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At least 1,441 records · Page 80

Low-Shear Microencapsulation and Electrostatic Coating

A report presents additional information on the topic of a microencapsulation electrostatic processing system. Information in the report includes micrographs of some microcapsules, a set of diagrams that schematically depict the steps of an encapsulation process, and brief descriptions of (1) alternative versions of the present encapsulation processes, (2) advantages of the present microencapsulation processes over prior microencapsulation processes, and (3) unique and advantageous features of microcapsules produced by the present processes.

Morrison, Dennis R.↗

Effect of ATF Cr-coated-Zircaloy on BWR In-vessel Accident Progression during a Station Blackout

The deposition of protective coatings on nuclear fuel cladding has been considered as a near-term Accident Tolerant Fuel (ATF) concept that will reduce the high-temperature oxidation rate and enhance accident tolerance of the cladding while providing additional benefits during normal and transient. In this study, the performance of the proposed ATF concept of Cr-coated-Zircaloy is assessed using a generic Boiling Water Reactor MELCOR plant model considering a Short-term Station Blackout (STSBO) scenario. Simulation results indicate that the use of Cr-coated-Zircaloy as cladding and canister material mitigates the core degradation process as compared to the traditional Zircaloy cladding and canister design. The onset of fuel degradation and collapse is delayed by over thirty minutes, and the extent of fuel degradation is reduced. Specifically, the gross in-vessel hydrogen generation decreased by almost a factor of three. Although the eutectic reaction between Cr-coating and Zircaloy could cause an early failure of the coating, the improvement in the delay of fuel degradation is still notable. In addition, a thicker coating is found helpful to obtain additional coping time and to decrease hydrogen generation. In addition to the eutectic formation that may compromise Cr-coated Zr, a different failure mode is identified for the Cr-coated-Zr when compared to Zircaloy; i.e., a complete melt of base material leads to component collapse before the coating is oxidized and consumed. These findings can help the industry focus on productive areas of research and development for accident-tolerant fuel concepts and enhancement of core safety margins.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Spin-on deposition of amorphous zeolitic imidazolate framework films for lithography applications

Amorphous zeolitic imidazolate framework (aZIF) films have been recently introduced as resists for electron beam and extreme ultraviolet lithography. aZIFs are also being considered for separation applications, including thin film membranes. However, the reported methods for aZIF deposition are currently based on highly empirical trial-and-error approaches that hinder control of film composition, thickness and uniformity as well as scale-up and transferability to different coating geometries. This work presents a method for depositing aZIF films with controllable thickness using dilute precursors mixed immediately before encountering the substrate. Importantly, the method is amenable to quantitative analysis by computational fluid dynamics to extract intrinsic deposition rates and limiting reactant transport diffusivities, enabling predictive physics-based modeling of the deposition process. This allows the deposition method to be adapted for spin coating on silicon wafers to prepare high-quality aZIF films with consistently controlled thickness. Using this approach, high-resolution resist performance and wafer-scale use for beyond extreme-ultraviolet lithography of aZIF films is demonstrated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Processes at lithium-hydride/deuteride surfaces upon low energy impact of H/D

Sputtering, reflection, and retention processes at amorphous and crystalline lithium hydride surfaces due to impact of low energy (1–100 eV) hydrogen and deuterium atoms over the range of 0 o −85 o angle of incidence at 300 K surface temperature were investigated by atomistic computational methods. Classical molecular dynamics simulations were performed with improved reactive bond-order force field (ReaxFF) potentials that include long-range polarization effects. In addition to probabilities of surface processes, the energy and angular spectra of ejected particles were obtained. Comparison of these results with those previously obtained on pristine lithium surfaces indicates the importance of saturation of the Li surface and near-surface region with hydrogen. We show that such saturation, which is typical in both laboratory and fusion device experiments with lithium coating of the plasma-facing surfaces, significantly changes the surface processes with hydrogen irradiation in the understudied low-energy region of impact energies.

