技术领域technical field
本发明涉及柔性应力传感器领域，具体涉及一种基于包芯纱-石墨烯网膜的应力传感器的制备方法。The invention relates to the field of flexible stress sensors, in particular to a method for preparing a stress sensor based on a core-spun yarn-graphene mesh.
背景技术Background technique
随着人工智能的高速发展和智能终端的普及，可穿戴电子设备呈现出巨大的市场前景。柔性应力传感器作为人造柔性电子器件的核心部分，在人体临床诊断、健康评估、健康监控、虚拟电子、柔性触摸屏、柔性电子皮肤,甚至工业机器人等领域拥有很大的应用潜力。With the rapid development of artificial intelligence and the popularization of smart terminals, wearable electronic devices present a huge market prospect. As the core part of artificial flexible electronic devices, flexible stress sensors have great application potential in the fields of human clinical diagnosis, health assessment, health monitoring, virtual electronics, flexible touch screen, flexible electronic skin, and even industrial robots.
目前，制造应变传感器的主流方式是将传感器的形变转变为电阻值的变化，即压电阻型应力传感器。其中一种较为常用的制备方法是在柔性基底表面嵌入或覆盖一层导电材料，得到多层结构的应变传感器。导电材料可以是金属膜或导电纳米材料通过各种工艺组装得到导电薄膜。石墨烯是目前世界上最薄且最硬的纳米材料，其电阻率极低，电子迁移速度极快。独特的二维结构和优异的导电性使石墨烯在应力传感领域表现出极大的应用前景。At present, the mainstream way to manufacture strain sensors is to convert the deformation of the sensor into the change of resistance value, that is, the piezoresistive stress sensor. One of the more commonly used preparation methods is to embed or cover a layer of conductive material on the surface of a flexible substrate to obtain a strain sensor with a multilayer structure. The conductive material can be a metal film or a conductive nano-material assembled to obtain a conductive film through various processes. Graphene is currently the thinnest and hardest nanomaterial in the world, with extremely low resistivity and extremely fast electron migration. The unique two-dimensional structure and excellent electrical conductivity make graphene show great application prospects in the field of stress sensing.
传统的基底材料为表面平整的弹性薄膜，如聚甲基乙烯基硅氧烷(PDMS)、Ecoflex、Dragon skin、橡胶等，其表面嵌入或覆盖的导电层也为平面结构。这种平面结构的传感器普遍存在灵敏度不够高，难以检测微小形变的缺点，限制了其发展和应用。因此，迫切需要一种高灵敏度，同时制备工艺简便的新型应力传感器。The traditional base material is an elastic film with a flat surface, such as polymethyl vinyl siloxane (PDMS), Ecoflex, Dragon skin, rubber, etc., and the conductive layer embedded or covered on the surface is also a planar structure. Sensors with this planar structure generally have the disadvantages of insufficient sensitivity and difficulty in detecting small deformations, which limits their development and application. Therefore, there is an urgent need for a new type of stress sensor with high sensitivity and simple fabrication process.
发明内容Contents of the invention
本发明的目的为针对当前技术存在的不足，提供一种新型高性能柔性应力传感器。该传感器使用复合网膜来替代传统的平面结构材料作为导电层，通过将二维层状还原石墨烯(RGO)包覆于包芯纱表面，得到导电的复合网膜。本发明极大提升了传感器的灵敏度，降低了检测限。The purpose of the present invention is to provide a novel high-performance flexible stress sensor for the deficiencies in the current technology. The sensor uses a composite mesh to replace the traditional planar structure material as the conductive layer, and a conductive composite mesh is obtained by coating the surface of the core-spun yarn with two-dimensional layered reduced graphene (RGO). The invention greatly improves the sensitivity of the sensor and reduces the detection limit.
本发明的技术方案为：Technical scheme of the present invention is:
一种柔性应力传感器，包括两个传感组件；每个传感组件包括PDMS粘性基底层和包芯纱-石墨烯复合网膜导电层，所述的基底层是由PDMS预聚物旋涂或滴涂，固化后成膜而得；所述的包芯纱-石墨烯复合网膜导电层是由石墨烯分散液组装于所述包芯纱骨架而得；两个传感组件贴合，其中，包芯纱-石墨烯复合网膜导电层一侧贴合，位于中间，柔性应力传感器形成“三明治”结构；每个传感器组件的包芯纱-石墨烯复合网膜导电层均连接一根导线。A flexible stress sensor comprising two sensing components; each sensing component comprises a PDMS adhesive base layer and a core-spun yarn-graphene composite mesh conductive layer, and the base layer is spin-coated by PDMS prepolymer or It is drip-coated and formed into a film after curing; the conductive layer of the core-spun yarn-graphene composite mesh is obtained by assembling the graphene dispersion on the core-spun yarn skeleton; the two sensing components are bonded together, wherein , one side of the conductive layer of the core-spun yarn-graphene composite mesh is laminated, located in the middle, and the flexible stress sensor forms a "sandwich" structure; the conductive layer of the core-spun yarn-graphene composite mesh of each sensor component is connected to a wire .
