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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Comparative S/TEM study of superconducting Ta quantum resonators by wet and dry etching types

Superconducting resonators play a pivotal role in various quantum technology applications, such as quantum computing and high-frequency communication systems. The performance of these resonators is closely tied to the properties of the superconducting films used in their fabrication. Here, in this study, we investigated the impact of wet and dry etching on tantalum (Ta) films leveraging advanced scanning transmission electron microscopy-based characterization methods and examined the morphological, chemical, and strain changes caused by the etching processes. Consequently, we report the significant differences between the two etching methods, with dry etching resulting in straight slanted sidewalls and a thinner oxidized layer, while wet etching produced curved sidewalls and undercuts. Both methods led to the formation of a residual Ta wedge at the lower part of the sidewall, causing lattice deformation, which could adversely influence the homogeneous operations of superconducting devices. These insights enhance our understanding of how etching influences superconducting films, offering valuable guidance for optimizing resonators and related devices. Our findings mark a significant stride in advancing quantum technologies and high-frequency communication by enhancing our practical understanding of superconducting material fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Temperature and oxygen concentration effects on anisotropy in chromium hard mask etching for nanoscale fabrication

Chromium and its oxides are valuable as functional materials and plasma-etching hard masks in micro- and nanofabrication. While the continuous decrease in feature sizes opens new opportunities for applications of patterned chromium, the demands placed on the patterning process require a new level of mechanistic understanding. In this work, we investigate plasma etching with chlorine/oxygen chemistry using temperature and oxygen concentration as a means to controllably pattern chromium at the nanometer level. Building on our previous studies on blanket film chromium etching, we look here at patterned trenches 15–100 nm wide in 20 and 10 nm thick chromium films. We vary oxygen concentrations from 1.5% to 81% at substrate temperatures of +20 and −50 °C, respectively. Feature and trench profiles are evaluated from high-resolution cross-sectional SEM images. The ternary chromium etch product shows very different profiles as oxygen, temperature, and feature size are varied. We find the highest anisotropy at −50 °C and 50% oxygen concentration. Etch results suggest that the redeposition of nonvolatile intermediate reaction compounds enhances anisotropy at low temperature, whereas re-emission of reactive species causes undercut at the higher etching temperature.

Staaks, Daniel (ORCID:0000000204825507)↗
DOE OSTI2020

Effects of O 2 addition on in-plasma photo-assisted etching of Si with chlorine

Addition of oxygen was used to control the in-plasma photo-assisted etching (PAE) of p-type Si(100) and poly-Si in a high density, inductively coupled, Faraday-shielded, Ar/Cl 2 (225/25 SCCM), 60 mTorr plasma. After etching, samples were transferred under vacuum to an UHV x-ray photoelectron spectroscopy chamber for surface analysis. Samples etched under PAE conditions (ion energies below the ionassisted etching, IAE, threshold) had a thicker surface oxide and lower [Cl] surface concentration, when compared to samples etched under IAE conditions (ion energies above the IAE threshold). PAE was found not to be affected by 0.1 or 0.25 SCCM O 2 addition, while etching stopped with more than 0.5 SCCM O 2 addition. IAE with RF power on the sample stage, resulting in -65 V self-bias, was not affected by up to 2 SCCM of oxygen addition but decreased rapidly when more than 5 SCCM O 2 was added to the plasma. These results imply that PAE may be completely suppressed, while IAE occurs unobstructed. The implications of these findings are discussed in view of applications involving continuous wave and pulsed-plasma processes.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Development of a deep potential model for F and CF 2 etching of Si and SiO 2

