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Results for “anisotropic wet etching”

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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11 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

6000 lines/mm blazed grating for a high-resolution x-ray spectrometer

We have designed and fabricated a high groove density blazed grating for a Resonant Inelastic X-ray Scattering spectrometer for the new Qerlin beamline at the Advanced Light Source (ALS) synchrotron facility. The gratings were fabricated using a set of nanofabrication techniques including e-beam lithography, nanoimprint, plasma etch, and anisotropic wet etching. Two gratings with groove density of 6000 lines/mm and 3000 lines/mm and optimized for operation in the 1st and 2nd negative diffraction order respectively were fabricated and tested. We report on fabrication details and characterization of the gratings at beamline 6.3.2 of the ALS.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Fabrication of low blaze angle gratings by replication and plasma etch

We suggest a new method of making ultra-low blaze angle gratings for synchrotron application. The method is based on reduction of the blaze angle of a master grating by replication followed by a plasma etch. A master blazed grating with a relatively large blaze angle is fabricated by anisotropic wet etching of a Si single crystal substrate. The surface of the master grating is replicated by a polymer material on top of a quartz substrate by nanoimprinting and then transferred into quartz by a plasma etch. Then a 2nd nanoimprint step is applied to transfer the saw-tooth surface into a resist layer on top of a Si grating substrate. The plasma etch through the patterned resist layer provides transfer of the grooves into the Si substrate and results in reduction of the blaze angle due to the difference in etch rates of the resist and Si. We investigated the impact of the replication process on the groove shape, facet surface roughness, and diffraction efficiency of the fabricated 200 lines/mm low blaze angle grating.

Park, Sooyeon↗
DOE OSTI2023

Advanced low blaze angle x-ray gratings via nanoimprint replication and plasma etch

We developed a new method of making ultra-low blaze angle diffraction gratings for x-ray applications. The method is based on reduction of the blaze angle of a master grating by nanoimprint replication followed by a plasma etch. A master blazed grating with a relatively large blaze angle is fabricated by anisotropic wet etching of a Si single crystal substrate. The surface of the master grating is replicated by a polymer material on top of a quartz substrate by nanoimprinting. Then a second nanoimprinting is performed using the 1st replica as a mold to replicate the saw-tooth surface into a resist layer on top of a Si grating substrate. A reactive ion etch is used to transfer the grating grooves into the Si substrate. The plasma etch provides reduction of the groove depth by a factor defined by the ratio of the etch rates for the resist and Si. We demonstrate reduction of the blaze angle of a master grating by a factor of 5 during fabrication of a 200 lines/mm blazed grating with a blaze angle of 0.2°. We investigated the quality and performance of the fabricated low blaze angle gratings and evaluate process accuracy and reproducibility. The new blaze angle reduction method preserves the planarity of the optical surface of the grating substrate and at the same time provides improvement in the grating groove quality during the reduction process.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Ferroelectricity of wurtzite Al 1−x Hf x N heterovalent alloys

Thin films of aluminum hafnium nitride (Al1−xHfxN) were synthesized via reactive magnetron sputtering for Hf contents up to x = 0.13. X-ray diffraction showed a single c-axis oriented wurtzite phase for all films. Hard x-ray photoelectron spectroscopy demonstrated homogeneous Al:Hf distribution through the thin films and confirmed their insulating character. A collection of complementary tests showed unambiguous polarization inversion, and thus ferroelectricity in multiple samples. Current density vs electric field hysteresis measurements showed distinct ferroelectric switching current peaks, the piezoelectric coefficient d 33,f,meas measured using a double beam laser interferometer (DBLI) showed a reversal in sign with similar magnitude, and anisotropic wet etching confirmed field-induced polarization inversion. This demonstrates the possibility of using tetravalent–and not just trivalent–alloying elements to enable ferroelectricity in AlN-based thin films, highlighting the compositional flexibility of ferroelectricity in wurtzites and greatly expanding the chemistries that can be considered for future devices.

