CN112679772A - Flexible conductive composite material for intelligent wearing and preparation method - Google Patents
Flexible conductive composite material for intelligent wearing and preparation method Download PDFInfo
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Abstract
The invention belongs to the technical field of electronic materials, and provides a flexible conductive composite material for intelligent wearing and a preparation method thereof. The method takes cotton fibers as a base material, adopts an in-situ polymerization method to prepare cotton fiber/polypyrrole composite fibers, and then carries out hydrothermal reduction reaction with graphene oxide dispersion liquid to prepare the flexible conductive composite material for intelligent wearing. Compared with the traditional method, the composite material prepared by the invention has good conductivity and good flexibility, is suitable for a conductive sensing control film and the like worn intelligently, has simple preparation process, is environment-friendly and pollution-free, and the prepared conductive film is soft and fine and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of electronic materials, and provides a flexible conductive composite material for intelligent wearing and a preparation method thereof.
Background
With the rapid development of portable electronic devices and the increased acceptance of the feasibility of applying miniature electronic devices to wearable devices, it is more and more important to prepare a flexible electronic device that can be stretched or bent to replace the conventional hard electronic device. How to realize good conductive sensing, control and the like in a soft state in intelligent wearing is a problem which is urgently needed and solved in intelligent wearing at present. Therefore, materials having good conductivity and flexibility are attracting attention.
The graphene material has high specific surface area, good conductivity, excellent electronic conductivity and mechanical properties. However, the graphene particles are difficult to form a film independently, and the graphene particles are hopefully combined with a flexible substrate to prepare a flexible conductive material. Most flexible polymers have poor conductivity, and the conductivity of graphene can be greatly influenced by dispersing the graphene in the flexible polymers. Therefore, the conductive polymer becomes the choice for preparing the flexible conductive material with the graphene. Polypyrrole is used as an important conductive polymer, has a special conjugated molecular structure and unique physical and chemical properties, and has a good application prospect in the field of electronic devices. Fanxin et al invented a preparation method of polypyrrole/graphene/manganese oxide composite material (chinese patent application No. 201611068192.5), utilizing the electrostatic tension between nitrogen with positive charge on the polypyrrole chain segment and the epoxy bond on the surface of graphene oxide to adsorb a large amount of graphene oxide on the surface of three-dimensional porous reticular polypyrrole, effectively preventing the graphene oxide from agglomerating, then adding potassium permanganate solution and excessive manganese sulfate solution into the polypyrrole/graphene oxide mixed solution, depositing the generated manganese dioxide on the graphene sheet, reducing the graphene oxide into graphene sheet by the excessive manganese sulfate, and depositing the generated trimanganese tetroxide on the graphene sheet to prepare the three-dimensional porous reticular polypyrrole/graphene/manganese oxide composite material. In addition, fantaso et al invented a graphene-polypyrrole nanoparticle composite thin film electrode and a preparation method thereof (chinese patent application No. 201610238089.4), which was formed by compounding graphene and polypyrrole nanoparticles, the polypyrrole nanoparticles being methyl orange doped polypyrrole nanoparticles with a size of 50-200 nm; the composite film electrode has flexibility, good mechanical property and good electrochemical property.
However, pure polypyrrole is difficult to be processed and difficult to be formed into a film because of being difficult to be dissolved in water. The direct mixing of graphene and polypyrrole can affect the dispersion uniformity, so that the conductive effect is affected.
Disclosure of Invention
The invention provides a preparation method of a flexible conductive composite material for intelligent wearing, which aims at solving the problems that the uniformity of graphene and polypyrrole is poor and the conductivity is affected directly. Compared with the traditional method, the composite material prepared by the invention has good conductivity and good flexibility, is suitable for a conductive sensing control film and the like worn intelligently, has simple preparation process, is environment-friendly and pollution-free, and the prepared conductive film is soft and fine and is suitable for industrial production. Further provided is a flexible conductive composite for smart wear that can be prepared by the method.