An understanding of plasma-surface interactions at increasingly smaller scales is invaluable for the development of novel technologies and processing techniques. Molecular dynamics (MD) simulations can provide insights into atomic-scale interactions, though they are restricted by the availability of interatomic potentials. Machine learning methods, such as Deep Potential Molecular Dynamics (DeepMD), provide a systematic framework for the development of accurate and flexible ab initio-based models. In this work, we develop DeepMD models for the ion-enhanced etching of Si and SiO 2 by F and CF 2 radicals. We employ an active learning process to expand the data set on which the model is trained and demonstrate its effect on the model accuracy. The DeepMD results are compared to data from classical MD simulations and experiments. Physical sputtering yields of SiO 2 by Ar + ions show good agreement with previous simulation results using conventional interatomic potentials, though the predicted depth profiles are different. Etching yields are calculated as a function of ion energy and neutral to ion flux ratio for the Ar + ion-enhanced etching of SiO 2 and Si by F atoms, as well as for etching of SiO 2 by CF 2 radicals, showing reasonable agreement with experimental data. Finally, an ion-enhanced surface kinetic model is fitted to the DeepMD etch yields, and the fitted parameters are compared to quantities computed directly from DeepMD simulations. This study illustrates how molecular dynamics simulations using machine learning potentials can provide an accurate model of etching processes relevant to device manufacturing.

Kounis-Melas, Andreas [Princeton Univ., NJ (United↗
NASA NTRS1986

Dry etching of beta-SiC in CF4 and CF4 + O2 mixtures

Dry etching of cubic (100) beta-SiC single-crystal thin films produced via chemical-vapor deposition (CVD) has been performed in CF4 and CF4 + O2 mixtures, in both the reactive-ion-etching (RIE) and plasma-etching modes. The latter process yielded measurable etch rates, but produced a dark surface layer which appears, from the results of secondary-ion mass spectrometry, to be residual SiC. The RIE samples had no residual layer, but Auger electron spectroscopy did reveal a C-rich surface. The optimal RIE conditions were obtained with 10 sccm of pure CF4 at 40 mtorr and a power density of 0.548 W/sq cm, giving an etch rate of 23.3 nm/min. Neither the increase of temperature between 293 and 573 K, nor the incremental addition of O2 to CF4 to 50 percent, produced any strong effect on the etch rates of SiC during RIE. Pictorial evidence of fine line structures produced by RIE of beta-SiC films are also presented.

Palmour, J. W.↗
NASA NTRS1988

Nonaqueous chemical etch for YBa2Cu3O(7-x)

A nonaqueous chemical etch, with Br as the active ingredient, is described which removes the insulating hydroxides and carbonates that form on high-temperature superconductor surfaces as a result of atmospheric exposure. X-ray photoemission spectra have been recorded before and after etching YBa2Cu3O(7-x) films. It is found that, after the etch, the high binding energy O 1s and Ba 3d peaks associated with surface contaminants are greatly reduced, the Y:Ba:Cu ratio is close to the expected 1:2:3, and the oxidation state of the Cu(2+) is not affected. The resistance of an etched film reaches zero at 78 K, compared to 81 K for a similar unetched film. The suitability of other nonaqueous halogen-based etches is discussed, as is the applicability of this etch to other high-Tc superconductors.

Vasquez, R. P.↗
NASA NTRS1991

Etching method for photoresists or polymers

A method for etching or removing polymers, photoresists, and organic contaminants from a substrate is disclosed. The method includes creating a more reactive gas species by producing a plasma discharge in a reactive gas such as oxygen and contacting the resulting gas species with a sacrificial solid organic material such as polyethylene or polyvinyl fluoride, reproducing a highly reactive gas species, which in turn etches the starting polymer, organic contaminant, or photoresist. The sample to be etched is located away from the plasma glow discharge region so as to avoid damaging the substrate by exposure to high energy particles and electric fields encountered in that region. Greatly increased etching rates are obtained. This method is highly effective for etching polymers such as polyimides and photoresists that are otherwise difficult or slow to etch downstream from an electric discharge in a reactive gas.