所述的包芯纱骨架为直径为10μm-30μm的纱线，纱线为氨纶或锦纶中的一种或两种。The skeleton of the core-spun yarn is a yarn with a diameter of 10 μm-30 μm, and the yarn is one or both of spandex or nylon.
所述的PDMS粘性基底层的厚度为200μm-500μm。The thickness of the PDMS adhesive base layer is 200 μm-500 μm.
所述的导线为铜线或铜箔，所述的导线通过导电胶与石墨烯导电层连接。The wires are copper wires or copper foils, and the wires are connected to the graphene conductive layer through conductive glue.
所述的导电胶采用导电银浆或导电碳浆。The conductive glue adopts conductive silver paste or conductive carbon paste.
所述的导线连接电化学测试设备，电化学测试设备包括电化学分析仪和数字万用表。The wires are connected to electrochemical test equipment, and the electrochemical test equipment includes an electrochemical analyzer and a digital multimeter.
所述的PDMS预聚物为市售牌号为道康宁Sylgard 184双组分套件硅橡胶的组分A和组分B，质量比组分A：组分B＝10-15:1。The PDMS prepolymer is a commercially available brand of Dow Corning Sylgard 184 two-component silicone rubber component A and component B, the mass ratio of component A: component B = 10-15:1.
所述的柔性应力传感器的制备方法，包括如下步骤：The preparation method of described flexible stress sensor, comprises the steps:
(1)制备浓度为0.01-0.4mg/mL的石墨烯分散液；(1) preparation concentration is the graphene dispersion liquid of 0.01-0.4mg/mL;
(2)配置PDMS溶液，将组分A与组分B按照质量比10-15:1，置于培养皿中搅拌10-30分钟，然后真空脱泡至表面无气泡，然后放入烘箱中55-65℃下预固化10-20min，得到PDMS溶液；(2) Configure the PDMS solution, place component A and component B in a petri dish at a mass ratio of 10-15:1 and stir for 10-30 minutes, then vacuum defoam until there are no bubbles on the surface, and then put it in an oven for 55 Pre-cure at -65°C for 10-20 minutes to obtain a PDMS solution;
(3)取步骤(2)中的PDMS溶液旋涂于PET基底上，55-65℃下固化15-25min后将薄膜从基底表面剥离，得到有粘性的PDMS薄膜，厚度为200μm-500μm；(3) Spin-coat the PDMS solution in step (2) on the PET substrate, and after curing at 55-65° C. for 15-25 minutes, peel off the film from the surface of the substrate to obtain a sticky PDMS film with a thickness of 200 μm-500 μm;
(4)制备包芯纱-RGO复合网膜：将包芯纱放入紫外-臭氧清洗仪中进行亲水化处理；再将包芯纱浸没入步骤(1)中的RGO分散液，浸泡5-30min后取出并烘干，得到包芯纱-RGO复合网膜。(4) Preparation of core-spun yarn-RGO composite omentum: put the core-spun yarn into an ultraviolet-ozone cleaner for hydrophilic treatment; then immerse the core-spun yarn into the RGO dispersion in step (1) and soak for 5 After -30min, it was taken out and dried to obtain the core-spun yarn-RGO composite omentum.
(5)组装器件：将包芯纱-RGO复合网膜贴在有粘性的PDMS薄膜表面，得到一个传感组件，将两个传感组件贴合，其中，包芯纱-RGO复合网膜的一侧相对；网膜两端连接导线，得到柔性应力传感器。(5) Assembling the device: paste the core-spun yarn-RGO composite omentum on the surface of the sticky PDMS film to obtain a sensing component, and attach the two sensing components together, wherein the core-spun yarn-RGO composite omentum One side is opposite; both ends of the omentum are connected with wires to obtain a flexible stress sensor.
本发明的实质性特点为：Substantive features of the present invention are:
本发明通过采用类弹簧结构的柔性包芯纱作为柔性骨架，表面包裹二维片层结构的石墨烯，得到包芯纱-石墨烯复合网膜作为应变传感器的导电层，来替代表面平整的平面导电层。由于得到的复合网膜特殊的类弹簧网状结构对外界微弱的应力极为敏感，使传感器在灵敏度和检测限等方面的性能都有很大的提高。In the present invention, a flexible core-spun yarn with a spring-like structure is used as a flexible skeleton, and graphene with a two-dimensional sheet structure is wrapped on the surface to obtain a core-spun yarn-graphene composite mesh as a conductive layer of a strain sensor to replace a plane with a flat surface conductive layer. Because the special spring-like mesh structure of the obtained composite omentum is extremely sensitive to external weak stress, the performance of the sensor in terms of sensitivity and detection limit has been greatly improved.
