CN107846785B - Method for preparing flexible transparent circuit - Google Patents
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/107—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by filling grooves in the support with conductive material
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/01—Dielectrics
- H05K2201/0104—Properties and characteristics in general
- H05K2201/0108—Transparent
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- Manufacturing & Machinery (AREA)
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- Parts Printed On Printed Circuit Boards (AREA)
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Abstract
本分案申请涉及柔性透明电路的制备方法。该方法是这样实现的：通过制备电路模板，在电路模板上用柔性透明高分子材料制成带有凹槽电路结构的固化透明载体，在固化透明载体的凹槽中涂布导电材料溶液，待溶剂挥发后，获得了具有高透明度和导电性的电路。本发明导电材料为固态且整个电路都是透明的，电路板导电性和透明性更好。电路可以根据需要进行设计和制备，精度可以达到微米或纳米级别。同时，本发明方法简单，重现性好，制备的电路更加轻便。电路可以多次拉伸、弯折或扭曲。同时电路质轻、具有很好的生物相容性。该方法制备的电路有望应用于智能隐形眼镜，可卷曲的透明电子设备，电子皮肤等众多领域。
This divisional application relates to a preparation method of a flexible transparent circuit. The method is realized as follows: by preparing a circuit template, a cured transparent carrier with a grooved circuit structure is made of a flexible transparent polymer material on the circuit template, a conductive material solution is coated in the groove of the cured transparent carrier, and the After evaporation of the solvent, a circuit with high transparency and conductivity was obtained. The conductive material of the present invention is solid and the entire circuit is transparent, and the circuit board has better conductivity and transparency. Circuits can be designed and fabricated as needed, with precision down to the micron or nanometer scale. At the same time, the method of the invention is simple, the reproducibility is good, and the prepared circuit is more portable. Circuits can be stretched, bent or twisted many times. At the same time, the circuit is light in weight and has good biocompatibility. The circuit prepared by this method is expected to be applied in many fields such as smart contact lenses, rollable transparent electronic devices, electronic skin and so on.
Description
本申请为申请号为2017103567120、申请日为2017年5月19日、发明名称为“一种柔性透明电路的制备方法”的分案申请。This application is a divisional application with an application number of 2017103567120, an application date of May 19, 2017, and the title of the invention as "a method for preparing a flexible transparent circuit".
技术领域technical field
本发明属于电路及电路板领域，具体涉及柔性透明电路的制备方法。The invention belongs to the field of circuits and circuit boards, and particularly relates to a preparation method of a flexible transparent circuit.
背景技术Background technique
随着可穿戴医疗设备和透明电子设备产业迅猛发展，柔性透明电路开始被越来越多的研究人员关注，柔性透明电路材料和方法的突破对以上两个领域都具有重要的意义。目前，只有很少数关于柔性透明电路的报道，其中最为常用的材料是石墨烯。但是关于石墨烯形成的透明电路，具有以下的弱点：With the rapid development of wearable medical devices and transparent electronic device industries, flexible and transparent circuits have begun to attract more and more researchers' attention. Breakthroughs in flexible and transparent circuit materials and methods are of great significance to the above two fields. Currently, there are only a few reports on flexible transparent circuits, of which the most commonly used material is graphene. But regarding the transparent circuit formed by graphene, it has the following weaknesses:
1.石墨烯薄膜容易形成褶皱，尤其是大面积的石墨烯薄膜1. Graphene film is easy to form wrinkles, especially large area graphene film
2.石墨烯薄膜很难进行精确的质量控制，薄膜上容易产生破损2. Graphene film is difficult to control accurately, and the film is prone to breakage
3.石墨烯薄膜很难进行大规模生产3. Graphene films are difficult to mass-produce
4.最好的石墨烯薄膜方块电阻在100欧姆左右，透明度仅达到90％4. The sheet resistance of the best graphene film is around 100 ohms, and the transparency only reaches 90%
最近，有研究者应用表面图案化的方法，用纳米粒子构筑柔性透明电路。但是这种方法工艺复杂，电路控制不精确，电路不能同时获得良好的导电性、透明度和柔韧性，限制其应用。Recently, some researchers have applied the method of surface patterning to construct flexible and transparent circuits with nanoparticles. However, this method is complicated in process and imprecise in circuit control, and the circuit cannot obtain good conductivity, transparency and flexibility at the same time, which limits its application.
