CN114098746B - Ultra-narrow high-density multi-relative independent-channel flexible electrode and preparation method and application thereof - Google Patents
Ultra-narrow high-density multi-relative independent-channel flexible electrode and preparation method and application thereof Download PDFInfo
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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
- A61B5/279—Bioelectric electrodes therefor specially adapted for particular uses
- A61B5/294—Bioelectric electrodes therefor specially adapted for particular uses for nerve conduction study [NCS]
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- A—HUMAN NECESSITIES
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- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/12—Manufacturing methods specially adapted for producing sensors for in-vivo measurements
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- A61B2562/12—Manufacturing methods specially adapted for producing sensors for in-vivo measurements
- A61B2562/125—Manufacturing methods specially adapted for producing sensors for in-vivo measurements characterised by the manufacture of electrodes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/16—Details of sensor housings or probes; Details of structural supports for sensors
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B2562/00—Details of sensors; Constructional details of sensor housings or probes; Accessories for sensors
- A61B2562/16—Details of sensor housings or probes; Details of structural supports for sensors
- A61B2562/164—Details of sensor housings or probes; Details of structural supports for sensors the sensor is mounted in or on a conformable substrate or carrier
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Abstract
A flexible electrode with ultra-narrow high-density multiple relatively independent channels, a preparation method and application thereof belong to the technical field of sensors. The method comprises the following steps: (1) spin coating a sacrificial layer on a wafer silicon wafer, and drying to form a film; (2) spin-coating the elastomer solution and drying; (3) After a mask plate is attached to a flexible substrate, sputtering or evaporating a metal conductive film to obtain a flexible electrode with a conductive path; (4) Covering metal films at two ends of the electrode, uniformly spin-coating the elastic body solution diluent on an uncovered area, and drying or drying the diluent to form a film and then attaching the film on the surface of the electrode; (5) Cutting the electrode, releasing the electrode from the wafer silicon wafer, and cutting off the redundant substrate at one end for detection to prepare the ultra-narrow high-density flexible electrode with multiple relatively independent channels. The flexible electrode prepared by the invention has good conductivity and high repeatability, the number of channels is large, the detection ends of the channels of the electrode are relatively independent, physiological electric signals at different sites can be detected simultaneously, and the flexible electrode can be attached to a machine body without relative sliding.
Description
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to an ultra-narrow high-density flexible electrode with multiple relatively independent channels, and a preparation method and application thereof.
Background
In recent years, electronic materials are diversified, the types of electronic equipment are rich, and various electronic detection or functional equipment for human bodies also become research hotspots, wherein the detection of specific neuron signals of human bodies is included. The nervous system is the dominant system for regulating the physiological activities of the organism, and action potentials generated by single neurons are basic signals of the neural activities on the cellular scale; the sum of action potentials of a large number of adjacent neurons seen from the tissue level is the local field potential. Nerve tissue is soft, compliant, and subject to continuous microscopic and macroscopic movements, such as the spinal cord and many peripheral nerves are under up to 20% tension during daily activities.
