Wet Etching Research Articles

Stoichiometrically Optimized Electrochromic Complex [V2O2+ξ(OH)3-ξ] Based Electrode: Prototype Supercapacitor with Multicolor Indicator.

The systematic structure modification of metal oxides is becoming more attractive, and effective strategies for structural tunning are highly desirable for improving their practical color-modulating energy storage performances. Here, the ability of a stoichiometrically tuned oxide-hydroxide complex of porous vanadium oxide, namely [V2O2+ξ(OH)3-ξ]ξ = 0:3 for multifunctional electrochromic supercapacitor application is demonstrated. Theoretically, the pre-optimized oxide complex is synthesized using a simple wet chemical etching technique in its optimized stoichiometry [V2O2+ξ(OH)3-ξ] with ξ=0, providing more electroactive surface sites. The multifunctional electrode shows a high charge storage property of 610Fg-1 at 1Ag-1, as well as good electrochromic properties with high color contrast of 70% and 50% at 428 and 640nm wavelengths, faster switching, and high coloration efficiency. When assembled in a solid-state symmetric electrochromic supercapacitor device, it exhibits an ultrahigh power density of 1066mWcm-2, high energy density of 246mWhcm-2, and high specific capacitance of 290mFcm-2 at 0.2mAcm-2. A prepared prototype device displays red when fully charged, green when half charged, and blue when fully discharged. A clear evidence of optimizing the multifunctional performance of electrochromic supercapacitor by stoichiometrical tuning is presented along with demonstrating a device prototype of a 25cm2 large device for real-life applications.

Origin of the High Density of Oxygen Vacancies at the Back Channel of Back-Channel-Etched a-InGaZnO Thin-Film Transistors.

This study reveals the pronounced density of oxygen vacancies (Vo) at the back channel of back-channel-etched (BCE) a-InGaZnO (a-IGZO) thin-film transistors (TFTs) results from the sputtered deposition rather than the wet etching process of the source/drain metal, and they are distributed within approximately 25 nm of the back surface. Furthermore, the existence and distribution depth of the high density of Vo defects are verified by means of XPS spectra analyses. Then, the mechanism through which the above Vo defects lead to the instability of BCE a-IGZO TFTs is elucidated. Lastly, it is demonstrated that the device instability under high-humidity conditions and negative bias temperature illumination stress can be effectively alleviated by etching and thus removing the surface layer of the back channel, which contains the high density of Vo defects. In addition, this etch method does not cause a significant deterioration in the uniformity of electrical characteristics and is quite convenient to implement in practical fabrication processes. Thus, a novel and effective solution to the device instability of BCE a-IGZO TFTs is provided.

Polymer Additives Promoted Texturization on Monocrystalline Silicon for Solar Cell

The solar photovoltaic was well recognized as one of the major constituent parts in future green energy system to achieving carbon neutrality. Among various technological routes to improve photoelectric conversion efficiency, rational surface texturization on monocrystalline silicon is one of the most crucial and fundamental processing steps, so as to well control the micro/nano surface structure and obtain lower light reflectivity. Chemical wet etching was the current mainstream technology in photovoltaic industry, yet there is an urgent need to update green, efficient, customized texturization additives to meet the industrial demand. This minireview summarizes the history, key breakthrough and recent advance in texturization additives based on organic and polymer molecules as crucial chemicals, and provides perspective to development directions of future texturization additives.

A 3-D GaAs-based Hall sensor design with dual active layers structure

A fully integrated 3-D Hall magnetic sensor with dual active structure was proposed. Results by technology computer-aided design simulation show that the proposed sensor provides a doubled magnitude improvement in sensitivity of vertical magnetic field direction and maintains a good level sensing of horizontal magnetic field direction compared with the sensor with single active layer. The designed sensor was fabricated by wet etching process and a method of preparing Ohmic contacts on the "pseudo-sidewalls" is proposed. The measurements show that the non-linearity does not exceed 0.5% and a voltage sensitivity of up to 0.046 T−1, which matches the simulation results. The proposed sensor boasts a simplified structure that allows for fabrication using different layers only through a planar process, which makes it more conducive to the integration of devices and systems.

