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At least 793 records · Page 44

Advancing Core Safety of Gen IV and Gen IV + Reactors by Encompassing High-Temperature Resistant Materials - 18673

The paper focuses on the development of materials for Gen IV/IV+ reactor core. It discusses the advancement of materials studied and their application in different components of the reactor core and other auxiliary components which will help in the development of future generation reactors. The paper summarizes the material study showing the characteristic behavior of different materials (coated with FeB and FeB{sub 2}), towards irradiation at near high temperatures and high energy neutron flux condition. The project includes different materials which are coated on the boundaries with varied thickness of FeB and FeB{sub 2}. The samples included Carbon steel, Stainless steel 310, Stainless steel 316, Inconel 718. All above-mentioned samples were received by Prof. J. Szpunar, through an industry with coatings of FeB and FeB{sub 2} with varied thickness along with a bare sample of each material. The samples were irradiated at the University of Saskatchewan reactor, with fast neutron flux of 1.1x10{sup 11} n.cm{sup -2}.sec{sup -1}. I worked on all the samples but the paper particularly focuses on, two carbon steel samples results, received so far. The methodology for the project been followed for all the samples is as follow: 1. Received samples were first polished. 2. Vickers Hardness Test. 3. Mirror polished. 4. Etched with the appropriate etchant for the material. 5. Microscopic study of the etched surface. 6. SEM imaging. 7. Sent for irradiation. 8. The same set of material testing done after irradiation, with an EBSD run on the boundary and main surface. The two Carbon Steel samples (sample 21 and 19) analyzed, were irradiated for 14 hrs. Sample 21 was a bare sample and sample 19 had a coating of FeB, FeB{sub 2} with a ∼0.0010'' thickness. The methodology was followed for material testing before and after the irradiation. The advantage of FeB and FeB{sub 2} coatings are: 1. Higher hardness - 10 times (FeB-1775 and FeB{sub 2}-1450), 2. High-stress capacity, 3. Lower abrasion, 4. Low corrosion. Through the test results obtained before and after the irradiation, I was able to get a view of coating damage at the boundaries of sample 19. The bare sample don't show any difference after irradiation but the coated sample do show cracks in the FeB layer. Which can be seen in the SEM images of sample 19. The hardness results are promising, as hardness didn't change significantly. The hardness test was done on the substrate as the coating was significantly narrow to perform the test. Though the hardness test on coatings was performed by the possessor company which show hardness higher by a factor of 10 when compared to uncoated surfaces. The XRD results, reveal irradiation effect on the crystal lattice, making it deformed, which though is usual during irradiation. The overall analysis along with EBSD done on the two samples are favorable and promising. Though it still needs to be cleared out, whether the cracks on the coating were due to irradiation or due to etching after the samples were irradiated.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

A Reactive Inkjet Printing Process for Fabricating Biodegradable Conductive Zinc Structures

A novel reactive inkjet printing (RIJ) process for fabricating environmentally benign, conductive zinc structures on biodegradable substrates is reported. A precursor consisting of oxidized zinc microparticles is formulated into a viscous ink for high‐resolution, high‐repeatability screen printing. A single RIJ process is performed to selectively dispense an acid‐based oxide etching agent onto the screen‐printed zinc ink to significantly improve its electrical conductivity, up to 4 × 10 4 S m −1 . The RIJ process enables precise control of the amount of deposited etching agent, allowing control of conductivity and avoiding damage caused by excessive acid exposure. The RIJ process deposits the etching agent selectively on the screen‐printed, water‐soluble zinc patterns, thus preserving the print fidelity by avoiding ink smearing that can occur when using a blanket treatment such as submersion. A printed biodegradable antenna with a minimum feature size of 500 μm for use with a batteryless radio frequency identification (RFID) chip is fabricated as demonstration. Due to the higher ink conductivity and improved pattern fidelity, the antenna fabricated by the RIJ process shows a ≈2.2× increase in reading distance compared with a similar antenna that is screen printed and activated using a drop‐casting process.

