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WO2023197130A1 - 一种多通道高密度的超窄可拉伸微电极及其制备方法和应用 - Google Patents

一种多通道高密度的超窄可拉伸微电极及其制备方法和应用 Download PDF

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WO2023197130A1
WO2023197130A1 PCT/CN2022/086231 CN2022086231W WO2023197130A1 WO 2023197130 A1 WO2023197130 A1 WO 2023197130A1 CN 2022086231 W CN2022086231 W CN 2022086231W WO 2023197130 A1 WO2023197130 A1 WO 2023197130A1
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flexible substrate
stretching
preparation
conductive layer
stretchable
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PCT/CN2022/086231
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English (en)
French (fr)
Inventor
刘志远
李韩飞
李光林
韩飞
谢瑞杰
赵行
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中国科学院深圳先进技术研究院
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Priority to PCT/CN2022/086231 priority Critical patent/WO2023197130A1/zh
Publication of WO2023197130A1 publication Critical patent/WO2023197130A1/zh

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
    • A61B5/25—Bioelectric electrodes therefor
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B5/00—Measuring for diagnostic purposes; Identification of persons
    • A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
    • A61B5/25—Bioelectric electrodes therefor
    • A61B5/279—Bioelectric electrodes therefor specially adapted for particular uses
    • A61B5/296—Bioelectric electrodes therefor specially adapted for particular uses for electromyography [EMG]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/02—Details
    • A61N1/04—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation

Definitions

  • the present invention relates to the technical field of flexible electrodes, and in particular to a multi-channel, high-density, ultra-narrow stretchable microelectrode and its preparation method and application.
  • flexible electrodes are prepared from flexible substrates and stretchable conductive materials (such as gold films).
  • stretchable conductive materials such as gold films.
  • the current flexible and stretchable electrode arrays are limited by the characteristics of the manufacturing process and materials.
  • the sensing points and width of the electrodes cannot be soft and stretchable in a small size, which hinders the development of higher-density flexible electrode arrays. Therefore, how to prepare high-density flexible microelectrodes to achieve precise signal collection from tiny objects is still a problem.
  • Multi-channel high-density ultra-narrow stretchable microelectrodes can achieve physiological electrical signal collection and electrical stimulation at higher spatial resolution.
  • the smaller the size of the stretchable electrode its stretchability and impedance will decrease. The more unstable it is. This results in the current inability to stably achieve the preparation of stretchable microelectrodes with a size below 20 microns.
  • the realization of patterning and packaging solutions in the preparation process of stretchable microelectrodes mainly rely on photolithography technology.
  • Photolithography technology does not have the simplicity of one-piece molding by physical mask method, and the stretchable electrodes prepared by it are gradually The reduction in size, increase in cost, and deterioration in performance have affected the development of stretchable microelectrodes to a certain extent.
  • Klas Tybrandt and others used gold-coated titanium dioxide nanowires embedded in a silica gel matrix to produce multi-channel high-density flexible stretchable electrodes with a minimum width of 30 ⁇ m and a stretch rate of 30%, and conducted long-term measurements of neural signals in the cerebral cortex of mice. Monitoring (Advanced Materials, 2018, 30(15):1706520.), this method has the disadvantages of cumbersome preparation process and high cost. Yuxin Liu et al. used soft conductive hydrogel and photolithography to prepare an electrode with a width of 20 ⁇ m and a stretch rate of 20%. Its advantages are obvious in low-voltage stimulation of the sciatic nerve in living mice, which is currently possible.
  • the present invention provides a multi-channel high-density ultra-narrow stretchable microelectrode and its preparation method and application.
  • the present invention uses the pre-stretched size enlargement method to enlarge the flexible substrate.
  • a conductive layer is prepared by pattern sputtering, and then the flexible substrate is released to restore its shape.
  • a multi-channel high-density layer can be obtained.
  • the number of channels, density, sensing point distribution and width of a single channel of ultra-narrow stretchable microelectrodes can be changed according to different needs.
