CN119463465A - Anisotropic paste-like conductive composite material prepared by blending method and preparation method and application thereof - Google Patents
Anisotropic paste-like conductive composite material prepared by blending method and preparation method and application thereof Download PDFInfo
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- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
- A61B5/263—Bioelectric electrodes therefor characterised by the electrode materials
- A61B5/265—Bioelectric electrodes therefor characterised by the electrode materials containing silver or silver chloride
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
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Abstract
The invention belongs to the field of flexible electronic materials, and particularly relates to an anisotropic pasty conductive composite material prepared by a blending method, and a preparation method and application thereof. The paste conductive composite material comprises the following components of a high polymer matrix material, multi-wall carbon nano tubes and silver nano sheets. The polymer matrix material is prepared by heating and reacting polyethylene glycol-polypropylene glycol-polyethylene glycol block copolymer, isophorone diisocyanate and a catalyst at 50-70 ℃ for 10-14 h. The invention also provides a preparation method of the paste electrode material. The paste electrode material can be used for collecting electrophysiological signals on the surfaces of various complex biological tissues, and solves the problems of electrophysiological signal distortion or loss, complicated steps of hair removal and the like in the prior art caused by rough and complex surfaces.
Description
Technical Field
The invention belongs to the field of flexible electronic materials, and particularly relates to an anisotropic pasty conductive composite material prepared by a blending method, and a preparation method and application thereof.
Background
The electrophysiological signals reflect the state of the human body, and a stable human-computer interface is important for improving the precision and accuracy of detecting the physiological signals. With the development of flexible sensors, reliable electrical connection of human-machine interfaces is increasingly required for convenient electrophysiological monitoring devices. To meet the demands of electrophysiological monitoring, a variety of flexible electrodes have been developed. One key feature of these electrodes is the ability to form conformal and seamless contact with animal tissue or skin surfaces. However, in the electrophysiological signal acquisition of a multipage skin surface, such a sufficient electrical connection is often difficult to achieve, e.g. head electroencephalogram (EEG) without shaving hair or non-invasive detection of animal signals, etc.
The paste conductive material has the main function of keeping stable electrical connection for a long time when facing various complex animal tissues or skin surfaces, thereby ensuring that the electrophysiological monitoring equipment can continuously acquire accurate electrophysiological signals. The invention develops a composite paste electrode by mixing a polymer matrix with a conductive nanofiller. The paste electrode may be conformally coated on a smooth or rough surface and have sufficient adhesiveness and a function of collecting an electrophysiological signal.
Disclosure of Invention
In order to solve the above problems, the present invention aims to overcome the adverse effect on the acquisition of electrophysiological signals caused by rough skin or tissue surface morphology, and provide stable electrical connection for human-machine interface to improve the stability and reliability of the electrophysiological monitoring device.
In order to solve the technical problems, the application provides the following technical scheme:
The invention provides an anisotropic paste conductive composite material prepared by a blending method, which comprises a high polymer matrix material, multi-wall carbon nanotubes and silver nano sheets, wherein the high polymer matrix material is prepared by heating and reacting polyethylene glycol-polypropylene glycol-polyethylene glycol block copolymer, isophorone diisocyanate (IPDI) and a catalyst for 10-14h at 50-70 ℃.
Polyethylene glycol the polyethylene glycol block copolymer was purchased from sigma-aldrich under the trade designation 435465.
Preferably, the polyethylene glycol polypropylene glycol polyethylene glycol block copolymer has a number average molecular weight (Mn) of 4000-6000.
Preferably, the catalyst is selected from dibutyltin dilaurate (DBTDL).
Preferably, the multi-walled carbon nanotubes have a diameter of 10-30nm and a length of 10-30 μm.
Preferably, the silver nano-sheet has a sheet diameter of 1-5 μm.
Preferably, the mass ratio of the polymer matrix material to the multiwall carbon nanotubes to the silver nanoplates is 18-22:0.5-1.5:10-14.
Preferably, the ratio of the amounts of the polyethylene glycol polypropylene glycol polyethylene glycol block copolymer and isophorone diisocyanate is 1:1 to 1.1:1 x 10 -4～3*10-4.
The invention also provides a preparation method of the anisotropic paste conductive composite material prepared by the blending method, which comprises the following steps:
S11, after dissolving a polyethylene glycol-polypropylene glycol-polyethylene glycol block copolymer, adding isophorone diisocyanate and a catalyst at room temperature (25+/-5 ℃), and heating at 50-70 ℃ for reaction for 10-14 hours to obtain a reaction solution;
S12, volatilizing a solvent in the reaction solution to obtain a high polymer matrix material;
s13, mixing the polymer matrix material and the multi-wall carbon nano tube for 160-200S to obtain a mixed material;
And S14, adding silver nano sheets into the mixed material, mixing for 160-200S, and then air-drying to obtain the anisotropic pasty conductive composite material prepared by the blending method.
