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NASA NTRS2020

Asteroid Cooling Rates Indicated by K-Feldspar Exsolution Textures in H4 Ordinary Chondrites

Undisturbed thermal metamorphism in ordinary chondrite (OC) asteroids, produced through the radioactive decay of 26Al, is expected to result in an onion-shell-like structure. In such a structure, the inner layers of the asteroid experience more extensive thermal metamorphism, as represented by higher petrologic type, than the exterior layers. Furthermore, cooling rates are expected to be slower for OCs of high petrologic type than those of low petrologic type. However, cooling rates determined using metallographic methods and pyroxene diffusion are inconsistent with onion-shell-style cooling and have resulted in new models. These models argue for the disruption of the asteroid after peak metamorphism followed by reaccretion into a rubble pile. Improved constraints on cooling rates would provide a better understanding of the timing and scale of disruptive events. Feldspar microtextures are another tool that can be used to determine asteroid cooling rates. In OC chondrules, plagioclase is present as either a primary phase, or a secondary phase forming from the crystallization of mesostasis glass through petrologic type 4, followed by chemical and textural equilibration. Potas-sium feldspar is observed in petrologic types 3.6-6, as either patches or lamellae exsolved from albite in a perthite texture, often near pores or fractures. Exsolution occurs most commonly, and most extensively, in petrologic type 4. Because the feldspar exsolution wavelength is related to the rate at which grains cooled from the solvus temperature, determined from the mineral’s bulk composition, the chondrite cooling rate can be measured from regions of exsolution. We have previously reported the perthite exsolution cooling rate of Avanhandava, an H4 chondrite, to be 1 °C per 1-4 months over a temperature interval of 765-670 °C. A peristerite exsolution texture was also present in the Na-rich lamellae for which we estimated a cooling rate of 1 °C in 103-104 years from 570-540 °C. Overall, the cooling rates determined from Avanhandava are consistent with pyroxene diffusion (fast cooling at high temperatures) and metallographic rates (slow cooling at low temperatures), hence with the rubble pile model of disruption and reaccretion. Here, we characterize feldspar microtextures in four additional H4 chondrites to test the consistency of feldspar cooling rates across a range of samples. We show that all H4s are similar and support rubble pile models.

Lewis, J. A.↗

NASA NTRS1994

The Large Impact Process Inferred from the Geology of Lunar Multiring Basins

The study of the geology of multiring impact basins on the Moon over the past ten years has given us a rudimentary understanding of how these large structures have formed and evolved on the Moon and other bodies. Two-ring basins on the Moon begin to form at diameters of about 300 km; the transition diameter at which more than two rings appear is uncertain, but it appears to be between 400 and 500 km in diameter. Inner rings tend to be made up of clusters or aligned segments of massifs and are arranged into a crudely concentric pattern; scarp-like elements may or may not be present. Outer rings are much more scarp-like and massifs are rare to absent. Basins display textured deposits, interpreted as ejecta, extending roughly an apparent basin radius exterior to the main topographic rim. Ejecta may have various morphologies, ranging from wormy and hummocky deposits to knobby surfaces; the causes of these variations are not known, but may be related to the energy regime in which the ejecta are deposited. Outside the limits of the textured ejecta are found both fields of satellitic craters (secondaries) and light plains deposits. Impact melt sheets are observed on the floors of relatively unflooded basins. Samples of impact melts from lunar basins have basaltic major-element chemistry, characterized by K, rare-earth elements (REE), P, and other trace elements of varying concentration (KREEP); ages are between 3.8 and 3.9 Ga. These lithologies cannot be produced through the fusion of known pristine (plutonic) rock types, suggesting the occurrence of unknown lithologies within the Moon. These melts were probably generated at middle to lower crustal levels. Ejecta compositions, preservation of pre-basin topography, and deposit morphologies all indicate that the excavation cavity of multiring basins is between about 0.4 and 0.6 times the diameter of the apparent crater diameter. Basin depths of excavation can be inferred from the composition of basin ejecta. A variety of mechanisms has been proposed to account for the formation of basin rings but none of them are entirely plausible. Mechanisms can be divided into two broad groups: (1) forcible uplift due to fluidization of the target; (2) concentric, brittle, fracturing and failure of the target, on regional (megaterraces) to global scales (lithospheric fracturing). Most basin rings are spaced at a constant factor on all planets. Evidence supports divergent ringforming models, so it may be that the ring-locating mechanism differs from the ring-forming mechanism. Thus, large-scale crustal foundering (megaterracing) could occur along concentric zones of weakness created by some type of resonant wave mechanism (fluidization and uplift); such immediate crustal adjustment could then be followed by long-term adjustment of the fractured lithosphere.

