CN109970023A - A kind of manufacturing method of flexible microelectrode - Google Patents
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- B81C1/00349—Creating layers of material on a substrate
- B81C1/00373—Selective deposition, e.g. printing or microcontact printing
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Abstract
本发明公开了一种柔性微电极的制造方法，属于柔性器件制造技术领域。该方法首先使用基于光诱导电化学方法沉积制造微电极，再将电极转移至PDMS柔性基底。本发明利用聚二甲基硅氧烷(PDMS)的粘附力，通过恒温加热，将使用光诱导电化学沉积制造的微电极从氢化非晶硅芯片基底转印至柔性PDMS基底，并使用晶元探针台测试出转印电极的电特性曲线。利用这种柔性微电极制造方法，可以制作出覆盖在柔性基底的微米尺度电极，本发明提出的新型柔性微电极制造方法，未来有望在柔性传感器、可穿戴电子器件等领域获得应用。
The invention discloses a manufacturing method of a flexible micro-electrode, which belongs to the technical field of flexible device manufacturing. This method first uses photo-induced electrochemical deposition to fabricate microelectrodes, and then transfers the electrodes to PDMS flexible substrates. The present invention utilizes the adhesive force of polydimethylsiloxane (PDMS) to transfer microelectrodes fabricated by photo-induced electrochemical deposition from a hydrogenated amorphous silicon chip substrate to a flexible PDMS substrate by heating at a constant temperature, and uses a crystal The element probe station tests the electrical characteristic curve of the transfer electrode. Using this flexible microelectrode manufacturing method, a micrometer-scale electrode covering a flexible substrate can be fabricated. The novel flexible microelectrode manufacturing method proposed by the present invention is expected to be applied in the fields of flexible sensors and wearable electronic devices in the future.
Description
技术领域technical field
本发明涉及柔性器件制造技术领域，具体涉及一种柔性微电极的制造方法。The invention relates to the technical field of flexible device manufacturing, in particular to a manufacturing method of a flexible micro-electrode.
背景技术Background technique
科技的发展给人们带来更便携的生活方式，科技产品朝着小型化、移动化及可折叠方向发展，电子产品由笨重的台式电脑发展为轻便的笔记本电脑，再到目前的智能手机，电子产品集成度越来越高、使用也更加便捷。柔性电子器件就是根据科技产品未来的发展趋势之一，柔性器件的优势在于其聚合物基底，有着良好的物理和化学性能，相对于硅基底或石英基具有优秀的生物兼容性、电绝缘性、光透性和热隔离性，因此被应用在光学、电子、生物、化学和医疗等领域，如OLED(有机发光二极管)、传感器、生物芯片、聚合物MEMS等。The development of science and technology has brought people a more portable way of life. Technology products are developing in the direction of miniaturization, mobility and foldability. Electronic products have developed from bulky desktop computers to light notebook computers, and then to the current smart phones, electronic products. Product integration is getting higher and higher, and the use is more convenient. Flexible electronic devices are one of the future development trends of scientific and technological products. The advantage of flexible devices lies in their polymer substrates, which have good physical and chemical properties. Compared with silicon substrates or quartz substrates, they have excellent biocompatibility, electrical insulation, Light transmittance and thermal isolation are therefore used in optical, electronic, biological, chemical and medical fields, such as OLED (Organic Light Emitting Diode), sensors, biochips, polymer MEMS, etc.
柔性电子学是以将有机或无机电子器件制作在柔性或薄金属基板上，形成具有特定功能和用途的柔性器件为研究对象的一门学科。柔性电子器件(Flexible Electronics)又可以称为印刷电子(Printed Electronics)或聚合物电子(Polymer Electronics)等。柔性电子器件有两方面含义：(1)指基底为柔性材料，使器件具有一定的柔性张力；(2)指电子器件本身是柔性物质，具有弯曲拉伸的特性，如电子纸张、柔性显示技术。Flexible electronics is a discipline in which organic or inorganic electronic devices are fabricated on flexible or thin metal substrates to form flexible devices with specific functions and uses. Flexible electronics can also be called printed electronics or polymer electronics. Flexible electronic devices have two meanings: (1) refers to the substrate is a flexible material, so that the device has a certain flexible tension; (2) refers to the electronic device itself is a flexible material, with the characteristics of bending and stretching, such as electronic paper, flexible display technology .
