技术领域technical field
本实用新型涉及一种一种用于粘度测试的微流控芯片，具体涉及一种基于压电发电效应的自供电粘度测试微流控芯片，属有机纳米功能材料及微流控技术领域。The utility model relates to a microfluidic control chip for viscosity testing, in particular to a self-powered viscosity testing microfluidic chip based on piezoelectric power generation effect, which belongs to the technical field of organic nano functional materials and microfluidic control.
背景技术Background technique
粘度是流体基于流体的动力学行为的非常重要的一个物理参数。在许多的实际应用中，对流体粘度的测量是一项必不可少的工作。比如，在凝血测试的过程中对血浆粘度的测量就是非常重要的一项工作，同样，基于蛋白质抗体以及一些大分子溶液的药物中，粘度也是该类药物一项非常重要的指标。另外，当今社会发病率较高的一些心血管疾病，很多情况都是因为血液中一些大分子有机物的浓度过高导致血液粘度的变化而引起的。Viscosity is a very important physical parameter of fluid-based dynamic behavior. In many practical applications, the measurement of fluid viscosity is an essential work. For example, the measurement of plasma viscosity in the process of coagulation testing is a very important task. Similarly, in drugs based on protein antibodies and some macromolecular solutions, viscosity is also a very important indicator of such drugs. In addition, some cardiovascular diseases with a high incidence rate in today's society are often caused by changes in blood viscosity due to the high concentration of some macromolecular organic substances in the blood.
现阶段已经商业化的一些粘度测试的仪器，其原理主要是基于各种不同的传感机理，比如说基于锥板、落球、旋球、振动以及毛细效应的一些粘度测试的设备。然而这些比较传统的粘度测试方法所需样品的量比较大且整个测试过程花费的时间相对较长。而一些比较精确的粘度测试设备一般体型较大，测试分析的过程较复杂。现阶段，对微量样品粘度的测试方法的研究也比较多。例如：Nguyen等人设计了一种基于压阻悬臂梁结构的微机电系统来测试微量液体的粘度（“Viscosity measurement based on the tapping-inducedfree vibration of sessile droplets using MEMS-based piezoresistivecantilevers”，《Lab on a chip 》，15： 3670-6（2015）），然而这种装置的微加工过程比较复杂且数据分析过程也比较复杂，另外测试过程中对周围环境也会有一定的要求。Asaf 等人设计了一种基于毛细管效应的粘度测试仪器（“Capillary viscometer for fullyautomated measurement of the concentration and shear dependence of theviscosity of macromolecular solutions”，《Analytical Chemistry》，84(24)：10732-6（2012））。而这种方法一般需要辅助一些外加的设备进行辅助测试分析。Some viscosity testing instruments that have been commercialized at this stage are mainly based on various sensing mechanisms, such as some viscosity testing equipment based on cone plate, falling ball, spinning ball, vibration and capillary effect. However, these traditional viscosity testing methods require a relatively large amount of samples and the entire testing process takes a relatively long time. However, some more accurate viscosity testing equipment are generally larger in size, and the process of testing and analysis is more complicated. At this stage, there are many researches on the testing methods of the viscosity of micro-sample. For example: Nguyen et al. designed a microelectromechanical system based on piezoresistive cantilever beam structure to test the viscosity of trace liquids ("Viscosity measurement based on the tapping-induced free vibration of sessile droplets using MEMS-based piezoresistivecantilevers", "Lab on a chip”, 15: 3670-6 (2015)), however, the microfabrication process of this device is relatively complicated and the data analysis process is also relatively complicated. In addition, there are certain requirements for the surrounding environment during the test process. Asaf et al. designed a viscometer based on the capillary effect (“Capillary viscometer for fully automated measurement of the concentration and shear dependence of the viscosity of macromolecular solutions”, Analytical Chemistry, 84(24): 10732-6 (2012) ). However, this method generally requires the assistance of some additional equipment for auxiliary test analysis.
微流控技术又称芯片实验室。利用该技术可将生物化学领域中所涉及的样品制备、反应、分离和检测等基本操作集成在几平方厘米甚至更小的芯片上。本申请发明人之先提出了一种《具有自供电功能的微流控芯片及其制作方法》（201510304240.5），是利用压电一维纳米材料可采集环境中微小机械能并将其转换为电能，并将该电势能输出供给敏感单元，从而组建带自供电功能的微流控芯片方法。所述微流控芯片分为四层，自下至上的各层分别为：石英玻璃基片、探测电极、KNN纳米纤维、带PDMS微通道的PDMS盖板。该微流控芯片制作方法是：先在基片上通过光刻、溅射以及剥离工艺制作探测电极，再采用静电纺丝法在探测电极上大面积制备铌酸钾钠纳米纤维，然后将PDMS微通道与基片键合。然而采用该四层结构的微流控芯片，并不能用于带一定粘度的液体测试，主要原因是：⑴在材料上，《具有自供电功能的微流控芯片及其制作方法》（201510304240.5）是采用KNN作为压电材料，该材料的刚性以及脆性较大且材料下方硬质的基片也会影响材料的形变，从而流体微小的的机械能对该材料产生的形变量有限，输出电压较小（仅为mV级），很难用于粘度的测试。⑵在结构上，《具有自供电功能的微流控芯片及其制作方法》（201510304240.5）的压电材料直接暴露在微通道中，微通道中的流体会直接与压电材料接触，当流体中有带电粒子存在时会对压电材料产生一种屏蔽作用，严重影响到提高压电材料的电压输出幅值，且这样也不利于该器件的稳定性和长期的应用。有鉴于此，《具有自供电功能的微流控芯片及其制作方法》（201510304240.5）所公开的微流控芯片尚不能应用于粘度测试。Microfluidic technology is also called lab-on-a-chip. Using this technology, the basic operations involved in the field of biochemistry, such as sample preparation, reaction, separation and detection, can be integrated on a chip of a few square centimeters or even smaller. The inventor of this application first proposed a "Microfluidic chip with self-power supply function and its manufacturing method" (201510304240.5), which uses piezoelectric one-dimensional nanomaterials to collect micro mechanical energy in the environment and convert it into electrical energy. And the potential energy output is supplied to the sensitive unit, so as to form a microfluidic chip method with a self-power supply function. The microfluidic chip is divided into four layers, and the layers from bottom to top are: quartz glass substrate, detection electrode, KNN nanofiber, and PDMS cover plate with PDMS microchannel. The fabrication method of the microfluidic chip is as follows: first, the detection electrodes are fabricated on the substrate by photolithography, sputtering and stripping processes, and then potassium sodium niobate nanofibers are prepared on the detection electrodes in a large area by electrospinning, and then the PDMS microfibers are The channel is bonded to the substrate. However, the microfluidic chip with this four-layer structure cannot be used for liquid testing with a certain viscosity. The main reasons are: (1) In terms of materials, "Microfluidic chip with self-power supply function and its manufacturing method" (201510304240.5) KNN is used as the piezoelectric material. The rigidity and brittleness of the material are relatively high, and the hard substrate under the material will also affect the deformation of the material. Therefore, the small mechanical energy of the fluid has limited deformation of the material, and the output voltage is small. (Only mV level), it is difficult to test the viscosity. (2) Structurally, the piezoelectric material in "Microfluidic Chip with Self-Power Supply Function and Its Fabrication Method" (201510304240.5) is directly exposed in the microchannel, and the fluid in the microchannel will directly contact the piezoelectric material. The presence of charged particles will produce a shielding effect on the piezoelectric material, which seriously affects the improvement of the voltage output amplitude of the piezoelectric material, and this is also not conducive to the stability and long-term application of the device. In view of this, the microfluidic chip disclosed in "Microfluidic chip with self-power supply function and its manufacturing method" (201510304240.5) cannot be applied to viscosity testing yet.
综上所述，一种可用于粘度测试的具有自供电功能的微流控芯片的设想及实践，未见于已公开的文献或专利技术中。In summary, the idea and practice of a self-powered microfluidic chip that can be used for viscosity testing has not been found in published literature or patented technologies.
发明内容Contents of the invention
本实用新型的目的是针对背景技术提出的问题，提供一种用于粘度测试的微流控芯片，是基于压电发电效应的在微流控芯片中进行粘度测试的微流控芯片。所述微流控芯片分为五层，自下而上各层依次是：带微形凹槽的PDMS底板、PDMS底板上微形凹槽两侧的一对电极、电极上方的一层PVDF纳米纤维薄膜、PVDF纳米纤维薄膜上的一层面积较大的PDMS薄膜、最上一层带微通道的PDMS盖板。所述微流控芯片制作方法是：先通过SU8光刻胶的光刻以及脱模技术制作带有微形凹槽和微通道的PDMS底板和盖板，再通过掩膜版磁控溅射的方法在PDMS底板的微形凹槽两侧制作一对探测电极，并将通过静电纺丝法制作的PVDF薄膜转移到电极上。盖板下方是一层通过匀胶并超声下来，再通过键合工艺与盖板键合在一起的PDMS薄膜，之后将盖板与底板键合在一起，形成完整的器件。通过在微流控芯片中采集不同粘度液体的机械能并转换为压电材料的电压输出，对输出电压进行测量分析，实现无需供电的粘度测试。通过该方法进行粘度测试进对样品需求量较少、对样品的种类没有要求、测试时间短，结构稳定，有利于微流控芯片的集成，有利于制作微流控芯片粘度计向小型化甚至手持式应用拓展。The purpose of the utility model is to provide a microfluidic chip for viscosity testing in view of the problems raised by the background technology, which is a microfluidic chip for viscosity testing in the microfluidic chip based on the piezoelectric power generation effect. The microfluidic chip is divided into five layers, and the layers from bottom to top are: a PDMS base plate with micro-grooves, a pair of electrodes on both sides of the micro-grooves on the PDMS base plate, and a layer of PVDF nanometer electrodes above the electrodes. A layer of PDMS film with a larger area on the fiber film, a PVDF nanofiber film, and a PDMS cover plate with microchannels on the top layer. The manufacturing method of the microfluidic chip is as follows: first, the PDMS base plate and the cover plate with micro-grooves and micro-channels are produced through the photolithography of SU8 photoresist and the demoulding technology, and then through the mask plate magnetron sputtering. Methods A pair of detection electrodes were fabricated on both sides of the micro-groove on the PDMS base plate, and the PVDF film produced by electrospinning was transferred to the electrodes. Below the cover plate is a layer of PDMS film that is glued and ultrasonically removed, and then bonded to the cover plate through a bonding process, and then the cover plate and the base plate are bonded together to form a complete device. By collecting the mechanical energy of liquids with different viscosities in the microfluidic chip and converting it into the voltage output of the piezoelectric material, the output voltage is measured and analyzed to realize the viscosity test without power supply. Viscosity testing by this method has less demand for samples, no requirements for the type of samples, short test time, and stable structure, which is conducive to the integration of microfluidic chips, and is conducive to the miniaturization and even miniaturization of the production of microfluidic chip viscometers. Handheld application expansion.
