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At least 703 records · Page 39

A novel hardmask-to-substrate pattern transfer method for creating 3D, multi-level, hierarchical, high aspect-ratio structures for applications in microfluidics and cooling technologies

Abstract This letter solves a major hurdle that mars photolithography-based fabrication of micro-mesoscale structures in silicon. Conventional photolithography is usually performed on smooth, flat wafer surfaces to lay a 2D design and subsequently etch it to create single-level features. It is, however, unable to process non-flat surfaces or already etched wafers and create more than one level in the structure. In this study, we have described a novel cleanroom-based process flow that allows for easy creation of such multi-level, hierarchical 3D structures in a substrate. This is achieved by introducing an ultra-thin sacrificial silicon dioxide hardmask layer on the substrate which is first 3D patterned via multiple rounds of lithography. This 3D pattern is then scaled vertically by a factor of 200–300 and transferred to the substrate underneath via a single shot deep etching step. The proposed method is also easily characterizable—using features of different topographies and dimensions, the etch rates and selectivities were quantified; this characterization information was later used while fabricating specific target structures. Furthermore, this study comprehensively compares the novel pattern transfer technique to already existing methods of creating multi-level structures, like grayscale lithography and chip stacking. The proposed process was found to be cheaper, faster, and easier to standardize compared to other methods—this made the overall process more reliable and repeatable. We hope it will encourage more research into hybrid structures that hold the key to dramatic performance improvements in several micro-mesoscale devices.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Light-trapping structures fabricated in situ for ultrathin III-V solar cells

Here, we describe a fully in situ method of fabricating light-scattering structures on III-V materials that generates a rough morphology via vapor phase etching and redeposition. Fully in situ methods support higher industrial throughput by utilizing the growth reactor to generate the light-trapping structures after device growth without removal from the reactor. We use HCl and PH 3 to etch and redeposit scattering morphologies on Ga 0.5 In 0.5 P in a dynamic hydride vapor phase epitaxy (D-HVPE) reactor. We show that the addition of PH 3 leads to redeposition during the vapor phase HCl etching of Ga 0.5 In 0.5 P and that HCl flow rate and time exposed to HCl-PH 3 each independently cause a linear increase in the redeposited feature size, indicating that redeposition proceeds by island growth in a III-Cl-limited, hydride-enhanced HVPE regime. Auger electron spectroscopy and scanning transmission electron microscopy with energy dispersive spectroscopy (STEM-EDS) reveal redeposition to be highly Ga-rich GaInP, i.e., Ga(In)P. The Ga-rich nature of the redeposition results from the higher thermodynamic driving force for Ga incorporation than for In during HVPE growth and the difference in the volatility of the III-Cl etch products. The resulting morphologies have high broadband scattering, as determined by normal specular reflectance and integrating sphere measurements, indicating effectiveness as light-scattering structures. In a 270-nm-thick GaAs photovoltaic device with a textured back surface, we achieve a 4.9% increase in short circuit current density (J SC ) without any loss in open-circuit voltage (V OC ) relative to a planar control using only a 60 s in situ texturing treatment.

14 SOLAR ENERGY↗

Characterization of Microwave Loss Using Multimode Superconducting Resonators

Measuring the losses arising from different materials and interfaces is crucial to improving the coherence of superconducting quantum circuits. Although this has been of interest for a long time, current studies can either only provide bounds to those losses, or require several devices for a complete characterization. In this work, we introduce a method to measure the microwave losses of materials and interfaces with a single multi-mode superconducting resonator. We demonstrate a formalism for analyzing the loss sensitivity of multi-mode systems and discuss the design strategies of multi-mode resonators for material loss studies. We present two types of multi-mode superconducting resonators for the study of bulk superconductors: the forky whispering-gallery-mode resonator (FWGMR) and the ellipsoidal cavity. We use these resonators to measure the surface dielectric, conductor, and seam losses of high-purity (5N5) aluminum and aluminum alloy (6061), as well as how they are affected by chemical etching, diamond turning, and thin-film coating. Here, we find that chemical etching and diamond turning reduce both the surface dielectric and conductive losses of high-purity aluminum, but provide no appreciable improvement to the seam. Coating the surfaces of diamond-turned aluminum alloys with e-beam evaporated or sputtered aluminum thinfilms significantly reduces all three losses under study. In addition, we study the effect of chemical etching on the surface of high-purity aluminum using transmission electron microscopy (TEM) and find that the chemical etching process creates a thinner and more uniform oxide layer, consistent with the observed improvement in the surface dielectric loss.

