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Diode manufactured by Micro Semiconductor and Semtech were tested. Main failure mode was surface inversions caused by leakage of contaminants through cracks in glass. Most failures in groups 2 and 3 were visual.
Solid-state batteries (SSBs) with silicon anodes could enable improved safety and energy density compared to lithium-ion batteries. However, degradation arising from the massive volumetric changes of silicon anodes during cycling is not well understood in solid-state systems. Here, we use operando X-ray computed microtomography to reveal micro- to macro-scale chemo-mechanical degradation processes of silicon anodes in SSBs. Mud-type channel cracks driven by biaxial tensile stress form across the electrode during delithiation. We also find detrimental cracks at the silicon/ solid electrolyte interface that form due to local reaction competition between neighboring domains of different sizes. Continuum phase-field damage modeling quantifies stress-driven channel cracking and shows that the lithiated silicon stress state is critical for determining the extent of interfacial fracture. This work reveals the mechanisms that govern SSBs compared to conventional lithium-ion batteries and provides guidelines for engineering chemomechanically resilient electrodes for high-energy batteries.
A preliminary investigation was conducted to assess the feasibility of monitoring acoustic emission signals from fatigue cracks during cyclic bend tests. Plate specimens of 6A1-4V titanium, 2219-T87 aluminum, and 18-Ni maraging steel were tested with and without crack starter notches. It was found that significant acoustic emission signals could be detected in the frequency range from 100 kHz to 400 kHz. Cracks emanating from starter notches were monitored by the ultrasonic pulse-echo technique and periodically measured by micro-optical examination. Methods used to reduce the effects of extraneous noises (i.e., machine noises, fretting) are described. A frequency spectrum analyzer was used to characterize the emissions and to evaluate methods used to acquire the signals (i.e., transducer location, bandwidth selection). The investigation indicated that it was possible to extract meaningful acoustic emission signals in a cyclic bend machine environment.
A preliminary investigation was conducted to assess the feasibility of monitoring acoustic emission signals from fatigue cracks during cyclic bend tests. Plate specimens of 6Al-4V titanium, 2219-T87 aluminum, and 18-Ni maraging steel were tested with and without crack starter notches. It was found that significant acoustic emission signals could be detected in the frequency range from 100 to 400 kHz. Cracks emanating from starter notches were monitored by the ultrasonic pulse-echo technique and periodically measured by micro-optical examination. The investigation indicated that it was possible to extract meaningful acoustic emission signals in a cyclic bend machine environment.
Fuel cell heavy-duty vehicles (HDVs) require increased durability of oxygen-reduction-reaction electrocatalysts, making knowledge of realistic degradation mechanisms critical. Here identical-location micro-X-ray fluorescence spectroscopy was performed on membrane electrode assemblies. The results exposed heavy in-plane movement of electrocatalyst after HDV lifetime, suggesting that electrochemical Ostwald ripening may not be a local effect. Development of local loading hotspots and preferential movement of electrocatalyst away from cathode catalyst layer cracks was observed. The heterogeneous degradation exhibited by a modified cathode gas diffusion layer membrane electrode assembly after HDV lifetime was successfully quantified by the identical-location approach. Further synchrotron micro-X-ray diffraction and micro-X-ray fluorescence experiments were performed to obtain the currently unknown correlation between electrocatalyst nanoparticle size increase and loading change. A direct correlation was discovered which developed only after HDV lifetime. Finally, the work provides a route to engineer immediate system-level mitigation strategies and to develop structured cathode catalyst layers with durable electrocatalysts.