Sui, Yongkun↗

Birefringent Glass‐Engraved Quasi‐Linear Nanograting Metasurface Based on Self‐Organizing Process for Large Aperture High Power Laser Applications

All-glass metasurface “nanograting” structures that exhibit birefringence in the formed layer are reported. The key enabler of this work is ion beam processing at an angle sufficiently off-normal incidence, inducing self-assembly of a deposited metal layer into quasi-linear metallic features that can function as an etching mask. As a result, a fused silica metasurface, monolithic to the underlying substrate, is demonstrated at 375 nm wavelength to exhibit a phase delay angle of 30° between the principal axes. The capability of an angled etch mask replenishment process is also demonstrated for achieving deeper etch depth and for increasing the grating period, another first – to the best of the knowledge. This is the first display of a technology capable of fabricating glass-engraved near-linear grating structure with a feature-to-feature period as small as 118.6 nm. Furthermore, this technology has the potential to generate grating-like structures with periods as small as 12.4 nm, as demonstrated here with reactive ion beam processing assisted mask assembly. Furthermore, these structures are shown to have reflectivity < 0.4% across the wavelength band 350 nm – 1000 nm. Such a technology can enable laser-durable grating structures for the deep-UV and even down to soft X-ray wavelengths.

Ray, Nathan J. [Lawrence Livermore National Labora↗

Copper Tantalate by a Sodium-Driven Flux-Mediated Synthesis for Photoelectrochemical CO 2 Reduction

Copper-tantalate, Cu 2 Ta 4 O 11 (CTO), shows significant promise as an efficient photocathode for multi-carbon compounds (C 2+ ) production through photoelectrochemical (PEC) CO 2 reduction, owing to its suitable energy bands and catalytic surface. However, synthesizing CTO poses a significant challenge due to its metastable nature and thermal instability. In this study, this challenge is addressed by employing a flux-mediated synthesis technique using a sodium-based flux to create sodium-doped CTO (Na-CTO) thin films, providing enhanced nucleation and stabilization for the CTO phase. To evaluate the PEC performance and catalytic properties of the films, copper(II) oxide (CuO) at the Na-CTO surface is selectively etched. The etched Na-CTO shows a lower dark current, with decreased contribution from photocorrosion, unlike the non-etched Na-CTO which has remaining CuO on the surface. Furthermore, Na-CTO exhibits 7.3-fold ethylene selectivity over hydrogen, thus highlighting its promising potential as a photocathode for C 2+ production through PEC CO 2 reduction.

copper tantalate↗

Simulation and design of a compact GaAs based tunable dual-wavelength diode laser system

We present our design of a compact, integrated and tunable dual-wavelength diode laser system emitting around 785 nm, which is of interest for several applications like Raman spectroscopy and the generation of THz radiation. To achieve a more compact device compared to previous GaAs based designs two etch depths are realized, leading to shallowly etched ridge waveguides in regions were optical gain is applied and deeply etched waveguides used to enable compact integrated waveguide components. The device parameters are optimized using a numerically efficient simulation tool for passive waveguides. Subsequently, the entire laser system is further analyzed applying a sophisticated traveling-wave equation based model for active devices giving access to internal intensity and carrier density distributions. It is shown that active laser simulations are crucial to deduce critical and performance limiting design aspects not accessible via an all-passive simulation.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Operando STM study of the interaction of imidazolium-based ionic liquid with graphite

Understanding interactions at the interfaces of carbon with ionic liquids (ILs) is crucially beneficial for the diagnostics and performance improvement of electrochemical devices containing carbon as active materials or conductive additives in electrodes and ILs as solvents or additives in electrolytes. The interfacial interactions of three typical imidazolium-based ILs, 1-alkyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (AMImTFSI) ILs having ethyl (C 2 ), butyl (C 4 ) and octyl (C 8 ) chains in their cations, with highly oriented pyrolytic graphite (HOPG) were studied in-situ by electrochemical scanning tunneling microscopy (EC-STM). The etching of HOPG surface and the exfoliation of graphite/graphene flakes as well as cation intercalation were observed at the HOPG/C 2 MImTFSI interface. The etching also takes place in C 4 MImTFSI at -1.5 V vs Pt but only at step edges with a much slower rate, whereas C 8 MIm + cations adsorbs strongly on the HOPG surface under similar conditions with no observable etching or intercalation. Finally, the EC-STM observations can be explained by the increase in van der Waals interaction between the cations and the graphite surface with increasing length of alkyl chains.

