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At least 1,117 records · Page 62

Physical properties of glasses exposed to Earth-facing and trailing-side environments on LDEF

The exposure of 108 glass samples and 12 glass-ceramic samples to Earth-orbit environments permitted measurements which establish the effects of each environment. Examination of five glass types and one glass ceramic located on both the Earth-facing side and the trailing edge revealed no reduction in strength within experimental limits. Strength measurements subjected less than 5 percent of the sample surface area to stresses above 90 percent of the glass's failure strength. Seven micrometeorite or space debris impacts occurred on trailing edge samples. One of those impacts occurred in a location which was subjected to 50 percent of the applied stress at failure. Micrometeorite or space debris impacts were not observed on Earth-facing samples. The physical shape and structure of the impact sites were carefully examined using stereographic scanning electron microscopy. These impacts induce a stress concentration at the damaged region which influences mechanical strength. The flaw size produced by such damage was examined to determine the magnitude of strength degradation in micrometeorite or space-debris impacted glasses. Scanning electron microscopy revealed topographical details of impact sites which included central melt zones and glass fiber production. The overall crater structure is similar to much larger impacts of large meteorite on the Moon in that the melt crater is surrounded by shocked regions of material which fracture zones and spall areas. Residual stresses arising from shock compression and cooling of the fused zone cannot currently be included in fracture mechanics analyses based on simple flaw size examination.

Wiedlocher, David E.↗

High Temperature High Vacuum Mechanical Property Assessment of Zirconium Nuclear Fuel Cladding

This report presents the mechanical characterization of a specific Zry-4 cladding batch serving as the foundation for a diverse range of fuel performance research at Oak Ridge National Laboratory (ORNL). This effort supports research needs for the U.S. Department of Energy (DOE), particularly regarding evaluating accident tolerant fuel (ATF) cladding coating concepts, expanding understanding of cladding response to loss-of-coolant accidents (LOCA) transients, refining post-critical heat flux (CHF) limits (t@T), and upcoming irradiation campaigns. The central objective was to define the baseline performance of the substrate Zircaloy-4 (Zry-4) material leveraged across ORNL Advanced Fuel Campaign (AFC) efforts through controlled high-temperature vacuum tensile testing. This work begins to address gaps in existing models where implementation based on nominal heat-treatment labels, such as stress relief annealed (SRA), often fail to capture the interplay of recovery, recrystallization, and grain growth. To quantify this, data was benchmarked against the Pacific Northwest National Laboratory (PNNL) stress strain model to determine where this material falls in comparison to assumed values for materials in the same heat treatment regime. Analysis of the tensile data revealed that this specific SRA batch exhibits a transitional microstructural state best described by an effective cold-work (CW) parameter of 0.09, diverging from the previous estimation of 0.5 for SRA materials. Additionally, comparative testing of Cr coated specimens demonstrated no distinct difference in axial strength relative to the bare substrate. This suggests that the strengthening benefits of Cr coatings observed in burst scenarios are driven by residual stress mechanisms acting solely in the hoop direction.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Elastic geothermobarometry: Corrections for the geometry of the host-inclusion system

Elastic geothermobarometry on inclusions is a method to determine pressure-temperature conditions of mineral growth independent of chemical equilibrium. Because of the difference in their elastic properties, an inclusion completely entrapped inside a host mineral will develop a residual stress upon exhumation, from which one can back-calculate the entrapment pressure. Current elastic geobarometric models assume that both host and inclusion are elastically isotropic and have an ideal geometry (the inclusion is spherical and isolated at the center of an infinite host). These conditions do not commonly occur in natural rocks, and the consequences for inclusion pressures can only be quantified with numerical approaches. In this paper, we report the results of numerical simulations of inclusions with the finite element method on elastically isotropic systems. We define and determine a geometrical factor (Γ) that allows measured residual pressures to be corrected for the effects of non-ideal geometry. We provide simple guidelines as to which geometries can safely be used for elastic geobarometry without correcting for the geometry. We also show that the discrepancies between elastic and conventional geobarometry reported in literature are not due to geometrical effects, and therefore result from other factors not yet included in current models.