In order to achieve the purpose, the invention relates to the following specific technical scheme:
a preparation method of a flexible conductive composite material for intelligent wearing is characterized in that cotton fibers are used as a base material, an in-situ polymerization method is adopted to prepare cotton fiber/polypyrrole composite fibers, then the cotton fiber/polypyrrole/graphene composite fibers and graphene oxide dispersion liquid are subjected to a hydrothermal reduction reaction to obtain the cotton fiber/polypyrrole/graphene composite material, and the flexible conductive composite material for intelligent wearing is prepared by the following specific steps:
(1) adding short cotton fibers and pyrrole into a solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film, further spraying ferric chloride solution on the film surface, carrying out in-situ polymerization reaction at 30-40 ℃ for 12-14h, washing and drying after the reaction is finished, and obtaining a cotton fiber/polypyrrole composite fiber film;
(2) and (2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into a dispersion liquid of graphene oxide, adding hydrazine hydrate, heating to 120-140 ℃ for carrying out a reduction reaction for 14-16h, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Preferably, the weight parts of the raw materials in the step (1) are 2-3 parts of short cotton fibers, 30-50 parts of pyrrole, 45-58 parts of solvent and 2-5 parts of ferric chloride solution.
Preferably, the ferric chloride solution in the step (1) is a saturated solution of ferric chloride.
Preferably, the solvent in step (1) is ethanol.
Preferably, the mass concentration of the dispersion liquid of graphene oxide in the step (2) is 3-5%.
Preferably, the hydrazine hydrate in the step (2) is added in an amount of 5-15% of the mass of the dispersion liquid.
The invention provides a flexible conductive composite material for intelligent wearing, which is prepared by the method.
The invention creatively takes cotton short fiber as a base material, and the cotton fiber/polypyrrole composite fiber membrane is prepared by dispersing and in-situ polymerizing with pyrrole, so that the base membrane has good flexibility, conductivity and adsorbability; further, in the dispersion liquid of the graphene oxide, under the action of a reducing agent hydrazine hydrate, the graphene oxide is subjected to hydrothermal reduction to form the graphene polypyrrole/graphene composite nanotube with high generation rate, high nanotube regularity and adjustable nanotube regular length-diameter ratio.
The invention also provides the flexible conductive composite material for intelligent wearing prepared by the preparation method. The composite material is prepared by taking cotton fibers and pyrrole as raw materials, ethanol as a solvent, p-toluenesulfonic acid as a dopant and ammonium persulfate as an initiator through an in-situ polymerization method, dispersing the cotton fibers/polypyrrole composite fibers in water, adding a graphene oxide dispersion liquid after ultrasonic stirring to perform a hydrothermal reduction reaction to form graphene attached to the surface of the cotton fibers/polypyrrole composite fibers, and further enabling the membrane material to have excellent conductivity.
The invention provides a flexible conductive composite material for intelligent wearing and a preparation method thereof, compared with the prior art, the flexible conductive composite material has the outstanding characteristics and excellent effects that:
1. the invention takes cotton fiber as a base material, and adopts an in-situ polymerization method to prepare the cotton fiber/polypyrrole composite fiber membrane material, so that the membrane material has good conductivity and flexibility.
2. According to the invention, the graphene oxide dispersion liquid is subjected to hydrothermal reduction reaction, so that the graphene oxide is reduced into graphene and stably fixed on the cotton fiber/polypyrrole composite fiber membrane material, the conductivity of the membrane material is improved, and the problem that the graphene and polypyrrole are difficult to disperse directly is solved.
3. The preparation method disclosed by the invention is simple in preparation process, environment-friendly and pollution-free, and the prepared conductive film is soft and fine and is suitable for industrial production.
Drawings
Fig. 1 is a photograph of a manually torn flexible conductive composite obtained in example 1, which is deformed and not torn.
Fig. 2 is a photograph of a manually torn flexible conductive composite obtained in comparative example 1, which was easily torn.
The film was torn by hand as shown.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Adding 2kg of cotton short fibers with the length of 1-5mm and 30kg of pyrrole into 45kg of ethanol solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film with the thickness of 0.5mm, further uniformly spraying 2kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 12h at 30 ℃, washing and drying after the reaction is finished, and preparing the cotton fiber/polypyrrole composite fiber film;
(2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into dispersion liquid of graphene oxide with the mass concentration of 3%, adding hydrazine hydrate, wherein the adding amount of the hydrazine hydrate is 10% of the mass of the dispersion liquid, heating to 120 ℃ to perform reduction reaction for 14 hours, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
The membrane material has good flexibility and strength, and as shown in figure 1, the membrane material is torn by hand, and only deforms but is not torn. The use requirement of intelligence wearing has been satisfied.
