Comparison of etch characteristics of KOH,TMAH and EDP for bulk micromachining of silicon (110)

Bulk micromachining in Si (110) wafer is an essential process for fabricating vertical microstructures by wet chemical etching. We compared the anisotropic etching properties of potassium hydroxide (KOH), tetra-methyl ammonium hydroxide (TMAH) and ethylene di-amine pyro-catechol (EDP) solutions. A series of etching experiments have been carried out using different etchant concentration and temperatures. Etching at elevated temperatures was found to improve the surface quality as well as shorten the etching time in all the etchants. At 120°C, we get a smooth surface (Ra = 21.2 nm) with an etching rate 12.2 μm/min in 40wt% KOH solution. At 125°C, EDP solution (88wt%) was found to produce smoothest surface (Ra = 9.4 nm) with an etch rate of 1.8 μm/min. In TMAH solution (25wt%), the best surface roughness was found to be 35.6 nm (Ra) at 90°C with an etch rate of 1.18 μm/min. The activation energy and pre-exponential factor in Arrhenius relation are also estimated from the corresponding etch rate data.

     

Investigation of fused silica glass etching using C4F8/Ar inductively coupled plasmas for through glass via (TGV) applications

Through glass via (TGV) technology is considered to be a cost effective enabler for the integration of micro electromechanical systems and radio frequency devices. Inductively coupled plasma and Bosch etching process comprise one of the most pervasive methods for through silicon via (TSV) formation. Unfortunately an equivalent process for glass etching remains elusive. In this paper, the influence of plasma etching for fused silica glass were investigated to find the best tradeoff between etch rate and profile of TGVs. The process parameters including bias power, gas flow rate, ratio of etching gases and reaction chamber pressure using Ar/C₄F₈ inductively coupled plasmas were studied. The etching results show that all these three parameters have a significant impact on the etch rate. Furthermore, the adjustment including total flow rate and ratio of Ar/C₄F₈ and chamber pressure can be used to control the via profile. Constant fused silica glass etch rate greater than 1 μm/min was obtained when chiller temperature was 40 °C with etching time of 60 min. The profile angle of TGVs with nearly 90° was also achieved.     

Resist-less patterning on SiO2 by combination of X-ray exposure and vapor HF etching

We succeeded in a resist-less patterning of SiO₂/Si substrates by a combination of X-ray exposure and vapor hydrogen fluoride (HF) etching. A 2 μm thick SiO₂ layer was formed on a Si substrate by employing a thermal oxidation process. An X-ray mask consisted of a 1 μm thick Ta absorber on a 2 μm thick Si₃N₄ membrane mounted on a 1 mm thick Si frame, and a honeycomb pattern where 640 nm diameter circle dots arranged in the corners of a hexagon with a pitch of 960 nm was processed. X-ray exposure experiments were carried out on a beamline BL-4 with a peak photon energy of 2 keV at the TERAS synchrotron radiation (SR) facility. When a dose energy was 750 mAh, the transfer of the patterns was confirmed, although irradiations with different dose energy were also conducted. Moreover, heating temperatures and total etching times of SiO₂/Si substrates in vapor HF etching were changed, and the shapes of etched patterns were observed by scanning electron microscope. It was learnt that an appropriate etching time existed between 30 and 60 min. Moreover, we observed discoloration of irradiated area by SR; and this seemed to be caused by changes in the etching rate of SiO₂/Si substrates that led to the development of resist-less patterning technique.     

Vertical Si nanowire with ultra-high-aspect-ratio by combined top-down processing technique

Vertical Si nanowires with ultra-high-aspect-ratio were fabricated using a combined process of deep reactive ion etching and sacrificial oxidation. The combined process starts with etching the Si substrates by the Bosch process to form micrometer-scale structures. The etched micrometer-scale structures are shrunk to nanometer-scale by sacrificial oxidation. The fabricated Si nanowires that were aligned vertically to the substrate had a diameter of less than 200 nm and a length greater than 10 μm. One of the fabricated Si nanowires had a diameter of 110 nm and a length of 11 μm. The resulting aspect-ratio reached 100, which is a value that is significantly high for vertical Si nanowires fabricated by using a top-down approach.     