Although the traditional hard implanted electrode has good chemical inertness and electrical conductivity, the traditional hard implanted electrode has poor mobility, low fitting degree with a human body, can not move synchronously with a nervous system, is easy to cause risks of tissue inflammation, necrosis and the like after long-term use, and is damaged or even can not be obtained based on detection signals. When the electrodes are used, physiological electric signals can not be detected in a large range due to the fact that the number of channels is small or the channels are mutually bound, and the detected signal data have certain contingency. Such mechanical mismatch of the hard sensor is unavoidable and often causes tissue damage and neuroinflammation when implanted in the body, and the use of soft electronics as implantable electrodes significantly improves the mechanical fit of the neural interface. While the existing soft electrode can detect physiological electric signals on the premise of conforming to the soft characteristic of the organism, the soft electrode with larger size can only detect the local potential of nerve tissue, and further detection of single neuron action potential is difficult to realize. In addition, the limited number of electrodes or mutual constraint among electrode channels can not realize the detection of physiological electric signals of a plurality of areas at the same time. In the closest prior art, patent application 201810209677.4 discloses a flexible stretchable multi-channel convex surface muscle electrode consisting essentially of an array of measuring electrodes, cylindrical pads, mesh substrates, interconnect wires, and a packaging layer. The electrode adopts a convex structure design, the sensing electrode is easier to be in close contact with human skin during testing, and the myoelectric signal can be measured comfortably and noninvasively for a long time. However, the number of the electrode channels is still limited, the detection sites are few, and the physiological electric signals in a large area are difficult to collect. In addition, the single detection electrode has a large size, and cannot accurately measure the physiological electric signal of a specified small area. The invention with the application number 201910418554.6 discloses a preparation method of a flexible array microelectrode. The method combines the flexible substrate with the high-conductivity material by using a soft photoetching coating process to prepare the flexible electrode with the size of less than sub-millimeter. However, the property of the flexible mold is easily changed by using the ionic bonding machine, so that the uncertainty of the electrode performance is enhanced, and the close fit between the conductive material and the flexible mold cannot be ensured. The invention relates to an ultra-narrow high-density multichannel flexible electrode with relatively independent channels, which can realize the multi-site simultaneous acquisition of nerve tissue electric signals on one hand, can realize the detection of specific neuron action potentials and the electric stimulation of a single neuron on the other hand, and can realize the acquisition of fixed-point physiological electric signals of small areas of a human body or the application of electric stimulation so as to assist clinical treatment.
Femtosecond laser cutting technology is mature gradually, and is applied to the medical field, such as eye vision correction and the like. The femtosecond cutting technology is introduced into the preparation of the flexible electrode, on one hand, the femtosecond laser cutting speed is in the femto-second level, and the rapid cutting of the flexible material can be realized; on the other hand, the laser beam can be adjusted, and the electrode with a specific shape can be cut through a set program to realize electrode patterning. In addition, the laser cutting accuracy is high, and the width of the cutting mark can be as low as 10 micrometers, so that the electrode with the width of tens of micrometers can be precisely cut, and the repeatability is high. According to the invention, a femtosecond cutting technology is introduced into flexible electrode processing, and the ultra-narrow high-density multi-relative independent channel flexible electrode can be rapidly prepared by changing preset power, cutting track and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide an ultra-narrow high-density flexible electrode with multiple relatively independent channels, and a preparation method and application thereof. The ultra-narrow high-density multi-relative independent channel flexible electrode prepared by the method has the characteristics of simple experimental process, low cost, convenience for large-scale production and the like.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized by comprising the following steps of:
(1) Spin-coating a sacrificial layer on the surface of a wafer silicon wafer, and drying to form a film;
(2) Spin-coating a layer of elastomer solution, and drying to obtain a flexible substrate;
(3) After a mask plate is attached to the flexible substrate obtained in the step (2), placing the flexible substrate into a magnetron sputtering or evaporation device for sputtering or evaporating a metal conductive film to obtain a flexible electrode with a conductive path; the flexible electrode realizes conductive patterning, and the mask plate is used for realizing local deposition of metal, so that the electrode with a specific shape is obtained. Wherein, two ends of the non-spin-coated elastomer solution are respectively used as a signal detection end and an electric signal transmission end;
(4) Covering the metal films at the two ends of the flexible electrode obtained in the step (3), uniformly spin-coating the elastomer solution diluent on the uncovered areas except the covering, removing the covering layer, and drying to obtain the flexible electrode with the insulating layer;
or spin-coating a sacrificial layer on a silicon wafer, spin-coating a layer of elastomer solution diluent, drying and releasing to obtain a film, and self-adhering the film on a substrate of the flexible electrode with a conductive path to obtain the flexible electrode with an insulating layer;
(5) Cutting the flexible electrode obtained in the step (4) by using a femtosecond laser cutting machine, releasing the flexible electrode from a wafer silicon wafer, cutting off an excessive substrate at one end for detection, and preparing the flexible electrode with ultra-narrow high-density multiple relatively independent channels, wherein the detection end of the electrode is relatively independent.
