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At least 235 records · Page 13

Synergistic foam stabilization and transport improvement in simulated fractures with polyelectrolyte complex nanoparticles: Microscale observation using laser etched glass micromodels

Inaccessibility to direct pore scale observation in hydrocarbon recovery of tight shale formations poses a great challenge to water-energy nexus initiatives and necessitates the use of high throughput technologies to emulate environmentally friendly processes. Herein, we employ a precise glass micromodel fabrication and visualization method to isolate the supercritical CO 2 bubbles surrounded by CO 2 -water lamella prepared in saline produced water stabilized with molecular complexation of zwitterionic surfactants (ZS) and polyelectrolyte complex nanoparticles (PECNP). The Selective Laser Enhanced Etching (SLE) technique was selected for micromodel simulation of high-pressure flow. Two representative designs, (1) fracture/micro-crack network 28 and (2) fracture/matrix were etched on fused silica glass with a laser printing machine and scCO 2 foam was injected to study the foamability, propagation, stability, and fluid loss properties. The highly monodispersed and uniformly distributed array of scCO 2 bubbles were detected in flow of scCO 2 foam in highly saline brine containing ionic complexes of positively charged PECNPs and ZS, whereas foam flow with the lamella containing ZS in fractures offered a noticeably large and polydisperse array of scCO 2 bubbles. scCO 2 bubble motion and deformation were traced, and local description of foam flow was visually examined. The confined array of scCO 2 bubbles stabilized by ZS in microcracks was affected by bubble growth and coalescence, whereas the super-populated array of monodispersed scC O2 bubbles with lamella containing complexes of PECNP and ZS were able to fill the channels with stable configurations within the timeframe of comparative stability measurements. The ability of complex fluid to prevent the formation damage was evaluated through fluid loss visualization in micromodels. Probing scCO 2 foam transport in homogenous porous media revealed smaller volume leak-off for scCO 2 foam containing PECNP-ZS ionic complexes.

04 OIL SHALES AND TAR SANDS↗

Three-dimensional (3D) analysis of white etching bands (WEBs) in AISI M50 bearing steel using automated serial sectioning

Dark etching regions (DER) and white etching bands (WEB) form in the subsurface stressed regions of bearing raceways and rolling elements. Also, “butterfly” formations form around non-metallic inclusions and large carbides. The formation of WEBs, DERs and butterfly are dependent on operating conditions, material alloying elements and heat treatment. The DER, WEB and butterfly formations are well studied in two dimensions (2D). The objective of this study was to analyze WEB formation in three dimensions (3D) that will allow better understanding of material transformation after stress cycling. Three rolling contact fatigue (RCF) tested vacuum induction melted vacuum arc re-melted (VIM-VAR) AISI M50 samples (from a bench test, sub-scale test and commercial gas turbine engine) were analyzed using automated serial sectioning to map WEB networks and a butterfly formation in 3D. Automated serial sectioning and 2D optical microstructural data for 3D reconstructions and analysis was done using a fully automated serial sectioning system – Robo-Met.3D®. 3D analysis was performed using Image-Pro Premier 3D. The data set allowed 3D visualization and analysis of the evolution and propagation of WEB and butterfly in M50 bearing steel, including the positive microscopic identification of a ceramic inclusion that was the source of a WEB.

36 MATERIALS SCIENCE↗

Template-free preparation and morphology evolution of (Cu, Ni) honeycomb structure via etching additive manufactured Fe-Cu-Ni alloy

Highlights: • (Cu, Ni) honeycomb structure with pore size of ~11 μm and wall thickness of ~200 nm was prepared. • The morphology evolution and the potential formation mechanism of the (Cu, Ni) honeycomb structure were investigated. • A new template-free method of additive manufacturing combined with etching was proposed to prepare ordered porous structure. • This work provides important insights into the preparation of ordered porous structure without template. - Abstract: Metallic ordered porous structures have attracted increasing attention due to their wide range of applications, but their preparation is usually accompanied with the employing of consumable templates. The development of template-free method to prepare metallic ordered porous structure can significantly reduce the cost as well as streamline the procedures. In the present work, a new template-free method of additive manufacturing combined with etching was proposed to prepare ordered porous structures. (Cu, Ni) honeycomb structure with pore size of ~11 μm and wall thickness of ~200 nm was successfully prepared from the Fe-Cu-Ni precursor alloy. The morphology evolution and the potential formation mechanism of the (Cu, Ni) honeycomb structure were studied. This work provides important insights into the preparation of ordered metallic porous structure without template.

