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At least 19 records

Anisotropic Wet Etching of Si as a Fabrication Tool Enabling 3-D Microphotonics Structures and Devices

It is shown that due to high speed and large volume of production, anisotropic wet etching of Si is a unique method of manufacturing high quality micropyramidal arrays for silicon photonics. Four types of arrays were fabricated: (i) square pyramids with the 54.7 slope of the sidewall surface, (ii) microcones with the 45 slope of sidewall surface, (iii) inverted square pyramids with 54.7 slope, and (iv) inverted triangular pyramids with different angles of the sidewalls. It is shown that the first type of arrays has a capability to produce tightly focused mid-wave infrared (MWIR) beams at the tips of the pyramids. Other arrays can be also used as light concentrators and various multifunctional microphotonic components.

Astratov, Vasily N.↗

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↗

Wet-Etching of Acoustically Spalled GaAs for Substrate Reuse

Acoustic spalling is a promising technique for substrate reuse in the fabrication of gallium arsenide (GaAs) photovoltaic cells. However, the acoustic spalling process can leave the substrate with areas of rough surface morphology that can interfere with subsequent cell growth and processing. In this work, we investigate the use of wet etchants to smooth the surface of acoustically spalled GaAs substrates. We evaluated six different etchants. Of those tested, an 8:1:1 mixture of sulfuric acid, hydrogen peroxide, and water at 30 degrees C and a moderate stirring rate showed the greatest roughness reduction per mass loss while producing the desired morphology. This etchant was then applied to an acoustically spalled 2-inch GaAs wafer. A single-junction GaAs cell was then grown via metalorganic vapor-phase epitaxy on this substrate, an acoustic spalled substrate without a smoothing etch, and an epi-ready substrate. Use of the 8:1:1 H2SO4:H2O2:H2O etchant produced cells an average efficiency of 12.8% as compared to that of 2.0% grown on the unetched acoustically spalled substrate and 16.3% grown on the epi-ready substrate. The results of this work demonstrate that wet etching is a viable method for smoothing the surface of spalled GaAs substrates, paving the way for substrate reuse via acoustic spalling at efficiencies that approach growth on epi-ready substrates.

etching↗

Deep photoenhanced wet material etching using high-power ultraviolet light emitting diodes

Methods and systems for etching a substrate using photoenhanced wet etching techniques are described. At least one light emitting diode source is used to create a high intensity of ultraviolet light at the surface of the substrate or at one or more layers formed on the substrate. Etching rates in GaN substrates and GaN layers are improved by an order of magnitude over conventional systems. Systems and methods for forming a device structure free of a substrate are described. The device structure is grown or applied over a release layer on a substrate. The device structure is exposed to photoenhanced wet etch environments to vertically and laterally etch the release layer to separate the device structure from the substrate.

36 MATERIALS SCIENCE↗

Wet-chemical etching of FIB lift-out TEM lamellae for damage-free analysis of 3-D nanostructures

Reducing ion beam damage from the focused ion beam (FIB) during fabrication of cross sections is a well-known challenge for materials characterization, especially cross sectional characterization of nanostructures. To address this, a new method has been developed for cross section fabrication enabling high resolution transmission electron microscopy (TEM) analysis of 3-D nanostructures free of surrounding material and free of damage detectable by TEM analysis. Before FIB processing, nanopillars are encapsulated in a sacrificial oxide which acts as a protective layer during FIB milling. Furthermore, the cross sectional TEM lamella containing the nanopillars is then mounted and thinned with some modifications to conventional FIB sample preparation that provide stability for the lamella during the following wet-chemical dip etch. The wet-chemical etch of the TEM lamella removes the sacrificial oxide layer, freeing the nanopillars from any material that would obscure TEM imaging. Both high resolution TEM and aberration corrected scanning TEM images of Si/SiGe pillars with diameters down to 30 nm demonstrate the successful application of this approach.

