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DOE OSTI2024

Effect of Acid Etching Time in Ti 3 C 2 MXene’s Interlayer Spacing and Conductivity

Materials with sheet-like morphologies often form interconnected networks of layers or flakes, offering continuous channels for electron and ion transport in electrochemical energy storage applications. One such material is the recently discovered class of 2-D transition metal carbides/nitrides, called MXene, whose general formula is M n+1 X n T x (where M = transition metal; n = 1, 2, or 3; X = carbon or nitrogen; and T x = termination group such as –F, –OH, and/or =O). Ti 3 C 2 , one of the most studied MXene, can be synthesized by selectively etching the aluminum layer in Ti 3 AlC 2 (also called MAX phase). The most straightforward technique to exfoliate this layer is by wet-chemical etching with high-concentration hydrofluoric acid (HF). In this study, the effect of etching time on the morphology, interlayer spacing, and electrical conductivity of the resultant MXene was studied.

25 ENERGY STORAGE↗

DOE OSTI2025

Deep potential molecular dynamics simulations of ion-enhanced etching of silicon by atomic chlorine

The continued development of plasma-assisted processing techniques requires a fundamental understanding of plasma-surface interactions. Molecular dynamics (MD) simulations have been employed to complement experimental studies and better understand the properties of such systems. Recently, machine learning (ML) methods have enabled the development of ab initio-based interatomic potentials, which can be generalized to complex combinations of multiple atom types. In this work, we use ML potentials developed using the Deep Potential Molecular Dynamics (DeepMD) framework to provide a model of ion-enhanced etching of Si by Cl atoms. We demonstrate the importance of proper selection of the training data set to the accuracy of the DeepMD model and compare our results to MD results using empirical potentials, as well as to experimental measurements. Exposure of undoped Si at 300 K to thermal Cl atoms yields a steady-state Cl coverage of 1.25 monolayers, which is slightly lower than the value obtained in previous experimental studies. Predictions of Si etch yields by simultaneous Cl atom and Ar + ion impacts as a function of ion energy, neutral to ion flux ratio, and angle of incidence of the ions are in reasonably good agreement with classical MD results and experimental measurements. Finally, etch yields and SiCl x mixed layer thicknesses during simultaneous bombardment of the Si(100) surface by Cl atoms and Cl + ions are in good agreement with experimental data. In conclusion, the present work is a necessary condition for the extension of the DeepMD procedure to more complex systems of interest in plasma-surface interactions.

Artificial neural networks↗

DOE OSTI2024

Optimizing Aluminum Bonding: Exploring Surface Roughness and Contact Angle Effects through Plasma and Acid Etching Contrasts

The use of adhesives to replace traditional techniques like welding and riveting has been on the rise in various industries as increasingly complex geometries and situations for bonding is required. It’s well known in the scientific community that an adhesive bond is only as efficient as the surface preparation used beforehand. Plasma treatments have been shown to gently clean the surface by only removing the top-most layer from the adherend and “charging” the surface instead of berating it. Whereas chemical treatments “etch” the surface in hopes of increasing surface area by increasing surface roughness. This method can be difficult to control quantitatively and can generate waste leading to serious environmental concerns. This study aims to address the encountered differences between plasma treatments and acid etching on aluminum substrates for adhesive bonding. Treating the surface of adherends plays a crucial role in promoting a good bond between adhesive and adherend. In this study, the effects of plasma and acid treatments are categorized using surface roughness measurements as well as contact angle which have been shown to correlate to mechanical strength. When evaluating different surface treatments, it is notable to mention that not only surface roughness and contact angle play a role in determining which method is most effective but also the consequences of the treatment itself. It was found that although chemical etching was the most effective in increasing roughness and decreasing contact angle, it generates a large amount of waste and is not sustainable compared to plasma work which uses a renewable process. The results from this work provide a deeper understanding of the relationship between surface treatments and surface roughness/contact angle and how this relates to a stronger adhesive bond.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Optimizing Aluminum Bonding: Exploring Surface Roughness and Contact Angle Effects through Plasma and Acid Etching Contrasts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1969

Multiple-mask chemical etching

Multiple masking techniques use lateral etching to reduce the total area of the high etch-rate oxide exposed to the chemical etchant. One method uses a short-term etch to remove the top layer from the silicon oxide surface, another acts before the top layer is grown.

Cannon, D. L.↗

NASA NTRS1975

An investigation of RF sputter etched silicon surfaces using helium ion backscatter

The effect of RF sputter etching on the (111) surface of silicon was studied by observing backscatter spectra from a 2 MeV, He-4(+) beam oriented along the silicon 111 orientation channel. Silicon samples were RF sputter etched in an argon discharge at electrode bias potentials ranging from 0.5 to 2.5 kV. The samples were sputter etched for a time sufficient for the lattice damage to reach saturation. Analysis of these samples revealed that the thickness of this damage layer and the concentration of trapped argon increased with electrode bias potential. An annealing study of these damaged surfaces was carried out to 900 C.