All levels of the unique hierarchical structure of bone, consisting of collagen and hydroxyapatite crystals at the nanoscale to osteon/lamellae structures at the microscale, contribute to its characteristic toughness and material properties. Elements of bone's density and size contribute to bone quantity (or bone mass), whereas elements of bone's material composition, material properties, internal structure, and organization describe bone quality. Furthermore, bone quantity and quality can be degraded by factors such as aging, disease, treatments, and irradiation, compromising its ability to resist fracture and sustain loading. Accessing the morphology and architecture of bone at the microscale to quantify microstructural features and assess the degree of mineralization and path of crack propagation in bone provides crucial information on how these factors are influencing bone quantity and quality. Synchrotron radiation micro-computed tomography (SRμCT) was first used to assess bone structure at the end of the 1990's. One of the main advantages of the technique is that it enables accurate three-dimensional (3D), non-destructive quantification of structure while traditional histomorphometry on histological sections is inherantly destructive to the sample and two-dimensional (2D). Additionally, SRμCT uses monochromatic, high-flux X-ray beams to provide high-resolution and high-contrast imaging of bone samples. This allows the quantification of small microstructural features (e.g. osteocyte lacunae, canals, trabeculae, microcracks) and direct gray value compositional mapping (e.g. mineral quantification, cement lines) with greater speed and fidelity than lab-based micro-computed tomography. In this article, we review how SRμCT has been applied to bone research to elucidate the mechanisms by which bone aging, disease, and other factors affect bone fragility and resistance to fracture.
Teflon(registered trademark) FEP (fluorinated ethylene-propylene) is commonly used on exterior spacecraft surfaces in the low Earth orbit (LEO) environment for thermal control. Silverized or aluminized FEP is used for the outer layer of thermal control blankets because of its low solar absorptance and high thermal emittance. FEP is also preferred over other spacecraft polymers because of its relatively high resistance to atomic oxygen erosion. Because of its low atomic oxygen erosion yield, FEP has not been protected in the space environment. Recent, long term space exposures such as on the Long Duration Exposure Facility (LDEF, 5.8 years in space), and the Hubble Space Telescope (HST, after 3.6 years in space) have provided evidence of LEO environmental degradation of FEP. These exposures provide unique opportunities for studying environmental degradation because of the long durations and the different conditions (such as differences in altitude) of the exposures. Samples of FEP from LDEF and from HST (retrieved during its first servicing mission) have been evaluated for solar induced embrittlement and for synergistic effects of solar degradation and atomic oxygen. Micro-indenter results indicate that the surface hardness increased as the ratio of atomic oxygen fluence to solar fluence decreased for the LDEF samples. FEP multilayer insulation (MLI) retrieved from HST provided evidence of severe embrittlement on solar facing surfaces. Micro-indenter measurements indicated higher surface hardness values for these samples than LDEF samples, but the solar exposures were higher. Cracks induced during bend testing were significantly deeper for the HST samples with the highest solar exposure than for LDEF samples with similar atomic oxygen fluence to solar fluence ratios. If solar fluences are compared, the LDEF samples appear as damaged as HST samples, except that HST had deeper induced cracks. The results illustrate difficulties in comparing LEO exposed materials from different missions. Because the HST FEP appears more damaged than LDEF FEP based on depth of embrittlement, other causes for FEP embrittlement in addition to atomic oxygen and ultraviolet (UV) radiation, such as thermal effects and the possible role of soft x-ray radiation, need to be considered. FEP that was exposed to soft x-rays in a ground test facility, showed embrittlement similar to that witnessed in LEO, which indicates that the observed differences between LDEF and HST FEP might be attributed to the different soft x-ray fluences during these two missions.
A micromechanics method is developed to investigate microcrack propagation in a liquid hydrogen composite tank at cryogenic temperature. The unit cell is modeled using square and hexagonal shapes depends on fiber and matrix layout from microscopic images of composite laminates. Periodic boundary conditions are applied to the unit cell. The temperature dependent properties are taken into account in the analysis. The laminate properties estimated by the micromechanics method are compared with empirical solutions using constituent properties. The micro stresses in the fiber and matrix phases based on boundary conditions in laminate level are calculated to predict the formation of microcracks in the matrix. The method is applied to an actual liquid hydrogen storage system. The analysis predicts micro stresses in the matrix phase are large enough to cause microcracks in the composite. Stress singularity of a transverse crack normal to a ply-interface is investigated to predict the fracture behavior at cryogenic conditions using analytical and finite element analysis. When a transverse crack touches a ply-interface of a composite layer with same fiber orientation, the stress singularity is equal to 1/2. When the transverse crack propagates to a stiffer layer normal to the ply-direction, the singularity becomes less than 1/2 and vice versa. Finite element analysis is performed to predict the fracture toughness of a laminated beam subjected to fracture loads measured by four-point bending tests at room and cryogenic temperatures. As results, the fracture load at cryogenic temperature is significantly lower than that at room temperature. However, when thermal stresses are taken into consideration, for both cases of room and cryogenic temperatures, the difference of the fracture toughness becomes insignificant. The result indicates fracture toughness is a characteristic property, which is independent to temperature changes. The experimental analysis is performed to investigate the effect of cryogenic cycling on permeability for various composite material systems. Textile composites have lower permeability than laminated composites even with increasing number of cryogenic cycle. Nano-particles dispersed in laminated composites do not show improvement on permeability. The optical inspection is performed to investigate the microcrack propagation and void content in laminated composites and compared the microscopic results before and after cryogenic cycling.
