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CN101913552B - Method for preparing suspension micro-sensitive structure based on aluminum sacrificial layer process - Google Patents

Method for preparing suspension micro-sensitive structure based on aluminum sacrificial layer process Download PDF

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CN101913552B
CN101913552B CN2010102446945A CN201010244694A CN101913552B CN 101913552 B CN101913552 B CN 101913552B CN 2010102446945 A CN2010102446945 A CN 2010102446945A CN 201010244694 A CN201010244694 A CN 201010244694A CN 101913552 B CN101913552 B CN 101913552B
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董景新
王嫘
韩丰田
刘云峰
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Tsinghua University
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Abstract

The invention discloses a method for preparing a suspension micro-sensitive structure based on an aluminum sacrificial layer process. The method comprises the following steps of: introducing a sacrificial layer into a three-layer suspension micro-sensitive structure to restrict a micro-sensitive suspension mass block during the processing, and connecting the suspension micro-sensitive structure and bulk silicon by using an aluminum light film so as to avoid influence of subsequent processing on the suspension structure; removing the sacrificial layer by wet etching; and finally replacing an etching solvent with clean water and ethanol, and drying. The method effectively ensures the integrity and mobility of the suspension micro-sensitive structure without changing the conventional process flow, does not reduce the performance of a micro-mechanical sensor because the mechanical restriction is not increased, reduces the process difficulty, improves the yield and can be widely used for processing various silicon micro-components with the suspension micro-sensitive structure.

Description

一种基于铝牺牲层工艺的悬浮微敏感结构制备方法A preparation method of suspended micro-sensitive structure based on aluminum sacrificial layer technology

技术领域 technical field

本发明涉及微硅器件加工的制备工艺领域,具体涉及一种基于铝牺牲层工艺的悬浮微敏感结构制备方法。The invention relates to the field of preparation technology for micro-silicon device processing, in particular to a method for preparing a suspended micro-sensitive structure based on an aluminum sacrificial layer technology.

背景技术 Background technique

微硅机电加工工艺是近年来随着集成电路工艺发展起来的微机电系统MEMS主流技术。微硅器件是采用微机电系统的微电子和微机械加工技术制造出来的,它具有体积小、重量轻、成本低、功耗低、可靠性高、适于批量化生产、易于集成和可实现智能化的特点。同时,在微米量级的特征尺寸使得它可以完成某些传统机械传感器所不能实现的功能,这样微机电系统的微电子和微机械加工技术越来越成为微硅器件制备工艺的主要发展方向。Micro-silicon electromechanical processing technology is the mainstream technology of micro-electro-mechanical systems MEMS developed with integrated circuit technology in recent years. Micro-silicon devices are manufactured using micro-electromechanical system microelectronics and micro-machining technology. It has small size, light weight, low cost, low power consumption, high reliability, suitable for mass production, easy integration and realizable Intelligent features. At the same time, the feature size on the order of microns enables it to perform functions that some traditional mechanical sensors cannot achieve, so microelectronics and micromachining technology of microelectromechanical systems are increasingly becoming the main development direction of microsilicon device manufacturing processes.

使用微机电系统的微电子和微机械加工技术加工的微硅器件方法中,玻璃-硅-玻璃三层式平板结构是其加工的微机械传感器的一种典型结构,即在硅微机械器件中通常含有一个感知加速度或力的悬浮质量块,这个微敏感悬浮质量块一般是从体硅上刻蚀而出,限于我国现有的体硅加工工艺,在加工过程中由于悬浮质量块没有或只有很小的机械约束,微敏感悬浮质量块很容易在后续的清洗、加工过程中引起结构畸变,或从硅腔中进出,造成器件特性劣化或破坏。解决此问题有两种方法:在设计过程中加大微敏感悬浮结构的机械约束和引入在加工结束后再将其去除的牺牲层。但是对于加大机械约束必然会引起微机械传感器性能的降低,同时由于玻璃-硅-玻璃三明治式结构内部空间狭小、结构相对较封闭,目前针对该种结构的牺牲层技术并不成熟,现在一些技术曾尝试引入二氧化硅牺牲层,但由于在去除牺牲层时对体硅有一定的损伤,大大增加了微硅器件的加工难度,致使微机械传感器普遍面临着加工难度大、加工成本高、成品率低等问题。In the microsilicon device method processed by the microelectronics and micromachining technology of the microelectromechanical system, the glass-silicon-glass three-layer flat plate structure is a typical structure of the micromechanical sensor processed by it, that is, in the silicon micromechanical device It usually contains a suspended mass that senses acceleration or force. This slightly sensitive suspended mass is generally etched from bulk silicon, which is limited to the existing bulk silicon processing technology in my country. During the processing process, the suspended mass has no or only With very small mechanical constraints, the micro-sensitive suspended mass can easily cause structural distortion during subsequent cleaning and processing, or enter and exit from the silicon cavity, resulting in degradation or destruction of device characteristics. There are two ways to solve this problem: increase the mechanical constraints of the micro-sensitive suspended structure during the design process and introduce sacrificial layers that are removed after processing. However, increasing the mechanical constraints will inevitably lead to a decrease in the performance of the micromechanical sensor. At the same time, due to the small internal space and relatively closed structure of the glass-silicon-glass sandwich structure, the current sacrificial layer technology for this structure is not mature. Now some Technology has tried to introduce a silicon dioxide sacrificial layer, but due to the certain damage to the bulk silicon when removing the sacrificial layer, the processing difficulty of micro-silicon devices has been greatly increased, resulting in micro-mechanical sensors generally facing difficulties in processing, high processing costs, Low yield and other issues.

发明内容 Contents of the invention

为了克服上述现有技术存在的不足,本发明的目的在于提供一种基于铝牺牲层工艺的悬浮微敏感结构制备工艺,通过在加工过程中对玻璃-硅-玻璃三层式的悬浮微敏感结构引入牺牲层对微敏感悬浮质量块加以约束,采用铝质薄膜将悬浮微敏感结构和体硅连接在一起,以避免后续加工对悬浮结构的影响,在完成后再用湿法刻蚀将牺牲层去除,最后用清水和乙醇将刻蚀溶剂置换出,将微其烘干;本方法在不改变原有工艺流程的基础上有效保证了悬浮微敏感结构的完整性和可动性,无须加大机械约束就不会引起微机械传感器性能的降低,同时降低了工艺难度、提高了成品率,可广泛使用于各种带有悬浮可动敏感结构的硅微器件加工。In order to overcome the deficiencies in the above-mentioned prior art, the object of the present invention is to provide a process for preparing a suspended micro-sensitive structure based on the aluminum sacrificial layer process, through the glass-silicon-glass three-layer suspended micro-sensitive structure in the process of processing Introduce a sacrificial layer to constrain the micro-sensitive suspended mass, and use an aluminum thin film to connect the suspended micro-sensitive structure and bulk silicon to avoid the impact of subsequent processing on the suspended structure. After completion, wet-etch the sacrificial layer Finally, replace the etching solvent with water and ethanol, and dry the microstructure; this method effectively ensures the integrity and mobility of the suspended microsensitive structure without changing the original process flow, and does not need to be enlarged. The mechanical constraint will not cause the degradation of the performance of the micromechanical sensor, and at the same time reduce the difficulty of the process and improve the yield, and can be widely used in the processing of various silicon microdevices with suspended movable sensitive structures.

为了达到上述目的,本发明所采用的技术方案是:In order to achieve the above object, the technical scheme adopted in the present invention is:

一种基于铝牺牲层工艺的悬浮微敏感结构制备方法,步骤如下:A method for preparing a suspended micro-sensitive structure based on an aluminum sacrificial layer process, the steps are as follows:

步骤1:用缓冲氟氢酸BHF湿法分别在顶层玻璃1和底层玻璃2的表面上刻蚀出一个以上的120~160nm深的电极凹槽3,每个电极凹槽3的外侧带有向外延伸的引线槽60,且按照从左到右的顺序,顶层玻璃1和底层玻璃2依次对应的每对电极凹槽3的大小和纵向位置一致,这样的每对电极凹槽3构成了差动电极凹槽,然后在每个电极凹槽3内溅射170~210nm厚的钛金合金,形成一个以上的电极41,并且在每个电极41的外侧面溅射出向外延伸的引线42进入对应的电极凹槽3的引线槽60,每个引线42的宽度不小于30μm,相邻引线42之间的间隔不小于10μm,这样就得到了带有电极41的顶层玻璃1和带有电极41的底层玻璃2,且每对差动电极凹槽3内的电极41及其引线42的数量、大小和位置也对应一致,该每对对应一致的电极41及其引线42构成一个差动电极4;Step 1: Etch more than one electrode groove 3 with a depth of 120 to 160 nm on the surface of the top glass 1 and the bottom glass 2 respectively by buffered hydrofluoric acid BHF wet method. Outwardly extending lead groove 60, and according to the order from left to right, the size and longitudinal position of each pair of electrode grooves 3 corresponding to the top glass 1 and the bottom glass 2 are consistent, such that each pair of electrode grooves 3 constitutes a differential Move the electrode groove, and then sputter 170-210nm thick titanium gold alloy in each electrode groove 3 to form more than one electrode 41, and sputter the lead wire 42 extending outward on the outer surface of each electrode 41 to enter Corresponding to the lead groove 60 of the electrode groove 3, the width of each lead 42 is not less than 30 μm, and the interval between adjacent lead wires 42 is not less than 10 μm, so that the top glass 1 with the electrode 41 and the top glass with the electrode 41 are obtained. The underlying glass 2, and the number, size and position of the electrodes 41 and their lead wires 42 in each pair of differential electrode grooves 3 are also correspondingly consistent, and each pair of correspondingly consistent electrodes 41 and their lead wires 42 constitutes a differential electrode 4 ;