The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized in that the sacrificial layer in the step (1) is easy to dissolve in water, and the sacrificial layer comprises poly (4-sodium styrene sulfonate) aqueous solution.
The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized in that the elastomer solution in the step (2) comprises PDMS or SEBS-toluene solution, and the concentration of the SEBS-toluene solution is 15-30wt%.
The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized in that the mask plate in the step (3) covers the edges and the middle rectangular area is exposed.
The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized in that the elastomer solution diluent in the step (4) comprises PDMS diluent or SEBS diluent, and the dilution ratio of the elastomer solution diluent to the solvent is 10-30:1.
The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized in that the cutting direction in the step (5) is the direction perpendicular to the exposed metal films at the two ends of the flexible electrode, the cutting position is the direction from the outer side of one exposed metal film to the outer side of the other exposed metal film, and the whole metal film and the flexible substrate under the metal film are cut.
The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized by comprising the following specific steps of: placing the cut electrode in a glass container filled with deionized water, and standing until the sacrificial layer is completely dissolved, namely separating the electrode from the wafer silicon wafer.
A flexible electrode with ultra-narrow high density and multiple relatively independent channels prepared by any one of the preparation methods.
A battery comprising the ultra-narrow high density multi-relative independent channel flexible electrode.
The application of the ultra-narrow high-density multi-relative independent channel flexible electrode in the multi-site simultaneous acquisition of nerve tissue electrical signals.
The method for preparing the ultra-narrow high-density multi-relative independent channel flexible electrode by using the femtosecond laser cutting technology has the characteristics of simple preparation steps, less time consumption, low cost, environmental friendliness, high repeatability and the like. The specific expression is as follows: (1) PSS (poly (4-sodium styrene sulfonate) aqueous solution) has good hydrophilicity, and the PSS can be used as a hydrophilic sacrificial layer to completely separate the ultra-narrow high-density multi-relative independent channel flexible electrode from a wafer silicon wafer; (2) The size of a single electrode channel is smaller, so that electrophysiological signal detection and selective electrical stimulation of a single neuron can be realized; (3) The femtosecond laser cutting technology can cut thousands of channel electrodes in a short time, the electrodes are mutually independent, and physiological electric signals of different sites can be detected in a large area at the same time; (4) The electrode has small size, softness, stretchability, simple structure and good driven performance, and can reduce side effects on tissues caused by implantation.
Compared with the prior art, the invention has the following beneficial effects:
1. The invention applies the femtosecond laser cutting technology to the preparation of the ultra-narrow high-density multi-independent-channel flexible electrode, the prepared flexible electrode has good conductivity and high repeatability, the number of channels can reach thousands, the channels of the electrode are independent relatively, physiological electric signals of different sites in a large area can be detected simultaneously theoretically, the size of a single channel of the flexible electrode is smaller, the size of the single channel of the flexible electrode can reach a micron level, and the action potential of certain single neurons can be detected theoretically. The electrode has small size, softness, stretchability, simple and flexible structure, can be well attached to tissues theoretically without generating relative slippage, and can reduce side effects on the tissues caused by implantation.
2. The preparation scheme of the ultra-narrow high-density multi-relative independent channel flexible electrode has the characteristics of less time consumption, high electrode precision, controllable and adjustable engineering parameters, simple experimental process, low cost, convenience for large-scale mass production and the like.
Drawings
FIG. 1 is a schematic front view and cross-sectional view of an ultra-narrow high density multi-relatively independent channel flexible electrode structure;
FIG. 2 is an SEM image of an ultra-narrow high density multi-relatively independent channel flexible electrode.