Abstract Cement is the prime barrier material to maintain zonal isolation during wellbore life-cycle. Different types of the cement have different performances on sealability. The primary objective of this study is evaluation of three types of cement systems, neat Class H, nano-synthetic graphite, and rock-based geopolymer cements, on interfacial bond integrity. Diametrical compressive tests are used on casing–cement–formation systems. Cement performances are tested in a conventional configuration (Berea Sandstone). A universal testing system is utilized to analyze the relationship applied load–axial strain and the digital image correlation (DIC) technique is used to generate the strain field maps. Based on the relationship and DIC results, bond strengths in different cement systems are evaluated. Additionally, microscope images provide insight explanations of the bond from micro-view. Based on the experimental results, failures of all cases initiate and propagate from the casing–cement interface. Then, radial cracks develop through the formation. This is because the mechanical interlocking bonds are formed only at the cement–sandstone interface to enhance the bond strength. The comparison of geopolymer and nano-modified cements with the conventional cement (neat Class H) shows that the unconventional cements have a lower maximum load and higher axial strain before failure of the samples. It indicates that both the two kinds of cements are more ductile than conventional cement and can support more deformation before the initiation of cracks.
Here, the dynamic cracking processes in porcine cortical bone were visualized in real-time using the high-speed synchrotron X-ray phase-contrast imaging (PCI) technique in three osteon orientations: in-plane transverse, out-of-plane transverse and in-plane longitudinal. The dynamic flexural loading applied on the pre-notched bone specimens was introduced by a modified Kolsky compression bar. High-speed X-ray images of the entire loading events were documented with a high-speed camera. Three-dimensional X-ray micro-computed tomography was conducted to examine the intact microstructures and obtain the basic material properties of the bone material used for mechanical characterizations. The onset location, where crack initiated, and the subsequent direction, along which the incipient crack propagated, were measured quantitatively using the high-speed X-ray images and the latter was found dependent on the osteon direction significantly. The crack propagation velocities were dependent on crack extension over the entire crack path significantly for all the three directions while the initial velocity for in-plane longitudinal direction was lower than the other two directions. Straight-through crack paths were observed for in-plane longitudinal specimens while the cracks were deflected and twisted in the in-plane transverse direction. For out-of-plane transverse direction, the cracks follow paths with tortuosity fall in between the other two directions, showing a mixed mode of fractures of the former two extreme cases. The toughening mechanisms, visualized by the high-speed X-ray images, and the corresponding fracture toughness, evaluated in terms of fracture initiation toughness and crack growth resistance curve (R-curve), were also found significantly different among the three osteon directions, suggesting an overall transition from brittle to ductile-like fracture behaviors at the dynamic displacement rate (5.4 m/s) as the osteon orientation varies from in-plane longitudinal to out-of-plane transverse, and to in-plane transverse eventually.
Oil and gas shales are a system where understanding the mechanical properties at the microscale is of paramount importance, e.g. to better understand the behavior of proppant-shale contacts and their role in the evolution of propped fractures in unconventional reservoirs. Here we show for the first time an experiment coupling indentation testing with in situ X-ray imaging in a Green River shale sample. A full compliance curve has been measured with the sample in water, allowing to visualize the indentation of the sample in function of axial load, in a purpose-built system for combined in situ indentation and X-ray imaging. A series of 3D datasets were used for a digital volume correlation study to obtain local strain fields. This analysis has been complemented with the analysis of cracks. Finally, geomechanical modeling has been carried out to replicate and generalize the observed behavior in the shale. This study validated this experimental approach, providing a breakthrough in understanding micro-mechanics in shales, and demonstrates how this class of experiments can be important for studies involving the prediction of the evolution of propped fractures in shale reservoirs, with possible applications in a much larger number of application fields (geothermal, materials science, etc.)
