Pyrex 7740玻璃深刻蚀掩模研究

玻璃湿法深刻蚀掩模常采用低压化学气相沉积(LPCVD)多晶硅、Cr/Au金属层+光刻胶等,但往往会在玻璃中引入应力,影响后期应用(如阳极键合),而且Cr/Au金属层价格昂贵。为避免以上缺点,引入了SX AR—PC 5000/40保护胶+WBR2075干膜作为玻璃的刻蚀掩模,在HF︰NH4F,HF︰HCl,HF︰HCl︰NH4F刻蚀溶液中进行了大量实验。实验结果表明:SX AR—PC 5000/40抗腐蚀能力强,且成功实现了对Pyrex 7740玻璃131μm的深刻蚀。整个工艺过程与IC工艺兼容,可以进行圆片级批量加工。实验结果对圆片级封装和其他MEMS器件的制作有一定参考作用。     

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.     

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.

     

Rapid soda-lime glass etching process for producing microfluidic channels with higher aspect ratio

This paper presents a simple method to produce microfluidic channels in soda-lime glasses with the aspect ratio >0.5 utilizing a modified wet etching protocol. A low-cost positive photoresist (PR) layer is used as the etching mask for the wet etching process. Prior to the PR and primer coating procedure, a UV activation process is adopted for enhancing the binding strength of the hexamethyldisilazane primer layer and the glass substrate, resulting in an better adhesion for the PR layer. A fast etching recipe is also developed by increasing the acidity and the temperature of the buffered oxide (BOE) etchant. Since the photoresist etching mask does not peel during the etching process shortly, the structure of the etching mask forms a barrier and results in a different diffusion rate for the etchant inside the etched trench structure. A slower etching rate for the glass is observed at the undercut region such that the proposed anisotropic etching pattern can be achieved. Results show that the etching rate of the modified glass etching process is as high as 7.7 μm/min which is much faster than that of pure BOE etchant (0.96 μm/min). Sealed microfluidic channel with the aspect ratio of around 0.62 is produced with the developed method. The method developed in the present study provides a rapid and efficient way to produce microfluidic channels with higher aspect ratio.     

A Rapid and Low-Cost Procedure for Fabrication of Glass Microfluidic Devices

In this paper, we present a simple, rapid, and low-cost procedure for fabricating glass microfluidic chips. This procedure uses commercially available microscopic slides as substrates and a thin layer of AZ 4620 positive photoresist (PR) as an etch mask for fabricating glass microfluidic components, rather than using expensive quartz glasses or Pyrex glasses as substrates and depositing an expensive metal or polysilicon/amorphous silicon layer as etch masks in conventional method. A long hard-baking process is proposed to realize the durable PR mask capable of withstanding a long etching process. In order to remove precipitated particles generated during the etching process, a new recipe of buffered oxide etching with addition of 20% HCl is also reported. A smooth surface microchannel with a depth of more than 110 mum is achieved after 2 h of etching. Meanwhile, a simple, fast, but reliable bonding process based on UV-curable glue has been developed which takes only 10 min to accomplish the efficient sealing of glass chips. The result shows that a high bonding yield (~ 100%) can be easily achieved without the requirement of clean room facilities and programmed high-temperature furnaces. The presented simple fabrication process is suitable for fast prototyping and manufacturing disposable microfluidic devices.     

Mechanical and electrical bonding between silicon wafer and glass wafer with etched channels containing metal tracks

In this paper a novel process to bond and, at the same time, to electrically connect a silicon wafer to a glass wafer is presented. It consists of a low temperature anodic bonding process between silicon and glass by using a glass wafer with etched channels in order to contain metal tracks. The glass-to-silicon anodic bonding process at low temperatures (not exceeding 300°C) assures a strong mechanical link (Berthold et al. in Transducers 1999, June:7–10, 1999). The electrical contacts between the metal pads on the backside of a silicon wafer and the metal pads on the glass wafer are achieved by sintering and diffusion of metals due to a kind of thermo compression bonding. This bonding method permits a high vertical control due to a well-controlled etching of the cavity depth and to the thickness precision of both metallization (pads on silicon wafers and metal tracks on glass wafer). This IC-processing compatible approach opens up the way to a new electrical connection concept keeping, at the same time, a strong mechanical bond between glass and silicon wafers for an easier fabrication of a more complex micro-system.     