Performance improvement of vapor compression heat pump with superhydrophobic finned-tube evaporator

Residential buildings frequently employ vapor compression heat pump for winter heating. Its advantages over electric and coal-fired heating include great energy effectiveness and low emissions. However, the outside evaporator's frosting negatively impacts the performance of heat pump systems in low-temperature and high-humidity environments. To ameliorate the frosting problem, a finned-tube heat exchanger with superhydrophobic surface wettability prepared by the wet chemical etching method was applied to a vapor compression heat pump in this study. The performance of a commercial evaporator unit and the superhydrophobic evaporator unit under five frosting conditions was investigated through experiments. The maximum heat transfer rate of the superhydrophobic heat exchanger unit was increased by 17%–44% compared with that of the commercial unit. The COP improvement of the superhydrophobic unit reached 11.2%, 14.3%, 18.8%, 20.9% and 31.9%, respectively. The total mass of frost formation of the superhydrophobic unit experienced a 59.2%–76.3% decrease. The operation time of the superhydrophobic evaporator unit before defrosting determination was significantly extended, reducing the number of defrosting times during a long-time operation. This study proves the advantages of superhydrophobic finned-tube evaporators used in heat pumps in terms of heat transfer performance and frost suppression performance, promoting the application of superhydrophobic finned-tube evaporators in heat pump air-conditioning systems.

Improvement of electrical characteristics and wet etching procedures for InGaTiO electrodes in organic light-emitting diodes through hydrogen doping

We investigated the effect of hydrogen doping on characteristics of InGaTiO (IGTO) electrode with high conductivity and transmittance during sputtering process. After hydrogen doping, the 300 nm-thick IGTO:H electrode showed lower sheet resistance of 13.79 Ω/square compared to sheet resistance (69.2 Ω/square) of pure IGTO electrode without change of optical transmittance. In addition, wet etching reaction rate of IGTO:H electrode for patterning process was significantly accelerated after hydrogen doping. Possible explanation for hydrogen doping effect on electrical properties and wet etching process of the IGTO:H electrode was suggested. The doped hydrogen influenced the electrical characteristics through the passivation of dangling bonds and oxygen vacancies. Moreover, it significantly impacts crystalline structure, consequently altering the etching rate. Using patterned IGTO:H electrodes, we fabricated red organic light emitting diodes (OLEDs) to show feasibility of the IGTO:H electrodes. External quantum efficiency and current efficiency of the red OLED with IGTO:H (10%) were higher than IGTO electrode without hydrogen doping, indicating that hydrogen doping is an effective method to improve the film properties and IGTO:H electrode can serve as a prospective transparent anode for both flexible and rigid OLEDs.

Analytical study of KOH wet etch surface passivation for III-nitride micropillars

III-Nitride micropillar structures show great promise for applications in micro light-emitting diodes and vertical power transistors due to their excellent scalability and outstanding electrical properties. Typically, III-Nitride micropillars are fabricated through a top-down approach using reactive ion etch which leads to roughened, nonvertical sidewalls that results in significant performance degradation. Thus, it isessential to remove this plasma etch induced surface damage. Here, we show that potassium hydroxide(KOH) acts as a crystallographic etchant for III-Nitride micropillars, preferentially exposing the vertical m-plane, and effectively removing dry etch damage and reducing the structure diameter at up to 36.6nm/min. Both KOH solution temperature and concentration have a dramatic effect on this wet etch progression. We found that a solution of 20% AZ400K (2% KOH) at 90°C is effective at producingsmooth, highly vertical sidewalls with RMS surface roughness as low as 2.59nm, ideal for high-performance electronic and optoelectronic devices.

Room temperature electrical characteristics of gold-hyperdoped silicon

Hyperdoped silicon is a promising material for near-infrared light detection, but to date, the device efficiency has been limited. To optimize photodetectors based on this material that operate at room temperature, we present a detailed study on the electrical nature of gold-hyperdoped silicon formed via ion implantation and pulsed-laser melting (PLM). After PLM processing, oxygen-rich and gold-rich surface layers were identified and a wet etch process was developed to remove them. Resistivity and Hall effect measurements were performed at various stages of device processing. The underlying gold-hyperdoped silicon was found to be semi-insulating, regardless of whether the surface gold was removed by etching or not. We propose a Fermi level pinning model to describe the band bending of the transformed surface layer and propose a promising device architecture for efficient Au-hyperdoped Si photodetectors.

Improvement of light extraction efficiency in AlGaInP-based vertical miniaturized-light-emitting diodes via surface texturing.

AlGaInP-based light-emitting diodes (LEDs) suffer from a low external quantum efficiency (EQE), which is mainly restrained by the poor light extraction efficiency. Here, we demonstrate AlGaInP-based vertical miniaturized-LEDs (mini-LEDs) with a porous n-AlGaInP surface using a wet etching process to boost light extraction. We investigated the effects of etching time on the surface morphology of the porous n-AlGaInP surface. We found that as the etching time is prolonged, the density of pores increases initially and decreases subsequently. In comparison with the vertical mini-LED with a smooth n-AlGaInP surface, the vertical mini-LEDs with the porous n-AlGaInP surface reveal improvement in light output power and EQE, meanwhile, without the deterioration of electrical performance. The highest improvement of 38.9% in EQE measured at 20 mA is observed from the vertical mini-LED with the maximum density of the pores. Utilizing a three-dimensional finite-difference time-domain method, we reveal the underlying mechanisms of improved performance, which are associated with suppressed total internal reflection and efficient light scattering effect of the pores.