步骤2:采用n型或p型、且电阻率为0.002~0.004Ω·cm的晶向单晶硅片5,进行标准清洗后,采用反应离子刻蚀RIE或感应耦合等离子体ICP干法在硅片5底表面进行刻蚀以形成一个以上的电极引线浅槽6,其深度为5~10μm,且按照从左到右的顺序,硅片5底表面的电极引线浅槽6能依次逐一容纳底层玻璃2中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗3-5分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3-5分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3-5分钟以去除硅片5上的金属玷污;Step 2: Use an n-type or p-type crystal-oriented single-crystal silicon wafer 5 with a resistivity of 0.002-0.004 Ω·cm. After standard cleaning, use reactive ion etching RIE or inductively coupled plasma ICP dry The bottom surface of the silicon wafer 5 is etched to form more than one electrode lead shallow groove 6, the depth of which is 5-10 μm, and in order from left to right, the electrode lead shallow grooves 6 on the bottom surface of the silicon wafer 5 can accommodate the bottom layers one by one. The lead 42 in the corresponding electrode groove 3 in the glass 2, and the protruding plane between each adjacent electrode lead shallow groove 6 constitutes the bonding table 52; wherein the standard cleaning is to use 80% pure sulfuric acid and 20% hydrogen peroxide mixed solution to clean the silicon chip 5 for 3-5 minutes to remove the organic matter on the silicon chip 5, then mix the ammonia water, hydrogen peroxide and pure water with a mass concentration of 60% according to the mass ratio of 1:1:5, and use The mixed solution cleans the silicon chip 5 for 3-5 minutes to remove the non-metallic contamination on the silicon chip 5, and finally mixes hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to the mass ratio of 1:1:5, and uses The mixed solution cleans the silicon wafer 5 for 3-5 minutes to remove metal contamination on the silicon wafer 5;

步骤3:接着对硅片5的底部表面以金属溅射的方式制作出一个以上的铝膜7作为牺牲层,这样就形成了带有铝膜7的硅片5,每个铝膜7的厚度为500~1000nm,所有铝膜的位置在硅片5的底部表面且在预设的悬浮微敏感结构51的边缘的纵向投影内;Step 3: then make more than one aluminum film 7 as a sacrificial layer on the bottom surface of the silicon wafer 5 by metal sputtering, thus forming a silicon wafer 5 with an aluminum film 7, the thickness of each aluminum film 7 500-1000nm, all aluminum films are located on the bottom surface of the silicon wafer 5 and within the preset vertical projection of the edge of the suspended micro-sensitive structure 51;

步骤4:用质量为80%的纯硫酸和20%双氧水相混合的溶液将带有铝膜7的硅片5清洗3-5分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗3-5分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗3-5分钟以去除硅片5上的金属玷污;然后进行底层玻璃-硅静电键合,即将带有铝膜7的硅片5和带有电极41的底层玻璃2接触在一起,且按照从左到右的顺序,该硅片5的底表面的电极引线浅槽6依次逐一和该底层玻璃2中对应的电极凹槽3相对,随后在350~450摄氏度下施加800~1500V的直流电压,硅片5连接直流电源正极,底层玻璃2连接直流电源的负极,接通该直流电压25~30分钟后键合完毕;Step 4: Clean the silicon chip 5 with the aluminum film 7 for 3-5 minutes with a mixed solution of 80% pure sulfuric acid and 20% hydrogen peroxide by mass to remove organic matter on the silicon chip 5, and then clean the silicon chip 5 with a mass concentration of 60% Ammonia, hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 is cleaned with the mixed solution for 3-5 minutes to remove non-metallic contamination on the silicon wafer 5, and finally Mix hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 with the aluminum film 7 for 3-5 minutes to remove the silicon wafer 5. metal pollution; then carry out the bottom glass-silicon electrostatic bonding, that is, the silicon wafer 5 with the aluminum film 7 and the bottom glass 2 with the electrode 41 are in contact together, and in order from left to right, the silicon wafer 5 The electrode lead shallow grooves 6 on the bottom surface of the bottom surface are in turn opposed to the corresponding electrode grooves 3 in the bottom glass 2 one by one, and then a DC voltage of 800-1500V is applied at 350-450 degrees Celsius, and the silicon chip 5 is connected to the positive pole of the DC power supply, and the bottom glass 2 Connect the negative pole of the DC power supply, and the bonding is completed after 25 to 30 minutes of switching on the DC voltage;

步骤5:底层玻璃-硅静电键合后,采用质量浓度为25%的四甲基氢氧化氨TMAH腐蚀液将该硅片5的厚度从其上端均匀腐蚀减薄至100~150μm,再使用质量浓度为25%的磷化液对该硅片5进行抛光,抛光时间为3-6分钟;Step 5: After the bottom glass-silicon is electrostatically bonded, the thickness of the silicon wafer 5 is uniformly etched and thinned from the upper end to 100-150 μm with a mass concentration of 25% tetramethylammonium hydroxide TMAH etching solution, and then used The silicon wafer 5 is polished with a phosphating solution with a concentration of 25%, and the polishing time is 3-6 minutes;

步骤6:采用反应离子刻蚀(RIE)或感应耦合等离子体(ICP)干法在该硅片5的上表面进行刻蚀以形成一个以上的电极引线浅槽6,其深度为5~10μm,且按照从左到右的顺序,硅片5上表面的电极引线浅槽6能依次逐一容纳顶层玻璃1中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗3-5分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3-5分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3-5分钟以去除硅片5上的金属玷污;Step 6: Reactive ion etching (RIE) or inductively coupled plasma (ICP) dry method is used to etch the upper surface of the silicon wafer 5 to form more than one electrode lead shallow groove 6, the depth of which is 5-10 μm, And according to the order from left to right, the shallow electrode lead grooves 6 on the upper surface of the silicon wafer 5 can accommodate the lead wires 42 in the corresponding electrode grooves 3 in the top glass 1 one by one, and each adjacent electrode lead shallow groove 6 The protruding planes in between constitute the bonding mesa 52; the standard cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 3-5 minutes to remove the organic matter on the silicon wafer 5, Next, mix ammonia water, hydrogen peroxide and pure water with a mass concentration of 60% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 3-5 minutes to remove non-metallic contamination on the silicon wafer 5, Finally, mix hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to a mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 3-5 minutes to remove metal contamination on the silicon wafer 5;

步骤7:接着采用感应耦合等离子体ICP干法,分别沿着预设的悬浮微敏感结构51的边缘及底层玻璃2的外侧带有向外延伸的引线槽60的电极凹槽3的边缘将该硅片5纵向刻透且不穿透铝膜7而形成悬浮微敏感结构51和导通硅54,硅片的其它部分为体硅53,该体硅53通过铝膜7和悬浮微敏感结构51相连接,另外在体硅53的侧面横向刻透出沟槽8,这样形成了带有悬浮微敏感结构51和导通硅54的底层玻璃-硅片组合片;Step 7: Then adopt the inductively coupled plasma ICP dry method, respectively place the electrode groove 3 along the edge of the preset floating micro-sensitive structure 51 and the edge of the electrode groove 3 with the outwardly extending lead groove 60 on the outside of the bottom glass 2. The silicon wafer 5 is carved vertically without penetrating the aluminum film 7 to form a suspended micro-sensing structure 51 and conductive silicon 54. The other parts of the silicon wafer are bulk silicon 53, and the bulk silicon 53 passes through the aluminum film 7 and the suspended micro-sensing structure 51. In addition, grooves 8 are carved laterally on the side of the bulk silicon 53, thus forming a bottom glass-silicon chip assembly with suspended micro-sensitive structures 51 and conductive silicon 54;

步骤8:对该底层玻璃-硅片组合片先用质量为80%的纯硫酸和20%双氧水相混合的溶液清洗3-5分钟以去除其上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗3-5分钟以去除其上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗3-5分钟以去除其上的金属玷污;然后进行顶层玻璃-硅静电键合,即将该底层玻璃-硅片组合片和带有电极41的顶层玻璃1接触在一起,且按照从左到右的顺序,该硅片5上表面的电极引线浅槽6依次逐一和该顶层玻璃1中对应的电极凹槽3相对,随后在350~450摄氏度下施加800~1500V的直流电压,体硅53连接直流电源正极,顶层玻璃1连接直流电源的负极,接通该直流电压25~30分钟后键合完毕得到三层式组合片;Step 8: Wash the bottom glass-silicon wafer combination sheet with a solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 3-5 minutes to remove organic matter on it, and then treat the ammonia water with a mass concentration of 60%, Hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer composite sheet is cleaned with the mixed solution for 3-5 minutes to remove the non-metallic contamination on it, and finally, the mass concentration is 30%. Hydrochloric acid, hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer assembly sheet is cleaned with the mixed solution for 3-5 minutes to remove the metal contamination on it; then the top glass -Silicon electrostatic bonding, that is, the bottom glass-silicon wafer composite sheet and the top glass 1 with electrodes 41 are in contact together, and in order from left to right, the electrode lead shallow grooves 6 on the upper surface of the silicon wafer 5 are sequentially One by one, it is opposite to the corresponding electrode grooves 3 in the top glass 1, and then a DC voltage of 800-1500V is applied at 350-450 degrees Celsius. The bulk silicon 53 is connected to the positive pole of the DC power supply, and the top glass 1 is connected to the negative pole of the DC power supply. After 25-30 minutes of DC voltage, the bonding is completed to obtain a three-layer composite sheet;

步骤9:将该三层式组合片浸入铝刻蚀剂中,加以超声波清洗20~30分钟,去除掉作为牺牲层的铝膜7,该铝刻蚀剂由质量质量浓度为85%的磷酸、质量浓度为70%的硝酸、乙酸以及水分别按照体积百分比10~30%、0.5~2%、5~10%以及60~80%的比例混合配比而成;Step 9: immerse the three-layer composite sheet in an aluminum etchant, and ultrasonically clean it for 20 to 30 minutes to remove the aluminum film 7 as a sacrificial layer. The aluminum etchant is composed of phosphoric acid with a mass concentration of 85%, Nitric acid, acetic acid and water with a mass concentration of 70% are mixed according to volume percentages of 10-30%, 0.5-2%, 5-10% and 60-80% respectively;

步骤10:随即将该三层式组合片从铝刻蚀剂中取出,在超声波环境中将其用清水清洗20~30分钟,置换出成悬浮微敏感结构51、导通硅54以及体硅53结构内部残留的反应物及铝刻蚀剂,再在超声波环境中将其用乙醇清洗10~30分钟置换出清水,这样就完成了基于铝牺牲层工艺的悬浮微敏感结构的制备。Step 10: Immediately take the three-layer composite chip out of the aluminum etchant, wash it with clean water for 20-30 minutes in an ultrasonic environment, and replace it with suspended micro-sensitive structure 51, conduction silicon 54 and bulk silicon 53 Residual reactants and aluminum etchant inside the structure are cleaned with ethanol for 10 to 30 minutes in an ultrasonic environment to replace clean water, thus completing the preparation of the suspended micro-sensitive structure based on the aluminum sacrificial layer process.