Spudis, Paul D.↗

DOE OSTI2024

Characterization of electromigration-induced short-range stress development in Al(0.25 at. % Cu) conductor line

Scanning x-ray microbeam topography and fluorescence experiments were conducted in situ to study the electromigration behavior of a 0.5 μm thick, 10 μm wide, and 200 μm long Al(0.25 at. % Cu) conductor line with 1.5 μm-thick SiO2 passivation on a single crystal Si substrate. The strain sensitivity of x-ray topography measurement allowed detailed examination of the electromigration-induced stress distribution and evolution in the conductor line in response to the depletion of Cu solute early in the electromigration process. Upon electromigration at 0.4 MA/cm2 and 303 °C, a short-range stress gradient was quickly induced by Al migration in the Cu-depleted cathode region to counteract further Al flow. The stress gradient was fully developed during the 5.3 h incubation time, extending over the critical Blech length of about 66 μm from the cathode end. Plastic deformation then occurred at the downstream end of the Cu-depleted region. The preferential electromigration of Cu did not cause detectable stress change outside the Cu-depleted region, except for the significant stress development from the Al2Cu precipitation at the anode end which appeared to initiate the fracture in the passivation. Preliminary finite difference modeling was undertaken to simulate the experimental observations, from which important parameters dictating electromigration in Al(Cu) line were extracted: an apparent effective valence of −5.6 and −1.9 for Cu and Al in Al(Cu), respectively, and a critical Cu concentration of 0.16 at. % above which Al grain boundary diffusion is effectively blocked.

Physics↗

DOE OSTI2025

Assessment of buffer-IPyC thermomechanical debonding behavior using new experimental strength data in BISON

TRIstructural ISOtropic (TRISO) fuel is a nuclear fuel commonly used in High Temperature Gas-cooled Reactors (HTGRs). A single sub-millimeter-diameter TRISO fuel particle consists of a spherical fuel kernel surrounded by four coating layers: a low-density pyrocarbon buffer layer, an inner pyrolytic carbon (IPyC) layer, a silicon carbide (SiC) layer, and an outer pyrolytic carbon (OPyC) layer. The kernel is commonly made of UO2 or a mixture of uranium carbide and uranium oxide (UCO). During reactor operation, the TRISO coating layers are subjected to irradiation-induced dimensional changes and the associated thermomechanical behavior of each layer. One of the observed behaviors is gap formation between the buffer and IPyC layer due to the porous buffer’s irradiation-induced shrinkage exceeding that of the IPyC layer. Not all irradiated particles will experience buffer-IPyC gap formation. The debonding may be partial, or it may be nearly total. However, from post-irradiation examination of UCO TRISO fuels irradiated as part of the Advanced Gas Reactor (AGR) Fuel Development and Qualification Program, it was concluded that partial buffer-IPyC debonding was the most common type of buffer-IPyC interaction. To predict TRISO thermomechanical performance, multi-physics models have been built that are being continually updated and refined. The BISON code is a finite element-based nuclear fuel performance code that may be used for 1D, 2D, and 3D TRISO particle simulations. This code is used to calculate fuel temperature, kernel swelling, buffer densification, thermal and irradiation creep, fracture, and fission gas production and release. One of the recent additions to the BISON code is the ability to model the process of layer debonding. This paper will focus on the simulation results of the improved BISON debonding model that will utilize updated strengths measured from irradiated AGR TRISO fuel particles. The new experimental strength data from micromechanical tests of irradiated TRISO fuel samples were exercised in the BISON simulations and compared to baseline strength data to assess their applicability in the models. This also includes updated buffer-IPyC bond strengths to simulate layer delamination. Based on current experimental observations it is noted that the buffer-IPyC separation occurs not exactly at the junction of these two layers, but more on the side of the buffer layer. That observation is also implemented in the TRISO interface debonding model. This improved modeling approach using experimental strength data to characterize buffer-IPyC debonding and its potential subsequent cracking will be presented in the paper along with comparisons to available experimental observations.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

On the thermal coarsening and transformation of nanoscale oxide inclusions in 316L stainless steel manufactured by laser powder bed fusion and its influence on impact toughness

