CN1240995C - Microcantilever sensor and its making method - Google Patents
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Abstract
本发明涉及一种微悬臂梁传感器及其制作方法,它包括一芯片,所述芯片上设置有至少一组传感单元,所述传感单元由组成惠斯通电桥的四个完全相同的力敏电阻和两个悬臂梁组成,其中两个所述力敏电阻位于所述芯片的衬底上,另外两个电阻分别位于所述两悬臂梁上,其中一个所述悬臂梁作为测量悬臂梁,另一个所述悬臂梁作为参考悬臂梁,其特征在于:在所述芯片上设置有一微槽,所述悬臂梁设置在所述微槽内,所述力敏电阻的材料采用单晶硅或多晶硅,在所述单晶硅或多晶硅正面掺杂有硼离子,在所述力敏电阻上、下表面设置有氮化硅或氧化硅保护层,共同组成所述悬臂梁,所述测量悬臂梁表面设置有敏感层。本发明在环境监测,临床的诊断和治疗、新药开发、食品安全、工业加工控制、军事等领域具有广泛的应用前景。
The invention relates to a micro-cantilever beam sensor and a manufacturing method thereof. It comprises a chip, on which at least one group of sensing units is arranged, and the sensing unit consists of four completely identical force sensors forming a Wheatstone bridge. The two force-sensitive resistors are located on the substrate of the chip, and the other two resistors are respectively located on the two cantilever beams, and one of the cantilever beams is used as a measuring cantilever beam. Another described cantilever beam is used as a reference cantilever beam, and it is characterized in that: a microgroove is set on the chip, the cantilever beam is arranged in the microgroove, and the material of the force sensitive resistor adopts single crystal silicon or polycrystalline silicon , boron ions are doped on the front surface of the single crystal silicon or polycrystalline silicon, and silicon nitride or silicon oxide protective layers are arranged on the upper and lower surfaces of the force sensitive resistor to form the cantilever beam together, and the surface of the measuring cantilever beam There are sensitive layers set. The invention has wide application prospects in the fields of environment monitoring, clinical diagnosis and treatment, new drug development, food safety, industrial process control, military affairs and the like.
Description
技术领域technical field
本发明涉及一种传感器及其制作方法,特别是关于一种悬臂梁呈矩形应用于生物、化学传感中的微悬臂梁传感器及其制作方法。The invention relates to a sensor and a manufacturing method thereof, in particular to a micro-cantilever sensor with a rectangular cantilever beam used in biological and chemical sensing and a manufacturing method thereof.
背景技术Background technique
过去的20年里,微电子技术最显著的进步之一是新的测试技术的发展。扫描探针显微镜是众所周知的检测技术之一,其中扫描隧道显微镜和扫描力显微镜是最具代表性的两种高灵敏度的检测仪器。扫描力显微镜的工作原理是将探针固定在一个对微弱力非常敏感的微悬臂梁上,并使之与待测样品表面原子之间存在力的相互作用,作用在探针与样品之间的力使悬臂梁发生形变,并被记录下来,由于微悬臂梁对微弱力的变化非常敏感,因此可以高分辨率成像材料表面形貌,研究表面性质。One of the most significant advances in microelectronics over the past 20 years has been the development of new test techniques. Scanning probe microscopy is one of the well-known detection techniques, among which scanning tunneling microscope and scanning force microscope are the two most representative high-sensitivity detection instruments. The working principle of the scanning force microscope is to fix the probe on a micro-cantilever beam that is very sensitive to weak force, and make it interact with the surface atoms of the sample to be tested, and the force between the probe and the sample The force causes the cantilever to deform and is recorded. Since the microcantilever is very sensitive to weak force changes, it can image the surface topography of the material with high resolution and study the surface properties.