  • the stretchable microelectrode provided by the present invention can reach the narrowest width of three electrode channels of 10 microns, and can still maintain stable tensile conductivity of more than 100% and tensile stability for thousands of cycles.
  • the present invention provides a method for preparing multi-channel, high-density, ultra-narrow stretchable microelectrodes, which includes the following steps:
  • the flexible substrate includes a stretching zone and a fixed zone; stretch and amplify the stretching zone; perform pattern sputtering on the stretched and amplified flexible substrate through a mask to prepare a conductive layer; release The stretching zone causes it to retract; after packaging, the multi-channel high-density ultra-narrow stretchable microelectrode is obtained.
  • the fixing zone is fixed by adhesion.
  • the fixing area is pasted and fixed with adhesive tape, which can ensure that during the stretching process, the stretching area deforms but the fixing area does not deform.
  • the transverse or longitudinal amplification rate is determined by the shape design of the electrode and the thickness and tensile properties of the flexible substrate. In order to prevent fracture, the magnification ratio does not exceed the stretch at break of the flexible substrate.
  • the pattern sputtering of the flexible substrate after stretching and amplification processing through a mask is pattern sputtering on the sticky surface of the flexible substrate after stretching and amplification processing;
  • the pattern sputtering of the flexible substrate after stretching and amplification through a mask is pattern sputtering on the flat surface of the flexible substrate after stretching and amplification; a mask is required in the pattern sputtering process, so It is necessary to ensure that the sputtering surface of the flexible substrate is flat, and the conductive layer prepared by sputtering on the flat surface has better performance;
  • the pattern sputtering is magnetron sputtering
  • the conductive layer is a gold conductive layer.
  • the size of the mask matches the size of the stretch-amplified flexible substrate.
  • the step of encapsulating the conductive layer is: exposing the electrode circuit area in the conductive layer that needs to be encapsulated, and encapsulating it;
  • the conductive layer encapsulation is a hydrogenated styrene-butadiene block copolymer (SEBS) film encapsulation;
  • SEBS hydrogenated styrene-butadiene block copolymer
  • the specific operation of the conductive layer encapsulation is: shielding the parts of the electrode circuits of the conductive layer that do not need to be encapsulated to expose the electrode circuit areas that need to be encapsulated: for example, using thin copper wires to block the sensing area , use cardboard to block the area connected to the printed circuit board (PCB); attach a hydrogenated styrene-butadiene block copolymer (SEBS) film to the conductive layer, remove the blockage, and complete the conductive layer encapsulation.
  • SEBS hydrogenated styrene-butadiene block copolymer
  • the hydrogenated styrene-butadiene block copolymer (SEBS) film will retract with the flexible substrate. While shrinking, the mutual adhesion of hydrogenated styrene-butadiene block copolymer (SEBS) films prevents them from falling off.
  • the preparation method of the hydrogenated styrene-butadiene block copolymer (SEBS) film is: adding a toluene solution of the hydrogenated styrene-butadiene block copolymer (SEBS) with a mass fraction of 5 to 15%. Drop it on the water phase liquid surface to obtain a thin film with a thickness of 100 ⁇ 200nm.
  • the flexible substrate is a stretchable and resilient flexible substrate with adhesiveness, selected from any one or more elastic polymer materials; preferably hydrogenated styrene-butadiene block Copolymer (SEBS) flexible substrate;
  • SEBS hydrogenated styrene-butadiene block Copolymer
  • the preparation method of the hydrogenated styrene-butadiene block copolymer (SEBS) flexible substrate is: placing a toluene solution of SEBS with a mass percentage of 5 to 15% on polytetrafluoroethylene In an ethylene (PTFE) mold, a SEBS film with a thickness of about 200 to 300 microns is obtained after air drying.
  • SEBS hydrogenated styrene-butadiene block copolymer
  • the side of the SEBS film obtained by the above method facing the bottom of the mold is in the form of an inverted mold of the polytetrafluoroethylene (PTFE) mold, which basically does not have Self-adhesive; after the other side is naturally air-dried, it will be in the form of a flat SEBS film with strong self-adhesiveness and mutual adhesion.