The thermal evolution of nanoscale oxide inclusions in 316L stainless steel (SS) manufactured by laser powder bed fusion additive manufacturing (AM) was explored. The size, chemical composition, morphology, and distribution of the oxides were characterized as the function of heat treatment conditions. The study revealed the mechanistic driving force of the rapid oxide coarsening during recrystallization. Ostwald ripening governs oxide coarsening. The active grain boundary-oxide interaction at the early stage of recrystallization accelerated oxide coarsening via enhanced solute diffusion along grain boundaries. Pipe diffusion along dislocation cellular boundaries has a negligible contribution to oxide coarsening. At high temperatures (T> 1065 °C), although lattice diffusion primarily controlled the oxide growth, the contribution from the grain-boundary diffusion was necessary. The transformation from MnSiO 3 to CrMn 2 O 4 took place in the un-recrystallized grains but was not observed when recrystallization started. The interaction of grain boundary and oxides during recrystallization resulted in a high fraction of oxides accumulated at grain boundaries. While oxide coarsening does not significantly alter the toughness value, grain-boundary oxides promote microvoid formation and intergranular fracture under Charpy impact in the recrystallized AM 316L SS.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Fracture Toughness and Fatigue Crack Growth Rate Testing of Baffle-Former Bolts Harvested from a Westinghouse Two-Loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP) has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation displacement damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long-term irradiation behavior and compared to results obtained in high flux experimental reactor conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Microstructural evolution in a precipitate-hardened (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 multi-principal element alloy during high-pressure torsion

Multi-principal element alloys demonstrate high strength, thermal stability, and irradiation resistance, making them excellent candidate materials for applications in nuclear reactors and other harsh environments. Some studies have examined the use of high-pressure torsion to strengthen MPEAs through grain size reduction and strain hardening. However, no studies have investigated the effect of HPT on secondary phases (precipitates) within an MPEA. Two alloys, (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 containing Ni(Ti, Al) B2 phase, and CrFe σ phase, and single-phase Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , were fabricated by casting and heat treatment. Both alloys were then processed with HPT to study microstructural evolution. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the alloys before and after HPT processing. HPT processing produced a nanocrystalline structure in both alloys, but (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 exhibited a significantly smaller grain size and higher dislocation density than Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 , with corresponding higher hardness. Before HPT, the (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 94 Ti 2 Al 4 alloy consisted of large grain (~ 400 μm) and precipitates, including B2 of ~ 38 μm average size, B2 of ~ 0.7 μm average size, and small amounts of σ of ~ 1.5 μm average size. After HPT, the larger B2 precipitates were decreased in size and volume fraction, while the smaller B2 precipitates were completely dissolved; the σ precipitates appeared unaffected by HPT, likely due to their much higher hardness. Finally, observation of the B2 precipitate distribution along radial distance indicates that the strain caused the precipitates to fracture at intermediate strain (γ = 125) and dissolve at high strain (γ = 280).

36 MATERIALS SCIENCE↗

DOE OSTI2025

Tribological behavior of spark plasma sintered Ti 3 SiC 2 MAX phase composites

Ti₃SiC₂ MAX phases are considered promising candidates for tribological applications; but, their low hardness (5-6 GPa) can lead to increased abrasive wear and higher wear rates. This study investigates the effect of incorporating hard SiC particles on microstructure, mechanical, and tribological behavior of Ti₃SiC₂-SiC-based MAX phase composites prepared using spark plasma sintering at 1400 °C, 40 MPa, 15-minute holding time. Phase and microstructural characterization of composites confirmed the formation of Ti₃SiC₂ MAX phase (90%) along with TiC as a minor phase (10%). For Ti₃SiC₂-SiC, homogeneous distribution of SiC grains within Ti₃SiC₂ matrix resulted in increased hardness from ~11.6 GPa to ~14.8 GPa; however, the flexural strength decreased from ~615 MPa to ~597 MPa due to coefficient of thermal expansion mismatch. Tribological behavior of Ti₃SiC₂-SiC MAX phase composites was assessed using unidirectional sliding ball-on-flat tests with a 52100 steel ball at different loads and a constant speed of 0.05 m/s. SiC reinforced composites exhibited a decreased friction coefficient from 0.39 to 0.29 and wear rates comparable to Ti₃SiC₂ (7-10×10⁻³ mm³/N·m). SEM and EDS analysis of the worn surfaces indicated material transfer from the steel ball counter body and its oxidation due to frictional heating, at lower loads (2N and 5N), whereas at higher load (10N), fracture of the transfer layer dominated, with the presence of microcracks, delamination, grain pull-outs, and wear debris. Improved mechanical properties and good adhesion of SiC with Ti₃SiC₂ matrix resulted in reduced microcracks and grain pull-outs, making Ti₃SiC₂-SiC/Steel tribo-pair more suitable for tribological applications.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Leveraging operational information from wastewater injection wells to evaluate CO 2 injection performance for carbon storage applications in the Appalachian Basin