通过该方法在底层玻璃-硅静电键合后,在硅片5上加工出悬浮微敏感结构51之前,引入作为牺牲层的铝膜7就能将后续加工出来的悬浮微敏感结构51和体硅53连在一起,一方面防止在刻蚀过程中悬浮微敏感结构51脱落,另一方面在进行顶层玻璃-硅静电键合过程中提供一个和键合产生的静电力方向相反的弹性力,使悬浮微敏感结构51在键合过程中不被吸在顶层玻璃1上。加上最后用铝刻蚀剂可轻易去除作为牺牲层的铝膜7。另外铝刻蚀剂中的硝酸将铝氧化成三氧化二铝,然后磷酸将其溶解成磷酸盐,乙酸主要用于降低腐蚀液表面张力,增大铝膜表面和腐蚀液的浸润,提高腐蚀的均匀性,起到缓冲作用,本方案在不改变原有工艺流程的基础上有效保证了悬浮微敏感结构51的完整性和可动性,无须加大机械约束就不会引起微机械传感器性能的降低,同时降低了工艺难度、提高了成品率,可广泛使用于各种带有悬浮可动敏感结构的硅微器件加工。By this method, after the bottom glass-silicon is electrostatically bonded, and before the suspended microsensitive structure 51 is processed on the silicon wafer 5, the aluminum film 7 as a sacrificial layer is introduced so that the subsequently processed suspended microsensitive structure 51 and the bulk silicon 53 together, on the one hand to prevent the suspended micro-sensitive structure 51 from falling off during the etching process, and on the other hand to provide an elastic force opposite to the electrostatic force generated by the bonding during the top glass-silicon electrostatic bonding process, so that The suspended microsensitive structures 51 are not attracted to the top glass 1 during the bonding process. In addition, the aluminum film 7 serving as the sacrificial layer can be easily removed with an aluminum etchant at the end. In addition, nitric acid in the aluminum etchant oxidizes aluminum into aluminum oxide, and then phosphoric acid dissolves it into phosphate. Acetic acid is mainly used to reduce the surface tension of the corrosion solution, increase the infiltration of the aluminum film surface and the corrosion solution, and improve the corrosion resistance. Uniformity plays a buffer role. This solution effectively ensures the integrity and mobility of the suspended micro-sensitive structure 51 without changing the original process flow, and will not cause performance degradation of the micro-mechanical sensor without increasing mechanical constraints. It can be widely used in the processing of various silicon micro devices with suspended movable sensitive structures.

附图说明 Description of drawings

图1是本发明步骤1中的顶层玻璃和底层玻璃的状态示意图。Fig. 1 is a schematic view of the state of the top glass and the bottom glass in step 1 of the present invention.

图2是本发明步骤1中的顶层玻璃的一个电极凹槽的结构示意图。Fig. 2 is a structural schematic diagram of an electrode groove of the top glass in step 1 of the present invention.

图3是本发明步骤1中的底层玻璃的一个电极凹槽的结构示意图。Fig. 3 is a schematic structural view of an electrode groove of the bottom glass in step 1 of the present invention.

图4是本发明步骤3中的硅片的结构示意图。Fig. 4 is a schematic structural diagram of the silicon wafer in step 3 of the present invention.

图5是本发明步骤7中的形成悬浮微敏感结构的状态示意图。Fig. 5 is a schematic diagram of the state of forming the suspended micro-sensitive structure in step 7 of the present invention.

图6是本发明步骤7中的带有铝膜的局部仰视结构示意图。Fig. 6 is a schematic bottom view of a partial structure with an aluminum film in step 7 of the present invention.

图7是本发明步骤7中的带有悬浮微敏感结构的局部俯视结构示意图。Fig. 7 is a schematic diagram of a partial top view structure with a suspended micro-sensitive structure in step 7 of the present invention.

图8是本发明完成了基于铝牺牲层工艺的悬浮微敏感结构的制备的状态示意图。Fig. 8 is a schematic diagram of the state of the present invention having completed the preparation of the suspended micro-sensitive structure based on the aluminum sacrificial layer process.

具体实施方式 Detailed ways

下面结合实施例对本发明作更详细的说明。Below in conjunction with embodiment the present invention is described in more detail.

实施例1:Example 1:

本实施例的基于铝牺牲层工艺的悬浮微敏感结构制备方法,步骤如下:The preparation method of the suspended micro-sensitive structure based on the aluminum sacrificial layer technology in this embodiment, the steps are as follows:

步骤1:用缓冲氟氢酸BHF湿法分别在顶层玻璃1和底层玻璃2的表面上刻蚀出三个120nm深的电极凹槽3,每个电极凹槽3的外侧带有向外延伸的引线槽60,且按照从左到右的顺序,顶层玻璃1和底层玻璃2依次对应的每对电极凹槽3的大小和纵向位置一致,这样的每对电极凹槽3构成了差动电极凹槽,然后在每个电极凹槽3内溅射170nm厚的钛金合金,形成四个电极41,并且在每个电极41的外侧面溅射出向外延伸的引线42进入对应的电极凹槽3的引线槽60,每个引线42的宽度为35μm,相邻引线42之间的间隔为15μm,这样就得到了带有电极41的顶层玻璃1和带有电极41的底层玻璃2,且每对差动电极凹槽3内的电极41及其引线42的数量、大小和位置也对应一致,该每对对应一致的电极41及其引线42构成一个差动电极4如图1、图2和图3所示;Step 1: Etch three 120nm-deep electrode grooves 3 on the surface of the top glass 1 and the bottom glass 2 respectively with buffered hydrofluoric acid BHF wet method, each electrode groove 3 has an outwardly extending Lead groove 60, and in order from left to right, the size and longitudinal position of each pair of electrode grooves 3 corresponding to the top glass 1 and the bottom glass 2 are consistent, and each pair of electrode grooves 3 constitutes a differential electrode groove groove, and then sputter 170nm thick titanium gold alloy in each electrode groove 3 to form four electrodes 41, and sputter outwardly extending leads 42 into the corresponding electrode groove 3 on the outer side of each electrode 41 lead groove 60, the width of each lead 42 is 35 μm, and the interval between adjacent lead 42 is 15 μm, so just obtain the top glass 1 with electrode 41 and the bottom glass 2 with electrode 41, and each pair The number, size and position of the electrodes 41 and their lead wires 42 in the differential electrode groove 3 are also correspondingly consistent, and each pair of correspondingly consistent electrodes 41 and their lead wires 42 constitute a differential electrode 4 as shown in Figures 1, 2 and Fig. 3 shown;

步骤2:采用n型且电阻率为0.002Ω·cm的晶向单晶硅片5,进行标准清洗后,采用反应离子刻蚀RIE法在硅片5底表面进行刻蚀以形成三个电极引线浅槽6,其深度为5μm,且按照从左到右的顺序,硅片5底表面的电极引线浅槽6能依次逐一容纳底层玻璃2中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗3分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3分钟以去除硅片5上的金属玷污;Step 2: Use an n-type crystal-oriented single crystal silicon wafer 5 with a resistivity of 0.002Ω·cm, perform standard cleaning, and then etch the bottom surface of the silicon wafer 5 by reactive ion etching (RIE) to form three electrode leads The shallow groove 6 has a depth of 5 μm, and according to the order from left to right, the electrode lead shallow groove 6 on the bottom surface of the silicon wafer 5 can successively accommodate the lead wires 42 in the corresponding electrode grooves 3 in the bottom glass 2 one by one, and each The protruding planes between the adjacent electrode lead shallow grooves 6 constitute the bonding mesa 52; the standard cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 3 minutes to remove The organic matter on the silicon chip 5 is then mixed with ammonia water, hydrogen peroxide and pure water with a mass concentration of 60% in a mass ratio of 1:1:5, and the silicon chip 5 is cleaned for 3 minutes with the mixed solution to remove the organic matter on the silicon chip 5. Finally, mix hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 3 minutes to remove the metal on the silicon wafer 5 tarnish;

步骤3:接着对硅片5的底部表面以金属溅射的方式制作出四个铝膜7作为牺牲层,这样就形成了带有铝膜7的硅片5,每个铝膜7的厚度为500nm,所有铝膜的位置在硅片5的底部表面且在预设的悬浮微敏感结构51的边缘的纵向投影内如图4所示;Step 3: then make four aluminum films 7 as sacrificial layers to the bottom surface of the silicon wafer 5 by metal sputtering, so that the silicon wafer 5 with the aluminum films 7 is formed, and the thickness of each aluminum film 7 is 500nm, the positions of all aluminum films are on the bottom surface of the silicon wafer 5 and in the longitudinal projection of the edge of the preset suspended micro-sensitive structure 51 as shown in Figure 4;

步骤4:用质量为80%的纯硫酸和20%双氧水相混合的溶液将带有铝膜7的硅片5清洗3分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗3分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗3分钟以去除硅片5上的金属玷污;然后进行底层玻璃-硅静电键合,即将带有铝膜7的硅片5和带有电极41的底层玻璃2接触在一起,且按照从左到右的顺序,该硅片5的底表面的电极引线浅槽6依次逐一和该底层玻璃2中对应的电极凹槽3相对,随后在350摄氏度下施加800V的直流电压,硅片5连接直流电源正极,底层玻璃2连接直流电源的负极,接通该直流电压25分钟后键合完毕;Step 4: Clean the silicon chip 5 with the aluminum film 7 with a mixed solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 3 minutes to remove the organic matter on the silicon chip 5, and then treat the ammonia water with a mass concentration of 60%, Hydrogen peroxide and pure water were mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 was cleaned for 3 minutes with the mixed solution to remove the non-metallic contamination on the silicon wafer 5, and finally with a mass concentration of 30 % hydrochloric acid, hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 is cleaned for 3 minutes with the mixed solution to remove metal contamination on the silicon wafer 5; then Bottom glass-silicon electrostatic bonding, that is, the silicon chip 5 with the aluminum film 7 and the bottom glass 2 with the electrode 41 are in contact together, and in order from left to right, the electrode leads on the bottom surface of the silicon chip 5 The shallow grooves 6 are in turn opposed to the corresponding electrode grooves 3 in the bottom glass 2 one by one, and then a DC voltage of 800V is applied at 350 degrees Celsius, the silicon chip 5 is connected to the positive pole of the DC power supply, the bottom glass 2 is connected to the negative pole of the DC power supply, and the The bonding is completed after 25 minutes of DC voltage;