58 GEOSCIENCES↗

Experimental and Finite Element Modeling of Near-Threshold Fatigue Crack Growth for the K-Decreasing Test Method

The experimental methods to determine near-threshold fatigue crack growth rate data are prescribed in ASTM standard E647. To produce near-threshold data at a constant stress ratio (R), the applied stress-intensity factor (K) is decreased as the crack grows based on a specified K-gradient. Consequently, as the fatigue crack growth rate threshold is approached and the crack tip opening displacement decreases, remote crack wake contact may occur due to the plastically deformed crack wake surfaces and shield the growing crack tip resulting in a reduced crack tip driving force and non-representative crack growth rate data. If such data are used to life a component, the evaluation could yield highly non-conservative predictions. Although this anomalous behavior has been shown to be affected by K-gradient, starting K level, residual stresses, environmental assisted cracking, specimen geometry, and material type, the specifications within the standard to avoid this effect are limited to a maximum fatigue crack growth rate and a suggestion for the K-gradient value. This paper provides parallel experimental and computational simulations for the K-decreasing method for two materials (an aluminum alloy, AA 2024-T3 and a titanium alloy, Ti 6-2-2-2-2) to aid in establishing clear understanding of appropriate testing requirements. These simulations investigate the effect of K-gradient, the maximum value of stress-intensity factor applied, and material type. A material independent term is developed to guide in the selection of appropriate test conditions for most engineering alloys. With the use of such a term, near-threshold fatigue crack growth rate tests can be performed at accelerated rates, near-threshold data can be acquired in days instead of weeks without having to establish testing criteria through trial and error, and these data can be acquired for most engineering materials, even those that are produced in relatively small product forms.

Smith, Stephen W.↗

Low Temperature Creep of Hot-Extruded Near-Stoichiometric NiTi Shape Memory Alloy: Effect of Thermal Cycling - Part 2

This paper is the first report on the effect prior low temperature creep on the thermal cycling behavior of NiTi. The isothermal low temperature creep behavior of near-stoichiometric NiTi between 300 and 473 K was discussed in Part I. The effect of temperature cycling on its creep behavior is reported in the present paper (Part II). Temperature cycling tests were conducted between either 300 or 373 K and 473 K under a constant applied stress of either 250 or 350 MPa with hold times lasting at each temperature varying between 300 and 700 h. Each specimen was pre-crept either at 300 or at 473 K for several months under an identical applied stress as that used in the subsequent thermal cycling tests. Irrespective of the initial pre-crept microstructures, the specimens exhibited a considerable increase in strain with each thermal cycle so that the total strain continued to build-up to 15 to 20 percent after only 5 cycles. Creep strains were immeasurably small during the hold periods. It is demonstrated that the strains in the austenite and martensite are linearly correlated. Interestingly, the differential irrecoverable strain, in the material measured in either phase decreases with increasing number of cycles, similar to the well-known Manson-Coffin relation in low cycle fatigue. Both phases are shown to undergo strain hardening due to the development of residual stresses. Plots of true creep rate against absolute temperature showed distinct peaks and valleys during the cool-down and heat-up portions of the thermal cycles, respectively. Transformation temperatures determined from the creep data revealed that the austenitic start and finish temperatures were more sensitive to the pre-crept martensitic phase than to the pre-crept austenitic phase. The results are discussed in terms of a phenomenological model, where it is suggested that thermal cycling between the austenitic and martensitic phase temperatures or vice versa results in the deformation of the austenite and a corresponding development of a back stress due to a significant increase in the dislocation density during thermal cycling.

Raj, S. V.↗

Summary of Activities for Health Monitoring of Composite Overwrapped Pressure Vessels

This three-year project (FY12-14) will design and demonstrate the ability of new Magnetic Stress Gages for the measurement of stresses on the inner diameter of a Composite Overwrapped Pressure Vessel overwrap. The sensors are being tested at White Sands Testing Facility (WSTF) where the results will be correlated with a known nondestructive technique acoustic emission. The gages will be produced utilizing Meandering Winding Magnetometer (MWM) and/or MWM array eddy current technology. The ultimate goal is to utilize this technology for the health monitoring of Composite Overwrapped Pressure Vessels for all future flight programs. The first full-scale pressurization test was performed at WSTF in June 2012. The goals of this test were to determine adaptations of the magnetic stress gauge instrumentation that would be necessary to allow multiple sensors to monitor the vessel's condition simultaneously and to determine how the sensor response changes with sensor selection and orientation. The second full scale pressurization test was performed at WSTF in August 2012. The goals of this test were to monitor the vessel's condition with multiple sensors simultaneously, to determine the viability of the multiplexing units (MUX) for the application, and to determine if the sensor responses in different orientations are repeatable. For both sets of tests the vessel was pressured up to 6,000 psi to simulate maximum operating pressure. Acoustic events were observed during the first pressurization cycle. This suggested that the extended storage period prior to use of this bottle led to a relaxation of the residual stresses imparted during auto-frettage. The pressurization tests successfully demonstrated the use of multiplexers with multiple MWM arrays to monitor a vessel. It was discovered that depending upon the sensor orientation, the frequencies, and the sense element, the MWM arrays can provide a variety of complementary information about the composite overwrapped pressure vessel load conditions. For example, low frequency measurements can be used to monitor the overwrap thickness and changes associated with pressure level. High frequency data is dominated by the properties of the overwrap, including the fiber orientations and lay-up of the layers.