柔性衬底的概念既可以指在柔性基底上通过沉积、光刻、转移等工艺制作器件结构，该器件可以是柔性也可以是刚性结构，也可以指把柔性衬底本身制作成功能层来充当器件，利用衬底本身良好的性能。常用的柔性材料有聚二甲基硅氧烷(Polydimethysiloxane,PDMS)、硅胶(Silicone rubber)、聚对苯二甲酸乙二醇酯(Polyethylene terephthalat,PET)聚氨酯-丙烯酸酯(Poly urethaneacrylate,PUA)、聚碳酸酯(Polycarbonate,PC)和SU-8胶等。The concept of flexible substrate can either refer to the fabrication of device structures on flexible substrates through processes such as deposition, lithography, and transfer. device, using the good performance of the substrate itself. Commonly used flexible materials are polydimethylsiloxane (Polydimethysiloxane, PDMS), silicone (Silicone rubber), polyethylene terephthalate (Polyethylene terephthalate, PET) polyurethane-acrylate (Poly urethaneacrylate, PUA), Polycarbonate (Polycarbonate, PC) and SU-8 glue, etc.
目前制造柔性微纳电子器件的主要加工方法有两种分类：(1)传统的聚合物微加工工艺，它包括光刻、三束(电子束、离子束和激光束)加工、微机械加工、薄膜沉积等技术；(2)非传统的聚合物加工技术一般是基于化学和材料的发展而形成的，如：转移印刷、纳米压印、、自组装、表面能转印等技术。There are currently two main processing methods for fabricating flexible micro-nano electronic devices: (1) traditional polymer micromachining processes, which include photolithography, three-beam (electron beam, ion beam and laser beam) processing, micromachining, (2) Non-traditional polymer processing technologies are generally formed based on the development of chemistry and materials, such as: transfer printing, nanoimprinting, self-assembly, surface energy transfer and other technologies.
传统加工方法如光刻、粒子束技术，是在光刻胶或掩膜板下，对硅基底进行刻蚀，但掩膜板的制造不仅昂贵而且技术复杂，给批量化生产带来很大的困难。针对柔性器件的制造，应用最为广泛和数量最多的技术为纳米压印和转印技术。纳米压印具有工艺灵活、加工快捷和成本低廉等优点，但面对工业生产的大批量需求，纳米压印的速度还远远达不到要求。Traditional processing methods, such as photolithography and particle beam technology, etch the silicon substrate under the photoresist or mask. difficulty. For the manufacture of flexible devices, the most widely used and most numerous technologies are nano-imprinting and transfer technology. Nano-imprinting has the advantages of flexible process, fast processing and low cost. However, in the face of the large-scale demand of industrial production, the speed of nano-imprinting is far from meeting the requirements.
发明内容SUMMARY OF THE INVENTION
针对现有技术中柔性器件制造方法的不足之处，本申请的目的在于提供一种柔性微电极的制造方法，该方法首先基于光诱导电化学沉积技术制造微电极，再将微电极转印至柔性PDMS柔性基底。In view of the deficiencies of the flexible device manufacturing methods in the prior art, the purpose of the present application is to provide a flexible microelectrode manufacturing method. Flexible PDMS flexible substrate.
为实现上述目的，本发明所采用的技术方案如下：For achieving the above object, the technical scheme adopted in the present invention is as follows:
一种柔性微电极的制造方法，该方法首先利用光诱导电化学沉积技术在氢化非晶硅芯片上沉积出任意形状的微电极，然后将芯片上的微电极转印至柔性PDMS基底，即获得所述柔性微电极。A manufacturing method of a flexible microelectrode, the method first uses a photo-induced electrochemical deposition technology to deposit a microelectrode of any shape on a hydrogenated amorphous silicon chip, and then transfers the microelectrode on the chip to a flexible PDMS substrate, that is, to obtain the flexible microelectrodes.
