CN115466544A - Preparation method of flexible electrode by utilizing magnetic induction carbon nano tube arrangement - Google Patents

Preparation method of flexible electrode by utilizing magnetic induction carbon nano tube arrangement Download PDF

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CN115466544A
CN115466544A CN202211145896.3A CN202211145896A CN115466544A CN 115466544 A CN115466544 A CN 115466544A CN 202211145896 A CN202211145896 A CN 202211145896A CN 115466544 A CN115466544 A CN 115466544A
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carbon nano
flexible electrode
preparing
nano tube
conductive ink
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李欣琳
王光伟
丛晨浩
李鸿江
肖焯楠
李山东
张鹏飞
金明亮
肖伟
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Qingdao University
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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    • C09D11/52—Electrically conductive inks
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder

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Abstract

The invention relates to the technical field of conductive carbon paste ink, and discloses a preparation method of a flexible electrode by utilizing magnetic induction carbon nano tube arrangement, which comprises the following steps: s1: adding corresponding dispersing agent into the carbon nano tube aqueous solution, and then adding Fe with different proportions 3 O 4 Solid particles, finally, carrying out ultrasonic treatment on all the solutions at the temperature of 10 ℃, and carrying out centrifugal separation at a fixed rotating speed; s2: under normal temperature and normal pressure, the water absorption solute and water are prepared according to a fixed proportion, stirred for 3 hours at a fixed rotating speed at the ambient temperature of 70 ℃, and finally prepared into the thickening agent of the conductive ink. The invention realizes the highly uniform directional arrangement of the carbon nano tubes at normal temperature and normal pressure, is suitable for preparing the carbon nano tube conductive ink on a large scale, leads the directionally arranged carbon nano tubes to be more compact through normal temperature ultrasonic treatment and vacuum filtration, and improves the mechanical property and the electricity of the carbon nano tube conductive inkAnd (4) performance.