25 ENERGY STORAGE↗

Self-Aligned Selective Area Front Contacts on Poly -Si/SiO x Passivating Contact c -Si Solar Cells

We report both polarity poly-Si/SiO x passivating contacts in a front/back device configuration may represent the next solar cell architecture after tunnel oxide passivating contacts (TOPCon) cells, but high parasitic absorption in the front poly -Si layer often limits its performance. This work explores a wet etching technique to remove the front poly -Si in the nonmetallized regions using self-aligned metal grids as an etch mask. We systematically examine various dielectric layers (SiN x ,Al 2 O 3 , and stacks thereof) to study the repassivation of the etched n + surface, and find that an SiN x /Al 2 O 3 passivation stack can effectively repassivate the etched surface, which we attribute to field-effect passivation from the positive fixed charge from the SiN x layer, and excellent chemical passivation property from Al 2 O 3 in the form of atomic H. We demonstrate a front/back poly-Si/SiO x passivating contact device, with an open-circuit voltage (V oc ) of 690 mV, short-circuit current density (J sc ) of 39.8 mA/cm 2 , fill factor of 78%, and power conversion efficiency of 21.4%. Furthermore, simulations using SunSolve and Quokka 3 show good agreement with both the optical and electrical properties of the experimental device. The power loss analysis reveals improvements in the optical loss from the back Ti adhesion and front SiN x layers would lead to a 23.5% device. Lastly, a techno-economic model compares the production cost of this improved cell with the current TOPCon cells. Our results highlight that further cost reductions in single-sided doped poly -Si layers are needed to compete with mainstream passivated emitter and rear cell, and TOPCon technologies.

14 SOLAR ENERGY↗

Dual-Wavelength Y-Branch DBR Lasers With 100 mW of CW Power Near 2 μm

In this study, the interband GaSb-based diode lasers emitting simultaneously in two narrow bands separated by either ~1.6 or ~3.3 THz were designed, fabricated and characterized. The device active region contained one asymmetric tunnel-coupled double quantum well with separation between two lowest electron subbands controlled by thickness of the tunnel barrier. The Y-branch 6th order distributed Bragg reflector devices have been fabricated with either deep or shallow etched ridge waveguides. The increase of the deeply etched ridge waveguide width from 10 to 20 μm improved laser threshold and efficiency thanks to reduction of the relative role of the sidewall defect recombination. Further improvement of the device performance parameter was achieved by shallow etching. The shallow etched lasers with stable dual-wavelength emission spectrum generated 100 mW of continuous wave output power at 20 °C

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A FeCrAl-Al2O3 Composite Produced via Laser Powder Bed Fusion of a Mixed Powder for Porous Catalyst Scaffolds