74 ATOMIC AND MOLECULAR PHYSICS↗

Investigation of rotor blade roughness effects on turbine performance

The cold air test program was completed on the SSME (Space Shuttle Main Engine) HPFTP (High Pressure Fuel Turbopump) turbine with production nozzle vane rings and polished coated rotor blades with a smooth surface finish of 30 microinch (0.76 micrometer) RMS (Root Mean Square). The smooth blades were polished by an abrasive flow machining process. The test results were compared with the air test results from production rough coated rotor blades with a surface finish of up to 400 microinch (10.16 micrometer) RMS. Turbine efficiency was higher for the smooth blades over the entire range tested. Efficiency increased 2.1 percentage points at the SSME 104 percent RPL (Rated Power Level) condition. This efficiency improvement could reduce the SSME HPFTP turbine inlet temperature by 57 degrees Rankine (32 degrees Kelvin) increasing turbine durability. The turbine flow parameter increased and the mid-span outlet swirl angle became more axial with the smooth rotor blades.

Boynton, J. L.↗

Microrectenna: A Terahertz Antenna and Rectifier on a Chip

A microrectenna that would operate at a frequency of 2.5 THz has been designed and partially fabricated. The circuit is intended to be a prototype of an extremely compact device that could be used to convert radio-beamed power to DC to drive microdevices (see Figure 1). The microrectenna (see Figure 2) circuit consists of an antenna, a diode rectifier and a DC output port. The antenna consists of a twin slot array in a conducting ground plane (denoted the antenna ground plane) over an enclosed quarter-wavelength-thick resonant cavity (denoted the reflecting ground plane). The circuit also contains a planar high-frequency low-parasitic Schottky-barrier diode, a low-impedance microstrip transmission line, capacitors, and contact beam leads. The entire 3-D circuit is fabricated monolithically from a single GaAs wafer. The resonant cavity renders the slot radiation pattern unidirectional with a half-power beam width of about 65. A unique metal mesh on the rear of the wafer forms the backplate for the cavity but allows the GaAs to be wet etched from the rear surface of the twin slot antennas and ground plane. The beam leads protrude past the edge of the chip and are used both to mount the microrectenna and to make the DC electrical connection with external circuitry. The antenna ground plane and the components on top of it are formed on a 2- m thick GaAs membrane that is grown in the initial wafer MBE (molecular beam epitaxy) process. The side walls of the antenna cavity are not metal coated and, hence, would cause some loss of power; however, the relatively high permittivity (epsilon=13) of the GaAs keeps the cavity modes well confined, without the usual surface-wave losses associated with thick dielectric substrates. The Schottky-barrier diode has the usual submicron dimensions associated with THz operation and is formed in a mesa process above the antenna ground plane. The diode is connected at the midpoint of a microstrip transmission line, which is formed on 1- m-thick SiO (permittivity of 5) laid down on top of the GaAs membrane. The twin slots are fed in phase by this structure. To prevent radio-frequency (RF) leakage past the slot antennas, low-loss capacitors are integrated into the microstrip transmission line at the edges of the slots. The DC current- carrying lines extend from the outer edges of the capacitors, widen approaching the edges of the chip, and continue past the edges of the chip to become the beam leads used in tacking down the devices. The structure provides a self-contained RF to DC converter that works in the THz range.

Siegel, Peter↗

Characterization of electroless nickel-phosphorus plating for ultracold-neutron storage

Electroless nickel plating is an established industrial process that provides a robust and relatively low-cost coating suitable for transporting and storing ultracold neutrons (UCN). Using roughness measurements and UCN-storage experiments we characterized UCN guides made from polished aluminum or stainless-steel tubes plated by several vendors. All electroless nickel platings were similarly suited for UCN storage with an average loss probability per wall bounce of 2.8 • 10 -4 to 4.1 • 10 -4 for energies between 90 neV and 190 neV, or a ratio of imaginary to real Fermi potential η of 1.7 • 10 -4 to 3.3 • 10 -4 . Measurements at different elevations indicate that the energy dependence of UCN losses is well described by the imaginary Fermi potential. Some special considerations are required to avoid an increase in surface roughness during the plating process and hence a reduction in UCN transmission. Increased roughness had only a minor impact on storage properties. In conclusion, based on these findings we chose a vendor to plate the UCN-production vessel that will contain the superfluid-helium converter for the new TRIUMF UltraCold Advanced Neutron (TUCAN) source, achieving acceptable UCN-storage properties with η = 3.5(5)•10 -4 .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A program continuation to develop processing procedures for advanced silicon solar cells

Shallow junctions, aluminum back surface fields and tantalum pentoxide (Ta205) antireflection coatings coupled with the development of a chromium-palladium-silver contact system, were used to produce a 2 x 4 cm wraparound contact silicon solar cell. One thousand cells were successfully fabricated using batch processing techniques. These cells were 0.020 mm thick, with the majority (800) made from nominal ten ohm-cm silicon and the remainder from nominal 30 ohm-cm material. Unfiltered, these cells delivered a minimum AMO efficiency at 25 C of 11.5 percent and successfully passed all the normal in-process and acceptance tests required for space flight cells.