36 MATERIALS SCIENCE↗

A facile in-situ etching route to hollow C@SnO2 nanocomposites and their gas-sensing properties

Highlights: • Hollow C@SnO{sub 2} nanostructure has been designed via a facile in-situ etching technique.. • The C@SnO{sub 2} products possess a high surface are and a hollow carbon core. • The growth of SnO{sub 2} nanosheets and the removal of silica template can be synchronously performed. • The C@SnO{sub 2} products manifest highly sensitive and selective to n-butanol as gas-sensing sensor. - Abstract: A novel hollow carbon@SnO{sub 2} nanocomposite has been developed via a high cost-effective and facile in-situ etching technique. The as-prepared C@SnO{sub 2} product has a high surface area of about 115 m{sup 2} g{sup −1} and a hollow carbon core, where a lot of SnO{sub 2} nanosheets grow onto the carbon shell. Particularly, the silica core as the sacrificial template can be fully removed by hydrofluoric acid (HF) byproduct during the reaction process. Moreover, the deposition of SnO{sub 2} sheets and the removal of the silica template can be synchronously performed by a simple one-step process. When applied as the gas-sensing material, the C@SnO{sub 2} product manifests highly sensitive and selective to n-butanol. The large surface area, hollow nanostructure and the perfect combination of SnO{sub 2} nanosheets and carbon layer contribute to the enhanced gas-sensing performances. The method described in our work can also be employed to design other hollow metal oxides@carbon hybrids for energy storage and catalysis.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Pinhole electrical conductivity in polycrystalline Si on locally etched SiN$_y$/SiO$_x$ passivating contacts for Si solar cells

State-of-the-art monocrystalline Si (c-Si) solar cells require passivating contacts to achieve a high degree of charge-carrier separation and collection. In this work, we focus on boron-doped polycrystalline Si on locally etched silicon nitride/silicon oxide (PLENO) passivating contacts. In PLENO contacts, excellent surface passivation is provided by the ~10 nm dielectric bilayer, while pinholes in the dielectric bilayer, that are filled with doped polycrystalline Si, provide charge-carrier selectivity and transport. During PLENO fabrication, etch undercut in the dielectric bilayer occurs. Here, using electrical characterization and microscopies, we show that undercut causes pinholes to be electrically resistive in PLENO. A processing sequence that eliminates the undercut in the final PLENO structure results in electrically conductive pinholes with low contact resistivity.

14 SOLAR ENERGY↗

Wet-chemical etching of FIB lift-out TEM lamellae for damage-free analysis of 3-D nanostructures

Reducing ion beam damage from the focused ion beam (FIB) during fabrication of cross sections is a well-known challenge for materials characterization, especially cross sectional characterization of nanostructures. To address this, a new method has been developed for cross section fabrication enabling high resolution transmission electron microscopy (TEM) analysis of 3-D nanostructures free of surrounding material and free of damage detectable by TEM analysis. Before FIB processing, nanopillars are encapsulated in a sacrificial oxide which acts as a protective layer during FIB milling. Furthermore, the cross sectional TEM lamella containing the nanopillars is then mounted and thinned with some modifications to conventional FIB sample preparation that provide stability for the lamella during the following wet-chemical dip etch. The wet-chemical etch of the TEM lamella removes the sacrificial oxide layer, freeing the nanopillars from any material that would obscure TEM imaging. Both high resolution TEM and aberration corrected scanning TEM images of Si/SiGe pillars with diameters down to 30 nm demonstrate the successful application of this approach.

