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At least 127 records · Page 7

In situ measurement of phase transformations and residual stress evolution during welding using spatially distributed fiber-optic strain sensors

Welding of high-strength steels can result in large tensile strains as the base metal and filler material cool from their molten state. To combat these large tensile strains, low-transformation-temperature (LTT) metal fillers have been proposed. These fillers undergo a martensitic phase transformation at a lower temperature which can ultimately reduce the tensile strain or can even introduce compressive strain adjacent to the weld metal. However, the process for optimizing the composition of the LTT material, as well as various weld parameters for each unique weld geometry, can be quite expensive, especially if the acceptance criterion requires using neutrons, x-ray beams, or destructive techniques to characterize residual stresses. This work describes a simple, low-cost method for quantifying residual stresses and phase transformations in situ during welding. Spatially distributed fiber-optic sensors were bonded to a cast iron plate, along with tack-welded thermocouples, to measure temperature and strain during multiple passes with LTT filler metals. Results show that the fiber-optic sensors can successfully resolve compressive strain adjacent to the weld region caused by the martensitic phase transformations in the LTT filler material.

47 OTHER INSTRUMENTATION↗

Optimizing Piezoelectric Nanocomposites by High‐Throughput Phase‐Field Simulation and Machine Learning

Abstract Piezoelectric nanocomposites with oxide fillers in a polymer matrix combine the merit of high piezoelectric response of the oxides and flexibility as well as biocompatibility of the polymers. Understanding the role of the choice of materials and the filler‐matrix architecture is critical to achieving desired functionality of a composite towards applications in flexible electronics and energy harvest devices. Herein, a high‐throughput phase‐field simulation is conducted to systematically reveal the influence of morphology and spatial orientation of an oxide filler on the piezoelectric, mechanical, and dielectric properties of the piezoelectric nanocomposites. It is discovered that with a constant filler volume fraction, a composite composed of vertical pillars exhibits superior piezoelectric response and electromechanical coupling coefficient as compared to the other geometric configurations. An analytical regression is established from a linear regression‐based machine learning model, which can be employed to predict the performance of nanocomposites filled with oxides with a given set of piezoelectric coefficient, dielectric permittivity, and stiffness. This work not only sheds light on the fundamental mechanism of piezoelectric nanocomposites, but also offers a promising material design strategy for developing high‐performance polymer/inorganic oxide composite‐based wearable electronics.

42 ENGINEERING↗

Bio‐Based Piezo‐ and Thermoresistive Photocurable Sensing Materials from Acrylated Epoxidized Soybean Oil

Abstract Bio‐based photocurable polymers are increasingly in demand as environmentally friendly materials for advanced applications. Together with functional fillers, these represent a next step for the generation of functional and active smart materials, compatible with additive manufacturing technologies. Herein, acrylated epoxidized soybean oil (AESO) mixed with different amounts of reduced graphene oxide (rGO) up to 6 wt% in order to obtain UV‐curable piezoresistive and thermoresistive materials, is reported. It is shown that the addition of rGO to AESO hinders the curing process, but always maintains double bond conversions higher than 50%. Composites are characterized by a good dispersion of micrometric filler clusters. Further, the thermal stabilities are close to 300 °C and crosslinking degrees are above 1.75 mmol cm –3 . The Young modulus of the composites decreases with the addition of the rGO fillers, in particular for the higher filler contents, and electrical conductivities up to 0.13 S m –1 are obtained for the composites with the highest rGO content. UV‐curable composites with piezoresistive and thermoresistive responses suitable for applications are thus obtained, characterized by gauge factors around 26 for deformations up to 2% and maximum thermoresistive sensitivity of S = 0.43, values similar to the values obtained for petroleum‐based materials.