Lerner, Narcinda R.↗
NASA NTRS1995

Image analysis used to count and measure etched tracks from ionizing radiation

We have developed techniques to use digitized scanning electron micrographs and computer image analysis programs to measure track densities in lunar soil grains and plastic dosimeters. Tracks in lunar samples are formed by highly ionizing solar energetic particles and cosmic rays during near surface exposure on the Moon. The track densities are related to the exposure conditions (depth and time). Distributions of the number of grains as a function of their track densities can reveal the modality of soil maturation. We worked on two samples identified for a consortium study of lunar weathering effects, 61221 and 67701. They were prepared by the lunar curator's staff as polished grain mounts that were etched in boiling 1 N NaOH for 6 h to reveal tracks. We determined that backscattered electron images taken at 10 percent contrast and approximately 50 percent brightness produced suitable high contrast images for analysis. We used the NIH Image program to cut out areas that were unsuitable for measurement such as edges, cracks, etc. We ascertained a gray-scale threshold of 25 to separate tracks from background. We used the computer to count everything that was two pixels or greater in size and to measure the area to obtain track densities. We found an excellent correlation with manual measurements for track densities below 1 x 10(exp 8) cm(exp -2). For track densities between 1 x 10(exp 8) cm(exp -2) to 1 x 10(exp 9) cm(exp -2) we found that a regression formula using the percentage area covered by tracks gave good agreement with manual measurements. We determined the track density distributions for 61221 and 67701. Sample 61221 is an immature sample, but not pristine. Sample 67701 is a submature sample that is very close to being fully mature. Because only 10 percent of the grains have track densities less than 10(exp 9) cm(exp -2), it is difficulty to determine whether the sample matured in situ or is a mixture of a mature and a submature soil. Although our analysis of plastic dosimeters is at an early stage of development, results are encouraging. The dosimeter was etched in 6.25 N NaOH at 70 deg C for 16 h. We took 200x secondary electron images of the sample and used the NIH Image software to count and measure major and minor diameters of the etched tracks. We calculated the relative track etch rate from a formula that relates it to the major and minor diameters. We made a histogram of the number of tracks versus their relative etch rate. The relative track etching rate is proportional to the linear energy transfer of the particle. With appropriate calibration experiments, the histogram could be used to calculate the radiation dose.

Blanford, George E.↗
NASA NTRS1998

Profile Evolution Simulation in Etching Systems Using Level Set Methods

Semiconductor device profiles are determined by the characteristics of both etching and deposition processes. In particular, a highly anisotropic etch is required to achieve vertical sidewalls. However, etching is comprised of both anisotropic and isotropic components, due to ion and neutral fluxes, respectively. In Ar/Cl2 plasmas, for example, neutral chlorine reacts with the Si surfaces to form silicon chlorides. These compounds are then removed by the impinging ion fluxes. Hence the directionality of the ions (and thus the ion angular distribution function, or IAD), as well as the relative fluxes of neutrals and ions determines the amount of undercutting. One method of modeling device profile evolution is to simulate the moving solid-gas interface between the semiconductor and the plasma as a string of nodes. The velocity of each node is calculated and then the nodes are advanced accordingly. Although this technique appears to be relatively straightforward, extensive looping schemes are required at the profile corners. An alternate method is to use level set theory, which involves embedding the location of the interface in a field variable. The normal speed is calculated at each mesh point, and the field variable is updated. The profile comers are more accurately modeled as the need for looping algorithms is eliminated. The model we have developed is a 2-D Level Set Profile Evolution Simulation (LSPES). The LSPES calculates etch rates of a substrate in low pressure plasmas due to the incident ion and neutral fluxes. For a Si substrate in an Ar/C12 gas mixture, for example, the predictions of the LSPES are identical to those from a string evolution model for high neutral fluxes and two different ion angular distributions.(2) In the figure shown, the relative neutral to ion flux in the bulk plasma is 100 to 1. For a moderately isotropic ion angular distribution function as shown in the cases in the left hand column, both the LSPES (top row) and rude's string method (bottom row) predict tapered profiles. The LSPES uses an AD with a FWHM = 13.5 degrees, and rude's model uses a ratio of sheath voltage to ion temperature of 50. The more anisotropic IADs produce profiles with more vertical sidewalls and a wider bottom surface, as shown in the right hand column. Here, the LSPES has an AD with a FWHM = 2 degrees, and rude's model uses a ratio of 500 of sheath voltage to ion temperature. The agreement between the LSPES and rude's model is excellent in both cases. We will present etching profiles generated by the LSPES, including calculations of the re-emitted fluxes of both neutrals and ions off of the profile walls. In addition, we will show the effect of geometric structures (overhangs, etc.) on the etching profiles. Other physical aspects, such as surface diffusion, will also be included in the model.

