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33 records · Page 2

Ultrahigh pressure compaction-resistant thin film crosslinked composite reverse osmosis membranes

In this study, we present a class of thin-film crosslinked (TFX) composite reverse osmosis (RO) membranes that resist physical compaction at ultrahigh pressures (up to 200 bar). Since RO membranes experience compaction at virtually all pressure ranges, the ability to resist compaction has widespread implications for RO membrane technology. The process described herein involves crosslinking a phase inverted porous polyimide (PI) support membrane followed by interfacial polymerization of a polyamide layer, thereby forming a fully thermoset composite membrane structure. We explore a range of phase inversion membrane formation parameters such as PI concentration, solvent-cosolvent ratios, coagulation bath composition, and crosslinking methods in addition to interfacial polymerization reaction chemistry and conditions. Overall, TFX membranes exhibit significantly less compaction compared to hand-cast and commercial high-pressure RO membranes, experiencing less than 10% decline in water permeance and maintaining salt rejection over 99% for NaCl solutions up to 180,000 mg/L with 200 bar applied pressure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Compact in situ probe for magnetotransport measurements of 2D materials under variable tensile strain

The recent development of freestanding oxide membranes has opened new opportunities for strain engineering of transition metal oxides beyond values accessible in bulk samples. While a number of studies have been performed with fixed strain, the ability to dynamically control the strain state during measurement would be greatly enabling. To this end, we present an in situ uniaxial strain probe optimized for transport measurements of tensile-strained 2D or quasi-2D materials down to 2 K. Utilizing a flexible polyimide substrate as the stress transfer medium, our platform simplifies the sample preparation process and allows precise alignment of strain fields relative to the crystalline axes. An in situ optical microscope monitors the macroscopic strain state operando and makes it possible to complete an entire magnetotransport study at cryogenic temperatures under continuous strain variations. We demonstrate the capabilities of the probe on a freestanding LaNiO 3 membrane, where we induce tensile strain up to 8% and observe a corresponding strong transport anisotropy. In view of the rapid developments in low-dimensional materials synthesis and the plethora of novel quantum phenomena they exhibit, this strain probe provides general instrumentation for examining and controlling these properties via strain.

2D materials

Calibration and characterization of the line-VISAR diagnostic at the HED-HIBEF instrument at the European XFEL

In dynamic-compression experiments, the line-imaging Velocity Interferometer System for Any Reflector (VISAR) is a well-established diagnostic used to probe the velocity history, including wave profiles derived from dynamically compressed interfaces and wavefronts, depending on material optical properties. Knowledge of the velocity history allows for the determination of the pressure achieved during compression. Such a VISAR analysis is often based on Fourier transform techniques and assumes that the recorded interferograms are free from image distortions. In this paper, we describe the VISAR diagnostic installed at the HED-HIBEF instrument located at the European XFEL along with its calibration and characterization. It comprises a two-color (532, 1064 nm), three-arm (with three velocity sensitivities) line imaging system. We provide a procedure to correct VISAR images for geometric distortions and evaluate the performance of the system using Fourier analysis. We finally discuss the spatial and temporal calibrations of the diagnostic. As an example, we compare the pressure extracted from the VISAR analysis of shock-compressed polyimide and silicon.

47 OTHER INSTRUMENTATION

Optimizing ablator thickness for laser shock experiments

In laser shock experiments, a well-defined, flat-top shock wave at the ablator/sample interface is important for accurately probing material response under uniaxial strain compression. However, the relationship between the ablator thickness and the resulting shock wave characteristics is insufficiently understood, limiting the ability to design optimal experiments. To address this need, we conducted a systematic experimental study using a 100 J laser to shock-compress polyimide ablators to peak stresses ranging from 20.4 to 111.6 GPa. Laser interferometry diagnostics measured the transmitted wave profiles at the ablator/sample interface, consistently showing a single jump followed by a constant peak state before the arrival of release waves. Here, by analyzing shock transit time, flat-top duration, and stress, our results establish a framework for selecting ablator thickness to maximize the flat-top duration, improving the precision and reproducibility of laser shock experiments.

design of experiments

Silicon wafer fracture stress for tracking sensors in particle physics experiments