本发明的有益效果为：The beneficial effects of the present invention are:
(1)利用柔性包芯纱作为骨架、纳米结构石墨烯片层作为敏感材料，包芯纱表面为类弹簧的纤维缠绕结构，外界微弱的震动可引起纤维间接触面积发生明显变化，形变传递到表面的石墨烯，使二维层状石墨烯发生接触-分离或相对滑移，有利于对微小应力的探测。与传统平面结构传感器相比，显著提高了检测分辨率。可用于检测压缩、弯曲、震动等不同种类的应力。本应力传感器的压缩检测限可达1.38pa，压缩灵敏度可达77.1kPa-1(如图4)，与平面结构的应力传感器相比灵敏度提高至少20倍。弯曲灵敏度为1.25cm-1(如图6)。可检测振幅为10μm的微弱震动(如图7)。(1) Using flexible core-spun yarn as the skeleton and nanostructured graphene sheets as the sensitive material, the surface of the core-spun yarn is a spring-like fiber winding structure, and weak external vibrations can cause significant changes in the contact area between fibers, and the deformation is transmitted to the The graphene on the surface makes the two-dimensional layered graphene contact-separate or relative slip, which is beneficial to the detection of micro-stress. Compared with traditional planar structure sensors, the detection resolution is significantly improved. It can be used to detect different kinds of stress such as compression, bending, vibration, etc. The compression detection limit of the stress sensor can reach 1.38Pa, and the compression sensitivity can reach 77.1kPa-1 (as shown in Figure 4), which is at least 20 times more sensitive than the stress sensor with a planar structure. The bending sensitivity is 1.25cm-1 (as shown in Figure 6). Weak vibrations with an amplitude of 10 μm can be detected (as shown in Figure 7).
(2)包裹于柔性纤维表面的导电层间接触面积为有效检测应力的面积，因此，该柔性应力传感器的尺寸可以做得非常小(长度和宽度均可做到小于1cm，厚度最薄可达500μm)，解决了现有传感器小型化困难的问题。适合应用于小型化和集成化设备，可检测人体心跳、呼吸等生理信号，用于制作检测人体健康的穿戴式设备。(2) The contact area between the conductive layers wrapped on the surface of the flexible fiber is the area for effective stress detection. Therefore, the size of the flexible stress sensor can be made very small (the length and width can be less than 1cm, and the thinnest thickness can reach 500 μm), which solves the problem of difficulty in miniaturization of existing sensors. Suitable for miniaturized and integrated equipment, it can detect physiological signals such as human heartbeat and respiration, and is used to make wearable devices that detect human health.
(3)制备工艺相对简单，制备条件容易实现。包芯纱-石墨烯导电网膜通过浸泡自组装等方法即可制备完成，且组装方便；该柔性应力传感器可在空气、常压环境下进行器件封装，能有效降低成本，适于大规模制备。(3) The preparation process is relatively simple, and the preparation conditions are easy to realize. The core-spun yarn-graphene conductive mesh can be prepared by soaking self-assembly and other methods, and the assembly is convenient; the flexible stress sensor can be packaged in the air and normal pressure environment, which can effectively reduce the cost and is suitable for large-scale preparation .
附图说明Description of drawings
图1为本发明的柔性应力传感器的结构示意图；Fig. 1 is the structural representation of flexible stress sensor of the present invention;
图2为石墨烯包裹于包芯纱骨架表面的微观结构图像；Fig. 2 is the microstructure image that graphene is wrapped in the core-spun yarn skeleton surface;
图3为本发明的柔性应力传感器的压缩响应曲线图；Fig. 3 is the compression response curve diagram of the flexible stress sensor of the present invention;
图4为本发明的柔性应力传感器的电导变化率随压强变化的曲线图；Fig. 4 is the graph that the conductance change rate of the flexible stress sensor of the present invention changes with pressure;
图5为本发明的柔性应力传感器的弯曲响应曲线图；Fig. 5 is the bending response curve diagram of the flexible stress sensor of the present invention;
图6为本发明的柔性应力传感器的电导变化率随曲率半径变化的曲线图；Fig. 6 is a graph showing the rate of change of conductance of the flexible stress sensor of the present invention as a function of the radius of curvature;
图7为本发明的柔性应力传感器的震动响应曲线图；Fig. 7 is a vibration response curve diagram of the flexible stress sensor of the present invention;
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
本发明涉及的石墨烯分散液为公知材料，是以氧化石墨烯为原料，通过化学还原法制备得到，石墨烯浓度为0.01mg/mL-0.4mg/mL，溶剂为水。The graphene dispersion involved in the present invention is a known material, and is prepared by chemical reduction using graphene oxide as a raw material. The concentration of graphene is 0.01mg/mL-0.4mg/mL, and the solvent is water.