25 ENERGY STORAGE↗

Growth, structure, defects and polarized absorption spectral properties of Er:Yb:YCa{sub 4}O(BO{sub 3}){sub 3} crystals

YCa{sub 4}O(BO{sub 3}){sub 3} (YCOB) crystals co-doped with 3 at% Er{sup 3+} and 20 at% Yb{sup 3+} were successfully grown by the Czochralski method. X-ray powder diffraction (XRPD) results show that the as-grown Er:Yb:YCOB crystal belongs to the monoclinic system with space group Cm. And the lattice parameters are a=8.076(8) Å, b=16.023(7) Å, c=3.528(4) Å and β=101.15(4)°. Crystal defects were revealed by chemical etching experiments. The density of etch pits, attributed to dislocations and observed on (010) planes, was found to be not uniform along the crystal diameter. The detailed polarized absorption spectra were measured. The polarized absorption cross sections at 977 nm are 1.01×10{sup −20}, 1.22×10{sup −20} and 1.05×10{sup −20} cm{sup 2} for E//X, E//Y and E//Z, respectively. And the polarized absorption cross sections at 1538 nm is about 1.86×10{sup −20} cm{sup 2} for both E//X and E//Z, but for E//Y the result is 1.03×10{sup −20} cm{sup 2}, which is much smaller. The relationship between the crystal structure and absorption spectra was discussed. - Graphical abstract: The as-grown bulk Er:Yb:YCOB crystal (the long axis is along the b-axis) and LeBail fit to the XRPD pattern of Er:Yb:YCOB (top) compared to the diffraction pattern of YCOB from the JCPDS data bank (bottom). Reflection markers indicate the calculated reflection positions. The middle trace gives the difference between observed and calculated intensity. Reflection indices corresponding to the strongest diffraction peaks are marked on the experimental pattern. - Highlights: • Er:Yb:YCOB crystal with a new composition was grown. • XRPD and FT-IR showed a certain degree of deformation in the crystal structure. • Detailed polarized absorption cross sections at 977 nm and 1538 nm were calculated. • Crystal defects were clearly revealed by chemical etching experiments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Polymer microfilters with nanostructured surfaces for the culture of circulating cancer cells

There is a critical need to improve the accuracy of drug screening and testing through the development of in vitro culture systems that more effectively mimic the in vivo environment. Surface topographical features on the nanoscale level, in short nanotopography, effect the cell growth patterns, and hence affect cell function in culture. We report the preliminary results on the fabrication, and subsequent cellular growth, of nanoscale surface topography on polymer microfilters using cell lines as a precursor to circulating tumor cells (CTCs). To create various nanoscale features on the microfilter surface, we used reactive ion etching (RIE) with and without an etching mask. An anodized aluminum oxide (AAO) membrane fabricated directly on the polymer surface served as an etching mask. Polymer filters with a variety of modified surfaces were used to compare the effects on the culture of cancer cell lines in blank culture wells, with untreated microfilters or with RIE-treated microfilters. We then report the differences of cell shape, phenotype and growth patterns of bladder and glioblastoma cancer cell lines after isolation on the various types of material modifications. Our data suggest that RIE modified polymer filters can isolate model cell lines while retaining ell viability, and that the RIE filter modification allows T24 monolayering cells to proliferate as a structured cluster. Copyright 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Makarova, Olga V.↗

Short communication: Assessment of the dislocation density using X-ray topography in Al single crystals annealed for long times near the melting temperature

Earlier work by the authors determined the dislocation density as a function of time in aluminum single crystals annealed near the melting temperature using etch-pits. It was found that the dislocation density is stable and unchanged even with annealing times up to one year for statically annealed Al single crystals with an initially low dislocation density. As several investigators have suggested that etch-pits are not reliable compared to transmission electron microscopy in assessing the dislocation density, the current study utilized x-ray topography at a synchrotron for dislocation density measurements. This work, then, is a short paper complementing the authors earlier work by using a new, reliable, but rarely utilized non-destructive technique to measure the dislocation density. The results confirm the trend of the earlier study using etch-pits by the authors.