Russell, Rick↗

Results of stainless steel canister corrosion studies and environmental sample investigations

This progress report describes work being done at Sandia National Laboratories (SNL) to assess the localized corrosion performance of container/cask materials used in the interim storage of used nuclear fuel. The work involves both characterization of the potential physical and chemical environment on the surface of the storage canisters and how it might evolve through time, and testing to evaluate performance of the canister materials under anticipated storage conditions. To evaluate the potential environment on the surface of the canisters, SNL is working with the Electric Power Research Institute (EPRI) to collect and analyze dust samples from the surface of in-service SNF storage canisters. In FY 13, SNL analyzed samples from the Calvert Cliffs Independent Spent Fuel Storage Installation (ISFSI); here, results are presented for samples collected from two additional near-marine ISFSI sites, Hope Creek NJ, and Diablo Canyon CA. The Hope Creek site is located on the shores of the Delaware River within the tidal zone; the water is brackish and wave action is normally minor. The Diablo Canyon site is located on a rocky Pacific Ocean shoreline with breaking waves. Two types of samples were collected: SaltSmart™ samples, which leach the soluble salts from a known surface area of the canister, and dry pad samples, which collected a surface salt and dust using a swipe method with a mildly abrasive ScotchBrite™ pad. The dry samples were used to characterize the mineralogy and texture of the soluble and insoluble components in the dust via microanalytical techniques, including mapping X-ray Fluorescence spectroscopy and Scanning Electron Microscopy. For both Hope Creek and Diablo Canyon canisters, dust loadings were much higher on the flat upper surfaces of the canisters than on the vertical sides. Maximum dust sizes collected at both sites were slightly larger than 20 μm, but Phragmites grass seeds ~1 mm in size, were observed on the tops of the Hope Creek canisters. At both sites, the surface dust could be divided into fractions generated by manufacturing processes and by natural processes. The fraction from manufacturing processes consisted of variably-oxidized angular and spherical particles of stainless steel and iron, generated by machining and welding/cutting processes, respectively. Dust from natural sources consisted largely of detrital quartz and aluminosilicates (feldspars and clays) at both sites. At Hope Creek, soluble salts were dominated by sulfates and nitrates, mostly of calcium. Chloride was a trace component and the only chloride mineral observed by SEM was NaCl. Chloride surface loads measured by the Saltsmart™ sensors were very low, less than 60 mg m –2 on the canister top, and less than 10 mg m –2 on the canister sides. At Diablo Canyon, sea-salt aggregates of NaCl and Mg-SO 4 , with minor K and Ca, were abundant in the dust, in some cases dominating the observed dust assemblage. Measured Saltsmart™ chloride surface loads were very low (<5 mg m –2 ); however, high canister surface temperatures damaged the Saltsmart™ sensors, and, in view of the SEM observations of abundant sea-salts on the package surfaces, the measured surface loads may not be valid. Moreover, the more heavily-loaded canister tops at Diablo Canyon were not sampled with the Saltsmart™ sensors. The observed low surface loads do not preclude chloride-induced stress corrosion cracking (CISCC) at either site, because (1) the measured data may not be valid for the Diablo Canyon canisters; (2) the surface coverage was not complete (for instance, the 45º offset between the outlet and inlet vents means that near-inlet areas, likely to have heavier dust and salt loads, were not sampled); and (3) CISCC has been experimentally been observed at salt loads as low as 5-8 mg/m 2 . Experimental efforts at SNL to assess corrosion of interim storage canister materials include three tasks in FY14. First, a full-diameter canister mockup, made using materials and techniques identical to those used to make interim storage canisters, was designed and ordered from Ranor Inc., a cask vendor for Areva/TN. The mockup will be delivered prior to the end of FY14, and will be used for evaluating weld residual stresses and degrees of sensitization for typical interim storage canister welds. Following weld characterization, the mockup will be sectioned and provided to participating organizations for corrosion testing purposes. A test plan is being developed for these efforts. In a second task, experimental work was carried out to evaluate crevice corrosion of 304SS in the presence of limited reactants, as would be present on a dustcovered storage canister. This work tests the theory that limited salt loads will limit corrosion penetration over time, and is a continuation of work carried out in FY13. Laser confocal microscopy was utilized to assess the volume and depth of corrosion pits formed during the crevice corrosion tests. Results indicate that for the duration of the current experiments (100 days), no stifling of corrosion occurred due to limitations in the amount of reactants present at three different salt loadings. Finally, work has been carried out this year perfecting an instrument for depositing sea-salts onto metal surfaces for atmospheric corrosion testing purposes. The system uses an X-Y plotter system with a commercial airbrush, and deposition is monitored with a quartz crystal microbalance. The system is capable of depositing very even salt loadings, even at very low total deposition rates.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Suppression of irradiation hardening in tungsten-coated ferritic steel for fusion reactor blanket applications