Sachse, G. W.↗

NASA NTRS1978

Ion beam sputter etching and deposition of fluoropolymers

Fluoropolymer etching and deposition techniques including thermal evaporation, RF sputtering, plasma polymerization, and ion beam sputtering are reviewed. Etching and deposition mechanism and material characteristics are discussed. Ion beam sputter etch rates for polytetrafluoroethylene (PTFE) were determined as a function of ion energy, current density and ion beam power density. Peel strengths were measured for epoxy bonds to various ion beam sputtered fluoropolymers. Coefficients of static and dynamic friction were measured for fluoropolymers deposited from ion bombarded PTFE.

Banks, B. A.↗

NASA NTRS1978

Ion beam sputter etching and deposition of fluoropolymers

Fluoropolymer etching and deposition techniques including thermal evaporation, RF sputtering, plasma polymerization, and ion beam sputtering are reviewed. Etching and deposition mechanisms and material characteristics are discussed. Ion beam sputter etch rates for polytetrafluoroethylene (PTFE) were determined as a function of ion energy, current density and ion beam power density. Peel strengths were measured for epoxy bonds to various ion beam sputtered fluoropolymers. Coefficients of static and dynamic friction were measured for fluoropolymers deposited from ion bombarded PTFE.

Banks, B. A.↗

NASA NTRS1979

Homogeneous alignment of nematic liquid crystals by ion beam etched surfaces

A wide range of ion beam etch parameters capable of producing uniform homogeneous alignment of nematic liquid crystals on SiO2 films are discussed. The alignment surfaces were generated by obliquely incident (angles of 5 to 25 deg) argon ions with energies in the range of 0.5 to 2.0 KeV, ion current densities of 0.1 to 0.6 mA sq cm and etch times of 1 to 9 min. A smaller range of ion beam parameters (2.0 KeV, 0.2 mA sq cm, 5 to 10 deg and 1 to 5 min.) were also investigated with ZrO2 films and found suitable for homogeneous alignment. Extinction ratios were very high (1000), twist angles were small ( or = 3 deg) and tilt-bias angles very small ( or = 1 deg). Preliminary scanning electron microscopy results indicate a parallel oriented surface structure on the ion beam etched surfaces which may determine alignment.

Wintucky, E. G.↗

NASA NTRS1982

Selective Etching of Semiconductor Glassivation

Selective etching technique removes portions of glassivation on a semi-conductor die for failure analysis or repairs. A periodontal needle attached to a plastic syringe is moved by a microprobe. Syringe is filled with a glass etch. A drop of hexane and vacuum pump oil is placed on microcircuit die and hexane is allowed to evaporate leaving a thin film of oil. Microprobe brings needle into contact with area of die to be etched.

Casper, N.↗

NASA NTRS1981

Ion beam sputter etching of orthopedic implanted alloy MP35N and resulting effects on fatigue

The effects of two types of argon ion sputter etched surface structures on the tensile stress fatigue properties of orthopedic implant alloy MP35N were investigated. One surface structure was a natural texture resulting from direct bombardment by 1 keV argon ions. The other structure was a pattern of square holes milled into the surface by a 1 keV argon ion beam through a Ni screen mask. The etched surfaces were subjected to tensile stress only in fatigue tests designed to simulate the cyclic load conditions experienced by the stems of artificial hip joint implants. Both types of sputter etched surface structures were found to reduce the fatigue strength below that of smooth surface MP35N.

Wintucky, E. G.↗

NASA NTRS1983

Etching of moldavities under natural conditions

The hypothesis that a part of the lechatellierites which originated by etching from a basic moldavite mass became broken off after deposition of moldavite in the sedimentation layer is advanced. Those found close to the original moldavite were measured for statistical averaging of length. The average length of lechatelierite fibers per cubic mm of moldavite mass volume was determined by measurement under a microscope in toluene. The data were used to calculate the depth of the moldavite layer that had to be etched to produce the corresponding amount of lechatelierite fragments. The calculations from five "fields" of moldavite surface, where layers of fixed lechatelierite fragments were preserved, produced values of 2.0, 3.1, 3.5, 3.9 and 4.5. Due to inadvertent loss of some fragments the determined values are somewhat lower than those found in references. The difference may be explained by the fact that the depth of the layer is only that caused by etching after moldavite deposition.