步骤5:底层玻璃-硅静电键合后,采用质量浓度为25%的四甲基氢氧化氨TMAH腐蚀液将该硅片5的厚度从其上端均匀腐蚀减薄至100μm,再使用质量浓度为25%的磷化液对该硅片5进行抛光,抛光时间为3分钟;Step 5: After the bottom glass-silicon is electrostatically bonded, the thickness of the silicon wafer 5 is uniformly etched from its upper end to 100 μm by using a tetramethylammonium hydroxide TMAH etching solution with a mass concentration of 25%, and then using a mass concentration of 25% phosphating solution is used to polish the silicon wafer 5, and the polishing time is 3 minutes;

步骤6:采用反应离子刻蚀RIE法在该硅片5的上表面进行刻蚀以形成一个以上的电极引线浅槽6,其深度为5μm,且按照从左到右的顺序,硅片5上表面的电极引线浅槽6能依次逐一容纳顶层玻璃1中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗3分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗3分钟以去除硅片5上的金属玷污;Step 6: Reactive ion etching (RIE) is used to etch the upper surface of the silicon wafer 5 to form more than one electrode lead shallow groove 6, the depth of which is 5 μm, and in order from left to right, on the silicon wafer 5 The electrode lead shallow grooves 6 on the surface can successively accommodate the leads 42 in the corresponding electrode grooves 3 in the top glass 1 one by one, and the protruding planes between each adjacent electrode lead shallow grooves 6 constitute a bonding table 52; Cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 3 minutes to remove the organic matter on the silicon wafer 5, and then use a mass concentration of 60% ammonia water, hydrogen peroxide and pure water according to the mass concentration. The ratio of 1: 1: 5 was mixed, and the silicon chip 5 was cleaned for 3 minutes with the mixed solution to remove the non-metallic pollution on the silicon chip 5, and finally the hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% were used according to the mass ratio of 1 : 1:5, and the silicon wafer 5 was cleaned for 3 minutes with the mixed solution to remove metal contamination on the silicon wafer 5;

步骤7:接着采用感应耦合等离子体ICP干法,分别沿着预设的悬浮微敏感结构51的边缘及底层玻璃2的外侧带有向外延伸的引线槽60的电极凹槽3的边缘将该硅片5纵向刻透且不穿透铝膜7而形成悬浮微敏感结构51和导通硅54,硅片的其它部分为体硅53,该体硅53通过铝膜7和悬浮微敏感结构51相连接,另外在体硅53的侧面横向刻透出沟槽8,这样形成了带有悬浮微敏感结构51和导通硅54的底层玻璃-硅片组合片如图5、图6及图7所示;Step 7: Then adopt the inductively coupled plasma ICP dry method, respectively place the electrode groove 3 along the edge of the preset floating micro-sensitive structure 51 and the edge of the electrode groove 3 with the outwardly extending lead groove 60 on the outside of the bottom glass 2. The silicon wafer 5 is carved vertically without penetrating the aluminum film 7 to form a suspended micro-sensing structure 51 and conductive silicon 54. The other parts of the silicon wafer are bulk silicon 53, and the bulk silicon 53 passes through the aluminum film 7 and the suspended micro-sensing structure 51. In addition, grooves 8 are carved laterally on the side of the bulk silicon 53, thus forming a bottom glass-silicon chip assembly with a suspended micro-sensitive structure 51 and conductive silicon 54, as shown in Figure 5, Figure 6 and Figure 7 shown;

步骤8:对该底层玻璃-硅片组合片先用质量为80%的纯硫酸和20%双氧水相混合的溶液清洗3分钟以去除其上的有机物,接着对浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗3分钟以去除其上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗3分钟以去除其上的金属玷污;然后进行顶层玻璃-硅静电键合,即将该底层玻璃-硅片组合片和带有电极41的顶层玻璃1接触在一起,且按照从左到右的顺序,该硅片5上表面的电极引线浅槽6依次逐一和该顶层玻璃1中对应的电极凹槽3相对,随后在350摄氏度下施加800V的直流电压,体硅53连接直流电源正极,顶层玻璃1连接直流电源的负极,接通该直流电压25分钟后键合完毕得到三层式组合片;Step 8: Clean the underlying glass-silicon chip combination with a solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 3 minutes to remove the organic matter on it, and then wash it with 60% ammonia water, hydrogen peroxide and pure Water is mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon chip assembly sheet is cleaned with the mixed solution for 3 minutes to remove the non-metallic contamination on it, and finally with 30% mass concentration of hydrochloric acid, hydrogen peroxide and Pure water is mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer assembly is cleaned with the mixed solution for 3 minutes to remove the metal contamination on it; then the top glass-silicon electrostatic bonding is carried out, that is, The bottom glass-silicon chip combination sheet is in contact with the top glass 1 with electrodes 41, and in the order from left to right, the electrode lead shallow grooves 6 on the upper surface of the silicon chip 5 are connected to the top glass 1 one by one. The corresponding electrode grooves 3 are facing each other, and then a DC voltage of 800V is applied at 350 degrees Celsius. The bulk silicon 53 is connected to the positive pole of the DC power supply, and the top glass 1 is connected to the negative pole of the DC power supply. After the DC voltage is turned on for 25 minutes, the bonding is completed to obtain three layers. combination piece;

步骤9:将该三层式组合片浸入铝刻蚀剂中,加以超声波清洗20分钟,去除掉作为牺牲层的铝膜7,该铝刻蚀剂由质量浓度为85%的磷酸、质量浓度为70%的硝酸、乙酸以及水分别按照体积百分比10%、0.5%、9.5%以及80%的比例混合配比而成;Step 9: immerse the three-layer composite sheet in an aluminum etchant, and ultrasonically clean it for 20 minutes to remove the aluminum film 7 as a sacrificial layer. The aluminum etchant is composed of phosphoric acid with a mass concentration of 85% and a mass concentration of 70% nitric acid, acetic acid and water are mixed according to volume percentage of 10%, 0.5%, 9.5% and 80% respectively;

步骤10:随即将该三层式组合片从铝刻蚀剂中取出,在超声波环境中将其用清水清洗20分钟,置换出成悬浮微敏感结构51、导通硅54以及体硅53结构内部残留的反应物及铝刻蚀剂,再在超声波环境中将其用乙醇清洗10分钟置换出清水,这样就完成了基于铝牺牲层工艺的悬浮微敏感结构的制备如图8所示。Step 10: Immediately take the three-layer composite chip out of the aluminum etchant, wash it with clean water for 20 minutes in an ultrasonic environment, and replace it with suspended micro-sensitive structure 51, conduction silicon 54 and bulk silicon 53 inside the structure The remaining reactants and aluminum etchant were cleaned with ethanol for 10 minutes in an ultrasonic environment to replace water, thus completing the preparation of the suspended micro-sensitive structure based on the aluminum sacrificial layer process, as shown in Figure 8.

实施例2:Example 2:

本实施例的基于铝牺牲层工艺的悬浮微敏感结构制备方法,步骤如下:The preparation method of the suspended micro-sensitive structure based on the aluminum sacrificial layer technology in this embodiment, the steps are as follows:

步骤1:用缓冲氟氢酸BHF湿法分别在顶层玻璃1和底层玻璃2的表面上刻蚀出三个140nm深的电极凹槽3,每个电极凹槽3的外侧带有向外延伸的引线槽60,且按照从左到右的顺序,顶层玻璃1和底层玻璃2依次对应的每对电极凹槽3的大小和纵向位置一致,这样的每对电极凹槽3构成了差动电极凹槽,然后在每个电极凹槽3内溅射190nm厚的钛金合金,形成四个电极41,并且在每个电极41的外侧面溅射出向外延伸的引线42进入对应的电极凹槽3的引线槽60,每个引线42的宽度为40μm,相邻引线42之间的间隔为20μm,这样就得到了带有电极41的顶层玻璃1和带有电极41的底层玻璃2,且每对差动电极凹槽3内的电极41及其引线42的数量、大小和位置也对应一致,该每对对应一致的电极41及其引线42构成一个差动电极4如图1、图2和图3所示;Step 1: Etch three 140nm-deep electrode grooves 3 on the surface of the top glass 1 and the bottom glass 2 respectively with buffered hydrofluoric acid BHF wet method, each electrode groove 3 has an outwardly extending Lead groove 60, and in order from left to right, the size and longitudinal position of each pair of electrode grooves 3 corresponding to the top glass 1 and the bottom glass 2 are consistent, and each pair of electrode grooves 3 constitutes a differential electrode groove groove, and then sputter 190nm thick titanium gold alloy in each electrode groove 3 to form four electrodes 41, and sputter outwardly extending leads 42 into the corresponding electrode groove 3 on the outer side of each electrode 41 lead groove 60, the width of each lead 42 is 40 μm, and the interval between adjacent lead 42 is 20 μm, so just obtain the top glass 1 with electrode 41 and the bottom glass 2 with electrode 41, and each pair The number, size and position of the electrodes 41 and their lead wires 42 in the differential electrode groove 3 are also correspondingly consistent, and each pair of correspondingly consistent electrodes 41 and their lead wires 42 constitute a differential electrode 4 as shown in Figures 1, 2 and Fig. 3 shown;

步骤2:采用n型且电阻率为0.002Ω·cm的晶向单晶硅片5,进行标准清洗后,采用感应耦合等离子体ICP干法在硅片5底表面进行刻蚀以形成三个电极引线浅槽6,其深度为7μm,且按照从左到右的顺序,硅片5底表面的电极引线浅槽6能依次逐一容纳底层玻璃2中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗4分钟以去除硅片5上的有机物,接着对浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗4分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗4分钟以去除硅片5上的金属玷污;Step 2: Use an n-type crystal-oriented single-crystal silicon wafer 5 with a resistivity of 0.002Ω·cm, perform standard cleaning, and etch the bottom surface of the silicon wafer 5 by inductively coupled plasma ICP dry method to form three electrodes Lead wire shallow groove 6, its depth is 7 μ m, and according to the order from left to right, the electrode lead wire shallow groove 6 on the bottom surface of silicon chip 5 can accommodate the lead wire 42 in the corresponding electrode groove 3 in the bottom glass 2 one by one, and The protruding plane between each adjacent electrode lead shallow groove 6 constitutes the bonding table top 52; wherein the standard cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 4 minutes. Remove the organic matter on the silicon wafer 5, then mix the ammonia water, hydrogen peroxide and pure water with a concentration of 60% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 4 minutes to remove the silicon wafer 5. Finally, mix hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 4 minutes to remove the metal on the silicon wafer 5 tarnish;