Mendes‐Felipe, Cristian↗

Multiscale characterization and comparison of historical and modern nuclear graphite grades

Beginning with Chicago Pile I, graphite has been used as a moderator material in nuclear power stations and is considered a potential material for use in future Generation IV advanced reactors. The microstructure of graphite is responsible for much of its mechanical and thermo-physical properties, and how it responds to irradiation. To understand graphite microstructure, it is necessary to understand its porosity at the macro- and micro-scales; and to understand its porosity, it is necessary to characterize the morphological connectivity of the void content and the two main phases of graphite: filler and binder. Here, using several microscopy and analytical techniques, a detailed examination of the heterogeneity, microstructure and pore structure of different graphite grades and their binder and filler phases is presented. Significant differences were found between coarser and finer nuclear grades. Coarse grades have a more diverse range of filler particles, pores and thermal cracks. Finer grades have a more well-defined pore size distribution, fewer variations of filler particles sizes and do not contain as many large thermal cracks. Fine grades tend to have a well-connected network of pores whereas coarser grades contain a larger content of closed porosity. The framework developed within this work can be applied and used to assess the various graphite grades that would down-select materials for specific use in graphite moderated reactor designs.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Pore-Confined Polymers Enhance the Thermal Conductivity of Polymer Nanocomposites

In this work, molecularly confined polymer fillers in nanopores were found to give superior mechanical properties of polymer nanocomposites. In this work, we study the thermal conductivity of such nanocomposites and unveil the effect of polymer confinement on thermal conductivity. Using the time-domain thermoreflectance method, we measure the cross-plane thermal conductivity of polymer nanocomposites that consist of polystyrene fillers confined within a nanoporous organosilicate matrix. Compared to unconfined bulk polystyrene fillers, we find that pore-confined polystyrene fillers enhance the thermal conductivity of the polymer nanocomposites. This enhancement is attributed to the better aligned and less entangled chains in the confined phase, where chain–chain phonon scatterings are reduced. Our work provides essential insights into the thermal conductivity of polymer nanocomposites for multifunctional thermal and mechanical applications.

36 MATERIALS SCIENCE↗

Charge-Density-Wave Thin-Film Devices Printed with Chemically Exfoliated 1T-TaS 2 Ink

In this work, we report on the preparation of inks containing fillers derived from quasi-two-dimensional charge-density-wave materials, their application for inkjet printing, and the evaluation of their electronic properties in printed thin-film form. The inks were prepared by liquid-phase exfoliation of CVT-grown 1T-TaS 2 crystals to produce fillers with nm-scale thickness and μm-scale lateral dimensions. Exfoliated 1T-TaS 2 was dispersed in a mixture of isopropyl alcohol and ethylene glycol to allow fine-tuning of filler particles thermophysical properties for inkjet printing. The temperature-dependent electrical and current fluctuation measurements of printed thin films demonstrated that the charge-density-wave properties of 1T-TaS 2 are preserved after processing. The functionality of the printed thin-film devices can be defined by the nearly commensurate to the commensurate charge-density-wave phase transition of individual exfoliated 1T-TaS 2 filler particles rather than by electron-hopping transport between them. The obtained results are important for the development of printed electronics with diverse functionality achieved by the incorporation of quasi-two-dimensional van der Waals quantum materials.

1T-TaS2↗

Anharmonicity in partially filled skutterudites Yb x Co 4 Sb 12

Here, we report an experimental investigation of Yb filler ion dynamics in partially filled skutterudite samples Yb x Co 4 Sb 12 ( x = 0.26 and x = 0.4). From extended x-ray absorption fine structure (EXAFS) measurements at the Yb L 2 -edge, the mean-square displacements of the Yb fillers were extracted over a wide temperature range from 10 to 500 K. We found that the low-temperature dynamics of Yb fillers are described well using a harmonic oscillator approximation with Einstein temperatures of 70 ± 5 K for both samples. This finding is consistent with the observed low-energy phonon mode at 5.3(5) meV in the inelastic x-ray scattering (IXS) data. However, the temperature dependence deviates from the harmonic approximation at high temperatures due to significant cubic anharmonicity, which was revealed in the EXAFS cumulant analysis. Our study also demonstrates that complementary information on filler dynamics in skutterudites can be acquired using EXAFS and IXS.

