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NASA NTRS2003

Artifacts for Calibration of Submicron Width Measurements

Artifacts that are fabricated with the help of molecular-beam epitaxy (MBE) are undergoing development for use as dimensional calibration standards with submicron widths. Such standards are needed for calibrating instruments (principally, scanning electron microscopes and scanning probe microscopes) for measuring the widths of features in advanced integrated circuits. Dimensional calibration standards fabricated by an older process that involves lithography and etching of trenches in (110) surfaces of single-crystal silicon are generally reproducible to within dimensional tolerances of about 15 nm. It is anticipated that when the artifacts of the present type are fully developed, their critical dimensions will be reproducible to within 1 nm. These artifacts are expected to find increasing use in the semiconductor-device and integrated- circuit industries as the width tolerances on semiconductor devices shrink to a few nanometers during the next few years. Unlike in the older process, one does not rely on lithography and etching to define the critical dimensions. Instead, one relies on the inherent smoothness and flatness of MBE layers deposited under controlled conditions and defines the critical dimensions as the thicknesses of such layers. An artifact of the present type is fabricated in two stages (see figure): In the first stage, a multilayer epitaxial wafer is grown on a very flat substrate. In the second stage, the wafer is cleaved to expose the layers, then the exposed layers are differentially etched (taking advantage of large differences between the etch rates of the different epitaxial layer materials). The resulting structure includes narrow and well-defined trenches and a shelf with thicknesses determined by the thicknesses of the epitaxial layers from which they were etched. Eventually, it should be possible to add a third fabrication stage in which durable, electronically inert artifacts could be replicated in diamondlike carbon from a master made by MBE and etching as described above.

Grunthaner, Frank↗

NASA NTRS2003

Wafer-Level Membrane-Transfer Process for Fabricating MEMS

A process for transferring an entire wafer-level micromachined silicon structure for mating with and bonding to another such structure has been devised. This process is intended especially for use in wafer-level integration of microelectromechanical systems (MEMS) that have been fabricated on dissimilar substrates. Unlike in some older membrane-transfer processes, there is no use of wax or epoxy during transfer. In this process, the substrate of a wafer-level structure to be transferred serves as a carrier, and is etched away once the transfer has been completed. Another important feature of this process is that two electrodes constitutes an electrostatic actuator array. An SOI wafer and a silicon wafer (see Figure 1) are used as the carrier and electrode wafers, respectively. After oxidation, both wafers are patterned and etched to define a corrugation profile and electrode array, respectively. The polysilicon layer is deposited on the SOI wafer. The carrier wafer is bonded to the electrode wafer by using evaporated indium bumps. The piston pressure of 4 kPa is applied at 156 C in a vacuum chamber to provide hermetic sealing. The substrate of the SOI wafer is etched in a 25 weight percent TMAH bath at 80 C. The exposed buried oxide is then removed by using 49 percent HF droplets after an oxygen plasma ashing. The SOI top silicon layer is etched away by using an SF6 plasma to define the corrugation profile, followed by the HF droplet etching of the remaining oxide. The SF6 plasma with a shadow mask selectively etches the polysilicon membrane, if the transferred membrane structure needs to be patterned. Electrostatic actuators with various electrode gaps have been fabricated by this transfer technique. The gap between the transferred membrane and electrode substrate is very uniform ( 0.1 m across a wafer diameter of 100 mm, provided by optimizing the bonding control). Figure 2 depicts the finished product.

