Reactive Etching Research Articles

High on-chip gain spiral Al2O3:Er3+ waveguide amplifiers

We demonstrate reactively sputtered Al2O3:Er3+ waveguide amplifiers with an erbium concentration of 3.9 × 1020 ions/cm3, capable of achieving over 30 dB small signal net gain at 1532 nm using bidirectional pumping at 1480 nm. We observe on chip output powers of 10.2-13.6 dBm of amplified signal power at 1532 nm for a 12.9 cm waveguide amplifier considering -25.4 dB of lumped coupling losses per facet. Annealing was used to improve the performance of the devices, which were patterned using electron beam lithography and reactive ion etching. This result, to our knowledge, represents record breaking on-chip internal net gain for Al2O3:Er3+ waveguide amplifiers, which show promise over other technologies due to wafer scalability and promise of easy monolithic integration with other material platforms to support a wide variety of applications.

Wet and dry etching of ultrawide bandgap LiGa5O8 and LiGaO2

Crystalline thin films of LiGa5O8 have recently been realized through epitaxial growth via mist-chemical vapor deposition. The single crystal, spinel cubic LiGa5O8 films show promising fundamental material properties and, therefore, make LiGa5O8 a potential enabling material for power electronics. In this work, chemical resistance and etch susceptibility were investigated for the first time on crystalline LiGa5O8 thin films with various wet chemistries. It was found that LiGa5O8 is very chemically resistive to acid solutions, with no apparent etching effects observed when placed in concentrated acid solutions of HCl, H2SO4, HF, or H3PO4 at room temperature. In contrast, orthorhombic (010) LiGaO2 shows effective etching in HCl solutions at varying dilution concentrations, with etch rates measured between 8.6 [1000:1 (DI water: HCl concentration)] and 6092 nm/min (37 wt. % HCl). The inductively coupled plasma reactive ion etching (ICP-RIE) of LiGa5O8 using BCl3/Ar and CF4/Ar/O2 gas chemistries was investigated. The etching rate and surface morphology of etched surfaces were examined as a function of RIE and ICP power. Using a CF4/Ar/O2 gas chemistry with an RIE power of 75 W and an ICP power of 300 W resulted in smooth etched planar surfaces while maintaining an etch rate of ∼24.6 nm/min. Similar dry etching studies were performed for LiGaO2. It was found that the BCl3/Ar gas chemistry was better suited for LiGaO2 etching, with similar surface morphology quality being obtained after etching as prior etching when a RIE power of 15 W and an ICP power of 400 W is utilized.

Spectral stability of V2 centres in sub-micron 4H-SiC membranes

Colour centres in silicon carbide emerge as a promising semiconductor quantum technology platform with excellent spin-optical coherences. However, recent efforts towards maximising the photonic efficiency via integration into nanophotonic structures proved to be challenging due to reduced spectral stabilities. Here, we provide a large-scale systematic investigation on silicon vacancy centres in thin silicon carbide membranes with thicknesses down to 0.25 μm. Our membrane fabrication process involves a combination of chemical mechanical polishing, reactive ion etching, and subsequent annealing. This leads to highly reproducible membranes with roughness values of 3–4 Å, as well as negligible surface fluorescence. We find that silicon vacancy centres show close-to lifetime limited optical linewidths with almost no signs of spectral wandering down to membrane thicknesses of ~0.7 μm. For silicon vacancy centres in thinner membranes down to 0.25 μm, we observe spectral wandering, however, optical linewidths remain below 200 MHz, which is compatible with spin-selective excitation schemes. Our work clearly shows that silicon vacancy centres can be integrated into sub-micron silicon carbide membranes, which opens the avenue towards obtaining the necessary improvements in photon extraction efficiency based on nanophotonic structuring.

Plasma‐Damage Free Efficiency Scaling of Micro‐LEDs by Metal‐Assisted Chemical Etching

AbstractSince its inception, LEDs have slowly transitioned from traditional solid‐state lighting applications to full‐color, self‐emissive displays. Micro‐LEDs (µLEDs) are poised to become the next mass‐market technology for displays in lower pixel‐density, large‐area and mobile devices alongside emerging applications for high pixel‐density augmented, virtual and mixed reality. However, it is well known that µLEDs suffer from efficiency cliff – a drastic efficiency reduction as device dimension reduces with increased severity at the single digit micron scale, often attributed to material damage from reactive ion etching (RIE) that is fundamental to the process. In this paper, a first‐ever demonstration of µLED devices ranging from 45 µm down to 5 µm fabricated by the plasma‐free metal‐assisted chemical etching (MacEtch) is presented. These devices demonstrate converging external quantum efficiencies (EQE) irrespective of mesa dimension with a spread of only 3.7% without optimization. Additionally, a multi‐pronged comparison between MacEtch and RIE is provided in terms of smoothness, material damage, macroscale uniformity and throughput. These findings carry profound implications for damage‐free scaling of multi‐heterojunction III‐V optoelectronic devices, providing a pathway for high‐density, high performance top‐down fabricated µLED arrays.