  • PTFE polytetrafluoroethylene
  • a stretchable and resilient flexible substrate with viscosity is used. After the stretching zone is released, it shrinks, and the conductive layer deforms accordingly to form an electrode structure with a specific pattern. According to the structure of the mask and The multiple of tensile deformation can control the structure of the pattern.
  • hydrogenated styrene-butadiene block copolymer (SEBS) is used as raw material, toluene is used as a solvent to prepare a flexible substrate, and a hydrogenated styrene-butadiene block with a thickness of 100 to 200 nm is used.
  • SEBS hydrogenated styrene-butadiene block copolymer
  • the copolymer (SEBS) film encapsulates the conductive layer. After the stretch zone is released, the hydrogenated styrene-butadiene block copolymer (SEBS) film shrinks and does not fall off due to the self-adhesiveness of SEBS.
  • the package uses anisotropic conductive tape to connect the gold finger portions of the electrodes to the channels on the printed circuit board in one-to-one correspondence to form a stable conductive path.
  • the high density means that the density of sensing points is greater than or equal to 1/mm 2 ;
  • the ultra-narrow means that the channel width of the electrode is less than or equal to 50 microns.
  • the present invention provides multi-channel, high-density, ultra-narrow stretchable microelectrodes obtained by the above preparation method.
  • the present invention provides an application of the above-mentioned ultra-narrow stretchable microelectrode in preparing a device for collecting physiological electrical signals or in collecting physiological electrical signals.
  • the present invention utilizes the soft characteristics of the flexible substrate, introduces the pre-stretching behavior of the flexible polymer into the preparation process of the electrode, prepares the electrode pattern on the size-enlarged substrate and then releases and retracts it to ultimately realize the miniaturization and pullability of the electrode. Stretchability.
  • the present invention finally prepares multi-channel high-density ultra-narrow stretchable microelectrodes by stretching to change the size of the flexible substrate, which is suitable for manual operation and mechanized mass production.
  • the multi-channel high-density ultra-narrow stretchable microelectrode prepared by the present invention not only successfully collected the physiological electrical signals of cells, but also realized the collection of myoelectric signals outside the subcutaneous muscle membrane of mice. And the data collected has high reliability.
  • the multi-channel high-density ultra-narrow stretchable microelectrodes provided by the present invention performed a series of electrical stimulation on nerve cells and mouse tissues, successfully achieving simultaneous stimulation and recording between different channels, that is, stimulating some channels. signal, and other channels collect stimulation signals.
  • the electrode provided by the present invention provides new ideas for the preparation of flexible and stretchable electrodes, whether it is a change in electrode pattern style or electrode size.
  • the present invention has the following advantages:
  • the preparation method provided by the present invention combines the microcracked gold film technology and the pre-stretched size enlargement of the flexible substrate. It can not only prepare the electrode into a multi-channel high-density ultra-narrow electrode (width 10 microns), but also ensures good electrode performance. Tensile properties and cyclic stability;
  • the preparation method provided by the present invention utilizes the size enlargement of the flexible substrate so that the conductive layer encapsulation layer after enlargement and release will not slip or shift, and the sensing point area of the electrode will be clearly exposed without being blocked, and can adapt to the release.
  • the change in size reduces the difficulty of overexposure of the sensing point area during the preparation of ultra-narrow electrodes, thereby achieving an ultra-narrow electrode path (width 10 microns), and the area of the exposed sensing point is also of the same size level (10 microns ⁇ 10 microns);
  • the present invention is simpler in the preparation process, has a high success rate, and has higher electrode efficiency.
  • the present invention does not require the participation of photolithography equipment, and accordingly reduces the preparation cost.
  • Figure 1 is a flow chart for the preparation of multi-channel, high-density, ultra-narrow stretchable microelectrodes in Example 1 of the present invention.