Fe-TiB 2 metal matrix composite, also called high-modulus steels (HMSs), are of great interest for applications in fuel-efficient transportation infrastructure, aerospace, and wear industries due to their high specific stiffness and yield strength. However, conventional cast Fe-TiB 2 HMSs often contain coarse and sharp-edged TiB 2 particles which easily trigger premature cracking during loading. Here, we synthesized a Fe-TiB 2 nanocomposite HMS via laser powder bed fusion (LPBF) additive manufacturing of mixed micro-sized powders of Fe, Ti, and Fe 2 B. We investigated the microstructure formation and mechanical behavior of the Fe-TiB 2 HMS. We found that in situ chemical reaction of Ti and Fe 2 B enables the formation of TiB 2 particles at nanoscale during rapid solidification of LPBF. These nanoscale TiB 2 particles can serve as heterogeneous nucleation sites and promote the formation of ultrafine and equiaxed α-Fe grains with random crystallographic textures, which differ from many other additively manufactured (AM) metal alloys characteristic of strong crystallographic textures. As such, isotropic mechanical properties were achieved in the AM Fe-TiB 2 nanocomposite HMS with a high elastic modulus of ~ 240 GPa, an exceptional yield strength of ~ 1450 MPa, and a large plasticity of ~ 20% under compression. Quantitative analysis reveals that the high yield strength primarily originates from strengthening contributions of the ultrafine grains with an average grain size of ~450 nm, the nanoscale TiB 2 reinforcing particles of 20–180 nm, and a high density of printing-induced dislocations of the order of 10 15 m –2 . In situ synchrotron high-energy X-ray diffraction unveils the load partitioning from the softer α-Fe matrix to the stiffer and stronger TiB 2 nanoparticles, contributing to the sustained strain hardening during compression. Our work not only provides a general pathway for achieving high-performance metal matrix nanocomposites by in situ chemical reaction and precipitation of ceramic nanoparticles during additive manufacturing, but also offers mechanistic insights into the deformation mechanism of nanoparticle-reinforced HMS composites.
A method for the signature analysis of pulses in the frequency domain and the time domain is presented. Fourier spectrum, Fourier transfer function, shock spectrum and shock spectrum ratio were examined in the frequency domain analysis, and pulse shape deconvolution was developed for use in the time domain analysis. Comparisons of the relative performance of each analysis technique are made for the characterization of acoustic emission pulses recorded by a measuring system. To demonstrate the relative sensitivity of each of the methods to small changes in the pulse shape, signatures of computer modeled systems with analytical pulses are presented. Optimization techniques are developed and used to indicate the best design parameters values for deconvolution of the pulse shape. Several experiments are presented that test the pulse signature analysis methods on different acoustic emission sources. These include acoustic emissions associated with: (1) crack propagation, (2) ball dropping on a plate, (3) spark discharge and (4) defective and good ball bearings. Deconvolution of the first few micro-seconds of the pulse train are shown to be the region in which the significant signatures of the acoustic emission event are to be found.
A method for the signature analysis of pulses in the frequency domain and the time domain is presented. Fourier spectrum, Fourier transfer function, shock spectrum and shock spectrum ratio were examined in the frequency domain analysis and pulse shape deconvolution was developed for use in the time domain analysis. Comparisons of the relative performance of each analysis technique are made for the characterization of acoustic emission pulses recorded by a measuring system. To demonstrate the relative sensitivity of each of the methods to small changes in the pulse shape, signatures of computer modeled systems with analytical pulses are presented. Optimization techniques are developed and used to indicate the best design parameter values for deconvolution of the pulse shape. Several experiments are presented that test the pulse signature analysis methods on different acoustic emission sources. These include acoustic emission associated with (a) crack propagation, (b) ball dropping on a plate, (c) spark discharge, and (d) defective and good ball bearings. Deconvolution of the first few micro-seconds of the pulse train is shown to be the region in which the significant signatures of the acoustic emission event are to be found.