所述将芯片上的微电极转印至柔性PDMS基底的过程具体包括如下步骤：The process of transferring the microelectrodes on the chip to the flexible PDMS substrate specifically includes the following steps:
(1)在氢化非晶硅芯片上制备PDMS薄膜；(1) Preparation of PDMS thin films on hydrogenated amorphous silicon chips;
(2)对芯片上的PDMS薄膜施加压力，使PDMS薄膜与微电极充分接触；(2) Apply pressure to the PDMS film on the chip to make the PDMS film fully contact with the microelectrode;
(3)分离PDMS薄膜与氢化非晶硅芯片，得到表面具有微电极的PDMS薄膜，即所述柔性微电极。(3) Separating the PDMS film and the hydrogenated amorphous silicon chip to obtain a PDMS film with microelectrodes on the surface, namely the flexible microelectrodes.
上述步骤(1)中，在氢化非晶硅芯片上制备PDMS薄膜的过程为：首先配置PDMS旋涂液，将PDMS旋涂液旋涂于氢化非晶硅芯片上；然后将芯片放入恒温干燥箱中，在75℃条件下放置4小时以上，芯片上的PDMS旋涂液固化为PDMS薄膜。In the above step (1), the process of preparing the PDMS thin film on the hydrogenated amorphous silicon chip is as follows: firstly configure the PDMS spin coating liquid, spin the PDMS spin coating liquid on the hydrogenated amorphous silicon chip; then put the chip into a constant temperature drying The PDMS spin coating solution on the chip is cured into a PDMS film after being placed in a box at 75°C for more than 4 hours.
所述PDMS旋涂液是由PDMS预聚体和对应固化剂组成的混合液。The PDMS spin coating liquid is a mixed liquid composed of PDMS prepolymer and corresponding curing agent.
上述步骤(3)中，采用机械剥离方法将PDMS薄膜与芯片分开。In the above step (3), a mechanical peeling method is used to separate the PDMS film from the chip.
上述步骤(3)之后，使用晶元探针台测试制备好的柔性微电极的电特性曲线。After the above step (3), use the wafer probe station to test the electrical characteristic curve of the prepared flexible microelectrode.
使用晶元探针台测量得到转印后微电极的U-I曲线，从而得到转印后微电极的电阻。The U-I curve of the microelectrode after transfer was obtained by using the wafer probe station to measure the resistance of the microelectrode after transfer.
本发明的优点与有益效果为：The advantages and beneficial effects of the present invention are:
1.本发明实现了无模板化的图形柔性微电极制造，微电极的制造是基于光诱导电化学沉积方法得到，可根据调节交流电信号参数控制沉积电极的形状和高度。1. The present invention realizes the manufacture of patterned flexible micro-electrodes without template. The manufacture of micro-electrodes is based on the photo-induced electrochemical deposition method, and the shape and height of the deposition electrodes can be controlled according to the adjustment of AC signal parameters.
2.本发明区别于传统的柔性器件的制造方法，提出了一种高效，快捷的增材制造方法。2. The present invention is different from the traditional flexible device manufacturing method, and proposes an efficient and fast additive manufacturing method.
3.实验装置相对于传统的微纳制造方法的实验设备要更加低廉，并且光敏材料加工均匀，整个芯片表面都可以沉积微电极。3. Compared with the experimental equipment of the traditional micro-nano manufacturing method, the experimental device is cheaper, and the photosensitive material is processed uniformly, and the micro-electrodes can be deposited on the entire chip surface.
4.柔性基底为PDMS，具有光学透性和良好的生物兼容性。可应用于透明电子器件和人体皮肤传感器的制造。4. The flexible substrate is PDMS, which has optical transparency and good biocompatibility. It can be applied to the manufacture of transparent electronic devices and human skin sensors.