Micro-mixer device with deep channels in silicon using modified RIE process: fabrication,packaging and characterization

In the present work, silicon based micromixer microfluidic devices have been fabricated in silicon substrates of 2-inch diameter. These devices are of 2-input and 1-output port configuration bearing channel depth in the range 80–280 µm. Conventional reactive ion etching (RIE) process used in integrated circuit fabrication was modified to get reasonably high silicon etch rate (~1.2 µm/min). It was anticipated that devices with channel depth in excess of 150 µm would become weak and susceptible to breakage. For such devices, a bonded pair of silicon having a 0.5 µm SiO₂ at the bonded interface was used as the starting substrate. The processed silicon wafer bearing channels was anodically bonded to a Corning^® 7740 glass plate of identical size for fluid confinement. Through-holes for input/output ports were made either in Si substrate or in glass plate before carrying out anodic bonding. Micro-channels were characterized using stylus and optical profiler. Surface roughness of the channel was observed to increase with increasing channel depth. The devices were packaged in a polycarbonate housing and pressure drop versus flow rate measurements were carried out. Reynolds number and friction factor were calculated for devices with 82 µm deep channels. It was observed that up to 25 sccm of gas and 10 ml/min of liquid, the flow was laminar in nature. It is envisaged that using bonded silicon wafer pair and combination of RIE and wet etching, it is possible to get an etch stop at the SiO₂ layer of the bonded silicon interface with much smaller value of surface roughness rendering smooth channel surface.     

Submicron polymer structures with X-ray lithography and hot embossing

This article describes the process chain for replication of submicron structures with varying aspect ratios (AR) up to 6 in polymethylmethacrylate (PMMA) by hot embossing to show the capability of the entire LIGA process to fabricate structures with these dimensions. Therefore a 4.7 μm thick layer of MicroChem 950k PMMA A11 resist was spin-coated on a 2.3 μm Ti/TiO _x membrane. It was patterned with X-ray lithography at the electron storage ring ANKA (2.5 GeV and λ _c ≈ 0.4 nm) at a dose of 4 kJ/cm³ using a Si₃N₄ membrane mask with 2 μm thick gold-absorbers. The samples were developed in GG/BDG and resulted in AR of 6–14. Subsequent nickel plating at 52°C resulted in a 200 μm thick nickel tool of 100 mm diameter, which was used to replicate slit-nozzles and columns in PMMA. Closely packed submicron cavities with AR 6 in the nickel shim were filled to 60% during hot embossing.     

Fabrication of flexible light guide plate using CO2 laser LIGA-like technology

The liquid crystal display (LCD) needs the back light module (BLM) for the light source. The light guide plate (LGP) is the main component of BLM to spread light source to the whole LCD surface and requires for the generation trend of lightweight, easy to carry, and bendable for LCD. In this article, we have demonstrated the fabrication of flexible LGP using CO₂ laser LIGA-like technology which includes the laser ablation of micro-groove polymethylmethacrylate (PMMA) master mold, pouring polydimethylsiloxane (PDMS) to the mold and casting the micro-groove microstructure for flexible LGP application. Different laser powers and micro-groove pitches were used to ablate the PMMA mold with varied groove depths and taper angles. Optical microscope was used to examine the morphology and profile of the final bendable LGP microstructure. Under the varied laser power of 1–12 W, the mean taper angles of PMMA micro-grooves ranged from 28° to 70° and the etching depths were from 44.5 to 281.8 μm. The flexible PDMS LGP had good microstructure duplication after casting. The optical uniformity and luminance of flexible LGP was concerned with structure of micro-grooves and measured using BM9 luminance meter. The maximal light uniformity and average luminance of LGP at some microstructure reaches 75 % and 119 cd/m², respectively.     