Abstract Geologic parameters, geophysical logging, injection testing, and operational metrics from wastewater injection wells were integrated to develop a preliminary design of a carbon storage facility in the Appalachian Basin. A scattered group of 10–20 commercial wastewater injection wells dispose off produced water from oil and gas wells in the region, utilizing a sequence of stacked deep saline formations for injection zones. These wastewater injection wells provide practical benchmarks for understanding the feasibility of carbon dioxide (CO 2 ) storage. Geologic models were developed based on characterization data from the wastewater injection wells. Reservoir simulations were calibrated according to injection testing and operational data from the wastewater injection wells. Long‐term operational data on injection flow rates and pressures measured in the wastewater injection wells were especially useful to evaluate the performance of carbon storage applications. The simulations were used to estimate injection pressures, radius of CO 2 saturation, and pressure response for industrial scale CO 2 storage applications. Results were also used to provide a design basis in terms of number of injection wells, well spacing, area of review, injection system components, monitoring plan, and CO 2 pipeline distribution system. The analysis demonstrates that there is sufficient injectivity in the deep saline formations in the west‐central Appalachian Basin to store commercial volumes of anthropogenic CO 2 . The geologic system appears suitable for supporting CO 2 injection rates of 0.5–1.0 million metric tons per year at injection pressures below formation fracture pressure in a single well. The long‐term operational data of wastewater injection wells within the study area suggested a lower permeability‐thickness values than indicated by initial reservoir tests. A workflow for developing realistic permeability values for input into reservoir simulations is presented. © 2020 Society of Chemical Industry and John Wiley & Sons, Ltd.

Valluri, Manoj↗

NASA NTRS2014

Properties of Desert Sand and CMAS Glass

As-received desert sand from a Middle East country has been characterized for its phase composition and thermal stability. X-ray diffraction analysis showed the presence of quartz (SiO2), calcite (CaCO3), gypsum (CaSO4.2H2O), and NaAlSi3O8 phases in as-received desert sand and showed weight loss of approx. 35 percent due to decomposition of CaCO3 and CaSO4.2H2O when heated to 1400 C. A batch of as-received desert sand was melted into calcium magnesium aluminosilicate (CMAS) glass at approx. 1500 C. From inductively coupled plasma-atomic emission spectrometry, chemical composition of the CMAS glass was analyzed to be 27.8CaO-4MgO-5Al2O3-61.6SiO2-0.6Fe2O3-1K2O (mole percent). Various physical, thermal and mechanical properties of the glass have been evaluated. Bulk density of CMAS glass was 2.69 g/cc, Young's modulus 92 GPa, Shear modulus 36 GPa, Poisson's ratio 0.28, dilatometric glass transition temperature (T (sub g)) 706 C, softening point (T (sub d)) 764 C, Vickers microhardness 6.3 +/- 0.4 GPa, indentation fracture toughness 0.75 +/- 0.15 MPa.m (sup 1/2), and coefficient of thermal expansion (CTE) 9.8 x 10 (exp -6)/degC in the temperature range 25 to 700 C. Temperature dependence of viscosity has also been estimated from various reference points of the CMAS glass using the Vogel-Fulcher-Tamman (VFT) equation. The glass remained amorphous after heat treating at 850 C for 10 hr but crystallized into CaSiO3 and Ca-Mg-Al silicate phases at 900 C or higher temperatures. Crystallization kinetics of the CMAS glass has also been investigated by differential thermal analysis (DTA). Activation energies for the crystallization of two different phases in the glass were calculated to be 403 and 483 kJ/mol, respectively.