5.转印至柔性基底的微电极具有良好的电学特性，为未来制作柔性微纳传感器打下良好的基础。5. The microelectrodes transferred to the flexible substrate have good electrical properties, which lays a good foundation for the fabrication of flexible micro/nano sensors in the future.
附图说明：Description of drawings:
图1为光诱导电化学沉积***示意图。Figure 1 is a schematic diagram of a photo-induced electrochemical deposition system.
图2为柔性微电极转印过程(A为示意图，B为实物图)。Figure 2 shows the flexible microelectrode transfer process (A is a schematic diagram, B is a physical image).
图3为转印后的微电极显微镜下图形(A为银电极，B为金电极)。Figure 3 is the micro-electrode micrograph after transfer (A is silver electrode, B is gold electrode).
图4为转印电极通过晶元探针台测量得到的UI曲线。Figure 4 shows the UI curve of the transfer electrode measured by the wafer probe station.
具体实施方式：Detailed ways:
以下结合实施例详述本发明。The present invention will be described in detail below in conjunction with the examples.
本发明为柔性微电极的制造方法，具体是使用基于光诱导电化学方法沉积制造微电极，再将电极转移至PDMS柔性基底。具体过程为：使用光诱导电化学沉积技术在氢化非晶硅基底沉积出设计形状的微电极，再将配置好的PDMS混合液滴到氢化非晶硅基底上，使用匀胶机将PDMS旋涂均匀，再将覆盖有PDMS的芯片放置于75℃的恒温干燥箱中4小时以上，之后将芯片从干燥箱中取出。对固化后的PDMS施加一定压力，最后将固化的PDMS与氢化非晶硅芯片分离，得到柔性PDMS基底的微电极(如图2)。使用晶元探针台对柔性基底电极进行电特性测量，得到稳定电学性质结果，证明了借助光诱导沉积技术和柔性转印技术可以实现柔性微电极的制造。The present invention is a manufacturing method of a flexible micro-electrode, specifically, using a photo-induced electrochemical method to deposit and manufacture a micro-electrode, and then transferring the electrode to a PDMS flexible substrate. The specific process is: use photo-induced electrochemical deposition technology to deposit microelectrodes of designed shape on the hydrogenated amorphous silicon substrate, then drop the prepared PDMS mixture on the hydrogenated amorphous silicon substrate, and use a spin coater to spin the PDMS. uniform, and then place the chip covered with PDMS in a constant temperature drying oven at 75°C for more than 4 hours, and then take the chip out of the drying oven. A certain pressure is applied to the cured PDMS, and finally the cured PDMS is separated from the hydrogenated amorphous silicon chip to obtain a flexible PDMS-based microelectrode (as shown in Figure 2). Using the wafer probe station to measure the electrical properties of the flexible substrate electrode, the results of stable electrical properties are obtained, which proves that the fabrication of flexible microelectrodes can be realized with the help of light-induced deposition technology and flexible transfer printing technology.
光诱导电化学沉积***如图1所示，采用该***在氢化非晶硅基底沉积微电极的过程为：将硝酸银(AgNO3)溶液通过毛细力注入到光诱导芯片中，在芯片两极施加交流电信号，并使用投影仪照射芯片，使得银离子在非均匀电场中得到电子沉积到氢化非晶硅基底，将光诱导芯片分离。The photo-induced electrochemical deposition system is shown in Figure 1. The process of depositing microelectrodes on hydrogenated amorphous silicon substrates using this system is as follows: inject silver nitrate (AgNO 3 ) solution into the photo-induced chip through capillary force, and apply a An alternating current signal is applied, and a projector is used to illuminate the chip, so that silver ions are electron-deposited on the hydrogenated amorphous silicon substrate in a non-uniform electric field, and the light-induced chip is separated.