High-performance, large-area flexible SERS substrates prepared by reactive ion etching for molecular detection

In the realm of molecular detection, the surface-enhanced Raman scattering (SERS) technique has garnered increasing attention due to its rapid detection, high sensitivity, and non-destructive characteristics. However, conventional rigid SERS substrates are either costly to fabricate and challenging to prepare over a large area, or they exhibit poor uniformity and repeatability, making them unsuitable for inspecting curved object surfaces. In this work, we present a flexible SERS substrate with high sensitivity as well as good uniformity and repeatability. First, the flexible polydimethylsiloxane (PDMS) substrate is manually formulated and cured. SiO2/Ag layer on the substrate can be obtained in a single process by using ion beam sputtering. Then, reactive ion etching is used to etch the upper SiO2 layer of the film, which directly leads to the desired densely packed nanostructure. Finally, a layer of precious metal is deposited on the densely packed nanostructure by thermal evaporation. In our proposed system, the densely packed nanostructure obtained by etching the SiO2 layer directly determines the SERS ability of the substrate. The bottom layer of silver mirror can reflect the penetrative incident light, the spacer layer of SiO2 and the top layer of silver thin film can further localize the light in the system, which can realize the excellent absorption of Raman laser light, thus enhancing SERS ability. In the tests, the prepared substrates show excellent SERS performance in detecting crystalline violet with a detection limit of 10−11 M. The development of this SERS substrate is anticipated to offer a highly effective and convenient method for molecular substance detection.

Plasma-based etching approach for GEM detector microfabrication at FBK for X-ray polarimetry in space

Gas Electron Multiplier (GEM) detectors are crucial for enabling high-resolution X-ray polarization of astrophysical sources when coupled to custom pixel readout ASIC in Gas Pixel Detectors (GPD), as in the Imaging X-ray Polarimetry Explorer (IXPE), the Polarlight cubesat pathfinder and the PFA telescope onboard the future large enhanced X-ray Timing and Polarimetry (eXTP) Chinese mission. The R&D efforts of the IXPE collaboration have resulted in mature GPD technology. However, limitations in the classical wet-etch or laser-drilled fabrication process of GEMs motivated our exploration of alternative methods. This work focuses on investigating a plasma-based etching approach for fabricating GEM patterns at Fondazione Bruno Kessler (FBK). The objective is to improve the aspect ratio of the GEM holes, to mitigate the charging of the GEM dielectric which generates rate-dependent gain changes. Unlike the traditional wet-etch process, Reactive Ion Etching (RIE) enables more vertical etching profiles and thus better aspect ratios. Moreover, the RIE process promises to overcome non-uniformities in the GEM hole patterns which are believed to cause systemic effects in the azimuthal response of GPDs equipped with either laser-drilled or wet-etch GEMs. We present a GEM geometry with 20 μm in diameter and 50 μm pitch, accompanied by extensive characterization (SEM and PFIB) of the structural features and aspect ratios. The collaboration with INFN Pisa and Turin enabled us to compare the electrical properties of these detectors and test their performance in their use as electron multipliers in GPDs. Although this R&D work is in its initial stages, it holds promise for enhancing the sensitivity of the IXPE mission in X-ray polarimetry measurements through GEM pattern with more vertical hole profiles. The outcomes of this study have the potential to advance the current technological platforms and improve the capabilities of future space-based X-ray polarimetry missions.

Exploiting graded triangular gratings for optimal nano-focusing: A novel approach to enhance SERS efficiency