Preferably, in the step S11, the polyethylene glycol polypropylene glycol polyethylene glycol block copolymer is dried under vacuum at 40 ℃ for 1-2 hours for purification before dissolution.
Preferably, in the step S11, the dissolution temperature is 60 ℃, and the method is stirring.
Preferably, the polyethylene glycol polypropylene glycol polyethylene glycol block copolymer is dissolved in chloroform, and the mass ratio of the chloroform to the polyethylene glycol polypropylene glycol polyethylene glycol block copolymer is 2-4:1.
The water washable paste electrode and the preparation method thereof comprise the steps of (a) mixing purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) with isophorone diisocyanate (IPDI) in chloroform solvent, performing polymerization reaction under the action of a catalyst to obtain a paste polymer matrix material, and (b) uniformly mixing the polymer matrix material with multi-wall carbon nano tubes and silver nano sheets by using a planetary mixer, and volatilizing redundant solvent.
Specifically, the preparation method of the anisotropic pasty conductive composite material prepared by the blending method comprises the following steps:
(1) Poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) (average Mn 5800) was vacuum dried at 40 ℃ for 1-2h to give purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol);
(2) Dissolving the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) in a solvent with the mass being 3 times, stirring, heating to 60 ℃ for full dissolution, dropwise adding isophorone diisocyanate (IPDI) and a catalyst at room temperature, wherein the mass ratio of the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) to isophorone diisocyanate (IPDI) is 1:1.03, stirring, heating to 60 ℃ for reaction for 12 hours, cooling, pouring into an evaporation dish, stirring at room temperature in a fume hood for 72 hours, and volatilizing the solvent to obtain the component A.
(3) 20 Parts by mass of component A was added to a PE material mixing tank (30 mL), and then 1 part by mass of multi-arm carbon nanotube was added thereto. And then sealing the mixing tank, and putting the sealed mixing tank into a planetary mixer to be stirred for 180 seconds.
(4) Opening a mixing tank, adding 12 parts by mass of silver nano-sheets into the mixing tank, sealing the mixing tank, and then placing the sealed mixing tank into a planetary mixer to stir for 180 seconds.
(5) And (5) placing the uniformly mixed composite material in a ventilation environment for drying, and then directly taking out for use.
The invention also provides a general type washable paste electrode for electrophysiological signal monitoring, which comprises the anisotropic paste conductive composite material prepared by the blending method.
Compared with the prior art, the technical scheme of the invention has the following advantages:
According to the pasty conductive composite material, the polymer chain segment is increased by further polymerizing the polymer material poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol), so that the crosslinking degree and viscosity of the polymer matrix material are improved, and in addition, a reliable conductive network is constructed by using the one-dimensional and two-dimensional nano conductive fillers, so that the consumption of the nano fillers is effectively reduced, and the excellent electrophysiological signal transmission quality is ensured.
Drawings
FIG. 1 is a graph comparing signal crosstalk between the paste-like composite material of example 1 and a commercial gel material.
Fig. 2 is a graph comparing adhesion performance of the paste composite of example 1 to a commercial gel material and a commercial patch electrode.
Fig. 3 is a photograph of a polymer matrix material.
Fig. 4 is a graph showing viscosity of a polymer matrix material.
Fig. 5 is a flow chart of the preparation of an anisotropic paste conductive composite prepared using a blending method.
FIG. 6 is a graph of loss modulus and storage modulus for the composite material prepared in example 1.