中国专利CN101505575A公开了一种基于PDMS生物可兼容性的柔性电路的制备方法，虽然该专利基材PDMS是透明的，但是电路部分液态金属锡铟鎵合金是非透明的，即形成的是基材透明而导电物质不透明的电路。同时，该柔性电路中导电部分是液态金属，导电器件和导线与液态金属接触的地方容易发生液体泄漏，不能随便插拔，否则会导致电路失效。由于柔性电路的导电部分是液态金属，必须在带有孔道的基材上覆盖另外一片片材，使片材和基材共同形成一个完整的封闭孔道，这样导电金属液体才能保持在孔道中不流失，因此对于孔道的密封性要求很高，封闭不好，容易发生液态金属的泄漏，造成短路。Chinese patent CN101505575A discloses a preparation method of a flexible circuit based on PDMS biocompatibility. Although the patented substrate PDMS is transparent, the liquid metal tin-indium-gallium alloy in the circuit part is non-transparent, that is, the substrate is transparent. And conductive material is not transparent circuit. At the same time, the conductive part of the flexible circuit is liquid metal, and liquid leakage is prone to occur where the conductive devices and wires are in contact with the liquid metal. Since the conductive part of the flexible circuit is a liquid metal, another sheet must be covered on the substrate with a channel, so that the sheet and the substrate together form a complete closed channel, so that the conductive metal liquid can be kept in the channel without loss. Therefore, the tightness of the channel is required to be high, and the sealing is not good, which is prone to leakage of liquid metal, resulting in a short circuit.
发明内容SUMMARY OF THE INVENTION
为弥补现有技术空白，本发明提供一种柔性透明电路的制备方法，该方法制备的柔性透明电路不仅基材是透明的，电路导体部分也是透明的，实现了真正意义上的透明电路。该透明电路不仅导电性好，还具有优异的拉伸、弯折、扭曲性能。该透明电路对柔性透明电子设备的开发和可穿戴医疗设备的开发具有重要意义。In order to make up for the blank of the prior art, the present invention provides a method for preparing a flexible transparent circuit. The flexible transparent circuit prepared by the method is not only transparent in the base material, but also transparent in the conductor part of the circuit, thus realizing a true transparent circuit. The transparent circuit not only has good conductivity, but also has excellent stretching, bending and twisting properties. This transparent circuit is of great significance for the development of flexible transparent electronic devices and the development of wearable medical devices.
为实现上述目的，本发明采用如下技术方案。一种柔性透明电路的制备方法，包括如下步骤：In order to achieve the above objects, the present invention adopts the following technical solutions. A preparation method of a flexible transparent circuit, comprising the following steps:
S1、制备电路模板；S1. Prepare a circuit template;
S2、在电路模板上用柔性透明高分子材料制成带有凹槽电路结构的固化透明载体；S2. Use a flexible transparent polymer material to make a solidified transparent carrier with a grooved circuit structure on the circuit template;
S3、在固化透明载体的凹槽中涂布含有导电材料的溶液，待溶剂挥发后，导电材料存在于凹槽电路结构中，形成柔性透明电路清除凹槽外面的导电材料，形成透明柔性电路。S3. Coat the solution containing the conductive material in the groove of the cured transparent carrier. After the solvent evaporates, the conductive material exists in the circuit structure of the groove to form a flexible transparent circuit. Remove the conductive material outside the groove to form a transparent flexible circuit.
步骤S1中所制备的电路模板的形状、大小、电路的长、宽、高可以根据实际需要自由进行设计。电路图案不局限于直线型一种，可以根据需要进行设计，即电路可以是曲线型、折线型、方波型、波形、圆形、椭圆形、环形等各种形状，或者是以上形状的任意组合。电路中每条线路的长、宽、高都是可以根据需要进行变化。电路模板也不局限于平面一种，还可以是曲面的，或者是3D的。The shape, size, length, width and height of the circuit template prepared in step S1 can be freely designed according to actual needs. The circuit pattern is not limited to the straight type, and can be designed according to the needs, that is, the circuit can be in various shapes such as curve type, broken line type, square wave type, waveform, circle, ellipse, ring, etc., or any of the above shapes. combination. The length, width and height of each line in the circuit can be changed as required. The circuit template is not limited to a plane, and can also be curved or 3D.
作为优选，所述步骤S1在硬质光滑材料上通过光刻，加工，热塑，电抛光，3D打印等任一种方法制备出具有突出表面结构的电路，得到电路模板；本发明中突出表面结构指电路图案的高度是高于整体材料平面的，也就是电路模板上电路是凸出来的。本发明中硬质光滑材料可以是硅片、金属、高分子材料中任一种，所述高分子材料可以是热敏性高分子材料，如酚醛树脂，也可以是硬性高分子材料，如聚四氟乙烯。Preferably, in the step S1, a circuit with a protruding surface structure is prepared on a hard and smooth material by any method such as photolithography, machining, thermoplastic, electropolishing, 3D printing, etc., to obtain a circuit template; in the present invention, the protruding surface is The structure means that the height of the circuit pattern is higher than the plane of the overall material, that is, the circuit on the circuit template is protruding. In the present invention, the hard and smooth material can be any one of silicon wafer, metal, and polymer material, and the polymer material can be a heat-sensitive polymer material, such as phenolic resin, or a hard polymer material, such as polytetrafluoroethylene vinyl.
本发明所述步骤S2可以通过两种方式来实现。The step S2 in the present invention can be implemented in two ways.