悬臂梁的微小弯曲通常由光学或电学方法来记录。光学检测方法可以获得小至0.01的垂直分辨率,其虽然具有较高的灵敏度,但庞大的光学测量系统及激光的精密校准限制了其广泛的应用:如超高真空、低温、液态条件下和阵列式悬臂梁测量中。摆脱这一问题的方法是集成电容、压电、力敏元件于悬臂梁中的电学检测方法,因为电学检测方法比光学方法更易于操作,易于转向实用化。在电学检测方法中,压阻式在位读出方法比其它检测技术更易于实现。The tiny bending of a cantilever is usually recorded optically or electrically. The optical detection method can obtain a vertical resolution as small as 0.01 Å. Although it has high sensitivity, the huge optical measurement system and the precise calibration of the laser limit its wide application: such as ultra-high vacuum, low temperature, liquid conditions and array cantilever beam measurements. The way to get rid of this problem is to integrate capacitance, piezoelectric, and force-sensitive elements into the electrical detection method of the cantilever beam, because the electrical detection method is easier to operate than the optical method, and it is easy to turn to practical use. Among the electrical detection methods, the piezoresistive in-situ readout method is easier to implement than other detection techniques.
近年来,将高灵敏度的微悬臂梁技术应用于生物、化学传感器成为传感器领域的研究热点。这类传感器可以在气态或液态条件下,探测微量生化分子的存在,如空气中的有机气体、有害气体、芳香剂,液体的DNA、蛋白质等。尽管悬臂梁生化传感器的研究工作取得了一些成果,但是离广泛应用还有一定距离,特别是在液态生物传感器的研究领域。同时,在悬臂梁式微传感器的制作工艺上还存在着制作工艺较复杂,成品率较低等问题。In recent years, the application of high-sensitivity micro-cantilever technology to biological and chemical sensors has become a research hotspot in the field of sensors. This type of sensor can detect the existence of trace biochemical molecules under gaseous or liquid conditions, such as organic gases, harmful gases, aromatics in the air, DNA and proteins in liquids, etc. Although the research work of the cantilever beam biochemical sensor has achieved some results, it still has a certain distance from wide application, especially in the field of liquid biosensor research. At the same time, there are still problems in the manufacturing process of the cantilever beam microsensor that the manufacturing process is relatively complicated and the yield is low.
发明内容Contents of the invention
本发明的目的是在现有技术的基础上提供一种测量灵敏度更高,制作工艺更简单的应用于生物、化学传感中的微悬臂梁传感器及其制作方法。The object of the present invention is to provide a micro-cantilever sensor and a manufacturing method thereof that are applied in biological and chemical sensing with higher measurement sensitivity and simpler manufacturing process on the basis of the prior art.
为实现上述目的,本发明采取以下技术方案:一种微悬臂梁传感器,它包括一芯片,所述芯片上设置有至少一组传感单元,所述传感单元由组成惠斯通电桥的四个完全相同的力敏电阻和两个悬臂梁组成,其中两个所述力敏电阻位于所述芯片的衬底上,另外两个分别位于所述两悬臂梁上,其中一个所述悬臂梁作为测量悬臂梁,另一个作为参考悬臂梁,其特征在于:在所述芯片上设置有一微槽,所述悬臂梁设置在所述微槽内,所述力敏电阻的材料采用单晶硅或多晶硅,在所述单晶硅或多晶硅正面掺杂有硼离子,在所述力敏电阻上、下表面设置有氮化硅或氧化硅保护层,共同组成所述悬臂梁,所述测量悬臂梁表面设置有敏感层。In order to achieve the above object, the present invention adopts the following technical solutions: a micro-cantilever beam sensor, which includes a chip, on which at least one group of sensing units is arranged, and the sensing units are composed of four Wheatstone bridges. Two identical force-sensitive resistors and two cantilever beams, wherein two force-sensitive resistors are located on the substrate of the chip, and the other two are respectively located on the two cantilever beams, and one of the cantilever beams is used as Measuring the cantilever beam, the other as a reference cantilever beam, is characterized in that: a microgroove is arranged on the chip, the cantilever beam is arranged in the microgroove, and the material of the force sensitive resistor adopts single crystal silicon or polycrystalline silicon , boron ions are doped on the front surface of the single crystal silicon or polycrystalline silicon, and silicon nitride or silicon oxide protective layers are arranged on the upper and lower surfaces of the force sensitive resistor to form the cantilever beam together, and the surface of the measuring cantilever beam There are sensitive layers set.
所述敏感层为高分子敏感材料。The sensitive layer is polymer sensitive material.
所述敏感层为生物活性分子。The sensitive layer is bioactive molecules.