  • Figure 2 is a physical diagram of a 32-channel high-density ultra-narrow stretchable microelectrode prepared in Example 1 of the present invention.
  • a 32-channel high-density ultra-narrow stretchable microelectrode is prepared.
  • the preparation method is shown in Figure 1, which specifically includes the following steps:
  • Pre-stretching and fixing of the flexible substrate Use tape to stick and fix the back of the flexible substrate, which is recorded as the fixed area; pre-stretch the flexible substrate, and the fixed area will not deform during the stretching process, but the stretched deformed area will The size is stretched from the initial 1 unit length ⁇ 1 unit length to 3 unit length ⁇ 2 unit length, and the deformed flexible base is fixed to prevent its shape from shrinking;
  • This embodiment uses hydrogenated styrene-butadiene block copolymer (SEBS) film as the encapsulation layer material of the conductive layer; hydrogenated styrene-butadiene with a mass fraction of 5% Drop the toluene solution of the block copolymer (SEBS) on the water to obtain a film with a thickness of 100nm; use copper wire to block the sensing area in the electrode circuit, and use cardboard to block the part of the electrode circuit connected to the printed circuit board (PCB). Attach the SEBS film to the conductive layer. After a few minutes, remove the shielding copper wire and cardboard to complete the encapsulation of the conductive layer. After that, release the fixation in step (2), the deformation area of the flexible substrate retracts, and the SEBS film is encapsulated. It shrinks accordingly and does not fall off due to its stickiness;
  • SEBS hydrogenated styrene-butadiene block copolymer
  • Electrode packaging Use heterogonal conductive tape to connect the gold finger part of the electrode to the channel on the printed circuit board in one-to-one correspondence to form a stable conductive path.