步骤3:接着对硅片5的底部表面以金属溅射的方式制作出四个铝膜7作为牺牲层,这样就形成了带有铝膜7的硅片5,每个铝膜7的厚度为700nm,所有铝膜的位置在硅片5的底部表面且在预设的悬浮微敏感结构51的边缘的纵向投影内如图4所示;Step 3: then make four aluminum films 7 as sacrificial layers to the bottom surface of the silicon wafer 5 by metal sputtering, so that the silicon wafer 5 with the aluminum films 7 is formed, and the thickness of each aluminum film 7 is 700nm, the positions of all aluminum films are on the bottom surface of the silicon wafer 5 and in the vertical projection of the edge of the preset suspended micro-sensitive structure 51 as shown in Figure 4;

步骤4:用质量为80%的纯硫酸和20%双氧水相混合的溶液将带有铝膜7的硅片5清洗4分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗4分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗4分钟以去除硅片5上的金属玷污;然后进行底层玻璃-硅静电键合,即将带有铝膜7的硅片5和带有电极41的底层玻璃2接触在一起,且按照从左到右的顺序,该硅片5的底表面的电极引线浅槽6依次逐一和该底层玻璃2中对应的电极凹槽3相对,随后在400摄氏度下施加1000V的直流电压,硅片5连接直流电源正极,底层玻璃2连接直流电源的负极,接通该直流电压28分钟后键合完毕;Step 4: Clean the silicon wafer 5 with the aluminum film 7 with a mixed solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 4 minutes to remove the organic matter on the silicon wafer 5, and then treat the ammonia water with a mass concentration of 60%, Hydrogen peroxide and pure water were mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 was cleaned for 4 minutes with the mixed solution to remove the non-metallic contamination on the silicon wafer 5, and finally with a mass concentration of 30 % hydrochloric acid, hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 is cleaned for 4 minutes with the mixed solution to remove metal contamination on the silicon wafer 5; then Bottom glass-silicon electrostatic bonding, that is, the silicon chip 5 with the aluminum film 7 and the bottom glass 2 with the electrode 41 are in contact together, and in order from left to right, the electrode leads on the bottom surface of the silicon chip 5 The shallow grooves 6 are in turn opposed to the corresponding electrode grooves 3 in the bottom glass 2 one by one, and then a DC voltage of 1000V is applied at 400 degrees Celsius, the silicon wafer 5 is connected to the positive pole of the DC power supply, the bottom glass 2 is connected to the negative pole of the DC power supply, and the The bonding is completed after 28 minutes of DC voltage;

步骤5:底层玻璃-硅静电键合后,采用质量浓度为25%的四甲基氢氧化氨TMAH腐蚀液将该硅片5的厚度从其上端均匀腐蚀减薄至100μm,再使用质量浓度为25%的磷化液对该硅片5进行抛光,抛光时间为5分钟;Step 5: After the bottom glass-silicon is electrostatically bonded, the thickness of the silicon wafer 5 is uniformly etched from its upper end to 100 μm by using a tetramethylammonium hydroxide TMAH etching solution with a mass concentration of 25%, and then using a mass concentration of 25% phosphating solution is used to polish the silicon wafer 5, and the polishing time is 5 minutes;

步骤6:采用反应离子刻蚀RIE法在该硅片5的上表面进行刻蚀以形成一个以上的电极引线浅槽6,其深度为8μm,且按照从左到右的顺序,硅片5上表面的电极引线浅槽6能依次逐一容纳顶层玻璃1中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗4分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗4分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗4分钟以去除硅片5上的金属玷污;Step 6: Reactive ion etching (RIE) is used to etch the upper surface of the silicon wafer 5 to form more than one electrode lead shallow groove 6, the depth of which is 8 μm, and in order from left to right, on the silicon wafer 5 The electrode lead shallow grooves 6 on the surface can successively accommodate the leads 42 in the corresponding electrode grooves 3 in the top glass 1 one by one, and the protruding planes between each adjacent electrode lead shallow grooves 6 constitute a bonding table 52; Cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 4 minutes to remove the organic matter on the silicon wafer 5, and then use a mass concentration of 60% ammonia water, hydrogen peroxide and pure water according to the mass concentration. The ratio of 1: 1: 5 was mixed, and the silicon wafer 5 was cleaned for 4 minutes with the mixed solution to remove the non-metallic contamination on the silicon wafer 5, and finally the hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% were used according to the mass ratio of 1 : 1:5, the silicon wafer 5 was cleaned for 4 minutes with the mixed solution to remove metal contamination on the silicon wafer 5;

步骤7:接着采用感应耦合等离子体ICP干法,分别沿着预设的悬浮微敏感结构51的边缘及底层玻璃2的外侧带有向外延伸的引线槽60的电极凹槽3的边缘将该硅片5纵向刻透且不穿透铝膜7而形成悬浮微敏感结构51和导通硅54,硅片的其它部分为体硅53,该体硅53通过铝膜7和悬浮微敏感结构51相连接,另外在体硅53的侧面横向刻透出沟槽8,这样形成了带有悬浮微敏感结构51和导通硅54的底层玻璃-硅片组合片如图5、图6及图7所示;Step 7: Then adopt the inductively coupled plasma ICP dry method, respectively place the electrode groove 3 along the edge of the preset floating micro-sensitive structure 51 and the edge of the electrode groove 3 with the outwardly extending lead groove 60 on the outside of the bottom glass 2. The silicon wafer 5 is carved vertically without penetrating the aluminum film 7 to form a suspended micro-sensing structure 51 and conductive silicon 54. The other parts of the silicon wafer are bulk silicon 53, and the bulk silicon 53 passes through the aluminum film 7 and the suspended micro-sensing structure 51. In addition, grooves 8 are carved laterally on the side of the bulk silicon 53, thus forming a bottom glass-silicon chip assembly with a suspended micro-sensitive structure 51 and conductive silicon 54, as shown in Figure 5, Figure 6 and Figure 7 shown;

步骤8:对该底层玻璃-硅片组合片先用质量为80%的纯硫酸和20%双氧水相混合的溶液清洗4分钟以去除其上的有机物,接着对浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗4分钟以去除其上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗4分钟以去除其上的金属玷污;然后进行顶层玻璃-硅静电键合,即将该底层玻璃-硅片组合片和带有电极41的顶层玻璃1接触在一起,且按照从左到右的顺序,该硅片5上表面的电极引线浅槽6依次逐一和该顶层玻璃1中对应的电极凹槽3相对,随后在400摄氏度下施加1000V的直流电压,体硅53连接直流电源正极,顶层玻璃1连接直流电源的负极,接通该直流电压28分钟后键合完毕得到三层式组合片;Step 8: Clean the bottom glass-silicon chip combination with a solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 4 minutes to remove the organic matter on it, and then wash it with 60% ammonia water, hydrogen peroxide and pure Water is mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon chip assembly sheet is cleaned with the mixed solution for 4 minutes to remove the non-metallic contamination on it, and finally with 30% mass concentration of hydrochloric acid, hydrogen peroxide and Pure water is mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer assembly is cleaned with the mixed solution for 4 minutes to remove the metal contamination on it; then the top glass-silicon electrostatic bonding is carried out, that is, The bottom glass-silicon chip combination sheet is in contact with the top glass 1 with electrodes 41, and in the order from left to right, the electrode lead shallow grooves 6 on the upper surface of the silicon chip 5 are connected to the top glass 1 one by one. The corresponding electrode grooves 3 are facing each other, and then a DC voltage of 1000V is applied at 400 degrees Celsius. The bulk silicon 53 is connected to the positive pole of the DC power supply, and the top glass 1 is connected to the negative pole of the DC power supply. After 28 minutes of connecting the DC voltage, the bonding is completed to obtain three layers. combination piece;

步骤9:将该三层式组合片浸入铝刻蚀剂中,加以超声波清洗20分钟,去除掉作为牺牲层的铝膜7,该铝刻蚀剂由质量浓度为85%的磷酸、质量浓度为70%的硝酸、乙酸以及水分别按照体积百分比15%、0.5%、4.5%以及80%的比例混合配比而成;Step 9: immerse the three-layer composite sheet in an aluminum etchant, and ultrasonically clean it for 20 minutes to remove the aluminum film 7 as a sacrificial layer. The aluminum etchant is composed of phosphoric acid with a mass concentration of 85% and a mass concentration of 70% nitric acid, acetic acid and water are mixed according to volume percentage of 15%, 0.5%, 4.5% and 80% respectively;

步骤10:随即将该三层式组合片从铝刻蚀剂中取出,在超声波环境中将其用清水清洗20分钟,置换出成悬浮微敏感结构51、导通硅54以及体硅53结构内部残留的反应物及铝刻蚀剂,再在超声波环境中将其用乙醇清洗10分钟置换出清水,这样就完成了基于铝牺牲层工艺的悬浮微敏感结构的制备如图8所示。Step 10: Immediately take the three-layer composite chip out of the aluminum etchant, wash it with clean water for 20 minutes in an ultrasonic environment, and replace it with suspended micro-sensitive structure 51, conduction silicon 54 and bulk silicon 53 inside the structure The remaining reactants and aluminum etchant were cleaned with ethanol for 10 minutes in an ultrasonic environment to replace water, thus completing the preparation of the suspended micro-sensitive structure based on the aluminum sacrificial layer process, as shown in Figure 8.