Fabrication of intermediate mask for deep x-ray lithography

 This paper presents the fabrication of intermediate x-ray mask for deep x-ray lithography. In order to have working mask with absorbers thickness larger than 10 μm, the intermediate mask should have absorbers of 0.7 μm in thickness. To demonstrate intermediate mask fabrication, x-ray zone plates are fabricated on the 1.2 μm low-stress silicon-rich silicon nitride (SiN_x) membrane with the tri-layer Chromium-Tungsten-Chromium (Cr–W–Cr) as the x-ray absorbers. The chromium layers both 200 angstroms are used as adhesion and for stress relief. The SiN_x film is deposited with low pressure chemical vapor deposition (LPCVD) and the free standing membrane are formed by KOH silicon backside etching. With the e-beam lithography and reactive ion etching, width of 0.8 μm of outmost zone of the x-ray zone plates has been achieved on the membrane. The scanning electron microscopy (SEM) images of the x-ray zone plates and pictures of intermediate masks are demonstrated. Received: 25 August 1997/Accepted: 3 September 1997     

Manufacture of microfluidic glass chips by deep plasma etching, femtosecond laser ablation, and anodic bonding

Two dry subtractive techniques for the fabrication of microchannels in borosilicate glass were investigated, plasma etching and laser ablation. Inductively coupled plasma reactive ion etching was carried out in a fluorine plasma (C₄F₈/O₂) using an electroplated Ni mask. Depth up to 100 μm with a profile angle of 83°–88° and a smooth bottom of the etched structure (Ra below 3 nm) were achieved at an etch rate of 0.9 μm/min. An ultrashort pulse Ti:sapphire laser operating at the wavelength of 800 nm and 5 kHz repetition rate was used for micromachining. Channels of 100 μm width and 140 μm height with a profile angle of 80–85° were obtained in 3 min using an average power of 160 mW and a pulse duration of 120 fs. A novel process for glass–glass anodic bonding using a conductive interlayer of Si/Al/Si has been developed to seal microfluidic components with good optical transparency using a relatively low temperature (350°C).     

Strategies in deep wet etching of Pyrex glass

This paper establishes the strategies for deep wet etching of one of the most common glasses: Pyrex. There are two way for increasing the etch depth: increasing the etch rate or increasing the resistance of the mask in the etching solution. The paper analyzes the methods for increasing the glass etch rate in HF solutions: annealing, concentration, ultrasonic agitation and temperature. The generation of the defects is investigated. The main factors that affect the degradation of the mask are: type, value and gradient of the residual stress and the hydrophilicity of the surface. Cr/Au mask is used for illustration. A new method for deep wet etching of glass using Cr/Au mask and photoresist is established. The result of this method is the best thus far as reported in the literature: 85 min deep wet etching in HF 49% which is equivalent to etching of more than 500 μm deep in the Pyrex glass material.     

Glass Blowing on a Wafer Level

A fabrication process for the simultaneous shaping of arrays of glass shells on a wafer level is introduced in this paper. The process is based on etching cavities in silicon, followed by anodic bonding of a thin glass wafer to the etched silicon wafer. The bonded wafers are then heated inside a furnace at a temperature above the softening point of the glass, and due to the expansion of the trapped gas in the silicon cavities the glass is blown into three-dimensional spherical shells. An analytical model which can be used to predict the shape of the glass shells is described and demonstrated to match the experimental data. The ability to blow glass on a wafer level may enable novel capabilities including mass-production of microscopic spherical gas confinement chambers, microlenses, and complex microfluidic networks     

CO2激光直写结合湿法刻蚀加工玻璃基微流控芯片

玻璃是制作微流控芯片的重要材料,其加工工艺主要基于光刻后湿法腐蚀,对设备和实验室要求较高.本文提出以普通指甲油和指甲油/金/铬为牺牲层,利用CO2激光烧蚀开窗口,辅以湿法腐蚀加工玻璃基微流控芯片的方法,并考察了激光加工参数,腐蚀液组成,牺牲层等因素对芯片质量的影响.该方法简便易行,不需要光刻的昂贵设备和繁杂步骤.     