如图1所示，根据本发明的一种柔性应力传感器，包括：上基底，上层包芯纱-石墨烯复合网膜，下层包芯纱-石墨烯复合网膜，下基底，导线。As shown in Figure 1, a kind of flexible stress sensor according to the present invention comprises: upper substrate, upper layer core-spun yarn-graphene composite omentum, lower layer core-spun yarn-graphene composite omentum, lower substrate, wire.
本发明提供所述的柔性应力传感器的制备方法，包括以下步骤：The present invention provides the preparation method of described flexible stress sensor, comprises the following steps:
实施例1：Example 1:
(1)制备RGO分散液：在氧化石墨烯(GO)水分散液(0.01mg/mL，100mL)中加入水合肼(375μL)92℃还原1h，多余沉淀用纱布滤除，得到RGO分散液(0.01mg/mL)。(1) Preparation of RGO dispersion: Add hydrazine hydrate (375 μL) to the graphene oxide (GO) aqueous dispersion (0.01 mg/mL, 100 mL) for reduction at 92 ° C for 1 h, and filter off excess precipitate with gauze to obtain the RGO dispersion ( 0.01mg/mL).
(2)制备包芯纱-RGO复合网膜：将包芯纱(混纺聚酰胺纤维85％，氨纶15％；直径15μm)放入紫外-臭氧清洗仪中利用紫外光照和臭氧处理2min，使其表面亲水，然后再完全浸润在RGO分散液中5min，然后铺平放置在培养皿中，60℃烘干2h，制得包芯纱-RGO复合网膜，如图2所示，将制好的网膜剪成1cm×3cm的矩形备用。(2) Preparation of core-spun yarn-RGO composite omentum: put the core-spun yarn (85% blended polyamide fiber, 15% spandex; diameter 15 μm) into a UV-ozone cleaner and treat it with ultraviolet light and ozone for 2 minutes to make it The surface is hydrophilic, and then completely soaked in the RGO dispersion for 5 minutes, then laid flat on the petri dish, and dried at 60°C for 2 hours to prepare the core-spun yarn-RGO composite omentum, as shown in Figure 2. The omentum was cut into a rectangle of 1cm×3cm for later use.
(3)制备PDMS薄膜：取市售牌号为道康宁Sylgard 184双组分套件硅橡胶的组分A与组分B按质量比10:1比例置于培养皿中搅拌20min，真空脱泡至表面无气泡，60℃预固化16min。(所述的组分A为主剂聚甲基乙烯基硅氧烷预聚物，组分B为带乙烯基侧链的预聚物及交联剂-以下实施例同)。将上述溶液旋涂于聚对苯二甲酸乙二醇酯(PET)基底表面，将旋涂好的PDMS薄膜放入60℃鼓风干燥箱中固化20min，将薄膜从PET基底表面剥离，得到厚度为200μm的PDMS薄膜作为传感器的上基底和下基底(此时PDMS薄膜仍有一定粘性)。(3) Preparation of PDMS film: Take the commercially available brand of Dow Corning Sylgard 184 two-component kit silicone rubber, component A and component B in a mass ratio of 10:1, put them in a petri dish and stir for 20 minutes, and vacuum defoam until the surface is free. Air bubbles, pre-cured at 60°C for 16 minutes. (The component A is a polymethylvinylsiloxane prepolymer as the main agent, and the component B is a prepolymer with vinyl side chains and a crosslinking agent—the same as in the following examples). Spin-coat the above solution on the surface of a polyethylene terephthalate (PET) substrate, put the spin-coated PDMS film in a 60°C blast drying oven to cure for 20min, peel the film from the surface of the PET substrate, and obtain the thickness A PDMS film with a diameter of 200 μm is used as the upper substrate and the lower substrate of the sensor (the PDMS film still has a certain viscosity at this time).
(4)组装传感器：将包芯纱-RGO复合网粘附于PDMS薄膜表面。把宽度为1cm，厚度0.02mm的铜片，用导电银胶固定在包芯纱-RGO复合网膜的两端(如图1所示)，中间留出1.5cm的距离作为传感响应区，制备得到一个传感组件。将两个传感组件面对面组装，压挤出多余的空气，把组装好的器件放入60℃鼓风干燥箱中3h，使PDMS薄膜固化完全，即得到三明治结构的柔性应力传感器。(4) Assembling the sensor: the core-spun yarn-RGO composite mesh was adhered to the surface of the PDMS film. Fix a copper sheet with a width of 1cm and a thickness of 0.02mm on both ends of the core-spun yarn-RGO composite omentum (as shown in Figure 1) with conductive silver glue, leaving a distance of 1.5cm in the middle as the sensor response area. A sensing component is prepared. Assemble the two sensing components face to face, squeeze out the excess air, and put the assembled device in a blast drying oven at 60°C for 3 hours, so that the PDMS film is completely cured, and a flexible stress sensor with a sandwich structure is obtained.