为了达到上述目的，本实用新型采用以下技术方案：In order to achieve the above object, the utility model adopts the following technical solutions:
一种用于粘度测试的微流控芯片，包括自下而上依层次分布的：PDMS底板、探测电极、纳米纤维薄膜、PDMS盖板；所述探测电极是在所述PDMS底板上通过公知的光刻、溅射及剥离工艺制作的一对导电电极；所述PDMS盖板下表面加工有包括干流通道和支流通道的PDMS微流通道，支流通道宽度小于干流通道宽度；干流通道部分相应的位于纳米纤维薄膜之上；其特征在于：A microfluidic chip for viscosity testing, comprising layered distribution from bottom to top: a PDMS base plate, a detection electrode, a nanofiber film, and a PDMS cover plate; the detection electrode is passed on the PDMS base plate through known A pair of conductive electrodes made by photolithography, sputtering and lift-off process; the lower surface of the PDMS cover plate is processed with a PDMS micro-flow channel including a main flow channel and a branch flow channel, and the width of the branch flow channel is smaller than the width of the main flow channel; on a nanofibrous film; characterized by:
所述纳米纤维薄膜是PVDF纳米纤维薄膜；The nanofiber film is a PVDF nanofiber film;
所述纳米纤维薄膜与PDMS盖板之间，还有一层PDMS薄膜；所述PDMS薄膜面积大于所述PVDF纳米纤维薄膜面积；所述PDMS盖板通过十字对准标志，按顺序将PDMS微流通道、PDMS薄膜和PVDF纳米纤维薄膜压紧并键合在PDMS底板的探测电极上；There is also a layer of PDMS film between the nanofiber film and the PDMS cover plate; the area of the PDMS film is larger than the area of the PVDF nanofiber film; the PDMS cover plate aligns the PDMS microfluidic channels in order , PDMS film and PVDF nanofiber film are pressed and bonded on the detection electrode of the PDMS base plate;
所述PDMS底板上，位于一对导电电极之间的下部，开有一个微型凹槽；A micro-groove is opened on the lower part between a pair of conductive electrodes on the PDMS base plate;
所述干流通道的宽度设定为：位于PDMS底板的微型通孔正上方部分通道宽度，小于其它位置通道宽度。The width of the main flow channel is set to be: the channel width of the part directly above the micro-through hole on the PDMS base plate is smaller than the channel width of other positions.
本实用新型有益效果是：The beneficial effects of the utility model are:
⑴采用压电系数以及柔性都非常好的PVDF压电纳米纤维作为纳米纤维薄膜压电材料，该材料能够承受超大幅度的应变且制备过程非常简单、转移利用的可操作性很强。(1) PVDF piezoelectric nanofibers with excellent piezoelectric coefficient and flexibility are used as the nanofiber film piezoelectric material, which can withstand ultra-large strains, and the preparation process is very simple, and the transfer and utilization are very operable.
⑵在PDMS盖板与PVDF纳米纤维薄膜压电材料之间增加一层非常薄的PDMS薄膜，该薄膜将流体与压电材料隔开，不仅可以避免流体中的带电粒子对压电材料的屏蔽作用降低电压输出，还能防止流体的长期冲击对压电材料的损坏而降低器件的使用寿命。(2) A very thin layer of PDMS film is added between the PDMS cover plate and the PVDF nanofiber film piezoelectric material. This film separates the fluid from the piezoelectric material, which can not only avoid the shielding effect of the charged particles in the fluid on the piezoelectric material Reducing the voltage output can also prevent the long-term impact of the fluid from damaging the piezoelectric material and reducing the service life of the device.
⑶在PDMS底板上，位于一对导电电极之间的下部加工的微型通孔，有利于微流体驱动压电材料形变，可提高形变量以提高压电材料的电压输出。(3) On the PDMS base plate, the micro-through hole processed at the lower part between a pair of conductive electrodes is conducive to the deformation of the piezoelectric material driven by microfluidics, which can increase the deformation to increase the voltage output of the piezoelectric material.
⑷位于盖板下表面的干流通道中，电极探测部分对应部分通道的宽度尺寸相对于其他部分要窄，流体在通过该段微通道时流速会增加，流体下方压电材料所受到的应力也会增加，因此探测电极两端电压输出相应的增加。(4) In the main flow channel located on the lower surface of the cover plate, the width of the channel corresponding to the electrode detection part is narrower than other parts. When the fluid passes through this micro channel, the flow rate will increase, and the stress on the piezoelectric material under the fluid will also increase. Increase, so the voltage output across the detection electrode increases accordingly.
如上所述一种用于粘度测试的微流控芯片制作方法包括如下步骤：As mentioned above, a method for making a microfluidic chip for viscosity testing comprises the following steps:
步骤一：通过SU8光刻胶的光刻以及脱模技术，制作带有微形凹槽的PDMS底板和微流通道的PDMS盖板；Step 1: Fabricate a PDMS base plate with micro-grooves and a PDMS cover plate with microfluidic channels through SU8 photoresist photolithography and demoulding technology;
步骤二：通过掩膜版磁控溅射的方法，在PDMS底板的微形凹槽两侧制作一对探测电极，并将所述PVDF薄膜转移到电极上；Step 2: Make a pair of detection electrodes on both sides of the micro-groove of the PDMS base plate by mask plate magnetron sputtering, and transfer the PVDF film to the electrodes;
步骤三：通过匀胶并超声波剥离一层PDMS薄膜，再通过键合工艺将所述PDMS薄膜键合在PDMS盖板下方；Step 3: Peel off a layer of PDMS film by uniform glue and ultrasonic wave, and then bond the PDMS film under the PDMS cover plate through a bonding process;
步骤四：将底板与盖板两部分键合在一起，制作成用于粘度测试的微流控芯片。Step 4: Bond the two parts of the bottom plate and the cover plate together to make a microfluidic chip for viscosity testing.
所述步骤一中制作带有微形凹槽和微流通道的PDMS底板和PDMS盖板的制备工艺包括：The preparation process of making a PDMS base plate and a PDMS cover plate with micro-shaped grooves and micro-fluidic channels in the step 1 includes:
（1）石英片清洗：取长宽均为10～30mm、厚度1～3mm的石英载玻片，依次放入丙酮、酒精、去离子水中分别进行超声波清洗，每次清洗时间10～12min，清洗完后将载波片浸入干净的去离子水中；(1) Cleaning of quartz slices: Take a quartz glass slide with a length and width of 10-30 mm and a thickness of 1-3 mm, and place them in acetone, alcohol, and deionized water for ultrasonic cleaning respectively, each cleaning time is 10-12 minutes, and the After that, immerse the slides in clean deionized water;
（2）涂覆光刻胶：自去离子水中取出载玻片→氮气吹干→放置50～80℃环境中烘烤8～12min→取出冷却10～12 min→在匀胶机上涂覆光刻胶→放置60～65℃环境中烘烤15～18min→升温至90～95℃烘烤110～130min→取出冷却10～12min；所述涂覆光刻胶的匀胶机转速为850～950r.p.m，涂覆时间设定为35～45s；(2) Coating photoresist: take out the glass slide from deionized water → dry it with nitrogen gas → place it in an environment of 50 ~ 80 ° C for 8 ~ 12 minutes → take it out and cool it for 10 ~ 12 minutes → apply photoresist on the coater Glue → place in 60 ~ 65 ° C environment and bake for 15 ~ 18 minutes → heat up to 90 ~ 95 ° C and bake for 110 ~ 130 minutes → take out and cool for 10 ~ 12 minutes; the speed of the uniform machine for coating photoresist is 850 ~ 950r. p.m, the coating time is set to 35~45s;
（3）制备微流通道母版：将设定尺寸的微流通道掩膜板放在上述已涂覆光刻胶的载玻片上，再将载玻片放入光刻机中曝光18～22s→取出并放置60～65℃环境中烘烤15～18min→升温至90～95℃烘烤40～45 min→取出冷却10～12min→在显影液中显影5～15min→取出后用异丙醇冲洗氮气吹干→放置115～135℃环境中坚膜110～130min，制成微流通道母版；所述设定尺寸的微流通道掩膜板的干流通道宽度为100～500μm，支流通道的宽度为50～100μm；所述载波片上，也光刻有与基片上的十字对准标志位置对应的十字对准标志；(3) Prepare the microfluidic channel master: place the microfluidic channel mask plate of the set size on the above-mentioned photoresist-coated glass slide, and then put the glass slide into the photolithography machine for exposure for 18-22s →Take it out and put it in an environment of 60-65°C for 15-18 minutes→raise the temperature to 90-95°C and bake for 40-45 minutes→take it out and cool it for 10-12 minutes→develop it in the developer for 5-15 minutes→use isopropanol after taking it out Rinse with nitrogen and blow dry → place the film in an environment of 115-135°C for 110-130min to make a micro-flow channel master; 50-100 μm; on the carrier film, a cross alignment mark corresponding to the position of the cross alignment mark on the substrate is also photoengraved;
（4）制备微形凹槽母版：将设定尺寸的微形凹槽掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光18～20s→取出并放置60～65℃环境中烘烤15～18min→升温至90～95℃烘烤40～45min→取出冷却10～12min→在显影液中显影5～15min→取出后用异丙醇冲洗氮气吹干→放置115～135℃环境中坚膜110～130min，制成微形凹槽母版；设定所述微形凹槽掩膜板长度为1～1.5mm、宽度为200～600μm；所述石英玻璃片上，也光刻有与PDMS盖板十字对准标志位置对应的十字对准标志；(4) Preparation of micro-groove master: put the micro-groove mask plate of the set size on the above-mentioned quartz glass sheet coated with photoresist, and then put the quartz glass sheet into the photolithography machine to expose for 18 ~20s→Take it out and put it in a 60~65℃ environment and bake for 15~18min→Raise the temperature to 90~95℃ and bake for 40~45min→Take it out and cool it for 10~12min→Develop in a developer for 5~15min→Take it out and use isopropyl Rinse with alcohol and dry with nitrogen gas → place the film at 115-135°C for 110-130 minutes to make a micro-groove master; set the length of the micro-groove mask to 1-1.5 mm and the width to 200-600 μm ; On the quartz glass sheet, a cross alignment mark corresponding to the position of the PDMS cover plate cross alignment mark is also photoengraved;
（5）制备PDMS混合物：按8:1～12:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物；(5) Preparation of PDMS mixture: According to the mass ratio of 8:1 to 12:1, polydimethylsiloxane (PDMS) prepolymer and curing agent are mixed and stirred evenly to make a PDMS mixture;
（6）制备带PDMS微流通道的PDMS盖板：将前述步骤（3）制备的微流通道母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至80～100℃环境中烘烤90～150min→取出冷却至室温→从微流通道母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微流通道以及微形凹槽，制成带微流通道的PDMS盖板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上；(6) Prepare the PDMS cover plate with PDMS microfluidic channel: Place the microfluidic channel master prepared in the previous step (3) horizontally in the petri dish → pour the PDMS mixture into the petri dish → let it stand in the petri dish Remove all the air bubbles in the microfluidic channel → take it out and put it in an environment of 80 ~ 100 ° C for 90 ~ 150 minutes → take it out and cool it to room temperature → peel off the cured PDMS mixture from the microfluidic channel master → cut out the required parts according to the set size The microfluidic channel and the microgroove are made into a PDMS cover plate with a microfluidic channel; when the master is placed in the petri dish, the side that has been coated with photoresist faces up;
（7）制备带微形凹槽的PDMS底板：将前述步骤（4）制备的微形凹槽母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至80～100℃环境中烘烤90～150min→取出冷却至室温→从微形凹槽母版上揭下已固化的PDMS混合物→按设定尺寸切取所需尺寸的微形凹槽，制成带微形凹槽的PDMS底板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。(7) Prepare the PDMS bottom plate with micro-grooves: Place the micro-groove master prepared in the previous step (4) horizontally in the petri dish → pour the PDMS mixture into the petri dish → let it stand in the petri dish All the air bubbles in it are discharged → take it out and put it in an environment of 80 ~ 100 ° C for 90 ~ 150 minutes → take it out and cool it to room temperature → peel off the cured PDMS mixture from the micro-groove master → cut out the required size according to the set size The micro-grooves of the size are made into a PDMS bottom plate with micro-grooves; when the master plate is placed in the petri dish, the side coated with photoresist faces upward.