Yang, Eui-Hyeok↗

DOE OSTI2020

Hybrid semiconductor-piezoacoustic radiofrequency device

An amplifying radiofrequency device includes a piezoelectric film and a semiconductor amplifier layer. The piezoelectric film is conformed as an acoustic waveguide. The piezoelectric film has a principal acoustic propagation direction parallel to the principal conduction direction of the amplifier layer. Interdigitated transducers are positioned on the piezoelectric film to respectively launch an acoustic wave in response to an input RF signal, and transduce the acoustic wave back to an output RF signal. There is a distance of less than the acoustic wavelength between the semiconductor amplifier layer and the piezoelectric film. The piezoelectric film has a thickness of less than the acoustic wavelength. According to a method for making such a device, a stack of III-V layers is epitaxially grown on a III-V substrate, wherein the stack comprises a first etch stop layer, a second etch stop layer, an amplifier layer, and a contact layer. The stack is bonded to a lithium niobate film. The III-V substrate is removed by etching down to the first etch stop layer. Deposition windows are opened by etching from the first etch stop layer down to the contact layer. Metal contact electrodes are deposited in the deposition windows.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Peak‐in‐Valley Metal Nano‐Architectures via E‐Beam‐Guided Metal Oxide Redox

Focused electron beams enable nanoscale material modification via localized etching or deposition. In liquid-phase electron-beam-mediated processing, radiolysis-driven redox reactions present an opportunity to control both etching and deposition simultaneously. Here, this duality using a water-ammonia solvent as a tunable redox mediator on copper surfaces is demonstrated. At lower ammonia concentrations, the oxidation process dominates, etching copper to sub-50-nm depths. The copper ions and ion-complexes released during this initial oxidation step are reduced by solvated electrons resulting in metal deposition into the etched sites, over longer e-beam exposures, producing characteristic peak-in-valley nanostructures. Conversely, at higher ammonia concentrations copper-ammine ion complexation and radiolytic oxidizing species scavenging by ammonia occur at higher rates, creating a reducing environment conducive to rapid beam-guided copper deposition. Reaction-transport simulations and experiments are performed to show the effects of ammonia-mediated radiolysis chemistry, describing the direct influence of solvent concentration on redox balance and the outcome of e-beam guided processing. By uniting both etching and deposition within a single framework, this work provides a versatile route for controlled surface nanostructuring.

copper nanostructures↗

DOE OSTI2018

Unraveling Kinetically-Driven Mechanisms of Gold Nanocrystal Shape Transformations Using Graphene Liquid Cell Electron Microscopy

Mechanisms of kinetically driven nanocrystal shape transformations were elucidated by monitoring single particle etching of gold nanocrystals using in situ graphene liquid cell transmission electron microscopy (TEM). By systematically changing the chemical potential of the oxidative etching and then quantifying the facets of the nanocrystals, nonequilibrium processes of atom removal could be deduced. Etching at sufficiently high oxidation potentials, both cube and rhombic dodecahedra (RDD)-shaped gold nanocrystals transform into kinetically stable tetrahexahedra (THH)-shaped particles. Whereas {100}-faceted cubes adopt an { hko }-faceted THH intermediate where h/k depends on chemical potential, {110}-faceted RDD adopt a {210}-faceted THH intermediate regardless of driving force. For cube reactions, Monte Carlo simulations show that removing 6-coordinate edge atoms immediately reveals 7-coordinate interior atoms. The rate at which these 6- and 7-coordinate atoms are etched is sensitive to the chemical potential, resulting in different THH facet structures with varying driving force. Conversely, when RDD are etched to THH, removal of 6-coordinate edge atoms reveals 6-coordinate interior atoms. Thus, changing the driving force for oxidation does not change the probability of edge atom versus interior atom removal, leading to a negligible effect on the kinetically stabilized intermediate shape. These fundamental insights, facilitated by single-particle liquid-phase TEM imaging, provide important atomic-scale mechanistic details regarding the role of kinetics and chemical driving force in dictating shape transformations at the nanometer length scale.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2016

Uncladded sensing fiber for refractive index measurement

The formation of chemically etched optical fiber for use in refractive index sensor is addressed. This presented design of a refractive index (RI) sensor is based on recording the power loss exhibited by radiation propagating through an etched multimode fiber (MMF) immersed in the liquid under study. The decreasing diameters of fibers are found to be strongly dependent on the temperature and etchant composition. This experiment was performed for different unclad etched fibers for same sensing length and the RI changes from 1.33 RIU to 1.38 RIU. When the multimode fiber (MMF) is etched for 12 hours the sensitivity of the sensor is approximately 204.25dBm/RIU, which is larger than without etched fiber having sensitivity 127.2dBm/RIU.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2016