实施例2：Example 2:
(1)制备RGO分散液：在氧化石墨烯(GO)水分散液(0.05mg/mL，100mL)(中加入水合肼(375μL)92℃还原1h，多余沉淀用纱布滤除，得到RGO分散液(0.05mg/mL)。(1) Preparation of RGO dispersion: add hydrazine hydrate (375 μL) to the graphene oxide (GO) aqueous dispersion (0.05mg/mL, 100mL) for reduction at 92°C for 1h, filter the excess precipitate with gauze to obtain the RGO dispersion (0.05mg/mL).
(2)制备包芯纱-RGO复合网膜：将包芯纱(混纺聚酰胺纤维85％，氨纶15％；直径20μm)在紫外-臭氧清洗仪中进行亲水化处理，完全浸润在RGO分散液中10min，然后铺平放置在培养皿中，60℃烘干2h，重复上述浸润步骤2次，制得包芯纱-RGO复合网膜，将制好的网膜剪成1cm×3cm的矩形备用。(2) Preparation of core-spun yarn-RGO composite omentum: the core-spun yarn (85% blended polyamide fiber, 15% spandex; diameter 20 μm) is hydrophilized in a UV-ozone cleaner, completely soaked in RGO dispersion 10 min in the liquid solution, then lay it flat on a petri dish, dry at 60°C for 2 h, repeat the above soaking step twice to prepare the core-spun yarn-RGO composite omentum, and cut the prepared omentum into a rectangle of 1cm×3cm spare.
(3)制备PDMS薄膜：取市售牌号为道康宁Sylgard 184双组分套件硅橡胶的组分A与组分B按质量比10:1比例置于培养皿中搅拌20min，真空脱泡至表面无气泡，60℃预固化16min。将上述溶液旋涂于聚对苯二甲酸乙二醇酯(PET)基底表面，将旋涂好的PDMS薄膜放入60℃鼓风干燥箱中固化30min，将薄膜从PET基底表面剥离，得到厚度为300μm的PDMS薄膜作为传感器的上基底和下基底(此时PDMS薄膜仍有一定粘性)。(3) Preparation of PDMS film: Take the commercially available brand of Dow Corning Sylgard 184 two-component kit silicone rubber, component A and component B in a mass ratio of 10:1, put them in a petri dish and stir for 20 minutes, and vacuum defoam until the surface is free. Bubbles, pre-cured at 60°C for 16 minutes. Spin-coat the above solution on the surface of a polyethylene terephthalate (PET) substrate, put the spin-coated PDMS film in a 60°C blast drying oven for 30 minutes, and peel the film from the surface of the PET substrate to obtain the thickness The PDMS film with a thickness of 300 μm is used as the upper substrate and the lower substrate of the sensor (at this time, the PDMS film still has a certain viscosity).
(4)组装传感器：将包芯纱-RGO复合网粘附于PDMS薄膜表面。把宽度为1cm，厚度0.02mm的铜片，用导电银胶固定在包芯纱-RGO复合网膜的两端(如图1所示)，中间留出1.5cm的距离作为传感响应区，制备得到一个传感组件。将两个传感组件面对面组装，压挤出多余的空气，把组装好的器件放入60℃鼓风干燥箱中3h，使PDMS薄膜固化完全，即得到三明治结构的柔性应力传感器。(4) Assembling the sensor: the core-spun yarn-RGO composite mesh was adhered to the surface of the PDMS film. Fix a copper sheet with a width of 1cm and a thickness of 0.02mm on both ends of the core-spun yarn-RGO composite omentum (as shown in Figure 1) with conductive silver glue, leaving a distance of 1.5cm in the middle as the sensor response area. A sensing component is prepared. Assemble the two sensing components face to face, squeeze out the excess air, and put the assembled device in a blast drying oven at 60°C for 3 hours, so that the PDMS film is completely cured, and a flexible stress sensor with a sandwich structure is obtained.
实施例3：Example 3:
(1)制备RGO分散液：在氧化石墨烯(GO)水分散液(0.1mg/mL，100mL)(中加入水合肼(375μL)92℃还原1h，多余沉淀用纱布滤除，得到RGO分散液(0.1mg/mL)。(1) Preparation of RGO dispersion: add hydrazine hydrate (375 μL) to the graphene oxide (GO) aqueous dispersion (0.1mg/mL, 100mL) for reduction at 92°C for 1h, and filter out the excess precipitate with gauze to obtain the RGO dispersion (0.1 mg/mL).
(2)制备包芯纱-RGO复合网膜：将包芯纱(混纺聚酰胺纤维85％，氨纶15％；直径20μm)在紫外-臭氧清洗仪中进行亲水化处理，完全浸润在RGO分散液中15min，然后铺平放置在培养皿中，60℃烘干2h，重复上述浸润步骤4次，制得包芯纱-RGO复合网膜，将制好的网膜剪成1cm×3cm的矩形备用。(2) Preparation of core-spun yarn-RGO composite omentum: the core-spun yarn (85% blended polyamide fiber, 15% spandex; diameter 20 μm) is hydrophilized in a UV-ozone cleaner, completely soaked in RGO dispersion solution for 15 minutes, then laid flat on a petri dish, dried at 60°C for 2 hours, and repeated the above infiltration steps 4 times to obtain a core-spun yarn-RGO composite omentum, and cut the prepared omentum into a rectangle of 1cm×3cm spare.