3-d nanostructure analysis↗

Cadmium Selective Etching in CdTe Solar Cells Produces Detrimental Narrow-Gap Te in Grain Boundaries

Recent advances in design and processing technology have made possible commercialization of polycrystalline (px)-CdTe as a photovoltaic absorber. Grain boundaries (GBs) are the most prominent structural defects in these devices and undergo significant changes during device fabrication. However, the effects of device fabrication processes on these GBs are not entirely understood. Prevailing models of GBs in thin-film photovoltaics consider individual GBs to have homogeneous properties in their area. Here, using an aberration-corrected scanning transmission electron microscope (STEM)-based low-loss and core-loss electron energy-loss spectroscopy (EELS), we show that back-surface etching of CdTe leads to inhomogeneity within individual grain boundaries. We observe that etching the back surface leads to the conversion of a region of GBs from CdTe to an elemental Te, which has an only 0.33 eV band gap, as deep as 1 μm from the back surface. The presence of elemental Te in GBs this deep into the absorber layer will increase recombination in the absorber layer and limit the extractable open-circuit voltage, thus reducing device efficiency. However, additive methods for back contact formation such as deposition of Te, ZnTe, or other materials preserve the CdTe stoichiometry of the GBs. Thus, especially for the next generations of CdTe-based cells having longer minority carrier diffusion length and/or thinner absorber layers, additive back contacting methods are superior.

36 MATERIALS SCIENCE↗

In Situ Tracking of Nonthermal Plasma Etching of ZIF-8 Films

Surface characterization is critical for understanding the processes used for preparing catalysts, sorbents, and membranes. Nonthermal plasma (NTP) is a process that achieves high reactivity at low temperatures and is used to tailor the surface properties of materials. In this work, we combine the capabilities of infrared reflection absorption spectroscopy (IRRAS) with NTP for the in situ interrogation of zeolitic imidazolate framework-8 (ZIF-8) thin films to probe modifications in the material induced by oxygen and nitrogen plasmas. The IRRAS measurements in oxygen plasma reveal etching of organic ligands with sequential removal of the methyl group and imidazole ring and with the formation of carbonyl moieties (C═O). In contrast, nitrogen plasma induces mild etching and grafting of nitrile groups (−C≡N). Scanning electron microscopy imaging shows that oxygen plasma, at prolonged times, significantly degrades the ZIF-8 film at the grain boundaries. Treatment of ZIF-8 membranes using mild plasma conditions yields a fivefold enhancement for H 2 /N 2 and CO 2 /CH 4 ideal selectivities and an eightfold enhancement for CO 2 /N 2 ideal selectivity. Additionally, the new tools described here can be used for spectroscopic in situ tracking of plasma-induced chemistry on thin films in general.

IRRAS↗

Nanoscale groove textured β -Ga 2 O 3 by room temperature inverse metal-assisted chemical etching and photodiodes with enhanced responsivity

β-Ga 2 O 3 is an emerging wide band-gap semiconductor that holds great promise for next generation power electronics and optoelectronics. β-Ga 2 O 3 based ultraviolet photodetectors have been the subject of active research for the last few years. However, no micro and nanostructure surface texturing has been demonstrated for efficient light management in β-Ga 2 O 3 optoelectronic applications yet. We hereby present nanoscale groove textured β-Ga 2 O 3 metal-semiconductor-metal photodiodes, enabled by the unique metal-assisted chemical etching (MacEtch) method at room temperature in liquid. Although the textured surface stoichiometry shows ~10% oxygen deficiency which results in a reduced Schottky barrier height and increased dark current, clear enhancement of the responsivity is demonstrated, compared to the planar untreated surface. Overall, the realization of MacEtch's applicability to β-Ga 2 O 3 opens the door for producing more sophisticated device structures for this material, without resorting to conventional dry etch and potential damage.