Description

Preparation method of flexible electrode by utilizing magnetic induction carbon nano tube arrangement
Technical Field
The invention relates to the technical field of conductive carbon paste ink, in particular to a preparation method of a flexible electrode by utilizing magnetic induction carbon nano tube arrangement.
Background
Since their appearance in 1991, carbon Nanotubes (CNTs) have attracted considerable attention for their good electrical, thermal and mechanical properties. And the good compatibility of the composite material is always taken as the first choice for forming and researching composite materials, including nano genetic engineering, nano biological engineering, nano medical engineering and the like. CNTs and graphene show great potential applications in industry due to their excellent mechanical, electrical and thermal properties. Unfortunately, neither CNT-and graphene-based macroscopic fibers nor films can retain the superior properties of their respective nanoscale components. For CNT fibers, due to the porous structural nature, 139 researchers found that insertion of graphene sheets into a CNT network can improve electrical and mechanical properties by closing the gaps between adjacent nanotubes. Different methods of hybridizing CNTs and graphene have been tried, including in situ methods such as simultaneous CVD synthesis of CNT/graphene and partial decompression of MWCNT, or ex situ methods such as by solution reaction of non-covalent and covalent bonds.
The arrangement of the carbon nanotubes determines the electrical conductivity thereof, and in order to obtain a carbon nanotube fiber having a good electrical conductivity, the arrangement can be changed to align the carbon nanotubes uniformly, thereby obtaining an excellent electrical conductivity. There are many factors that influence the CNT alignment, such as the degree of dispersion, mechanical stretching, electric field, magnetic field, etc. of the CNTs, and because the magnetic field required to induce the alignment of the multi-walled CNTs is easy to control, the magnetic field induced multi-walled CNTs (MWCNTs) to align in order to prepare conductive ink is a relatively convenient and feasible important method, and the mechanical and electrical properties of the composite material aligned by the magnetic field induced alignment are greatly improved.
According to the current research, iron oxide is the first choice among magnetic materials formed with carbon nanotubes, and the iron oxide is characterized by low price and excellent magnetic property, and related CNT @ Fe 3 O 4 Related studies such as induction of apoptosis in chronic myelogenous leukemia, glucose biofuel cell, lithium storage performance container, etc. have been confirmed with CNT @ Fe 3 O 4 The composite material has good performance. When trying to achieve high electrical and physical properties, it is preferred to arrange the nano-or micro-fibril elements in a macroscopic material. For example, unidirectional carbon fiber reinforced composites have higher tensile strength in the direction of fiber alignment. For carbon nanotube composites, good CNT dispersion (no aggregation) in a polymer matrix with preferential alignment directions can result in mechanical properties several times higher than their counterparts with aggregated and random CNT distribution.
Disclosure of Invention
The present invention is directed to a method for preparing a flexible electrode using magnetic induction of carbon nanotube alignment, which solves the problems of the background art mentioned above.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a flexible electrode using magnetic induction carbon nanotube arrangement comprises the following steps:
s1: adding corresponding dispersing agent into the carbon nano tube aqueous solution, and then adding Fe with different proportions 3 O 4 Solid particles, finally, carrying out ultrasonic treatment on all the solutions at the temperature of 10 ℃, and carrying out centrifugal separation at a fixed rotating speed;
s2: under normal temperature and normal pressure, preparing a water absorption solute and water according to a fixed proportion, stirring for 3 hours at a fixed rotating speed at an ambient temperature of 70 ℃, and finally preparing a thickener of the conductive ink;
s3: mixing carbon nanotubes with Fe 3 O 4 The composite solution and the thickening agent are mixed according to different proportions at normal temperatureGrinding and stirring the mixture in a grinding bowl for 10 minutes until the mixture is uniform, and finally obtaining the conductive ink of the composite material;
s4: placing the conductive ink obtained in the step S3 on a die, and directly scraping the conductive ink by using a magnetic scraper with magnetic force to prepare a flexible electrode in which the carbon nano tubes are arranged by utilizing magnetic induction;
s5: and repeating the step S4.
Preferably, fe in step S1 3 O 4 The particle size of the solid particles is 20 to 30nm.
Preferably, the dispersant in the step S1 includes one or more of acetone, ethanol and ethyl acetate.
Preferably, the water-absorbing solute in the step S2 includes one or more of polyethylene oxide and methyl cellulose.
Preferably, the concentration of the carbon nanotube aqueous solution in the step S1 is 0.4% -1.0%, and the concentration unit is wt/vol.
Preferably, the concentration of the thickener solution prepared in the S2 step is 7-12%, and the concentration unit is wt/vol.
Preferably, the blade coating time in the S4 step is 1mm/S.
Preferably, the number of repetitions in step S5 is 2~3.
The invention provides a preparation method of a flexible electrode by utilizing magnetic induction carbon nano tube arrangement. The preparation method of the flexible electrode by utilizing magnetic induction carbon nanotube arrangement has the following beneficial effects:
(1) The method realizes the highly uniform directional arrangement of the carbon nanotubes at normal temperature and normal pressure, is suitable for large-scale preparation of the carbon nanotube conductive ink, and leads the directionally arranged carbon nanotubes to be more compact through normal-temperature ultrasonic treatment and vacuum filtration, thereby improving the mechanical property and the electrical property of the carbon nanotube conductive ink.