This study proposes a novel approach for synthesizing and etching bicontinuous FeCrAl-Al2O3 composites as a means for replacing FeCrAl foams as catalyst scaffolds in bio-driven alcohol reactors for jet-fuel production. Conventional FeCrAl foams suffer from poor availability and consequent high costs. New additive manufacturing techniques provide an opportunity to produce tailored foams in reasonable times and at acceptable costs. This research aimed to generate a porous FeCrAl structure by etching a bicontinuous FeCrAl-Al2O3 composite produced by laser powder bed fusion of amalgamated FeCrAl and Al2O3 powders. The composite powder for laser powder bed fusion is created by ball-milling FeCrAl and Al2O3 powders. This research focuses on achieving a bi-continuous FeCrAl-Al2O3 structure, essential for the selective removal of the ceramic phase. The influence of laser processing parameters on the microstructure was examined across a range of laser powers (60-120 W) and scan speeds (100-400 mm/s), showing that higher powers and speeds produce finer metal struts. A bi-continuous microstructure was consistently obtained, marking a key achievement. The Al2O3 removal process involved a two-step etching method using hydrochloric and phosphoric acids, tested across various etching times. The alumina phase was reduced from 36 vol% to 17 vol% (corresponding to an increase in porosity from 24 vol% to 43 vol%), showing the potential for use as a porous catalyst scaffold. This research demonstrates the potential for using additive manufacturing to produce porous FeCrAl structures capable of replacing hard-to-source FeCrAl foams.

Son, Kwangtae↗

Atomic layer deposition frequency-multiplied Fresnel zone plates for hard x-rays focusing

The design and fabrication of Fresnel zone plates for hard x-ray focusing up to 25 keV photon energies with better than 50 nm imaging half-pitch resolution is reported as performed by forming an ultrananocrystalline diamond (UNCD) scaffold, subsequently coating it with atomic layer deposition (ALD) with an absorber/phase shifting material, followed by back side etching of Si to form a diamond membrane device. The scaffold is formed by chemical vapor-deposited UNCD, electron beam lithography, and deep-reactive ion etching of diamond to desired specifications. The benefits of using diamond are as follows: improved mechanical robustness to prevent collapse of high-aspect-ratio ring structures, a known high-aspect-ratio etch method, excellent radiation hardness, extremely low x-ray absorption, and significantly improved thermal/dimensional stability as compared to alternative materials. Central to the technology is the high-resolution patterning of diamond membranes at wafer scale, which was pushed to 60 nm lines and spaces etched 2.2-mu m-deep, to an aspect ratio of 36:1. The absorber growth was achieved by ALD of Ir, Pt, or W, while wafer-level processing allowed to obtain up to 121 device chips per 4 in. wafer with yields better than 60%. X-ray tests with such zone plates allowed resolving 50 nm lines and spaces, at the limit of the available resolution test structures.

36 MATERIALS SCIENCE↗

Manufacturing-induced contamination in common multilayerdielectric gratings

Contamination of pulse compression gratings during the manufacturing process is known to give rise to reduced laser damage performance and represents an issue that has not yet been adequately resolved. The present work demonstrates that the currently used etching methods introduce carbon contamination inside the etched region extending to a 50- to 80-nm layer below the surface. This study was executed using custom samples prepared in both, a laboratory setting and by established commercial vendors, showing results that are very similar. The laser-induced-damage performance of the etched and unetched regions in the grating-like samples suggest that contaminants introduced by etching process are contributing to the reduction of the laser-induced damage threshold.

42 ENGINEERING↗

Genesis of topography in buffered chemical polishing of niobium for application to superconducting radiofrequency accelerator cavities

Topography arising from the final etch step in preparing niobium superconducting radiofrequency (SRF) accelerator cavities is understood to significantly impact cavity performance at high field levels. This study investigated the effect of process temperature and time on the etch rate and topography arising from the widely-used buffered chemical polishing (BCP). This study aims to understand more thoroughly the genesis of topography in BCP of polycrystalline niobium, with the ultimate aim of finding a path to surface smoothness comparable to that obtained by electro-polishing (EP). It was found that the etch process is controlled by the surface reaction; and that the etch rate varies with crystallographic orientation. The familiar micron-scale roughening necessarily results. Gas evolution has an impact, but is secondary. The major outcome is that surface smoothness comparable to EP appears to be inherently unachievable for polycrystalline niobium using BCP, setting an upper limit to the gradient for which it is useful.