W-coated reduced activation ferritic steels have been developed for use as plasma facing components in fusion reactor blankets, offering excellent sputtering resistance and structural strength. Previous high-temperature coating methods, such as diffusion bonding and brazing, caused interfacial deterioration due to thermal stress from mismatched thermal expansion between W and reduced activation ferritic steel. To address this, underwater explosive welding was introduced as a high-velocity cold process that joins dissimilar materials while maintaining a strong, thin interface without the thermal issues associated with traditional methods. In this study, the effects of neutron irradiation on the hardness and microstructure in W-coated F82H reduced activation ferritic steel (W/F82H) joined by underwater explosive welding are investigated. Following neutron irradiation at 290 °C, irradiation hardening is suppressed in W, F82H, and their interface within the W/F82H material. Furthermore, microstructural observations indicate that the recovery of work hardening and relaxation of elastic strain introduced during coating significantly contribute to the suppression of irradiation hardening in W/F82H. In conclusion, W/F82H exhibits significantly suppressed irradiation hardening compared with those in stand-alone materials. This suppression is explained by residual stress from thermal expansion mismatch and the unique microstructure at the interface. These results provide valuable insights for the development of more durable materials in nuclear fusion applications.

36 MATERIALS SCIENCE↗

A FEASIBILITY STUDY ON CRACK REPAIR IN AUSTENITIC STAINLESS STEEL DRY STORAGE CANISTERS USING ISOTHERMAL FRICTION STIR WELDING

In recent time, solid state crack repair techniques in spent nuclear fuel dry storage canisters (SNF-DSC) have garnered significant interest. Plates of austenitic stainless steels are usually arc welded to fabricate the cylindrical canisters which are prone to chloride-induced stress corrosion cracking. Friction stir welding (FSW) is considered to be a potential candidate for damage repair. In this work, electrical discharge machining was used to simulate cracks in 304L stainless steel plates of 12.7 mm thickness. Subsequently, isothermal FSW was carried out at two different temperatures (725 and 825°C) in order to repair the simulated crack. Microstructure-mechanical property correlations in FSWed plates were studied in detail. Significant grain refinement observed in the stir zone (SZ) was attributed to dynamic recrystallization occurring during FSW. A comparison of Vickers microhardness showed higher hardness and homogeneity in the 725°C SZ than its 825°C counterpart. The fraction of S3 boundary is found to be low in the SZ as compared to base metal (BM). Yield strength of the joints was found to be approximately 100 MPa higher than that of the BM accompanied by a drop in ductility by a factor of 2. Residual stress profile across 825°C weld was measured using x-ray diffraction.

Bhattacharyya, Madhumanti↗

Cold Spray Deposition of 304L Stainless Steel to Mitigate Chloride-Induced Stress Corrosion Cracking in Canisters for Used Nuclear Fuel Storage

A feasibility study of the cold spray deposition process of 304L stainless steel on 304L stainless steel substrates as a mitigation method for chloride-induced stress corrosion cracking (CISCC) has been investigated under various substrate conditions. The study is aimed at the application of this technology to mitigate CISCC that may potentially occur in or nearthe fusion welded regions of stainless steel canisters in Dry Cask Storage System (DCSS) for used nuclear fuels. Spherical gas-atomized 304L stainless steel powder, in the size range of 25 µm to 44 µm, was used as a feedstock powder for the cold spray process. The powder was deposited on four types of 304L substrates with various surface conditions: as-polished, oxidized, cold-rolled, plates with prototypical CISCC. The effects of cold spray parameters on quality of cold spray coatings were investigated. Thickness, porosity, and phases in the as-deposited materials were evaluated using scanning electron microscopy (SEM) and X-ray diffraction (XRD), and correlated with microhardness and adhesion strength measured via micro-indentation and ASTM C633 pulling test, respectively. XRD analysis of the coatings was also conducted to examine the effects of cold spray condition on residual stress state in the coating. Detailed cross-sectional examination of coating/substrate interfaces was performed with transmission electron microscopy (TEM) equipped with energy dispersive spectroscopy (EDS). Dense and continuous coatings with good adhesion strength and hardness were produced for the various substrate conditions by adjusting cold spray parameters. The results demonstrate that cold spray stainless steel coating is a viable option to provide a physical barrier against CISCC in fusion weld regions of stainless steel in corrosive chloride salt-bearing environments.