Knobloch, V.↗

NASA NTRS1985

Trapped Xe components in etched samples of the Murray (C2) and Murchison (C2) carbonaceous chondrites

Xe isotopic measurements are described. The samples analyzed were bulk chips of the Murray (C2) and Murchison (C2) carbonaceous chondrites that had been freeze-thaw disaggregated, etched with H2O2, and then split into colloidal and noncolloidal fractions using methanol. The etching removed a substantial portion of the trapped Xe and increased variations in measured isotopic ratios compared with bulk sample analyses. The Murray samples appeared to contain a binary mixture of U-Xe and H+L-Xe. The Murchison data concur with the Murray data for the heavy isotopes, but the structure at the light isotopes is obscured by spallation Xe. There is no evidence in these data for the separability of H-Xe and L-Xe. The fact that H2O2 etching removes Xe without prior demineralization supports the view that the carrier of a substantial portion of trapped Xe may reside on grain surfaces.

Jones, C. M.↗

NASA NTRS1986

Apparatus for edge etching of semiconductor wafers

A device for use in the production of semiconductors, characterized by etching in a rapidly rotating etching bath is described. The fast rotation causes the surface of the etching bath to assume the form of a paraboloid of revolution, so that the semiconductor wafer adjusted at a given height above the resting bath surface is only attacked by etchant at the edges.

Casajus, A.↗

NASA NTRS1987

Deep, Precise Etching in Semiconductors

Semiconductors made to accept precise etching after pretreatment. Combination of material destabilization and anisotropic etching permits formation of precise perpendicular-wall cavities in silicon wafers and other semiconductors. New technique extends capabilities of current micromachining technology to fabrication of submillimeter waveguide arrays and filters. Pre-etching process currently used to fabricate thin-walled arrays of submillimeter waveguides for use as dichroic bandpass filters. Possible applications include integration of sensor probes and processing of circuitry on same silicon chip.

Shlichta, P. J.↗

NASA NTRS1991

Identification of dislocation etch pits in n-type GaAs by NIR transmission microscopy

An optical method is described for identifying dislocation etch pits in n-type GaAS, using near-IR brightfield transmission microscopy. Dislocations are revealed in a nondestructive manner through contrasts that are likely due to impurity decoration of the dislocation lines. By subjecting the same wafers to a photoetching technique, it was established that each etch pit on the surface is associated with a dislocation and that the termination of each (decorated) dislocation is an etch pit.

Cao, X. Z.↗

NASA NTRS1995

Etching Semiconductors With Beams Of Reactive Atoms

Method of etching semiconductors with energetic beams of electrically neutral, but chemically reactive, species undergoing development. Enables etching of straight walls into semiconductor substrates at edges of masks without damage to underlying semiconductor material. In addition to elimination of charge damage, technique reduces substrate bombardment damage because translational energy of neutral species in range 2-12 eV, below damage threshold of many semiconductor materials. Furthermore, low-energy neutrals cause no mask erosion allowing for etching features with very high aspect ratios.

Minton, Timothy K.↗

NASA NTRS1999

Diagnostic for Plasma Enhanced Chemical Vapor Deposition and Etch Systems

In order to meet NASA's requirements for the rapid development and validation of future generation electronic devices as well as associated materials and processes, enabling technologies ion the processing of semiconductor materials arising from understanding etch chemistries are being developed through a research collaboration between Stanford University and NASA-Ames Research Center, Although a great deal of laboratory-scale research has been performed on many of materials processing plasmas, little is known about the gas-phase and surface chemical reactions that are critical in many etch and deposition processes, and how these reactions are influenced by the variation in operating conditions. In addition, many plasma-based processes suffer from stability and reliability problems leading to a compromise in performance and a potentially increased cost for the semiconductor manufacturing industry. Such a lack of understanding has hindered the development of process models that can aid in the scaling and improvement of plasma etch and deposition systems. The research described involves the study of plasmas used in semiconductor processes. An inductively coupled plasma (ICP) source in place of the standard upper electrode assembly of the Gaseous Electronics Conference (GEC) radio-frequency (RF) Reference Cell is used to investigate the discharge characteristics and chemistries. This ICP source generates plasmas with higher electron densities (approximately 10(exp 12)/cu cm) and lower operating pressures (approximately 7 mTorr) than obtainable with the original parallel-plate version of the GEC Cell. This expanded operating regime is more relevant to new generations of industrial plasma systems being used by the microelectronics industry. The motivation for this study is to develop an understanding of the physical phenomena involved in plasma processing and to measure much needed fundamental parameters, such as gas-phase and surface reaction rates. species concentration, temperature, ion energy distribution, and electron number density. A wide variety of diagnostic techniques are under development through this consortium grant to measure these parameters. including molecular beam mass spectrometry (MBMS). Fourier transform infrared (FTIR) spectroscopy, broadband ultraviolet (UV) absorption spectroscopy, a compensated Langmuir probe. Additional diagnostics. Such as microwave interferometry and microwave absorption for measurements of plasma density and radical concentrations are also planned.

Cappelli, Mark A.↗