Electrical resistivity (ER) measurements are a possible health monitoring technique for CMC components in future aerospace applications. In order to use ER measurements to detect and identify damage, it is necessary to understand how each specific damage state will affect the ER response. In this paper, finite element models are developed and applied to quantify the effect of specific damage states on the electrical resistivity response in a melt-infiltrated silicon carbide (SiC) fiber-reinforced silicon carbide composite. The electrical resistivity of several damage states are calculated by simulating the electric current flow through the damaged micro-structure. This is achieved by performing the numerical solution of the steady-state conservation of charge density equation. Numerical results reveal that cracking of the inter-tow matrix has the most profound effect on the composite electrical resistivity. Also, fiber/matrix debonding at matrix cracks in the 0° tows (tows aligned with the loading direction) may cause a significant increase in the electrical resistivity, but only if the fiber coating resistivity is 1000 Ω-cm or less. Cracks in the 90° tows and the crack opening displacement have very little effect on the composite electrical resistivity.
Wind power plant operations and maintenance (O&M) costs remain an appreciable contributor to the overall cost of wind energy. Premature of wind turbine gearboxes failures are often a result of abrasive wear, micropitting, scuffing, white-etch cracks, and macropitting issues. Micropitting is a fatigue phenomenon that occurs in Hertzian contacts in both gears and rolling-element bearings that operate in mixed or micro elastohydrodynamic lubrication regimes. Micropitting is influenced by and manifests itself in many different ways depending on operating conditions such as load, speed and operating temperature, and on factors such as gear geometry and accuracy, tooth flank roughness, percentage of tooth sliding, and lubricant composition. Despite much research by many investigators, micropitting remains complex, unpredictable, and difficult to control and remains a problem in wind turbine gearboxes. The purpose of this report is to document and describe the micropitting damage observed in a wind turbine gearbox, thereby facilitating further analysis and examination in future reports.
This report summarizes the activities performed in FY-25 to support fuel performance modeling for the Advanced Gas Reactor (AGR) Fuel Development and Qualification Program. This includes implementation of a new uranium oxycarbide (UCO) kernel swelling rate model, inner pyrolytic carbon (IPyC) cracking behavior and failure predictions, development of new UCO and silicon carbide (SiC) cesium diffusion parameters, and the thermomechanical behavior of particle layers using experimental data from micro-tensile strength testing.
The drying of cement-based materials is intimately related to their durability, which has significant economic, social and environmental repercussions. The evolution of the saturation of the pore network and the associated drying shrinkage are in fact leading causes of cracking and of the ensuing penetration of aggressive chemicals. This process is highly heterogeneous, due to the thermo-hydric spatial gradients developing in the material from the exposed surfaces to its core and because of local effects, driven by the intrinsically heterogeneous micro-structure (e.g., by the distribution of pores and aggregates). It follows that macroscopic, sample-scale measurements cannot fully disclose the complexity of the underlying processes. In the last few decades, significant advances in full-field techniques have allowed an unprecedented insight into these local processes. For cement-based materials, x-ray and neutron tomography lend themselves as ideal, and highly complementary, tools for the study of their thermo-hydro-mechanical behavior. Notably, the high sensitivity to density variations of x-ray imaging gives access to the developments of fractures, in 4D (3D + time). On the other hand, neutron tomography allows the study of the evolution of the moisture field in 4D, thanks to its high hydrogen sensitivity. The combination of these two techniques provides a unique insight in thermo-hydro-mechanical couplings, e.g., the effect of cracks on the water content field. This contribution presents novel 5D datasets (3D tomographies along time, plus truly simultaneous x-ray and Neutron rapid acquisitions) in-operando of a cement paste and of a concrete sample heated at moderate temperatures (up to 140{sup ∘}C). The analysis of this 5D data-set (once aligned in time and across modalities) allows for example a quantification of the 4D moisture profiles which were found to predict an overall water loss at hydric equilibrium coherent with the corresponding analytical analysis. In the cement paste sample, the x-ray dataset captures the evolution of an extensive cracking network, opening and propagation toward the core of the sample. A novel analysis procedure is here proposed which allows the extraction of these fractures and the analysis of their interplay with local drying as captured through neutron imaging. This for example reveals the depth of penetration of drying in the vicinity of the fractures along time, which is essential for the assessment and calibration of hydro-mechanical coupled models.