Dry Cask Storage Systems, cold spray, 304L stainle↗

Irradiation-assisted cracking of SA508-304L weldments with 308L groove filler and 309L butter in hot water immersion constant rate extension tests

Low alloy SA508 bainitic steel is often welded to 300 series austenitic stainless steel in nuclear power plants. These dissimilar metal weldments use 309L butter applied to the low alloy steel and 308L groove filler material to join the 309L to austenite. High alloy steels (such as the 308L and 309L material used here) have been identified as having greater susceptibility to irradiation-assisted stress corrosion cracking (IASCC). Evidence is presented here of cracking under tensile loads in 309L weldment butter in LWR hydrothermal conditions that correlates irradiation induced changes at δ ferrite–γ austenite phase boundaries and γ–γ grain boundaries; specifically intergranular Cr 23 C 6 precipitates. Cracking is not observed in irradiated 308L groove filler under the same conditions. Both the 309L butter and 308L filler material have a duplex or mixed δ–γ phase microstructure due to solidification during the welding procedure. We have performed constant extension rate autoclave immersion tests in BWR normal water chemistry hot water (288 °C, 10 MPa, 2000 wt. ppb dissolved oxygen, <100 nS/cm conductivity, neutral pH) of proton irradiated (2 MeV, approximately 3 displacements per atom at a depth of 10 μm) tensile specimens. Proton irradiation to the dpa levels used here induced Cr 23 C 6 carbide precipitation at γ–γ grain boundaries and δ–γ phase boundaries in the 309L butter but not the 308L filler. Cracking was observed in the proton-irradiated volume of 309L at these interfaces in the vicinity of the Cr 23 C 6 precipitates. We hypothesis the SA508 is the source of carbon in the 309L butter. Cr depletion at γ–γ grain boundaries was also observed and may also be a root cause of cracking. Furthermore, the 309L butter is under significant tensile residual stress in the weldment that adds to applied tensile loads and this too may be a contributing factor.