Desert sand↗

DOE OSTI2023

The Linkage Between Electro-Chemical Mechanical Instabilities in Battery Materials

Battery chemistry must be diversified to achieve a sustainable energy landscape by effectively utilizing renewable energy sources. Alkali metal-ion, all-solid-state, metal–air batteries, and multivalent batteries offer unique cost, safety, raw material abundance, energy, and power density solutions. However, realizing these “beyond Li-ion batteries” must uncover their working principles and performance & property relationships. In this aspect, mitigating chemo-mechanical instabilities in the structure and surface of the electrodes plays a crucial role in their performance. Unfortunately, the coupling between electrochemical and mechanical interactions is often poorly understood due to a lack of operando characterization. Here, this review article explains the working principles of curvature measurement and digital image correlation for measuring stress and strain generations in battery materials. We provided specific examples of how these operando mechanical measurements shed light on instabilities in alkali metal ion electrodes, solid electrolytes, Li-O 2 batteries, and aqueous Zn-ion batteries. Operando mechanical measurements offer an effective way to map changes in the physical fingerprint of the battery materials, therefore providing crucial information to elucidate instabilities in battery materials.

25 ENERGY STORAGE↗

NASA NTRS1998

Development and Characterization of SiC)/ MoSi2-Si3N4(p) Hybrid Composites

Intermetallic compound MoSi2 has long been known as a high temperature material that has excellent oxidation resistance and electrical/thermal conductivity. Also its low cost, high melting point (2023 C), relatively low density (6.2 g/cu cm versus 9 g/cu cm for current engine materials), and ease of machining, make it an attractive structural material. However, the use of MoSi2 has been hindered due to its poor toughness at low temperatures, poor creep resistance at high temperatures, and accelerated oxidation (also known as 'pest' oxidation) at temperatures between approximately 450 and 550 C. Continuous fiber reinforcing is very effective means of improving both toughness and strength. Unfortunately, MoSi2 has a relatively high coefficient of thermal expansion (CTE) compared to potential reinforcing fibers such as SiC. The large CTE mismatch between the fiber and the matrix resulted in severe matrix cracking during thermal cycling. Addition of about 30 to 50 vol % of Si3N4 particulate to MoSi2 improved resistance to low temperature accelerated oxidation by forming a Si2ON2 protective scale and thereby eliminating catastrophic 'pest failure'. The Si3N4 addition also improved the high temperature creep strength by nearly five orders of magnitude, doubled the room temperature toughness and significantly lowered the CTE of the MoSi2 and eliminated matrix cracking in SCS-6 reinforced composites even after thermal cycling. The SCS-6 fiber reinforcement improved the room temperature fracture toughness by seven times and impact resistance by five times. The composite exhibited excellent strength and toughness improvement up to 1400 C. More recently, tape casting was adopted as the preferred processing of MoSi2-base composites for improved fiber spacing, ability to use small diameter fibers, and for lower cost. Good strength and toughness values were also obtained with fine diameter Hi-Nicalon tow fibers. This hybrid composite remains competitive with ceramic matrix composites as a replacement for Ni-base superalloys in aircraft engine applications.

Hebsur, Mohan G.↗

DOE OSTI2024

Stress Relaxation Cracking in 347H Stainless Steel Arc Welds: Susceptibility Evaluation of Heat-Affected Zone

Stress relaxation cracking (SRC) is considered one of the major failure mechanisms for 347H stainless steel welds at elevated service temperatures or during post weld heat treatment (PWHT), especially within the heat-affected zone (HAZ). This work focuses on the characterization of SRC susceptibility within 347H physically simulated arc welded HAZ at elevated temperatures. A four-step SRC thermomechanical test in combination with finite element modeling (FEM) of the welding and testing processes is developed to establish a susceptibility map for HAZ. The test first runs a thermal cycle with three different peak temperatures (1335, 1275, and 1150 °C) to duplicate representative HAZ subzone microstructures, followed by time-to-failure examination under a variety of pre-stress (260–600 MPa) and pre-strain conditions (0.03–0.19) as a function of reheat temperatures between 750 and 1050 °C. With the aid of FEM, SRC susceptibility maps are generated to identify the threshold stress, plastic strain, and creep strain as a function of test temperature. It was found out that HAZ subzone with a lower peak temperature (1150 °C) appears to be slightly less susceptible to SRC than the other two subzones that experienced higher peak temperatures. Generally, time-to-fracture reduces with increasing initially applied stress and strain for all test temperatures. The pre-stress thresholds decrease from about 500 to 330 MPa as the testing temperature increases from 800 to 1050 °C, while the corresponding initial plastic strain thresholds reduces from 0.15 to 0.06. The SRC susceptibility was also evaluated through the Larson–Miller Parameter (LMP) analysis as a function of plastic strain, initial stress and starting stress upon reaching the testing temperature, respectively. The 1050 °C test with a high pre-applied strain (0.1) exhibits an extremely short time to failure (t = 3 s) that lies outside the general trend in LMP analysis. Additionally, it was identified that a plastic strain above 0.07 is identified to significantly reduce the bulk creep strain tolerance to fracture and therefore increases SRC susceptibility. Hardness measurement and fractography analysis indicated that the strain aging of niobium carbonitrides and other potential phases in conjunction with intergranular precipitates contributes to an increase in microhardness and increased intergranular cracking susceptibility.

