate the nonlinearities induced by poor interlayer bonding in polymer-based additive manufactured parts in the phase-space domain. It is convenient to characterize the nonlinearity in the phase-space domain because it provides a geometrical representation of a system's states. Two types of low quality interlayer bond are considered. The first type is simulated artificially while the second type is manufactured by reducing the bond quality during the printing process. The analysis verified that the received ultrasonic signals exhibit classical nonlinear behavior in the phase-space domain while interacting with simulated poor interlayer bonds. In addition, the results showed that the behavior of ultrasonic waves is amplitude-dependent and evolves into models that have not been previously reported. Furthermore, Largest Lyapunov Exponent (LLE) is used to quantify the behavior of nonlinear ultrasonic waves while interacting with poor interlayer bonds. Using LLE, it was observed that the divergence rate of the phase-space trajectories depends on the amplitude of the excitation. This observation quantitatively proves that nonlinear behavior of ultrasound while interacting with poor interlayer bonds can be amplitude-dependent. The results of both simulated and inherent poor interlayer bond cases showed that LLE can be used as a reliable quantitative damage-sensitive feature to detect and potentially characterize weak bonds, which are difficult to detect using conventional approaches. Additionally, the reported results in the phase-space domain provide a basis for proposing a new mathematical model for ultrasonic waves interacting with poor interlayer bonds.

36 MATERIALS SCIENCE↗

Characterization of the Fast-Neutron Irradiator and the Fast-Flux Tube Irradiation Fixtures at the Pennsylvania State Breazeale Reactor

Accurate knowledge of the neutron spectrum at a nuclear research reactor is a prerequisite for planning irradiation experiments, as well as for evaluating irradiation exposure results. The neutron-flux spectrum in the fast-neutron irradiator (FNI) and the fast-flux tube (FFT) irradiation fixtures at the Pennsylvania State Breazeale Reactor (PSBR) were characterized using the multi-foil neutron activation method. These irradiation fixtures make use of graded shielding to produce unique neutron fields. Multiple foil sets were irradiated in the fixtures with different exposure times and reactor powers to understand the stability over a wide range of operating conditions. Measured results were evaluated against a MCNP6 simulation to produce a measurement-informed neutron flux-energy spectrum for each fixture using STAYSL_PNNL. Simulated estimates of the FNI fixture, a newer fixture (~25 years old), demonstrated excellent agreement with measured results; the FFT did not. Thermal neutron measurements from the FFT suggest there is additional thermal leakage not captured in the simulation model. In conclusion, possible explanations for the discrepancy include burn-out or degradation (i.e., micro-cracking, gaps, etc.) in the boral and cadmium liners over the lifetime of the fixture (~40 years old).

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Stress-sensitivity of fracture conductivity of Tuscaloosa Marine Shale cores

Production decline from wells producing from shale rocks is typically quite rapid. One possible factor responsible for such decline is loss in fracture conductivity. This is true in the case of the Tuscaloosa Marine shale reservoir. In this work, the stress-dependent fracture conductivity of TMS core samples is investigated using five propped cores under varying stress conditions. In addition, the effects of static rock mechanical properties and rock mineralogy on conductivity decline are investigated. The mineralogy of each core sample was determined by X-ray Diffraction analysis. Fracture conductivity was measured using a Hassler-type pressure core holder with a pressure rating of 15,000 psi (103.42 MPa). Estimated rock mechanical properties showed that shale anisotropy could affect fracture conductivity. The time decline in conductivity revealed two possible decline trends, a) decline from the reduction in induced fracture width, and b) decline from the healing of developed micro-cracks. An exponential decline in fracture conductivity with increasing confinement pressure was observed with an average decline rate constant of 3.15 x 10 -10 mPa -1 . While rock mineralogy did not have any clear relationship with conductivity decline, the effects of rock mechanical properties were only important at 10.34 MPa confinement pressure and above. The observation showed that a high Young's modulus correlate to high conductivity, whereas a high Poisson's ratio correlate to low conductivity. This study provides useful observations for optimizing fracture design to enhance well productivity in the TMS.

02 PETROLEUM↗

Oil miscible phosphonium-phosphate ionic liquid as novel antiwear and antipitting additive for low-viscosity rear axle lubricants

Here we explored the feasibility of using a phosphonium phosphate ionic liquid as a candidate anti-wear and anti-pitting additive for rear axle lubricant. This particular IL was first added to a VHVI8 base oil at 2–3% concentration and demonstrated effective surface protection for wear and micro-cracking under rolling-sliding contacts. The promising results directed to a step further to produce a series of IL-containing low-viscosity (about a half of SAE 75W-90) fully formulated gear oils. Selected IL-containing experimental oils showed superior mitigation of rolling contact fatigue to a commercial SAE 75W-90 gear oil in bench-scale rolling-sliding tests. Full-scale hub dynamometer tests were then conducted and demonstrated more than 3% power output and torque generation for an IL-containing low-viscosity gear oil benchmarked against commercial baselines.