第一种方式：将组成柔性透明高分子材料的单体混合物或反应物的混合液浇注到电路模板的表面，待透明高分子材料进行固化反应后，将固化的透明材料从电路模板上剥离，得到具有凹槽电路结构的固化透明载体；The first method: pour the monomer mixture or reactant mixture that constitutes the flexible transparent polymer material onto the surface of the circuit template, and after the transparent polymer material undergoes a curing reaction, peel off the cured transparent material from the circuit template, A solidified transparent carrier with a groove circuit structure is obtained;
将柔性透明高分子材料单体混合物如聚二甲基硅氧烷的A液和B液，或反应物的混合液如制备硅水凝胶混合液，制备水凝胶的混合液，将上述混合物或混合液浇注到带有电路的模板上，进行固化反应，柔性透明高分子材料最初是液态，通过反应最终为固态，并能一直保持固态形状。上述柔性透明高分子材料不局限于已列举的几种材料还可以包括如聚乙烯醇水凝胶，壳聚糖水凝胶等材料。电路模板凸出的电路图案，致使固化的柔性透明高分子上具有凹槽型电路图案。有些高分子材料如聚乙烯醇水凝胶在固化前需要去除气泡，最后透明高分子材料以透明固体形式存在。The flexible transparent polymer material monomer mixture, such as the liquid A and liquid B of polydimethylsiloxane, or the mixed liquid of the reactants, such as the mixed liquid for preparing the silicon hydrogel, the mixed liquid for preparing the hydrogel, and the above mixture is mixed. Or the mixed liquid is poured onto a template with a circuit for a curing reaction. The flexible and transparent polymer material is initially liquid, and finally becomes a solid state through the reaction, and can always maintain a solid shape. The above-mentioned flexible and transparent polymer materials are not limited to the listed materials and may also include materials such as polyvinyl alcohol hydrogel, chitosan hydrogel and the like. The protruding circuit pattern of the circuit template causes the cured flexible transparent polymer to have a groove-type circuit pattern. Some polymer materials such as polyvinyl alcohol hydrogel need to remove air bubbles before curing, and finally the transparent polymer material exists in the form of a transparent solid.
第二种方式：应用3D打印技术，直接应用柔性透明高分子材料如PDMS，硅水凝胶，壳聚糖水凝胶等进行3D打印，得到具有凹槽电路结构的固化透明载体。The second way is to use 3D printing technology to directly apply flexible and transparent polymer materials such as PDMS, silicon hydrogel, chitosan hydrogel, etc. for 3D printing to obtain a solidified transparent carrier with a grooved circuit structure.
步骤S3中，首先将导电材料分散于可挥发溶剂中，在固化透明载体的凹槽中涂布含有导电材料的溶液，并将涂于凹槽外的导电材料清理干净。待溶剂挥发后，导电材料均以固体形态存在于凹槽电路结构中，形成柔性透明电路；所述导电材料不局限于银纳米线，铜纳米线，金纳米线，导电水凝胶，碳纳米管，石墨烯，纳米金链或纳米粒子中一种或一种以上。在固化透明载体的凹槽中涂布导电材料，可以采用直接涂布，喷涂，旋涂等任一种涂布形式。In step S3, the conductive material is first dispersed in a volatile solvent, a solution containing the conductive material is coated in the groove of the cured transparent carrier, and the conductive material coated outside the groove is cleaned. After the solvent is volatilized, the conductive material exists in the groove circuit structure in a solid form to form a flexible transparent circuit; the conductive material is not limited to silver nanowires, copper nanowires, gold nanowires, conductive hydrogels, carbon nanowires One or more of tubes, graphene, nano-gold chains or nanoparticles. The conductive material is coated in the groove of the cured transparent carrier, and any coating form such as direct coating, spray coating, and spin coating can be used.
电路形成后，为了保护凹槽内的导电材料，增加导电材料在透明基质上的稳定性和抗氧化性，可增加步骤S4：在柔性透明电路的表面上铺展柔性透明高分子材料。将电路夹心于两种透明材料中央，可以起到保护电路并防止氧化的作用。凹槽内的导电材料之间互相形成连接，导电材料在凹槽内分布均匀，使电路板具有良好的导电性。After the circuit is formed, in order to protect the conductive material in the groove and increase the stability and oxidation resistance of the conductive material on the transparent substrate, step S4 may be added: spreading the flexible transparent polymer material on the surface of the flexible transparent circuit. Sandwiching the circuit in the center of the two transparent materials can protect the circuit and prevent oxidation. The conductive materials in the grooves are connected to each other, and the conductive materials are evenly distributed in the grooves, so that the circuit board has good conductivity.
上述方法中还可以包括步骤S5：将透明柔性电路与外界导通。所述导通是导电材料通过与电子器件或外界电源或能够导电的导线的连接来实现。柔性电路与电子器件或电源的导通，是通过将电子器件的导电部分或导线与柔性透明电路凹槽内的导电物质连接形成回路。电子器件或导线可以预埋或***到柔性透明导电材料内部。The above method may further include step S5: conducting the transparent flexible circuit with the outside world. The conduction is realized by connecting the conductive material with electronic devices or external power sources or conductive wires. The conduction between the flexible circuit and the electronic device or the power source is to form a loop by connecting the conductive part or wire of the electronic device with the conductive substance in the groove of the flexible transparent circuit. Electronic devices or wires can be embedded or inserted into the flexible transparent conductive material.