14 SOLAR ENERGY↗

DOE OSTI2022

Graphene coating on silicon anodes enabled by thermal surface modification for high-energy lithium-ion batteries

Silicon is a high-energy density anode material for lithium-ion batteries, but it possesses shortcomings such as poor electronic conductivity, interfacial instability and mechanical fracturing that hinder its battery cycling. Carbon coating has been an important strategy for stabilizing silicon anodes, but the effects of the silicon surface properties on carbon coating morphology and the consequent silicon cycling stability have not been clearly elucidated. Herein, we find that thermal oxidation of the silicon anodes followed by chemical vapor deposition of carbonaceous precursors leads to a well-ordered graphene coating, whereas disordered graphite coating is formed on the native silicon surface. Graphene-coated silicon exhibits superior cycling performance, retaining a discharge capacity of ~1300 mAh g -1 after 300 cycles, whereas the disordered graphite-coated silicon suffers continuous degradation, retaining only~600 mAh g -1 after 300 cycles. Cryogenic electron microscopy reveals the mechanism behind the difference in cycling stabilities; graphene coated silicon is able to withstand the large mechanical strains induced during extended cycling, whereas disordered graphite coating is ruptured, exposing silicon surfaces to the electrolyte, leading to extensive buildup of SEI and poor cycling performance. Characterization of the silicon surface reveals that thermal treatment yields an oxygen-rich surface layer, which is hypothesized to play a decisive role in dictating the carbon coating. This work highlights the effect of silicon surface properties on carbon coating microstructure, and presents thermal treatment as a facile avenue to attain graphene coating on silicon anodes.

25 ENERGY STORAGE↗

NASA NTRS2016

Evaluation of the Effect of Surface Finish on High-Cycle Fatigue of SLM-IN718

The surface finish of parts produced by additive manufacturing processes is much rougher than the surface finish generated by machining processes, and a rougher surface can reduce the fatigue strength of a part. This paper discusses an effort to quantify that reduction of strength in high-cycle fatigue for selective laser melt (SLM) coupons. A high-cycle fatigue (HCF) knockdown factor was estimated for Inconel 718, manufactured with the SLM process. This factor is the percentage reduction from the maximum stress in fatigue for low-stress ground (LSG) specimens to the maximum stress of those left with the original surface condition at the same fatigue life. Specimens were provided by a number of vendors, free to use their "best practice"; only one heat treat condition was considered; and several test temperatures were characterized, including room temperature, 800F, 1000F, and 1200F. The 1000F data had a large variance, and was omitted from consideration in this document. A first method used linear approximations extracted from the graphs, and only where data was available for both. A recommended knockdown factor of the as-built surface condition (average roughness of approximately 245 micro-inches/inch) versus low-stress ground condition (roughness no more than 4 micro-inches/inch) was established at approximately 1/3 or 33%. This is to say that for the as-built surface condition, a maximum stress of 2/3 of the stress for LSG can be expected to produce a similar life in the as-built surface condition. In this first evaluation, the knockdown factor did not appear to be a function of temperature. A second approach, the "KP method", incorporated the surface finish measure into a new parameter termed the pseudo-stress intensity factor, Kp, which was formulated to be similar to the fracture mechanics stress intensity factor. Using Kp, the variance seemed to be reduced across all sources, and knockdown factors were estimated using Kp over the range where data occurred. A plot of the results suggests that the knockdown factor is a function of temperature, and that for low lives the knockdown might be lower than the knockdown observed above about one million cycles, where it tended to stabilize. This was not universal for all temperatures tested. The higher temperature tests are thought to be influenced by the test temperature, which perhaps continued the aging process. Further evaluation of the method is suggested.