36 MATERIALS SCIENCE↗

Advanced Non-Tread Materials for Fuel-Efficient Tires

PPG Industries, Inc. proposes to develop a new silica filler that can increase fuel efficiency by 2% while maximizing key performance properties in non-tread tire components compared to current carbon black/silica filler blends. In this project PPG focused on a sidewall compound. The developed compounds/components will reduce energy losses by approximately 25%, with no more than a 5% loss of resistance to degradative forces (targeting better performance). PPG plans to achieve this goal by characterizing the impact the silica filler can have on rubber properties and then tuning the silica morphology and surface chemistry for this end use. PPG will also provide guidance in optimizing the compound formulation to make the best use of this new filler. A key aspect is to understand and maintain, if not improve, the aging performance as evaluated by crack growth resistance under ozone environment. Two key strategies were used to meet the rolling resistance goal while maintaining other performance properties. The first factor was understanding the surface treatments and chemical makeup of the silica and its effects on compound performance. The second factor was using the best performing silicas and determining the optimum compound modifications to achieve the final sidewall compound performance. Using statistical analysis throughout the optimization process, it was determined that changing the silica morphology played a role in improving the reduction of tear strength while reducing rolling resistance and the improvements observed varied depending on the CB type.

36 MATERIALS SCIENCE↗

Experimental and Computational Studies of Stress Corrosion Cracking of Alloys 308/309 and 82/182 Weldments in Corrosive and Radiation Environment

The goal of the project was to determine factors that influence SCC and IASCC in weldments found in LWR nuclear power plants. We focused on a SA508-304L SS weldment fabricated by EPRI using gas tungsten arc welding and used an aggressive BWR normal water chemistry (NWC) immersion environment. This weldment used 309L butter and 308L groove filler material. The microstructure of the 309L butter was non-uniform, exhibiting a 20–30μm thick martensitic layer closest to the SA508 interface, a 1–4 mm thick single γ austenite phase dilution zone, and a γ–δ duplex region extending to the 308L groove filler. The 308L groove filler had an entirely γ–δ duplex microstructure. Two approximately 1-inch thick 304L and SA508 plates approximately 12 by 6 square inches were joined using standard nuclear grade welding techniques. This included a post weld heat treatment of the 309L butter after application, a 0.32 cm fit-up root opening, and 57 bead lines of 308L groove filler applied in 18 layers. A 60 degree weld bevel angle was used and the 309L butter was 1.5 cm thick. Displacement cascade damage was induced using proton irradiation at the Michigan Ion Beam Laboratory. The incident proton energy was 2 MeV, the sample temperature was 360 ºC, and the calculated dpa value at 10 μm (60% of the Bragg peak depth of ~18 μm) was 5 dpa using the quick Kinchin-Pease model. Proton irradiation to this damage level required approximately 125 hours of beam time. Two types of samples were irradiated, tensile specimens and TEM bars. Samples were selected from all regions of the weldment, including the SA508-309L butter interface, the 309L-308L interface, and 308L-304L interface. The stainless steel alloys (304L, 308L, and 309L) within the heat affected zone are characterized by a duplex skeletal morphology of δ-ferrite and γ-austenite resulting from the recrystallization associated with weld fabrication. Approximately 7 to 8 mm of length along the specimen was irradiated. The gauge volume surfaces were mechanically polished and then electro-polished to remove mechanical damage from the mechanical polishing step prior to irradiation. Immersion tests were performed in a recirculating autoclave under BWR NWC conditions (2000 ppb wt. dissolved oxygen, neutral pH, 288 ºC, 10 MPa, and inlet water conductivity <100 nS/cm) to accelerate corrosion. Constant strain rate tests were performed either to failure or to approximately 5% strain. Strain rates of 10 -7 to 10 -6 mm/mm/s were used and typical immersion testing required four to six weeks to achieve failure or strains near 5%. Analysis primarily used advanced electron microscopy techniques of FIB lift out specimens.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Stress Relaxation Cracking of Alloys at Temperatures Higher Than 540°C