(2) The dispersant and the thickener used in the invention do not damage the conductivity of the carbon nanotube conductive ink too high, and the compatibility of mechanical property and electrical property is realized.
(3) The conductive ink prepared by the invention can be printed on various flexible bases or non-flexible substrates, different ink proportions and thickener proportions are configured according to different substrate requirements, and the expansibility is extremely high.
(4) The scheme of the invention has low cost, is easier to realize large-scale preparation compared with the existing method, and is more suitable for preparing products such as carbon-based chips, light-emitting diodes, flexible wearable sensing equipment, solar energy or battery electrodes and the like.
Drawings
FIG. 1 is a schematic view of a blade coating test in a method for manufacturing a flexible electrode using magnetically induced carbon nanotube alignment according to the present invention;
FIG. 2 is a schematic SEM image of aligned carbon nanotubes without magnetic blade coating in a method for preparing a flexible electrode using magnetically induced carbon nanotube alignment according to the present invention;
FIG. 3 is a SEM image of aligned carbon nanotubes coated with magnetic knife in the method for preparing a flexible electrode using magnetically induced carbon nanotube alignment of the present invention;
FIG. 4 is a schematic diagram of an X-ray diffraction spectrum of the composite material in a method for manufacturing a flexible electrode using magnetically induced carbon nanotube alignment according to the present invention.
Detailed Description
As shown in fig. 1-4:
example 1: a preparation method of a flexible electrode using magnetic induction carbon nanotube arrangement comprises the following steps:
s1: weighing 0.5g of multi-walled carbon nanotube, adding the multi-walled carbon nanotube into 100ml of distilled water in a 500ml beaker to obtain a carbon nanotube aqueous solution with the concentration of 0.5 percent (wt/vol), then adding 0.5g of sodium polystyrene sulfonate for dispersing polymer particles and clustered carbon nanotube structures, and then adding 1.5g of Fe with the particle size of 20-30nm 3 O 4 Uniformly mixing the particles with the carbon nano tube aqueous solution, ultrasonically dispersing the carbon nano tube aqueous solution, adding the dispersed mixed solution into a centrifugal tube, centrifuging for 30min at 10000 rpm, and taking supernatant liquid to obtain supernatant liquid;
s2: weighing 8g of polyoxyethylene powder, adding the polyoxyethylene powder into 100ml of distilled water in a 500ml beaker to obtain 8% (wt/vol) polyoxyethylene aqueous solution, and stirring the polyoxyethylene aqueous solution at the temperature of 70 ℃ for 3 hours at a fixed rotating speed of 200rmp/min to prepare a thickening agent of the conductive ink;
s3: mixing the carbon nanotubes with Fe 3 O 4 The composite solution and the thickening agent are placed in a grinding bowl according to the proportion of 1.5 at normal temperature, and are ground and stirred for 10 minutes until the mixture is uniform, so that the conductive ink of the composite material is obtained;
s4: placing the conductive ink on a die, directly scraping the conductive ink by using a magnetic scraper with magnetic force, and controlling the scraping speed to be 1mm/s to obtain the flexible electrode arranged by utilizing the magnetic induction carbon nano tubes;
s5: repeat S4 step 2~3 times.
Example 2
A preparation method of a flexible electrode using magnetic induction carbon nanotube arrangement comprises the following steps:
s1: weighing 0.8g of multi-walled carbon nanotube, adding the multi-walled carbon nanotube into 100ml of distilled water in a 500ml beaker to obtain a carbon nanotube aqueous solution with the concentration of 0.8% (wt/vol), then adding 0.8g of sodium polystyrene sulfonate for dispersing polymer particles and clustered carbon nanotube structures, and then adding 1.5g of Fe with the particle size of 20-30nm 3 O 4 Uniformly mixing the particles with the carbon nano tube aqueous solution, performing ultrasonic dispersion on the carbon nano tube aqueous solution, adding the dispersed mixed solution into a centrifugal tube, centrifuging the mixture at 10000 rpm for 30min, and taking supernatant liquid to obtain supernatant liquid;
s2: weighing 8 parts of polyvinyl butyral powder, adding the polyvinyl butyral powder into 50ml of diethylene glycol butyl ether in a 500ml beaker to obtain a polyvinyl butyral solution with the concentration of 16% (wt/vol), and stirring the polyvinyl butyral solution at the temperature of 70 ℃ for 3 hours at a fixed rotating speed of 200rmp/min to prepare a thickening agent of the conductive ink;
s3: mixing the carbon nanotubes with Fe 3 O 4 The composite solution and the thickening agent are put in a grinding bowl according to the proportion of 1.5 at normal temperature, and are ground and stirred for 10 minutes until the mixture is uniform, and the conductive ink of the composite material is obtained;
s4: and (3) placing the conductive ink on a mould, directly carrying out blade coating on the conductive ink by using a magnetic scraper with magnetic force, and controlling the blade coating speed to be 1mm/s to obtain the flexible electrode utilizing the magnetic induction carbon nano tube arrangement.
Comparative example 1
A preparation method of a flexible electrode using magnetic induction carbon nanotube arrangement comprises the following steps:
s1: weighing 1.5g of multi-walled carbon nanotubes, adding the multi-walled carbon nanotubes into 100ml of distilled water in a 500ml beaker to obtain a 1.5% (wt/vol) carbon nanotube aqueous solution, then adding 1.5g of sodium polystyrene sulfonate for dispersing polymer particles and cluster-shaped carbon nanotube structures, and then adding 1.5g of Fe with the particle size of 20-30nm 3 O 4 Uniformly mixing the particles with the carbon nano tube aqueous solution, ultrasonically dispersing the carbon nano tube aqueous solution, adding the dispersed mixed solution into a centrifugal tube, centrifuging for 30min at 10000 rpm, and taking supernatant liquid to obtain supernatant liquid;