Plasmonic graded nano-gratings enable rainbow trapping of multiple resonant modes over a wide wavelength spectrum, useful for multi-channel Surface Enhanced Raman Spectroscopy (SERS) of molecular species. However, rectangular nano-gratings have limitations in achieving efficient rainbow trapping and localizing a wide spectrum of plasmonic modes due to their stepwise geometry, which induces high dissipation of surface plasmon polaritons into the substrate. An alternative platform of graded triangular nano-gratings enables increased localization and more efficient adiabatic transformation between neighboring grooves. Varying groove angles, depths, and periods in the tapered geometry allow for smooth adjustment of the surface plasmon polariton propagation constant, reducing losses and maximizing nano-focusing inside the groove tips. To overcome the limitation of low aspect ratio in wet-etching silicon, we employed a multi-step process of reactive ion etching of a SiO2 barrier layer to generate aperture width, followed by anisotropic wet-etching. The resulting graded triangular nano-gratings showed excellent SERS enhancement along three laser wavelength excitations. The enhancement factors of 638 and 785 nm wavelengths are 8.5 × 109 and 9 × 108, respectively, for the detection of 1 µM Rhodamine 6G. In addition, graded triangular nano-gratings show similar enhancement factors for other species, specifically the lipid DPEE-PEG, at the 532 nm laser excitation wavelength with an excellent SERS enhancement factor of 1.5 × 109. Owing to the ability of the graded triangular gratings to elicit pronounced SERS responses across three distinct laser excitations, they unequivocally qualify as “rainbow trapping” structures. Wider apertures, lower ohmic losses, and the ability to tune the groove angle beyond conventional etching methods bode well for graded triangular gratings as a superior platform for miniature sensors.

Multiple fano resonances based on all-dielectric metastructure for refractive index sensing

We investigate an optical refractive index sensor based on an all-dielectric metastructure in the near-infrared regime for achieving high sensitivity and high quality factor (Q-factor). By introducing the asymmetry in the metastructure, four sharp Fano resonances with high Q-factor are generated owing to the transition from symmetry-protected bound states in the continuum (BIC) to quasi-BIC, and the magnetic quadrupole (MQ) resonance, magnetic dipole (MD) resonance, and toroidal dipole (TD) resonance are analyzed by a combination of the field distributions. By evaluating the sensing performance with finite difference time domain (FDTD), the highest Q-factor can reach 6900, the modulation depth is close to 100 %, the sensitivity can reach 288 nm/RIU, and the figure of merit (FOM) is 888 RIU−1. Furthermore, the sensor is prepared using electron beam lithography (EBL), and inductively coupled plasma reactive ion etch (ICP-RIE), and high sensitivity is achieved in liquids with different refractive indices in the near-infrared. The results show a good sensing performance of the designed metastructure. Our findings will give access to the development of applications in non-linear devices, narrow-band filters, optical switches, and quantum nanophotonics.

Performance comparison of InGaN-based 40–80 μm micro-LEDs fabricated with and without plasma etching

The fabrication of InGaN-based blue 4✕4 array micro-LEDs (μLEDs) with 40 μm ✕40 μm chip size and 2✕2 array μLEDs with 80 μm ✕80 μm chip size etching by the inductive coupled plasma reactive ion etching (ICPRIE) and defect-free neutral beam etching (NBE) processes was studied in this work. In μLEDs of this size, the influence of defects formation in the sidewalls on EQE was evaluated. There was almost no difference in EQE between μLEDs array etched by the NBE process no matter 40 μm ✕40 μm and 80 μm ✕80 μm, but the dependence was observed in the ICPRIE. Even with this size, it was found that the size effect of EQE is smaller than that in case of using ICPRIE for defect-free neutral beam etching. This impact is substantial since μLED predominantly operated at low current density, around 1–5 A/cm2. Consequently, the reduction of defect density, encompassing both internal and sidewall defects, becomes imperative even in 40–80 μm InGaN-based μLEDs. This not only improves the overall efficiency of μLEDs but also fortifies the brightness stability of μLED displays if process etching by NBE. It was also found that the etching shape had an influence on EQE. It could be attributed to fact that the etching profile angle of NBE was more vertical than that of ICPRIE. Because the different angles of the mesa resulted in different light intensity. The μLEDs emitting with a wavelength of 450 nm, the light extraction efficiency and intensity at a mesa angle 58° of NBE etching μLEDs was about 8% lower than those of an angle (38°) of ICPRIE etching μLEDs by simulation.

Volume detection based on porous silicon waveguide for CO2 mid-infrared spectroscopy

A mid-infrared (mid-IR) porous silicon (PSi) waveguide gas sensor was fabricated. PSi guiding and confinement layers were prepared by electrochemical anodization. Ridge waveguides were patterned using standard i-line photolithography and reactive ion etching. Due to the open pores, light and gas molecules interact in the inside volume, unlike bulk material in which the interaction takes place with the evanescent part of the light. Propagation losses are measured for a wavelength range spanning from λ = 3.9 to 4.55 µm with a value of 11.4 dB/cm at λ = 4.28 µm. The influence of native oxidation and ageing on the propagation losses was investigated. Limit of detection (LoD) of 1000 ppm is obtained with the waveguide sensor at the carbon dioxide (CO2) absorption peak at λ = 4.28 µm.