实施例3:Example 3:

本实施例的基于铝牺牲层工艺的悬浮微敏感结构制备方法,步骤如下:The preparation method of the suspended micro-sensitive structure based on the aluminum sacrificial layer technology in this embodiment, the steps are as follows:

步骤1:用缓冲氟氢酸BHF湿法分别在顶层玻璃1和底层玻璃2的表面上刻蚀出三个155nm深的电极凹槽3,每个电极凹槽3的外侧带有向外延伸的引线槽60,且按照从左到右的顺序,顶层玻璃1和底层玻璃2依次对应的每对电极凹槽3的大小和纵向位置一致,这样的每对电极凹槽3构成了差动电极凹槽,然后在每个电极凹槽3内溅射205nm厚的钛金合金,形成四个电极41,并且在每个电极41的外侧面溅射出向外延伸的引线42进入对应的电极凹槽3的引线槽60,每个引线42的宽度为45μm,相邻引线42之间的间隔为25μm,这样就得到了带有电极41的顶层玻璃1和带有电极41的底层玻璃2,且每对差动电极凹槽3内的电极41及其引线42的数量、大小和位置也对应一致,该每对对应一致的电极41及其引线42构成一个差动电极4如图1、图2和图3所示;Step 1: Etch three 155nm-deep electrode grooves 3 on the surface of the top glass 1 and the bottom glass 2 respectively with buffered hydrofluoric acid BHF wet method, and the outer side of each electrode groove 3 has an outwardly extending Lead groove 60, and in order from left to right, the size and longitudinal position of each pair of electrode grooves 3 corresponding to the top glass 1 and the bottom glass 2 are consistent, and each pair of electrode grooves 3 constitutes a differential electrode groove groove, and then sputter 205nm thick titanium gold alloy in each electrode groove 3 to form four electrodes 41, and sputter outwardly extending leads 42 into the corresponding electrode groove 3 on the outer side of each electrode 41 lead groove 60, the width of each lead 42 is 45 μm, and the interval between adjacent lead 42 is 25 μm, so just obtain the top glass 1 with electrode 41 and the bottom glass 2 with electrode 41, and each pair The number, size and position of the electrodes 41 and their lead wires 42 in the differential electrode groove 3 are also correspondingly consistent, and each pair of correspondingly consistent electrodes 41 and their lead wires 42 constitute a differential electrode 4 as shown in Figures 1, 2 and Fig. 3 shown;

步骤2:采用n型且电阻率为0.003Ω·cm的晶向单晶硅片5,进行标准清洗后,采用感应耦合等离子体ICP干法在硅片5底表面进行刻蚀以形成三个电极引线浅槽6,其深度为9μm,且按照从左到右的顺序,硅片5底表面的电极引线浅槽6能依次逐一容纳底层玻璃2中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗5分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗5分钟以去除硅片5上的非金属玷污,最后用对质量质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗5分钟以去除硅片5上的金属玷污;Step 2: Use an n-type crystal-oriented monocrystalline silicon wafer 5 with a resistivity of 0.003Ω·cm, perform standard cleaning, and etch the bottom surface of the silicon wafer 5 by inductively coupled plasma ICP dry method to form three electrodes Lead wire shallow groove 6, its depth is 9 μm, and according to the order from left to right, the electrode lead wire shallow groove 6 on the bottom surface of silicon wafer 5 can accommodate the lead wire 42 in the corresponding electrode groove 3 in the bottom glass 2 one by one, and The protruding plane between each adjacent electrode lead shallow groove 6 constitutes the bonding table top 52; wherein the standard cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 5 minutes. Remove the organic matter on the silicon wafer 5, then mix ammonia water, hydrogen peroxide, and pure water with a mass concentration of 60% in a mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 5 minutes to remove the silicon wafer 5. For non-metallic contamination on the surface, finally mix hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer 5 for 5 minutes to remove the silicon wafer 5 metal contamination on

步骤3:接着对硅片5的底部表面以金属溅射的方式制作出四个铝膜7作为牺牲层,这样就形成了带有铝膜7的硅片5,每个铝膜7的厚度为900nm,所有铝膜的位置在硅片5的底部表面且在预设的悬浮微敏感结构51的边缘的纵向投影内如图4所示;Step 3: then make four aluminum films 7 as sacrificial layers to the bottom surface of the silicon wafer 5 by metal sputtering, so that the silicon wafer 5 with the aluminum films 7 is formed, and the thickness of each aluminum film 7 is 900nm, the positions of all aluminum films are on the bottom surface of the silicon wafer 5 and in the longitudinal projection of the edge of the preset suspended micro-sensitive structure 51 as shown in Figure 4;

步骤4:用质量为80%的纯硫酸和20%双氧水相混合的溶液将带有铝膜7的硅片5清洗4分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗4分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜7的硅片5清洗4分钟以去除硅片5上的金属玷污;然后进行底层玻璃-硅静电键合,即将带有铝膜7的硅片5和带有电极41的底层玻璃2接触在一起,且按照从左到右的顺序,该硅片5的底表面的电极引线浅槽6依次逐一和该底层玻璃2中对应的电极凹槽3相对,随后在420摄氏度下施加1300V的直流电压,硅片5连接直流电源正极,底层玻璃2连接直流电源的负极,接通该直流电压29分钟后键合完毕;Step 4: Clean the silicon wafer 5 with the aluminum film 7 with a mixed solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 4 minutes to remove the organic matter on the silicon wafer 5, and then treat the ammonia water with a mass concentration of 60%, Hydrogen peroxide and pure water were mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 was cleaned for 4 minutes with the mixed solution to remove the non-metallic contamination on the silicon wafer 5, and finally with a mass concentration of 30 % hydrochloric acid, hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the silicon wafer 5 with the aluminum film 7 is cleaned for 4 minutes with the mixed solution to remove metal contamination on the silicon wafer 5; then Bottom glass-silicon electrostatic bonding, that is, the silicon chip 5 with the aluminum film 7 and the bottom glass 2 with the electrode 41 are in contact together, and in order from left to right, the electrode leads on the bottom surface of the silicon chip 5 The shallow grooves 6 are opposed to the corresponding electrode grooves 3 in the bottom glass 2 one by one, and then a DC voltage of 1300V is applied at 420 degrees Celsius. The silicon wafer 5 is connected to the positive pole of the DC power supply, and the bottom glass 2 is connected to the negative pole of the DC power supply. The bonding is completed after 29 minutes of DC voltage;

步骤5:底层玻璃-硅静电键合后,采用质量浓度为25%的四甲基氢氧化氨TMAH腐蚀液将该硅片5的厚度从其上端均匀腐蚀减薄至100μm,再使用质量浓度为25%的磷化液对该硅片5进行抛光,抛光时间为6分钟;Step 5: After the bottom glass-silicon is electrostatically bonded, the thickness of the silicon wafer 5 is uniformly etched from its upper end to 100 μm by using a tetramethylammonium hydroxide TMAH etching solution with a mass concentration of 25%, and then using a mass concentration of 25% phosphating solution is used to polish the silicon wafer 5, and the polishing time is 6 minutes;

步骤6:采用反应离子刻蚀RIE法在该硅片5的上表面进行刻蚀以形成一个以上的电极引线浅槽6,其深度为8μm,且按照从左到右的顺序,硅片5上表面的电极引线浅槽6能依次逐一容纳顶层玻璃1中对应的电极凹槽3内的引线42,而各个相邻的电极引线浅槽6之间的突起平面构成了键合台面52;其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片5清洗4分钟以去除硅片5上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗4分钟以去除硅片5上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片5清洗4分钟以去除硅片5上的金属玷污;Step 6: Reactive ion etching (RIE) is used to etch the upper surface of the silicon wafer 5 to form more than one electrode lead shallow groove 6, the depth of which is 8 μm, and in order from left to right, on the silicon wafer 5 The electrode lead shallow grooves 6 on the surface can successively accommodate the leads 42 in the corresponding electrode grooves 3 in the top glass 1 one by one, and the protruding planes between each adjacent electrode lead shallow grooves 6 constitute a bonding table 52; Cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer 5 for 4 minutes to remove the organic matter on the silicon wafer 5, and then use a mass concentration of 60% ammonia water, hydrogen peroxide and pure water according to the mass concentration. The ratio of 1: 1: 5 was mixed, and the silicon wafer 5 was cleaned for 4 minutes with the mixed solution to remove the non-metallic contamination on the silicon wafer 5, and finally the hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% were used according to the mass ratio of 1 : 1:5, the silicon wafer 5 was cleaned for 4 minutes with the mixed solution to remove metal contamination on the silicon wafer 5;

步骤7:接着采用感应耦合等离子体ICP干法,分别沿着预设的悬浮微敏感结构51的边缘及底层玻璃2的外侧带有向外延伸的引线槽60的电极凹槽3的边缘将该硅片5纵向刻透且不穿透铝膜7而形成悬浮微敏感结构51和导通硅54,硅片的其它部分为体硅53,该体硅53通过铝膜7和悬浮微敏感结构51相连接,另外在体硅53的侧面横向刻透出沟槽8,这样形成了带有悬浮微敏感结构51和导通硅54的底层玻璃-硅片组合片如图5、图6及图7所示;Step 7: Then adopt the inductively coupled plasma ICP dry method, respectively place the electrode groove 3 along the edge of the preset floating micro-sensitive structure 51 and the edge of the electrode groove 3 with the outwardly extending lead groove 60 on the outside of the bottom glass 2. The silicon wafer 5 is carved vertically without penetrating the aluminum film 7 to form a suspended micro-sensing structure 51 and conductive silicon 54. The other parts of the silicon wafer are bulk silicon 53, and the bulk silicon 53 passes through the aluminum film 7 and the suspended micro-sensing structure 51. In addition, grooves 8 are carved laterally on the side of the bulk silicon 53, thus forming a bottom glass-silicon chip assembly with a suspended micro-sensitive structure 51 and conductive silicon 54, as shown in Figure 5, Figure 6 and Figure 7 shown;

步骤8:对该底层玻璃-硅片组合片先用质量为80%的纯硫酸和20%双氧水相混合的溶液清洗4分钟以去除其上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗4分钟以去除其上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗4分钟以去除其上的金属玷污;然后进行顶层玻璃-硅静电键合,即将该底层玻璃-硅片组合片和带有电极41的顶层玻璃1接触在一起,且按照从左到右的顺序,该硅片5上表面的电极引线浅槽6依次逐一和该顶层玻璃1中对应的电极凹槽3相对,随后在400摄氏度下施加1000V的直流电压,体硅53连接直流电源正极,顶层玻璃1连接直流电源的负极,接通该直流电压28分钟后键合完毕得到三层式组合片;Step 8: Wash the bottom glass-silicon chip combination with a solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 4 minutes to remove the organic matter on it, and then wash it with 60% ammonia water, hydrogen peroxide and Pure water is mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer composite sheet is cleaned with the mixed solution for 4 minutes to remove the non-metallic contamination on it, and finally the hydrochloric acid and hydrogen peroxide with a mass concentration of 30% and pure water are mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer assembly is cleaned with the mixed solution for 4 minutes to remove the metal contamination on it; then the top glass-silicon electrostatic bonding is carried out, That is to say, the bottom glass-silicon wafer composite sheet is in contact with the top glass 1 with electrodes 41, and in order from left to right, the electrode lead shallow grooves 6 on the upper surface of the silicon wafer 5 are successively connected to the top glass 1 one by one. The corresponding electrode grooves 3 are opposite to each other, and then a DC voltage of 1000V is applied at 400 degrees Celsius. The bulk silicon 53 is connected to the positive pole of the DC power supply, and the top glass 1 is connected to the negative pole of the DC power supply. After 28 minutes of connecting the DC voltage, the bonding is completed to obtain three Layered combination sheet;