Type 347H stainless steel (347H SS), used in commercial concentrating solar power (CSP) thermal energy storage to store solar-salt at a temperature of 565°C, has been reported in the literature to be susceptible to stress-relaxation cracking (SRC). The welded heat-affected zone (HAZ) and fusion zone (FZ) of 347H SS, particularly in thick sections, are known to be susceptible to failure during post-weld heat treatment (reheat cracking). SRC could also occur after months or years under an elevated-temperature service environment. Two conditions must be present for failure to occur in the HAZ and/or FZ: 1) a modified or sensitized microstructure and 2) sufficiently high tensile residual stresses present at the elevated service temperature. The overarching goal of this project is to recommend SRC mitigation protocols to avoid susceptibility to fail through SRC at temperatures relevant for CSP. Post weld heat treatment conditions and alternative alloys are investigated as potential mitigation solutions to SRC. We used Gleeble thermomechanical simulation tests and finite element (FE) models to understand the susceptibility of 347H SS to SRC as a function of temperature, stress, and microstructure. We started with a literature review of weldability issues with 347H SS and techniques to mitigate SRC in 347H SS weldments. Next, we used Gleeble experiments to determine reheat cracking susceptibility in the simulated HAZ of 347SS weldments and an alternative alloy, 316L SS (NUCL 167 SPH) with boron added. We also performed Gleeble experiments to compare the reheat cracking susceptibility of 347H cross welded with two different fillers: E347, which is used in some commercial CSP TES tanks, and E16.8.2. We validated the experimental results with FE models of the residual stresses. We found that although the 316L (NUCL 167 SPH) is less susceptible to reheat cracking, it is slightly weaker than 347H and ASME BP&V codes limit its use to a service condition of 565°C. We also found that welds using E16.8.2 as the weld filler are less susceptible to failure than those using E347, likely due to the higher creep ductility of E16.8.2, and that it may be used as an alternative filler for repair welding of 347H welds or as the primary choice of filler for newly developed weld joints. We also found that post weld heat treatment could be a viable solution for mitigating stress in E347-347H SS thick, constrained welds, like those found in CSP tanks, and propose several options for mitigating SRC in existing and future TES tanks.

14 SOLAR ENERGY↗

Dual-Purpose Canister Filling Demonstration Project Progress Report at ORNL, 2023

The US DOE Office of Nuclear Energy is investigating the feasibility of direct disposal of dual-purpose canisters (DPCs) in a hypothetical geological repository to offset the potential requirement to repackage spent nuclear fuel (SNF) from existing DPCs into smaller, disposal-ready canisters. Oak Ridge National Laboratory (ORNL) is currently evaluating the feasibility of filling void space in loaded DPCs with an engineered material to prevent a criticality event caused by groundwater/moderator intrusion. Metal alloys are being investigated as a filler material because of their relatively low viscosities when molten, which may facilitate their injection via an existing drainpipe that runs almost the full length of the DPC. ORNL’s strategy for evaluating filler viability includes simulations and physical demonstrations of filling and casting behavior, as well as evaluations of materials for compatibility in the repository environment. Filling of DPCs in this manner is expected to mitigate the risk associated with a post-closure criticality event during the repository performance assessment time frame (10,000 years or greater). Efforts in this fiscal year focused on (1) destructive analysis of experimental filler castings made in FY 2022, (2) a report outlining a conceptual design of a DPC filling facility (Fortner et al., 2023, M3SF 23OR010305044/ ORNL/SPR-2023/2921, May 31, 2023), (3) a report on affected features, events, and processes (FEPs) due to DPC filling (Price et al., 2023, M3SF-23SN010305093, issuance pending), (4) developing and testing a more practical alloy filler based upon a Sn-Al eutectic, and (5) modeling the heating and cooling dynamics of a DPC subjected to molten metal filling. The preliminary results from each of these tasks support the feasibility of filling DPCs with metal as a strategy against the possibility of criticality in the repository. The FY 2022 casting was found to penetrate even very small orifices in the mold and internal structures. Preliminary testing of the Sn-Al eutectic indicate little interaction of the melt with Zircaloy cladding. Thermal modelling shows that a filled DPC will cool to manageable temperatures within 2-3 days, which is likely manageable in a facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of in-situ polymerized intrinsically conductive resin and low-cost carbon pigments offering high conductivity for sensing, EMI shielding and lighting protection

Electrically conductive composites are emerging across diverse industries such as electronic, automotive, aerospace, advanced air mobility, biomedical, infrastructure, defense and security offering static charge dissipation, electromagnetic interference shielding, lighting protection, sensing, dicing, corrosion monitoring, etc. Conductivity enhanced composites provide several advantages compared to conventional metals including weight reduction, corrosion resistance, energy efficient processability, tunable properties and multifunctionality. Polymers are typically insulating in nature and require conducting filler for electron transport. However, dispersion and polymer-filler interphases are critical and often disrupt conducting pathways. Besides, conductive fillers such as graphene, carbon nanotube, MXene, silver nanowire, etc. are expensive, limiting their wide adoption in composite industry. On the other hand, a limited number of intrinsically conductive polymers are available among which polyaniline (PANI) has been widely studied due to its high conductivity, thermal and chemical stability. However, PANI is difficult to process and exhibits weak mechanical properties. In brief, there is a significant demand for electrically conductive polymer formulation with cost-effective conducting fillers that offer processability in scale to expand the market of conductivity enhanced materials.