36 MATERIALS SCIENCE↗
DOE OSTI2020

X-ray verification of sol-gel resist shrinkage in substrate-conformal imprint lithography for a replicated blazed reflection grating

Surface-relief gratings fabricated through nanoimprint lithography (NIL) are prone to topographic distortion induced by resist shrinkage. Characterizing the impact of this effect on blazed diffraction efficiency is particularly important for applications in astrophysical spectroscopy at soft x-ray wavelengths ( λ ≈ 0.5 − 5 nm) that call for the mass-production of large-area grating replicas with sub-micron, sawtooth surface-relief profiles. A variant of NIL that lends itself well for this task is substrate-conformal imprint lithography (SCIL), which uses a flexible, composite stamp formed from a rigid master template to imprint nanoscale features in an inorganic resist that cures thermodynamically through a silica sol-gel process. While SCIL enables the production of several hundred imprints before stamp degradation and avoids many of the detriments associated with large-area imprinting in NIL, the sol-gel resist suffers shrinkage dependent on the post-imprint cure temperature. Through atomic force microscopy and diffraction-efficiency testing at beamline 6.3.2 of the Advanced Light Source, the impact of this effect on blaze response is constrained for a ∼160-nm-period grating replica cured at 90 ° C. Results demonstrate a ∼2 ° reduction in blaze angle relative to the master grating, which was fabricated by anisotropic wet etching in 〈311〉-oriented silicon to yield a facet angle close to 30 ° .

McCoy, Jake A. (ORCID:0000000216057517)↗
DOE OSTI2022

Numerical and Experimental Investigation of Nanostructure-Based Asymmetric Light Transmission Interfaces for Solar Concentrator Applications

Research in asymmetric light transmission interfaces has been recently gaining traction. While traditionally considered for optical circuitry applications, there is a new interest to use these interfaces in luminescent solar concentrators. Previous studies have shown that applying them to the top surface of a concentrator could mitigate surface losses. This paper presents experimental results for proof-of-concept asymmetric light transmission interfaces that may have potential applications in luminescent solar concentrators. The interfaces and the underneath substrate were created in a single step from polydimethylsiloxane using silicon molds fabricated on <100> wafers via anisotropic wet etching. The resulting structures were pyramidal in shape. Large surface areas of nanostructures repeating at 800 nm, 900 nm, and 1000 nm were tested for backward and forward transmission using a spectrometer. Results showed a 21%, 10%, and 0% average transmissivity difference between the forward and backward directions for each periodicity, respectively. The trends seen experimentally were confirmed numerically via COMSOL simulations.

Oliveto, Vincent↗
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 OSTI2021

Effective Dielectric Passivation Scheme in Area-Selective Front/Back Poly-Si/SiOx Passivating Contact Solar Cells

Despite the high efficiencies reached by heavily doped poly-Si/SiO x passivating contact solar cells, challenges like the high front parasitic absorption still limit their performance. Previously, we showed a wet etching technique using self-aligned metal grids to remove the front poly-Si in the non-metallized region. Here, we focus on the effective dielectric passivation on this tunneling oxide/n + in-diffused region. The effect of poly-Si thickness was studied to balance between the passivation quality and the current gain. We then compared various dielectric passivation schemes using SiN x , Al 2 O 3 , and stacks thereof via injection-level dependent lifetime and the transfer length method. We demonstrate a SiN x /Al 2 O 3 stack yielded the best passivation performance within device process limitation and obtained an improved front/back poly-Si/SiO x passivating contact device, with a short circuit current density of 41.8 mA/cm 2 and an efficiency of 21.8%.

anisotropic wet etching↗
DOE OSTI2021

Isotropic etchback method of linewidth tailoring multilayer dielectric diffraction gratings for improvement of laser damage resistance and diffraction efficiency

A method of fabricating a multilayer dielectric (MLD) diffraction grating by providing a multilayer stack having a grating layer, and anisotropically etching the grating layer to form grating lines having an initial lineheight, an initial linewidth, and an initial grating duty cycle, that are greater than a target lineheight, a target linewidth, and a target grating duty cycle, respectively. An isotropic wet etch solution is then used to etch back the grating lines to the target lineheight, the target linewidth, and the target grating duty cycle so as to minimize electric field intensities and maximize diffraction efficiency for a given set of MLD illumination conditions.