步骤9:将该三层式组合片浸入铝刻蚀剂中,加以超声波清洗20分钟,去除掉作为牺牲层的铝膜7,该铝刻蚀剂由质量浓度为85%的磷酸、质量浓度为70%的硝酸、乙酸以及水分别按照体积百分比15%、0.5%、4.5%以及80%的比例混合配比而成;Step 9: immerse the three-layer composite sheet in an aluminum etchant, and ultrasonically clean it for 20 minutes to remove the aluminum film 7 as a sacrificial layer. The aluminum etchant is composed of phosphoric acid with a mass concentration of 85% and a mass concentration of 70% nitric acid, acetic acid and water are mixed according to volume percentage of 15%, 0.5%, 4.5% and 80% respectively;

步骤10:随即将该三层式组合片从铝刻蚀剂中取出,在超声波环境中将其用清水清洗20分钟,置换出成悬浮微敏感结构51、导通硅54以及体硅53结构内部残留的反应物及铝刻蚀剂,再在超声波环境中将其用乙醇清洗10分钟置换出清水,这样就完成了基于铝牺牲层工艺的悬浮微敏感结构的制备如图8所示。Step 10: Immediately take the three-layer composite chip out of the aluminum etchant, wash it with clean water for 20 minutes in an ultrasonic environment, and replace it with suspended micro-sensitive structure 51, conduction silicon 54 and bulk silicon 53 inside the structure The remaining reactants and aluminum etchant were cleaned with ethanol for 10 minutes in an ultrasonic environment to replace water, thus completing the preparation of the suspended micro-sensitive structure based on the aluminum sacrificial layer process, as shown in Figure 8.

通过实施例1、实施例2以及实施例3的基于铝牺牲层工艺的悬浮微敏感结构制备方法,其在底层玻璃-硅静电键合后,在硅片5上加工出悬浮微敏感结构51之前,引入作为牺牲层的铝膜7就能将后续加工出来的悬浮微敏感结构51和体硅53连在一起,一方面防止在刻蚀过程中悬浮微敏感结构51脱落,另一方面在进行顶层玻璃-硅静电键合过程中提供一个和键合产生的静电力方向相反的弹性力,使悬浮微敏感结构51在键合过程中不被吸在顶层玻璃1上。加上最后用铝刻蚀剂可轻易去除作为牺牲层的铝膜7。另外铝刻蚀剂中的硝酸将铝氧化成三氧化二铝,然后磷酸将其溶解成磷酸盐,乙酸主要用于降低腐蚀液表面张力,增大铝膜表面和腐蚀液的浸润,提高腐蚀的均匀性,起到缓冲作用,本方案在不改变原有工艺流程的基础上有效保证了悬浮微敏感结构51的完整性和可动性,无须加大机械约束就不会引起微机械传感器性能的降低,同时降低了工艺难度、提高了成品率,可广泛使用于各种带有悬浮可动敏感结构的硅微器件加工。According to the preparation method of the suspended micro-sensitive structure based on the aluminum sacrificial layer process in Example 1, Example 2 and Example 3, after the bottom glass-silicon is electrostatically bonded, before the suspended micro-sensitive structure 51 is processed on the silicon wafer 5 , the introduction of the aluminum film 7 as a sacrificial layer can connect the suspended micro-sensitive structure 51 and the bulk silicon 53 together. On the one hand, it prevents the suspended micro-sensitive structure 51 from falling off during the etching process; During the glass-silicon electrostatic bonding process, an elastic force opposite to the electrostatic force generated by the bonding is provided, so that the suspended micro-sensitive structure 51 is not attracted to the top glass 1 during the bonding process. In addition, the aluminum film 7 serving as the sacrificial layer can be easily removed with an aluminum etchant at the end. In addition, nitric acid in the aluminum etchant oxidizes aluminum into aluminum oxide, and then phosphoric acid dissolves it into phosphate. Acetic acid is mainly used to reduce the surface tension of the corrosion solution, increase the infiltration of the aluminum film surface and the corrosion solution, and improve the corrosion resistance. Uniformity plays a buffer role. This solution effectively ensures the integrity and mobility of the suspended micro-sensitive structure 51 without changing the original process flow, and will not cause performance degradation of the micro-mechanical sensor without increasing mechanical constraints. It can be widely used in the processing of various silicon micro devices with suspended movable sensitive structures.

Claims (1)