Fabrication of multilayer systems combining microfluidic andmicrooptical elements for fluorescence detection

This paper presents the fabrication of a microchemical chip for the detection of fluorescence species in microfluidics. The microfluidic network is wet-etched in a Borofloat 33 (Pyrex) glass wafer and sealed by means of a second wafer. Unlike other similar chemical systems, the detection system is realized with the help of microfabrication techniques and directly deposited on both sides of the microchemical chip. The detection system is composed of the combination of refractive microlens arrays and chromium aperture arrays. The microfluidic channels are 60 μm wide and 25 μm deep. The utilization of elliptical microlens arrays to reduce aberration effects and the integration of an intermediate (between the two bonded wafers) aluminum aperture array are also presented. The elliptical microlenses have a major axis of 400 μm and a minor axis of 350 μm. The circular microlens diameters range from 280 to 300 μm. The apertures deposited on the outer chip surfaces are etched in a 3000-Å-thick chromium layer, whereas the intermediate aperture layer is etched in a 1000-Å-thick aluminum layer. The overall thickness of this microchemical system is less than 1.6 mm. The wet-etching process and new bonding procedures are discussed. Moreover, we present the successful detection of a 10-nM Cy5 solution with a signal-to-noise ratio (SNR) of 21 dB by means of this system     

Design and fabrication of an electrostatically suspended microgyroscope using UV-LIGA technology

A micromachined electrostatically suspended gyroscope, with a wheel-like rotor housed by top stator and bottom stator, using UV-LIGA microfabrication technology, was presented. The designed structure and basic operating principle of the gyroscope are described. The key steps in the fabrication process, such as wet etching of Pyrex glass pits for soldering, and integration of thick nickel structures by removal of SU-8 mold, were considered in detail and well solved. Cr/Pt/photoresist was used as etching mask and the etched pits, in depth of near 30 μm, with aspect ratio (depth to undercutting) of 0.75, were obtained. With metal foundations constructed for consolidation, successful integration of the nickel structures, in thickness of 200 μm, was achieved by successful removal of the SU-8 mold using oleum. After the two stators and the rotor were fabricated separately, they were assembled and soldering bonded to form axial and radial small gaps, hence, the initial prototype of the microgyroscope was realized. The key techniques described in this paper can be applied to fabrication of other micro devices. The metal foundation method, associated with removal of SU-8 mold by oleum, is expected to make SU-8 wider applications in making integrated microstructures with fabricated circuitry on the same chip.     

Fabrication of polystyrene microfluidic devices using a pulsed CO<Subscript>2</Subscript> laser system

In this article, we described a simple and rapid method for fabrication of droplet microfluidic devices on polystyrene substrate using a CO₂ laser system. The effects of the laser power and the cutting speed on the depth, width and aspect ratio of the microchannels fabricated on polystyrene were investigated. The polystyrene microfluidic channels were encapsulated using a hot press bonding technique. The experimental results showed that both discrete droplets and laminar flows could be obtained in the device.     

Evaluation of eutectic bond strength and assembly of Al-based microfluidic structures

Metal-based microscale heat exchangers have potential advantages over similar Si-based devices. Bonding and assembly are critical for building functional metal-based microfluidic devices from metallic high-aspect-ratio microscale structures (HARMS). In this paper, we report eutectic bonding of Al specimens with Al–Ge thin film intermediate layers. Quantitative evaluation of bond strengths was carried out as a function of various bonding parameters, including bonding temperature, applied pressure, and Al–Ge intermediate layer thickness. With this eutectic bonding strategy, successful assembly of multilayered Al microfluidic structures is demonstrated.     

Microstenciling: a generic technology for microscale patterning of vapor deposited materials

The fabrication of microstencils for patterning on unconventional substrates was demonstrated. Stencil feature sizes ranging from 6 to 370 /spl mu/m with aspect ratios (stencil feature height :width) in the range of 0.5 : 1 to 15 : 1 were fabricated using ICP etching of silicon. The stenciling process was demonstrated for the deposition of metals (Ti/Au) and dielectrics (silicon dioxide) onto silicon, glass, and polymer based substrates for microfluidic system development. The results demonstrated some dependency of the deposition rate on the stencil feature size and aspect ratio. Results from adhesion studies showed excellent adhesion on all substrates with the exception of PMMA.     