3-d nanostructure analysis↗

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↗

Electrochemical Method of Making Porous Particles Using a Constant Current Density

Provided is a particle that includes a first porous region and a second porous region that differs from the first porous region. Also provided is a particle that has a wet etched porous region and that does have a nucleation layer associated with wet etching. Methods of making porous particles are also provided.

Ferrari, Mauro↗

Evaluation and mitigation of trace 210Pb contamination on copper surfaces

Clean materials are required to construct and operate many low-background physics experiments. High-purity copper has found broad use because of its physical properties and availability. In this paper, we describe methods to assay and mitigate Pb-210 contamination on copper surfaces, such as from exposure to environmental radon or coming from bulk impurities. We evaluated the efficacy of wet etching on commercial samples and observed that Po-210 contamination from the copper bulk does not readily pass into solution. During the etch, the polonium appears to trap at the copper-etchant boundary, such that it is effectively concentrated at the copper surface. We observed a different behavior for Pb-210; high-sensitivity measurements of the alpha emissivity versus time indicate the lowest level of Pb-210 contamination ever reported for a commercial copper surface: 0 +/- 12 nBq/cm2 (1-sigma). Additionally, we have demonstrated the effectiveness of mitigating trace Pb-210 and Po-210 surface backgrounds using custom, high-purity electroplating techniques. These approaches were evaluated utilizing assays performed with an XIA UltraLo-1800 alpha spectrometer.

radon, copper, copper cleaning, dark matter, Pb-21↗

Selective Plasma Deposition of Fluorocarbon Films on SAMs

A dry plasma process has been demonstrated to be useful for the selective modification of self-assembled monolayers (SAMs) of alkanethiolates. These SAMs are used, during the fabrication of semiconductor electronic devices, as etch masks on gold layers that are destined to be patterned and incorporated into the devices. The selective modification involves the formation of fluorocarbon films that render the SAMs more effective in protecting the masked areas of the gold against etching by a potassium iodide (KI) solution. This modification can be utilized, not only in the fabrication of single electronic devices but also in the fabrication of integrated circuits, microelectromechanical systems, and circuit boards. In the steps that precede the dry plasma process, a silicon mold in the desired pattern is fabricated by standard photolithographic techniques. A stamp is then made by casting polydimethylsiloxane (commonly known as silicone rubber) in the mold. The stamp is coated with an alkanethiol solution, then the stamp is pressed on the gold layer of a device to be fabricated in order to deposit the alkanethiol to form an alkanethiolate SAM in the desired pattern (see figure). Next, the workpiece is exposed to a radio-frequency plasma generated from a mixture of CF4 and H2 gases. After this plasma treatment, the SAM is found to be modified, while the exposed areas of gold remain unchanged. This dry plasma process offers the potential for forming masks superior to those formed in a prior wet etching process. Among the advantages over the wet etching process are greater selectivity, fewer pin holes in the masks, and less nonuniformity of the masks. The fluorocarbon films formed in this way may also be useful as intermediate layers for subsequent fabrication steps and as dielectric layers to be incorporated into finished products.

Crain, Mark M., III↗

Precise wet-chemical etching

Controlled amount of etchant applied to surface of rotating sample removes only few angstroms of material. Technique is suited to study of chemical and crystal structures. Rate can be varied through control of spin frequency, liquid viscosity, droplet size, total etchant volume, etchant concentration.

Grunthaner, F. J.↗

Investigation of etching techniques for superconductive Nb/Al-Al2O3/Nb fabrication processes

Wet etching, CF4 and SF6 reactive ion etching (RIE), RIE/wet hybrid etching, Cl-based RIE, ion milling, and liftoff techniques have been investigated for use in superconductive Nb/Al-Al2O3/Nb fabrication processes. High-quality superconductor-insulator-superconductor (SIS) junctions have been fabricated using a variety of these etching methods; however, each technique offers distinct tradeoffs for a given process an wafer design. In particular, it was shown that SF6 provides an excellent RIE chemistry for low-voltage anisotropic etching of Nb with high selectivity to Al. The SF6 tool has greatly improved the trilevel resist junction insulation process. Excellent repeatability, selectivity with respect to quartz, and submicron resolution make Cl2 + BCl3 + CHCl3 RIE a very attractive process for trilayer patterning.