所述悬臂梁为长50~500μm,宽10~100μm,厚100~5000nm矩形。The cantilever beam is rectangular with a length of 50-500 μm, a width of 10-100 μm, and a thickness of 100-5000 nm.
所述力敏电阻尺寸为长20~200μm,宽5~50μm。The size of the force sensitive resistor is 20-200 μm in length and 5-50 μm in width.
一种微悬臂梁传感器的制作方法,其特征在于它包括以下步骤:A method for making a micro-cantilever beam sensor is characterized in that it comprises the following steps:
1、采用具有氧化层、单晶硅器件层的SOI硅片,并减薄器件层作为芯片衬底;或者采用单面抛光p型硅片,进行常规清洗后,在硅片表面等离子体增强化学气相淀积氮化硅,然后在氮化硅表面低压化学汽相淀积多晶硅作为芯片衬底;1. Use an SOI silicon wafer with an oxide layer and a single crystal silicon device layer, and thin the device layer as the chip substrate; or use a single-sided polished p-type silicon wafer. After conventional cleaning, plasma-enhanced chemical Vapor deposition of silicon nitride, and then low-pressure chemical vapor deposition of polysilicon on the surface of silicon nitride as the chip substrate;
2、对单晶硅或多晶硅正面硼离子注入进行掺杂;2. Doping boron ion implantation on the front side of monocrystalline silicon or polycrystalline silicon;
3、用掩膜板对经步骤2的芯片进行第一次光刻,经刻蚀,形成力敏电阻;3. Carry out photolithography for the first time on the chip after
4、对经步骤3的芯片表面通过等离子体增强化学气相淀积氮化硅,在氮气中退火;4. Deposit silicon nitride on the chip surface through
5、用掩膜板对经步骤4的芯片进行第二次光刻,经刻蚀,形成力敏电阻接触孔和悬臂梁;5. Carry out photolithography for the second time on the chip after
6、对经步骤5的芯片表面通过电子束,溅射铬/金双金属膜;6. Pass the electron beam through the chip surface through step 5, and sputter the chromium/gold bimetallic film;
7、用掩膜板对经步骤6的芯片进行第三次光刻,经腐蚀,形成连接各力敏电阻的金属线;7. Carry out photolithography for the third time on the chip after step 6 with a mask plate, and corrode to form metal lines connecting each force sensitive resistor;
8、在整个芯片上进行单个传感器的划片;8. Scribe a single sensor on the entire chip;
9、用氢氧化钾腐蚀经步骤8的芯片,释放悬臂梁;9. Corrode the chip through step 8 with potassium hydroxide to release the cantilever beam;
10、对芯片上力敏电阻接触孔内的金属线与芯片衬底进行合金处理;10. Alloying the metal wire in the contact hole of the force sensitive resistor on the chip and the chip substrate;
11、将整个芯片裂片为单个传感器;11. Split the entire chip into a single sensor;
12、在每两个悬臂梁中的一个悬臂梁表面设置敏感层。12. A sensitive layer is set on the surface of one cantilever beam in every two cantilever beams.
其中步骤5,在形成力敏电阻接触孔和悬臂梁的同时形成芯片上的微槽。In step 5, the microgroove on the chip is formed at the same time as the force sensitive resistor contact hole and the cantilever beam are formed.
其中步骤1,SOI硅片的氧化层厚度为200~800nm,器件层厚度为100~500nm。Wherein step 1, the thickness of the oxide layer of the SOI silicon wafer is 200-800nm, and the thickness of the device layer is 100-500nm.
其中步骤1,在硅片表面进行等离子体增强化学气相淀积氮化硅时,氮化硅的厚度为100~1000nm。Wherein step 1, when plasma-enhanced chemical vapor deposition of silicon nitride is performed on the surface of the silicon wafer, the thickness of the silicon nitride is 100-1000 nm.
其中步骤1,在低压化学汽相淀积多晶硅时,多晶硅的厚度为100~500nm。Wherein step 1, when polysilicon is deposited by low pressure chemical vapor phase, the thickness of polysilicon is 100-500nm.
