CN108428567B - Preparation method of graphene-based series linear supercapacitor - Google Patents
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- 239000012362 glacial acetic acid Substances 0.000 claims description 4
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- 229920002994 synthetic fiber Polymers 0.000 claims description 4
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 claims description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 2
- 229920006052 Chinlon® Polymers 0.000 claims description 2
- 229920000742 Cotton Polymers 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229920004933 Terylene® Polymers 0.000 claims description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000000840 electrochemical analysis Methods 0.000 claims description 2
- 238000007667 floating Methods 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- XQHAGELNRSUUGU-UHFFFAOYSA-M lithium chlorate Chemical compound [Li+].[O-]Cl(=O)=O XQHAGELNRSUUGU-UHFFFAOYSA-M 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 150000002989 phenols Chemical class 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 239000003755 preservative agent Substances 0.000 claims description 2
- 230000002335 preservative effect Effects 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 210000002268 wool Anatomy 0.000 claims description 2
- 238000010277 constant-current charging Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000012360 testing method Methods 0.000 description 6
- 229920001940 conductive polymer Polymers 0.000 description 5
- 229920000297 Rayon Polymers 0.000 description 3
- 239000011245 gel electrolyte Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- -1 poly (p-phenylene vinylene) Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
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- 238000004146 energy storage Methods 0.000 description 1
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- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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- 238000012544 monitoring process Methods 0.000 description 1
- 229920000553 poly(phenylenevinylene) Polymers 0.000 description 1
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- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a preparation method of a graphene-based series linear supercapacitor, which is characterized in that discontinuous composite conductive active materials are utilized to enable yarns to be locally conductive, so that continuous insulating and conductive yarns arranged at intervals are formed, and a plurality of supercapacitor series devices can be directly assembled by coating colloid electrolyte on the insulating yarns. The device has the advantages of small volume, high output voltage, good flexibility, simple preparation process and easy operation.
Description
Technical Field
The invention relates to a preparation method of a graphene-based series linear supercapacitor, in particular to a preparation method of a continuous conductive-insulating discontinuous yarn and an ultrahigh output voltage linear supercapacitor, and belongs to the technical field of textile and electrochemistry.
Background
In recent years, wearable devices are rapidly developed and have wide application prospects in the fields of intelligent skin, health monitoring, stretchable loops and the like, so that an energy source for supplying power to the wearable devices is particularly important. Rechargeable batteries are widely used as energy storage devices due to their high energy density, but their development is being limited by low power density and poor cycling stability, and their flexibility is poor, and they are limited in the use of wearable electronics. The linear supercapacitor is a flexible energy source, has light weight, high power density, long cycle life, small volume and soft texture, but the low energy density of the linear supercapacitor compared with a battery or a flat capacitor limits further application.
For a supercapacitor, the energy density depends mainly on the specific capacitance and the potential window range, and in order to increase the potential window, a plurality of devices can be integrated in series. The learner winds a single-time long conductive polymer fiber spirally on an elastic yarn, wherein a part of the elastic yarn is coated with a gel electrolyte to serve as an inner electrode of a first super capacitor, the rest of the elastic yarn is used as a lead, a part of a strand of double-time long conductive polymer fiber is wound outside the inner electrode of the first super capacitor to serve as an outer electrode, and the rest of the elastic yarn is wound spirally on the elastic yarn. The gel electrolyte is coated on the surface of the rest part of the double-length conductive polymer as the inner electrode of a second super capacitor, and the rest part is used as a lead to connect two adjacent super capacitors. Repeating the steps, and coating the elastic gel electrolyte on the surface of each section of lead wire to obtain the linear supercapacitor group integrated device (CN106592009) with a plurality of supercapacitors connected in series.
So far, a method for directly forming a conductive and insulating part on one yarn and coating electrolyte on the insulating part to prepare a super capacitor has not been reported yet, and a formed series integrated device has good flexibility, can be woven and has high output voltage.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing super capacitor has the defects of complex preparation process, poor flexibility, non-weaving, large volume, low output voltage and the like.
In order to solve the problems, the invention adopts the technical scheme that: a preparation method of a graphene-based series linear supercapacitor is characterized in that discontinuous composite conductive active materials are utilized to enable yarns to be locally conductive, so that continuous insulating and conductive yarns arranged at intervals are formed, and a plurality of supercapacitor series devices can be directly assembled by coating colloid electrolyte on the insulating yarns.