Hwang, Helen H.↗
NASA NTRS2005

New Deep Reactive Ion Etching Process Developed for the Microfabrication of Silicon Carbide

Silicon carbide (SiC) is a promising material for harsh environment sensors and electronics because it can enable such devices to withstand high temperatures and corrosive environments. Microfabrication techniques have been studied extensively in an effort to obtain the same flexibility of machining SiC that is possible for the fabrication of silicon devices. Bulk micromachining using deep reactive ion etching (DRIE) is attractive because it allows the fabrication of microstructures with high aspect ratios (etch depth divided by lateral feature size) in single-crystal or polycrystalline wafers. Previously, the Sensors and Electronics Branch of the NASA Glenn Research Center developed a DRIE process for SiC using the etchant gases sulfur hexafluoride (SF6) and argon (Ar). This process provides an adequate etch rate of 0.2 m/min and yields a smooth surface at the etch bottom. However, the etch sidewalls are rougher than desired, as shown in the preceding photomicrograph. Furthermore, the resulting structures have sides that slope inwards, rather than being precisely vertical. A new DRIE process for SiC was developed at Glenn that produces smooth, vertical sidewalls, while maintaining an adequately high etch rate.

Evans, Laura J.↗
NASA NTRS2004

Step Structures Produced by Hydrogen Etching of Initially Step-Free (0001) 4H-SiC Mesas

This paper presents new observations resulting from in-situ high temperature hydrogen etching of 4H-SiC mesas that were step-free prior to initiation of etching. In particular, it was found that well-ordered pyramidal-shaped step train structures could be produced on mesa top surfaces via stepflow etching proceeding inward from the sides of mesas. In many cases, the height of steps etched inward from {112 0} mesa sides is 0.5 nm (2 Si-C bilayers), while the height of steps etched inward from {11 00} sides of the same mesa is 1.0 nm (4 Si-C bilayers, the repeat distance of the 4H-SiC polytype). We propose that stepflow etching starting from the mesa sidewall and involving step-to-step repulsive forces produces the observed step train structures.

Powell, J. Anthony↗
DOE OSTI2023

Unraveling Anisotropic and Pulsating Etching of ZnO Nanorods in Hydrochloric Acid via Correlative Electron Microscopy

Despite much technical progress achieved so far, the exact surface and shape evolution during wet chemical etching is less unraveled, especially in ionically bonded ceramics. Herein, by using in situ liquid cell transmission electron microscopy, a repeated two-stage anisotropic and pulsating periodic etching dynamic is discovered during the pencil shape evolution of a single crystal ZnO nanorod in aqueous hydrochloric acid. Specifically, the nanopencil tip shrinks at a slower rate along [0001̅] than that along the $\langle$101̅0$\rangle$ directions, resulting in a sharper ZnO pencil tip. Afterward, rapid tip dissolution happens due to accelerated etching rates along various crystal directions. Concurrently, the vicinal base region of the original nanopencil tip emerges as a new tip followed by the repeated sequence of tip shrinking and removal. The high-index surfaces, such as {101̅m} (m = 0, 1, 2, or 3) and {21̅1̅n} (n = 0, 1, 2, or 3), are found to preferentially expose in different ratios. Our 3D electron tomography, convergent beam electron diffraction, middle-angle bright-field STEM, and XPS results indicate the dissociative Cl – species were bound to the Zn-terminated tip surfaces. Furthermore, DFT calculation suggests the preferential Cl – passivation over the {101̅1} and (0001) surfaces of lower energy than others, leading to preferential surface exposures and the oscillatory variation of different facet etching rates. The boosted reactivity due to high-index nanoscale surface exposures is confirmed by comparatively enhanced chemical sensing and CO 2 hydrogenation activity. In conclusion, these findings provide an in-depth understanding of anisotropic wet chemical etching of ionic nanocrystals and offer a design strategy for advanced functional materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