Avery, J. E.↗

Lyotropic Liquid Crystal Mediated Assembly of Donor Polymers Enhances Efficiency and Stability of Blade-Coated Organic Solar Cells

Conjugated polymers can undergo complex, concentration-dependent self-assembly during solution processing, yet little is known about its impact on film morphology and device performance of organic solar cells. Herein, lyotropic liquid crystal (LLC) mediated assembly across multiple conjugated polymers is reported, which generally gives rise to improved device performance of blade-coated non-fullerene bulk heterojunction solar cells. Using D18 as a model system, the formation mechanism of LLC is unveiled employing solution X-ray scattering and microscopic imaging tools: D18 first aggregates into semicrystalline nanofibers, then assemble into achiral nematic LLC which goes through symmetry breaking to yield a chiral twist-bent LLC. The assembly pathway is driven by increasing solution concentration – a common driving force during evaporative assembly relevant to scalable manufacturing. This assembly pathway can be largely modulated by coating regimes to give 1) lyotropic liquid crystalline assembly in the evaporation regime and 2) random fiber aggregation pathway in the Landau–Levich regime. The chiral liquid crystalline assembly pathway resulted in films with crystallinity 2.63 times that of films from the random fiber aggregation pathway, significantly enhancing the T80 lifetime by 50-fold. The generality of LLC-mediated assembly and enhanced device performance is further validated using polythiophene and quinoxaline-based donor polymers.

14 SOLAR ENERGY↗

Photoelectrochemical and Photovoltaic Performance of As-deposited Ink-based CuInS 2 Heterojunction Thin Film

In this report, we demonstrate low-temperature ink-based fabrication of CuInS 2 -based photoelectrodes for hydrogen production capable of producing photocurrent densities as high as 8.8mA.cm -2 . In this process, molecular ink made of metal chlorides and thiourea dissolved in methanol was spin coated onto Mo-coated soda lime glass substrates. Samples were then placed on a hot plate (sample surface temperature: 250°C) to induce CuInS 2 formation and remove the solvent and by-products. No further processing, such as high temperature sulfurization, was performed. Further, the CuInS 2 films were then integrated as photocathode for hydrogen evolution by photoelectrodeposition of Pt nanoparticles. Photocurrent density of 0.4mA.cm -2 at 0V vs. RHE was detected from such electrodes. However, samples coated with CdS/ZnO/ITO overlayers forming heterojunction prior to Pt deposition exhibited significant improvement of the photocurrent density, reaching 8.8mA.cm -2 at 0V vs. RHE, highlighting the improved charge transfer by the p-n junction formed at the CuInS 2 /CdS interface. The charge transfer resistance of the CuInS 2 /CdS/ZnO/ITO-Pt photoelectrode was almost 5 times lower than that of the CuInS 2 -Pt photoelectrode as revealed by electrochemical impedance spectroscopy analysis. In addition, the onset potential was shifted by ca. 0.45V toward the anodic direction, reaching 0.75V vs. RHE. Solar cell made of identical structure (Mo/CuInS 2 /CdS/ZnO/ITO) showed power conversion efficiency of 2.1% with short-circuit photocurrent density and open circuit voltage of 7.4mA.cm -2 and 820mV, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructure detection of Mg-Zi-Ti-Si amorphous composite coating prepared by SMAT