309L weld butter↗

HIGH-STRENGTH LIGHTWEIGHT ENGINES FOR HEAVY-DUTY DIESEL TRUCKS

This project with Cummins supports the development of next generation heavy duty diesel engines that can achieve a 50% or better Break Thermal Efficiency (BTE). The fuel efficiency roadmap for the 50% BTE engine considers six main areas for efficiency improvement in the baseline engine, several of which involve making more efficient use of thermal energy (heat) in the engine. Increased operating temperatures and improved thermal management are expected to enable significant increases in $power$ $density$, thus resulting in greater power output for the same sized engine or engine downsizing (or light weighting) for the same power output. However, it has become apparent that several key components will be exposed to temperatures beyond the capabilities of current engine and exhaust materials, requiring the availability of the next generation of high temperature materials to allow the engine to reach the targeted efficiencies, commercially viable durability, and emission targets. The objective of this project was to identify and/or develop key materials, and evaluate their critical properties to enable the design and development of a lightweight, higher efficiency engine, with enhanced temperature capability and reduced heat-loss to the atmosphere in order to facilitate waste heat recovery and improved efficiency. An increase in the temperature capability of exhaust manifold materials, and piston materials were identified as having a positive influence on the efficiency of the next generation diesel engines. Since the current materials (High SiMo cast irons used in exhaust manifolds, and 4140 steel in pistons) are already operating near their limits of their temperature and strength capabilities, it was determined that new materials with the right combination of properties are required for these components. Oxidation and constrained thermal fatigue tests were used to down-select CF8C plus (CF8CP), a cast austenitic stainless steel, for exhaust manifolds capable of operating at higher temperatures. A prototype exhaust manifold was fabricated using CF8CP and successfully tested in a marine engine. A functionally graded multiple-layer thermal barrier coating system was designed with four layers of mixed bondcoat alloy (NiCoCrAlYHfSi) and yttria stabilized zirconia (YSZ) and was shown to reduce the effective thermal conductivity of the coating-substrate (steel and Ti-6Al-4V) system. The graded alloy and YSZ mixture were intended to achieve better match of thermal expansion coefficient (CTE) and minimize thermal stresses. Such coatings can increase the temperature capability of pistons fabricated from steel and Ti-alloys. Effect of oil additives and friction conformal contact friction tests showed there was a 15-30% reduction in friction by the polymer-graphite composite coating compared to the uncoated steel piston. Standalone Mn-P coating had little beneficial impact. Changing the oil from CJ-4 to PC-11 had little impact on the friction behavior in boundary lubrication. Wear behavior was tested under a point contact configuration with a high contact pressure. The candidate CK-4 oil showed similar or slightly better lubricity compared to the CJ-4 oil while the candidate FA-4 oil decisively increased the piston skirt wear. Although both coatings prevented scuffing failure observed for the uncoated steel skirt in a base oil without an additive package, they surprisingly caused a higher piston wear rate when tested in any of the fully formulated engine oil. The detrimental impact was attributed to the Mn-P film, either as a standalone coating, or a coating interlayer. The porous and brittle Mn-P film was broken during the wear test and the released hard Mn-P grains are suspected to cause third-body abrasion to accelerate the wear process. This work also evaluated the feasibility of developing an improved high temperature, low mass, cost-neutral turbocharger compressor wheel for heavy-duty engine applications from TiAl using additive manufacturing, utilizing its unique ability to fabricate high strength, low weight structures. This work has shown that the phase transforming nature of the TiAl alloys enable obtaining equiaxed microstructures in the as-built state without the need for tedious beam parameter manipulations. The HIPed structures have good RT tensile properties that will enable them to be surface machined to the required tolerance that can 2 then be heat treated to obtain the desired microstructures. Additionally, the negligible residual stresses stemming from the high build chamber temperatures ensure the parts are formed without cracks (one of the major issues in traditional manufacturing of these intermetallics).

33 ADVANCED PROPULSION SYSTEMS↗

IACMI Project 4.2: Thermoplastic Composite Development for Wind Turbine Blades

(Section 5.1) Composites made from Arkema’s Elium® thermoplastic resin and Johns Manville fiberglass were researched during this project for applications in wind blade manufacturing. A techno-economic model was developed to model this wind blade manufacturing process using these materials in place of traditional composites made with thermoset resin. This model was based on manufacturing a 61.5-meter wind blade, which showed a 4.7% reduction in wind blade cost as compared traditional thermoset materials. These cost savings were not from the thermoplastic material costing less than traditional thermoset materials, but rather from decreased capital costs, faster cycle times and reduced energy requirements and labor costs. (Section 5.2) An infusion and curing model was developed for thermoplastic composite wind blades using PAM-RTM. The primary goal was to demonstrate the infusion simulation for the Elium® resin system on a 13-meter wind blade. Additionally, the exotherm temperature was predicted and compared to measurements, which showed model results within 10% of actual measurements. (Section 5.3) Composite laminate panels and composite sandwich panels with a balsa core were produced; specimens were cut and characterized. Similar composite specimens were made with Elium® thermoplastic resin and Hexion thermoset epoxy (RIMR135/RIMH1366) to enable comparisons between these resin systems. The static test methods included: tensile, compression, in-plane shear, interlaminar shear, flexural, sandwich core shear flexure, and single cantilever beam tests for sandwich beams. Fatigue testing at room temperature was completed to composite laminate panels at a stress ratio of R=0.1 and R=10. In addition, fatigue testing to laminate panels was completed at -30°C, and at room temperature after conditioning specimens at 70°C and 90% relative humidity. Overall, mechanical test results from Elium® composites are similar to epoxy composites. (Section 5.4) Elium composite panels were produced with intentional defects such as voids and nonwetting of fibers to begin to understand performance sensitivity to defects. A thermal digital image correlation (TDIC) method provides high spatial resolution strain field at elevated temperatures and can be used to identify defective regions within composite panels. Flexural modulus differences of 21% were seen between defect and non-defect panels. Other Elium® composite panels were forced to be defective by boiling the resin after infusion, which created voids throughout the composite laminate. X-ray computed tomography scanning was used to view the internal structure of the defect panels. Defect panels had a significant reduction in fatigue life as compared to baseline panels produced without intentional defects. (Section 5.5) Lap shear specimens were fabricated to compare the lap shear strength of an off-the-shelf adhesive (Plexus MA590) and two new adhesives developed by Arkema (Bostik SAF30 90 and Bostik SAF30 120). ISO standard 4587:2003 was used to standardize the testing method and sample fabrication. Lap shear specimens were made at 1mm, 3mm, and 10mm thicknesses. The Bostik adhesive lap shear test results were similar to Plexus for all thicknesses. (Section 5.6) Fiber-reinforced polymer (FRP) composites are typically used in high-performance applications (e.g., aerospace), and their expansion into high-volume industries (e.g. consumer automotive and wind turbine blade manufacturer or similar) is hindered by their cost and a lack of efficient manufacturing techniques. Monitoring the curing process of these composites during manufacturing can improve the efficiency of the process, and therefore reduce the manufacturing cost. Cure monitoring techniques were developed that use probabilistic estimation methods and surface temperature measurements made using infrared cameras. These techniques enable real-time monitoring of the infusion process to locate manufacturing flaws, and they can, potentially, estimate residual stresses in the part. Their commercialization will help facilitate expansion of FRP composites in high-volume industries. (Section 5.7) A 13-meter composite wind blade was produced with Elium® resin and Johns Manville fiberglass; this blade was made with VARTM processing similar to how megawatt-scale wind blades are currently manufactured, but no post-mold heating was used for this thermoplastic composite blade. The wind blade underwent full-scale validation for static loading (4-different load orientations) and flapwise fatigue loading to simulate 20-years of operational loads. The thermoplastic composite wind blade withstood the loading without any noted issues and performed similar to results from a previous full-scale validation to an equivalent epoxy composite wind blade produced with the same blade molds. (Section 5.8) A study was conducted to determine the feasibility of recycling composite wind turbine blade components fabricated with glass fiber reinforced Elium® thermoplastic resin. Dissolution, which is a process unique to thermoplastic matrices, allows recovery of both the polymer matrix and full-length glass fibers, while maintaining their stiffness and strength throughout the recovery process. The economics of recycling is favorable if 50% of the glass fiber is recovered and resold for a process of $\$$ 0.28/kg, and 90% of the resin is recovered and resold at a price of $\$$ 2.50/kg.(Section 10) Recommendations are outlined for commercializing thermoplastic resin for composite wind blade production, in addition to recommended areas for future research.