所述步骤二中静电纺丝法制备PVDF纳米纤维的过程如下：The process of preparing PVDF nanofibers by electrospinning in said step 2 is as follows:
（1） PVDF前驱液的配置：将二甲基甲酰胺（DMF）与丙酮按体积百分比为10%∶90%～50%∶50%的比例混合并搅拌均匀；按PVDF的浓度为0.09～0.15g/ml的比例向所述DMF和丙酮的混合液中加入PVDF粉末，并在50～80℃的条件下密封搅拌30～90min，直至整个溶液为澄清透明状；(1) Configuration of PVDF precursor solution: Mix dimethylformamide (DMF) and acetone at a ratio of 10%:90% to 50%:50% by volume and stir evenly; the concentration of PVDF is 0.09 to 0.15 Add PVDF powder to the mixed solution of DMF and acetone at the ratio of g/ml, and seal and stir at 50-80°C for 30-90min until the whole solution is clear and transparent;
（2） 静电纺丝接受板的制作：设定接受极板是边长为10×10～30×30cm的正方形有机玻璃板，所述有机玻璃板中心并列贴两块尺寸相同的铝箔片，设定铝箔片宽1～3cm、长5～8cm，两铝箔片之间长边平行并相距5～25mm，宽边在同一条直线上；(2) Production of the electrospinning receiving plate: the receiving plate is set to be a square plexiglass plate with a side length of 10×10-30×30 cm, and two aluminum foils of the same size are pasted side by side in the center of the plexiglass plate. The width of the aluminum foil is 1-3cm, the length is 5-8cm, the long sides between the two aluminum foils are parallel and the distance is 5-25mm, and the wide sides are on the same straight line;
（3） 静电纺丝：将步骤（1）中制备的PVDF前驱液吸入注射器中，并将注射器安装到微量注射泵上，再将注射器针头接入直流电压源的正极，贴在接受极板上的两片铝箔接直流电压源负极；针头的方向与接受极板面垂直，针头与接收极板的距离为10～20cm，直流电压源电压为9～20kV，微量注射泵的推进速度为20～80ul/min，环境湿度控制在40%以下、温度控制在25～35℃；PVDF纳米线用洗净的硅片进行接收，所述硅片置于贴在接受极板上的两片铝箔片之间；静电纺丝时间为5～30min；(3) Electrospinning: Inhale the PVDF precursor solution prepared in step (1) into the syringe, install the syringe on the micro-syringe pump, connect the needle of the syringe to the positive pole of the DC voltage source, and attach it to the receiving plate The two pieces of aluminum foil are connected to the negative electrode of the DC voltage source; the direction of the needle is perpendicular to the surface of the receiving plate, the distance between the needle and the receiving plate is 10-20cm, the voltage of the DC voltage source is 9-20kV, and the advancing speed of the micro-injection pump is 20-20cm. 80ul/min, the ambient humidity is controlled below 40%, and the temperature is controlled at 25-35°C; the PVDF nanowires are received by a cleaned silicon wafer, and the silicon wafer is placed between two pieces of aluminum foil attached to the receiving plate time; electrospinning time is 5 ~ 30min;
所述步骤三中PDMS薄膜的制备工艺如下：The preparation process of the PDMS film in the step 3 is as follows:
（1）制备PDMS混合物：按8:1～12:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物，静置1～2h至气泡全部排出；(1) Preparation of PDMS mixture: According to the mass ratio of 8:1 to 12:1, take polydimethylsiloxane (PDMS) prepolymer and curing agent, mix and stir evenly to make PDMS mixture, and let it stand for 1 ~2h until all the air bubbles are discharged;
（2）涂覆PDMS混合物：自去离子水中取出提前裁好的长宽均为10～30mm的载玻片→氮气吹干→在匀胶机上涂覆PDMS混合物→匀胶机先以600～800r.p.m旋转10～20s 再以3000～5000r.p.m旋转40～60s→取下后静置12h后，再在烘箱中以75～95℃烘烤30～90min→取出冷却10～12min；(2) Coating the PDMS mixture: Take out the pre-cut glass slides with a length and width of 10-30mm from the deionized water → blow dry with nitrogen gas → coat the PDMS mixture on the homogenizer → the homogenizer first with a temperature of 600-800r Rotate at .p.m for 10-20s, then rotate at 3000-5000r.p.m for 40-60s → take it off and let it stand for 12 hours, then bake it in an oven at 75-95°C for 30-90 minutes → take it out and cool it for 10-12 minutes;
（3）PDMS薄膜的脱模：将前面涂膜并固化后的带有PDMS薄膜的载璃片于丙酮中在40～60℃条件下超声波30～90min→取出后在去离子水中在40～60℃继续超声波90～120至薄膜脱落→将薄膜从玻片上撕下用氮气吹干待用。(3) Demolding of PDMS film: Put the glass slide with PDMS film that has been coated and cured in acetone at 40-60°C for 30-90 minutes → take it out and place it in deionized water at 40-60°C Continue to ultrasonic at 90-120°C until the film falls off → tear off the film from the glass slide and dry it with nitrogen gas for later use.
所述步骤四中将底板与盖板两部分键合在一起，完成用于粘度测试的微流控芯片器件工艺包括：In the step four, bonding the two parts of the bottom plate and the cover plate together to complete the microfluidic chip device process for viscosity testing includes:
（1）取按步骤一制作的带微形凹槽的PDMS底板，用提前设计好金属掩膜版在Ar气氛下以60100W溅射功率，采用公知标准溅射工艺在带微形凹槽的PDMS底板的表面溅射80～180s铂电极；(1) Take the PDMS bottom plate with micro-grooves produced according to step 1, use the metal mask designed in advance to sputter with 60100W sputtering power under Ar atmosphere, and use the known standard sputtering process to sputter on the PDMS with micro-grooves. Platinum electrodes are sputtered on the surface of the bottom plate for 80-180s;
（2）将通过静电纺丝法制作的PVDF纳米纤维薄膜，用小刀切取（1～1.5）mm×（2～3）mm面积，在显微镜的辅助下转移到溅射的铂电极上，完成盖板制作；(2) Use a knife to cut the PVDF nanofiber film made by electrospinning into an area of (1-1.5) mm×(2-3) mm, and transfer it to the sputtered platinum electrode with the aid of a microscope to complete the cover. board making;
（3）取按步骤一制作的带微通道的PDMS盖板以及，按步骤三制作的PDMS薄膜，放在功率为16～18W、波长为254nm的紫外灯箱中照射2.5～3.5h后，取出贴合压紧保持12h，完成底板制作；(3) Take the PDMS cover plate with microchannels made according to step 1 and the PDMS film made according to step 3, put them in a UV light box with a power of 16~18W and a wavelength of 254nm for 2.5~3.5h, take out the sticker Press and hold for 12 hours to complete the production of the bottom plate;
（4）将盖板和底板放在功率为16～18W、波长为254nm的紫外灯箱中，照射2.5～3.5h，取出后将盖板和底板贴合压紧，保持12h使其键合在一起，制作成具有自供电功能的粘度测试微流控芯片。(4) Put the cover plate and the bottom plate in a UV light box with a power of 16-18W and a wavelength of 254nm, and irradiate them for 2.5-3.5 hours. After taking them out, press the cover plate and the bottom plate tightly, and keep them for 12 hours to make them bond together , made into a viscosity testing microfluidic chip with self-power supply function.
附图说明Description of drawings
图1是本实用新型实施例提供的PVDF纳米纤维显微示意图；Fig. 1 is a schematic microscopic view of the PVDF nanofiber provided by the embodiment of the present invention;
图2是做微流通道所用的掩膜板示意图；Fig. 2 is a schematic diagram of a mask plate used for making a microfluidic channel;
图3是做微形凹槽时所用的掩膜版示意图；Fig. 3 is a schematic diagram of a mask plate used when making microgrooves;
图4是做探测电极所用的掩膜板示意图；Fig. 4 is a schematic diagram of a mask used as a detection electrode;
图5是PDMS底板微形凹槽、探测电极以及PVDF纳米线薄膜的示意图；Fig. 5 is the schematic diagram of PDMS bottom plate microgroove, detection electrode and PVDF nanowire film;
图6是PDMS上层盖板微通道及微通道上的PDMS薄膜示意图；Fig. 6 is the schematic diagram of the PDMS film on the PDMS upper cover plate microchannel and the microchannel;
图7是PDMS底板、探测电极、PVDF纳米纤维、PDMS薄膜及PDMS微通道之间位置示意图；Fig. 7 is a schematic diagram of the positions among the PDMS base plate, detection electrodes, PVDF nanofibers, PDMS films and PDMS microchannels;
图8是本实用新型实施例键合完成并组装好的可用于粘度测试的微流控芯片器件示意图；Fig. 8 is a schematic diagram of a microfluidic chip device that has been bonded and assembled and can be used for viscosity testing in an embodiment of the present invention;
图9是不同尺寸的微流控芯片在相同的输入压强条件下电压输出的柱状图；Figure 9 is a histogram of the voltage output of microfluidic chips of different sizes under the same input pressure conditions;
图10是不同的输入压强条件下，芯片电压输出与时间之间的关系折线图；Figure 10 is a line diagram of the relationship between chip voltage output and time under different input pressure conditions;
图11是通过对图9的统计得出的输入压强与输出电压之间关系的折线图以及拟合图；Fig. 11 is a broken line diagram and a fitting diagram of the relationship between the input pressure and the output voltage obtained through the statistics of Fig. 9;
图12是不同粘度的液体在相同的测试条件下芯片电压输出与时间之间的关系折线图；Fig. 12 is a line graph of the relationship between chip voltage output and time under the same test conditions for liquids with different viscosities;
图13是通过对图12的统计得出的不同粘度液体与输出电压之间的关系的折线图以及拟合图。FIG. 13 is a line graph and a fitting graph of the relationship between liquids of different viscosities and the output voltage obtained from the statistics of FIG. 12 .