使用晶元探针台对柔性基底电极进行电特性测量的过程为：将转印后的微电极放在晶元探针台上，使用两个探针接触微电极两端，使用半导体分析仪施加阶跃电压，得到电流值，从而得到柔性基底上微电极的U-I曲线。The process of using the wafer probe station to measure the electrical characteristics of the flexible substrate electrode is as follows: place the transferred microelectrode on the wafer probe station, use two probes to contact both ends of the microelectrode, and use a semiconductor analyzer to apply Step voltage, get the current value, thus get the U-I curve of the microelectrode on the flexible substrate.
所述光诱导芯片为“三明治”结构，下层为氢化非晶硅芯片，中间为溶液层，最上面为ITO玻璃，氢化非晶硅芯片为三层结构组成，从上至下依次为：氢化非晶硅层、ITO玻璃层和玻璃层。The light-induced chip has a "sandwich" structure, the lower layer is a hydrogenated amorphous silicon chip, the middle is a solution layer, the top is ITO glass, and the hydrogenated amorphous silicon chip is composed of a three-layer structure, from top to bottom: hydrogenated amorphous silicon chip. Crystalline silicon layer, ITO glass layer and glass layer.
所述硝酸银溶液注入到光诱导芯片，是将硝酸银溶液通过毛细现象的毛细力注入光诱导介电泳芯片内，基于光诱导电化学沉积原理是在光照条件下，氢化非晶硅芯片激发出非均匀电场，在非均匀电场的溶液中银离子得到电子从而沉积到氢化非晶硅表面。The silver nitrate solution is injected into the light-induced chip by injecting the silver nitrate solution into the light-induced dielectrophoresis chip through the capillary force of the capillary phenomenon. Based on the principle of light-induced electrochemical deposition, the hydrogenated amorphous silicon chip is excited under illumination conditions. Non-uniform electric field, in the solution of non-uniform electric field, silver ions get electrons and deposit on the surface of hydrogenated amorphous silicon.
所述的PDMS混合液为Dow Corning公司生产的PDMS硅胶基A剂(Sylgard184silicone elastomer)和固化剂B剂(Sylgard 184elastomer cu-ring agent)。将PDMS的A剂和B剂以质量比为10:1的比例混合，并充分搅拌均匀，静置混合溶液使搅拌产生的气泡上浮消失，残余的小气泡可以使用滴管吹出。The PDMS mixed solution is PDMS silica gel-based agent A (Sylgard 184 silicone elastomer) and curing agent B (Sylgard 184 elastomer cu-ring agent) produced by Dow Corning Company. Mix PDMS agent A and agent B in a mass ratio of 10:1, stir well, and let the mixed solution stand still to make the bubbles generated by stirring float up and disappear, and the remaining small bubbles can be blown out with a dropper.
所述旋涂PDMS是将配比好并完全去除气泡后的PDMS混合溶液滴到通过光诱导电化学沉积银电极的氢化非晶硅芯片上，使用匀胶机旋涂PDMS将微电极完全覆盖。The spin-coating of PDMS is to drop the PDMS mixed solution with a good proportion and complete removal of bubbles onto the hydrogenated amorphous silicon chip by photo-induced electrochemical deposition of silver electrodes, and use a spin coater to spin PDMS to completely cover the micro-electrodes.
实施例1Example 1
1.将含有100mMol/L的硝酸银溶液通过毛细现象注入到光诱导芯片中，将光诱导芯片固定在三维移动平台上，在电脑中绘制设计的电极图形，再调节投影仪光源使之照射到芯片中溶液位置。1. Inject the silver nitrate solution containing 100mMol/L into the light-induced chip through capillary phenomenon, fix the light-induced chip on the three-dimensional mobile platform, draw the designed electrode pattern on the computer, and then adjust the projector light source to illuminate it The position of the solution in the chip.