Fig. 7 is a diagram showing the distribution of the conductive filler in the polymer matrix material.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Example 1
An anisotropic paste conductive composite material prepared by a blending method comprises the following steps:
(1) Poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) (average Mn 5800) was dried under vacuum at 40 ℃ for 2h to give purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol);
(2) Dissolving the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) in 3 times of solvent chloroform, stirring, heating to 60 ℃ for full dissolution, dropwise adding isophorone diisocyanate (IPDI) and a catalyst at room temperature of 25 ℃, wherein the mass ratio of the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) to isophorone diisocyanate (IPDI) is 1:1.03:2 x10 -4, stirring, heating to 60 ℃ for reaction 12h, cooling, pouring into an evaporation dish, stirring at room temperature for 72h in a fume hood, volatilizing the solvent, and obtaining a high polymer matrix material;
(3) 10g of the polymer matrix material was charged into a PE material mixing tank (30 mL), and then 0.5g of multi-walled carbon nanotubes was added thereto. Then sealing the mixing tank and then placing the sealed mixing tank into a planetary mixer to be stirred for 180 seconds, wherein the total mass of a counterweight system of the mixer is 500g, the revolution speed of the mixer is 1500r/min, and the rotation speed of the mixer is 1000r/min;
(4) Opening a mixing tank, adding 6g of silver nano-sheets into the mixing tank, sealing the mixing tank, and then placing the sealed mixing tank into a planetary mixer for stirring for 180 seconds, wherein the total mass of a counterweight system of the mixer is 500g, the revolution speed of the mixer is 1500r/min, and the rotation speed of the mixer is 1000r/min;
(5) The mixed composite material is placed in a fume hood for air drying.
Example 2
An anisotropic paste conductive composite material prepared by a blending method comprises the following steps:
(1) Poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) (average Mn 5800) was dried under vacuum at 40 ℃ for 2h to give purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol);
(2) Dissolving the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) in 2-4 times of solvent chloroform, stirring, heating to 60 ℃ for full dissolution, dropwise adding isophorone diisocyanate (IPDI) and a catalyst at room temperature of 25 ℃, wherein the mass ratio of the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) to isophorone diisocyanate (IPDI) is 1:1.03:1 x 10 -4, stirring, heating to 50 ℃ for reaction for 10 hours, cooling, pouring into an evaporation dish, stirring at room temperature for 72 hours in a fume hood, volatilizing the solvent, and obtaining a high polymer matrix material;
(3) 9g of polymer matrix material was added to a PE material mixing tank, and then 0.25g of multi-walled carbon nanotubes were added thereto. The diameter of the multiwall carbon nanotube is 10nm, and the length is 10 mu m;
Then sealing the mixing tank, and putting the sealed mixing tank into a planetary mixer for stirring for 160 seconds, wherein the revolution speed of the mixer is 1500r/min, and the rotation speed of the mixer is 1000r/min;
(4) Opening a mixing tank, adding 5g of silver nano sheets with the sheet diameter of 1 mu m into the mixing tank, sealing the mixing tank, and then placing the sealed mixing tank into a planetary mixer for stirring for 180 seconds, wherein the revolution speed of the mixer is 1500r/min, and the rotation speed of the mixer is 1000r/min;
(5) The mixed composite material is placed in a fume hood for air drying.
Example 3
An anisotropic paste conductive composite material prepared by a blending method comprises the following steps:
(1) Poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) (average Mn 5800) was dried under vacuum at 40 ℃ for 2h to give purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol);
(2) Dissolving the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) in 4 times of solvent chloroform, stirring, heating to 60 ℃ for full dissolution, dropwise adding isophorone diisocyanate (IPDI) and a catalyst at room temperature of 25 ℃, wherein the mass ratio of the purified poly (ethylene glycol) -block-poly (propylene glycol) -block-poly (ethylene glycol) to isophorone diisocyanate (IPDI) is 1:1.03:3 x10 -4, stirring, heating to 70 ℃ for reaction 14h, cooling, pouring into an evaporation dish, stirring at room temperature for 72h in a fume hood, volatilizing the solvent, and obtaining a high polymer matrix material;
(3) 11g of a polymer matrix material was added to a PE material mixing tank, and then 0.75g of multi-walled carbon nanotubes were added thereto. The diameter of the multiwall carbon nanotube is 30nm, and the length is 30 mu m;
Then sealing the mixing tank, and putting the sealed mixing tank into a planetary mixer to be stirred for 200s, wherein the revolution speed of the mixer is 1500r/min, and the rotation speed of the mixer is 1000r/min;
(4) Opening a mixing tank, adding 7g of silver nano sheets with the sheet diameter of 5 mu m into the mixing tank, sealing the mixing tank, and then placing the sealed mixing tank into a planetary mixer for stirring for 180 seconds, wherein the revolution speed of the mixer is 1500r/min, and the rotation speed of the mixer is 1000r/min;
(5) The mixed composite material is placed in a fume hood for air drying.