Composite photonic microobjects with anisotropic photonic properties from a controlled wet etching approach

Colloidal photonic microobjects with anisotropic properties find diverse applications, from building blocks of tunable displays to miniaturized optoelectronic devices. Microfluidics is a robust platform for the construction of colloidal photonic microobjects. Generally, creating colloidal photonic microobjects with Janus structures via microfluidics involves either injecting different colloidal photonic streams to form Janus photonic microbjects or applying a selective coating of a metallic layer to one side of the as-prepared photonic microobjects. However, those approaches either are time-consuming or may pose negative impact on the photonic properties of the photonic microobjects. In this report, we introduce a facile yet highly reproducible approach to fabricate photonic microobjects with Janus photonic property. To achieve this, colloidal photonic microspheres that are composed of a photonic resin dispersion of single-sized SiO2 nanoparticles (NPs) are prepared via a single emulsion-based microfluidics. Subsequently, one hemisphere of each microsphere is embedded into a polystyrene (PS) film, serving as a protection matrix. The microspheres embedded PS film is overturned and placed in a controlled amount of HF solution to etch the SiO2 NPs in the unprotected domain, yielding Janus photonic microobjects. The ratio of opal to inverse-opal structure on the surface of the photonic microobjects can be accurately controlled by playing the etching parameters. The porous structure of the etched part of the microobjects can be further functionalized by polymer infiltration, featuring the microobjects with fluorescence property. These multifunctionalized microobjects may find potential applications in the fields of advanced pigments, anticounterfeiting materials, etc. This strategy paves a facile way for the design and construction other miniaturized devices.

Topological signatures of Mo2TiC2O2

Mo2TiC2 is the Ordered Double Transitional Metal Layered Carbides (ODTMLC) derived from its parent MAX phases Mo2TiAlC2 by a wet chemical etching. Its oxidation was done by a new ablated plasma thrust method in which the MXenes were at 750 °C under an oxygen background in the pulsed laser deposition chamber. The reflective high electron energy diffraction technique assures the oxidation at the ambient gas pressure p = 0.1 mbar, which was described in the previous paper. The obtained Mo2TiC2O2 was transferred for their topological test under angle-resolved photoemission spectroscopy, circular dichroism test, and Chemical Potential (CP) analysis. An indirect energy bandgap of 125 meV was obtained. The sine function of α along with period π and β with period 2π shows that there is a possibility of helical spin textures in both α (electron-like pocket around Γ̄) and β (elliptical electron-like pocket around M̄). The CP analysis shows the possibility of at least 100 meV bandgap creation on a single surface so that the surface charges will flow without any effect of bulk. The Mo2TiC2O2 can be used as topological insulating material.

Exploring mc‐Silicon Wafers: Utilizing Machine Learning to Enhance Wafer Quality Through Etching Studies

AbstractThis paper provides a method for improving the photovoltaic conversion efficiency and optical attributes of silicon solar cells manufactured from as‐cut boron doped p‐type multi‐crystalline silicon wafers using acid‐based chemical texturization via machine learning. A decreased reflectance, which can be attained by the right chemical etching conditions, is one of the key elements for raising solar cell efficiency. In this work, the mc‐Silicon wafer surface reflectance is obtained under (<2%) after optimization of wet chemical etching. The HF + HNO3 + CH3COOH chemical etchant is used in the ratio 1:3:2 at different conditions of the etching duration of 1 min, 2 min, 3 min, and 4 min, respectively. The as‐cut boron doped p‐type mc‐silicon wafers are analysed with ultraviolet–visible spectroscopy, optical microscopy, Fourier transforms infrared spectroscopy, thickness profilometer, and scanning electron microscopy before and after etching. The chemical etching solution produces good results in 3 min etched wafer, with a reflectivity value of <2%.The reflectivity and optical images are inputs to the convolutional neural network model and the linear regression model to obtain the etching rate for better reflectivity. The classification model provides 99.6% accuracy and the regression model results in the minimum mean squared error (MSE) of 0.062.