Simple fabrication of an uncooled Al/SiO2 microcantilever IR detector based on bulk micromachining

A simple microfabrication process to make an uncooled aluminum/silicon dioxide bi-material microcantilever infrared (IR) detector using silicon bulk micromachining technology is presented in this work. This detector is based on high banding of the microcantilever due to the large dissimilar in thermal expansion coefficients between the two materials. It consists of a 1 μm SiO₂ layer deposited by 200 nm thin Al layer. Since no sacrificial layer is used in this process, complexity related to releasing sacrificial layer is avoided. Moreover Al is protected in Si etchant using dual-doped tetramethyl ammonium hydroxide. The other advantage of this process is that only three masks are used with four photolithography process. Thermal and thermal mechanical behaviors of this structure are obtained using finite element analysis, and the maximum temperature and displacement at the end of cantilever at 100 pW/μm² absorbed IR power density on top surface are 7.82°K and 1.924 μm, respectively.     

Micromachined ultrasonic transducers based on lead zirconate titanate (PZT) films

The design, fabrication and measuring of piezoelectric micromachined ultrasonic transducers (pMUTs), including the deposition and patterning of PZT films, was investigated. The (100) preferential orientation of PZT film have been deposited on Pt/Ti/SiO₂/Si (100) substrates by modified sol–gel method. PZT film and Pt/Ti electrode were patterned by novel lift-off using ZnO as a sacrificial layer avoiding shortcomings of dry and wet etching methods. pMUT elements have been fabricated by an improved silicon micromachining process and their properties were also characterized. As measured results, the pMUT tends to operate in a standard plate-mode. The receive sensitivity and transmit sensitivity of pMUT element whose active area only has 0.25 mm² are ?218 dB (ref. 1 V/μPa) and 139 dB (ref. 1 μPa/V), respectively.     

Comparison of etch characteristics of KOH, TMAH and EDP for bulk micromachining of silicon (110)

Bulk micromachining in Si (110) wafer is an essential process for fabricating vertical microstructures by wet chemical etching. We compared the anisotropic etching properties of potassium hydroxide (KOH), tetra-methyl ammonium hydroxide (TMAH) and ethylene di-amine pyro-catechol (EDP) solutions. A series of etching experiments have been carried out using different etchant concentration and temperatures. Etching at elevated temperatures was found to improve the surface quality as well as shorten the etching time in all the etchants. At 120°C, we get a smooth surface (Ra?=?21.2?nm) with an etching rate 12.2???m/min in 40wt% KOH solution. At 125°C, EDP solution (88wt%) was found to produce smoothest surface (Ra?=?9.4?nm) with an etch rate of 1.8???m/min. In TMAH solution (25wt%), the best surface roughness was found to be 35.6?nm (Ra) at 90°C with an etch rate of 1.18???m/min. The activation energy and pre-exponential factor in Arrhenius relation are also estimated from the corresponding etch rate data.     

Defect-free wet etching through pyrex glass using Cr/Au mask

This paper reports the highest etch depth of annealed Pyrex glass achieved by wet etching in highly concentrated HF solution, using a low stress chromium–gold with assistance of photoresist as masking layer. The strategies to achieve that are: increasing the etch rate of glass and simultaneously increasing the resistance of Cr/Au mask in the etchant. By annealing the Pyrex glass and using a highly concentrated HF acid, a high etch rate can be obtained. Furthermore, a method to achieve a good resistance of the Cr/Au masking layer in the etching solution is to control the residual stress and to increase the thickness of Au deposition up to 1 μm. In addition, the presence of a hard baked photoresist can improve the etching performance. As a result, a 500-μm thick Pyrex glass wafer was etched through.