Bench scale glass-to-glass bonding for microfluidic prototyping

Microfluidics, an increasingly ubiquitous technology platform, has been extensively utilized in assorted research areas. Commonly, microfluidic devices are fabricated using cheap and convenient elastomers such as poly(dimethylsiloxane) (PDMS). However, despite the popularity of these materials, their disadvantages such like deformation under moderate pressure, chemical incompatibility, and surface heterogeneity have been widely recognized as impediments to expanding the utility of microfluidics. Glass-based microfluidic devices, on the other hand, exhibit desirable properties including rigidity, chemically inertness, and surface chemistry homogeneity. That the universal adoption of glass-based microfluidics has not yet been achieved is largely attributable to the difficulties in device fabrication and bonding, which usually require large capital investment. Therefore, in this work, we have developed a bench-scale glass-to-glass bonding protocol that allows the automated bonding of glass microfluidic devices within 6 h via a commercially available furnace. The quality of the bonds was inspected comprehensively in terms of bonding strength, channel deformation and reliability. Additionally, femtosecond pulsed laser micromachining was employed to rapidly engrave channels on a glass substrate with arbitrary-triangular in this case-cross-section. Bonded glass microfluidic devices with machined channels have been used to verify calculated capillary entry pressures. This combination of fast laser micromachining that produces arbitrary cross-sectioned microstructures and convenient bench-scale glass bonding protocol will facilitate a broad range of micro-scale applications.

     

Silver (Ag) as a novel masking material in glass etching for microfluidics applications

In this paper, we report the use of a single masking film for deep glass etching in hydrofluoric acid (HF). Thin film silver (Ag) is the key masking material in this work enabling a simple and low cost fabrication of microfluidic structures. The Ag film was deposited by evaporation and etched in a diluted nitric acid and de-ionized water solution at a ratio of 1:3. Surface morphology for different thicknesses of Ag film and its correlation to the maximum achievable etch depth is analyzed. AFM results shows low roughness values (<5 nm), indicating the Ag films are of smooth surface. With a 100 nm Ag film, a 220 μm etch depth in borosilicate glass substrates were produced and by further thickening the Ag to 300 nm, etch depths exceeding 300 μm were successfully achieved. SEM images show that thinner Ag films are of finer grains, potentially a source for pinholes formation where rapid penetration of HF along the grain boundaries peels off the Ag film from the glass surface. However, the Ag film was found not to react with HF. The process was demonstrated in the fabrication of cavities for integration with other microfluidic devices.     

A Nano Initiator Realized by Integrating Al/CuO-Based Nanoenergetic Materials With a Au/Pt/Cr Microheater

A nano initiator is developed by integrating Al/CuO-based nanoenergetic materials with a Au/Pt/Cr thin-film microheater realized onto a glass substrate. It is fabricated by using standard microsystem techniques that allow batch fabrication and high level of integration and reliability. The nano initiator is characterized by open-air combustion testing with an ignition success rate of 98%. The ejected combustion flame is seen clearly with a potential exceeding 2000 $^{circ}hbox{C}$. The ignition power, ignition delay, and ignition energy are 1.16 W, 0.1–0.6 ms, and 0.12–0.70 mJ, respectively. The energy output is calculated to be around 60 mJ.$hfill$[2008-0035]      

Application of nanoparticles dispersed polymer to micropowder blasting mask

Improvements in micropowder blasting have been realized for rapid prototyping of channels in glass substrates. The technique presented in this study consists of laser patterning of Au nanoparticles dispersed polymer and micropowder blasting. The patterned polymer was utilized as a mask material for the subsequent mechanical removal of the glass by the micropowder blasting. Five different polymers were tested for the matrix material. Using a line and space mask pattern of 110 /spl mu/m in width, fabricated channels were created in the glass with a maximum aspect ratio of 2.1. The validity of the micropowder blasting using Au nanoparticles dispersed polymer mask was confirmed; additionally, we demonstrated that the micropowder blasting technique with elevated polymer mask temperature was able to reduce erosion of the polymer mask.