42 ENGINEERING↗

Controlling Pinhole Radius and Areal Density in a-Si/SiOx Using Metal-Assisted Chemical Etching

Polysilicon on silicon oxide (poly-Si/SiOx) passivating contacts with predominant charge-carrier transport via pinholes are currently prepared via a>1000 degrees C thermal step to induce oxide break-up. Herein, we develop the precursor of a pinhole-enabled poly-Si/SiOx contact utilizing room temperature metal-assisted chemical etching (MACE) to form pinholes in the SiOx. The pinholes were created via electroless Ag nanoparticle (Ag NP) deposition followed by the MACE of intrinsic amorphous hydrogenated silicon (a-Si:H) on SiOx, creating isolated mesopores through the film stack. By varying the MACE etching solution (HF:H2O2) concentration, we were able to vary the pinhole areal density over four orders of magnitude (104-107 cm-2). We observed the Ostwald ripening of the Ag NP to enable control over the pinhole radii. Our work demonstrates proof-of-concept for a-Si:H/SiOx with mesopores across the film stack, which may serve as precursor for the development of poly-Si/SiOx passivating contacts of both polarities.

MATERIALS SCIENCE,SOLAR ENERGY↗

Physical patterning of high-Q superconducting niobium resonators via ion beam etching

The development of superconducting quantum circuits increasingly involves the exploration of chemically distinct materials and complex multilayered structures. Accelerating this trend may benefit from low-damage, materials-agnostic patterning techniques that are compatible with a broad range of materials. Here, in this work, we investigate the utility of low-energy ion beam etching (IBE), a physical patterning technique, as an alternative to reactive ion etching for fabricating low-loss superconducting resonators. We use niobium (Nb) resonators as a test platform, leveraging their well-characterized performance metrics for benchmarking. To address IBE-induced surface redeposition, we introduce an in situ aluminum capping layer combined with targeted post-fabrication chemical treatment. This strategy yields resonators with internal quality factors as high as 6 × 10 5 in the single-photon regime at 50 mK. These results establish low-energy IBE as a promising patterning technique for superconducting devices, with the potential to accelerate development across chemically diverse and multilayered material platforms.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Thermoplasmonic laser-induced backside wet etching of sapphire

The technology of thermoplasmonic laser-induced backside wet etching is proposed to microstructure such solid and difficult-to-process materials as sapphire. In this technology, the laser absorbing medium is silver nanoparticles obtained from a precursor (AgNO{sub 3}) and providing significant laser radiation absorption due to the presence of plasmonic absorption with the formation of a substantially localised region with extremely high temperatures and pressures. This approach makes it possible to process sapphire both in the ‘gentle’ regime with the formation of nanometre structures and in the ‘strong’ regime to allow for the formation of ‘deep’ structures with etching rates up to several micrometers per pulse and high aspect ratio. The possibility of formation of periodic structures in sapphire in the above-threshold regime is shown. (in memory of professor v.n. bagratashvili (1947 – 2018))

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Wet-Etching of Acoustically Spalled GaAs for Substrate Reuse

Acoustic spalling is a promising technique for substrate reuse in the fabrication of gallium arsenide (GaAs) photovoltaic cells. However, the acoustic spalling process can leave the substrate with areas of rough surface morphology that can interfere with subsequent cell growth and processing. In this work, we investigate the use of wet etchants to smooth the surface of acoustically spalled GaAs substrates. We evaluated six different etchants. Of those tested, an 8:1:1 mixture of sulfuric acid, hydrogen peroxide, and water at 30 degrees C and a moderate stirring rate showed the greatest roughness reduction per mass loss while producing the desired morphology. This etchant was then applied to an acoustically spalled 2-inch GaAs wafer. A single-junction GaAs cell was then grown via metalorganic vapor-phase epitaxy on this substrate, an acoustic spalled substrate without a smoothing etch, and an epi-ready substrate. Use of the 8:1:1 H2SO4:H2O2:H2O etchant produced cells an average efficiency of 12.8% as compared to that of 2.0% grown on the unetched acoustically spalled substrate and 16.3% grown on the epi-ready substrate. The results of this work demonstrate that wet etching is a viable method for smoothing the surface of spalled GaAs substrates, paving the way for substrate reuse via acoustic spalling at efficiencies that approach growth on epi-ready substrates.

etching↗

Effect of Misorientation and Preliminary Etching of the Substrate on the Structural and Optical Properties of Integrated GaAs/Si(100) Heterostructures Produced by Vapor Phase Epitaxy