Reece, Charles↗

Stainless Steel Coating Test Report

A process was developed to coat 316L stainless steel pieces having very low levels of fixed contamination on their surface (~100 dpm/100 cm²). The coating process served to significantly decrease the likelihood of any fixed contamination becoming loose contamination due to physical shocks. Prior to coating, the stainless steel was etched with a commercial methane sulfonic acid (MSA) solution in a heated ultrasonic bath, rinsed with deionized water, cleaned with a basic detergent solution, and then rinsed with deionized water. The MSA etched the surface of the stainless-steel pieces, creating a more favorable surface on which the coating could adhere. Due to the short timeline of the project, only commercially available clear coating products were considered. The clear coating had to be wear-resistant, shock resistant, radiation resistant, and have high adhesion to the surface of the stainless steel. Adhesion of coatings to stainless steel is notoriously difficult. A commercial, high molecular weight polymer coating was found that met these requirements. The adhesion properties of this coating to stainless steel are very good, and are significantly improved by the etching process. The etching process results in a higher surface area that is free of debris and other residues, making the surface much more wetable, and at the same time creating a favorable surface topography for adhesion. The polymer in its uncured form is a low viscosity liquid. It can be applied by brush or pipette, and it cures in air alone, but heat is required to speed up curing and attain the highest performance of the cured polymer. As the project progressed, the project team became interested in the composition of the selected commercial polymer coating, and in ways that this polymer coating could be made more wear resistant and potentially more radiation resistant. Nano-particle addition was chosen as the preferred way to achieve higher performance. Therefore, a series of tests were planned and performed. This report summarizes these tests, and presents the results.

36 MATERIALS SCIENCE↗

Final Report: Next Generation Diamond Drumhead X-Ray Optics

Problem / Opportunity Statement: Future high-impact scientific applications at synchrotron and Free-Electron Laser (FEL) X-ray sources require the development of processing and mounting methods for ultra-thin diamond crystals to meet the most challenging needs of pioneering research at next generation light source facilities. These methods should be capable of manufacturing crystal plates as thin as 10 micrometers over an area of a few mm2, and with a surface cut in different crystal orientations, such as the diamond {100}, {111}, {110} and {113} planes. Project Purpose and Approach: In Phase I, Great Lakes Crystal Technologies (GLCT) partnered with Stonybrook University (SUNY) to created thin diamond drumhead crystals. The purpose of the Phase I project is to transfer the drumhead membrane window etching technology from SUNY to GLCT. Testing of a device using the beamline at Stanford Linear Accelerator Laboratory was initially planned, however, a delay on the part of a third party service provided required us to get beamline testing done at Argonne National Laboratory. Phase I Taskwork: Testing of a high purity diamond plate thinning and etching process was performed. By SUNY and GLCT. Plates were sent to a third party service provider for thinning to ~100 microns, however, delays required that GLCT develop an in-house thinning process to complete the taskwork. GLCT successfully developed this in-house capability even though it was initially planned to be part of the Phase II Taskwork. Multiple practice and deliverable plates were provided to SUNY to be etched into the target drumhead devices. GLCT practiced and refined an in-house plate thinning process and produced five plates with thicknesses in the 60 – 150 micron range. Processing of the plates has begun and will continue in a no-cost extension period necessitated by the third party service provider delay. GLCT also procured and installed a reactive ion etching/inductively coupled plasma system. In addition, one of the thinned plates was measured at the Applied Photon Source at APL for a pre-processing assessment of the crystalline strain. After processing the plate into a drumhead and annealing, a post-processing assessment of the strain will be performed. Phase I Results: The initial data from GLCT’s plate thinning process development, SUNY’s drumhead etching processing, and characterization at APS/ANL demonstrate our teams capabilities to achieve the project goals. Commercial Applications & Benefits: The proposed technology will benefit advanced x-ray science performed at BNL and the 70+ additional advanced beamlines around the world. There are also a number of medical and homeland security applications which could benefit from the technology.