17 WIND ENERGY↗

Update on Investigations of Viability of Cold Spray and FSW as a Spent Nuclear Fuel Dry Storage Canister Mitigation Tool

The purpose of this work is to investigate the use of cold spray and friction stir welding or processing (FSW/P) for repair and mitigation of chloride-induced stress corrosion cracking (CISCC) in dry cask storage system (DCSS) canisters to ensure integrity far beyond their original license period. This report provides a viability analysis of cold spray and friction stir welding for repair and fabrication of DCSS canisters. This report presents experimental work and a research strategy to optimize and evaluate cold spray and FSW/P for CISCC resistance. The literature reports that the following three conditions must exist for CISCC to occur: tensile stress, corrosive environment, and susceptible material. These conditions must be understood and accounted for while evaluating CISCC susceptibility. Furthermore, non-obvious factors, such as surface conditions and geometric confinement, can dramatically increase the intensity of one or more of the three listed conditions for CISCC. Arc welding should be considered for either temporary or permanent repair when combined with a mitigation technology. It is known that alloys used in the existing inventory of spent nuclear fuel storage canisters become sensitized in areas around fusion welds. Technologies, such as cold spray or FSW, can mitigate the sensitization caused by fusion welds. FSW/P and cold spray, potential alternatives for fabrication and repair, are solid-phase processes. No melting occurs and the energy input can be controlled such that no harm is done to the base metal during these processes. FSW/P should be considered for use in new fabrication of canisters and repair of existing canisters. Low heat input and grain refinement result in material with improved mechanical properties and comparable generalized corrosion performance relative to base metal. FSW/P offers the potential of through-thickness CISCC resistance. Cold spray should be considered for production, mitigation, and repair of canisters. Cold spray has demonstrated the ability to deposit stainless steel, Inconel alloys, and other alloys on stainless steel 304L such that galvanic potential is matched and resistance to pitting is improved. The technical basis for cold spray mitigation and repair within the overpack using remote robotic equipment is established. A non-obvious application to the research community is the sealing of crevices. All reported instances of CISCC in the fielded nuclear applications were associated with crevice corrosion. This can be avoided by cold spraying to seal crevices. The bulk of the work planned for FY 2020 will be generating coupons for CISCC testing by collaborative projects at Pacific Northwest National Laboratory and Sandia National Laboratories. First an exploratory study will be executed that will include screening studies and process optimization. This task will identify the effect of process parameters on microstructure and CISCC resistance. Optimized parameters will be used to produce a smaller number of coupons for full testing and evaluation. Test methods for evaluating CISCC resistance must meet the following criteria: (1) normalized surface geometry and exposed process microstructure, (2) account for residual stresses, (3) be in a controlled and appropriate test environment, and (4) be numerically quantifiable and repeatable. Failure to meet these criteria could lead to results that cannot be used for comparative analysis of processes and materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Silicon Oxide‐Rich Diamond‐Like Carbon: A Conformal, Ultrasmooth Thin Film Material with High Thermo‐Oxidative Stability