Lambert, D. M.↗

NASA NTRS2013

A Test for Characterizing Delamination Migration in Carbon/Epoxy Tape Laminates

A new test method is presented for the purpose of investigating migration of a delamination between neighboring ply interfaces in fiber-reinforced, polymer matrix tape laminates. The test is a single cantilever beam configuration consisting of a cross-ply laminate with a polytetrafluoroethylene insert implanted at the mid-plane and spanning part way along the length of the specimen. The insert is located between a 0- degree ply (specimen length direction) and a stack of four 90-degree plies (specimen width direction). The specimen is clamped at both ends onto a rigid baseplate and is loaded on its upper surface via a piano hinge. Tests were conducted with the load-application point located on the intact portion of the specimen in order to initiate delamination growth onset followed by migration of the delamination to a neighboring 90/0 ply interface by kinking through the 90-degree ply stack. Varying this position was found to affect the distance relative to the load-application point at which migration initiated. In each specimen, migration initiated by a gradual transition of the delamination at the 0/90 interface into the 90-degree ply stack. In contrast, transition of the kinked crack into the 90/0 interface was sudden. Fractography of the specimens indicated that delamination prior to migration was generally mixed mode-I/II. Inspection of the kink surface revealed mode-I fracture. In general, use of this test allows for the observation of the growth of a delamination followed by migration of the delamination to another ply interface, and should thus provide a means for validating analyses aimed at simulating migration.

Ratcliffe, James G.↗

DOE OSTI2023

Environmental impact of solution pH on the formation and migration of iron colloids in deep subsurface energy systems

Deep subsurface stimulation processes often promote fluid-rock interactions that can lead to the formation of small colloidal particles that are suspected to migrate through the rock matrix, partially or fully clog pores and microfractures, and promote the mobilization of contaminants. Thus, the goal of this work is to understand the geochemical changes of the host rock in response to reservoir stimulation that promote the formation and migration of colloids. Two different carbonate-rich shales were exposed to different solution pHs (pH = 2 and 7). In this study, iron and other mineral transformations at the shale-fluid interface were first characterized by synchrotron-based XRF mapping. Then, colloids that were able to migrate from the shale into the bulk fluid were characterized by synchrotron-based extended X-ray absorption structure (EXAFS), scanning electron microscopy (SEM), and single-particle inductively coupled plasma time-of-flight mass spectrometry (sp-icpTOF-MS). When exposed to the pH = 2 solution, extensive mineral dissolution and secondary precipitation was observed; iron-(oxyhydr)oxide colloids colocated with silicates were observed by SEM at the fluid-shale interfaces, and the mobilization of chromium and nickel with these iron colloids into the bulk fluid was detected by sp-icpTOF-MS. Iron EXAFS spectra of the solution at the shale-fluid interface suggests the rapid (within minutes) formation of ferrihydrite-like nanoparticles. Thus, we demonstrate that the pH neutralization promotes the mobilization of existing silicate minerals and the rapid formation of new iron colloids. These Fe colloids have the potential to migrate through the shale matrix and mobilize other heavy metals (such as Cr and Ni, in this study) and impacting groundwater quality, as well produced waters from these hydraulic fracturing operations.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Cubic-meter scale laboratory fault re-activation experiments to improve the understanding of induced seismicity risks

Abstract To understand fluid induced seismicity, we have designed a large-scale laboratory experiment consisting of a one-cubic-meter sandstone with an artificial fault cut and fluid-injection boreholes. The sandstone block is assembled in a true triaxial loading frame and equipped with 38 piezoelectric sensors to locate and characterise acoustic emission events. The differential stress on the artificial fault is increased in stages to bring it towards a critically stressed state. After each stage of differential stress increase, fluids are injected at low pressures through boreholes to test the potential of fault re-activation. In addition, a high-pressure injection was conducted that created a hydraulic fracture from the injection borehole towards the artificial fault. The newly generated fluid pathway resulted in an activation of the complete block through a stick–slip movement. We compare acoustic emission measurements from the laboratory experiment with seismicity observations from the field-scale CO 2 injection at Decatur, Illinois, U.S., and conclude that the existence of fluid pathways plays a decisive role for the potential of induced seismicity.

47 OTHER INSTRUMENTATION↗