Kumar, Vipin [Oak Ridge National Laboratory (ORNL)↗

Radial particle-based terrestrial thermocline for high temperature thermal storage

A system or method for thermal storage includes a recess or containment unit having a first storage layer and a second storage layer comprising a permeable filler material. An intermediate layer is disposed between the storage layers. A primary well traverses the layer in the recess. The primary well is in thermal communication with the first permeable filler material and the second permeable filler material. A heat source is provided for heating an inlet fluid. An input pump is in fluid communication with the primary well and the heat source. The primary well receives heated inlet fluid from the inlet pump and injects the fluid into the second layers. The heated inlet fluid transfers heat to the respective permeable filler material radially from the primary well toward an outer periphery of the thermocline recess.

Ho, Clifford K.↗

Identifying Bounds of Inorganic Content in Solventless Processing of Hybrid Solid Electrolytes

Solid-state lithium batteries require safe, robust electrolytes to enable higher energy densities and improved safety over conventional cells. Hybrid polymer–ceramic electrolytes are a promising solution, combining the processability of polymers with the high ionic conductivity and mechanical strength of inorganic fillers. In this work, we demonstrate a solventless, UV-curing method to produce hybrid solid electrolytes using a poly(ethylene glycol) dimethyl ether (PEGDME)-based photocurable matrix incorporating Li 1.5 Al 0.5 Ge 1.5 (PO 4 ) 3 (LAGP) or Li 7 La 3 Zr 2 O 12 (LLZO) ceramic electrolyte. Inorganic filler loadings up to ∼55 wt.% could be successfully incorporated via this process which was the highest inorganic content at which the slurry remains processable and cured into a uniform film. The resulting UV-cured composite electrolytes remain flexible and exhibit room-temperature ionic conductivities on the order of 10 −4 S·cm −1 , along with notably improved lithium-ion transference numbers compared to conventional polymer electrolytes. Similar performance and processing limits were observed for both LAGP and LLZO, indicating that ceramic filler chemistry does not significantly affect the UV-curing process or the electrolyte's ion transport properties in this regime. Eliminating solvents from fabrication not only simplifies processing and mitigates environmental concerns but also enables higher solid contents that enhance mechanical strength and help suppress lithium dendrite formation. In conclusion, this scalable approach thus paves the way for manufacturing robust composite solid electrolytes for next-generation solid-state batteries (SSBs).

Batteries↗

Balancing Functionality and Printability: High-Loading Polymer Resins for Direct Ink Writing

Although direct ink writing (DIW) allows the rapid fabrication of unique 3D printed objects, the resins—or “inks”—available for this technique are in short supply and often offer little functionality, leading to the development of new, custom inks. However, when creating new inks, the ability of the ink to lead to a successful print, or the “printability,” must be considered. Thus, this work examined the effect of filler composition/concentration, printing parameters, and lattice structure on the printability of new polysiloxane inks incorporating high concentrations (50–70 wt%) of metallic and ceramic fillers as well as emulsions. Results suggest that strut diameter and spacing ratio have the most influence on the printability of DIW materials and that the printability of silica- and metal-filled inks is more predictable than ceramic-filled inks. Additionally, higher filler loadings and SC geometries led to stiffer printed parts than lower loadings and FCT geometries, and metal-filled inks were more thermally stable than ceramic-filled inks. The findings in this work provide important insights into the tradeoffs associated with the development of unique and/or multifunctional DIW inks, printability, and the final material’s performance.