High-Power Mid-Infrared Quantum Cascade Laser with Large Emitter Width

High-power quantum cascade lasers (QCLs) have a wide application prospect. In this paper, a high-power high-beam-quality device with a large ridge width is demonstrated. The effect of different ridge widths on mode loss was studied, and the results showed that the mode loss decreased as the ridge width increased. Furthermore, as the width of the ridge increased, the temperature of the active region rose. In the experiment, the wafers were grown by metal–organic chemical vapor deposition (MOCVD), and the ridge width of the device was controlled by wet etching. A laser with a ridge width of 15 µm and a length of 5 mm achieved an output of 2.2 W under 288 K continuous wave (CW) operation, with a maximum slow-axis divergence angle of 27.2° and a device wavelength of 5 μm. The research results of this article promote the industrial production of base transverse mode QCL.

Research on the mitigation of redeposition defects on the fused silica surface during wet etching process.

The laser-induced damage of ultraviolet fused silica optics is a critical factor that limits the performance enhancement of high-power laser facility. Currently, wet etching technology based on hydrofluoric acid (HF) can effectively eliminate absorbing impurities and subsurface defects, thereby significantly enhancing the damage resistance of fused silica optics. However, with an increase in the operating fluence, the redeposition defects generated during wet etching gradually become the primary bottleneck that restricts its performance improvement. The composition and morphology of redeposition defects were initially identified in this study, followed by an elucidation of their formation mechanism. A mitigation strategy was then proposed, which combines a reduction in the generation of precipitation with an acceleration of the precipitation dissolution process. Additionally, we systematically investigated the influence of various process parameters such as extrinsic impurity, etching depth, and megasonic excitation on the mitigation of deposition defects. Furthermore, a novel multiple-step dynamic etching method was developed. Through comprehensive characterization techniques, it has been confirmed that this new etching process not only effectively mitigate redeposition defects under low fluence conditions but also exhibits significant inhibition effects on high fluence precursors. Consequently, it significantly enhances the laser damage resistance performance of fused silica optics.

Post-trench restoration for vertical GaN power devices

The impact of the post-trench restoration on the electrical characteristics of vertical GaN power devices is systematically investigated in this work. Following the achievement of microtrench-free GaN trench structure with modified dry etching conditions, the post-trench tetramethylammonium hydroxide (TMAH)-based wet etching and UV/Ozone-based oxidation process are employed to further refine the trench profile. It is shown that the c-plane trench bottom is restored to the level of unetched surface, as evidenced by the improved Schottky interface. Additionally, the post-trench treatment exhibits the anisotropic characteristics with the preferred rounded corner profile on m-plane sidewall compared to a-plane sidewall. The simulations and experimental results demonstrate that the trench MOS barrier Schottky (TMBS) rectifier based on m-plane sidewall could suppress the electric field crowding at the trench corner and, hence, reduce the reverse leakage current by 1–2 orders of magnitude. Furthermore, the MOSCAP test structures were fabricated on the trenches. The extracted interface trap density (Dit) confirms the effective restoration of trench bottom. However, the sidewall surface exhibits the relatively large Dit, which emphasizes the necessity of optimizing the sidewall, particularly for devices incorporating sidewall channel. The demonstrated post-trench restoration technique improves the surface quality and trench structure for the significantly enhanced electrical performances, which is essential for the development of vertical GaN power devices.

An innovative methodology for monitoring the sacrificial layer removal process in MEMS structures

The sacrificial layer is a key component for the fabrication of a released structure in the MEMS sensors and actuators. Wet etching is a practical microfabrication process that minimizes costs compared to dry etching. Since the sacrificial layer exists between the structural layer and the substrate, characterization of the etching process is unavailable to observe and evaluate directly. This research, for the first time, presents a methodology for monitoring sacrificial layer removal. It takes advantage of using a transparent substrate (during process development) to observe the removal process from the backside. This method can be used as a separate test during surface micromachining to monitor and optimize the release process of the MEMS device. To evaluate the efficiency of the method, the copper sacrificial layer was selected. The removal process was investigated for typical structures used in MEMS sensors and actuators including the etch-holes, the cantilever beams, comb fingers, and the pads. The experimental test showed the removal of the sacrificial layer, the non-uniformity of the etching, and all the veritable chemical reactions and phenomena under the structural layer. In addition, the etch-rate were obtained in the order of 0.35–5.5 μm min−1 for various structural features. The procedure developed in this research is an approach to the process monitoring of the sacrificial layer removal. Therefore, it can be used to organize the quality control in the released structures of MEMS and optimization in batch processing. This method can be adopted for non-metallic sacrificial layers and dry etching as well.