(3)制备PDMS薄膜：取市售牌号为道康宁Sylgard 184双组分套件硅橡胶的组分A与组分B按质量比10:1比例置于培养皿中搅拌20min，真空脱泡至表面无气泡，60℃预固化16min。将上述溶液旋涂于聚对苯二甲酸乙二醇酯(PET)基底表面，将旋涂好的PDMS薄膜放入60℃鼓风干燥箱中固化35min，将薄膜从PET基底表面剥离，得到厚度为400μm的PDMS薄膜作为传感器的上基底和下基底(此时PDMS薄膜仍有一定粘性)。(3) Preparation of PDMS film: Take the commercially available brand of Dow Corning Sylgard 184 two-component kit silicone rubber, component A and component B in a mass ratio of 10:1, put them in a petri dish and stir for 20 minutes, and vacuum defoam until the surface is free. Air bubbles, pre-cured at 60°C for 16 minutes. Spin-coat the above solution on the surface of a polyethylene terephthalate (PET) substrate, put the spin-coated PDMS film in a 60°C blast drying oven for 35 minutes, and peel the film from the surface of the PET substrate to obtain the thickness A PDMS film with a thickness of 400 μm is used as the upper substrate and the lower substrate of the sensor (the PDMS film still has a certain viscosity at this time).
(4)组装传感器：将包芯纱-RGO复合网粘附于PDMS薄膜表面。把宽度为1cm，厚度0.02mm的铜片，用导电银胶固定在包芯纱-RGO复合网膜的两端(如图1所示)，中间留出1.5cm的距离作为传感响应区，制备得到一个传感组件。将两个传感组件面对面组装，压挤出多余的空气，把组装好的器件放入60℃鼓风干燥箱中3h，使PDMS薄膜固化完全，即得到三明治结构的柔性应力传感器。(4) Assembling the sensor: the core-spun yarn-RGO composite mesh was adhered to the surface of the PDMS film. Fix a copper sheet with a width of 1cm and a thickness of 0.02mm on both ends of the core-spun yarn-RGO composite omentum (as shown in Figure 1) with conductive silver glue, leaving a distance of 1.5cm in the middle as the sensor response area. A sensing component is prepared. Assemble the two sensing components face to face, squeeze out the excess air, and put the assembled device in a blast drying oven at 60°C for 3 hours, so that the PDMS film is completely cured, and a flexible stress sensor with a sandwich structure is obtained.
实施例4：Example 4:
(1)制备RGO分散液：在氧化石墨烯(GO)水分散液(0.2mg/mL，100mL)(中加入水合肼(375μL)92℃还原1h，多余沉淀用纱布滤除，得到RGO分散液(0.2mg/mL)。(1) Preparation of RGO dispersion: add hydrazine hydrate (375 μL) to the graphene oxide (GO) aqueous dispersion (0.2mg/mL, 100mL) for reduction at 92°C for 1h, and filter the excess precipitate with gauze to obtain the RGO dispersion (0.2 mg/mL).
(2)制备包芯纱-RGO复合网膜：将包芯纱(混纺聚酰胺纤维85％，氨纶15％；直径30μm)在紫外-臭氧清洗仪中进行亲水化处理，完全浸润在RGO分散液中20min，然后铺平放置在培养皿中，60℃烘干2h，重复上述浸润步骤6次，制得包芯纱-RGO复合网膜，将制好的网膜剪成1cm×3cm的矩形备用。(2) Preparation of core-spun yarn-RGO composite omentum: the core-spun yarn (85% blended polyamide fiber, 15% spandex; diameter 30 μm) was hydrophilized in a UV-ozone cleaner, completely soaked in RGO dispersion solution for 20 minutes, then laid flat on a petri dish, dried at 60°C for 2 hours, and repeated the above soaking steps 6 times to obtain a core-spun yarn-RGO composite omentum, and cut the prepared omentum into a rectangle of 1cm×3cm spare.