本发明另一个目的是请求保护一种多层柔性透明电路，按照本发明所述任一种方法制备至少两个柔性透明电路，将其叠加在一起，通过导电材料贯穿，得到多层柔性透明电路。Another object of the present invention is to claim a multi-layer flexible transparent circuit, by preparing at least two flexible transparent circuits according to any method described in the present invention, superimposing them together, and passing through conductive materials to obtain a multi-layer flexible transparent circuit .
与现有技术相比，本发明的有益效果是：Compared with the prior art, the beneficial effects of the present invention are:
本发明形成柔性电路具有高透明度，不仅电路的柔性高分子材料载体是透明的，而且导电材料也是透明的。具有优异的导电性，形成电路的导电物质为干态，底部凹槽无需封闭，导电器件和导线可以随时***或拔出电路，导电物质不会流失而导致电路失效。本发明的柔性透明载体重量轻、均具有生物可兼容性的特点，在柔性透明载体上形成的透明电路可以方便贴附于人或动物的身体表面或植入体内，电路不会受动物或人的行动影响而停止工作。利用柔性基底的柔性，实现电路良好的拉伸、扭曲和弯折性能，***导电器件和导线进行正反180度多次折叠，仍保持优秀的耐弯折，拉伸和扭曲性能。电路根据需要进行设计和制备，精度可以达到微米或纳米级别。The flexible circuit formed by the invention has high transparency, not only the flexible polymer material carrier of the circuit is transparent, but also the conductive material is transparent. It has excellent conductivity, the conductive substance forming the circuit is in a dry state, the bottom groove does not need to be closed, the conductive devices and wires can be inserted or pulled out of the circuit at any time, and the conductive substance will not be lost and cause the circuit to fail. The flexible transparent carrier of the present invention is light in weight and has the characteristics of biocompatibility. The transparent circuit formed on the flexible transparent carrier can be easily attached to the body surface of a human or animal or implanted in the body, and the circuit will not be affected by animals or humans. stop working due to the influence of actions. The flexibility of the flexible substrate is used to achieve good tensile, twisting and bending properties of the circuit, and the conductive devices and wires are inserted to perform multiple folds of 180 degrees front and back, and still maintain excellent resistance to bending, stretching and twisting. Circuits are designed and fabricated as needed, with precision down to the micron or nanometer level.
本发明制备过程简单，重现性好，获得的电路更加轻便。该方法制备电路有望应用于智能隐形眼镜，可卷曲的透明电子设备，电子皮肤等众多领域。The preparation process of the invention is simple, the reproducibility is good, and the obtained circuit is more portable. The circuit prepared by this method is expected to be applied in many fields such as smart contact lenses, rollable transparent electronic devices, electronic skin and so on.
附图说明Description of drawings
本发明附图共四幅：There are four accompanying drawings of the present invention:
图1是柔性透明电路制备流程图；Fig. 1 is the flow chart of flexible transparent circuit preparation;
以带有光刻胶图案的硅片模板作为电路模板，以银纳米线为导电材料，形成具有微结构的柔性透明电路制备方法流程图。A flow chart of a preparation method for forming a flexible transparent circuit with a microstructure by using a silicon wafer template with a photoresist pattern as a circuit template and silver nanowires as a conductive material.
图2是本发明方法制备的导电材料经多次正反弯折后电阻变化曲线；Fig. 2 is the resistance change curve after the conductive material prepared by the method of the present invention is bent repeatedly;
图3是本发明制备的柔性透明电路在亮灯情况下的拉伸图；Fig. 3 is the stretching diagram of the flexible transparent circuit prepared by the present invention under the condition of lighting;
图4是本发明制备的柔性透明电路的亮灯照片。FIG. 4 is a lighting photo of the flexible transparent circuit prepared by the present invention.
具体实施方式Detailed ways
下面结合具体实施例对本发明的技术方案进一步的说明，但本发明不以任何形式受限于实施例内容。实施例中所述实验方法如无特殊说明，均为常规方法，如无特殊说明，所述化学试剂和材料，均可从商业途径获得。下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。本发明所用的乙醇，为优级纯。The technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited to the content of the embodiments in any form. The experimental methods described in the examples are conventional methods unless otherwise specified, and the chemical reagents and materials can be obtained from commercial sources unless otherwise specified. The following non-limiting examples may enable those of ordinary skill in the art to more fully understand the present invention, but do not limit the present invention in any way. The ethanol used in the present invention is excellent grade pure.