Example 2
(1) Adding 3kg of cotton short fibers with the length of 1-5mm and 40kg of pyrrole into 45kg of ethanol solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film with the thickness of 0.5mm, further uniformly spraying 3kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 12h at 30 ℃, washing and drying after the reaction is finished, and preparing the cotton fiber/polypyrrole composite fiber film;
(2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into dispersion liquid of graphene oxide with the mass concentration of 3%, adding hydrazine hydrate, wherein the adding amount of the hydrazine hydrate is 5% of the mass of the dispersion liquid, heating to 120 ℃ to perform reduction reaction for 16 hours, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Example 3
(1) Adding 3kg of cotton short fibers with the length of 1-5mm and 50kg of pyrrole into 58kg of ethanol solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film with the thickness of 0.5mm, further uniformly spraying 5kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 12h at 40 ℃, washing and drying after the reaction is finished, and preparing the cotton fiber/polypyrrole composite fiber film;
(2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into dispersion liquid of graphene oxide with the mass concentration of 3%, adding hydrazine hydrate, wherein the adding amount of the hydrazine hydrate is 10% of the mass of the dispersion liquid, heating to 120 ℃ to perform reduction reaction for 15 hours, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Example 4
(1) Adding 3kg of cotton short fibers with the length of 1-5mm and 50kg of pyrrole into 50kg of ethanol solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film with the thickness of 0.5mm, further uniformly spraying 4kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 14h at 40 ℃, washing and drying after the reaction is finished, and preparing the cotton fiber/polypyrrole composite fiber film;
(2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into a dispersion liquid of graphene oxide with the mass concentration of 5%, adding hydrazine hydrate, wherein the adding amount of the hydrazine hydrate is 15% of the mass of the dispersion liquid, heating to 140 ℃ to perform a reduction reaction for 16 hours, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain a cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Example 5
(1) Adding 2kg of cotton short fibers with the length of 1-5mm and 30kg of pyrrole into 58kg of ethanol solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film with the thickness of 0.5mm, further uniformly spraying 5kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 12h at 30 ℃, washing and drying after the reaction is finished, and preparing the cotton fiber/polypyrrole composite fiber film;
(2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into dispersion liquid of graphene oxide with the mass concentration of 3%, adding hydrazine hydrate, wherein the adding amount of the hydrazine hydrate is 15% of the mass of the dispersion liquid, heating to 140 ℃ to perform reduction reaction for 16h, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Comparative example 1
(1) Adding 30kg of pyrrole into 45kg of ethanol solvent, ultrasonically dispersing into slurry, adjusting the pH value to 3.5, then blade-coating into a film with the thickness of 0.5mm, further uniformly spraying 2kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 12h at the temperature of 30 ℃, washing and drying after the reaction is finished, thus preparing the polypyrrole film;
(2) and (2) immersing the polypyrrole film prepared in the step (1) into a dispersion liquid of graphene oxide with the mass concentration of 3%, adding hydrazine hydrate, wherein the addition amount of the hydrazine hydrate is 10% of the mass of the dispersion liquid, heating to 120 ℃ to perform a reduction reaction for 14h, reducing the graphene oxide into graphene attached to the polypyrrole film surface, washing, and drying to obtain the polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Comparative example 1 no cotton fiber was added to the polypyrrole film, and the flexibility and strength of one film were poor; as shown in fig. 2, the film was very easily torn. On the other hand, when graphene oxide is infiltrated, the absorption of graphene inside the membrane is limited, so that the conductivity of the membrane is influenced.
Comparative example 2
(1) Adding 2kg of cotton short fibers with the length of 1-5mm and 30kg of pyrrole into 45kg of ethanol solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film with the thickness of 0.5mm, further uniformly spraying 2kg of ferric chloride saturated solution on the film surface, carrying out in-situ polymerization reaction for 12h at 30 ℃, washing and drying after the reaction is finished, and preparing the cotton fiber/polypyrrole composite fiber film;
(2) and (2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into a dispersion liquid of graphene with the mass concentration of 3%, so that the graphene is attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
Comparative example 1 does not adopt a graphene oxide reduction method, but immerses the cotton fiber/polypyrrole composite fiber film in the graphene dispersion liquid, and since graphene is not formed in a reduction method, graphene bonding is poor and conductivity is poor.