其中步骤2,对单晶硅或多晶硅正面硼离子注入进行掺杂时,注入硼离子的浓度为5×1013cm-2~5×1015cm-2,注入能量30keV~80keV。Wherein
其中步骤4,等离子体增强化学气相淀积氮化硅时,氮化硅厚度为100~1000nm,然后在氮气中900~1100℃退火20~30分钟。Wherein
本发明由于采取以上技术方案,其具有以下优点:1、本发明由于将惠斯通电桥中的两电阻分别设置在两悬臂梁上,一个作为测量电阻,另一个作为参考电阻,而不是将参考电阻设置在芯片的衬底上,因此测量时,当外部环境噪声使悬臂梁形变时,这个附加的信号可以通过参考悬臂梁被滤掉,使测量结果更加精确。2、本发明的悬臂梁呈阵列式排列,且以相邻的两悬臂梁为一组,因此可以通过在悬臂梁上涂设不同的高分子敏感层、生物活性分子,使每一对悬臂梁都可以通过敏感层完成一种测量功能,进而可以实现对不同物质各种特性指标的同时测量。3、本发明在悬臂梁的制作工艺中,将金属引线与力敏电阻连接的接触孔、悬臂梁和芯片上的微槽采用同一块掩膜板定义,亦即在本发明中仅采用了三个掩膜板,相比现有技术,本发明有效地简化了工艺流程。4、本发明由于选用金作为金属引线,因此可以抵抗长时间的KOH腐蚀,同时由于采用先划片后KOH腐蚀的方法,有效地避免了释放完悬臂梁后再划片造成的悬臂梁损坏,进而有效地提高了成品率。5、本发明可以通过正面腐蚀技术和硅~玻璃(聚合物)键合技术将悬臂梁设计、制备在液体可流动的微槽中,这样可直接用于液态生物分子的检测。The present invention has the following advantages due to the adoption of the above technical scheme: 1, the present invention is due to two resistors in the Wheatstone bridge being respectively arranged on two cantilever beams, one is used as a measurement resistor, and the other is used as a reference resistor instead of using the reference resistor The resistance is set on the substrate of the chip, so when the external environment noise deforms the cantilever beam during measurement, this additional signal can be filtered out through the reference cantilever beam to make the measurement result more accurate. 2. The cantilever beams of the present invention are arranged in an array, and two adjacent cantilever beams are used as a group. Therefore, different polymer sensitive layers and bioactive molecules can be coated on the cantilever beams to make each pair of cantilever beams A measurement function can be completed through the sensitive layer, and then the simultaneous measurement of various characteristic indicators of different substances can be realized. 3. In the manufacturing process of the cantilever beam of the present invention, the contact hole, the cantilever beam and the microgroove on the chip that are connected to the metal lead wire and the force sensitive resistor are defined by the same mask plate, that is, only three masks are used in the present invention. mask plate, compared with the prior art, the present invention effectively simplifies the process flow. 4. Since the present invention uses gold as the metal lead, it can resist long-term KOH corrosion. At the same time, due to the method of scribing first and then KOH corrosion, it effectively avoids the damage of the cantilever beam caused by scribing after releasing the cantilever beam. Thus, the yield rate is effectively improved. 5. In the present invention, the cantilever beam can be designed and prepared in the liquid-flowable microgroove through front-side etching technology and silicon-glass (polymer) bonding technology, so that it can be directly used for the detection of liquid biomolecules.