实施例1Example 1
本发明所用的银纳米线(AgNWs)乙醇溶液，规格为：直径30nm，长度100～200um，浓度20mg/ml，溶剂为无水乙醇。The silver nanowire (AgNWs) ethanol solution used in the present invention has specifications as follows: diameter 30nm, length 100-200um, concentration 20mg/ml, and the solvent is absolute ethanol.
(一)制备电路模板(1) Preparation of circuit template
利用光刻技术，用SU-2050光刻胶在4英寸的硅片上刻出具有突出表面结构的电路，得到电路模板。Using photolithography technology, SU-2050 photoresist was used to engrave a circuit with a protruding surface structure on a 4-inch silicon wafer to obtain a circuit template.
(二)制备PDMS透明载体(2) Preparation of PDMS transparent carrier
将聚二甲基硅氧烷(Polydimethylsiloxane，PDMS)的A液和B液按照10:1的比例混合均匀，倒入用光刻有电路图形的硅片制成的模板上，放入真空干燥器中将PDMS中的气泡抽干净，用时1小时左右，再放入80℃的烘箱中加热固化1小时，得到带有电路凹槽的固化透明PDMS载体。Mix solution A and solution B of polydimethylsiloxane (PDMS) in a ratio of 10:1, pour it onto a template made of a silicon wafer with photoetched circuit patterns, and place it in a vacuum desiccator The air bubbles in the PDMS were evacuated for about 1 hour, and then placed in an oven at 80° C. for heating and curing for 1 hour to obtain a cured transparent PDMS carrier with circuit grooves.
(三)制备柔性透明电路(3) Preparation of flexible transparent circuits
A.配置AgNWs乙醇溶液0.3mg/ml。A. Prepare AgNWs ethanol solution 0.3mg/ml.
B.吸取AgNWs溶液40uL滴于固化透明PDMS载体表面，并于旋涂加速度300rpm，旋涂转速3000rpm的条件下旋涂40s。B. Drop 40uL of AgNWs solution onto the surface of the cured transparent PDMS carrier, and spin for 40s at a spin coating acceleration of 300rpm and a spin coating speed of 3000rpm.
C.再重复步骤B两次，将AgNWs乙醇溶液涂布于电路板凹槽中，等乙醇溶液完全挥发后，利用3M胶带粘掉凹槽外多余的AgNWs，得到柔性透明电路板，利用手持式四探针电阻仪测其表面电阻，利用紫外分光光度计测其在550nm波长下的透过率。经测试得到电阻为3.21Ω，透过率为92.48％的透明柔性电路。C. Repeat step B two more times to coat the AgNWs ethanol solution in the groove of the circuit board. After the ethanol solution is completely volatilized, use 3M tape to stick off the excess AgNWs outside the groove to obtain a flexible transparent circuit board. The surface resistance was measured by a four-probe resistance meter, and the transmittance at a wavelength of 550 nm was measured by an ultraviolet spectrophotometer. After testing, a transparent flexible circuit with a resistance of 3.21Ω and a transmittance of 92.48% was obtained.
实施例2Example 2
本发明所用的铜纳米线(CuNWs)乙醇溶液，规格为：直径20nm，长度80um，浓度20mg/ml，溶剂为无水乙醇。The copper nanowire (CuNWs) ethanol solution used in the present invention has specifications as follows: diameter 20nm, length 80um, concentration 20mg/ml, and the solvent is absolute ethanol.
(一)制备电路模板(1) Preparation of circuit template
利用光刻技术，用SU-2050光刻胶在4英寸的硅片上刻出所需电路的模板。Using photolithography technology, SU-2050 photoresist is used to engrave the template of the desired circuit on a 4-inch silicon wafer.
(二)制备PDMS透明载体(2) Preparation of PDMS transparent carrier
将聚二甲基硅氧烷(Polydimethylsiloxane，PDMS)的A液和B液按照10:1的比例混合均匀，倒入用光刻有电路图形的硅片制成的模板上，放入真空干燥器中将PDMS中的气泡抽干净，用时1小时，再放入80℃的烘箱中加热固化1小时，得到带有电路凹槽的PDMS透明载体。Mix solution A and solution B of polydimethylsiloxane (PDMS) in a ratio of 10:1, pour it onto a template made of a silicon wafer with photoetched circuit patterns, and place it in a vacuum desiccator The air bubbles in the PDMS were evacuated for 1 hour, and then placed in an oven at 80° C. for heating and curing for 1 hour to obtain a PDMS transparent carrier with circuit grooves.
(三)制备柔性透明电路(3) Preparation of flexible transparent circuits
A.配置CuNWs乙醇溶液0.4mg/ml。A. Prepare CuNWs ethanol solution 0.4mg/ml.
B.吸取CuNWs溶液60uL滴于PDMS透明载体表面，并于旋涂加速度300rpm，旋涂转速3000rpm的条件下旋涂40s。B. Pipette 60uL of CuNWs solution onto the surface of the PDMS transparent carrier, and spin for 40s at a spin coating acceleration of 300rpm and a spin coating speed of 3000rpm.