Highlights: • The Mg-Zn-Ti-Si amorphous composite coating was prepared on Mg alloy via SMAT. • Except for amorphous portion, the phases of coating include Zn, Mg{sub 7}Zn{sub 3}, and Si. • The coating was thick and rough but it was well combined with the matrix. • During SMAT, the matrix surface was also strengthened because of solid-solution and grain refinement. - Abstract: The Mg-Zn-Ti-Si coating was prepared on Mg alloy through surface mechanical attrition treatment (SMAT) which was simple and low-cost. The microstructure and phase composition of coating were detected through a scanning electron microscope (SEM), an X-ray diffractometer (XRD) and a high resolution transmission electron microscope (HRTEM). The results demonstrated that the layer thickness, which depended on the rotation speed, was 20–80 μm. Although the coating was rough, it was well combined with the matrix. The XRD pattern and HRTEM image analysis demonstrated that the coating contained both amorphous and crystalline phases (Zn, Mg{sub 7}Zn{sub 3} and Si). The process also led to matrix surface strengthening; the mechanisms are solid solution and grain refinement.

36 MATERIALS SCIENCE↗

Modeling and analysis of solvent removal during Li-ion battery electrode drying

In this paper, we study the design aspects and process dynamics of solvent removal from Lithium-ion battery electrode coatings. For this, we use a continuum level mathematical model to describe the physical phenomenon of cathode drying involving coupled simultaneous heat and mass transfer with phase change. Our results indicate that around 90% of solvent is removed in less than half of the overall drying time. We study the effect of varying temperature and air velocity on the drying process. We show that the overall drying energy can be reduced by at least 50% by using a multi-zone drying process. Also, the peak solvent flux can be reduced by at least 40%. We further present the effect of using an aqueous solvent instead of N-Methyl-2-pyrrolidone (NMP) in electrode drying. Our results indicate that Water dries nearly 4.5 times faster as compared to NMP and requires nearly 10 times less overall drying energy per kg of solvent.

25 ENERGY STORAGE↗

Enhanced Catalyst Durability for Bio-Based Adipic Acid Production by Atomic Layer Deposition

Harsh reaction environments challenge the lifetime productivity of conventional catalysts and impede emerging biobased chemical processes. Condensed-phase processing of muconic acid, a biobased platform chemical, leads to problematic levels of catalyst leaching and fouling. Atomic layer deposition (ALD) can improve catalyst durability using protective metal oxide coatings; however, a targeted coating strategy and cost models thereof are needed for application-specific deactivation challenges that can surmount these challenges while accounting for process implications. Herein, we utilize thin (<5 wt% Al) Al2O3 ALD coatings to increase the lifetime productivity of Pd/TiO2 during muconic acid hydrogenation to adipic acid. The ALD coating decreases Pd leaching by >3x and markedly improves the thermal stability of Pd and TiO2. Economic analysis for an adipic acid biorefinery supports that increased material costs and reduced catalyst productivity can be justified through lifetime extension. Broadly, this work lays the foundation for reducing the cost of biobased chemical processes through catalyst stability.

Settle, Amy↗

Solvent-Free Coating of Organic Semiconductor Membranes with Centimetric Crystalline Domains

Organic semiconductors (OSCs) have shown great promise in a variety of applications. Although solution processing of OSCs has resulted in high-quality films, exquisite control of structural development to minimize defect formation during large-scale fabrication remains formidable. Compounding this challenge is the use of halogenated organic solvents, which poses significant health and environmental hazards. However, the solvent-free techniques introduced thus far impose additional limitations on solidification kinetics; the resulting OSC thin films are often more defective than those processed from solution. Here, a solvent-free technique is reported to prepare OSC membranes with centimetric crystalline domains. Leveraging the tendency for liquid crystalline materials to preferentially orient, OSCs are “prealigned” by depositing them from the melt over a metal frame to form a freely suspended membrane. Additionally, crystallization from this prealigned phase affords membranes with unprecedented structural order across macroscopic distances. Field-effect transistors comprising membranes of dioctyl[1]-benzothieno[3,2-b][1]benzothiophene (C8BTBT) and didodecyl[1]-benzothieno[3,2-b][1]benzothiophene (C12BTBT) having centimeter-sized domains as active layers exhibit a hole mobility of ≈8.6 cm2 V -1 s -1 , superseding the mobility of any transistors whose active layers are deposited from melt. This technique is scalable to yield membranes with large crystalline domains over wafer dimensions, making it amenable for broad applications in large-area organic electronics.