Britten, Jerald A.↗
DOE OSTI2020

Large-Scale Plasmonic Hybrid Framework with Built-In Nanohole Array as Multifunctional Optical Sensing Platforms

Light coupling with patterned subwavelength hole arrays induces enhanced transmission supported by the strong surface plasmon mode. In this work, a nanostructured plasmonic framework with vertically built-in nanohole arrays at deep-subwavelength scale (6 nm) is demonstrated using a two-step fabrication method. The nanohole arrays are formed first by the growth of a high-quality two-phase (i.e., Au–TiN) vertically aligned nanocomposite template, followed by selective wet-etching of the metal (Au). Such a plasmonic nanohole film owns high epitaxial quality with large surface coverage and the structure can be tailored as either fully etched or half-way etched nanoholes via careful control of the etching process. The chemically inert and plasmonic TiN plays a role in maintaining sharp hole boundary and preventing lattice distortion. Optical properties such as enhanced transmittance and anisotropic dielectric function in the visible regime are demonstrated. Numerical simulation suggests an extended surface plasmon mode and strong field enhancement at the hole edges. Furthermore, two demonstrations, including the enhanced and modulated photoluminescence by surface coupling with 2D perovskite nanoplates and the refractive index sensing by infiltrating immersion liquids, suggest the great potential of such plasmonic nanohole array for reusable surface plasmon-enhanced sensing applications.

42 ENGINEERING↗
DOE OSTI2020

Sapphire advanced mitigation process: wet etch to expose sub-surface damage and increase laser damage resistance and mechanical strength

In this study, a novel, to the best of our knowledge, method of wet chemical etching of sapphire workpieces (such as optics, wafers, windows, and cones), called the sapphire advanced mitigation process (or sapphire AMP), has been developed that exposes sub-surface mechanical damage created during the optical fabrication process and significantly enhances the surface laser damage resistance (> 2×) and mechanical strength (up to ~ 2.6×). Sapphire AMP involves first treating the workpiece with a mixture of sulfuric and phosphoric acid ([H 2 SO 4 ]:[H 3 PO 4 ]= 1 : 3) at 220°C, followed with phosphoric acid at 160°C, then with sodium hydroxide base (NaOH) and surfactant at 40°C, and finally with a high-pressure deionized water spray rinse. Sapphire AMP has been demonstrated on both A- and C-plane sapphire workpieces. The mechanism of this etch process involves the reaction of the sapphire (Al 2 O 3 ) surface with sulfuric acid (H 2 SO 4 ) forming aluminum sulfate [Al2(SO4)3], which has low solubility. The high phosphoric acid content in the first and second steps of sapphire AMP results in the efficient conversion of Al 2 (SO 4 ) 3 to aluminum phosphate (AlPO 4 ), which is very soluble, greatly reducing reaction product redeposition on the workpiece surface. Sapphire AMP is shown to expose sub-surface mechanical damage on the sapphire surface created during the grinding and polishing processes, whose etched morphology has either isotropic or anisotropic evolution depending on the nature of the initial surface damage. Sapphire AMP was also designed to remove the key known surface, laser absorbing precursors (namely, foreign chemical impurities, the fracture surface layer of preexisting sub-surface damage, and reaction product or foreign species redeposition or precipitation). Static and sliding indention induced surface microfractures on sapphire are shown after sapphire AMP to have a significant decrease in the fast photoluminescence intensity (a known metric for measuring the degree of laser damaging absorbing precursors). In addition, the onset of laser damage (at 351 nm 3 ns) on sapphire AMP treated workpieces was shown to increase in fluence from ~ 4 to >9.5J/cm 2 . Finally, biaxial ball-on-ring mechanical tests on sapphire disks showed an increase in the failure stress from 340 MPa (with pre-existing 28 µm flaws) to ~ 900MPa after sapphire AMP, which is attributed to the blunting of the surface microfractures.

36 MATERIALS SCIENCE↗