C.再重复B中步骤两次，等乙醇溶液完全挥发后，利用3M胶带粘掉凹槽内CuNWs，得到透明柔性电路板，利用手持式四探针电阻仪测其表面电阻，利用紫外分光光度计测其在550nm波长下的透过率。经测试得到电阻为5.62Ω，透过率为93.17％的透明柔性电路。C. Repeat step B twice again. After the ethanol solution is completely volatilized, use 3M tape to stick the CuNWs in the groove to obtain a transparent flexible circuit board. Use a handheld four-probe resistance meter to measure its surface resistance, and use ultraviolet The transmittance at a wavelength of 550 nm was measured. After testing, a transparent flexible circuit with a resistance of 5.62Ω and a transmittance of 93.17% was obtained.
实施例3Example 3
本发明所用的金纳米线(AuNWs)乙醇溶液，规格为：直径3nm，长度50um，浓度20mg/ml，溶剂为无水乙醇。The ethanol solution of gold nanowires (AuNWs) used in the present invention has specifications as follows: diameter 3nm, length 50um, concentration 20mg/ml, and the solvent is absolute ethanol.
(一)制备电路模板(1) Preparation of circuit template
利用光刻技术，用SU-2050光刻胶在4英寸的硅片上刻出所需电路的模板。Using photolithography technology, SU-2050 photoresist is used to engrave the template of the desired circuit on a 4-inch silicon wafer.
(二)制备PDMS透明载体(2) Preparation of PDMS transparent carrier
将聚二甲基硅氧烷(Polydimethylsiloxane，PDMS)的A液和B液按照10:1的比例混合均匀，倒入用光刻有电路图形的硅片制成的模具上，放入真空干燥器中将PDMS中的气泡抽干净，大概用时1小时，再放入80℃的烘箱中加热固化1小时，得到带有电路凹槽的PDMS透明载体。Mix solution A and solution B of polydimethylsiloxane (PDMS) in a ratio of 10:1, pour it into a mold made of a silicon wafer with photoetched circuit patterns, and put it into a vacuum desiccator The air bubbles in the PDMS were evacuated for about 1 hour, and then placed in an oven at 80° C. for heating and curing for 1 hour to obtain a PDMS transparent carrier with circuit grooves.
(三)制备柔性透明电路(3) Preparation of flexible transparent circuits
A.配置AuNWs乙醇溶液0.5mg/ml。A. Prepare AuNWs ethanol solution 0.5mg/ml.
B.吸取AuNWs溶液30uL滴于透明硅水凝胶芯片的凹槽里，等乙醇溶液挥发后，再继续涂两次。B. Draw 30uL of AuNWs solution and drop it into the groove of the transparent silicon hydrogel chip. After the ethanol solution evaporates, continue to apply it twice.
C.等乙醇溶液完全挥发后，利用3M胶带粘掉凹槽外的AuNWs，得到透明柔性电路板，利用手持式四探针电阻仪测其表面电阻，利用紫外分光光度计测其在550nm波长下的透过率。经测试得到电阻为2.38Ω，透过率为95.02％的透明柔性电路。C. After the ethanol solution is completely volatilized, use 3M tape to stick the AuNWs outside the groove to obtain a transparent flexible circuit board. Use a handheld four-probe resistance meter to measure its surface resistance, and use an ultraviolet spectrophotometer to measure its surface resistance at 550nm wavelength. transmittance. A transparent flexible circuit with a resistance of 2.38Ω and a transmittance of 95.02% was obtained after testing.
实施例4Example 4
本发明所用的金纳米线(AuNWs)乙醇溶液，规格为：直径3nm，长度50um，浓度20mg/ml，溶剂为无水乙醇；The gold nanowire (AuNWs) ethanol solution used in the present invention has the specifications: diameter 3nm, length 50um, concentration 20mg/ml, and the solvent is absolute ethanol;
(一)制备电路模板(1) Preparation of circuit template
利用铝合金金属加工技术，在铝合金上打磨出所需电路的具有突出表面结构的电路模板。Using aluminum alloy metal processing technology, a circuit template with a prominent surface structure of the desired circuit is polished on the aluminum alloy.
(二)制备硅水凝胶柔性透明载体(2) Preparation of silicone hydrogel flexible transparent carrier
将引发剂偶氮二异丁腈(用量为总剂量的0.2wt％)和交联剂N,N-亚甲基双丙烯酸酰胺(用量为总剂量的1.0wt％)完全溶解于8:1:1质量比的甲基丙烯酸羟乙酯，N-乙烯基吡咯烷酮和γ-(甲基丙烯酰氧)丙基三甲氧基硅烷混合溶液中，磁力搅拌30分钟，均匀混合各物质并过滤后，倒入铝合金模板上，放入90℃真空烘箱中反应2小时，固化后脱模，得到带有电路凹槽的硅水凝胶柔性透明载体。The initiator azobisisobutyronitrile (the dosage is 0.2wt% of the total dosage) and the cross-linking agent N,N-methylenebisacrylamide (the dosage is 1.0wt% of the total dosage) are completely dissolved in 8:1: 1 mass ratio of hydroxyethyl methacrylate, N-vinylpyrrolidone and γ-(methacryloyloxy)propyltrimethoxysilane mixed solution, magnetically stirred for 30 minutes, uniformly mixed each material and filtered, poured Put it on an aluminum alloy template, put it into a 90° C. vacuum oven to react for 2 hours, and demold it after curing to obtain a silicone hydrogel flexible transparent carrier with circuit grooves.