Design criteria for XeF{sub 2} enabled deterministic transformation of bulk silicon (100) into flexible silicon layer

Isotropic etching of bulk silicon (100) using Xenon Difluoride (XeF{sub 2}) gas presents a unique opportunity to undercut and release ultra-thin flexible silicon layers with pre-fabricated state-of-the-art Complementary Metal Oxide Semiconductor (CMOS) electronics. In this work, we present design criteria and mechanism with a comprehensive mathematical model for this method. We consider various trench geometries and parametrize important metrics such as etch time, number of cycles and area efficiency in terms of the trench diameter and spacing so that optimization can be done for specific applications. From our theoretical analysis, we conclude that a honeycomb-inspired hexagonal distribution of trenches can produce the most efficient release of ultra-thin flexible silicon layers in terms of the number of etch cycles, while a rectangular distribution of circular trenches provides the most area efficient design. The theoretical results are verified by fabricating and releasing (varying sizes) flexible silicon layers. We observe uniform translation of design criteria into practice for etch distances and number of etch cycles, using reaction efficiency as a fitting parameter.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

Distribution of Tritium in the Near Surface of Type 316 Stainless Steel

The distribution of tritium in the near surface of stainless steel, type 316, has been measured using a combination of a ZnCl 2 wash and acid etching with diluted aqua regia. This method improves upon etching measurements reported in the literature: results show depth resolutions of ~10 nm using the diluted aqua regia. The ZnCl 2 wash results show very high surface concentrations (~1.5 x10 13 Bq/cm 3 ), which decreases by a factor of 10 6 after etching to a depth of ~10 um. Further, the tritium concentrations in the near surface (<10 um) of unmodified stainless-steel samples do not change significantly over the course of 233 days, which indicates a quasi-equilibrium state has been reached. Tritium migration to the surface from the subsurface region was measured by etching a sample, then storing it in air for 2 to 4 days. After storing in air, the surface concentrations increased a thousandfold and rapidly decreased to base levels after etching an additional ~2 um. Finally, these measurements indicate that perturbing the quasi-equilibrium concentration profile results in tritium migration to the surface in order to reestablish the prior equilibrium state.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Processing of GaN/Si(111) Epitaxial Structures for MEMS Applications

Two different approaches for the etching of the gallium nitride epitaxial layers grown on Si(111) substrates by plasma-assisted molecular beam epitaxy have been elaborated. It is demonstrated that anisotropic etch profiles can be achieved by both photoenhanced wet chemical etching and reactive plasma-chemical etching methods. Moreover, it is shown, that the photoenhanced wet chemical etching allows to remove GaN layer without damaging silicon substrate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Interaction between dissolution and precipitation during olivine carbonation: Implications for CO 2 mineralization

Large-scale carbonation of olivine is considered a promising approach for in situ mineral carbonation, offering a permanent and stable method for CO 2 storage. A critical aspect of this process is understanding how dissolution and precipitation interact, as this could drive fracturing and enhance further reactions. In this study, we conducted carbonation experiments on olivine using CO 2 -saturated aqueous solutions of NaHCO 3 and NaCl. Two experimental setups were used: one representing an open geochemical system and the other a closed system, corresponding to reaction-limited and flow-limited scenarios, respectively. Further, post-reaction textural analysis using scanning electron microscopy (SEM) revealed surface coatings of reaction products in the closed system, while etch pits and etch channels were prevalent in the open system. Although no direct evidence of reaction-driven fracturing was observed, etch pits and etch channels may serve as initiation points for subcritical crack formation and growth, potentially maintaining permeability and exposing new unreacted surfaces. Using linear elastic fracture mechanics (LEFM) model, we estimate that microcracks could propagate under a pressure of 0.1 GPa if reaction products accumulate within the etch pits. Our findings offer new insights into the mechanisms governing olivine carbonation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Enhanced stability of silicon for photoelectrochemical water oxidation through self-healing enabled by an alkaline protective electrolyte

