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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

ScAIN etch mask for highly selective etching

A fabrication process employing the use of ScAlN as an etch mask is disclosed. The ScAlN etch mask is chemically nonvolatile in fluorine-based etch chemistries and has a low sputter yield, resulting in greater etch mask selectivity and reduced surface roughness for silicon and other semiconductor materials. The ScAlN etch mask has an etch mask selectivity of greater than 200,000:1 relative to silicon compared to an etch mask selectivity of less than 40,000:1 for a prior art AlN etch mask relative to silicon. Further, due to reduced sputtering of the ScAlN etch mask, and thus reduced micromasking, the ScAlN etch mask yielded a surface roughness of 0.6 μm compared to a surface roughness of 2.8 μm for an AlN etch mask.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Evidence for anti-synergism between ion-assisted etching and in-plasma photoassisted etching of silicon in a high-density chlorine plasma

Etching of p-Si in 60 mTorr 10%Cl2/90%Ar Faraday-shielded inductively coupled high density plasmas was investigated under both ionassisted etching (IAE) and photoassisted etching (PAE) conditions. Real-time etching rates and after-etching Si surface chemical compositions were obtained by laser interferometry and vacuum-transfer x-ray photoelectron spectroscopy (XPS), respectively. Precisely controlled ion energy distributions (IEDs) were generated by applying pulsed negative DC bias on the conductive sample stage. Above a 36 eV threshold at a total flow rate of 250 SCCM, the IAE rate increased with the square root of the ion energy. In contrast to the DC bias, etching under RF bias did not exhibit a threshold ion energy because of the wide IED. XPS spectra revealed that the surface layer under PAE conditions had a significantly lower chlorine content, composed of only SiCl. Under IAE conditions, however, silicon dangling bonds (Si•), SiCl 2 , and SiCl 3 were found on the surface, in addition to SiCl, with a relative abundance of SiCl > SiCl 2 , and SiCl 3 . The absence of higher chlorides and Si• under PAE conditions suggested that vacuum ultraviolet photons and above threshold-energy ions interact with the surface very differently. By varying the duty cycle of the pulsed DC bias, it was found that the IAE rate scaled with the energetic ion dose, but only for low duty cycles. For higher duty cycles, the apparent IAE yield fell off with an increasing Cl coverage on the surface, as the duty cycle went up, which pointed to a negative synergy (antisynergism) between PAE and IAE as the explanation. This antisynergism was further supported by the observed decrease of the total etching rate with an increasing period of the pulsed DC bias. A plausible mechanism is that increasing the pulsing period causes more near-surface damage, creating more recombination centers that lead to a higher loss rate of electron-hole pairs through recombination, thereby reducing the PAE rate.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2021

Impact of carrier wafer on etch rate, selectivity, morphology, and passivation during GaN plasma etching

The choice of carrier wafer was found to significantly influence etch rates, selectivity, and morphology in GaN micropillar etching in a Cl 2 -Ar high-density inductively coupled plasma. 7 × 7 mm 2 GaN on sapphire chips with a plasma-enhanced chemical vapor deposition SiO 2 hard mask was etched on top of 4-in. fused silica, silicon carbide, silicon, sapphire, aluminum nitride, and high purity aluminum carriers. Silicon and silicon carbide carriers reduced GaN:SiO 2 selectivity because incidental SiCl x and CCl x etch products from the carriers attack the SiO 2 mask. Aluminum nitride and high-purity aluminum carriers yielded the highest GaN:SiO 2 selectivities due to the deposition of Al-based etched by-products, while the highest GaN etch rate was achieved using the sapphire carrier since it was the most inert carrier and did not sink any Cl 2 . Overall, results indicate that SiO 2 and Al may be used as passivation materials during GaN etching, as vertical profiles were achieved when SiO 2 or Al is redeposited from the fused silica and aluminum carriers, respectively. Floor pitting, trenching, sidewall roughness, and faceting were all influenced by carrier wafer type and will be discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Etch Products of Copper Atomic Layer Etching by Oxidation and Formic Acid Vapor