(3)制备PDMS薄膜：取市售牌号为道康宁Sylgard 184双组分套件硅橡胶的组分A与组分B按质量比10:1比例置于培养皿中搅拌20min，真空脱泡至表面无气泡，60℃预固化16min。将上述溶液旋涂于聚对苯二甲酸乙二醇酯(PET)基底表面，将旋涂好的PDMS薄膜放入60℃鼓风干燥箱中固化35min，将薄膜从PET基底表面剥离，得到厚度为400μm的PDMS薄膜作为传感器的上基底和下基底(此时PDMS薄膜仍有一定粘性)。(3) Preparation of PDMS film: Take the commercially available brand of Dow Corning Sylgard 184 two-component kit silicone rubber, component A and component B in a mass ratio of 10:1, put them in a petri dish and stir for 20 minutes, and vacuum defoam until the surface is free. Air bubbles, pre-cured at 60°C for 16 minutes. Spin-coat the above solution on the surface of a polyethylene terephthalate (PET) substrate, put the spin-coated PDMS film in a 60°C blast drying oven for 35 minutes, and peel the film from the surface of the PET substrate to obtain the thickness A PDMS film with a thickness of 400 μm is used as the upper substrate and the lower substrate of the sensor (the PDMS film still has a certain viscosity at this time).
(4)组装传感器：将包芯纱-RGO复合网粘附于PDMS薄膜表面。把宽度为1cm，厚度0.02mm的铜片，用导电银胶固定在包芯纱-RGO复合网膜的两端(如图1所示)，中间留出1.5cm的距离作为传感响应区，制备得到一个传感组件。将两个传感组件面对面组装，压挤出多余的空气，把组装好的器件放入60℃鼓风干燥箱中3h，使PDMS薄膜固化完全，即得到三明治结构的柔性应力传感器。(4) Assembling the sensor: the core-spun yarn-RGO composite mesh was adhered to the surface of the PDMS film. Fix a copper sheet with a width of 1cm and a thickness of 0.02mm on both ends of the core-spun yarn-RGO composite omentum (as shown in Figure 1) with conductive silver glue, leaving a distance of 1.5cm in the middle as the sensor response area. A sensing component is prepared. Assemble the two sensing components face to face, squeeze out the excess air, and put the assembled device in a blast drying oven at 60°C for 3 hours, so that the PDMS film is completely cured, and a flexible stress sensor with a sandwich structure is obtained.
实施例5：Example 5:
(1)制备RGO分散液：在氧化石墨烯(GO)水分散液(0.4mg/mL，100mL)(中加入水合肼(375μL)92℃还原1h，多余沉淀用纱布滤除，得到RGO分散液(0.4mg/mL)。(1) Preparation of RGO dispersion: Add hydrazine hydrate (375 μL) to the graphene oxide (GO) aqueous dispersion (0.4mg/mL, 100mL) for reduction at 92°C for 1h, filter the excess precipitate with gauze to obtain the RGO dispersion (0.4 mg/mL).
(2)制备包芯纱-RGO复合网膜：将包芯纱(混纺聚酰胺纤维85％，氨纶15％；直径30μm)在紫外-臭氧清洗仪中进行亲水化处理，完全浸润在RGO分散液中30min，然后铺平放置在培养皿中，60℃烘干2h，重复上述浸润步骤8次，制得包芯纱-RGO复合网膜，将制好的网膜剪成1cm×3cm的矩形备用。(2) Preparation of core-spun yarn-RGO composite omentum: the core-spun yarn (85% blended polyamide fiber, 15% spandex; diameter 30 μm) was hydrophilized in a UV-ozone cleaner, completely soaked in RGO dispersion solution for 30 minutes, then laid flat on a petri dish, dried at 60°C for 2 hours, and repeated the above soaking steps 8 times to obtain a core-spun yarn-RGO composite omentum, and cut the prepared omentum into a rectangle of 1cm×3cm spare.
(3)制备PDMS薄膜：取市售牌号为道康宁Sylgard 184双组分套件硅橡胶的组分A与组分B按质量比10:1比例置于培养皿中搅拌20min，真空脱泡至表面无气泡，60℃预固化16min。将上述溶液旋涂于聚对苯二甲酸乙二醇酯(PET)基底表面，将旋涂好的PDMS薄膜放入60℃鼓风干燥箱中固化45min，将薄膜从PET基底表面剥离，得到厚度为500μm的PDMS薄膜作为传感器的上基底和下基底(此时PDMS薄膜仍有一定粘性)。(3) Preparation of PDMS film: Take the commercially available brand of Dow Corning Sylgard 184 two-component kit silicone rubber, component A and component B in a mass ratio of 10:1, put them in a petri dish and stir for 20 minutes, and vacuum defoam until the surface is free. Air bubbles, pre-cured at 60°C for 16 minutes. Spin-coat the above solution on the surface of a polyethylene terephthalate (PET) substrate, put the spin-coated PDMS film in a 60°C blast drying oven for 45 minutes, and peel the film from the surface of the PET substrate to obtain the thickness A PDMS film with a thickness of 500 μm is used as the upper substrate and the lower substrate of the sensor (the PDMS film still has a certain viscosity at this time).