Alkaline electrolytes impede the corrosion of Si photoanodes under positive potentials and/or illumination, due to the formation of a SiO x layer that etches 2–3 orders of magnitude more slowly than Si. Hence during water oxidation under illumination, pinholes in protection layers on Si photoanodes result in the local formation of a protective, stabilizing passive oxide on the Si surface. However, operation under natural diurnal insolation cycles additionally requires protection strategies that minimize the dark corrosive etching rate of Si at pinholes. We show herein that addition of [Fe(CN) 6 ] 3- to 1.0 M KOH(aq) results in a self-healing process that extends the lifetime to >280 h of an np + -Si(100) photoanode patterned with an array of Ni catalyst islands operated under simulated day/night cycles. The self-healing [Fe(CN) 6 ] 3- additive caused the exposed Si(100) surface to etch >180 times slower than the Si etch rate in 1.0 M KOH(aq) alone. No appreciable difference in etch rate or facet preference was observed between Si(100) and Si(111) surfaces in 1.0 M KOH(aq) with [Fe(CN) 6 ] 3- , indicating that the surface conformally oxidized before Si dissolved. The presence of [Fe(CN) 6 ] 3- minimally impacted the faradaic efficiency or overpotential of p + -Si/Ni electrodes for the oxygen-evolution reaction.

25 ENERGY STORAGE↗

DOE OSTI2021

Carbon nanospike coated nanoelectrodes for measurements of neurotransmitters

Here, carbon nanoelectrodes enable the detection of neurotransmitters at the level of single cells, vesicles, synapses and small brain structures. Previously, the etching of carbon fibers and 3D printing based on direct laser writing have been used to fabricate carbon nanoelectrodes, but these methods lack the ability of mass manufacturing. In this paper, we mass fabricate carbon nanoelectrodes by growing carbon nanospikes (CNSs) on metal wires. CNSs have a short, dense and defect-rich surface that produces remarkable electrochemical properties, and they can be mass fabricated on almost any substrate without using catalysts. Tungsten wires and niobium wires were electrochemically etched in batch to form sub micrometer sized tips, and a layer of CNSs was grown on the metal wires using plasma-enhanced chemical vapor deposition (PE-CVD). The thickness of the CNS layer was controlled by the deposition time, and a thin layer of CNSs can effectively cover the entire metal surface while maintaining the tip size within the sub micrometer scale. The etched tungsten wires produced tapered conical nanotips, while the etched niobium wires were long and thin. Both showed excellent sensitivity for the detection of outer sphere ruthenium hexamine and the inner sphere test compound ferricyanide. The CNS nanosensors were used for the measurement of dopamine, serotonin, ascorbic acid and DOPAC with fast-scan cyclic voltammetry. The CNS nanoelectrodes had a large surface area and numerous defect sites, which improved the sensitivity, electron transfer kinetics and adsorption. Finally, the CNS nanoelectrodes were compared with other nanoelectrode fabrication methods, including flame etching, 3D printing, and nanopipettes, which are slower to make and more difficult for mass fabrication. Thus, CNS nanoelectrodes are a promising strategy for the mass fabrication of nanoelectrode sensors for neurotransmitters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Nanoscale morphological evolution of monocrystalline Pt surfaces during cathodic corrosion

This paper studies the cathodic corrosion of a spherical single crystal of platinum in an aqueous alkaline electrolyte, to map out the detailed facet dependence of the corrosion structures forming during this still largely unexplored electrochemical phenomenon. We find that anisotropic corrosion of the platinum electrode takes place in different stages. Initially, corrosion etch pits are formed, which reflect the local symmetry of the surface: square pits on (100) facets, triangular pits on (111) facets, and rectangular pits on (110) facets. We hypothesize that these etch pits are formed through a ternary metal hydride corrosion intermediate. In contrast to anodic corrosion, the (111) facet corrodes the fastest, and the (110) facet corrodes the slowest. For cathodic corrosion on the (100) facet and on higher-index surfaces close to the (100) plane, the etch pit destabilizes in a second growth stage, by etching faster in the (111) direction, leading to arms in the etch pit, yielding a concave octagon-shaped pit. In a third growth stage, these arms develop side arms, leading to a structure that strongly resembles a self-similar diffusion-limited growth pattern, with strongly preferred growth directions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Large area nanoscale patterning of functional materials using organosilicate ink based nanotransfer printing