Quayle, Paul↗

Alternate Methods for Cleaning Zirconium Plate

The United States High Performance Research Reactor Conversion Program identified the need to transition from highly enriched uranium fuel to lowly enriched uranium fuel for high power research and civil reactors. One of the fuel configurations selected for these reactors was a uranium (U) foil alloyed with 10% molybdenum (Mo). The U-10Mo fuel foil was then covered with a zirconium (Zr) interlayer and pressed into an aluminum cladding. Idaho National Laboratory prescribed a need to remove surface oxidation on the Zr prior to bonding it with U-10Mo fuel foil. To determine the best method of oxidation removal, a variety of polishing methods, including hand polishing with a diamond paste or Scotch-Brite™ pads, mechanically wet-polishing with abrasive belts, and chemical etching with hydrofluoric/nitric acid mixtures, were investigated on pre-polished Zircaloy 702 sheets purchased directly from the manufacturer. No change in surface roughness was detected using any of these methods relative to the as-received material. In fact, scanning electron microscopy detected grit from hand polishing with Amplex Grade 30 waste soluble diamond paste and Scotch-Brite™ pads. Visible staining was found, and fluorine detected via X-ray photoelectron spectroscopy on the flash etching samples. These contaminants were not seen on the as-received material. In addition to the need to remove the oxide layer on the Zr prior to co-rolling, there are concerns that the Neolube debonding agent on the co-rolling can may contaminate the Zr surface after co-rolling. The experimental results found that zirconium in contact with Neolube coated steel plates was easily cleaning with ethanol wiping after heat treated and no carbide inclusions remained on the surface. Overall, all cleaning methods tested did not significantly change the surface roughness of the plates or reduce the oxide layer present on the zirconium. Carbon was found on all the samples, before and after cleaning, except for the flash etch samples which detected fluorine instead. The insignificant changes seen in the cleaned plates relative to the as received plates question the need for cleaning prior to rolling. Further investigation in the requirements for cleaning at this step is recommended. Current methods for cleaning the surface after hot rolling with alcohol appear sufficient. After hot rolling, if Neolube does peel off the can and onto the zirconium coated foil surface, a dry abrasive or diamond paste polish is not recommended due to the chance of abrasive being embedded into the surface. However, the ability of an etchant to lift the lubricant off the zirconium surface indicates that a spot etch method could work to clean specific spots where Neolube is present, if the need arises.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microfluidic Fabrication Techniques for High-Pressure Testing of Microscale Supercritical CO 2 Foam Transport in Fractured Unconventional Reservoirs

Pressure limitations of many microfluidic platforms have been a significant challenge in microfluidic experimental studies of fractured media. As a result, these platforms have not been fully exploited for direct observation of high-pressure transport in fractures. This work introduces microfluidic platforms that enable direct observation of multiphase flow in devices featuring surrogate permeable media and fractured systems. Such platforms provide a pathway to address important and timely questions such as those related to CO 2 capture, utilization and storage. This work provides a detailed description of the fabrication techniques and an experimental setup that may serve to analyze the behavior of supercritical CO 2 (scCO 2 ) foam, its structure and stability. Such studies provide important insights regarding enhanced oil recovery processes and the role of hydraulic fractures in resource recovery from unconventional reservoirs. This work presents a comparative study of microfluidic devices developed using two different techniques: photolithography/wet-etching/ thermal-bonding versus Selective Laser-induced Etching. Both techniques result in devices that are chemically and physically resistant and tolerant of high pressure and temperature conditions that correspond to subsurface systems of interest. Both techniques provide pathways to high-precision etched microchannels and capable lab-on-chip devices. Photolithography/wet-etching, however, enables fabrication of complex channel networks with complex geometries, which would be a challenging task for laser etching techniques. This work summarizes a step-by-step photolithography, wet-etching and glass thermal-bonding protocol and, presents representative observations of foam transport with relevance to oil recovery from unconventional tight and shale formations. In conclusion, this work describes the use of a high resolution monochromatic sensor to observe scCO 2 foam behavior where the entirety of the permeable medium is observed simultaneously while preserving the resolution needed to resolve features as small as 10 μm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