  • the actual picture of the 32-channel microelectrode prepared in this embodiment is shown in Figure 2.
  • the density of sensing points is 3/ 0.01mm2 ; the channel width is 10 microns.
  • the prepared 32-channel microelectrode was used to conduct a physiological electrical signal collection experiment. Not only the physiological electrical signals of cells were successfully collected, but also the electromyographic signals outside the subcutaneous muscle membrane of mice were collected, and all results were obtained. got reliable data.
  • the prepared 32-channel microelectrode was used to perform a series of electrical stimulation on nerve cells and mouse tissue, and successfully realized simultaneous stimulation and recording between different channels, that is, some channels gave stimulation signals, and other channels collected stimulation signals.

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Abstract

本发明公开了一种多通道高密度的超窄可拉伸微电极及其制备方法和应用。其中，制备方法包括如下步骤：提供一柔性基底；柔性基底包括拉伸区和固定区；对拉伸区进行拉伸放大处理；通过掩模版对拉伸放大处理后的柔性基底进行图案溅射制备导电层；释放拉伸区使其回缩；封装后即得到多通道高密度超窄可拉伸微电极。本发明提供的制备方法结合微裂纹金膜技术与柔性基底的预拉伸尺寸放大，不仅可以将电极制备成多通道高密度的超窄电极，还保证电极良好的拉伸性能以及循环稳定性能。

Description

一种多通道高密度的超窄可拉伸微电极及其制备方法和应用 技术领域
本发明涉及柔性电极技术领域，尤其涉及一种多通道高密度的超窄可拉伸微电极及其制备方法和应用。
背景技术
现有技术中，柔性电极由柔性基底与可拉伸导电材料(如金薄膜)制备得到。其中，薄膜式柔性可拉伸电极的制备工艺逐渐成熟，大规模制作与图案化都已实现(Advanced Materials,2019,31(35):1901360.)。当前的柔性可拉伸电极阵列受限于制作工艺和材料的特性，电极的感应点和宽度无法在很小尺寸上实现柔软可拉伸，阻碍了更高密度的柔性电极阵列的发展。因此如何制备高密度柔性微电极实现对微小对象的精准信号采集仍然是一个难题。
多通道高密度超窄可拉伸微电极可以在更高的空间分辨率上实现生理电信号的采集以及电刺激，然而，可拉伸电极的尺寸越小，其可拉伸性和阻抗就会越不稳定。这导致目前无法稳定实现20微米尺寸以下级别的可拉伸微电极的制备。另外，可拉伸微电极的制备过程中图案化的实现以及封装方案主要依赖于光刻技术，光刻技术不具备物理掩模法一体成型式的简便，且其制备的可拉伸电极随着尺寸的减小，成本增加，性能变差，导致可拉伸微电极的发展受到一定的影响。
例如，Klas Tybrandt等人利用镀金二氧化钛纳米线嵌入到硅胶基体中，制作了最小宽度30μm，拉伸率为30％的多通道高密度柔性可拉伸电极，并对老鼠大脑皮层神经信号进行了长期监测(Advanced Materials,2018,30(15):1706520.)，该方法存在制备过程繁琐、成本较高的缺点。Yuxin Liu等人利用软导电水凝胶加光刻的方法制备了一种宽度20μm拉伸率20％的电极，其在活体小鼠坐骨神经低电压刺激中的优势比较明显，这也是目前能做到的柔性可拉伸电极尺寸的最 小极限(Nature biomedical engineering,2019,3(1):58-68.)。虽然光刻法能够将电极图案的尺寸微小化，但是其操作复杂，对基底以及导电材料要求较高，还有可能对电极造成一定程度的破坏，工艺条件苛刻，封装工艺相对复杂，成本偏高，导致其不能实际应用。随着软电子微型化需求的提高，柔性电极在记录和刺激上需更加精准化和微型化，因此利用材料特性开发新的柔性电极是实现该目标的可靠策略。