2.打开电脑中的CCD图像采集程序，调节CCD镜头高度是投影图形清晰，调节三维移动平台，是投影图像在观察范围中心，并对焦氢化非晶硅基底。2. Open the CCD image acquisition program in the computer, adjust the height of the CCD lens so that the projected image is clear, adjust the three-dimensional moving platform so that the projected image is in the center of the observation range, and focus on the hydrogenated amorphous silicon substrate.
3.通过信号发生器对光诱导芯片输入交流电信号，幅值为10Vpp，频率为100KHz的正弦波信号，持续时间为5s～40s，使溶液中的银离子在光照图形区域发生化学还原反应，产生银单质吸附和沉积于氢化非晶硅基底，形成与光照图形相同的金属微电极。3. Input AC signal to the light-induced chip through the signal generator, the amplitude is 10Vpp, the frequency is 100KHz sine wave signal, the duration is 5s ~ 40s, so that the silver ions in the solution undergo chemical reduction reaction in the light pattern area, The silver element is adsorbed and deposited on the hydrogenated amorphous silicon substrate to form the same metal microelectrode as the light pattern.
4.使用Dow Corning公司生产的PDMS硅胶基A剂(Sylgard184siliconeelastomer)和固化剂B剂(Sylgard 184elastomer cu-ring agent)。将PDMS的A剂和B剂以质量比为10:1的比例混合，并充分搅拌均匀，静置混合溶液使搅拌产生的气泡上浮消失，残余的小气泡可以使用滴管吹出。4. Use PDMS silica gel-based agent A (Sylgard 184 silicone elastomer) and curing agent B (Sylgard 184 elastomer cu-ring agent) produced by Dow Corning Company. Mix PDMS agent A and agent B in a mass ratio of 10:1, stir well, and let the mixed solution stand still to make the bubbles generated by stirring float up and disappear, and the remaining small bubbles can be blown out with a dropper.
5.将混合配置好的PDMS溶液滴到氢化非晶硅基底，再使用匀胶机使PDMS旋涂于氢化非晶硅表面，尽量使PDMS的厚度降低，不同位置的厚度相同。5. Drop the mixed and prepared PDMS solution onto the hydrogenated amorphous silicon substrate, and then use a glue spinner to spin the PDMS on the surface of the hydrogenated amorphous silicon to reduce the thickness of the PDMS as much as possible, and the thickness at different positions is the same.
6.将旋涂有PDMS的氢化非晶硅芯片放入恒温干燥箱中，设置干燥箱温度为75℃，保温放置4小时以上，使PDMS完全固化。6. Put the hydrogenated amorphous silicon chip spin-coated with PDMS into a constant temperature drying oven, set the drying oven temperature to 75°C, and keep it for more than 4 hours to completely cure the PDMS.
7.达到预定时间后将芯片从恒温干燥箱中取出，对覆盖在微电极上的固化PDMS施加一定压力，保证两者充分接触，使用金属箔片将PDMS与氢化非晶硅芯片分离。转印后的微电极在显微镜下的图形如图3所示。7. After reaching the predetermined time, take the chip out of the constant temperature drying box, apply a certain pressure to the cured PDMS covered on the microelectrode to ensure that the two are in full contact, and separate the PDMS from the hydrogenated amorphous silicon chip with a metal foil. Figure 3 shows the microscopic image of the transferred microelectrode.
8.将转印至柔性PDMS基底的微电极放在晶元探针台上，使用探针基座固定好探针，将两个探针接触到微电极两端，使用半导体分析仪对转印至柔性基底的微电极施加阶跃电压，幅值为-300mV至300mV，阶跃步长为3mV，测量得到相应的电流值，图4为经由MatLab绘制的U-I曲线。8. Place the microelectrode transferred to the flexible PDMS substrate on the wafer probe station, use the probe base to fix the probe, touch the two probes to both ends of the microelectrode, and use a semiconductor analyzer to analyze the transfer. A step voltage was applied to the microelectrode of the flexible substrate, the amplitude was -300mV to 300mV, and the step size was 3mV, and the corresponding current value was measured. Figure 4 is the U-I curve drawn by MatLab.
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