附图说明Description of drawings
图1是本发明结构示意图Fig. 1 is a structural representation of the present invention
图2是本发明惠斯通电桥示意图Fig. 2 is the schematic diagram of Wheatstone bridge of the present invention
图3是本发明微悬臂梁设置在芯片一侧的放大示意图Fig. 3 is the enlarged schematic diagram of the micro-cantilever beam of the present invention arranged on one side of the chip
图4a~4j是本发明工艺流程示意图Fig. 4a~4j is the schematic diagram of technological process of the present invention
具体实施方式Detailed ways
如图1、图2、图3所示,本发明属于压阻式微传感器,它包括一芯片1,其上设置有一微槽2,在微槽2两侧对称设置有四组传感单元3,每组传感单元3包括两个悬臂梁4和一组惠斯通(Wheatstone)电桥5。每组惠斯通电桥5由四个完全相同的力敏电阻R1、R2、R3、R4组成,将其中两个电阻R1、R4分别连接在两悬臂梁4上,一个作为测量悬臂梁4’,另一个作为参考悬臂梁4”。再将另外两个电阻R2、R3分别连接在芯片1的衬底上。将参考电阻R4设计在参考悬臂梁4”上,而不是设置在芯片1衬底上是考虑当外部环境噪声及热机械震动噪声使悬臂梁4形变时,这个附加的信号可以通过参考悬臂梁4”滤掉。在悬臂梁4’表面根据测量物质的不同需要,可以在测量悬臂梁4’的表面涂设高分子敏感材料、生物活性分子或金属等作为敏感层(图中未示出)。As shown in Fig. 1, Fig. 2, Fig. 3, the present invention belongs to piezoresistive microsensor, and it comprises a chip 1, is provided with a
比如:在悬臂梁4’表面固定DNA、蛋白质等生物活性分子,通过DNA分子间的杂化反应或蛋白质间的特异性结合反应实现DNA、蛋白质等微量生物分子的识别。测定DNA的传感器在悬臂梁表面固定已知序列的单链DNA分子(也称为ssDNA探针),被检测的生物分子是一条互补的ssDNA分子(也称为目标DNA),两者杂化反应的结果形成双链的DNA,反应过程中的力使悬臂梁弯曲,表现出一定的输出信号的变化。测定蛋白质的传感器通常将抗体固定在悬臂梁表面,基于两种分子间的结构互补性与亲和性,形成抗原抗体复合物,抗原抗体结合(电荷引力、范登华引力、氢键结合力、疏水结合力)使悬臂梁产生弯曲。悬臂梁4的微小弯曲改变力敏电阻R1的阻值,差分电压信号记录被检测的生物分子与敏感层分子间的反应。For example, bioactive molecules such as DNA and protein are immobilized on the surface of the cantilever beam 4', and the recognition of trace biomolecules such as DNA and protein is realized through the hybridization reaction between DNA molecules or the specific binding reaction between proteins. The sensor for measuring DNA immobilizes a single-stranded DNA molecule of known sequence (also called ssDNA probe) on the surface of the cantilever beam. The detected biomolecule is a complementary ssDNA molecule (also called target DNA), and the hybridization reaction between the two As a result of the formation of double-stranded DNA, the force during the reaction makes the cantilever bend, showing a certain change in the output signal. The sensor for measuring protein usually immobilizes the antibody on the surface of the cantilever. Based on the structural complementarity and affinity between the two molecules, an antigen-antibody complex is formed. force) to bend the cantilever beam. The slight bending of the
上述实施例中,悬臂梁4的设计尺寸可以是:长50~500μm,宽10~100μm,厚100~5000nm。组成对称惠斯通电桥5的四个完全相同的力敏电阻尺寸可以是:长20~200μm,宽5~50μm。悬臂梁受力后,应力的分布取决于悬臂梁的力矩M和转动惯量I,可以证明最大的应力通常发生在悬臂梁表面,从理论上推出此时悬臂梁臂上的纵向应力σ与悬臂梁端点的力F及垂直位移Δz的关系为:In the above embodiment, the designed dimensions of the
其中l、w和t为悬臂梁的长度,、宽度和厚度L为力敏电阻的长度,t为悬臂梁的厚度,E为杨氏模量,Δz为悬臂梁端点的垂直位移。Where l, w and t are the length of the cantilever, L, width and thickness L is the length of the force sensitive resistor, t is the thickness of the cantilever, E is Young's modulus, Δz is the vertical displacement of the cantilever end.
如果仅考虑纵向应力,力敏电阻的相对变化率ΔR/R可由下式给出:If only the longitudinal stress is considered, the relative change rate ΔR/R of the force sensitive resistor can be given by the following formula:
其中π为纵向压阻系数。测量悬臂梁由于力的作用产生形变时,悬臂梁力敏电阻的阻值变化为ΔR,在偏压V作用于Wheatstone电桥时,Wheatstone电桥的输出信号为:where π is the longitudinal piezoresistive coefficient. When measuring the deformation of the cantilever beam due to the action of force, the resistance value change of the cantilever beam force-sensitive resistor is ΔR. When the bias voltage V acts on the Wheatstone bridge, the output signal of the Wheatstone bridge is:
悬臂梁的测量灵敏度定义为电阻的相对变化与悬臂梁端点偏移量的比。将(1)式计算的应力结果代入公式(2),则可得到电阻的相对变化随力的变化关系,并根据虎克定律(Hook’s)和弹性系数的定义,悬臂梁的测量灵敏度可表示为:The measurement sensitivity of a cantilever is defined as the ratio of the relative change in resistance to the offset of the cantilever's endpoints. Substituting the stress result calculated by formula (1) into formula (2), the relationship between the relative change of resistance and the change of force can be obtained, and according to Hooke's law (Hook's) and the definition of elastic coefficient, the measurement sensitivity of the cantilever beam can be expressed as :
式中K=Eπl为应变灵敏度系数,。Where K = Eπ l is the strain sensitivity coefficient,.