And (3) conductivity test: the conductivity of examples 1 to 5 and comparative example 1 was measured by the four-probe method, and the obtained data are shown in table 1.
And (3) testing mechanical properties: the tensile properties of the film were determined by reference to GB/T1040-2018, as shown in Table 1.
Table 1:
| performance index | Conductivity (S/cm) | Tensile Strength (MPa) |
| Example 1 | 8.22 | 17.8 |
| Example 2 | 8.10 | 16.3 |
| Example 3 | 8.15 | 18.1 |
| Example 4 | 9.02 | 19.2 |
| Example 5 | 8.17 | 17.5 |
| Comparative example 1 | 7.10 | 6.3 |
| Comparative example 2 | 5.32 | 18.5 |
Claims (7)
1. A preparation method of a flexible conductive composite material for intelligent wearing is characterized in that cotton fibers are used as a base material, an in-situ polymerization method is adopted to prepare cotton fiber/polypyrrole composite fibers, then the cotton fiber/polypyrrole/graphene composite fibers and graphene oxide dispersion liquid are subjected to a hydrothermal reduction reaction to obtain the cotton fiber/polypyrrole/graphene composite material, and the flexible conductive composite material for intelligent wearing is prepared by the following specific steps:
(1) adding short cotton fibers and pyrrole into a solvent, ultrasonically dispersing to form slurry, adjusting the pH value to 3.5, then blade-coating to form a film, further spraying ferric chloride solution on the film surface, carrying out in-situ polymerization reaction at 30-40 ℃ for 12-14h, washing and drying after the reaction is finished, and obtaining a cotton fiber/polypyrrole composite fiber film;
(2) and (2) immersing the cotton fiber/polypyrrole composite fiber membrane prepared in the step (1) into a dispersion liquid of graphene oxide, adding hydrazine hydrate, heating to 120-140 ℃ for carrying out a reduction reaction for 14-16h, reducing the graphene oxide into graphene attached to the surface of the cotton fiber/polypyrrole composite fiber membrane, washing, and drying to obtain the cotton fiber/polypyrrole/graphene composite material, namely the flexible conductive composite material for intelligent wearing.
2. The preparation method of the flexible conductive composite material for intelligent wearing according to claim 1, wherein the preparation method comprises the following steps: the weight parts of the raw materials in the step (1) are 2-3 parts of cotton short fibers, 30-50 parts of pyrrole, 45-58 parts of solvent and 2-5 parts of ferric chloride solution.
3. The preparation method of the flexible conductive composite material for intelligent wearing according to claim 1, wherein the preparation method comprises the following steps: the ferric chloride solution in the step (1) is saturated ferric chloride solution.
4. The preparation method of the flexible conductive composite material for intelligent wearing according to claim 1, wherein the preparation method comprises the following steps: the solvent in the step (1) is ethanol.
5. The preparation method of the flexible conductive composite material for intelligent wearing according to claim 1, wherein the preparation method comprises the following steps: and (3) the mass concentration of the dispersion liquid of the graphene oxide in the step (2) is 3-5%.
6. The preparation method of the flexible conductive composite material for intelligent wearing according to claim 1, wherein the preparation method comprises the following steps: and (3) adding hydrazine hydrate in the step (2) in an amount of 5-15% of the mass of the dispersion liquid.
7. The flexible conductive composite material for intelligent wearing prepared by the preparation method of any one of claims 1 to 6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265873A (en) * | 2021-05-14 | 2021-08-17 | 南开大学 | Flexible sensing fabric carrying metal oxide, conductive polymer and two-dimensional nano material, preparation method and application thereof |
| WO2023155833A1 (en) * | 2022-02-16 | 2023-08-24 | 宁波亨励数字科技有限公司 | Flexible electronic material, breathable moisture-permeable electronic element, flexible circuit, and method |
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2021
- 2021-01-11 CN CN202110029641.XA patent/CN112679772A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265873A (en) * | 2021-05-14 | 2021-08-17 | 南开大学 | Flexible sensing fabric carrying metal oxide, conductive polymer and two-dimensional nano material, preparation method and application thereof |
| WO2023155833A1 (en) * | 2022-02-16 | 2023-08-24 | 宁波亨励数字科技有限公司 | Flexible electronic material, breathable moisture-permeable electronic element, flexible circuit, and method |
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