1.一种基于铝牺牲层工艺的悬浮微敏感结构制备方法,其特征在于,步骤如下:1. A method for preparing a suspended micro-sensitive structure based on aluminum sacrificial layer technology, characterized in that the steps are as follows: 步骤1:用缓冲氟氢酸BHF湿法分别在顶层玻璃(1)和底层玻璃(2)的表面上刻蚀出一个以上的120~160nm深的电极凹槽(3),每个电极凹槽(3)的外侧带有向外延伸的引线槽(60),且按照从左到右的顺序,顶层玻璃(1)和底层玻璃(2)依次对应的每对电极凹槽(3)的大小和纵向位置一致,这样的每对电极凹槽(3)构成了差动电极凹槽,然后在每个电极凹槽(3)内溅射170~210nm厚的钛金合金,形成一个以上的电极(41),并且在每个电极(41)的外侧面溅射出向外延伸的引线(42)进入对应的电极凹槽(3)的引线槽(60),每个引线(42)的宽度不小于30μm,相邻引线(42)之间的间隔不小于10μm,这样就得到了带有电极(41)的顶层玻璃(1)和带有电极(41)的底层玻璃(2),且每对差动电极凹槽(3)内的电极(41)及其引线(42)的数量、大小和位置也对应一致,该每对对应一致的电极(41)及其引线(42)构成一个差动电极(4);Step 1: Etch more than one electrode groove (3) with a depth of 120-160nm on the surface of the top glass (1) and the bottom glass (2) respectively with buffered hydrofluoric acid BHF wet method, each electrode groove The outer side of (3) has an outwardly extending lead groove (60), and in order from left to right, the size of each pair of electrode grooves (3) corresponding to the top glass (1) and the bottom glass (2) in turn Consistent with the longitudinal position, each pair of electrode grooves (3) constitutes a differential electrode groove, and then sputters a 170-210nm thick titanium-gold alloy in each electrode groove (3) to form more than one electrode (41), and on the outer surface of each electrode (41), the lead wires (42) extending outwards are sputtered into the lead wire slots (60) of the corresponding electrode grooves (3), and the width of each lead wire (42) is not is less than 30 μm, and the interval between adjacent lead wires (42) is not less than 10 μm, so that the top glass (1) with electrodes (41) and the bottom glass (2) with electrodes (41) are obtained, and each pair The number, size and position of the electrodes (41) and their lead wires (42) in the differential electrode groove (3) are also correspondingly consistent, and each pair of correspondingly consistent electrodes (41) and their lead wires (42) constitute a differential electrode (41) and their lead wires (42). electrode (4); 步骤2:采用n型或p型、且电阻率为0.002~0.004Ω·cm的晶向单晶硅片(5),进行标准清洗后,采用反应离子刻蚀RIE或感应耦合等离子体ICP干法在硅片(5)底表面进行刻蚀以形成一个以上的电极引线浅槽(6),其深度为5~10μm,且按照从左到右的顺序,硅片(5)底表面的电极引线浅槽(6)能依次逐一容纳底层玻璃(2)中对应的电极凹槽(3)内的引线(42),而各个相邻的电极引线浅槽(6)之间的突起平面构成了键合台面(52);其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片(5)清洗3-5分钟以去除硅片(5)上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片(5)清洗3-5分钟以去除硅片(5)上的非金属玷污,最后用浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片(5)清洗3-5分钟以去除硅片(5)上的金属玷污;Step 2: Use an n-type or p-type crystal-oriented single-crystal silicon wafer (5) with a resistivity of 0.002-0.004Ω·cm, perform standard cleaning, and use reactive ion etching RIE or inductively coupled plasma ICP dry method Etching is performed on the bottom surface of the silicon wafer (5) to form more than one electrode lead shallow groove (6), the depth of which is 5-10 μm, and in order from left to right, the electrode leads on the bottom surface of the silicon wafer (5) The shallow grooves (6) can successively accommodate the lead wires (42) in the corresponding electrode grooves (3) in the bottom glass (2) one by one, and the protruding planes between each adjacent electrode lead shallow grooves (6) constitute the key combined table top (52); where the standard cleaning is to use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer (5) for 3-5 minutes to remove the organic matter on the silicon wafer (5), and then Mix the ammonia water, hydrogen peroxide and pure water with a mass concentration of 60% according to the mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer (5) for 3-5 minutes to remove the non-toxic impurities on the silicon wafer (5). For metal contamination, mix 30% hydrochloric acid, hydrogen peroxide and pure water in a mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer (5) for 3-5 minutes to remove the silicon wafer (5) metal contamination on 步骤3:接着对硅片(5)的底部表面以金属溅射的方式制作出一个以上的铝膜(7)作为牺牲层,这样就形成了带有铝膜(7)的硅片(5),每个铝膜(7)的厚度为500~1000nm,所有铝膜的位置在硅片(5)的底部表面且在预设的悬浮微敏感结构(51)的边缘的纵向投影内;Step 3: Next, make more than one aluminum film (7) as a sacrificial layer on the bottom surface of the silicon wafer (5) by metal sputtering, thus forming a silicon wafer (5) with an aluminum film (7) , the thickness of each aluminum film (7) is 500-1000nm, and the position of all aluminum films is on the bottom surface of the silicon wafer (5) and within the longitudinal projection of the edge of the preset suspended micro-sensitive structure (51); 步骤4:用质量为80%的纯硫酸和20%双氧水相混合的溶液将带有铝膜(7)的硅片(5)清洗3-5分钟以去除硅片(5)上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜(7)的硅片(5)清洗3-5分钟以去除硅片(5)上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将带有铝膜(7)的硅片(5)清洗3-5分钟以去除硅片(5)上的金属玷污;然后进行底层玻璃-硅静电键合,即将带有铝膜(7)的硅片(5)和带有电极(41)的底层玻璃(2)接触在一起,且按照从左到右的顺序,该硅片(5)的底表面的电极引线浅槽(6)依次逐一和该底层玻璃(2)中对应的电极凹槽(3)相对,随后在350~450摄氏度下施加800~1500V的直流电压,硅片(5)连接直流电源正极,底层玻璃(2)连接直流电源的负极,接通该直流电压25~30分钟后键合完毕;Step 4: Clean the silicon wafer (5) with the aluminum film (7) for 3-5 minutes with a mixed solution of 80% pure sulfuric acid and 20% hydrogen peroxide to remove organic matter on the silicon wafer (5), then Mix ammonia water, hydrogen peroxide, and pure water with a mass concentration of 60% in a mass ratio of 1:1:5, and use the mixed solution to clean the silicon wafer (5) with the aluminum film (7) for 3-5 minutes to remove For the non-metallic contamination on the silicon wafer (5), mix hydrochloric acid, hydrogen peroxide, and pure water with a mass concentration of 30% at a mass ratio of 1:1:5, and use the mixed solution to coat the aluminum film (7) The silicon wafer (5) is cleaned for 3-5 minutes to remove metal contamination on the silicon wafer (5); then carry out the bottom glass-silicon electrostatic bonding, that is, the silicon wafer (5) with the aluminum film (7) and the electrode The bottom glass (2) of (41) is in contact together, and according to the order from left to right, the electrode lead shallow grooves (6) on the bottom surface of the silicon wafer (5) are in turn corresponding to the bottom glass (2) one by one. The electrode groove (3) is opposite to each other, and then a DC voltage of 800-1500V is applied at 350-450 degrees Celsius, the silicon wafer (5) is connected to the positive pole of the DC power supply, the bottom glass (2) is connected to the negative pole of the DC power supply, and the DC voltage is turned on After 25 to 30 minutes, the bonding is completed; 步骤5:底层玻璃-硅静电键合后,采用质量浓度为25%的四甲基氢氧化氨TMAH腐蚀液将该硅片(5)的厚度从其上端均匀腐蚀减薄至100~150μm,再使用质量浓度为25%的磷化液对该硅片(5)进行抛光,抛光时间为3-6分钟;Step 5: After the bottom glass-silicon is electrostatically bonded, the thickness of the silicon wafer (5) is uniformly etched from the upper end to 100-150 μm by using tetramethylammonium hydroxide TMAH etching solution with a mass concentration of 25%, and then Polishing the silicon wafer (5) with a phosphating solution with a mass concentration of 25%, and the polishing time is 3-6 minutes; 步骤6:采用反应离子刻蚀或感应耦合等离子体干法在该硅片(5)的上表面进行刻蚀以形成一个以上的电极引线浅槽(6),其深度为5~10μm,且按照从左到右的顺序,硅片(5)上表面的电极引线浅槽(6)能依次逐一容纳顶层玻璃(1)中对应的电极凹槽(3)内的引线(42),而各个相邻的电极引线浅槽(6)之间的突起平面构成了键合台面(52);其中标准清洗是先采用质量为80%的纯硫酸和20%双氧水相混合的溶液将硅片(5)清洗3-5分钟以去除硅片(5)上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片(5)清洗3-5分钟以去除硅片(5)上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将硅片(5)清洗3-5分钟以去除硅片(5)上的金属玷污;Step 6: Etching the upper surface of the silicon wafer (5) by reactive ion etching or inductively coupled plasma dry method to form more than one electrode lead shallow groove (6), the depth of which is 5-10 μm, and according to From left to right, the electrode lead shallow grooves (6) on the upper surface of the silicon wafer (5) can accommodate the lead wires (42) in the corresponding electrode grooves (3) in the top glass (1) one by one, and each phase The protruding plane between the adjacent electrode lead shallow grooves (6) constitutes the bonding table (52); wherein the standard cleaning is to first use a solution of 80% pure sulfuric acid and 20% hydrogen peroxide to clean the silicon wafer (5) Clean for 3-5 minutes to remove the organic matter on the silicon wafer (5), then mix ammonia, hydrogen peroxide and pure water with a mass concentration of 60% according to the mass ratio of 1:1:5, and use the mixed solution to place the silicon wafer ( 5) Wash for 3-5 minutes to remove non-metallic contamination on the silicon wafer (5), and finally mix hydrochloric acid, hydrogen peroxide and pure water with a mass concentration of 30% according to the mass ratio of 1:1:5, and use the mixed solution Cleaning the silicon wafer (5) for 3-5 minutes to remove metal contamination on the silicon wafer (5); 步骤7:接着采用感应耦合等离子体ICP干法,分别沿着预设的悬浮微敏感结构(51)的边缘及底层玻璃(2)的外侧带有向外延伸的引线槽(60)的电极凹槽(3)的边缘将该硅片(5)纵向刻透且不穿透铝膜(7)而形成悬浮微敏感结构(51)和导通硅(54),硅片的其它部分为体硅(53),该体硅(53)通过铝膜(7)和悬浮微敏感结构(51)相连接,另外在体硅(53)的侧面横向刻透出沟槽(8),这样形成了带有悬浮微敏感结构(51)和导通硅(54)的底层玻璃-硅片组合片;Step 7: Then adopt the inductively coupled plasma ICP dry method, respectively along the edge of the preset suspended micro-sensitive structure (51) and the outer side of the bottom glass (2) with the electrode recesses extending outwards with the lead groove (60) The edge of the groove (3) vertically cuts through the silicon wafer (5) without penetrating the aluminum film (7) to form a suspended micro-sensitive structure (51) and conductive silicon (54), and the other parts of the silicon wafer are bulk silicon (53), the bulk silicon (53) is connected to the suspended micro-sensing structure (51) through the aluminum film (7), and in addition, grooves (8) are carved laterally on the side of the bulk silicon (53), forming a band A bottom glass-silicon wafer combination sheet having a suspended micro-sensitive structure (51) and conducting silicon (54); 步骤8:对该底层玻璃-硅片组合片先用质量为80%的纯硫酸和20%双氧水相混合的溶液清洗3-5分钟以去除其上的有机物,接着对质量浓度60%的氨水、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗3-5分钟以去除其上的非金属玷污,最后用质量浓度30%的盐酸、双氧水以及纯水按照质量比例1∶1∶5相混合,用该混合后的溶液将该底层玻璃-硅片组合片清洗3-5分钟以去除其上的金属玷污;然后进行顶层玻璃-硅静电键合,即将该底层玻璃-硅片组合片和带有电极(41)的顶层玻璃(1)接触在一起,且按照从左到右的顺序,该硅片(5)上表面的电极引线浅槽(6)依次逐一和该顶层玻璃(1)中对应的电极凹槽(3)相对,随后在350~450摄氏度下施加800~1500V的直流电压,体硅(53)连接直流电源正极,顶层玻璃(1)连接直流电源的负极,接通该直流电压25~30分钟后键合完毕得到三层式组合片;Step 8: Wash the bottom glass-silicon wafer combination sheet with a solution of 80% pure sulfuric acid and 20% hydrogen peroxide for 3-5 minutes to remove organic matter on it, and then treat the ammonia water with a mass concentration of 60%, Hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer composite sheet is cleaned with the mixed solution for 3-5 minutes to remove the non-metallic contamination on it, and finally, the mass concentration is 30%. Hydrochloric acid, hydrogen peroxide and pure water are mixed according to the mass ratio of 1:1:5, and the bottom glass-silicon wafer assembly sheet is cleaned with the mixed solution for 3-5 minutes to remove the metal contamination on it; then the top glass -Silicon electrostatic bonding, that is, the bottom glass-silicon wafer composite sheet and the top glass (1) with electrodes (41) are in contact together, and in order from left to right, the upper surface of the silicon wafer (5) The electrode lead shallow grooves (6) face the corresponding electrode grooves (3) in the top glass (1) one by one, and then apply a DC voltage of 800-1500V at 350-450 degrees Celsius, and the bulk silicon (53) is connected to a DC power supply Positive electrode, top glass (1) connected to the negative electrode of the DC power supply, and the bonding is completed after the DC voltage is switched on for 25 to 30 minutes to obtain a three-layer composite sheet; 步骤9:将该三层式组合片浸入铝刻蚀剂中,加以超声波清洗20~30分钟,去除掉作为牺牲层的铝膜(7),该铝刻蚀剂由质量浓度为85%的磷酸、质量浓度为70%的硝酸、乙酸以及水分别按照体积百分比10~30%、0.5~2%、5~10%以及60~80%的比例混合配比而成;Step 9: immerse the three-layer composite sheet in an aluminum etchant, and ultrasonically clean it for 20 to 30 minutes to remove the aluminum film (7) as a sacrificial layer. The aluminum etchant is made of phosphoric acid with a mass concentration of 85%. 1. Nitric acid, acetic acid and water with a mass concentration of 70% are mixed according to volume percentages of 10-30%, 0.5-2%, 5-10% and 60-80% respectively; 步骤10:随即将该三层式组合片从铝刻蚀剂中取出,在超声波环境中将其用清水清洗20~30分钟,置换出成悬浮微敏感结构(51)、导通硅(54)以及体硅(53)结构内部残留的反应物及铝刻蚀剂,再在超声波环境中将其用乙醇清洗10~30分钟置换出清水,这样就完成了基于铝牺牲层工艺的悬浮微敏感结构的制备。Step 10: Immediately take the three-layer composite chip out of the aluminum etchant, wash it with clean water for 20 to 30 minutes in an ultrasonic environment, and replace it with a suspended microsensitive structure (51) and conductive silicon (54) As well as the residual reactants and aluminum etchant inside the bulk silicon (53) structure, and then wash it with ethanol for 10 to 30 minutes in an ultrasonic environment to replace the water, thus completing the suspended micro-sensitive structure based on the aluminum sacrificial layer process preparation.
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