Abstract Silicon oxide‐containing diamond‐like carbon (a‐C:H:Si:O) films are a promising class of protective coatings for environmentally‐demanding applications owing to their lower residual stresses and superior thermal stability and oxidation resistance relative to undoped diamond‐like carbon. However, existing versions of a‐C:H:Si:O deposited by traditional methods such as plasma‐enhanced chemical vapor deposition (PECVD) undergo substantial degradation and oxidation at temperatures above 250 °C. This, together with the difficulty of PECVD in depositing conformal coatings on complex geometries such as high‐aspect‐ratio features, has limited the applicability of a‐C:H:Si:O. Here, the unique capabilities of plasma immersion ion implantation and deposition (PIIID) to grow silicon oxide‐rich diamond‐like carbon materials that are ultrasmooth, continuous, and conformal on high‐aspect‐ratio topographies are explored. The high concentration of silicon and oxygen in PIIID‐grown films (23 ± 5 at.% and 11 ± 4 at.%, respectively) is unrivalled for this class of materials, and drastically increases the resistance to oxidation at high temperatures, compared with PECVD‐grown films. The results open the path for using a‐C:H:Si:O in applications involving exposure of materials to extreme environments.

Mangolini, Filippo↗

Parameter estimation in a thermoelastic composite problem via adjoint formulation and model reduction

Advances in nondestructive material characterization are providing a wealth of information that could be exploited to gain insight into general aspects of material performance and, in particular, discover relationships between microstructure and thermo-mechanical properties in polycrystalline and other complex composite materials. Here, in order to facilitate the integration of such measurements into existing models, as well as inform new physics-based predictions, we developed a C++/MPI computational framework for sensitivity analysis and parameter estimation. The framework utilizes a micro-mechanical modeling based on fast Fourier transforms, direct and adjoint formulations, and Markov chain Monte Carlo sampling techniques. We illustrate the characteristics of this framework and demonstrate its utility by computing the residual stresses arising from thermal expansion of an elastic composite and using data from simulated experiments. Lastly, we show that the availability of nondestructive 3-D measurements is crucial to reduce the uncertainty in predictions, emphasizing the importance of an integrated experimental/modeling/data analysis approach for improved material characterization and design.

36 MATERIALS SCIENCE↗

Investigating Chain Dynamics in Highly Crosslinked Polymers using Solid–State 1 H NMR Spectroscopy

Solid state 1 H NMR line–shape analysis and (double quantum) DQ 1 H NMR experiments have been used to investigate the segmental and polymer chain dynamics as a function of temperature for a series of thermosetting epoxy resins produced using different diamine curing agents. In these thermosets, chemical crosslinks introduce topological constraints leading to residual stresses during curing. Materials containing a unique ferrocene–based diamine (FcDA) curing agent were evaluated to address the role of the ferrocene fluxional process on the atomic–level polymer dynamics. Here, at temperatures above the glass transition temperature ( T g), the DQ 1 H NMR experiments provided a measure of the relative effective crosslink and entanglement densities for these materials and revealed significant polymer chain dynamic heterogeneity in the FcDA–cured thermosets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermal Performance of Perovskite-Based Photovoltaics for Operation in Low Earth Orbit

Perovskite-based photovoltaics are attractive for applications in space. The space environment is harsh with ionizing radiation, atomic oxygen, UV radiation, extreme temperatures, and thermal cycling. Herein, the thermal performance of perovskite active layer and perovskite photovoltaic devices in low earth orbit is analyzed. A 1 μm silicon oxide layer coupled with 500 nm zirconia thin film aid in cell thermal management is determined. The residual stresses between various layers in a device are modeled and it is proved that thermally induced mechanical failure of the perovskite (time > 460 years) is unlikely during operating lifetime of any mission. In conclusion, target power conversion efficiencies are also shared to manage maximum operating temperature of a perovskite-based device.

14 SOLAR ENERGY↗