发明内容
针对上述技术问题，本发明提供一种多通道高密度的超窄可拉伸微电极及其制备方法和应用。本发明利用预拉伸尺寸放大法将柔性基底放大，在放大后的柔性基底上，通过图案溅射制备导电层，然后释放柔性基底，使其回复形状，封装后即可得到多通道高密度的超窄可拉伸微电极，其通道数、密度、感应点分布以及单个通道的宽度都可以根据不同需求去改变。本发明提供的可拉伸微电极最窄可达到三个电极通道的宽度为10微米，并且仍能保持超过100％的稳定的拉伸导电性，以及上千次循环的拉伸稳定性。
为实现上述目的，本发明采取的技术方案为：
一方面，本发明提供一种多通道高密度的超窄可拉伸微电极的制备方法，包括如下步骤：
提供一柔性基底；所述柔性基底包括拉伸区和固定区；对所述拉伸区进行拉伸放大处理；通过掩模版对拉伸放大处理后的柔性基底进行图案溅射制备导电层；释放所述拉伸区使其回缩；封装后即得到所述多通道高密度超窄可拉伸微电极。
作为优选地实施方式，所述拉伸区进行拉伸放大处理中，所述固定区通过粘贴固定。在某些具体的实施方式中，通过胶带将所述固定区粘贴固定，能够保证在拉伸过程中，所述拉伸区产生形变，而所述固定区则不发生形变。
在本发明的技术方案中，所述拉伸区进行拉伸放大处理中，横向或纵向的 放大率由所述电极的形状设计以及所述柔性基底的厚薄和拉伸性能等决定，为了防止发生断裂，所述放大率不超过所述柔性基底的断裂拉伸率。
作为优选地实施方式，所述通过掩模版对拉伸放大处理后的柔性基底进行图案溅射为对拉伸放大处理后的柔性基底的具有粘性的面进行图案溅射；
优选地，所述通过掩模版对拉伸放大处理后的柔性基底进行图案溅射为对拉伸放大处理后的柔性基底的平整的面进行图案溅射；图案溅射过程中需要掩模版，因此需要保证柔性基底的溅射面的平整，另外平整的面上溅射制备的导电层性能更好；
优选地，所述图案溅射为磁控溅射；
优选地，所述导电层为金导电层。
作为优选地实施方式，所述通过掩模版对拉伸放大处理后的柔性基底进行图案溅射中，所述掩模版的尺寸与所述拉伸放大处理后的柔性基底的尺寸相匹配。
作为优选地实施方式，还包括导电层封装的步骤，所述导电层封装的步骤为：暴露出所述导电层中需要封装的电极线路区域，对其进行封装；
优选地，所述导电层封装为氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜封装；
在某些具体的实施方式中，所述导电层封装的具体操作为：将导电层的电极线路中不需要封装的部分遮挡以暴露出需要封装的电极线路区域：如用细铜丝遮挡感应区域，用纸板遮挡与印刷电路板(PCB)连接的区域；将氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜贴附于所述导电层上，去除遮挡，完成导电层封装。采用氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜对导电层进行封装，拉伸区释放后，氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜会随柔性基底的回缩而收缩，氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜的互粘性可以防止其脱落。
其中，所述氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜的制备方法为：将质量分数为5～15％的氢化苯乙烯-丁二烯嵌段共聚物(SEBS)的甲苯溶液滴于水相 液面上，得到厚度为100～200nm的薄膜。
作为优选地实施方式，所述柔性基底为具有粘性的可拉伸回弹柔性基底，选自弹性高分子聚合物材料中的任意一种或多种；优选为氢化苯乙烯-丁二烯嵌段共聚物(SEBS)柔性基底；
在某些具体的实施方式中，所述氢化苯乙烯-丁二烯嵌段共聚物(SEBS)柔性基底的制备方法为：将质量百分数为5～15％的SEBS的甲苯溶液置于聚四氟乙烯(PTFE)模具中，风干后得到厚度约为200～300微米的SEBS薄膜，通过上述方法得到的SEBS薄膜朝向模具底部的一面为聚四氟乙烯(PTFE)模具的倒模形态，基本不具备自粘性；另一面自然风干后为平整的SEBS膜形态，具有较强的自粘性和互粘性。
在本发明的技术方案中，采用具有粘性的可拉伸回弹柔性基底，释放拉伸区后，其发生收缩，导电层随之形变，形成具有特定图案的电极结构，根据掩模版的结构以及拉伸形变的倍数可以控制图案的结构。