(三)制备柔性透明电路(3) Preparation of flexible transparent circuits
A.配置金纳米线乙醇溶液0.5mg/ml。A. Prepare gold nanowire ethanol solution 0.5mg/ml.
B.吸取金纳米线溶液30uL滴于透明硅水凝胶芯片的凹槽里，等乙醇溶液挥发后，再继续涂两次。B. Draw 30uL of the gold nanowire solution and drop it into the groove of the transparent silicon hydrogel chip. After the ethanol solution evaporates, continue to apply it twice.
C.等乙醇溶液完全挥发后，利用3M胶带粘掉孔道外的金纳米线，得到透明柔性电路板，利用手持式四探针电阻仪测其表面电阻，利用紫外分光光度计测其在550nm波长下的透过率。经测试得到电阻为4.52Ω，透过率为94.36％的透明柔性电路。C. After the ethanol solution is completely volatilized, use 3M tape to stick the gold nanowires outside the channel to obtain a transparent flexible circuit board. Use a handheld four-probe resistance meter to measure its surface resistance, and use an ultraviolet spectrophotometer to measure its wavelength at 550nm. lower transmittance. After testing, a transparent flexible circuit with a resistance of 4.52Ω and a transmittance of 94.36% was obtained.
实施例5Example 5
本发明所用的碳纳米管(CNTs)为羟基化的单壁长纳米管，规格为：直径1.1nm，长度50um，溶剂为乙醇溶液。The carbon nanotubes (CNTs) used in the present invention are hydroxylated single-walled long nanotubes, the specifications are: diameter 1.1 nm, length 50um, and the solvent is ethanol solution.
(一)制备电路模板(1) Preparation of circuit template
利用打磨技术，在聚四氟乙烯上打磨出所需电路。Using the sanding technique, sand out the desired circuit on the Teflon.
(二)制备聚乙烯醇(PVA)水凝胶透明载体(2) Preparation of polyvinyl alcohol (PVA) hydrogel transparent carrier
称取5克聚合度为1750±50的PVA样品，以蒸馏水为溶剂配置1g/mL的PVA水溶液。将配置好的PVA水溶液置于磨口烧瓶中，用恒温水浴加热至90℃，搅拌至完全溶解。在60℃静置30分钟，除去溶液中的气泡。然后倒入到聚四氟乙烯的电路模板上，在-20℃冰箱中进行极速冷却。15个小时后取出在室温中解冻6小时。解冻后继续放入-20℃冰箱中进行极速冷却。15个小时后取出在室温中解冻6小时。重复冷冻-解冻循环10次。得到硬度较高并具有凹槽电路结构的聚乙烯醇(PVA)水凝胶透明载体。Weigh 5 grams of PVA samples with a degree of polymerization of 1750 ± 50, and use distilled water as a solvent to prepare a 1 g/mL PVA aqueous solution. The prepared PVA aqueous solution was placed in a grinding-mouth flask, heated to 90°C with a constant temperature water bath, and stirred until completely dissolved. Let stand at 60°C for 30 minutes to remove air bubbles in the solution. It is then poured onto a PTFE circuit template and cooled rapidly in a -20°C freezer. After 15 hours, take out and thaw at room temperature for 6 hours. After thawing, continue to place in -20 ℃ refrigerator for rapid cooling. After 15 hours, take out and thaw at room temperature for 6 hours. Repeat freeze-
(三)制备柔性透明电路(3) Preparation of flexible transparent circuits
A.配置CNTs的乙醇溶液0.5mg/ml。A. Prepare 0.5mg/ml ethanol solution of CNTs.
B.吸取CNTs的乙醇溶液30uL滴于聚乙烯醇水凝胶透明载体的凹槽里，等乙醇溶液挥发后，再继续涂两次。B. Draw 30uL of the ethanol solution of CNTs and drop it into the groove of the transparent carrier of the polyvinyl alcohol hydrogel. After the ethanol solution volatilizes, continue to apply it twice.
C.等乙醇溶液完全挥发后，利用3M胶带粘掉凹槽外的多余的CNTs，得到透明柔性电路板，利用手持式四探针电阻仪测其表面电阻，利用紫外分光光度计测其在550nm波长下的透过率。经测试得到电阻为24.52Ω，透过率为80.36％的透明柔性电路。C. After the ethanol solution is completely volatilized, use 3M tape to stick off the excess CNTs outside the groove to obtain a transparent flexible circuit board. Use a handheld four-probe resistance meter to measure its surface resistance, and use an ultraviolet spectrophotometer to measure its surface resistance at 550nm. transmittance at wavelengths. After testing, a transparent flexible circuit with a resistance of 24.52Ω and a transmittance of 80.36% was obtained.