ICP etching of GaN microstructures in a Cl 2 –Ar plasma with subnanometer-scale sidewall surface roughness

In this work, substrate temperature, RF power, and ICP power were investigated for their effects on GaN micropillar sidewall roughness and etch characteristics. Elevated substrate temperature was shown to improve the sidewall etch morphology at low RF powers (reduced physical bombardment) and low ICP powers (lower plasma densities). Increased lateral etching is observed with both increased ICP power and substrate temperature, which both act to increase the chemical component of the etch. Etch conditions with a high chemical driving force resulted in faceting along the a-plane on the sidewalls. This faceting produced extremely smooth surfaces with root-meansquare roughness (R q ) as low as 0.20 nm which is comparable to typical epitaxy-ready surfaces and smaller than the a-plane lattice spacing of 0.3186 nm. The smooth surfaces produced in this study enable possibilities for laser facets or for new device structures that require high quality surfaces for GaN regrowth.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Reactive ion etched, self-aligned, selective area poly-Si/SiO 2 passivated contacts

Front/back poly-Si/SiO 2 contact devices suffer from low short-circuit current density, J sc , due to parasitic optical absorption in the front poly-Si layer. Thin poly-Si (~20 nm) allows for high J sc but is not compatible with screen-printed fire-through contacts. We therefore study the effects of post-deposition etching of a thick poly-Si (200 nm) front layer by reactive ion etching (RIE) using the metal grid lines as a self-aligned mask. We show that passivation is maintained in the device during RIE and that J sc is increased by a gain in the blue quantum efficiency response. However, our specific etching parameters cause non-uniform etching of the poly-Si leading to premature loss of passivation without optimal gain in J sc . Etched, unpassivated layers can be re-passivated with a H-containing dielectric layer leading to a gain in Jsc, open circuit voltage, V oc , Fill-Factor, FF, and efficiency.

14 SOLAR ENERGY↗
DOE OSTI2021

Elucidating the Role of Halides and Iron during Radiolysis-Driven Oxidative Etching of Gold Nanocrystals Using Liquid Cell Transmission Electron Microscopy and Pulse Radiolysis

Graphene liquid cell transmission electron microscopy (TEM) has enabled the observation of a variety of nanoscale transformations. Yet understanding the chemistry of the liquid cell solution and its impact on the observed transformations remains an important step toward translating insights from liquid cell TEM to benchtop chemistry. Gold nanocrystal etching can be used as a model system to probe the reactivity of the solution. FeCl 3 has been widely used to promote gold oxidation in bulk and liquid cell TEM studies, but the roles of the halide and iron species have not been fully elucidated. In this work, we observed the etching trajectories of gold nanocrystals in different iron halide solutions. We observed an increase in gold nanocrystal etch rate going from Cl - - to Br - - to I - -containing solutions. Furthermore, this is consistent with a mechanism in which the dominant role of halides is as complexation agents for oxidized gold species. Additionally, the mechanism through which FeCl 3 induces etching in liquid cell TEM remains unclear. Ground-state bleaching of the Fe(III) absorption band observed through pulse radiolysis indicates that iron may react with Cl 2 · - radicals to form an oxidized transient species under irradiation. Complete active space self-consistent field (CASSCF) calculations indicate that the FeCl 3 complex is oxidized to an Fe species with an OH radical ligand. Together our data indicate that an oxidized Fe species may be the active oxidant, while halides modulate the etch rate by tuning the reduction potential of gold nanocrystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Etching sharp tips from thin metallic wires for tuning-fork-based scanning probe microscopy