About the Data Analysis of Optical Emission Spectra of Reactive Ion Etching Processes—The Method of Spectral Redundancy Reduction

In this study, we present the Method of Spectral Redundancy Reduction (MSRR) for analyzing OES (optical emission spectroscopy) data of dry etching processes based on the principles of spectral clustering. To achieve this, the OES data are transformed into abstract graph matrices whose associated eigenvectors directly indicate anomalies in the data set. We developed an approach that allows for the reduction in temporally resolved optical emission spectra from plasma structuring processes in such a way that individual emission lines can be algorithmically detected, which exhibit a temporal behavior different from the collective behavior of the temporally resolved overall spectrum. The proportion of emission lines that behave consistently throughout the entire process duration is not considered. Our work may find applications in which OES is used as a process-monitoring technique, especially for low-pressure plasma processing. The major benefit of the developed method is that the scale of the original data is kept, making physical interpretations possible despite data reductions.

Pressure resistance evaluation of an ultrathin SiNx membrane etched by a gas cluster ion beam

In this study, reactive etching of a SiNx free-standing membrane with a thickness of a few nanometers was performed using a gas cluster ion beam (GCIB) and the pressure resistance of the membrane with respect to its thickness was evaluated. The low-damage irradiation effect of a 7 keV GCIB in an acetylacetone (Hacac) atmosphere enabled the etching to retain its pressure resistance compared with that of 400 eV Ar+ beam irradiation. In a previous study, it was shown that irradiation of SiNx films with Ar plasma of several hundred eV causes defects in the bonding network of the Si–N bond and the network is easily oxidized. XPS measurements on SiNx films after GCIB etching with Hacac and Ar+ beam irradiation showed that the composition of the Si–O bond was smaller with GCIB irradiation compared to Ar+ beam irradiation. This indicates that GCIB etching with Hacac can suppress the formation of defects in the Si–N network, which reduces the degradation of the pressure resistance.

Wafer-scale silicon microfabrication technology toward realization of low-cost sub-THz waveguide devices

This paper presents a wafer-scale silicon microfabrication technology for the sub-terahertz (sub-THz) waveguide device mass production. Based on the effective scheme, a WR-5 (140–220 GHz) straight rectangular waveguide and a WR-2.8 (260–400 GHz) rectangular waveguide bandpass filter are implemented as demonstrated examples. The silicon deep reactive ion etching (DRIE) process is employed to etch through the total thickness of the silicon wafer and form the main waveguide channels. Then, a low-temperature thermal compression process is used to bond the trough-etched wafer with the top and bottom metallised silicon wafers to form the closed waveguide structures without any precise alignment process. The fabricated waveguide has the benefit of low transmission loss (0.03–0.05 dB mm−1) at the whole G band. Besides, to measure the fabricated WR-2.8 waveguide filter and solve the measuring equipment standard waveguide difference, silicon micromachined waveguide transitions are explored and fabricated to match two different frequency-band modules for measuring the waveguide filters in the desired full frequency band, which also has a potential application for the different size waveguide conversion. The measured results agree well with the simulated ones. The measured 3 dB bandwidth is 9.3%, with a central frequency of 343 GHz; the average insertion loss (IL) is about 1.6 dB in the pass band, including two extra straight waveguides of 8 mm length on input/output ends and two external waveguide-to-waveguide transitions. The proposed method provides a feasible and cost-effective solution for the mass production of high-performance waveguide devices and integrated systems in sub-THz frequency bands and beyond.

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.

THERMOREGULATION SYSTEM FOR BIOSENSORS BASED ON FIELD-EFFECT TRANSISTORS WITH A NANOWIRE CHANNEL

In this work we present an automatic thermoregulation system for biosensors based on field-effect transistors with a nanowire channel, which provides full control on the required temperature regime in bioanalytical analises. The system elements, including field-effect transistors with a nanowire channel, temperature sensors and heaters, were fabricated on a single silicon cristal using electron beam lithography, reactive ion etching and high-vacuum deposition techniques. Unicue electronics have been developed to control and maintain temperature. The dependence of thermometer readout on heating power was measured, which is in good agreement with the results of numerical simulation. A demonstration of a thermoregulation system with PID-feedback was carried out, ensuring the establishment of a desiered temperature in the range of 30-70◦ C in 18 s in liquid. A demonstration of a thermoregulation system for detecting nucleic acids was carried out using synthetic single-stranded DNA, which is a gene fragment from the bacterium Escherichia coli. The minimal detectable response was observed for a sample with a concentration of 3 fM.