36 MATERIALS SCIENCE↗

Mutual modulation between surface chemistry and bulk microstructure within secondary particles of nickel-rich layered oxides

Abstract Surface lattice reconstruction is commonly observed in nickel-rich layered oxide battery cathode materials, causing unsatisfactory high-voltage cycling performance. However, the interplay of the surface chemistry and the bulk microstructure remains largely unexplored due to the intrinsic structural complexity and the lack of integrated diagnostic tools for a thorough investigation at complementary length scales. Herein, by combining nano-resolution X-ray probes in both soft and hard X-ray regimes, we demonstrate correlative surface chemical mapping and bulk microstructure imaging over a single charged LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) secondary particle. We reveal that the sub-particle regions with more micro cracks are associated with more severe surface degradation. A mechanism of mutual modulation between the surface chemistry and the bulk microstructure is formulated based on our experimental observations and finite element modeling. Such a surface-to-bulk reaction coupling effect is fundamentally important for the design of the next generation battery cathode materials.

25 ENERGY STORAGE↗

Tough and circular glass fiber composites via a tailored dynamic boronic ester interface

Glass fiber reinforced polymer (GFRP) composites are valued for their strength and cost-effectiveness. However, traditional GFRPs often face challenges for end-of-life recycling due to their non-depolymerizable thermoset matrices, and long-term performance due to inadequate interfacial adhesion, which can lead to fiber–matrix delamination. Here, in this work, we have designed dynamic fiber–matrix interfaces to allow tough and closed-loop recyclable GFRPs by utilizing a vitrimer, derived from upcycled polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene (SEBS) with boronic ester (S-Bpin) and amine-based diol crosslinker. The boronic ester groups in S-Bpin form dynamic covalent bonds with the naturally present hydroxyl groups on the unsized GF surface, which eliminates the need for fiber sizing and enables facile closed-loop recyclability of both the fibers and the vitrimer matrix. The resulting strong fiber–matrix interface, depicted by the Raman mapping, leads to a 552% increase in-plane shear toughness (6.2 ± 0.3 MJ m -3 ) and 27% ultimate tensile strength (361 ± 89.2 MPa) compared to those of the conventional epoxy-based matrix (0.95 ± 0.05 MJ m -3 and 264 ± 59.7 MPa, respectively). The network rearrangement through dynamic boronic ester exchange enables fast thermoformability and repairability of micro-cracks at elevated temperatures. Additionally, both the matrix and composite demonstrate strong adhesion to various surfaces including steel and glasses exhibiting ≥6 MPa lap shear strength, which expands their suitability for diverse industrial applications. The readily created dynamic interface between boronic ester functionalized vitrimer and neat GFs presents a promising strategy for developing closed-loop recyclable, multifunctional structural materials, offering a sustainable alternative to non-recyclable thermoset GFRPs and contributes to a circular economy in composite materials.

36 MATERIALS SCIENCE↗

Shrinkage, microstructure, and mechanical properties of sintered 3D-printed silica via stereolithography

Stereolithography has been used to create ceramic parts with complex geometry that is difficult to achieve with conventional fabrication techniques. Here this study used stereolithography to print silica honeycomb structures with a commercial Formlabs Form2 printer. The printed samples were sintered at different temperatures, and the print shape was retained up to 1300°C, but significant distortion from partial melting occurred at 1400°C. Higher sintering temperatures lead to more shrinkage, but it is non-uniform among directions, with the open cell plane shrinking more than the dense plane of the sample. As expected, the density of samples also increases with the sintering temperature. At higher sintering temperatures, there is an increase in cristobalite and a decrease in quartz, tridymite, and amorphous silica. Regarding mechanical properties, the out-of-plane compressive strength is approximately one order of magnitude higher than the in-plane compressive strength. When compressed along the out-of-plane direction, the samples sintered at lower temperatures surprisingly exhibit higher strength, which is explained by the micro-cracking mechanism. As expected, the samples sintered at higher temperatures display higher strength when compressed along the in-plane direction.

36 MATERIALS SCIENCE↗

Understanding Carbon Dioxide Transfer in Direct Methanol Fuel Cells Using a Pore-Scale Model

Abstract The gas flow of carbon dioxide from the catalyst layer (CL) through the microporous layer (MPL) and gas diffusion layer (GDL) has great impacts on the water and fuel management in direct methanol fuel cells (DMFCs). This work has developed a liquid–vapor two-phase model considering the counter flow of carbon dioxide gas, methanol, and water liquid solution in porous electrodes of DMFC. The model simulation includes the capillary pressure as well as the pressure drop due to flow resistance through the fuel cell components. The pressure drop of carbon dioxide flow is found to be about two to three orders of magnitude higher than the pressure drop of the liquid flow. The big difference between liquid and gas pressure drops can be explained by two reasons: volume flowrate of gas is three orders of magnitude higher than that of liquid; only a small fraction of pores (<5%) in hydrophilic fuel cell components are available for gas flow. Model results indicate that the gas pressure and the mass transfer resistance of liquid and gas are more sensitive to the pore size distribution than the thickness of porous components. To buildup high gas pressure and high mass transfer resistance of liquid, the MPL and CL should avoid micro-cracks during manufacture. Distributions of pore size and wettability of the GDL and MPL have been designed to reduce the methanol crossover and improve fuel efficiency. The model results provide design guidance to obtain superior DMFC performance using highly concentrated methanol solutions or even pure methanol.

Electrochemistry↗