1—PDMS底板，2—PDMS底板上的微形凹槽，3—探测电极，4—十字对准标志，5—PVFD纳米纤维膜，6—PDMS盖板，7—PDMS薄膜，8—探测电极接线孔，9—进气口，10—进液口， 11—流体出口。1—PDMS base plate, 2—micro groove on PDMS base plate, 3—detection electrode, 4—cross alignment mark, 5—PVFD nanofiber membrane, 6—PDMS cover plate, 7—PDMS film, 8—detection electrode Wiring hole, 9—air inlet, 10—liquid inlet, 11—fluid outlet.
具体实施方式detailed description
以下结合附图对本实用新型实施例作进一步说明：Below in conjunction with accompanying drawing, the utility model embodiment is further described:
如附图7、图8所示，本实用新型用于粘度测试的具有自供电功能的微流控芯片，是基于压电发电效应的在微流控芯片中进行粘度测试的方法。所述微流控芯片分为五层，自下而上各层依次是：带微形凹槽的PDMS底板、PDMS底板上微形凹槽两侧的电极对、电极上方的一层PVDF纳米纤维薄膜、PVDF纳米纤维薄膜上的一层面积较大的PDMS薄膜、最上一层带微流通道的PDMS盖板。所述微流控芯片制作方法是：先通过SU8光刻胶的光刻以及脱模技术制作带有微形凹槽的PDMS底板和微流通道PDMS盖板，再通过掩膜版磁控溅射的方法在PDMS底板的微形凹槽两侧制作一对探测电极，并将提前通过静电纺丝法制作的PVDF薄膜转移到电极上。盖板下方是一层通过匀胶并超声下来通过键合工艺与盖板键合在一起的PDMS薄膜。最后将盖板与底板键合在一起，形成完整的器件。通过在微流控芯片中采集不同粘度液体的机械能并转换为压电材料的电压输出，对输出电压进行测量分析实现一种无需供电的粘度测试。通过该方法进行粘度测试对样品的需求量较小、对样品的种类没有要求、测试时间短，无需供电、结构稳定且有利于微流控芯片的集成，有利于制作微流控芯片粘度计向小型化甚至手持式应用拓展。As shown in accompanying drawings 7 and 8, the self-powered microfluidic chip used for viscosity testing of the present invention is a method for viscosity testing in the microfluidic chip based on the piezoelectric power generation effect. The microfluidic chip is divided into five layers, and the layers from bottom to top are: PDMS bottom plate with micro-shaped grooves, electrode pairs on both sides of the micro-shaped grooves on the PDMS bottom plate, and a layer of PVDF nanofibers above the electrodes. A PDMS film with a larger area on the film, a PVDF nanofiber film, and a PDMS cover plate with a microfluidic channel on the top layer. The manufacturing method of the microfluidic chip is as follows: first, the PDMS base plate with micro-shaped grooves and the PDMS cover plate of the microfluidic channel are produced through the photolithography of SU8 photoresist and the demoulding technology, and then the magnetron sputtering is carried out through the mask plate. The method made a pair of detection electrodes on both sides of the micro-groove of the PDMS base plate, and transferred the PVDF film prepared by electrospinning in advance to the electrodes. Below the cover plate is a layer of PDMS film bonded to the cover plate through a bonding process through glue leveling and ultrasonic down. Finally, the cover plate and the base plate are bonded together to form a complete device. By collecting the mechanical energy of liquids with different viscosities in the microfluidic chip and converting it into the voltage output of the piezoelectric material, the output voltage is measured and analyzed to realize a viscosity test without power supply. Viscosity testing by this method has a small demand for samples, no requirements for the type of samples, short test time, no power supply, stable structure, and is conducive to the integration of microfluidic chips, which is conducive to the production of microfluidic chip viscometers. Miniaturization and even handheld application expansion.
参见附图2～附图8，本实用新型用于粘度测试的微流控芯片，包括自下而上依层次分布的：PDMS底板1、探测电极3、纳米纤维薄膜5、PDMS盖板6；所述探测电极3是在所述PDMS底板上通过公知的光刻、溅射及剥离工艺制作的一对导电电极；所述PDMS盖板6下表面加工有包括干流通道和支流通道的PDMS微流通道，支流通道宽度小于干流通道宽度；干流通道部分相应的位于纳米纤维薄膜5之上。所述纳米纤维薄膜是PVDF纳米纤维薄膜5；所述PVDF纳米纤维薄膜5与PDMS盖板6之间，还有一层PDMS薄膜7；所述PDMS薄膜7的面积大于所述PVDF纳米纤维薄膜5面积；所述PDMS盖板6通过十字对准标志，按顺序将PDMS微流通道、PDMS薄膜7、PVDF纳米纤维薄5膜压紧并键合在PDMS底板1的探测电极3上；所述PDMS底板上1，位于二探测电极3之间的下部，开有一个微型凹槽2，该凹槽有利于微流体驱动压电材料形变，可提高形变量以提高压电材料的电压输出。Referring to accompanying drawings 2 to 8, the microfluidic chip used for viscosity testing of the present invention includes: PDMS bottom plate 1, detection electrode 3, nanofiber film 5, PDMS cover plate 6 distributed in layers from bottom to top; The detection electrodes 3 are a pair of conductive electrodes fabricated on the PDMS base plate through known photolithography, sputtering and stripping processes; the lower surface of the PDMS cover plate 6 is processed with a PDMS micro flow channel including a main flow channel and a branch flow channel. The width of the branch flow channel is smaller than the width of the main flow channel; the part of the main flow channel is correspondingly located on the nanofiber film 5 . The nanofiber film is a PVDF nanofiber film 5; between the PVDF nanofiber film 5 and the PDMS cover plate 6, there is also a layer of PDMS film 7; the area of the PDMS film 7 is greater than the area of the PVDF nanofiber film 5 The PDMS cover plate 6 presses and bonds the PDMS microfluidic channel, the PDMS film 7, and the PVDF nanofiber thin film 5 on the detection electrode 3 of the PDMS base plate 1 in order through the cross alignment mark; the PDMS base plate The upper part 1, located at the lower part between the two detection electrodes 3, is provided with a micro-groove 2, which is beneficial to the micro-fluid to drive the deformation of the piezoelectric material, and can increase the amount of deformation to increase the voltage output of the piezoelectric material.
所述干流通道的宽度设定为位于PDMS底板的微型通孔正上方部分通道宽度，小于其它位置通道宽度。The width of the main flow channel is set to be the width of the part of the channel directly above the micro-through hole of the PDMS base plate, which is smaller than the channel width of other positions.
采用压电系数以及柔性都非常好的PVDF压电纳米纤维作为纳米纤维薄膜压电材料，该材料能够承受超大幅度的应变且制备过程非常简单、转移利用的可操作性很强。PVDF piezoelectric nanofibers with very good piezoelectric coefficient and flexibility are used as the nanofiber film piezoelectric material. The material can withstand ultra-large strains, and the preparation process is very simple, and the transfer and utilization are very operable.
在PDMS盖板6与PVDF纳米纤维薄膜5压电材料之间增加一层非常薄的PDMS薄膜，该薄膜将流体与压电材料隔开，不仅可以避免流体中的带电粒子对压电材料的屏蔽作用降低电压输出，还能防止流体的长期冲击对压电材料的损坏而降低器件的使用寿命。Add a very thin layer of PDMS film between the PDMS cover plate 6 and the PVDF nanofiber film 5 piezoelectric material, this film separates the fluid from the piezoelectric material, not only can avoid the shielding of the piezoelectric material by the charged particles in the fluid The effect is to reduce the voltage output, and it can also prevent the long-term impact of the fluid from damaging the piezoelectric material and reducing the service life of the device.
位于PDMS盖板6下表面的干流通道中，与电极探测部分对应的通道宽度尺寸相对于其他部分要窄，流体在通过该段微通道时流速会增加，流体下方压电材料所受到的应力也会增加，因此探测电极两端电压输出相应的增加。In the main flow channel located on the lower surface of the PDMS cover plate 6, the channel width dimension corresponding to the electrode detection part is narrower than other parts. When the fluid passes through this microchannel, the flow rate will increase, and the stress on the piezoelectric material under the fluid will also increase. Will increase, so the voltage output across the detection electrode will increase accordingly.
本实用新型一种用于粘度测试的微流控芯片的制作过程包括如下步骤：A manufacturing process of a microfluidic chip used for viscosity testing of the utility model comprises the following steps:
步骤一：通过SU8光刻胶的光刻以及脱模技术，制作带有微形通孔和微流通道的PDMS底板和PDMS盖板；Step 1: Fabricate the PDMS base plate and PDMS cover plate with micro-shaped through-holes and micro-fluidic channels through the photolithography of SU8 photoresist and the release technology;
步骤二：通过掩膜版磁控溅射的方法，在PDMS底板的微形通孔两侧制作一对探测电极，并将所述PVDF薄膜转移到电极上；Step 2: Make a pair of detection electrodes on both sides of the micro-shaped through hole of the PDMS base plate by mask plate magnetron sputtering, and transfer the PVDF film to the electrodes;
步骤三：通过匀胶并超声波剥离一层PDMS薄膜，再通过键合工艺将所述PDMS薄膜键合在PDMS盖板下方；Step 3: Peel off a layer of PDMS film by uniform glue and ultrasonic wave, and then bond the PDMS film under the PDMS cover plate through a bonding process;
步骤四：将底板与盖板两部分键合在一起，制作成用于粘度测试的微流控芯片。Step 4: Bond the two parts of the bottom plate and the cover plate together to make a microfluidic chip for viscosity testing.
以下三个实施例，是通过采用不同制作工艺及不同内部结构尺寸的选定而进行的制作方法，用以说明本实用新型一种用于粘度测试的微流控芯片的实现：The following three examples are the production methods by adopting different production processes and the selection of different internal structure sizes to illustrate the realization of a microfluidic chip for viscosity testing of the present invention:
实施例一：Embodiment one:
1.1静电纺丝法制备PVDF纳米纤维1.1 Preparation of PVDF nanofibers by electrospinning
1.1.1 PVDF前驱液的配置：将二甲基甲酰胺（DMF）与丙酮按体积百分比为30%∶70%的比例混合并搅拌均匀；按PVDF的浓度为0.12g/ml的比例向所述DMF和丙酮的混合液中加入PVDF粉末，并在60℃的条件下密封搅拌60min，直至整个溶液为澄清透明状。1.1.1 Configuration of PVDF precursor solution: mix dimethylformamide (DMF) and acetone at a ratio of 30%:70% by volume and stir evenly; Add PVDF powder to the mixture of DMF and acetone, and seal and stir at 60°C for 60 min until the whole solution is clear and transparent.