36 MATERIALS SCIENCE↗

Growth and Stability of Titanium Dioxide Nanoclusters on Graphene/Ru(0001)

Titanium dioxide/graphene composites have recently been demonstrated to improve the photocatalytic activity of TiO2 in visible light. To better understand the interactions of TiO2 with graphene we have investigated the growth of TiO2 nanoclusters on single-layer graphene/Ru(0001) using scanning tunneling microscopy (STM) and Auger electron spectroscopy (AES). Deposition of Ti in the O2 background at 300 K resulted in the formation of nanoclusters nucleating on intrinsic defects in the graphene (Gr) layer. The saturation nanocluster density decreased as the substrate temperature was increased from 300 to 650 K, while deposition at 700 K resulted in the significant etching of the Gr layer. We have also prepared nanoclusters with Ti2O3 stoichiometry using lower O2 pressures at 650 K. Thermal stability of the TiO2 nanoclusters prepared at 300 K was evaluated with AES and STM. No change in oxidation state for the TiO2 nanoclusters or etching of the Gr layer was observed up to ~900 K. Annealing studies characterized using STM revealed that cluster ripening proceeds via a Smoluchowski mechanism below 800 K and that Ostwald ripening dominates above 800 K. At even higher temperatures, the nanoclusters undergo reduction to TiOx (x ≈ 1 - 1.5) which is accompanied by oxidation and etching of the Gr. Our studies demonstrate that highly thermally stable TiOx nanoclusters of controlled composition and morphology can be prepared on Gr supports.

Auger electron spectroscopy↗

Layer-by-Layer Thinning of PdSe 2 Flakes via Plasma Induced Oxidation and Sublimation

Controlled O2/Ar plasma exposure and subsequent low temperature inert atmosphere annealing of chemical vapor deposition (CVD) grown PdSe2 flakes etch PdSe2 layer-by-layer in an atomic layer etching-like (ALE) process. X-ray photoelectron spectroscopy (XPS) shows that exposure to a remote inductively coupled plasma (ICP) oxygen plasma oxidizes the top layer of the PdSe2 to form PdO2 and SeO2. After an in situ annealing, XPS shows no trace of PdO2 or SeO2, suggesting the byproducts are volatile at low temperature. Atomic force microscopy of PdSe2 exposed to various O2 + Ar plasmas (O2 = 25–100%) demonstrates a clear trend between the oxygen concentration and the number of layers etched per cycle. PdSe2 field effect transistors (FETs) were characterized at various stages of two ALE-like cycles, and the electrical properties are correlated to the oxidation and byproduct desorption and layer reduction.

Hoffmann, Anna↗

Reactive Intermediates or Inert Graphene? Temperature- and Pressure-Determined Evolution of Carbon in the CH 4 –Ni(111) System

Atomic-level identification of carbon intermediates under reaction conditions is essential for carbon-related heterogeneous catalysis. Using the in operando technique of near-ambient-pressure X-ray photoelectron spectroscopy, we have identified in this paper various carbon intermediates during the thermal decomposition of CH 4 on Ni(111), including *CH, *C 1 /Ni 3 C, *C n (n ≥ 2), and clock-reconstructed Ni 2 C at different temperature regions (300–900 K). These “reactive” carbon precursors can either react with probing molecules such as O 2 at room temperature or be etched away by CH 4 . They can also develop into graphene flakes under controlled conditions: a temperature between 800 and 900 K and a suitable CH 4 pressure (10 –3 –10 –1 mbar, depending on temperature). The growth rate of graphene is significantly restrained at higher CH 4 pressures, due to the accelerated etching of its carbon precursors. The identification of in operando carbon intermediates and the control of their evolution have great potential in designing heterogeneous catalysts for the direct conversion of methane. Finally, the observed carbon aggregation/etching equilibrium reveals an underlying mechanism in coking prevention and in the fabrication of large-area single-crystal graphene, where the suppression of seeding density and etching up of small grains are required.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Microscopic Observation of Solid Electrolyte Interphase Bilayer Inversion on Silicon Oxide