Lichtenberger, A. W.↗

Effect of fabrication processes on BaTiO 3 capacitor properties

There is an increasing desire to utilize complex functional electronic materials such as ferroelectrics in next-generation microelectronics. As new materials are considered or introduced in this capacity, an understanding of how we can process these materials into those devices must be developed. Here, the effect of different fabrication processes on the ferroelectric and related properties of prototypical metal oxide (SrRuO 3 )/ferroelectric (BaTiO 3 )/metal oxide (SrRuO 3 ) heterostructures is explored. Two different types of etching processes are studied, namely, wet etching of the top SrRuO 3 using a NaIO 4 solution and dry etching using an Ar + -ion beam (i.e., ion milling). Polarization-electric-field hysteresis loops for capacitors produced using both methods are compared. For the ion-milling process, it is found that the Ar + beam can introduce defects into the SrRuO 3 /BaTiO 3 /SrRuO 3 devices and that the milling depth strongly influences the defect level and can induce a voltage imprint on the function. Realizing that such processing approaches may be necessary, work is performed to ameliorate the imprint of the hysteresis loops via ex situ “healing” of the process-induced defects by annealing the ferroelectric material in a barium-and-oxygen-rich environment via a chemical-vapor-deposition-style process. This work provides a pathway for the nanoscale fabrication of these candidate materials for next-generation memory and logic applications.

36 MATERIALS SCIENCE↗

A Dry-Etch Process for Low Temperature Superconducting Transition Edge Sensors for Far Infrared Bolometer Arrays

The next generation of ultra-low power bolometer arrays, with applications in far infrared imaging, spectroscopy and polarimetry, utilizes a superconducting bilayer as the sensing element to enable SQUID multiplexed readout. Superconducting transition edge sensors (TES s) are being produced with dual metal systems of superconductinghormal bilayers. The transition temperature (Tc) is tuned by altering the relative thickness of the superconductor with respect to the normal layer. We are currently investigating MoAu and MoCu bilayers. We have developed a dry-etching process for MoAu TES s with integrated molybdenum leads, and are working on adapting the process to MoCu. Dry etching has the advantage over wet etching in the MoAu system in that one can achieve a high degree of selectivity, greater than 10, using argon ME, or argon ion milling, for patterning gold on molybdenum. Molybdenum leads are subsequently patterned using fluorine plasma.. The dry-etch technique results in a smooth, featureless TES with sharp sidewalls, no undercutting of the Mo beneath the normal metal, and Mo leads with high critical current. The effects of individual processing parameters on the characteristics of the transition will be reported.

Allen, Christine A.↗

Vertical Etching of Scandium Aluminum Nitride Thin Films Using TMAH Solution

A wide bandgap, an enhanced piezoelectric coefficient, and low dielectric permittivity are some of the outstanding properties that have made Sc x Al 1-x N a promising material in numerous MEMS and optoelectronics applications. One of the substantial challenges of fabricating Sc x Al 1-x N devices is its difficulty in etching, specifically with higher scandium concentration. In this work, we have developed an experimental approach with high temperature annealing followed by a wet etching process using tetramethyl ammonium hydroxide (TMAH), which maintains etching uniformity across various Sc compositions. The experimental results of etching approximately 730 nm of Sc x Al 1-x N (x = 0.125, 0.20, 0.40) thin films show that the etch rate decreases with increasing scandium content. Nevertheless, sidewall verticality of 85°~90° (±0.2°) was maintained for all Sc compositions. Based on these experimental outcomes, it is anticipated that this etching procedure will be advantageous in the fabrication of acoustic, photonic, and piezoelectric devices.

36 MATERIALS SCIENCE↗