Application example 1
Two points which are 10cm apart are selected along the axial direction of the arm on the arm, the anisotropic paste conductive composite material prepared in the embodiment 1 of the invention is taken out as a paste electrode and uniformly smeared on the two selected points, a thin copper sheet is used as a receiving electrode to collect human body electromyographic signals (EMG) (note that the thin copper sheet is directly placed on the arm and cannot be collected), and the thin copper sheet is placed on the surface of the paste electrode which is smeared uniformly to be tightly adhered. After the electromyographic signals are collected and recorded, the electromyographic signals are washed by pure water, and then commercial electrode patches (purchased from the Likang HealForce) are attached to the same two positions, and are used for collecting the electromyographic signals under the same action, and the electromyographic signals collected in the two modes have a corresponding signal-to-noise ratio through calculation and comparison.
Application example 2
On the premise of not removing hair, the brain electrical signal of the head position of the human body is monitored. Two points (10-20 cm apart) are selected in the area covering the hair, a proper amount of the paste electrode is uniformly smeared on the two selected points, a thin copper sheet is adopted as a receiving electrode in the same application example 1, the thin copper sheet is placed on the paste electrode for connection, and after signals are collected and recorded, the smeared area is washed by clean water to be removed. Likewise, commercial electrode patches are stuck at the selected two points to monitor brain electrical signals, and the commercial electrode patches cannot monitor the brain electrical signals of He Boduan under the condition that any hair is not removed.
Application example 3
The performance stability of the material is important to the long-term monitoring of electrophysiological signals, and compared with commercial gel with the same function commonly used in the market, the paste electrode provided by the invention has more excellent long-term stability. Specific comparison measures are for example:
(a) The paste electrode material and the commercial gel material are placed in the same environment, the respective mass changes are measured after 24 hours, the mass of the commercial gel is reduced to about 10% of the original mass after the commercial gel is placed for 24 hours due to the water loss of the commercial gel, and the paste electrode mass is hardly changed.
(B) The paste electrode material and the commercial gel material are placed in the same environment, the respective viscosity changes are measured after 24 hours, the commercial gel becomes solid after being placed for 24 hours, and the paste electrode viscosity hardly changes.
Application example 4
The signal crosstalk problem is also an important factor affecting the electrophysiological signal acquisition quality, the skin impedance is measured by adopting metal electrodes with a distance of 2mm, the pasty electrode and the commercial gel material are respectively and uniformly coated between the electrodes and the skin, then the coated strip-shaped copper counter electrode is attached to the skin of an arm to measure the skin impedance of a human body, the two materials are coated on the two metal electrodes separately for the first time, the two materials are coated uniformly in the whole area between the two metal electrodes for the second time (the two metal detection electrodes are connected with each other through the coated pasty electrode or the commercial gel material), and the measured skin impedance is obviously reduced when the whole commercial gel material is coated after test and comparison, so that the signal crosstalk phenomenon caused by short circuit is shown. The paste electrode prepared by the invention has no abnormal phenomenon.
In addition, the adhesive property of the paste electrode material has obvious advantages compared with that of a commercial electrode patch and a commercial gel material, and the paste electrode material can ensure that the electrophysiological detection port is directly pressed on the paste electrode material without falling off and other conditions, so that the output of electrophysiological signals is unstable.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (10)
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Citations (5)
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| US20100140564A1 (en) * | 2006-03-07 | 2010-06-10 | Gerardus Cornelis Overbreek | Conductive ink |
| CN110563920A (en) * | 2019-09-12 | 2019-12-13 | 长春工业大学 | Conductive mixed isocyanate type polyurethane material and preparation method thereof |
| CN111433248A (en) * | 2017-10-04 | 2020-07-17 | 赫尔克里士有限公司 | Elastic and stretchable gel polymer electrolytes |
| CN118165501A (en) * | 2024-03-12 | 2024-06-11 | 暨南大学 | Antibacterial and conductive high-elongation degradable film material and vocal cord sensing application thereof |
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- 2024-11-15 CN CN202411631574.9A patent/CN119463465A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100140564A1 (en) * | 2006-03-07 | 2010-06-10 | Gerardus Cornelis Overbreek | Conductive ink |
| CN101418192A (en) * | 2007-10-24 | 2009-04-29 | 天津大学 | Hydrophilicity hot melt type polyurethane contact adhesive and preparation method and use |
| CN111433248A (en) * | 2017-10-04 | 2020-07-17 | 赫尔克里士有限公司 | Elastic and stretchable gel polymer electrolytes |
| CN110563920A (en) * | 2019-09-12 | 2019-12-13 | 长春工业大学 | Conductive mixed isocyanate type polyurethane material and preparation method thereof |
| CN118165501A (en) * | 2024-03-12 | 2024-06-11 | 暨南大学 | Antibacterial and conductive high-elongation degradable film material and vocal cord sensing application thereof |
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