Atomic layer etching (ALE) of metals offers a path to greater control of selectivity, etch rate, and etch profile. However, tailoring a process to meet these demands requires an understanding of the volatile etch product, which is challenging to detect due to low product concentrations and the paramagnetism of many metalorganic products. Here, in this work, several complementary analysis techniques were used to determine the volatile etch product and residual surface species of a Cu ALE process based on plasma oxidation and formic acid vapor etching of the oxidized layer. It was shown that the volatile product was copper formate with a Cu 2+ paramagnetic center, in concordance with prior density functional theory (DFT) calculations. While copper formate tetrahydrate was formed, it was determined that the tetrahydrate product was confined to the surface, with anhydrous copper formate being the volatile etch product.

Smith, Taylor G. [Univ. of California, Los Angeles↗
DOE OSTI2021

Scaling of atomic layer etching of SiO 2 in fluorocarbon plasmas: Transient etching and surface roughness

Fabricating sub-10 nm microelectronics places plasma processing precision at atomic dimensions. Atomic layer etching (ALE) is a cyclic plasma process used in semiconductor fabrication that has the potential to remove a single layer of atoms during each cycle. In self-limiting ideal ALE, a single monolayer of a material is consistently removed in each cycle, typically expressed as EPC (etch per cycle). In plasma ALE of dielectrics, such as SiO 2 and Si 3 N 4 , using fluorocarbon gas mixtures, etching proceeds through deposition of a thin polymer layer and the process is not strictly self-terminating. As a result, EPC is highly process dependent and particularly sensitive to the thickness of the polymer layer. In this paper, results are discussed from a computational investigation of the ALE of SiO 2 on flat surfaces and in short trenches using capacitively coupled plasmas consisting of a deposition step (fluorocarbon plasma) and an etch step (argon plasma). We found that ALE performance is a delicate balance between deposition of polymer during the first half cycle and etching (with polymer removal) during the second half cycle. In the absence of complete removal of the overlying polymer in each cycle, ALE may be transient as the polymer thickness grows with each cycle with a reduction in EPC until the thickness is too large to enable further etching. Small and statistical amounts of polymer left from a previous cycle can produce statistical variation in polymer thickness on the next cycle, which in turn can lead to a spatially dependent EPC and ALE roughness. Based on synergy between T i (sputtering time) and T p (passivation time), dielectric ALE can be described as having three modes: deposition, roughening surface (transitioning to etch-stop), and smooth surface with steady-state EPC.

Materials Science↗
NASA NTRS2006

Deep Reactive Ion Etching (DRIE) of High Aspect Ratio SiC Microstructures using a Time-Multiplexed Etch-Passivate Process

High aspect ratio silicon carbide (SiC) microstructures are needed for microengines and other harsh environment micro-electro-mechanical systems (MEMS). Previously, deep reactive ion etching (DRIE) of low aspect ratio (AR less than or = 1) deep (greater than 100 micron) trenches in SiC has been reported. However, existing DRIE processes for SiC are not well-suited for definition of high aspect ratio features because such simple etch-only processes provide insufficient control over sidewall roughness and slope. Therefore, we have investigated the use of a time-multiplexed etch-passivate (TMEP) process, which alternates etching with polymer passivation of the etch sidewalls. An optimized TMEP process was used to etch high aspect ratio (AR greater than 5) deep (less than 100 micron) trenches in 6H-SiC. Power MEMS structures (micro turbine blades) in 6H-SiC were also fabricated.