For the construction of the ATLAS Inner Tracker strip detector, silicon strip sensor modules are glued directly onto carbon fibre support structures using a soft silicone gel. During tests at temperatures below -35°C, several of the sensors were found to crack due to a mismatch in coefficients of thermal expansion between polyimide circuit boards with copper metal layers (glued onto the sensor) and the silicon sensor itself. While module assembly procedures were developed to minimise variations between modules, cold tests showed a wide range of temperatures at which supposedly comparable modules failed. The observed variance (fracture temperatures between -35°C and -70°C) for supposedly comparable modules suggests an undetected variation between modules suspected to be intrinsic to the silicon wafer itself. Therefore, a test programme was developed to investigate the fracture stress of representative sensor wafer cutoffs. This paper presents results for the fracture stress of silicon sensors used in detector modules.

Detector design and construction technologies and

Rapid Prototyping Techniques for Organic Direct-Bonded-Copper Power Modules

Organic Direct-Bonded-Copper (ODBC) is a novel packaging technology for power modules which allows higher flexibility in layout design. In this work, a set of rapid prototyping techniques are developed for ODBC modules based on a polyimide dielectric material. These techniques enable fast and low-cost fabrication of modules with 3-Dimensional (3D) layout features. An example half-bridge (HB) silicon carbide (SiC) metal oxide semiconductor field effect transistor (MOSFET) module is designed and prototyped using the proposed techniques aiming at ultra-low power loop inductance. Finite element analysis (FEA)-circuit co-simulations results and experimental results validate an approximately 0.71nH power loop inductance for the example module design.

36 MATERIALS SCIENCE

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

A&L Annual Report: Kapton Strength

Exploding Foil Initiator (EFI) systems function by launching a polymer flyer (often referred to as a slapper) at a high explosive (HE) pellet, which is intended to shock-initiate the HE. Flyer characteristics (e.g., shape, planarity, etc.) are extremely important in this respect, governing their ability to initiate the HE. Polymer models currently used in these systems are largely unvalidated, potentially compromising the integrity of magneto-hydrodynamic (MHD) predictions of EFI function. An improved EFI MHD modelling capability is expected to: (1) expedite optimization of EFI-based initiation system design, (2) enable consideration of EFI-related aging and corresponding lifetime predictions, and (3) potentially minimize the number of costly experiments required to certify EFI designs. To address this knowledge gap, several years ago we began a computational project to develop a higher-fidelity model for Kapton, a Polyimide copolymer most commonly employed as the flyer material in EFI devices.

36 MATERIALS SCIENCE

Laser-induced graphene gas sensors for environmental monitoring

Artemesia tridentatais a foundational plant taxon in western North America and an important medicinal plant threatened by climate change. Low-cost fabrication of sensors is critical for developing large-area sensor networks for understanding and monitoring a range of environmental conditions. However, the availability of materials and manufacturing processes is still in the early stages, limiting the capacity to develop cost-effective sensors at a large scale. In this study, we demonstrate the fabrication of low-cost flexible sensors using laser-induced graphene (LIG); a graphitic material synthesized using a 450-nm wavelength bench top laser patterned onto polyimide substrates. We demonstrate the effect of the intensity and focus of the incident beam on the morphology and electrical properties of the synthesized material. Raman analyses of the synthesized LIG show a defect-rich graphene with a crystallite size in the tens of nanometers. This shows that the high level of disorder within the LIG structure, along with the porous nature of the material provide a good surface for gas adsorption. The initial characterization of the material has shown an analyte response represented by a change in resistance of up to 5% in the presence of volatile organic compounds (VOCs) that are emitted and detected byArtemisiaspecies. Bend testing up to 100 cycles provides evidence that these sensors will remain resilient when deployed across the landscapes to assess VOC signaling in plant communities. The versatile low-cost laser writing technique highlights the promise of low-cost and scalable fabrication of LIG sensors for gas sensor monitoring.