在本发明的技术方案中，采用氢化苯乙烯-丁二烯嵌段共聚物(SEBS)为原料，甲苯为溶剂制备的柔性基底，采用厚度为100～200nm的氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜对导电层进行封装，释放拉伸区后，由于SEBS的自粘性，氢化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜随之收缩且不脱落。
作为优选地实施方式，所述封装为用异方导电胶带将所述电极的金手指部分与印刷电路板上的通道一一对应连接，形成稳定的导电通路。
在本发明的技术方案中，所述高密度为感应点的密度大于等于1个/mm 2；所述超窄为电极的通道宽度小于等于50微米。
又一方面，本发明提供上述制备方法得到的多通道高密度的超窄可拉伸微电极。
又一方面，本发明提供上述超窄可拉伸微电极在制备采集生理电信号的设备中的应用或在采集生理电信号中的应用。
上述技术方案具有如下优点或者有益效果：
本发明利用柔性基底的柔软特性，对柔性高聚物的预拉伸行为引入到电极的制备过程中，将电极图案制备到尺寸放大的基底上然后释放回缩最终实现电极的微型化以及可拉伸性。本发明通过拉伸改变柔性基底的大小最终制备得到了多通道高密度的超窄可拉伸微电极，适用于人工操作以及机械化大批量生产。本发明制备出的多通道高密度的超窄可拉伸微电极通过生理电信号的采集实验，不仅成功采集了细胞的生理电信号，而且实现了老鼠皮下肌膜外的肌电信号的采集，且采集的数据具有较高的可靠性。同时，本发明提供的多通道高密度的超窄可拉伸微电极对神经细胞以及老鼠组织进行了一系列的电刺激，成功实现了不同通道间的刺激与记录同时进行，即部分通道给予刺激信号，其他通道采集刺激信号。本发明提供的电极不管是电极图案样式的变更，还是电极尺寸的变更，对柔性可拉伸电极的制备提供新思路。
相对于现有技术，本发明具备以下优点：
(1)本发明提供的制备方法结合微裂纹金膜技术与柔性基底的预拉伸尺寸放大，不仅可以将电极制备成多通道高密度的超窄电极(宽度10微米)，还保证电极良好的拉伸性能以及循环稳定性能；
(2)本发明提供的制备方法利用柔性基底的尺寸放大，使其放大后释放后的导电层封装层不滑脱不移位，并且使电极的感应点区域暴露清晰不遮挡，并能适应释放后尺寸的变化，降低制备超窄电极过程中感应点面积暴露过大的难点，从而实现了超窄的电极通路(宽度10微米)，并且暴露的感应点的面积也是同样尺寸级别的(10微米×10微米)；
(3)本发明在制备流程上更加简单，成功率高，且电极的效率也更高，本发明无需光刻设备的参与，相应地降低了制备成本。
附图说明
图1是本发明实施例1中多通道高密度的超窄可拉伸微电极的制备流程图。
图2是本发明实施例1制备出的32通道高密度的超窄可拉伸微电极的实物 图。
具体实施方式
下述实施例仅仅是本发明的一部分实施例，而不是全部的实施例。因此，以下提供的本发明实施例中的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明的实施例，本领域技术人员在没有作出创造性劳动的前提下所获得的所有其他实施例，都属于本发明的保护范围。
在本发明中，若非特指，所有的设备和原料等均可从市场购得或是本行业常用的。下述实施例中的方法，如无特别说明，均为本领域的常规方法。
实施例1：
本实施例制备了32通道的高密度超窄可拉伸微电极，制备方法如图1所示，具体包括如下步骤：
(1)制备柔性基底：将质量百分数为15％的SEBS甲苯溶液倒入方形的聚四氟乙烯(PTFE)模具中，风干后得到厚度约为300微米的SEBS薄膜，该SEBS薄膜朝向模具内底部的一面具有模具的倒模形态，为雾状不完全平整状态，记为背面，另一面为自然风干后的平整形态，具有较强的粘性和自粘性质，记为正面；
(2)柔性基底的预拉伸以及固定：用胶带将柔性基底背面粘贴固定，记为固定区；对柔性基底进行预拉伸，拉伸过程中固定区不发生形变，而拉伸形变区域的大小由初始1单位长度×1单位长度拉伸为3单位长度×2单位长度，将形变后的柔性基底固定，防止其形状回缩；
(3)制备导电层：在拉伸放大后的柔性基底的平整的一面上放置与放大后的柔性基底尺寸匹配的掩模版，通过磁控溅射法制备具有特殊图案设计的金导电层；
(4)导电层封装以及释放：本实施例采用氢化苯乙烯-丁二烯嵌段共聚物 (SEBS)薄膜作为导电层的封装层材料；将质量分数为5％的氢化苯乙烯-丁二烯嵌段共聚物(SEBS)的甲苯溶液滴于水面上，得到厚度为100nm的薄膜；用铜丝遮挡电极线路中的感应区域，用纸板遮挡电极线路中与印刷电路板(PCB)连接的部分，将SEBS薄膜贴附于导电层上，几分钟之后，去掉遮挡的铜丝和纸板，完成导电层的封装；之后，释放步骤(2)中的固定，柔性基底的形变区域回缩，SEBS薄膜封装随之收缩，且因为粘性不发生脱落；