Sharp tips are critical for obtaining high resolution images in scanning probe microscopy (SPM), particularly in samples with large variations in topography. For tuning-fork-based SPM, such tips are commonly obtained by electrochemical etching of metallic wires (e.g., tungsten). Electrochemical etching of metallic wires is the preferred means of preparing tips for scanning tunneling microscopy (STM), and techniques for obtaining sharp tips have been investigated extensively. However, the requirements for STM and tuning-fork-based SPM are different. In particular, the wires used in STM are typically 250-500 μ m in diameter, while the wires used for tuning-fork-based SPM are usually an order of magnitude narrower in order to minimize loading of the tuning fork: 25-50 μ m and sometimes down to a few micrometers in diameter. Consequently, many of the recipes developed for etching thicker metallic wires for STM tips do not give optimal results for smaller diameter wires. The authors describe here a modification of the etching circuit of Ibe et al . that significantly improves the reproducibility and reliability of the etching process for thin wires, and discuss the parameters that affect the aspect ratio of produced tips.

42 ENGINEERING↗
DOE OSTI2021

Etching with electron beam-generated plasmas: Selectivity versus ion energy in silicon-based films

In the ideal case, plasma-enhanced atomic layer etching enables the ability to not only remove one monolayer of material but also leave adjacent layers undamaged. This dual mandate requires fine control over the flux of species to ensure efficacy, while maintaining an often arduously low ion energy. Electron beam-generated plasmas are well-suited for etching at low ion energies as they are generally characterized by highly charged particle densities (10 10 –10 11 cm –3 ) and low electron temperatures (<1.0 eV), which provide the ability to deliver a large flux of ions whose energies are <5 eV. Raising the ion energy with substrate biasing thus enables process control over an energy range that extends down to values commensurate with the bond strength of most material systems. In this work, we discuss silicon nitride etching using pulsed, electron beam-generated plasmas produced in argon-SF6 backgrounds. We pay particular attention to the etch rates and selectivity versus oxidized silicon nitride and polycrystalline silicon as a function of ion energy from a few eV up to 50 eV. Here, we find the blanket etch rate of Si 3 N 4 to be in the range of 1 A/s, with selectivities (versus SiO 2 and poly-Si) greater than 10:1 when ion energies are below 30 eV.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

In-plasma photo-assisted etching of Si with chlorine aided by an external vacuum ultraviolet source

Photo-assisted etching of p-type Si was previously found to occur in a chlorine-containing, Faraday-shielded, inductively coupled plasma (ICP), and this was attributed to the vacuum ultraviolet (VUV) light generated by the plasma. Other causes for the very high etching rates were ruled out, including ion bombardment. In the present study, the substrate in the main Cl2/Ar ICP was subjected to extra VUV light that was generated in an independently controlled, auxiliary Ar/He ICP in tandem with the main ICP. The ICPs were separated by a tungsten mesh and a bundle of high-aspect-ratio quartz tubes in a honeycomb configuration. There was no measurable perturbation of the main plasma by the auxiliary plasma. The etching rate was found to be enhanced by 11%–51% with the additional VUV light provided by the auxiliary ICP. With absolute measurements of the auxiliary ICP photon flux at the sample surface, as described elsewhere, incredibly large etching yields of 90–240 Si atoms per photon were obtained. It is argued that etching is not a result of electron–hole pair formation but is instead ascribed to a photocatalytic chain reaction.

42 ENGINEERING↗