     

Monolithic integration of Pb(Zr,Ti)O3 thin film based resonators using a complete dry microfabrication process

Monolithic fabrication of lead zirconate titanate [Pb(Zr,Ti)O₃ or PZT] based thin film resonant devices such as microcantilevers, Lamb wave and bulk acoustic wave resonators are demonstrated. High-performance PZT thin films with a thickness of 2.6 μm are prepared on a silicon on insulator wafer by a sputtering deposition process. A highly selective reactive ion etching process is employed for micro-patterning of PZT, platinum electrodes, and SiO₂ insulation layer. Self-actuation of the PZT microcantilevers is demonstrated and the frequency response is characterized using a laser Doppler vibrometer. The frequency response of the Lamb wave resonator is evaluated by measuring its transmission characteristic using a network analyzer. For a Lamb wave resonator with a length of 240 μm and an interdigital period of 80 μm, the 1st order and 2nd resonance frequencies are 15.3 and 41.8 MHz, respectively.     

Post micromachining of MPW based CMOS–MEMS comb resonator and its mechanical and thermal characterization

In recent years micro electro mechanical system (MEMS) based micro resonant sensors have been given a lot of attention due to their potential as a platform for the development of many novel physical, chemical, and biological sensors. That is why this paper covers post processing of the structures fabricated through Multi-Project-Wafer using 0.35 µm MIMOS CMOS technology with particular focus on dry etching of Si and SiO₂ from the front side of CMOS–MEMS chip that is optimized using aluminum coated carrier wafer and achieved results are debris free as compared to photoresist coated carrier wafer. The device is etched through from the front side to avoid parasitic capacitances and squeeze film damping by keeping minimum size of the die. The etching of SiO₂ as well as deep Si etch-through using the same plasma etcher (SS110A Tegal) is successfully demonstrated in this work. Finally, after the successful post CMOS micromachining of the device, resonance frequency i.e. 8164 Hz and quality factor i.e. 51.34, is determined. The joule heating effect due to the passing of current through the central shuttle of the device is characterized. The maximum temperature close to the anchors of the comb resonator where the piezoresistors are located is determined through temperature coefficient of resistance measurement using PE-4RF type probe station and it is found to be 37.62 °C.     

The manufacturing of packaged capillary action microfluidic systems by means of CO2 laser processing

In this article we demonstrate a simple yet robust rapid prototyping manufacturing technique for the construction of autonomous microfluidic capillary systems by means of CO₂ laser processing. The final packaging of the microfluidic device is demonstrated using thermal lamination bonding and allows for a turnaround time of approximately 30 min to 3 h from activation of the laser system to device use. The low-cost CO₂ laser system is capable of producing repeatable microfluidic structures with minimum feature sizes superior than 100–150 μm over channel depths of more than 100 μm. This system is utilised to create capillary pump and valve designs within poly (methyl methacrylate) (PMMA) substrates. Such components are part of advanced systems that can self initiate and maintain the flow of various volumes of fluids from an input to a collection reservoir, whilst also controlling the progression of the flow through the various demonstrated valve type structures. The resulting systems could prove a very useful alternative to traditional, non-integrated, fluidic actuation and flow control systems found on-chip, which generally require some form of energy input, have limited portable capabilities and require more complex fabrication procedures.     

Effects of aperture size and pressure on XeF2 etching of silicon

 We developed a XeF₂ pulse etching system and clarified the Si etching characteristics. Dependencies of Si etching rates and etched roughness on the crystallographic orientation, number of pulses, pulse duration time, aperture size and etching pressure were measured. An etching depth and an etched roughness were 12.9 μm and 115 nm, respectively under charge pressure of 390 Pa, a pulse number of 10 and pulse duration time of 60 s. The etching depth increased by 36% with increasing the aperture width from 25 to 175 μm. This aperture size effect decreased from 36 to 20% with decreasing charge pressure from 390 to 65 Pa. The etched roughness decreases also with decreasing the etching pressure. The roughness was 25 nm under the charge pressure of 65 Pa, 50 pulses, 60 s. Received: 3 August 2001/Accepted: 29 October 2001     