It is shown for the first time that the structural and optical functional characteristics of integrated GaAs/Si(100) heterostructures can be controlled by using misoriented Si(100) substrates and their preliminary etching. The growth of an epitaxial GaAs layer on a Si substrate without the formation of antiphase domains can be carried out on a substrate deviated from the (100) singular plane by an angle smaller than 4°–6° or without a transition layer of GaAs nanocolumns. Preliminary treatment of the silicon substrate by etching makes it possible to use it for the vapor-phase epitaxial growth of a single-crystal GaAs film with a considerably smaller relaxation coefficient, which has a positive effect on the structural quality of the film. These data are in good agreement with the results of IR reflectance spectroscopy and photoluminescence and ultraviolet spectroscopy. The features of the optical properties of integrated GaAs/Si(100) heterostructures in the infrared and ultraviolet spectral regions are also defined by the relaxation coefficient.

36 MATERIALS SCIENCE↗

Characterization of CdZnTeSe Nuclear Detector Chemically Etched in Bromine Methanol

Semiconductor nuclear radiation detectors made from tertiary and quaternary compounds of cadmium telluride (CdTe) can operate at room temperature without cryogenic cooling. One of such materials that have become of great interest is cadmium zinc telluride selenide (CdZnTeSe). Compared to other CdTe-based materials, such as cadmium zinc telluride (CdZnTe), CdZnTeSe can be grown with much less Te inclusions and sub-grain boundary networks. Chemical etching is often used to smoothen wafer surfaces during detector fabrication. This paper presents the characterization of CdZnTeSe that is chemically etched using bromine methanol solution. Infrared imaging shows that the wafer has no sub-grain boundary networks that often limit detector performance. The current-voltage (I-V) characterization experiment gave a resistivity of 4.6 × 10 10 Ω-cm for the sample. The I-V curve was linear in the ±10 to ±50 volts range. An energy resolution of 7.2% was recorded at 100 V for the 59.6-keV gamma line of 241 Am.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Advanced Inductively Coupled Plasma Etching Processes for Fabrication of Resonator-Quantum Well Infrared Photodetector

Resonator-quantum well infrared photodetectors (R-QWIPs) are the next generation of QWIP detectors that use resonances to increase the quantum efficiency (QE). To achieve the expected performance, the detector geometry must be produced in precise specification. In particular, the height of the diffractive elements (DE) and the thickness of the active resonator must be uniformly and accurately realized to within 0.05 lm accuracy and the substrates of the detectors have to be removed totally. To achieve these specifications, two optimized inductively coupled plasma (ICP) etching processes are developed. Using these etching techniques, we have fabricated a number of R-QWIP test detectors and FPAs with the required dimensions and completely removed the substrates of the test detectors and FPAs. Their QE spectra were tested to be in close agreement with the theoretical predictions. The operability and spectral non-uniformity of the FPA is about 99.57% and 3% respectively.

plasma etching process↗

An Improved Design and Versatile New Lamination Fabrication Method for Twin Electrode Thin Layer Cells Utilizing Track‐etch Membranes

Abstract Reported here are laminated membrane electrodes, an improved design and more advantageous method of fabrication for previously reported thin layer cell electrode systems developed on track‐etch membranes. The laminated membrane approach potentially further improves flow resistance by dramatically reducing the surface area to volume ratio, but also produces a cohesive device that can be more readily applied to a broad range of applications. In addition, this new fabrication method was implemented in a scalable, commercial process and resulting product demonstrations indicate that volume manufacturing is feasible. Characterization of laminated membrane electrodes reveal redox cycling amplification factors as high as 30 with linear responses to variable concentrations of redox couple. These performance characteristics are shown to be comparable to similar generator‐collector systems fabricated through much more laborious laboratory methods. This combination of added versatility, cost‐reduced fabrication and exceptional performance clearly reveals unrealized potential of track‐etch membrane approaches and boosts their candidacy as powerful new options for generator‐collector electrode systems.

Hauke, Adam↗