实施例6Example 6
本发明所用的金纳米链，规格为：直径5nm，长度90um，浓度0.5mg/ml，溶剂为乙醇溶液。The gold nano-chain used in the present invention has specifications as follows: a diameter of 5 nm, a length of 90 um, a concentration of 0.5 mg/ml, and an ethanol solution as a solvent.
(一)制备电路模板(1) Preparation of circuit template
利用热塑技术，在酚醛树脂上制得具有突出表面结构的电路。Using thermoplastic technology, circuits with prominent surface structures were fabricated on phenolic resins.
(二)制备壳聚糖水凝胶透明载体(2) Preparation of chitosan hydrogel transparent carrier
称取1.2克壳聚糖于洁净的烧杯中，加入40mL 2％的醋酸溶液，搅拌溶解；加入16mL 3％戊二醛，搅拌，55℃恒温1h得黄色透明壳聚糖水凝胶溶液；将溶液倒入带有电路的酚醛塑料的模板上，室温下放置48小时。得到黄色透明的壳聚糖水凝胶载体。Weigh 1.2 grams of chitosan into a clean beaker, add 40 mL of 2% acetic acid solution, stir to dissolve; add 16 mL of 3% glutaraldehyde, stir, and keep the temperature at 55 °C for 1 h to obtain a yellow transparent chitosan hydrogel solution; Pour onto a phenolic stencil with circuits and let stand at room temperature for 48 hours. A yellow transparent chitosan hydrogel carrier was obtained.
(三)制备柔性透明电路(3) Preparation of flexible transparent circuits
A.配置金纳米链乙醇溶液1mg/ml。A. Prepare gold nanochain ethanol solution 1mg/ml.
B.吸取金纳米链溶液30uL滴于透明硅水凝胶芯片的凹槽里，等乙醇溶液挥发后，再继续涂两次。B. Draw 30uL of the gold nanochain solution and drop it into the groove of the transparent silicon hydrogel chip. After the ethanol solution evaporates, continue to apply it twice.
C.等乙醇溶液完全挥发后，利用3M胶带粘掉凹槽外多余的金纳米链，得到透明柔性电路板，利用手持式四探针电阻仪测其表面电阻，利用紫外分光光度计测其在550nm波长下的透过率。经测试得到电阻为7.52Ω，透过率为93.21％的透明柔性电路。C. After the ethanol solution is completely volatilized, use 3M tape to stick off the excess gold nano-chains outside the groove to obtain a transparent flexible circuit board. Use a handheld four-probe resistance meter to measure its surface resistance, and use an ultraviolet spectrophotometer to measure its surface resistance. Transmittance at 550nm wavelength. After testing, a transparent flexible circuit with a resistance of 7.52Ω and a transmittance of 93.21% was obtained.
对本发明制备的柔性透明电路进行性能测试。The performance test of the flexible transparent circuit prepared by the present invention is carried out.
如图2所示以PDMS为透明高分子材料，以银纳米线为导电材料，形成的具有直线型电路的材料的弯折实验数据。该电路进行了正反180度的弯折，随着弯折度数的增加，正反弯折后电路的电阻基本不变。经电路可以进行2500次的正反弯折，弯折后电阻略有增加，但是增加的量很小。Figure 2 shows the bending experimental data of a material with a linear circuit formed by using PDMS as a transparent polymer material and silver nanowires as a conductive material. The circuit is bent forward and reverse 180 degrees. With the increase of the bending degree, the resistance of the circuit after the forward and reverse bending is basically unchanged. 2500 times of forward and reverse bending can be performed by the circuit, and the resistance increases slightly after bending, but the increase is very small.
如图3所示以PDMS为透明高分子材料，以银纳米线为导电材料，形成的具有直线型电路的拉伸实验。LED灯亮说明电路的通畅性，LED灯在没有拉伸和拉伸伸长了近35％时，灯的亮度基本没有改变，说明该电路的可拉伸性能良好。As shown in Figure 3, a tensile experiment with a linear circuit formed by using PDMS as a transparent polymer material and silver nanowires as a conductive material. When the LED light is on, it indicates the smoothness of the circuit. When the LED light is not stretched and stretched by nearly 35%, the brightness of the light does not change basically, indicating that the stretchability of the circuit is good.
如图4所示以PDMS为透明柔性材料的复杂电路板，在中心圆形线路中***LED灯，线路的宽度是200微米。说明本发明方法可以制备微米级别的柔性透明电路。As shown in Figure 4, a complex circuit board with PDMS as a transparent flexible material is inserted into a central circular circuit with an LED light, and the width of the circuit is 200 microns. It is illustrated that the method of the present invention can prepare micron-scale flexible transparent circuits.
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