1.1.2 静电纺丝：将步骤1.1.1制备的PVDF前驱液吸入注射器中，并将注射器安装到微量注射泵上，再将注射器针头接入直流电压源的正极，贴在接受极板上的两片铝箔接直流电压源负极；针头的方向与接受极板面垂直，针头与接收极板的距离为15cm，直流电压源电压为15kV，微量注射泵的推进速度为50ul/min，环境湿度控制在40%以下、温度控制在25℃以上；PVDF纳米线用洗净的硅片进行接收，所述硅片置于贴在接受极板上的两片铝箔片之间；静电纺丝时间为30min。1.1.2 Electrospinning: Inhale the PVDF precursor solution prepared in step 1.1.1 into the syringe, install the syringe on the micro-injection pump, connect the needle of the syringe to the positive pole of the DC voltage source, and attach it to the receiving plate. Two pieces of aluminum foil are connected to the negative electrode of the DC voltage source; the direction of the needle is perpendicular to the surface of the receiving plate, the distance between the needle and the receiving plate is 15cm, the voltage of the DC voltage source is 15kV, the propulsion speed of the micro-injection pump is 50ul/min, and the ambient humidity is controlled Below 40%, the temperature is controlled above 25°C; PVDF nanowires are received by a cleaned silicon wafer, and the silicon wafer is placed between two pieces of aluminum foil attached to the receiving plate; the electrospinning time is 30min .
1.2微流通道盖板以及带微形凹槽的PDMS底板制备1.2 Preparation of microfluidic channel cover plate and PDMS bottom plate with micro-grooves
1.2.1石英片清洗：取长宽均为20mm、厚度2mm的石英载玻片，依次放入丙酮、酒精、去离子水中分别进行超声波清洗，每次清洗时间10min，清洗完后将载波片浸入干净的去离子水中。1.2.1 Cleaning of quartz slices: Take a quartz glass slide with a length and width of 20 mm and a thickness of 2 mm, put them in acetone, alcohol, and deionized water for ultrasonic cleaning respectively, and each cleaning time is 10 minutes. After cleaning, immerse the slide in the clean deionized water.
1.2.2涂覆光刻胶：自去离子水中取出石英玻璃片→氮气吹干→放置80℃环境中烘烤12min→取出冷却10min→在匀胶机上涂覆光刻胶→放置在60℃环境中烘烤15min→升温至95℃烘烤120min→取出冷却10min；所述涂覆光刻胶的匀胶机转速为900r.p.m，涂覆时间设定为40s。1.2.2 Coating photoresist: Take out the quartz glass sheet from deionized water → dry it with nitrogen gas → place it in an environment of 80°C for 12 minutes → take it out and cool it for 10 minutes → apply photoresist on a coater → place it in an environment of 60°C Baking at medium temperature for 15 minutes → raising the temperature to 95°C and baking for 120 minutes → taking out and cooling for 10 minutes; the speed of the coater for coating the photoresist is 900r.p.m, and the coating time is set at 40s.
1.2.3制备微流通道母版：将设定尺寸的微流通道掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光20s→取出并放置60℃环境中烘烤15min→升温至90℃烘烤40min→取出冷却10min→在显影液中显影15min→取出后用异丙醇冲洗氮气吹干→放置135℃环境中坚膜120min，制成微流通道母版；所述设定尺寸的微流通道掩膜板的主干流通道宽度为600μm，支流通道的宽度为300μm；芯片探测部分干流通道宽度为300μm，所述石英玻璃片上，也光刻有与PDMS底板十字对准标志位置对应的十字对准标志。1.2.3 Preparation of the microfluidic channel master: place the microfluidic channel mask plate of the set size on the above-mentioned quartz glass plate coated with photoresist, then put the quartz glass plate into the photolithography machine for exposure for 20 seconds → take it out And put it in the environment of 60 ℃ and bake for 15 minutes → raise the temperature to 90 ℃ and bake for 40 minutes → take it out and cool it for 10 minutes → develop it in the developer for 15 minutes → take it out and rinse it with isopropanol and blow it dry with nitrogen → place it in the environment of 135 ℃ for 120 minutes to make the film The microfluidic channel master plate; the width of the main flow channel of the microfluidic channel mask plate of the set size is 600 μm, and the width of the branch flow channel is 300 μm; the width of the main flow channel of the chip detection part is 300 μm. A cross alignment mark corresponding to the position of the cross alignment mark on the PDMS base plate is engraved.
1.2.4制备微形凹槽母版：将设定尺寸的微形凹槽掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光20s→取出并放置60℃环境中烘烤15min→升温至90℃烘烤40min→取出冷却10min→在显影液中显影15min→取出后用异丙醇冲洗氮气吹干→放置135℃环境中坚膜120min，制成微形凹槽母版；设定所述微形凹槽掩膜板尺寸的长度为1mm，宽度为400μm；所述石英玻璃片上，也光刻有与PDMS盖板十字对准标志位置对应的十字对准标志。1.2.4 Preparation of micro-groove master: place the micro-groove mask plate of the set size on the above-mentioned quartz glass sheet coated with photoresist, and then put the quartz glass sheet into the photolithography machine for exposure for 20s →Take it out and bake it at 60°C for 15 minutes→raise the temperature to 90°C and bake it for 40 minutes→take it out and cool it for 10 minutes→develop it in the developer for 15 minutes→take it out and rinse it with isopropanol and dry it with nitrogen gas→place it at 135°C for 120 minutes to harden the film. Make a micro-groove master; set the length of the micro-groove mask to 1 mm and the width to 400 μm; the quartz glass is also photoengraved with a cross alignment mark corresponding to the position of the PDMS cover plate cross alignment sign.
1.2.5制备PDMS混合物：按10:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物。1.2.5 Preparation of PDMS mixture: According to the mass ratio of 10:1, polydimethylsiloxane (PDMS) prepolymer and curing agent were mixed and stirred evenly to prepare a PDMS mixture.
1.2.6制备带PDMS微流通道的PDMS盖板：将所述微流通道母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至90℃环境中烘烤90min→取出冷却至室温→从微流通道母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微流通道，制成带微通道的PDMS盖板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。1.2.6 Preparation of PDMS cover plate with PDMS microfluidic channel: place the microfluidic channel master horizontally in a petri dish → pour the PDMS mixture into the petri dish → let it stand until all the air bubbles in the petri dish are discharged →Take it out and put it in an environment of 90°C and bake for 90min→Take it out and cool it to room temperature→Peel off the cured PDMS mixture from the microfluidic channel master→Cut out the required microfluidic channel according to the set size to make a microchannel PDMS cover plate; when the master plate is placed in the petri dish, the side that has been coated with photoresist is facing up.
1.2.7制备带微形凹槽的PDMS底板：将所述微形凹槽母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至90℃环境中烘烤90min→取出冷却至室温→从微形凹槽母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微形凹槽，制成带微形凹槽的PDMS底板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。1.2.7 Prepare the PDMS bottom plate with micro-grooves: Place the micro-groove master horizontally in the petri dish → pour the PDMS mixture into the petri dish → let it stand until all the air bubbles in the petri dish are discharged → Take it out and put it in an environment of 90°C and bake for 90 minutes → Take it out and cool it to room temperature → Remove the cured PDMS mixture from the micro-groove master → Cut out the required micro-groove according to the set size to make a tape A PDMS base plate with micro-grooves; when the master plate is placed in a petri dish, the side coated with photoresist faces upward.
1.3 PDMS薄膜制备工艺1.3 Preparation process of PDMS film
1.3.1制备PDMS混合物：按10:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物，静置1h至气泡全部排出。1.3.1 Preparation of PDMS mixture: According to the mass ratio of 10:1, take polydimethylsiloxane (PDMS) prepolymer and curing agent, mix and stir evenly to make PDMS mixture, let it stand for 1h until all the bubbles are discharged .
1.3.2涂覆PDMS混合物：自去离子水中取出提前裁好的长宽均为20mm的载玻片→氮气吹干→在匀胶机上涂覆PDMS混合物→匀胶机先以600r.p.m旋转10s再以4000r.p.m旋转40s→取下后静置12h后在烘箱中以90℃烘烤60min→取出冷却10min。1.3.2 Coating the PDMS mixture: Take out the pre-cut glass slides with a length and width of 20mm from deionized water → blow dry with nitrogen → coat the PDMS mixture on the homogenizer → first rotate the homogenizer at 600r.p.m for 10s Then rotate at 4000r.p.m for 40s → take it off and let it stand for 12 hours, then bake it in an oven at 90°C for 60 minutes → take it out and cool it for 10 minutes.
1.3.3 PDMS薄膜的脱模：将前面涂膜并固化后的带有PDMS薄膜的载璃片于丙酮中在50℃条件下超声60min→取出后在去离子水中在50℃继续超声120min 至薄膜脱落→将薄膜从玻片上撕下用氮气吹干待用。1.3.3 Demolding of PDMS film: Sonicate the previously coated and cured glass slide with PDMS film in acetone at 50°C for 60 minutes → take it out and continue ultrasonication at 50°C for 120 minutes to the film Falling off→Tear off the film from the glass slide and dry it with nitrogen gas for later use.
1.4 器件组装工艺1.4 Device assembly process
1.4.1将步骤1.2制备的带有微形凹槽的PDMS底板用提前设计好金属掩膜版掩膜，在Ar气氛下，以80W溅射功率，采用标准溅射工艺在PDMS底板表面溅射120s的铂电极。1.4.1 Use the pre-designed metal mask on the PDMS base plate with micro-grooves prepared in step 1.2, and sputter on the surface of the PDMS base plate with a standard sputtering process in an Ar atmosphere with a sputtering power of 80W 120s of platinum electrodes.
1.4.2取按步骤1.1制备的PVDF纳米纤维薄膜用小刀切取1mm×3mm大小，在显微镜的辅助下转移到溅射的铂电极上，制成盖板。1.4.2 Take the PVDF nanofiber film prepared in step 1.1 and cut it with a knife to a size of 1mm×3mm, and transfer it to the sputtered platinum electrode with the aid of a microscope to make a cover plate.
1.4.3将带有微通道的PDMS盖板以及PDMS薄膜放在功率为18W、波长为254nm的紫外灯箱中照射3h，再取出将PDMS盖板与PDMS薄膜贴合压紧并保持12h，制成底板。1.4.3 Put the PDMS cover plate and PDMS film with microchannels in an ultraviolet light box with a power of 18W and a wavelength of 254nm for 3h, then take it out, stick the PDMS cover plate and PDMS film tightly and keep it for 12h, the finished product bottom plate.
1.4.4将制成的盖板和底板放在功率为18W、波长为254nm的紫外灯箱中照射3h后取出，将盖板与底板贴合压紧，保持12h使其键合在一起形成完整的具有自供电功能的粘度测试微流控芯片。1.4.4 Put the finished cover and base plate in an ultraviolet light box with a power of 18W and a wavelength of 254nm for 3 hours, then take it out, press the cover plate and the base plate tightly, and keep it for 12 hours to bond them together to form a complete Viscosity testing microfluidic chip with self-powered function.