Detailed Description
The invention will be further illustrated by the following figures and examples.
Example 1:
The specific experimental scheme is as follows:
(1) SEBS-toluene solution with specific concentration is prepared for standby, and the concentration of SEBS-toluene solution is usually 15% (wt%) to 30% (wt%).
(2) And uniformly coating the poly (4-sodium styrene sulfonate) (PSS) -aqueous solution on a commercial wafer silicon wafer, drying the commercial wafer silicon wafer, and processing the commercial wafer silicon wafer into the hydrophilic material.
(3) And (3) uniformly spin-coating the SEBS-toluene solution on the wafer silicon wafer processed in the step (2), and standing until toluene is completely volatilized.
(4) Covering a mask plate (covering the edges and exposing the middle rectangular area) on the flexible substrate prepared in the step (3), and sputtering a metal film in a magnetron sputtering device to obtain the flexible electrode with stable conduction.
(5) And (3) covering two ends (a group of opposite sides of the rectangular area) of the rectangular gold film part of the flexible electrode in the step (4) with a mask plate, uniformly spin-coating PDMS diluent on the uncovered area, and taking down the mask plate after drying to finish the encapsulation of the flexible electrode.
(6) And (3) cutting the packaged flexible electrode prepared in the step (5) into an ultra-narrow high-density multi-relative independent channel flexible electrode by using a femtosecond laser cutting technology, wherein the cutting direction is perpendicular to the exposed two sections of gold films, and the cutting position is from the outer side of one exposed gold film to the outer side of the other exposed gold film, namely, the gold film and the flexible substrate under the gold film are ensured to be completely cut into strips, as shown in figures 1 and 2.
(7) Placing the electrode prepared in the step (6) in a glass container filled with deionized water, standing for 1h until PSS is completely dissolved, and separating the flexible electrode from the silicon wafer. This process is only hydrophilic dissolution of PSS and does not destroy the integrity of the electrode.
(8) And (3) fishing out the flexible electrode obtained in the step (7) from deionized water, cutting along a cutting frame shown by a dotted line in fig. 1, namely cutting off redundant flexible substrates outside the dotted line, so as to prepare the ultra-narrow high-density multi-independent-channel flexible electrode with mutually independent signal channels (including detection ends), wherein redundant flexible substrates are reserved at the signal transmission ports and are not completely dispersed, and therefore the space distance of the multi-channel electrode is ensured (the whole electrode is similar to a fringe shape).
Claims (8)
1. The preparation method of the ultra-narrow high-density multi-relative independent-channel flexible electrode is characterized by comprising the following steps of:
(1) Spin-coating a sacrificial layer on the surface of a wafer silicon wafer, and drying to form a film;
(2) Spin-coating a layer of elastomer solution, and drying to obtain a flexible substrate;
(3) After a mask plate is attached to the flexible substrate obtained in the step (2), placing the flexible substrate into a magnetron sputtering or evaporation device for sputtering or evaporating a metal conductive film to obtain a flexible electrode with a conductive path;
(4) Covering the metal films at the two ends of the flexible electrode obtained in the step (3), uniformly spin-coating the elastomer solution diluent on the uncovered areas except the covering, removing the covering layer, and drying to obtain the flexible electrode with the insulating layer;
or spin-coating a sacrificial layer on a silicon wafer, spin-coating a layer of elastomer solution diluent, drying and releasing to obtain a film, and self-adhering the film on a substrate of the flexible electrode with a conductive path to obtain the flexible electrode with an insulating layer;
(5) Cutting the flexible electrode obtained in the step (4) by using a femtosecond laser cutting machine, releasing the flexible electrode from a wafer silicon wafer, and cutting off an excessive substrate at one end for detection to prepare an ultra-narrow high-density flexible electrode with multiple relatively independent channels;
the sacrificial layer is poly (4-sodium styrene sulfonate) aqueous solution;
The elastomer solution in the step (2) is PDMS or SEBS-toluene solution;
The elastomer solution diluent in the step (4) comprises PDMS diluent or SEBS diluent;
The specific step of releasing the electrode cut in the step (5) from the wafer silicon wafer is as follows: placing the cut electrode in a glass container filled with deionized water, and standing until the sacrificial layer is completely dissolved, namely separating the electrode from the wafer silicon wafer;
The cutting direction is perpendicular to the direction of the exposed metal films at the two ends of the flexible electrode, the cutting position is that the exposed metal film at one end is directly cut to the outer side of the other exposed metal film, and the whole metal film and the flexible substrate under the metal film are cut; the excess flexible substrate remains at the signal transmission port.