Silicon has been investigated in recent years as an alloying anode material to enhance gravimetric energy density in lithium-ion batteries. Although recent developments have suggested that silicon oxides exhibit improved cycling stability over pure Si, the origin of the improved cycling performance is still poorly understood. The initial solid electrolyte interphase (SEI) formation mechanisms on Si wafers with both native oxide and chemically etched thermal oxide coatings are investigated structurally, chemically, and morphologically in the nanoscale. After one electrochemical cycle, microscopy reveals that SEI formed on native SiO x features the typical SEI bilayer structure with a carbon-rich outer SEI layer and an inorganic-rich inner SEI layer. In contrast, the SEI formed on chemically etched thermal oxide shows an inversion in the structure. This work observes distinct initial SEI formation mechanisms on the HF-etched SiO 2 surface, which may be partially responsible for improved cycle life observed in SiO x -based anode materials.

25 ENERGY STORAGE↗

Nonlocal Metasurfaces with Lithographically Defined Vertical Symmetry Breaking

Nonlocal metasurfaces have garnered significant interest for applications that require customized and enhanced light–matter interactions in a flat form factor. These metasurfaces are distinctive for their ability to systematically control some of the fundamental properties of optical resonances by manipulating the in-plane symmetry of the lattice. Recent theoretical works have suggested that engineering the symmetry of a metasurface not just within the plane of the metasurface but also in the vertical or out-of-plane direction enables improved control of additional fundamental properties, especially chirality. However, standard nanofabrication processes cannot readily support elaborate vertical symmetry breaking such as nanostructure heights or slopes that deliberately vary across the footprint of a metasurface. Here, in this work, we experimentally demonstrate a scalable method to lithographically define the vertical symmetry of nonlocal metasurfaces by selectively eroding the etch mask during the etch process. Moreover, as the etch mask erosion rates depend on the in-plane size of individual nanostructures, we introduce and experimentally demonstrate a compatible design framework that enables versatile control over the properties of optical resonances. The results hold promise for chiral nonlocal metasurfaces with highly customized behavior.

metamaterial↗

MPCVD-Grown Nanodiamond Microelectrodes with Oxygen Plasma Activation for Neurochemical Applications

Nanodiamonds (NDs) are a carbon nanomaterial that has a diamond core with heteroatoms and defects at the surface. The large surface area, defect sites, and functional groups on NDs make them a promising material for electrochemical sensing. Previously, we dip-coated ND onto carbon-fiber microelectrodes (CFMEs) and found increases in sensitivity, but the coating was sparse. Here, for this work, we directly grew thin films of ND on niobium wires using microwave plasma chemical vapor deposition (MP-CVD) to provide full surface coverage. ND microelectrodes show a reliable performance in neurotransmitter detection with good antifouling properties. To improve sensitivity, we oxygen plasma etched ND films to activate the surface and intentionally add defects and oxygen surface functional groups. For fast-scan cyclic voltammetry detection of dopamine, oxygen plasma-etching increases the sensitivity from 21 nA/μM to 90 nA/μM after treatment. Fouling was tested by repeated injections of serotonin or tyramine, and both ND and plasma oxidized nanodiamond (NDO) microelectrodes maintain their currents better compared to CFMEs and therefore are more antifouling. Furthermore, a biofouling test in brain slices shows that ND microelectrodes barely have any current drop, while the more hydrophilic NDO microelectrodes decrease more, but still not as much as CFMEs. Overall, grown ND microelectrodes are promising in neurotransmitter detection with excellent fouling resistance, whereas oxygen plasma etching slightly lowers the fouling resistance but dramatically increases sensitivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Mosaic lateral heterostructures in two-dimensional perovskite