Understanding the contributions of F–, HF, and HF2– to the etching of SiO2 and unveiling the reaction kinetics to represent etching behavior of SiO2 up to pH 5

Understanding of the silicon dioxide (SiO2) etching mechanism in hydrofluoric acid (HF) solutions is important in semiconductor manufacturing processes. A study on the previous SiO2 etching mechanism claimed that only difluoride (HF2–) participated in SiO2 etching. However, in this study, it was observed that the etching of SiO2 occurred in the HF solution, where difluoride barely existed. Hence, a new SiO2 etching mechanism and reaction rate were proposed. Various concentrations of HF and ammonium fluoride (NH4F) under varying pH conditions were used to etch SiO2, leading to an SiO2 etching rate of 510[F–] + 610[HF] + 2890[HF2–] (Å/min). HF2– was the primary contributor to SiO2 etching; however, unlike the previous SiO2 etching mechanism, the effects of F– and HF on the etching of SiO2 were included in the rate of SiO2 etching. The SiO2 etching rate, considering the reactions between various fluorine species with varying SiO2 surface states, effectively represented the SiO2 etching behavior under various conditions over a broader pH range, up to pH 5. Controlling the ratio of the fluorine species, F–, HF, and HF2–, our etching model could also be extended to the selective etching of SiO2.

Composite nanostructure comprising silver nanopyramids and silver nanoparticles for plasmon-enhanced fluorescence

In this study, a composite silver nanostructure is presented to serve as the platform for highly efficient plasmon-enhanced fluorescence (PEF). The composite nanostructure is realized by first employing nanosphere lithography (NPL) combined with reactive ion etching (RIE) technology to create a silver nanopyramid array, which is then further modified with silver nanoparticles. Utilizing DCJTB as the fluorophore, this composite nanostructure is found to outperform the use of either silver nanoparticles or silver nanopyramid array. Notably, it not only enhances the photoluminescence (PL) but also reduces the carrier lifetime. The influence of the particle size of silver nanoparticles and the height of the silver nanopyramids is also investigated. It is found that larger silver nanoparticles and higher silver nanopyramids lead to stronger local surface plasmon resonance (LSPR), thereby enhancing the PEF phenomenon. Compared with the performance of using bare glass substrate, the PL intensity of using the composite nanostructure is enhanced to 19.4 times and the carrier lifetime is shortened by 61%.

Enhancing anti-reflective properties of electronic glass through two-step chemical etching

With the rapid growth of the electronic display industry, aluminosilicate glass has emerged as a replacement for traditional soda lime silica glass as the cover plate of various display devices because of its excellent physical and chemical properties. High transmittance and low reflectivity are the inevitable requirements of its application. However, few studies have been reported about the antireflection of aluminosilicate glass. In this study, a two-step etching method was employed to treat both sides of the alkali-aluminosilicate glass to obtain surface antireflection. Analytical methods such as EPMA, AFM, and UV spectrophotometry were utilized to evaluate the effect of the etching process and resultant surface microstructure on the optical properties of the glass. Furthermore, comparative research was conducted to distinguish the etching reaction differences between alkali-aluminosilicate glass and other glass compositions like soda-lime glass and high-boron-silicon glass. The results demonstrated that the controlled two-step etching process created a micro-porous surface structure, with a gradient refractive index. Subsequent to the secondary etching, the glass exhibits an impressive average transmittance of 98.88% within the visible light spectrum (380–780 nm). Moreover, identical etchant across different composition glasses leads to discernible differences in transmittance.

The Impact of AI on Contact Resistance and Its Suitability in Fine Pitch Interconnects

Integration issues for a three-dimensional (3D) interconnect in a Face-to-Face (F2F) configuration are discussed. In particular, the effect of AI and organic dielectrics under the bump and their effect in chip-package-interaction (CPI) stresses as well as AI contact resistance issues that arise as the interconnection pitch is decreased. This paper will present a finite-element model created to study the stresses in advanced 3D microelectronic package. To assess the reliability of the 3D packages a submodeling approach is used to capture the CPI stresses. The modeling study presented indicates that it is beneficial to continue using AI pads as it has significatly lower stresses compared to copper pads/vias. In the second portion of the paper, the effect of PBO developer on AI corrosion is presented. Reactive ion etching (RIE) chemistries and wet chemistries were optimized using contact resistance as the success metric. Process robustness was achieved by decoupling the hard dielectric opening from the PBO via opening. Time of Flight Secondary Ion Mass Spectrometry (ToF-SIMS), Scanning Electron Microscopy (SEM), X-ray Photoelectron Spectroscopy (XPS) analysis were used to add clarity to the bump contact resistance values.