2. The method of claim 1, wherein the sacrificial layer in step (1) is readily soluble in water.
3. The method for preparing an ultra-narrow high density multi-relatively independent channel flexible electrode according to claim 1, wherein the concentration of said SEBS-toluene solution in said step (2) is 15-30wt%.
4. The method for preparing the ultra-narrow high-density multi-relative independent channel flexible electrode according to claim 1, wherein the mask plate in the step (3) covers the edges and the middle rectangular area is exposed.
5. The method of claim 1, wherein the dilution ratio of the elastomer solution diluent in the step (4) is 10-30:1.
6. An ultra-narrow high density multi-relatively independent channel flexible electrode made by the method of any one of claims 1-5.
7. A battery comprising the ultra-narrow high density multi-relatively independent channel flexible electrode of claim 6.
8. Use of the ultra-narrow high density multi-relatively independent channel flexible electrode of claim 6 for simultaneous multi-site acquisition of electrical signals from nerve tissue.
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| PCT/CN2021/137595 WO2023065496A1 (en) | 2021-10-18 | 2021-12-13 | Ultra-narrow, high-density flexible electrode having multiple independent channels, preparation method therefor, and use thereof |
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| CN111006801A (en) * | 2019-12-17 | 2020-04-14 | 华中科技大学 | Flexible variable-mode sensor for physiological information monitoring, application and preparation method |
| CN113185912A (en) * | 2021-03-16 | 2021-07-30 | 浙江大学 | Flexible thermal protection substrate for wearable electronic equipment and preparation method thereof |
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| CN101172184B (en) * | 2007-10-10 | 2010-09-01 | 中国科学院上海微系统与信息技术研究所 | Three-dimensional flexible nervus and preparation method |
| CN101149364A (en) * | 2007-11-10 | 2008-03-26 | 大连理工大学 | Water-soluble sacrificial layer micro-flow control chip preparation method |
| CN101912666B (en) * | 2010-08-18 | 2014-12-03 | 中国科学院上海微系统与信息技术研究所 | PDMS-based flexible implanted neural microelectrode and manufacturing method |
| TW201313189A (en) * | 2011-09-30 | 2013-04-01 | Nat Univ Tsing Hua | A flexible micro-electrode and manufacture method thereof |
| CN102920452B (en) * | 2012-11-02 | 2015-02-11 | 上海交通大学 | Graphene-based flexible coronary electrocardio-electrode and preparation method thereof |
| CN103199020B (en) * | 2013-03-05 | 2016-03-16 | 中国科学院上海微系统与信息技术研究所 | Based on preparation method and the detection method of the liquid grid-type graphene field effect pipe of PI |
| US10791946B2 (en) * | 2014-04-03 | 2020-10-06 | The Trustees Of The University Of Pennsylvania | Transparent, flexible, low-noise electrodes for simultaneous electrophysiology and neuro-imaging |
| CN106667475B (en) * | 2016-12-20 | 2019-05-07 | 国家纳米科学中心 | A kind of implanted flexible nervus comb and preparation method thereof and method for implantation |
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| CN111006801A (en) * | 2019-12-17 | 2020-04-14 | 华中科技大学 | Flexible variable-mode sensor for physiological information monitoring, application and preparation method |
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