Lateral heterostructures are important for exploring exotic physics, developing new devices and achieving device miniaturization. Endo-epitaxial growth occurring in patterned templates presents a promising strategy to realize extensive patterned areas in heterostructures, as recently demonstrated with two-dimensional (2D) covalent materials. However, the conventional lithography and etching processes used to prepare patterned templates are too aggressive for 2D lead halide perovskites, owing to their inherently soft and unstable ionic lattice. Here we create square holes of controllable size within 2D lead halide perovskites, enabling the fabrication of continuous lateral heterostructures over large areas. We demonstrate that the square holes form through spontaneous etching, a process initiated by internal strain and stabilized along the [100]/[010] crystallographic direction. Furthermore, the size of the square holes can be controlled by adjusting the etching time and temperature. Moreover, by incorporating a rapid solvent evaporation growth technique, the edges of the square holes act as templates for epitaxial growth of another type of perovskite, incorporating different halide or metal ions. Finally, we realized a series of mosaic lateral heterostructures that can emit various colours for light-emitting devices. As a result, this synthesis of diverse 2D perovskite mosaic lateral heterostructures provides valuable insights into the structural characteristics of perovskites and offers a versatile material platform for the development of complex integrated emitting devices.

Organic–inorganic nanostructures↗

Solution processes for ultrabroadband and omnidirectional graded-index glass lenses with near-zero reflectivity in high concentration photovoltaics

Abstract Concentrator photovoltaic (CPV) systems, where incident direct solar radiation is tightly concentrated onto high-efficiency multi-junction solar cells by geometric optical elements, exhibit the highest efficiencies in converting the sun’s energy into electric power. Their energy conversion efficiencies are greatly limited, however, due to Fresnel reflection losses occurring at three air/optics interfaces in the most sophisticated dual-stage CPV platforms. This paper describes a facile one-step wet-etching process to create a nanoporous surface with a graded-index profile on both flat and curved glasses, with capabilities of achieving ~99% average transmission efficiency in a wide wavelength range from 380 nm to 1.3 µm and for a wide range of incident angles up to ±40° regardless of the polarization state of incident sunlight. The simplicity of the etching process remarkably increases their versatility in various optical elements that require unconventional form factors such as Fresnel lenses and microlens arrays, and/or demanding curvatures along with much reduced dimensions such as ball lenses. Etched glass surfaces on two-stage optical concentrating systems yield enhancements in total optical transmission efficiencies by 13.8% and in the photocurrent by 14.3%, as experimentally determined by measurements on microscale triple-junction solar cells. The presented strategy can be widely adapted in a variety of applications such as image sensors, display systems, and other optoelectronic devices.

36 MATERIALS SCIENCE↗

Mitigating coherent loss in superconducting circuits using molecular self-assembled monolayers

In planar superconducting circuits, decoherence due to materials imperfections, especially two-level-system (TLS) defects at different interfaces, is a primary hurdle for advancing quantum computing and sensing applications. Traditional methods for mitigating TLS loss, such as etching oxide layers at metal and substrate interfaces, have proven to be inadequate due to the persistent challenge of oxide regrowth. In this work, we introduce a novel approach that employs molecular self-assembled monolayers (SAMs) to chemically bind at different interfaces of superconducting circuits. This technique is specifically tested here on coplanar waveguide (CPW) resonators, in which this method not only impedes oxide regrowth after surface etching but can also tailors the dielectric properties at different resonators interfaces. The deployment of SAMs results in a consistent improvement in the measured quality factors across multiple resonators, surpassing those with only oxide-etched resonators. The efficiency of our approach is supported by microwave measurements of multiple devices conducted at millikelvin temperatures and correlated with detailed X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) characterizations of SAM-passivated resonators. The compatibility of SAMs materials with the established fabrication techniques offers a promising route to improve the performance of superconducting quantum devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