36 MATERIALS SCIENCE↗

Structural and Dynamical Insights into the Formation Process of a Cross-Linked Polymer Network in Acrylic Adhesives During Thermal Curing

Many modern adhesives, sealants, and coatings rely on the controlled transition from a liquid to a solid state by forming a three-dimensional cross-linked polymer network, often referred to as curing. The curing process, which is initiated by the mixing of reactive components or an external trigger, defines the structure of a network and further controls the final mechanical properties of cured materials. However, the curing mechanism is not fully understood yet due to the lack of experimental tools capable of directly probing the structure and dynamics of a network over relevant time- and length scales. Here, in this paper, we report the curing process of a commercial two-component methyl methacrylate (MMA) adhesive using in operando X-ray photon correlation spectroscopy (XPCS), a method that closely simulates the target manufacturing environment of the adhesive. The results are then integrated with those obtained by rheology, differential scanning calorimetry (DSC), and transmission electron microscopy to establish the structure–dynamics–process–property relationship. The XPCS results identify four distinct stages in the curing process after the mixing, extrusion, and deposition of the acrylic adhesive: (i) At a cure time (or “aging time”, t age ) of less than 1 min, nanodomains of polymerized MMA are formed within a liquid monomeric MMA matrix. The average size is several nm and remains constant over t age , while the dynamics of the nanodomains are slowed down with t age due to an increase in the viscosity of the MMA matrix. (ii) After t age > 1 min, the size of the nanodomains increases with t age until the gel point (= 6.3 min after mixing as determined by rheology). The dynamics of the nanodomains also increase due to the heat generated by the exothermic reaction. (iii) At the gel point, the nanodomains begin to interconnect each other, resulting in a network structure with a characteristic length of about 100 nm. This characteristic network size does not change for the rest of the curing process up to t age = 500 min. The dynamics of the network structure, however, show a rapid slowing down with t age up to t age ≈ 12 min, corresponding to the onset of vitrification (as determined by rheology). (iv) At t age > 12 min, when the DSC and rheology data can no longer provide meaningful information, the XPCS data show a further slowing down of the network dynamics associated with vitrification. Our results provide rich and complex insights into the physics and material design of thermosets in commercially relevant processes, which are essential for future industrial applications.

36 MATERIALS SCIENCE↗

Preparation of nickel oxide thin films at different annealing temperature by sol-gel spin coating method

Preparation of NiO thin films at different annealing temperature by sol-gel method was conducted to synthesize the quality of the surface thin films. The effects of annealing temperature on the surface topology were systematically investigated. Our studies confirmed that the surface roughness of the thin films was increased whenever annealing temperature was increase. NiO thin films morphology structure analysis was confirmed by field emission scanning electron microscope. Surface roughness of the thin films was investigated by atomic force microscopy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Cathodic Cage Plasma Pre-treatment of TiN-Coated AISI-304 Stainless Steel for Enhancement of Mechanical Strength and Wear Resistance

Although austenitic stainless steels (ASSs) are known for their superior corrosion resistance properties, the use of such materials in motion contact parts is limited due to their low wear resistance. Previous studies reveal that titanium nitride (TiN) coating of ASS significantly improves its hardness and surface morphology but not the wear resistance due to weak interfacing with the substrate. Since plasma nitriding is a flexible and multifunctional case-hardening process, an attempt was made to improve the wear resistance of TiN-coated AISI-304 stainless steel by subjecting it to pre-treatment by pulsed DC cathodic cage plasma nitriding (CCPN) in the abnormal glow region. The hardness of the TiN-coated steel samples (with and without CCPN pre-treatment) was measured using Vickers micro-hardness tester. This test revealed maximum hardness of 2284 HV after plasma treatment of TiN-coated steel. The untreated TiN-coated steel exhibited 10.6 times lower hardness than the plasma pre-treated TiN-coated steel (CCPN-TiN). XRD analysis of the untreated TiN-coated steel showed strong diffraction peaks of TiN (311) and (400) in the spectrum, whereas plasma pre-treated sample contained dominant peaks of TiN (111), (200) and (220). The ball-on-disk wear tester was used to investigate the wear behavior of the samples. Very small wear rate and friction coefficient were reported for CCPN-TiN-coated steel. The observed low wear rate was probably due to the development of a subsurface (i.e., nitrided surface) on TiN-coated steel during CCPN pre-treatment.

36 MATERIALS SCIENCE↗