s2: weighing 8g of polyoxyethylene powder, adding the polyoxyethylene powder into 100ml of distilled water in a 500ml beaker to obtain 8% (wt/vol) polyoxyethylene aqueous solution, and stirring the polyoxyethylene aqueous solution at the temperature of 70 ℃ for 3 hours at a fixed rotating speed of 200rmp/min to prepare a thickening agent of the conductive ink;
s3: mixing the carbon nanotubes with Fe 3 O 4 The composite solution and the thickening agent are put in a grinding bowl according to the proportion of 1.5 at normal temperature, and are ground and stirred for 10 minutes until the mixture is uniform, and the conductive ink of the composite material is obtained;
s4: and (3) placing the conductive ink on a mould, directly carrying out blade coating on the conductive ink by using a magnetic scraper with magnetic force, and controlling the blade coating speed to be 1mm/s to obtain the flexible electrode utilizing the magnetic induction carbon nano tube arrangement.
Comparative example 2
A preparation method of a flexible electrode using magnetic induction carbon nanotube arrangement comprises the following steps:
s1: 0.5g of multi-walled carbon nanotubes are weighed and added into 100ml of distilled water in a 500ml beaker to obtain a 0.5% (wt/vol) concentration aqueous solution of carbon nanotubes, and then 0.5g of sodium polystyrene sulfonate is added for useDispersing polymer particles and clustered carbon nanotube structure, and adding 2.5g of Fe with particle diameter of 20-30nm 3 O 4 Uniformly mixing the particles with the carbon nano tube aqueous solution, ultrasonically dispersing the carbon nano tube aqueous solution, adding the dispersed mixed solution into a centrifugal tube, centrifuging for 30min at 10000 rpm, and taking supernatant liquid to obtain supernatant liquid;
s2: weighing 8g of polyoxyethylene powder, adding the polyoxyethylene powder into 100ml of distilled water in a 500ml beaker to obtain 8% (wt/vol) polyoxyethylene aqueous solution, and stirring the polyoxyethylene aqueous solution at the temperature of 70 ℃ for 3 hours at a fixed rotating speed of 200rmp/min to prepare a thickening agent of the conductive ink;
s3, mixing the carbon nano tube with Fe 3 O 4 The composite solution and the thickening agent are put in a grinding bowl according to the proportion of 1.5 at normal temperature, and are ground and stirred for 10 minutes until the mixture is uniform, and the conductive ink of the composite material is obtained;
s4: and (3) placing the conductive ink on a mould, directly scraping the conductive ink by using a magnetic scraper with magnetic force, and controlling the scraping speed to be 1mm/s to obtain the flexible electrode arranged by utilizing the magnetic induction carbon nano tubes.
Comparative example 3
A preparation method of a flexible electrode using magnetic induction carbon nanotube arrangement comprises the following steps:
s1: weighing 0.5g of multi-walled carbon nanotube, adding the multi-walled carbon nanotube into 100ml of distilled water in a 500ml beaker to obtain a carbon nanotube aqueous solution with the concentration of 0.5 percent (wt/vol), then adding 0.5g of sodium polystyrene sulfonate for dispersing polymer particles and clustered carbon nanotube structures, and then adding 1.5g of Fe with the particle size of 20-30nm 3 O 4 Uniformly mixing the particles with the carbon nano tube aqueous solution, ultrasonically dispersing the carbon nano tube aqueous solution, adding the dispersed mixed solution into a centrifugal tube, centrifuging for 30min at 10000 rpm, and taking supernatant liquid to obtain supernatant liquid;
s2: weighing 8g of polyoxyethylene powder, adding the polyoxyethylene powder into 100ml of distilled water in a 500ml beaker to obtain 8% (wt/vol) polyoxyethylene aqueous solution, and stirring the polyoxyethylene aqueous solution at the temperature of 70 ℃ for 3 hours at a fixed rotating speed of 200rmp/min to prepare a thickening agent of the conductive ink;
s3: placing the composite solution of the carbon nanotubes and the Fe3O4 and the thickening agent in a grinding bowl according to the proportion of 1.5 at normal temperature, grinding and stirring for 10 minutes until the mixture is uniformly mixed, and obtaining the conductive ink of the composite material;
s4: and (3) placing the conductive ink on a mould, directly carrying out blade coating on the conductive ink by using a magnetic scraper with magnetic force, and controlling the blade coating speed to be 1mm/s to obtain the flexible electrode utilizing the magnetic induction carbon nano tube arrangement.
Test method
The resistance of the highly aligned carbon nanotube flexible electrode prepared in example 1~2 and the carbon nanotube flexible electrode prepared in comparative example 1~3 was measured at 300k using a multimeter, and the results are shown in table 1 below, which shows that the highly aligned carbon nanotube transparent film prepared in this scheme has good conductivity.
Figure 688748DEST_PATH_IMAGE001
When the preparation method of the flexible electrode arranged by utilizing the magnetic induction carbon nano tubes is used, the multi-walled carbon nano tubes are used as main conductive fillers, water is used as a solvent, the magnetism of the carbon nano tubes and a magnetic conductive network formed by Fe3O4 form a highly aligned array structure, the obtained conductive ink is subjected to vacuum filtration, so that the directionally arranged carbon nano tube network is more compact, the whole thickness of the conductive ink is thinner, the thickening agent enables the conductive ink to be more effectively attached to a flexible or non-flexible substrate and cannot be easily separated, and the conductive ink cannot fall off in a complex environment such as a continuous stirring state.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.