(5)电极封装：使用异方导电胶带将电极的金手指部分与印刷电路板上的通道一一对应连接，形成稳定的导电通路。
本实施例制备的32通道微电极的实物图见图2，其感应点密度为3个/0.01mm 2；通道宽度为10微米。
本实施例利用制备的32通道微电极进行了生理电信号的采集实验，不仅成功地对细胞的生理电信号进行了采集，也对老鼠皮下肌膜外的肌电信号进行了采集，并且都得到了可靠的数据。本实施例利用制备的32通道微电极对神经细胞以及老鼠组织进行了一系列的电刺激，成功实现了不同通道间的刺激与记录同时进行，即部分通道给予刺激信号，其他通道采集刺激信号。
以上所述仅是本发明的优选实施方式，应当指出：对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (14)

  1. 一种多通道高密度的超窄可拉伸微电极的制备方法，其特征在于，包括如下步骤：
    提供一柔性基底；所述柔性基底包括拉伸区和固定区；对所述拉伸区进行拉伸放大处理；通过掩模版对拉伸放大处理后的柔性基底进行图案溅射制备导电层；释放所述拉伸区使其回缩；封装后即得到所述多通道高密度超窄可拉伸微电极。
  2. 根据权利要求1所述的制备方法，其特征在于，所述拉伸区进行拉伸放大处理中，所述固定区通过粘贴固定。
  3. 根据权利要求1所述的制备方法，其特征在于，所述拉伸区进行拉伸放大处理中，横向或纵向的放大率不超过所述柔性基底的断裂拉伸率。
  4. 根据权利要求1所述的制备方法，其特征在于，所述通过掩模版对拉伸放大处理后的柔性基底进行图案溅射为对拉伸放大处理后的柔性基底的具有粘性的面进行图案溅射。
  5. 根据权利要求4所述的制备方法，其特征在于，所述通过掩模版对拉伸放大处理后的柔性基底进行图案溅射为对拉伸放大处理后的柔性基底的平整的面进行图案溅射。
  6. 根据权利要求1所述的制备方法，其特征在于，所述图案溅射为磁控溅射。
  7. 根据权利要求1所述的制备方法，其特征在于，所述导电层为金导电层。
  8. 根据权利要求1所述的制备方法，其特征在于，所述通过掩模版对拉伸放大处理后的柔性基底进行图案溅射中，所述掩模版的尺寸与所述拉伸放大处理后的柔性基底的尺寸相匹配。
  9. 根据权利要求1所述的制备方法，其特征在于，还包括导电层封装的步骤，所述导电层封装的步骤为：暴露出所述导电层中需要封装的电极线路区域，对其进行封装。
  10. 根据权利要求9所述的制备方法，其特征在于，所述导电层封装为用氢 化苯乙烯-丁二烯嵌段共聚物(SEBS)薄膜封装。
  11. 根据权利要求1所述的制备方法，其特征在于，所述柔性基底为具有粘性的可拉伸回弹柔性基底，选自弹性高分子聚合物材料中的任意一种或多种；优选为氢化苯乙烯-丁二烯嵌段共聚物柔性基底。
  12. 根据权利要求1所述的制备方法，其特征在于，所述封装为用异方导电胶带将所述电极的金手指部分与印刷电路板上的通道一一对应连接，形成稳定的导电通路。
  13. 权利要求1-12任一所述的制备方法得到的多通道高密度的超窄可拉伸微电极。
  14. 权利要求13所述的超窄可拉伸微电极在制备采集生理电信号的设备中的应用或在采集生理电信号中的应用。
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Publication number Priority date Publication date Assignee Title
CN102544052A (zh) * 2012-03-08 2012-07-04 中国科学院深圳先进技术研究院 柔性颅内皮层微电极芯片及其制备和封装方法及封装结构
CN106847688A (zh) * 2017-01-11 2017-06-13 北京大学 一种基于双轴预拉伸的可拉伸电极制备方法
CN109381182A (zh) * 2018-10-11 2019-02-26 北京印刷学院 一种柔性可拉伸生物传感器及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102544052A (zh) * 2012-03-08 2012-07-04 中国科学院深圳先进技术研究院 柔性颅内皮层微电极芯片及其制备和封装方法及封装结构
CN106847688A (zh) * 2017-01-11 2017-06-13 北京大学 一种基于双轴预拉伸的可拉伸电极制备方法
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