Chemistry

Impacts of Curing-Induced Phase Segregation in Silicon Nanoparticle-Based Electrodes

We report the investigation of silicon nanoparticle composite anodes for Li-ion batteries, using a combination of two nm-scale atomic force microscopy-based techniques: scanning spreading resistance microscopy for electrical conduction mapping and contact resonance and force volume for elastic modulus mapping, along with scanning electron microscopy-based energy dispersion spectroscopy, nanoindentation, and electrochemical analysis. Thermally curing the composite anode—made of polyethylene oxide-treated Si nanoparticles, carbon black, and polyimide binder—reportedly improves the anode electrochemical performance significantly. This work demonstrates phase segregation resulting from thermal curing, where alternating bands of carbon and silicon active material are observed. This electrode morphology is retained after extensive cycling, where the electrical conduction of the carbon-rich bands remains relatively unchanged, but the mechanical modulus of the bands decreases distinctly. These electrical and mechanical factors may contribute to performance improvement, with carbon bands serving as a mechanical buffer for Si deformation and providing electrical conduction pathways. This work motivates future efforts to engineer similar morphologies for mitigating capacity loss in silicon electrodes.

25 ENERGY STORAGE

High performance Calcium Copper Titanate/Polyimide dielectrics composites enabled through colloidal stabilization

Transition to electrified transportation demands advanced power electronic components with the capability to improve range, reliability, and cost of ownership to accelerate mass market adoption. Thus, improvement in the current designs, manufacturing processes, materials, and components capable of providing reliable and efficient operation at higher temperatures play important roles in meeting future needs. To address these challenges, this article focuses on novel dielectric materials designed to reduce the volume of the most important and bulky component of a power electronic system, a capacitor. A new composite dielectric material was developed by integrating the positive attributes of both polymer and ceramic capacitors to overcome the challenges of state-of-the-art dielectric materials. Further, the developed composite properties have been evaluated and showed promising results, achieving a dielectric constant of 250 at 100 Hz, 25°C, unseen in current literature. Additionally, these materials can function at high temperatures (>150°C) with good breakdown strength, providing promising working conditions for capacitors, especially in electric vehicle applications.

36 MATERIALS SCIENCE

A comprehensive study on two types of supercapacitor composite electrodes comprising MnO 2 and activated carbon nanofibers: Self-supporting membrane and ground powder

Manganese dioxide (MnO 2 )@carbon composites have been attractively considered as electrode materials for supercapacitors (SCs) due to synergistic effects. This work systematically investigated the structure of MnO 2 @carbon nanofiber (CNF) composite electrodes with the different forms of CNFs and the corresponding electrochemical performance of SCs. In brief, novel activated carbon nanofibers were first fabricated by electrospinning the hydroxyl-containing poly(amic acid) solution, and then the preferred CNF material was decorated by MnO 2 crystals in the form of self-supporting membrane and ground powders, respectively. Additionally, the synthesis parameters were investigated and optimized based on the electrochemical performance of SCs. The results reveal that the powdered composite electrode exhibits a higher specific surface area of 501 m 2 g –1 compared to the self-supporting membrane composite electrode under the same conditions, resulting in a promising specific capacity of 214.1 mAh g –1 (770.8 Fg –1 ) in 6M KOH solution at 0.5 A g –1 . In addition, the capacitance of the symmetrical SC device assembled by G-HMC-1:3–80 reaches 179.8 Fg –1 , coupled with an energy density of 24.86 Whkg –1 at 230 Wkg –1 power density. This work provides valuable hints for designing SC composite electrode materials with outstanding performance.

25 ENERGY STORAGE

Dielectric properties of neutron and proton irradiated polymeric nanocomposite insulation for superconducting magnets of fusion power plants

Studies on radiation-resistant electrical insulation for superconducting magnets of nuclear fusion power plants are discussed. Metal oxide nanoparticle-incorporated organic polymer composite (MONAP) insulation films were manufactured and studied for their dielectric breakdown strength after exposure to neutrons and proton radiation at varying levels. Samples with up to 5 wt% of nanoparticles (NPs) of SiO 2 , MgO, and ZrO 2 were studied. The samples were exposed to radiation of up to 2 × 10 16 neutrons/cm 2 and 200 Mrad of protons. The addition of the nanoparticles improved the radiation resistance of the MONAP, and the performance depended on the type of NPs and the radiation exposure. Dielectric breakdown measurements at 77 K showed little degradation. Enhancement of dielectric strength was observed in some instances.

36 MATERIALS SCIENCE