Mechanical strengthening of Si cantilever by chemical KOH etching and its surface analysis by TEM and AFM

Mechanical strengthening of a Si cantilever by applying KOH wet etching was investigated. Two kinds of Si cantilever specimens having the different crystallographic orientations of the sidewall surfaces, i.e., Si{100} and Si{110}, were fabricated from the same SOI wafer by a Bosch process. The typical height and pitch of the scalloping formed on the sidewall were 248 and 917 nm, respectively. A 50 % KOH (40 °C) chemical wet etching was applied to increase the fracture stress of the Si cantilever. The fracture stress in the both of Si{100} and Si{110} cantilevers increased with the advance of the etching. The obtained maximum fracture stress in Si{100} and Si{110} were 4.2 and 3.7 GPa, respectively. Sidewall surface of the cantilever was analyzed to investigate the mechanical strengthening of Si cantilever by wet etching. The etched surface crystalline was analyzed by the transmission electron microscope (TEM), and confirmed that the thickness of the affected flow layer was less than 10 nm from the obtained TEM image. Then the change of the surface roughness by the KOH etching was analyzed by the atomic force microscope. The surface was smoothened with the advance of the KOH etching. The roughness value of Ra in Si{100} and Si{110} decreased to 12.1 and 37.7 nm, respectively.     

Low temperature carbon nanotube and hexagonal diamond deposition with photo-enhanced chemical vapor deposition

Deposition of carbon nanotube and hexagonal diamond thin films at low substrate temperature with photo-enhanced chemical vapor deposition is described here. Extensive experimentation is conducted to optimize the catalyst layer utilized for deposition by varying Al/Ni/Al metal layer thicknesses on SiO₂ coated Si substrates. The coated substrates are annealed to transform the thin metal layers into nanoparticles. Suitable catalyst layer thicknesses obtained are 3/2/3, 5/1/5 and 5/3/5 nm for Al/Ni/Al sandwich metal layers. Suitable annealing conditions are in the range of 350–450 °C for substrate temperature and from 0.22 to 10 Torr for chamber pressure in ammonia ambient for 25 min. Carbon tetrachloride (CCl₄) is used as a carbon precursor in this work. Argon to CCl₄ flow ratio is varied in 1.5–19 range, chamber pressure is varied in 3–10 Torr range, and the substrate temperature is varied in 350–450 °C range. Carbon nanotubes (CNT) growth is observed at lower chamber pressure, lower partial pressure of CCl₄, lower substrate temperature and for thin Ni catalyst layer. The optimal CNT deposition condition observed is 5 Torr total chamber pressure, 9:1 partial pressure ratio of Ar to CCl₄, 400 °C substrate temperature and 5/1/5 nm thick Al/Ni/Al catalyst layers. The hexagonal diamond deposition is observed at a higher chamber pressure, higher partial pressure of CCl₄, higher substrate temperature and for a thicker Ni catalyst layer. The optimal condition for hexagonal diamond deposition observed is 10 Torr total chamber pressure, 7:3 partial pressure ratio of Ar to CCl₄, 450 °C substrate temperature and 5/3/5 nm thick Al/Ni/Al catalyst sandwich layers.     

Etching processes for High Aspect Ratio Micro Systems Technology (HARMST)