1.5 芯片的测试1.5 Chip testing
1.5.1将按步骤四制得微流控芯片，分别在微通道气液进出口以及电极的引线处扎上小孔，用提前做好的测试平台将微流控芯片固定在测试平台上，并在电极两端压上压针并连接到测试电表上，在PDMS微通道进出口插上针管并用流体程控仪从气液进口往微通道中注入气体和液体。电表测试的电压数据通过LabVIEW软件实时显示并记录在电脑上。1.5.1 The microfluidic chip will be prepared according to step 4, and small holes will be made at the gas-liquid inlet and outlet of the microchannel and the lead wire of the electrode, and the microfluidic chip will be fixed on the test platform with the test platform prepared in advance. And press pins on both ends of the electrodes and connect them to the test meter, insert needle tubes at the inlet and outlet of the PDMS microchannel, and use a fluid program controller to inject gas and liquid into the microchannel from the gas-liquid inlet. The voltage data tested by the meter is displayed and recorded on the computer in real time through LabVIEW software.
1.5.2用流体程控仪以不同的压强往微流控芯片中打入同一粘度的液体和气体，检测电极两端的电压输出情况。1.5.2 Use a fluid program controller to inject liquid and gas of the same viscosity into the microfluidic chip at different pressures, and detect the voltage output at both ends of the electrodes.
1.5.3用流体程控仪以同一压强往微流控芯片中打入不同粘度的液体和气体，检测电极两端的电压输出情况。1.5.3 Use a fluid program controller to inject liquids and gases of different viscosities into the microfluidic chip at the same pressure, and detect the voltage output at both ends of the electrodes.
实施例二：Embodiment two:
2.1通过静电纺丝法制备PVDF纳米纤维2.1 Preparation of PVDF nanofibers by electrospinning
2.1.1 PVDF前驱液的配置：将二甲基甲酰胺（DMF）与丙酮按体积百分比为30%∶70%的比例混合并搅拌均匀；按PVDF的浓度为0.12g/ml的比例向所述DMF和丙酮的混合液中加入PVDF粉末，并在60℃的条件下密封搅拌60min，直至整个溶液为澄清透明状。2.1.1 Configuration of PVDF precursor solution: Mix dimethylformamide (DMF) and acetone at a ratio of 30%:70% by volume and stir evenly; Add PVDF powder to the mixture of DMF and acetone, and seal and stir at 60°C for 60 min until the whole solution is clear and transparent.
2.1.2 静电纺丝：将步骤2.1.1制备的PVDF前驱液吸入注射器中，并将注射器安装到微量注射泵上，再将注射器针头接入直流电压源的正极，贴在接受极板上的两片铝箔接直流电压源负极；针头的方向与接受极板面垂直，针头与接收极板的距离为15cm，直流电压源电压为15kV，微量注射泵的推进速度为50ul/min，环境湿度控制在40%以下、温度控制在25℃以上；PVDF纳米线用洗净的硅片进行接收，所述硅片置于贴在接受极板上的两片铝箔片之间；静电纺丝时间为30min。2.1.2 Electrospinning: Inhale the PVDF precursor solution prepared in step 2.1.1 into the syringe, install the syringe on the micro-injection pump, connect the needle of the syringe to the positive pole of the DC voltage source, and attach it to the receiving plate. Two pieces of aluminum foil are connected to the negative electrode of the DC voltage source; the direction of the needle is perpendicular to the surface of the receiving plate, the distance between the needle and the receiving plate is 15cm, the voltage of the DC voltage source is 15kV, the propulsion speed of the micro-injection pump is 50ul/min, and the ambient humidity is controlled Below 40%, the temperature is controlled above 25°C; PVDF nanowires are received by a cleaned silicon wafer, and the silicon wafer is placed between two pieces of aluminum foil attached to the receiving plate; the electrospinning time is 30min .
2.2 微流通道盖板以及带微形凹槽的PDMS底板的制备2.2 Preparation of microfluidic channel cover plate and PDMS bottom plate with micro-grooves
2.2.1石英片清洗：取长宽均为20mm、厚度2mm的石英载玻片，依次放入丙酮、酒精、去离子水中分别进行超声波清洗，每次清洗时间10min，清洗完后将载波片浸入干净的去离子水中。2.2.1 Cleaning of quartz slices: Take a quartz glass slide with a length and width of 20 mm and a thickness of 2 mm, put them in acetone, alcohol, and deionized water for ultrasonic cleaning respectively, each cleaning time is 10 minutes, and immerse the slide in the clean deionized water.
2.2.2涂覆光刻胶：自去离子水中取出石英玻璃片→氮气吹干→放置80℃环境中烘烤12min→取出冷却10min→在匀胶机上涂覆光刻胶→放置在60℃环境中烘烤15min→升温至95℃烘烤120min→取出冷却10min；所述涂覆光刻胶的匀胶机转速为900r.p.m，涂覆时间设定为40s。2.2.2 Coating photoresist: Take out the quartz glass sheet from deionized water → dry it with nitrogen gas → place it in an environment of 80 ° C for 12 minutes → take it out and cool it for 10 minutes → apply photoresist on a coater → place it in an environment of 60 ° C Baking at medium temperature for 15 minutes → raising the temperature to 95°C and baking for 120 minutes → taking out and cooling for 10 minutes; the speed of the coater for coating the photoresist is 900r.p.m, and the coating time is set at 40s.
2.2.3制备微流通道母版：将设定尺寸的微流通道掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光20s→取出并放置60℃环境中烘烤15min→升温至90℃烘烤40min→取出冷却10min→在显影液中显影15min→取出后用异丙醇冲洗氮气吹干→放置135℃环境中坚膜120min，制成微流通道母版；所述设定尺寸的微流通道掩膜板的主干流通道宽度为400μm，支流通道的宽度为200μm；芯片探测部分干流通道宽度为200μm，所述石英玻璃片上，也光刻有与PDMS底板十字对准标志位置对应的十字对准标志。2.2.3 Preparation of the microfluidic channel master: place the microfluidic channel mask plate of the set size on the above-mentioned quartz glass sheet coated with photoresist, then put the quartz glass sheet into the photolithography machine for exposure for 20 seconds → take it out And put it in the environment of 60 ℃ and bake for 15 minutes → raise the temperature to 90 ℃ and bake for 40 minutes → take it out and cool it for 10 minutes → develop it in the developer for 15 minutes → take it out and rinse it with isopropanol and blow it dry with nitrogen → place it in the environment of 135 ℃ for 120 minutes to make the film The microfluidic channel master plate; the width of the main flow channel of the microfluidic channel mask plate of the set size is 400 μm, and the width of the branch flow channel is 200 μm; the width of the main flow channel of the chip detection part is 200 μm, and the optical A cross alignment mark corresponding to the position of the cross alignment mark on the PDMS base plate is engraved.
2.2.4制备微形凹槽母版：将设定尺寸的微形凹槽掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光20s→取出并放置60℃环境中烘烤15min→升温至90℃烘烤40min→取出冷却10min→在显影液中显影15min→取出后用异丙醇冲洗氮气吹干→放置135℃环境中坚膜120min，制成微形凹槽母版；所述设定尺寸的长度为1mm，宽度为300μm；所述石英玻璃片上，也光刻有与PDMS盖板十字对准标志位置对应的十字对准标志。2.2.4 Preparation of micro-groove master: place the micro-groove mask plate of the set size on the above-mentioned quartz glass sheet coated with photoresist, and then put the quartz glass sheet into the photolithography machine for exposure for 20s →Take it out and bake it at 60°C for 15 minutes→raise the temperature to 90°C and bake it for 40 minutes→take it out and cool it for 10 minutes→develop it in the developer for 15 minutes→take it out and rinse it with isopropanol and dry it with nitrogen gas→place it at 135°C for 120 minutes to harden the film. A micro-groove master is made; the length of the set size is 1 mm, and the width is 300 μm; a cross alignment mark corresponding to the position of the cross alignment mark on the PDMS cover is also photoengraved on the quartz glass plate.
2.2.5制备PDMS混合物：按10:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物。2.2.5 Preparation of PDMS mixture: According to the mass ratio of 10:1, polydimethylsiloxane (PDMS) prepolymer and curing agent were mixed and stirred evenly to prepare a PDMS mixture.
2.2.6制备带PDMS微流通道的PDMS盖板：将所述微流通道母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至90℃环境中烘烤90min→取出冷却至室温→从微流通道母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微流通道，制成带微通道的PDMS盖板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。2.2.6 Preparation of PDMS cover plate with PDMS microfluidic channel: place the microfluidic channel master horizontally in a petri dish → pour the PDMS mixture into the petri dish → let it stand until all the air bubbles in the petri dish are discharged →Take it out and put it in an environment of 90°C and bake for 90min→Take it out and cool it to room temperature→Peel off the cured PDMS mixture from the microfluidic channel master→Cut out the required microfluidic channel according to the set size to make a microchannel PDMS cover plate; when the master plate is placed in the petri dish, the side that has been coated with photoresist is facing up.
2.2.7制备带微形凹槽的PDMS底板：将所述微形凹槽母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至90℃环境中烘烤90min→取出冷却至室温→从微形凹槽母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微形凹槽，制成带微形凹槽的PDMS底板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。2.2.7 Prepare the PDMS bottom plate with micro-grooves: Place the micro-groove master horizontally in the petri dish → pour the PDMS mixture into the petri dish → let it stand until all the air bubbles in the petri dish are discharged → Take it out and put it in an environment of 90°C and bake for 90 minutes → Take it out and cool it to room temperature → Remove the cured PDMS mixture from the micro-groove master → Cut out the required micro-groove according to the set size to make a tape A PDMS base plate with micro-grooves; when the master plate is placed in a petri dish, the side coated with photoresist faces upward.
2.3 PDMS薄膜的制备工艺2.3 Preparation process of PDMS film
2.3.1制备PDMS混合物：按10:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物，静置1h至气泡全部排出。2.3.1 Preparation of PDMS mixture: According to the mass ratio of 10:1, take polydimethylsiloxane (PDMS) prepolymer and curing agent, mix and stir evenly to make PDMS mixture, let it stand for 1h until all the bubbles are discharged .
2.3.2涂覆PDMS混合物：自去离子水中取出提前裁好的长宽均为20mm的载玻片→氮气吹干→在匀胶机上涂覆PDMS混合物→匀胶机先以600r.p.m旋转10s再以4000r.p.m旋转40s→取下后静置12h后在烘箱中以90℃烘烤60min→取出冷却10min。2.3.2 Coating the PDMS mixture: Take out the pre-cut glass slides with a length and width of 20mm from deionized water → blow dry with nitrogen → coat the PDMS mixture on the homogenizer → first rotate the homogenizer at 600r.p.m for 10s Then rotate at 4000r.p.m for 40s → take it off and let it stand for 12 hours, then bake it in an oven at 90°C for 60 minutes → take it out and cool it for 10 minutes.