Claims (8)

1. A preparation method of a flexible electrode using magnetic induction carbon nano tube arrangement is characterized in that: the method comprises the following steps:
s1: adding corresponding dispersing agent into the carbon nano tube aqueous solution, and then adding Fe with different proportions 3 O 4 Solid particles, finally, carrying out ultrasonic treatment on all the solutions at the temperature of 10 ℃, and carrying out centrifugal separation at a fixed rotating speed;
s2: under normal temperature and normal pressure, preparing a water absorption solute and water according to a fixed proportion, stirring for 3 hours at a fixed rotation speed at an ambient temperature of 70 ℃, and finally preparing a thickening agent of the conductive ink;
s3: mixing carbon nanotubes with Fe 3 O 4 The composite solution and the thickening agent are put in a grinding bowl according to different proportions at normal temperature for grinding and stirring for 10 minutes until the mixture is uniform, and finally the conductive ink of the composite material can be obtained;
s4: placing the conductive ink obtained in the step S3 on a die, and directly scraping the conductive ink by using a magnetic scraper with magnetic force to prepare a flexible electrode in which the carbon nano tubes are arranged by utilizing magnetic induction;
s5: and repeating the step S4.
2. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: fe in step S1 3 O 4 The particle size of the solid particles is 20 to 30nm.
3. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: the dispersant in the step S1 comprises one or more of acetone, ethanol and ethyl acetate.
4. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: the water absorption solute in the step S2 comprises one or more of polyethylene oxide and methyl cellulose.
5. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: the concentration of the carbon nano tube aqueous solution in the step S1 is 0.4% -1.0%, and the concentration unit is wt/vol.
6. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: the concentration of the thickener solution prepared in the step S2 is 7% -12%, and the concentration unit is wt/vol.
7. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: the blade coating time in the step S4 is 1mm/S.
8. The method of claim 1, wherein the step of preparing the flexible electrode comprises the steps of: the number of repetitions in step S5 is 2~3.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150302948A1 (en) * 2014-02-12 2015-10-22 South Dakota Board Of Regents Composite materials with magnetically aligned carbon nanoparticles having enhanced electrical properties and methods of preparation
CN113651314A (en) * 2021-09-08 2021-11-16 湖北中烟工业有限责任公司 Preparation method of highly oriented carbon nanotube transparent film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150302948A1 (en) * 2014-02-12 2015-10-22 South Dakota Board Of Regents Composite materials with magnetically aligned carbon nanoparticles having enhanced electrical properties and methods of preparation
CN113651314A (en) * 2021-09-08 2021-11-16 湖北中烟工业有限责任公司 Preparation method of highly oriented carbon nanotube transparent film

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
国家知识产权局专利局专利审查协作江苏中心主编: "《热点专利技术分析与运用 第1辑》", 知识产权出版社, pages: 207 *

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