 This paper reports on the development of a dry etching based HARMS-Technology which will offer the potential to manufacture micro-engines, micro-turbines, micro-sensors, micro-actuators, and electronic circuits onto a single silicon IC chip. This technology is based on the highly anisotropic and selective dry etching of Si-monocrystals. The suitability of reactive ion etching for the fabrication of micro electro mechanical systems (MEMS) has been evaluated by characterising the change of lateral dimensions vs. depth in etching deep structures in silicon. Fluorine, chlorine and bromine containing gases have provided the basis for this investigation. A conventional planar RIE (Reactive Ion Etching) reactor has been used, in some cases with magnetic field enhancement or ICP (Inductive Coupled Plasma) Source and low substrate temperature. For reactive ion etching based on Cl₂ or Cl₂/HBr plasma a slightly “positive” (top wider than bottom) slope is achieved when etching structures with a depth of several 10 μm, whereas a “negative” slope is obtained when etching with an SF₆/CCl₂F₂ based plasma. Pattern transfer with vertical walls is obtained for reactive ion etching based on SF₆ (with O₂ added) when maintaining the substrate at low temperature (in range ≈−100 °C). Further optimisation of plasma chemistries and reactive ion etching procedures should result in runouts in the order or 0.1 μm/100 μm depth in Si as well as in organic materials. Etching processes for HARMST is demonstrated in the realisation in Si microturbine. Axes or stators (nonmoving parts) are etched into the initial Si-wafer. The movable parts (rotors, beams, etc.) are prepared from electro-chemically etched Si-membranes with defined thicknesses that, all movable parts are created lithographically on the SiN_xO_y surface. This is followed by dry etching the mono-crystalline Si-membrane down to the SiN_xO_y sacrificial layer on the back side of the membrane by an RIE-process. The wafer with the movable parts is flipped onto the wafer with the already etched axis and then positioned and centred. The SiN_xO_y-sacrificial layer is then dissolved by a chemical wet or vapour etch process. Subsequent bonding with a Pyrex glass wafer seals the parts. Received: 30 October 1995/Accepted: 20 May 1996     

Surface modification of a-Si<Subscript>0.60</Subscript>C<Subscript>0.40</Subscript>:H films by Al-assisted photochemical etching: humidity sensing application

The paper investigates the formation of thin porous amorphous silicon carbide (PASiC) by Al-assisted photochemical etching using HF/AgNO₃ solution under UV illumination at λ = 254 nm. Different etching times varying from 2 to 10 min have been used on thin a-Si_0.60C_0.40:H films, which are elaborated by co-sputtering DC magnetron using a single crystal Si target and who deposited onto 86 of hot pressed polycrystalline 6H-SiC stripes of 12.5 mm³. Because of the high electrical resistivity of the thin a-Si_0.60C_0.40:H film higher than 2 MΩ cm, and in order to facilitate the chemical etching, a thin metallic film of high purity aluminum (Al) has been deposited under vacuum, follow-up of a thin palladium deposited under a grid to reduce attacked surface and reinforced solution etching. The etched surface was characterized by scanning electron microscopy, infrared spectroscopy, spectrophotometer UV, and photoluminescence. Results show that the morphology of etched a-Si_0.60C_0.40:H surface evaluates with etching time and presents a spongy and macroporous layers. Where, the diameter of pore size increases with the increasing etching time. A humidity sensors were fabricated through evaporating coplanar interdigital gold electrodes on PASiC and the humidity sensing properties were tested, it show, that the measured resistance Au-PASiC structure, depends highly on the applied bias voltage. Finally, the sensing performances are attributed to the unique surface structure, morphology of the pore and its size, that provide an effective pathway for vapor transportation and enlarged the sensing area of Au-PASiC.     

Capillary filling speed of ferrofluid in hydrophilic microscope slide nanochannels

The capillary filling speed of ferrofluid in hydrophilic nanofluidic channels is investigated under various temperature and constant magnetic field conditions. Nanochannels with depths ranging from 50 to 150 nm and widths of 30 to 200 μm are fabricated on borosilicate glass substrates using buffered oxide wet etching and glass–glass fusion bonding techniques. The capillary filling speed of the ferrofluid is measured experimentally and compared with the theoretical results predicted by the classical Washburn equation. It is found that the experimental filling speed is significantly slower than the theoretical filling speed due to the erroneous assumption in the Washburn model of a constant contact angle irrespective of the flow rate and the presence of flow obstructions. The experimental results show that the filling speed reduces with a reducing channel depth, an increasing ferrofluid concentration, a lower operating temperature and an increased filling length. However, the filling speed is enhanced in the presence of an external magnetic field.