Abstract This paper presents a versatile nanotransfer printing method for achieving large-area sub-micron patterns of functional materials. Organosilicate ink formulations combined with effective release layers have been shown to facilitate patterning of materials through the commonly used patterning approaches—lift off, physical etching and chemical etching. In this paper, we demonstrate that organosilicate ink formulations function as an effective resist owing to its superior physico-chemical stability whereas the release layers ensure clean removal of the resist post patterning. We successfully demonstrate patterning of sub-micron structures (800 nm feature sizes) of chromium metal through the lift off approach, silicon through reactive ion etching technique and silicon dioxide through wet chemical etching technique illustrating the versatility of the reported method. This patterning methodology represents a significant advancement in enabling nanostructure fabrication within resource-constrained laboratories. The approach requires nothing more than a master mold containing the desired structures, a spin coater, a low-temperature hotplate, and a desktop reactive ion etch tool.

Engineering↗

NASA NTRS1973

On particle track detectors

Aqueous sodium hydroxide is widely used to develop charged particle tracks in polycarbonate film, particularly Lexan. The chemical nature of the etching process for this system has been determined. A method employing ultra-violet absorbance was developed for monitoring the concentration of the etch products in solution. Using this method it was possible to study the formation of the etching solution saturated in etch products. It was found that the system super-saturates to a significant extent before precipitation occurs. It was also learned that the system approaches its equilibrium state rather slowly. It is felt that both these phenomena may be due to the presence of surfactant in the solution. In light of these findings, suggestions are given regarding the preparation and maintenance of the saturated etch solution. Two additional research projects, involving automated techniques for particle track analysis and particle identification using AgCl crystals, are briefly summarized.

Benton, E. V.↗

NASA NTRS1978

Studies and testing of antireflective (AR) coatings for soda-lime glass

Processes for producing antireflection films on glass are concentrated in three areas: acid etching of glass, plasma etching of glass, and acid development of sodium silicate films on glass. The best transmission was achieved through the acid etching technique, while the most durable films were produced from development of sodium silicate films. Control of the acid etching technique is presently inadequate for production implementation. While films having excellent antireflective properties were fabricated by plasma etching techniques, all were water soluble.

Pastirik, E. M.↗

NASA NTRS1978

Ion beam sputtering of fluoropolymers

Ion beam sputter processing rates as well as pertinent characteristics of etched targets and films are described. An argon ion beam source was used to sputter etch and deposit the fluoropolymers PTFE, FEP, and CTFE. Ion beam energy, current density, and target temperature were varied to examine effects on etch and deposition rates. The ion etched fluoropolymers yield cone or spire-like surface structures which vary depending upon the type of polymer, ion beam power density, etch time, and target temperature. Sputter target and film characteristics documented by spectral transmittance measurements, X-ray diffraction, ESCA, and SEM photomicrographs are included.

Sovey, J. S.↗

NASA NTRS1979

Process Development for Automated Solar Cell and Module Production. Task 4: Automated Array Assembly

A baseline sequence for the manufacture of solar cell modules was specified. Starting with silicon wafers, the process goes through damage etching, texture etching, junction formation, plasma edge etch, aluminum back surface field formation, and screen printed metallization to produce finished solar cells. The cells were then series connected on a ribbon and bonded into a finished glass tedlar module. A number of steps required additional developmental effort to verify technical and economic feasibility. These steps include texture etching, plasma edge etch, aluminum back surface field formation, array layup and interconnect, and module edge sealing and framing.

Source record↗