Evans, Laura J.↗
DOE OSTI2020

Metal-assisted etch combined with regularizing etch

In an aspect of the disclosure, a process for forming nanostructuring on a silicon-containing substrate is provided. The process comprises (a) performing metal-assisted chemical etching on the substrate, (b) performing a clean, including partial or total removal of the metal used to assist the chemical etch, and (c) performing an isotropic or substantially isotropic chemical etch subsequently to the metal-assisted chemical etch of step (a). In an alternative aspect of the disclosure, the process comprises (a) performing metal-assisted chemical etching on the substrate, (b) cleaning the substrate, including removal of some or all of the assisting metal, and (c) performing a chemical etch which results in regularized openings in the silicon substrate.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Voltage waveform tailoring for high aspect ratio plasma etching of SiO 2 using Ar/CF 4 /O 2 mixtures: Consequences of ion and electron distributions on etch profiles

The quality of high aspect ratio (HAR) features etched into dielectrics for microelectronics fabrication using halogen containing low temperature plasmas strongly depends on the energy and angular distribution of the incident ions (IEAD) onto the wafer, as well as potentially that of the electrons (EEAD). Positive ions, accelerated to high energies by the sheath electric field, have narrow angular spreads and can penetrate deeply into HAR features. Electrons typically arrive at the wafer with nearly thermal energy and isotropic angular distributions and so do not directly penetrate deeply into features. These differences can lead to positive charging of the insides of the features that can slow etching rates and produce geometric defects such as twisting. In this work, we computationally investigated the plasma etching of HAR features into SiO 2 using tailored voltage waveforms in a geometrically asymmetric capacitively coupled plasma sustained in an Ar/CF 4 /O 2 mixture at 40 mTorr. The tailored waveform consisted of a sinusoidal wave and its higher harmonics with a fundamental frequency of 1 MHz. We found that some degree of control of the IEADs and EEADs is possible by adjusting the phase of higher harmonics φ through the resulting generation of electrical asymmetry and electric field reversal. However, the IEADs and EEADs cannot easily be separately controlled. The control of IEADs and EEADs is inherently linked. The highest quality feature was obtained with a phase angle φ = 0° as this value generated the largest (most negative) DC self-bias and largest electric field reversal for accelerating electrons into the feature. That said, the consequences of voltage waveform tailoring (VWT) on etched features are dominated by the change in the IEADs. Although VWT does produce EEADs with higher energy and narrower angular spread, the effect of these electrons on the feature compared to thermal electrons is not large. Finally, this smaller impact of VWT produced EEADs is attributed to thermal electrons being accelerated into the feature by electric fields produced by the positive in-feature charging.

47 OTHER INSTRUMENTATION↗
NASA NTRS1989

Polymer etching in the oxygen afterglow - Increased etch rates with increased reactor loading

Reactor loading has an effect on the etch rate (rate of decrease of film thickness) of films of polyvinylfluoride (Tedlar) and polyethylene exposed in the afterglow of an RF discharge in oxygen. The etch rate is found to increase with the total surface area of the polymer exposed in the reactor. The etch rates of polypyromellitimide (Kapton H) and polystyrene under these conditions are very low. However, the etch rate of these polymers is greatly enhanced by adding either Tedlar or polyethylene to the reactor. A kinetic model is proposed based on the premise that the oxygen atoms produced by the RF discharge react with Tedlar or polyethylene to produce a much more reactive species, which dominates the etching of the polymers studied.

Lerner, N. R.↗
DOE OSTI2021

Etched-And-Regrown GaN P–N Diodes with Low-Defect Interfaces Prepared by In Situ TBCl Etching

The ability to form pristine interfaces after etching and regrowth of GaN is a prerequisite for epitaxial selective area doping, which in turn is needed for the formation of lateral PN junctions and advanced device architectures. In this work, we report the electrical properties of etched-and-regrown GaN PN diodes using an in situ Cl-based precursor, tertiary butylchloride (TBCl). We demonstrated a regrowth diode with I–V characteristics approaching that from a continuously grown reference diode. The sources of unintentional contamination from the silicon (Si) impurity and the mediating effect of Si during the TBCl etching are also investigated in this study. Furthermore, this work points to the potential of in situ TBCl etching toward the realization of GaN lateral PN junctions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Investigation of the distribution of laser-induced damage precursors in etched grating sidewalls fabricated using inductively coupled plasma reactive-ion etching