36 MATERIALS SCIENCE↗

Polypropylene Composites Reinforced With Recycled Waste Cellulosic Fiber/Fine Mixture: The Impact of Cellulose Sieving on Performance

This study explores how a sieving step of waste cellulosic fiber and fine (WCFF) mixture affects the performance of WCFF‐loaded polypropylene (PP) composites and whether the separation of fines from fibers offers an added benefit. The WCFF samples were downsized, and four different filler size ranges were sieved using a series of mesh sizes from 4 to 0.85 mm. The WCFF/PP composites were then compounded at 20 wt.% loading of WCFF using a twin‐screw extruder. Incorporating WCFF increased the tensile strength to 41.28 MPa and the modulus to 3207 MPa, accounting for 28% and 38% enhancements, respectively. Interestingly, the greatest improvements were associated with the nonsieved WCFF case, and the sieved WCFF fibers provided only marginal enhancements over virgin PP. The outperformance of nonsieved WCFF was attributed to the synergistic reinforcement of hybrid fibers and fines as well as the maintenance of longer fibers in the system. However, the strain at break and impact strength of PP decreased after introducing WCFF. Moreover, the complex viscosity and storage modulus increased with an increase in the filler size, due to the formation of a more effective percolative network. The PP's crystallinity exhibited a relatively strong dependency on the sieving, where WCFF samples with short‐aspect‐ratio fillers promoted the crystallinity significantly. It was also found that the WCFF degradation onset temperature increased once it was incorporated into PP. This study suggests that waste cellulosic feedstocks can be utilized as a reinforcement without additional sieving to manufacture high‐performance and cost‐effective composites.

36 MATERIALS SCIENCE↗

Surface modification of ZIF ‐90 with triptycene for enhanced interfacial interaction in mixed‐matrix membranes for gas separation

Abstract Zeolite imidazole framework (ZIF‐90) nanoparticles were chemically modified by grafting triptycene moieties. The modified nanoparticles were introduced into a triptycene‐based polyimide as fillers to generate mixed matrix membranes (MMMs) for gas separation. The incorporation of “hook‐like” triptycene moieties in both dispersed and continuous phases led to intimate contact between the two phases and thus defect‐free interfacial morphology, due to the supramolecular interlocking and π–π stacking interaction between triptycene units presented in both phases. The filler/polymer solution showed shear thickening behavior due to such strong interfacial interaction. The separation performance of the prepared composite membranes was investigated as a function of filler loading and particle surface grafting density. Pure‐gas permeation results showed that the gas permeabilities increased expectedly as the filler loading increased, with stable or improved selectivities. The reduced permeability relative to pristine polyimide film is likely due to the pore blockage of ZIF‐90 upon grafting triptycene moieties on the particle surface. Reducing the grafting density of triptycene moieties led to improved permeability and selectivity suggesting good tunability of this series of new composite membranes. Overall, modification of nanofiller with hierarchical triptycene moieties offers a fundamentally new avenue for creation of composite membranes with unique properties in gas separations.

Zhang, Qinnan↗

Multiscale porosity characterization in additively manufactured polymer nanocomposites using micro-computed tomography

Extrusion-based additive manufacturing (AM) of polymer composites exhibits complex thermally driven phenomena that introduce severe discontinuities in the internal structure across length scales, especially voids or porosity. This study utilizes a high-throughput porosity characterization technique to analyze large datasets from numerous micro-computed tomography (mu CT) scans to capture the influence of AM print parameters on the size, shape, and location of porosity across multiple print layers (up to a few cm) on fused granular fabrication (FGF) printers. The materials investigated include nanocomposite formulations based on commercially relevant nylon-12 and polyether ketone ketone (PEKK) materials comprising nano- or micro- sized fillers. The estimated global porosity follows an inverse linear correlation against the bulk density of the printed samples. Increasing the extrusion multiplier (EM) and the nozzle temperature while decreasing the print speeds reduces the global porosity. Outlier analyses (local porosity morphology) show that faster print speeds and higher extrusion rates result in long, slender inter-layer voids, while lower nozzle temperatures lead to large, symmetrical, inter-bead voids (at the bead junction). Lack of active chamber temperature increases inter-layer and intra-bead voids with a two-fold increase in global porosity. Overall, the micro filler-reinforced composites exhibit higher global porosity than nanofiller-reinforced composites, which is attributed to the increased mismatch in the thermal expansion coefficient between the filler and the polymers used in the study.

36 MATERIALS SCIENCE↗