力敏悬臂梁的最小可探测位移(MDD)定义为悬臂梁的信号噪声比为1∶1的条件下悬臂梁的垂直位移量,它不仅取决于悬臂梁的探测灵敏度,同时受力敏电阻噪声的制约。令Wheatston电桥输出电压信号Vo等于总噪声,悬臂梁的MDD即可表示为:The minimum detectable displacement (MDD) of the force-sensitive cantilever is defined as the vertical displacement of the cantilever under the condition that the signal-to-noise ratio of the cantilever is 1:1. It not only depends on the detection sensitivity of the cantilever, but also is affected by the noise of the force-sensitive resistor constraints. Let the Wheatston bridge output voltage signal V o equal to the total noise, the MDD of the cantilever beam can be expressed as:
上式中,中括弧中的第一项对应着力敏电阻的1/f噪声,第二项对应着力敏电阻的Johnson噪声。In the above formula, the first term in the brackets corresponds to the 1/f noise of the force sensitive resistor, and the second term corresponds to the Johnson noise of the force sensitive resistor.
由公式5可看出,噪声和灵敏度是一个平衡过程,实际设计尺寸要结合工艺条件选择。力敏电阻尺寸首先影响力敏电阻的噪声,尺寸越大噪声越小。悬臂梁尺寸同样影响悬臂梁的灵敏度和噪声,It can be seen from formula 5 that noise and sensitivity are a balanced process, and the actual design size should be selected in combination with process conditions. The size of the force sensitive resistor first affects the noise of the force sensitive resistor, the larger the size, the smaller the noise. The cantilever size also affects the sensitivity and noise of the cantilever,
本发明通过对工艺流程进行了优化设计,在微悬臂梁的制作中仅采用了三个掩膜板,相比其它制作方法,在工艺流程上进行了较大的简化。下面是本发明的制作In the present invention, by optimizing the design of the technological process, only three mask plates are used in the manufacture of the micro-cantilever beam, which greatly simplifies the technological process compared with other manufacturing methods. The following is the making of the present invention
实施例:Example:
1、制作芯片衬底,其可以采用单晶硅或多晶硅两种方式,1. Make the chip substrate, which can be made of single crystal silicon or polycrystalline silicon.
(1)制作多晶硅悬臂梁时,可以是单面抛光p型硅片10,对硅片10进行常规清洗后,在硅片10表面进行等离子体增强化学气相淀积(PECVD)氮化硅(Si3N4)11(如图4a所示),用于密封力敏电阻的底层,厚度为150nm;然后低压化学汽相淀积(LPCVD)多晶硅12(如图4b所示),厚度为200nm,形成多晶硅力敏电阻层。(1) When making a polysilicon cantilever beam, it can be a single-sided polished p-
(2)制作单晶硅悬臂梁时,可以是SOI(绝缘体上的硅结构)硅片,对其表面进行处理,减薄器件层,氧化层厚度为:400nm,器件层厚度为:200nm,器件层即为单晶硅力敏电阻层。(2) When making a single crystal silicon cantilever beam, it can be an SOI (silicon structure on insulator) silicon wafer, and its surface is treated to thin the device layer. The thickness of the oxide layer is: 400nm, and the thickness of the device layer is: 200nm. Layer is the single crystal silicon force sensitive resistor layer.