(4)组装传感器：将包芯纱-RGO复合网粘附于PDMS薄膜表面。把宽度为1cm，厚度0.02mm的铜片，用导电银胶固定在包芯纱-RGO复合网膜的两端(如图1所示)，中间留出1.5cm的距离作为传感响应区，制备得到一个传感组件。将两个传感组件面对面组装，压挤出多余的空气，把组装好的器件放入60℃鼓风干燥箱中3h，使PDMS薄膜固化完全，即得到三明治结构的柔性应力传感器。(4) Assembling the sensor: the core-spun yarn-RGO composite mesh was adhered to the surface of the PDMS film. Fix a copper sheet with a width of 1cm and a thickness of 0.02mm on both ends of the core-spun yarn-RGO composite omentum (as shown in Figure 1) with conductive silver glue, leaving a distance of 1.5cm in the middle as the sensor response area. A sensing component is prepared. Assemble the two sensing components face to face, squeeze out the excess air, and put the assembled device in a blast drying oven at 60°C for 3 hours, so that the PDMS film is completely cured, and a flexible stress sensor with a sandwich structure is obtained.
图3为实例1中的传感器对压缩形变的循环响应曲线。在1kPa压力，传感器表现出良好的循环响应性能。图4为实例1中的传感器电导变化率随压强变化的曲线，斜率可反应传感器的压缩灵敏度。压强<0.3kPa，灵敏度高达77.1kPa-1。同时，传感器具有很宽的检测范围，最低可用于检测1.38pa的微小压力，最高可检测80kPa的压力。图5为实例1中的传感器对弯曲形变的响应曲线图。在曲率半径为1.5cm，传感器表现出稳定且灵敏的循环响应性能。图6为实例1中的传感器电导变化率随曲率半径变化的曲线，弯曲灵敏度为1.25cm-1。图7为实例1中的传感器对微弱正旋震动的循环响应曲线。振幅为10μm，频率为1HZ，传感器表现出明显的响应信号。以上电化学数据通过上海辰华电化学工作站CHI-760E测试，采用恒电位模式，电压为1V。各种形变通过动态机械分析仪DMA(Q800,TA Instruments)提供。FIG. 3 is the cyclic response curve of the sensor in Example 1 to compression deformation. At 1kPa pressure, the sensor exhibits good cyclic response performance. FIG. 4 is a curve of the change rate of the conductance of the sensor in Example 1 as a function of the pressure, and the slope can reflect the compression sensitivity of the sensor. Pressure <0.3kPa, sensitivity up to 77.1kPa-1 . At the same time, the sensor has a wide detection range, which can be used to detect a small pressure of 1.38pa at the lowest and a pressure of 80kPa at the highest. FIG. 5 is a graph showing the response of the sensor in Example 1 to bending deformation. At a radius of curvature of 1.5 cm, the sensor exhibits stable and sensitive cyclic response performance. Fig. 6 is a curve of the conductance change rate of the sensor in Example 1 as a function of the radius of curvature, and the bending sensitivity is 1.25 cm-1 . FIG. 7 is the cyclic response curve of the sensor in Example 1 to weak positive rotation vibration. The amplitude is 10μm, the frequency is 1HZ, and the sensor shows a clear response signal. The above electrochemical data were tested by Shanghai Chenhua Electrochemical Workstation CHI-760E, using constant potential mode with a voltage of 1V. Various deformations were provided by a dynamic mechanical analyzer DMA (Q800, TA Instruments).
本应力传感器通过使用复合网膜来替代传统的平面结构材料作为导电层，极大提升了传感器的灵敏度，降低了检测限，适用于多种形变的高效检测。The stress sensor uses the composite omentum to replace the traditional planar structure material as the conductive layer, which greatly improves the sensitivity of the sensor, reduces the detection limit, and is suitable for efficient detection of various deformations.
本发明的柔性应力传感器的工作原理为：所述柔性应力传感器初始状态，上下两部分传感组件部分接触，形成导通结构。在外界应力作用下，基底发生形变并传导至包芯纱骨架及骨架表面的导电层，骨架的形变使表面导电层的接触面积发生变化，引起石墨烯片层之间发生接触-分离和相对滑移，从而导致传感器电导率发生变化。The working principle of the flexible stress sensor of the present invention is as follows: in the initial state of the flexible stress sensor, the upper and lower sensing components are partially in contact to form a conductive structure. Under the action of external stress, the substrate deforms and conducts to the skeleton of the core-spun yarn and the conductive layer on the surface of the skeleton. The deformation of the skeleton changes the contact area of the surface conductive layer, causing contact-separation and relative sliding between graphene sheets. shift, resulting in a change in the conductivity of the sensor.
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within range.
本发明未尽事宜为公知技术。Matters not covered in the present invention are known technologies.
| Application Number | Priority Date | Filing Date | Title |
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| CN201810396657.2ACN108332887B (en) | 2018-04-28 | 2018-04-28 | Flexible stress sensor |
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| CN201810396657.2ACN108332887B (en) | 2018-04-28 | 2018-04-28 | Flexible stress sensor |
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| CN201810396657.2AActiveCN108332887B (en) | 2018-04-28 | 2018-04-28 | Flexible stress sensor |
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