2.3.3 PDMS薄膜的脱模：将前面涂膜并固化后的带有PDMS薄膜的载璃片于丙酮中在50℃条件下超声60min→取出后在去离子水中在50℃继续超声120min 至薄膜脱落→将薄膜从玻片上撕下用氮气吹干待用。2.3.3 Demolding of PDMS film: Sonicate the previously coated and cured glass slide with PDMS film in acetone at 50°C for 60 minutes → take it out and continue ultrasonication at 50°C for 120 minutes to the film Falling off→Tear off the film from the glass slide and dry it with nitrogen gas for later use.
2.4 器件组装工艺2.4 Device assembly process
2.4.1将步骤2.2制备的带有微形凹槽的PDMS底板用提前设计好金属掩膜版掩膜，在Ar气氛下以80W溅射功率，采用标准的溅射工艺在PDMS底板表面先溅射120s的铂电极。2.4.1 Use the pre-designed metal mask on the PDMS bottom plate with micro-grooves prepared in step 2.2, and use a standard sputtering process to sputter on the surface of the PDMS bottom plate with a sputtering power of 80W in an Ar atmosphere. Shoot the platinum electrode for 120s.
2.4.2取按步骤2.1制备的PVDF纳米纤维薄膜，用小刀切取1×3mm大小，在显微镜的辅助下转移到溅射的铂电极上，制成盖板。2.4.2 Take the PVDF nanofiber film prepared in step 2.1, cut it into a size of 1×3 mm with a knife, and transfer it to the sputtered platinum electrode with the aid of a microscope to make a cover plate.
2.4.3取带有微通道的PDMS盖板以及PDMS薄膜放在功率为18W、波长为254nm的紫外灯箱中照射3h，再取出将PDMS盖板与PDMS薄膜贴合压紧保持12h，制成底板。2.4.3 Take the PDMS cover plate and PDMS film with microchannels and put them in an ultraviolet light box with a power of 18W and a wavelength of 254nm for 3 hours, then take out the PDMS cover plate and PDMS film and press them tightly for 12 hours to make a bottom plate .
2.4.4将制成的盖板和底板同时放在功率为18W、波长为254nm的紫外灯箱中照射3h后取出贴合压紧保持12h使其键合在一起，形成完整的具有自供电功能的粘度测试微流控芯片。2.4.4 Put the finished cover plate and bottom plate in an ultraviolet light box with a power of 18W and a wavelength of 254nm for 3 hours, then take them out and press them tightly for 12 hours to bond them together to form a complete self-power supply Viscosity testing microfluidic chip.
2.5 芯片的测试2.5 Chip testing
2.5.1将按步骤四制得微流控芯片，分别在微通道气液进出口以及电极的引线处扎上小孔，用提前做好的测试平台将微流控芯片固定在测试平台上，并在电极两端压上压针并连接到测试电表上，在PDMS微通道进出口插上针管并用流体程控仪从气液进口往微通道中注入气体和液体。电表测试的电压数据通过LabVIEW软件实时的显示并记录在电脑上。2.5.1 The microfluidic chip will be prepared according to step 4, and small holes will be made at the gas-liquid inlet and outlet of the microchannel and the lead wire of the electrode, and the microfluidic chip will be fixed on the test platform with the test platform prepared in advance. And press pins on both ends of the electrodes and connect them to the test meter, insert needle tubes at the inlet and outlet of the PDMS microchannel, and use a fluid program controller to inject gas and liquid into the microchannel from the gas-liquid inlet. The voltage data tested by the meter is displayed and recorded on the computer in real time through LabVIEW software.
2.5.2用流体程控仪以不同的压强往微流控芯片中打入同一粘度的液体和气体，检测电极两端的电压输出情况。2.5.2 Use a fluid program controller to inject liquid and gas of the same viscosity into the microfluidic chip at different pressures, and detect the voltage output at both ends of the electrodes.
2.5.3用流体程控仪以同一压强往微流控芯片中打入不同粘度的液体和气体，检测电极两端的电压输出情况。2.5.3 Use a fluid program controller to inject liquids and gases with different viscosities into the microfluidic chip at the same pressure, and detect the voltage output at both ends of the electrodes.
实施例三：Embodiment three:
3.1通过静电纺丝法制备PVDF纳米纤维3.1 Preparation of PVDF nanofibers by electrospinning
3.1.1 PVDF前驱液的配置：将二甲基甲酰胺（DMF）与丙酮按体积百分比为30%∶70%的比例混合并搅拌均匀；按PVDF的浓度为0.12g/ml的比例向所述DMF和丙酮的混合液中加入PVDF粉末，并在60℃的条件下密封搅拌60min，直至整个溶液为澄清透明状。3.1.1 Configuration of PVDF precursor solution: mix dimethylformamide (DMF) and acetone at a ratio of 30%:70% by volume and stir evenly; Add PVDF powder to the mixture of DMF and acetone, and seal and stir at 60°C for 60 min until the whole solution is clear and transparent.
3.1.2 静电纺丝：将步骤3.1.1制备的PVDF前驱液吸入注射器中，并将注射器安装到微量注射泵上，再将注射器针头接入直流电压源的正极，贴在接受极板上的两片铝箔接直流电压源负极；针头的方向与接受极板面垂直，针头与接收极板的距离为15cm，直流电压源电压为15kV，微量注射泵的推进速度为50ul/min，环境湿度控制在40%以下、温度控制在25℃以上；PVDF纳米线用洗净的硅片进行接收，所述硅片置于贴在接受极板上的两片铝箔片之间；静电纺丝时间为30min。3.1.2 Electrospinning: Inhale the PVDF precursor solution prepared in step 3.1.1 into the syringe, install the syringe on the micro-injection pump, connect the needle of the syringe to the positive pole of the DC voltage source, and attach it to the receiving plate. Two pieces of aluminum foil are connected to the negative electrode of the DC voltage source; the direction of the needle is perpendicular to the surface of the receiving plate, the distance between the needle and the receiving plate is 15cm, the voltage of the DC voltage source is 15kV, the propulsion speed of the micro-injection pump is 50ul/min, and the ambient humidity is controlled Below 40%, the temperature is controlled above 25°C; PVDF nanowires are received by a cleaned silicon wafer, and the silicon wafer is placed between two pieces of aluminum foil attached to the receiving plate; the electrospinning time is 30min .
3.2 微流通道盖板以及带微形凹槽的PDMS底板的制备3.2 Preparation of microfluidic channel cover plate and PDMS bottom plate with micro-grooves
3.2.1石英片清洗：取长宽均为20mm、厚度2mm的石英载玻片，依次放入丙酮、酒精、去离子水中分别进行超声波清洗，每次清洗时间10min，清洗完后将载波片浸入干净的去离子水中。3.2.1 Cleaning of quartz slices: Take a quartz glass slide with a length and width of 20 mm and a thickness of 2 mm, and put them in acetone, alcohol, and deionized water for ultrasonic cleaning respectively. Each cleaning time is 10 minutes. After cleaning, immerse the slide in the clean deionized water.
3.2.2涂覆光刻胶：自去离子水中取出石英玻璃片→氮气吹干→放置80℃环境中烘烤12min→取出冷却10min→在匀胶机上涂覆光刻胶→放置在60℃环境中烘烤15min→升温至95℃烘烤120min→取出冷却10min；所述涂覆光刻胶的匀胶机转速为900r.p.m，涂覆时间设定为40s。3.2.2 Coating photoresist: Take out the quartz glass sheet from deionized water → dry it with nitrogen gas → place it in an environment of 80 ° C for 12 minutes → take it out and cool it for 10 minutes → apply photoresist on a coater → place it in an environment of 60 ° C Baking at medium temperature for 15 minutes → raising the temperature to 95°C and baking for 120 minutes → taking out and cooling for 10 minutes; the speed of the coater for coating the photoresist is 900r.p.m, and the coating time is set at 40s.
3.2.3制备微流通道母版：将设定尺寸的微流通道掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光20s→取出并放置60℃环境中烘烤15min→升温至90℃烘烤40min→取出冷却10min→在显影液中显影15min→取出后用异丙醇冲洗氮气吹干→放置135℃环境中坚膜120min，制成微流通道母版；所述设定尺寸的微流通道掩膜板的主干流通道宽度为200μm，支流通道的宽度为100μm；芯片探测部分干流通道宽度为100μm，所述石英玻璃片上，也光刻有与PDMS底板十字对准标志位置对应的十字对准标志。3.2.3 Preparation of the microfluidic channel master: place the microfluidic channel mask plate of the set size on the above-mentioned quartz glass sheet coated with photoresist, and then put the quartz glass sheet into the photolithography machine for exposure for 20 seconds → take it out And put it in the environment of 60 ℃ and bake for 15 minutes → raise the temperature to 90 ℃ and bake for 40 minutes → take it out and cool it for 10 minutes → develop it in the developer for 15 minutes → take it out and rinse it with isopropanol and blow it dry with nitrogen → place it in the environment of 135 ℃ for 120 minutes to make the film The microfluidic channel master plate; the width of the main flow channel of the microfluidic channel mask plate of the set size is 200 μm, and the width of the branch flow channel is 100 μm; the width of the main flow channel of the chip detection part is 100 μm. A cross alignment mark corresponding to the position of the cross alignment mark on the PDMS base plate is engraved.
3.2.4制备微形凹槽母版：将设定尺寸的微形凹槽掩膜板放在上述已涂覆光刻胶的石英玻璃片上，再将石英玻璃片放入光刻机中曝光20s→取出并放置60℃环境中烘烤15min→升温至90℃烘烤40min→取出冷却10min→在显影液中显影15min→取出后用异丙醇冲洗氮气吹干→放置135℃环境中坚膜120min，制成微形凹槽母版；所述设定尺寸的长度为1mm，宽度为200μm；所述石英玻璃片上，也光刻有与PDMS盖板十字对准标志位置对应的十字对准标志。3.2.4 Preparation of micro-groove master: place the micro-groove mask plate with a set size on the above-mentioned quartz glass sheet coated with photoresist, and then put the quartz glass sheet into the photolithography machine for exposure for 20s →Take it out and bake it at 60°C for 15 minutes→raise the temperature to 90°C and bake it for 40 minutes→take it out and cool it for 10 minutes→develop it in the developer for 15 minutes→take it out and rinse it with isopropanol and dry it with nitrogen gas→place it at 135°C for 120 minutes to harden the film. A micro-groove master is made; the length of the set size is 1 mm, and the width is 200 μm; a cross alignment mark corresponding to the position of the cross alignment mark on the PDMS cover is also photoengraved on the quartz glass plate.
3.2.5制备PDMS混合物：按10:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物。3.2.5 Preparation of PDMS mixture: According to the mass ratio of 10:1, polydimethylsiloxane (PDMS) prepolymer and curing agent were mixed and stirred evenly to prepare a PDMS mixture.