2、将经步骤1处理的单晶硅或多晶硅硅片作为芯片衬底,对其正面硼离子注入进行掺杂13(如图4c所示),注入硼离子的浓度5×1013或5×1015cm-2,注入能量30keV。2. Use the monocrystalline silicon or polycrystalline silicon wafer treated in step 1 as the chip substrate, and dope 13 boron ion implantation on the front side (as shown in Figure 4c), and the implanted boron ion concentration is 5×10 13 or 5× 10 15 cm -2 , the injection energy is 30keV.
3、采用掩膜板进行力敏电阻的图形转换,对掺杂后的单晶硅或多晶硅进行SF6(六氟化硫)反应离子刻蚀(RIE),形成力敏电阻R(如图4d所示)。3. Use a mask plate to convert the pattern of the force sensitive resistor, and perform SF 6 (sulfur hexafluoride) reactive ion etching (RIE) on the doped single crystal silicon or polycrystalline silicon to form a force sensitive resistor R (as shown in Figure 4d shown).
4、为完全密封力敏电阻R,等离子体增强化学气相淀积氮化硅11(如图4e所示),淀积厚度150nm,然后在N2中1050℃退火20分钟。4. To completely seal the force-sensitive resistor R, plasma-enhanced chemical vapor deposition of silicon nitride 11 (as shown in FIG. 4e ) with a thickness of 150 nm, and then annealing in N 2 at 1050° C. for 20 minutes.
5、采用微槽、接触孔、悬臂梁为一体的掩膜板进行光刻(如图4f所示),如果悬臂梁4设置之芯片1的一侧,可以不设置微槽,对Si3N4进行CHF3+SF6(三氟甲烷+六氟化硫)反应离子刻蚀,刻蚀掉微槽14及力敏电阻接触孔15上的Si3N4,同时刻蚀掉悬臂梁臂周围的Si3N4;5. Use a mask plate integrating microgrooves, contact holes, and cantilever beams for photolithography (as shown in Figure 4f). If the
6、通过电子束溅射铬/金(Cr/Au)双金属膜16(如图4g所示),铬厚度为40nm,用来使金较好地附着在芯片衬底上,金厚度400nm,采用金而不是铝是因为金可以抵抗氢氧化钾(KOH)的腐蚀。6. By electron beam sputtering chromium/gold (Cr/Au) bimetallic film 16 (as shown in Figure 4g), the thickness of chromium is 40nm, which is used to make gold better adhere to the chip substrate, the thickness of gold is 400nm, Gold is used instead of aluminum because gold is resistant to corrosion by potassium hydroxide (KOH).
7、采用金属掩膜板(如图4h所示),光刻后,腐蚀金属,完成金属线17的成形;7. Using a metal mask (as shown in FIG. 4h ), after photolithography, corrode the metal to complete the forming of the
8、在整个芯片1上进行单个传感器的划片(如图4i所示),在进行氢氧化钾腐蚀前先划片保证划片过程中不损坏悬臂梁。8. Carry out scribing of a single sensor on the entire chip 1 (as shown in FIG. 4i ), and scribing is performed before potassium hydroxide etching to ensure that the cantilever beam is not damaged during the slicing process.
9、进行氢氧化钾腐蚀硅,释放悬臂梁(如图4j所示),利用氢氧化钾对硅的各向异性凸角腐蚀的性质,在足够长的腐蚀时间下,悬臂梁下面的硅可以完全腐蚀干净,腐蚀后的槽深约60μm。9. Carry out potassium hydroxide corrosion silicon, release cantilever beam (as shown in Figure 4j), utilize potassium hydroxide to the character of the anisotropic salient corner corrosion of silicon, under long enough corrosion time, the silicon below the cantilever beam can be It is completely etched clean, and the depth of the etched groove is about 60 μm.
10、将力敏电阻接触孔内金属和硅进行合金化处理,使其形成欧姆接触,合金条件:320℃,20分钟。10. Alloy the metal and silicon in the contact hole of the force sensitive resistor to form an ohmic contact. Alloy conditions: 320°C, 20 minutes.
11、将整个芯片从上述划片处裂片为单个传感器。11. Split the entire chip into individual sensors from the above-mentioned dicing place.
12、在每两个悬臂梁中的一个悬臂梁,即测量悬臂梁4’表面涂镀敏感层。12. Coating a sensitive layer on the surface of one of the two cantilever beams, i.e. the measuring cantilever beam 4'.