CHARGE SPECTRUM OF HEAVY AND SUPERHEAVY COMPONENTS OF GALACTIC COSMIC RAYS: RESULTS OF THE OLIMPIYA EXPERIMENT

The aim of the OLIMPIYA experiment is to search for and identify traces of heavy and superheavy nuclei of galactic cosmic rays (GCR) in olivine crystals from stony–iron meteorites serving as nuclear track detectors. The method is based on layer-by-layer grinding and etching of particle tracks in these crystals. Unlike the techniques of other authors, this annealing-free method uses two parameters: the etching rate along the track ( V {sub etch}) and the total track length ( L ), to identify charge Z of a projectile. A series of irradiations with different swift heavy ions at the accelerator facilities of GSI (Darmstadt) and IMP (Lanzhou) were performed in order to determine and calibrate the dependence of projectile charge on V {sub etch} and L . To date, one of the most essential results of the experiment is the obtained charge spectrum of GCR nuclei within the range of Z > 40, based on about 11.6 thousand processed tracks. As the result of data processing, 384 nuclei with charges Z ≥ 75 have been identified, including 10 nuclei identified as actinides (90 < Z < 103). Three tracks were identified to be produced by nuclei with charges 113 < Z < 129. Such nuclei may be part of the Island of Stability of transfermium elements.

79 ASTRONOMY AND ASTROPHYSICS↗

Characterization of lunar nitrogen components

Rocks of known and disparate cosmic-ray ages are analyzed to find the spallation production rate of N-15. A soil breccia of known formation age was analyzed for its bearing on the antiquity of the isotopically light component. Further stepwise heating analysis of soils shed further light on occurrences of the components. Lunar soil samples were etched slightly by fluorine, revealing significant differences in isotopic ratios between carbon on grain surfaces and bulk carbon; the surface carbon is not retained during agglutinate formation. Etching revealed that about 25% of the total nitrogen resides on the surface of grains; the nitrogen is isotopically heavy. Etching also revealed about 50% of helium in soils residing below the readily etched outermost 1% of soil grain surfaces.

Becker, R. H.↗

Effect of multiblade slurry saw induced damage on silicon solar cells

A correlation between the optimum etch loss and the depth of damage is established using wafers produced by the Multiblade Slurry (MBS) and the Internal Diameter (ID) saws. The observations are based on the measurement of the performance of solar cells fabricated on these wafers. Sample preparation and test results are described and the following conclusions are made: (1) the amount of silicon removal necessary for optimum solar cell performance coincides with the depth of saw-induced damage; (2) optimization of cell performance is not affected by the method of silicon removal; (3) sawing conditions should be optimized to minimize the extent of saw-induced damage; (4) the MBS saw is found to induce damage to a lesser extent; (5) since the extent of damage in MBS-sawn wafers is in the limit of etch loss required in texture etching, it is possible to achieve optimum improvement in cell performance by merely texture etching the surface of as-sawn wafers.

Daud, T.↗

Method for applying photographic resists to otherwise incompatible substrates

A method for applying photographic resists to otherwise incompatible substrates, such as a baking enamel paint surface, is described wherein the uncured enamel paint surface is coated with a non-curing lacquer which is, in turn, coated with a partially cured lacquer. The non-curing lacquer adheres to the enamel and a photo resist material satisfactorily adheres to the partially cured lacquer. Once normal photo etching techniques are employed the lacquer coats can be easily removed from the enamel leaving the photo etched image. In the case of edge lighted instrument panels, a coat of uncured enamel is placed over the cured enamel followed by the lacquer coats and the photo resists which is exposed and developed. Once the etched uncured enamel is cured, the lacquer coats are removed leaving an etched panel.

Fuhr, W.↗