Inductively coupled plasma reactive-ion etching for grating fabrication is explored with emphasis on the type and distribution of process-induced defects that can act as precursors to laser-induced damage initiation. To provide flexibility in the ability to perform a variety of material characterization methods, grating-like features with large pitch were fabricated in silica monolayers. The results indicate that the etch process introduces surface fluorine and subsurface carbon-containing contamination, which reduces the laser-induced damage threshold. The local relative concentrations of the laser-damage precursors introduced during the etch step of the manufacturing process were investigated using angle-resolved damage testing, taking advantage of the shift of the location of the peak electric-field intensity incident on the grating sidewall. The results suggest an increased level of etch-related defects near the base of the sidewall, with directly fluorinated silicon identified as the primary defect.

Dent, R. [Univ. of Rochester, NY (United States). ↗
DOE OSTI2021

Removing or preventing dry etch-induced damage in Al/In/GaN films by photoelectrochemical etching

A method comprises providing a substrate comprising an n-type Al/In/GaN semiconductor material. A surface of the substrate is dry-etched to form a trench therein and cause dry-etch damage to remain on the surface. The surface of the substrate is immersed in an electrolyte solution and illuminated with above bandgap light having a wavelength that generates electron-hole pairs in the n-type Al/In/GaN semiconductor material, thereby photoelectrochemically etching the surface to remove at least a portion of the dry-etch damage.

Monavarian, Morteza↗
DOE OSTI2023

Removing or preventing dry etch-induced damage in Al/In/GaN films by photoelectrochemical etching

A method comprises providing a substrate comprising an n-type Al/In/GaN semiconductor material. A surface of the substrate is dry-etched to form a trench therein and cause dry-etch damage to remain on the surface. The surface of the substrate is immersed in an electrolyte solution and illuminated with above bandgap light having a wavelength that generates electron-hole pairs in the n-type Al/In/GaN semiconductor material, thereby photoelectrochemically etching the surface to remove at least a portion of the dry-etch damage.

Monavarian, Morteza↗
NASA NTRS1998

Testing and Further Development of Improved Etches and Etching Methods for the Analysis of Bridgman Grown Semiconductor Crystals with an Emphasis on Lead-Tin-Telluride

The goals outlined for the research project for this year have been completed, and the following supporting documentation is attached: 1. A copy of the proposal outlining the principal goals: (a) Improve the characterization of semiconductor crystals through new etches and etching procedures. (b) Developed a novel voltammetric method to characterize semiconductor crystals as a result of searching for improved etches for lead-tin-telluride. (c) Presented paper at ACCG- 10. (d) Prepared manuscripts for publication. Completed additional testing suggested by reviewers and re-submitted manuscripts. (e) Worked with an undergraduate student on this project to provide her an opportunity to have a significant research experience prior to graduation. 2. In addition to the anticipated goals the following were also accomplished: (a) Submitted the newly developed procedures for consideration as a patent or a NASA Tech Brief. (b) Submitted a paper for presentation at the forthcoming ICCG- 12 conference. 3. A copy of the final draft of the publication as submitted to the editors of the Journal of Crystal Growth.

Barber, Patrick G.↗
DOE OSTI2020

Improved control of electron computer-generated holographic grating groove profiles using ion beam gas-assisted etching

In a transmission electron microscope, electrons are described by matter-waves with wavelengths five orders of magnitude smaller than optical electromagnetic waves. Analogous to optical holography, electron wavefronts can be shaped using nanoscale holographic gratings. Here we demonstrate a novel, scalable nanofabrication method for creating off-axis holographic gratings that demonstrate near ideal diffraction efficiencies for binary, sinusoidal, and blazed grating groove profiles. We show that this method can produce up to 50 µm diameter area gratings that diffract up to 68% of the transmitted electron wave into a desired diffraction order with less than 7% into any other order. Additionally, we find that the amount of inelastically scattered electrons from the material gratings remaining in the coherent diffraction orders from the gratings is negligible in the far field.

Johnson, Cameron W.↗