Novel Approach to Color‐Neutral Transparent Solar Cells: An Organic‐Si Hybrid Achieved by Laser Microhole Drilling

AbstractTransparent solar cells (TSCs) hold promise for applications in building‐integrated photovoltaics (BIPVs) and vehicles. However, existing TSCs often have compromised color neutrality and efficiency because of the distinctive colors arising from their photoactive materials. The study proposes a novel fabrication method for TSCs based on Si wafers with the average visible transmittance (AVT) controlled by creating a microhole pattern through a combination of nanosecond laser drilling and subsequent wet etching. Through this ambient‐air process, organic–Si hybrid TSCs are successfully realized by integrating an organic PEDOT:PSS layer onto this structure with a neutral color. The power conversion efficiency (PCE) is adjusted by the fraction of the perforated region, and it attained 6.20% at 30% AVT, 5.37% at 40% AVT, and 4.67% at 50% AVT. In this hybrid TSC approach, the CIE color coordinates are closely aligned with the neutral‐color points (0, 0), resulting in color rendering index (CRI) values exceeding 99. The strategy represents a significant step toward the development of efficient color‐neutral TSCs for transparent solar applications.

Water collection and transportation on superhydrophilic/superhydrophobic bioinspired heterogeneous wettability surface

In recent years, the ability of superhydrophilic/superhydrophobic bioinspired heterogeneous wettability (SSBHW) surfaces to collect freshwater has gained significant attention due to their potential to mitigate water scarcity. Inspired by nature’s creatures, this paper presents an SSBHW surface that can efficiently collect freshwater resources from the atmosphere, drawing inspiration from cactus needles and spider silk spindles. The superhydrophobic (SHO) surface was prepared by wet etching and low surface energy modification on copper surface. Based on the SHO surface, the superhydrophilic (SHI) patterns consisting of spindle-shaped and wedge-shaped were constructed by laser ablation. The prepared SHI pattern was not only trapped airborne droplets but also enabled the directional transport of droplets. To enhance the efficiency of water collection, the smaller spindle-shaped pattern spacing in the SHO region was designed, which help to transport the condensed water quickly towards the SHI region because of the surface energy gradient force. The synergistic effect between the advantages offered by the SHO and SHI surfaces results in a significant improvement in water collection efficiency. The water collection efficiency of the SSBHW surface is 870 mg cm−2 h−1, which is 3.32 and 2.2 times higher than that of the SHI and SHO surfaces, respectively. In addition, the mechanism of enhancement of the moisture harvesting behavior of inhomogeneous wettable surfaces was analyzed. This work provides a new strategy for the study of catchment surfaces, making it an effective solution for obtaining fresh water resources in arid regions.

Sound-Based Depth Estimation of Glass Microchannel in Laser-Induced Backside Wet Etching Using Wavelet Transform

Laser-induced backside wet etching (LIBWE) has been proposed to fabricate high-quality micromachined components on transparent materials. However, the process is limited by poor repeatability when fabricating high-aspect-ratio structures, even under the same conditions due to uncertainties arising from the thermal process and the complex mechanisms associated with the indirect irradiation of the etching process. Such errors could lead to redundant trials and wastages when trying to achieve the desired dimension. To identify the factors causing these variations, we targeted the process sounds generated during the etching. This study uses a microphone to measure factors that result in variations in material removal quantity during the etching process under the same conditions. The sound was filtered at frequencies between 3 and 6 kHz, which were selected as characteristic frequencies for the process under various laser conditions. By integrating the root mean squared value of the detail coefficient of the wavelet transform, the depth estimation closely matched the measured depth of the fabricated part. This finding suggests that determining the etching rate from sound at a certain characteristic frequency during the LIBWE process is feasible; this approach can improve the accuracy and repeatability of the process. Based on this estimation mechanism, we designed a closed-loop feedback control system capable of fabricating highly accurate microchannels in the range of 80–120 μm with a maximum error of 5.6%.

Single femtosecond pulse writing of a bifocal lens.

In this Letter, a method for the fabrication of bifocal lenses is presented by combining surface ablation and bulk modification in a single laser exposure followed by the wet etching processing step. The intensity of a single femtosecond laser pulse was modulated axially into two foci with a designed computer-generated hologram (CGH). Such pulse simultaneously induced an ablation region on the surface and a modified volume inside the fused silica. After etching in hydrofluoric acid (HF), the two exposed regions evolved into a bifocal lens. The area ratio (diameter) of the two lenses can be flexibly adjusted via control of the pulse energy distribution through the CGH. Besides, bifocal lenses with a center offset as well as convex lenses were obtained by a replication technique. This method simplifies the fabrication of micro-optical elements and opens a highly efficient and simple pathway for complex optical surfaces and integrated imaging systems.