3.2.6制备带PDMS微流通道的PDMS盖板：将所述微流通道母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至90℃环境中烘烤90min→取出冷却至室温→从微流通道母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微流通道，制成带微通道的PDMS盖板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。3.2.6 Preparation of PDMS cover plate with PDMS microfluidic channel: place the microfluidic channel master horizontally in the petri dish → pour the PDMS mixture into the petri dish → let it stand until all the air bubbles in the petri dish are discharged →Take it out and put it in an environment of 90°C and bake for 90min→Take it out and cool it to room temperature→Peel off the cured PDMS mixture from the microfluidic channel master→Cut out the required microfluidic channel according to the set size to make a microchannel PDMS cover plate; when the master plate is placed in the petri dish, the side that has been coated with photoresist is facing up.
3.2.7制备带微形凹槽的PDMS底板：将所述微形凹槽母版水平放置在培养皿中→往培养皿中倒入所述PDMS混合物→静置至培养皿中的气泡全部排出→取出并放至90℃环境中烘烤90min→取出冷却至室温→从微形凹槽母版上揭下已固化的PDMS混合物→按设定尺寸切取所需要的微形凹槽，制成带微形凹槽的PDMS底板；所述母版放置在培养皿中时，已涂覆光刻胶的一面朝上。3.2.7 Preparation of PDMS bottom plate with micro-grooves: place the micro-groove master horizontally in a petri dish → pour the PDMS mixture into the petri dish → let it stand until all the air bubbles in the petri dish are discharged → Take it out and put it in an environment of 90°C and bake for 90 minutes → Take it out and cool it to room temperature → Remove the cured PDMS mixture from the micro-groove master → Cut out the required micro-groove according to the set size to make a tape A PDMS bottom plate with micro-grooves; when the master plate is placed in a petri dish, the side that has been coated with photoresist faces upward.
3.3 PDMS薄膜的制备工艺3.3 Preparation process of PDMS film
3.3.1制备PDMS混合物：按10:1的质量比例，取聚二甲基硅氧烷（PDMS）预聚物和固化剂进行混合并搅拌均匀，制成PDMS混合物，静置1h至气泡全部排出。3.3.1 Preparation of PDMS mixture: According to the mass ratio of 10:1, take polydimethylsiloxane (PDMS) prepolymer and curing agent, mix and stir evenly to make PDMS mixture, let it stand for 1h until all the bubbles are discharged .
3.3.2涂覆PDMS混合物：自去离子水中取出提前裁好的长宽均为20mm的载玻片→氮气吹干→在匀胶机上涂覆PDMS混合物→匀胶机先以600r.p.m旋转10s再以4000r.p.m旋转40s→取下后静置12h后在烘箱中以90℃烘烤60min→取出冷却10min。3.3.2 Coating the PDMS mixture: Take out the pre-cut glass slides with a length and width of 20mm from deionized water → blow dry with nitrogen → coat the PDMS mixture on the homogenizer → first rotate the homogenizer at 600r.p.m for 10s Then rotate at 4000r.p.m for 40s → take it off and let it stand for 12 hours, then bake it in an oven at 90°C for 60 minutes → take it out and cool it for 10 minutes.
3.3.3PDMS薄膜的脱模：将前述涂膜并固化后的带有PDMS薄膜的载璃片于丙酮中在50℃条件下超声60min→取出后在去离子水中在50℃继续超声120min 至薄膜脱落→将薄膜从玻片上撕下用氮气吹干待用。3.3.3 Demolding of PDMS film: Put the coated and cured glass slide with PDMS film in acetone at 50°C for 60 minutes → take it out and continue ultrasonication at 50°C for 120 minutes in deionized water until the film falls off → Tear off the film from the glass slide and dry it with nitrogen gas for later use.
3.4 器件组装工艺3.4 Device assembly process
3.4.1取按步骤3.2制得的带有微形凹槽的PDMS底板，用提前设计好金属掩膜版掩膜，在Ar气氛下以80W溅射功率采用标准的溅射工艺在表面先溅射120s的铂电极。3.4.1 Take the PDMS base plate with micro-grooves prepared according to step 3.2, use a pre-designed metal mask mask, and use a standard sputtering process to sputter on the surface under an Ar atmosphere with a sputtering power of 80W Shoot the platinum electrode for 120s.
3.4.2取按步骤3.1制备的PVDF纳米纤维薄膜，用小刀切取1×3mm大小，在显微镜的辅助下转移到溅射的铂电极上，制成盖板。3.4.2 Take the PVDF nanofiber film prepared in step 3.1, cut it into a size of 1×3 mm with a knife, and transfer it to the sputtered platinum electrode with the aid of a microscope to make a cover plate.
3.4.3取前面带有微流通道的PDMS盖板以及PDMS薄膜放在功率为18W、波长为254nm的紫外灯箱中照射3h后取出贴合压紧保持12h，制成底板。3.4.3 Take the PDMS cover plate and PDMS film with the microfluidic channel on the front and put it in an ultraviolet light box with a power of 18W and a wavelength of 254nm for 3 hours, then take it out, stick it, press it and keep it for 12 hours to make a bottom plate.
3.4.4取盖板和底板同时放在功率为18W、波长为254nm的紫外灯箱中照射3h，再取出并将盖板与底板贴合压紧保持12h，使其键合在一起形成完整的具有自供电功能的粘度测试微流控芯片。3.4.4 Take the cover plate and the bottom plate and put them in an ultraviolet light box with a power of 18W and a wavelength of 254nm for 3 hours, then take them out and press the cover plate and the bottom plate tightly for 12 hours to bond them together to form a complete Self-powered microfluidic chip for viscosity testing.
3.5芯片的测试3.5 Chip testing
3.5.1将按步骤3.4组装好的微流控芯片，分别在微通道气液进出口以及电极的引线处扎上小孔，用提前做好的测试平台将微流控芯片固定在测试平台上，并在电极两端压上压针并连接到测试电表上，在PDMS微通道进出口插上针管并用流体程控仪从气液进口往微通道中注入气体和液体。电表测试的电压数据通过LabVIEW软件实时的显示并记录在电脑上；3.5.1 Put the microfluidic chip assembled according to step 3.4 into small holes at the gas-liquid inlet and outlet of the microchannel and the lead wire of the electrode, and fix the microfluidic chip on the test platform with the test platform prepared in advance , and press pins on both ends of the electrode and connect it to the test meter, insert a needle tube at the inlet and outlet of the PDMS microchannel, and use a fluid program controller to inject gas and liquid into the microchannel from the gas-liquid inlet. The voltage data tested by the meter is displayed and recorded on the computer in real time through LabVIEW software;
3.5.2用流体程控仪以不同的压强往微流控芯片中打入同一粘度的液体和气体，检测电极两端的电压输出情况；3.5.2 Use the fluid program controller to inject liquid and gas of the same viscosity into the microfluidic chip at different pressures, and detect the voltage output at both ends of the electrodes;
3.5.3用流体程控仪以同一压强往微流控芯片中打入不同粘度的液体和气体，检测电极两端的电压输出情况；3.5.3 Use the fluid program controller to inject liquids and gases of different viscosities into the microfluidic chip at the same pressure, and detect the voltage output at both ends of the electrodes;
以上仅为本实用新型的实施例，但并不用于限制本实用新型，凡在本实用新型的精神和原则之内所做的任何修改、等同替换或改进等，均应包含在本实用新型的权利要求范围之内。The above are only embodiments of the present utility model, but are not intended to limit the present utility model. Any modifications, equivalent replacements or improvements made within the spirit and principles of the present utility model shall be included in the scope of the present utility model. within the scope of the claims.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620446357.7UCN205700594U (en) | 2016-05-17 | 2016-05-17 | A kind of micro-fluidic chip for viscosity test |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620446357.7UCN205700594U (en) | 2016-05-17 | 2016-05-17 | A kind of micro-fluidic chip for viscosity test |
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| CN205700594Utrue CN205700594U (en) | 2016-11-23 |
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| CN201620446357.7UWithdrawn - After IssueCN205700594U (en) | 2016-05-17 | 2016-05-17 | A kind of micro-fluidic chip for viscosity test |
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| CN105932151A (en)* | 2016-05-17 | 2016-09-07 | 湖北大学 | Micro-fluidic chip for viscosity testing, and preparation method |
| CN108414401A (en)* | 2018-01-30 | 2018-08-17 | 中国科学院电子学研究所 | Unicellular endochylema viscosity measuring device and method |
| CN108802135A (en)* | 2018-07-13 | 2018-11-13 | 复旦大学 | Using organic semiconductor as liquid viscosity sensor of light-sensitive material and preparation method thereof |
| CN109142452A (en)* | 2018-10-26 | 2019-01-04 | 浙江师范大学 | It is declined the blood viscoelastic force measuring device and method of hanging bridge sensor based on pressure drag |
| CN109158137A (en)* | 2018-10-26 | 2019-01-08 | 江苏德林环保技术有限公司 | A kind of preparation method of micro-fluidic chip |
| CN115178313A (en)* | 2022-08-05 | 2022-10-14 | 天津工业大学 | Design method of hollow micro-nano composite beam for biochemical molecule detection |
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105932151A (en)* | 2016-05-17 | 2016-09-07 | 湖北大学 | Micro-fluidic chip for viscosity testing, and preparation method |
| CN105932151B (en)* | 2016-05-17 | 2018-11-09 | 湖北大学 | Micro-fluidic chip and production method for viscosity test |
| CN108414401A (en)* | 2018-01-30 | 2018-08-17 | 中国科学院电子学研究所 | Unicellular endochylema viscosity measuring device and method |
| CN108414401B (en)* | 2018-01-30 | 2020-12-11 | 中国科学院电子学研究所 | Single-cell cytoplasmic viscosity measurement device and method |
| CN108802135A (en)* | 2018-07-13 | 2018-11-13 | 复旦大学 | Using organic semiconductor as liquid viscosity sensor of light-sensitive material and preparation method thereof |
| CN108802135B (en)* | 2018-07-13 | 2020-12-22 | 复旦大学 | Liquid viscosity sensor using organic semiconductor as photosensitive material and preparation method thereof |
| CN109142452A (en)* | 2018-10-26 | 2019-01-04 | 浙江师范大学 | It is declined the blood viscoelastic force measuring device and method of hanging bridge sensor based on pressure drag |
| CN109158137A (en)* | 2018-10-26 | 2019-01-08 | 江苏德林环保技术有限公司 | A kind of preparation method of micro-fluidic chip |
| CN109158137B (en)* | 2018-10-26 | 2021-02-02 | 江苏德林环保技术有限公司 | Preparation method of micro-fluidic chip |
| CN109142452B (en)* | 2018-10-26 | 2021-03-26 | 浙江师范大学 | Blood viscoelasticity measurement device and method based on piezoresistive microsuspension bridge sensor |
| CN115178313A (en)* | 2022-08-05 | 2022-10-14 | 天津工业大学 | Design method of hollow micro-nano composite beam for biochemical molecule detection |
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| C14 | Grant of patent or utility model | ||
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| AV01 | Patent right actively abandoned | Granted publication date:20161123 Effective date of abandoning:20181109 | |
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