上述方法中,In the above method,
步骤1,在硅片表面进行等离子体增强化学气相淀积氮化硅时,其厚度可以是100~1000nm;SOI硅片的氧化层厚度可以为200~800nm,器件层厚度可以为100~500nm。In step 1, when plasma-enhanced chemical vapor deposition of silicon nitride is performed on the surface of the silicon wafer, its thickness may be 100-1000 nm; the thickness of the oxide layer of the SOI silicon wafer may be 200-800 nm, and the thickness of the device layer may be 100-500 nm.
步骤1,低压化学汽相淀积多晶硅作为力敏电阻层时,其厚度可以是100~500nm;氮化硅或氧化硅保护层的厚度决定了悬臂梁的厚度,而悬臂梁的厚度又决定了其灵敏度,可由公式(4)看出。Step 1, when polysilicon is deposited by low-pressure chemical vapor phase as the force-sensitive resistor layer, its thickness can be 100-500 nm; the thickness of the silicon nitride or silicon oxide protective layer determines the thickness of the cantilever beam, and the thickness of the cantilever beam determines Its sensitivity can be seen from formula (4).
步骤2,对单晶硅或多晶硅正面硼离子注入进行掺杂时,注入硼离子的浓度可以是5×1013cm-2~5×1015cm-2,能量30keV~80keV;掺杂浓度越高,悬臂梁的噪声越低,但灵敏度同时降低。离子注入能量决定硼离子在电阻层中扩散的深浅,从而影响悬臂梁的灵敏度。
步骤4,等离子体增强化学气相淀积氮化硅时,淀积厚度可以是100~1000nm,然后在氮气中900~1100℃退火20~30分钟,淀积厚度决定了悬臂梁的厚度,而悬臂梁的厚度又决定了其灵敏度,可由公式(4)看出。
步骤5,铬/金双金属膜的厚度可以适当调整。Step 5, the thickness of the chromium/gold bimetallic film can be adjusted appropriately.
上述制作方法中,芯片光刻后,无论是在气体中刻蚀,还是在液体中腐蚀,其所使用的气体或液体都是可以根据需要变化的。In the above manufacturing method, after the chip is photolithographically etched, whether it is etched in gas or etched in liquid, the gas or liquid used can be changed as required.
上述实施例中,悬臂梁4的数量可以根据测量项目的需要设置,但其数量应为偶数,即两个悬臂梁为一组,与在两悬臂梁和芯片衬底上设置的四个力敏电阻组成一独立的传感单元,完成一个测量项目,因此,一个芯片上具有两个悬臂梁,便可以组成一个传感器;若设置多组悬臂梁,则形成阵列式传感器,传感器可以不设置微槽,使悬臂梁位于芯片的一侧(如图3所示),也可以设置微槽,使悬臂梁位于微槽两侧(如图1所示)。In the above-described embodiment, the quantity of the
本发明可以通过正面腐蚀技术和硅~玻璃(聚合物)键合技术将悬臂梁设计、制备在液体可流动的微槽中,这样可直接用于液态生物分子的检测。In the present invention, the cantilever beam can be designed and prepared in the liquid-flowable microgroove through the front-side etching technology and the silicon-glass (polymer) bonding technology, so that it can be directly used for the detection of liquid biomolecules.
本发明单元式或阵列式压阻悬臂梁无论是应用在气体传感器上,还是生物传感器上,都将在减小器件尺寸、提高器件灵敏度以及实现传感器的多功能性上发挥重要作用。悬臂梁式传感器在环境监测,临床的诊断和治疗、新药开发、食品安全、工业加工控制、军事等领域具有广泛的应用前景。Whether the unit type or array type piezoresistive cantilever beam of the present invention is applied to a gas sensor or a biosensor, it will play an important role in reducing the size of the device, improving the sensitivity of the device and realizing the multifunctionality of the sensor. Cantilever beam sensors have broad application prospects in environmental monitoring, clinical diagnosis and treatment, new drug development, food safety, industrial process control, military and other fields.
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| CN105974104B (en) * | 2016-05-12 | 2017-12-15 | 南京信息工程大学 | Cantilever beam biochemical sensor and cantilever beam preparation method based on huge piezo-resistive arrangement |
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