Preferably, the above preparation method comprises the steps of:
step 1): preparing graphene oxide by using a Hummers method, magnetically stirring and concentrating the prepared graphene oxide dispersion liquid to be in a gel state, and transferring the gel state to a culture dish for later use;
step 2): winding the insulating yarn on a hollow rectangular support in an S shape, immersing the lower end of the support into graphene oxide, taking out after 30-60 minutes, washing with deionized water to remove the graphene oxide floating on the surface, and drying in a drying oven at 30-50 ℃; repeating for 2-10 times to ensure that the graphene oxide is fully and uniformly attached to the surface of the insulating yarn;
step 3): locally reducing the prepared graphene oxide filament to prepare continuous insulated and conductive yarn arranged at intervals;
step 4): and coating the insulating part of the continuous insulating and conducting yarns which are arranged at intervals with colloid electrolyte, standing for 12-24 hours, and airing to prepare the graphene-based series linear supercapacitor.
More preferably, the temperature of the magnetic stirring in the step 1) is 40 ℃, and if the temperature is too high, the graphene oxide is carbonized, and if the temperature is too low, the moisture volatilization speed is slow.
More preferably, the bracket in the step 2) is made of metal wires, and insulated yarns are wound after the surface of the bracket is wrapped by the preservative film, so that the surface oxides of the metal wires are prevented from polluting the yarns; the insulating yarn is made of natural fibers or synthetic fibers.
More preferably, the natural fibers are cotton, wool or silk; the synthetic fiber is terylene, chinlon or acrylon.
More preferably, the width of the stent in the step 2) is 3 to 5mm, and the length of the end portion thereof immersed in the conductive active material is 1 to 2 mm. The support is made of the metal wires which are extremely fine and have certain strength, so that the contact part of the yarns and the support is reduced, the influence of the support on the self-assembly of the graphene oxide is reduced, the length of discontinuous yarns can be reduced, the ion transport distance is shortened, the invalid length is reduced, and the output voltage density is improved.
More preferably, the graphene oxide is reduced in the step 3) by using a laser, a direct reduction method or other methods. Other reduction methods can also be adopted, but attention needs to be paid to reducing graphene oxide and simultaneously not damaging the structure of the yarn, namely the integrity and partial insulativity of the yarn need to be protected.
More preferably, the reducing agent used in the direct reduction method is hydrazine hydrate, phenols, dimethylhydrazine or a sulfur-containing compound.
More preferably, the reduction method is specifically: suspending the insulated yarn in HI acid and glacial acetic acid, and sealing; and (3) putting the beaker into an oil bath kettle at the temperature of 40 ℃ for reaction for 24-48 hours, cooling, taking out, washing with deionized water and ethanol, and drying. The mixed solution of HI acid and glacial acetic acid is heated at high temperature, and graphene oxide is reduced by steam, so that the prepared graphene/viscose yarn is low in impedance and high in conductivity.
More preferably, the colloidal electrolyte in step 4) is a polyvinyl alcohol aqueous solution of any one or more of potassium hydroxide, sodium chloride, potassium chloride, ammonium sulfate, sodium sulfate, potassium sulfate, ammonium nitrate, sodium nitrate, potassium nitrate, sulfuric acid, phosphoric acid, hydrochloric acid and lithium chlorate; the prepared graphene-based series linear super capacitor is subjected to electrochemical test, and specifically is a Cyclic Voltammetry (CV) method or a cross-flow charging and discharging (GCD) method; wherein the scanning speed in the cyclic voltammetry is 0.005-100V/s, and the current density in the cross-current charging and discharging method is 0.1-1000 mA/cm2。
The graphene in the invention may also be made of other conductive active substances, such as conductive polymer materials, metal materials or carbon-based materials, and the conductive polymer materials may be polyacetylene, polyaniline, polypyrrole, polythiophene, poly (p-phenylene vinylene) or poly (p-phenylene).
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method is quick and simple and is easy to popularize;
2. the prepared continuous conductive-insulating spacing yarn as an electrode material has high output voltage and good flexibility, and can be directly woven;
3. the super capacitor made of the yarn as the electrode material is excellent in electrochemical performance and expected to have wide application prospect in the wearable field.
Drawings
FIG. 1 is a graph comparing the charge and discharge times of a single element and four devices in series in example 1 (current density of 0.1 mA/cm)2)。
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below.
Example 1
A preparation method of an ultra-high output voltage linear super capacitor comprises the following steps:
preparing a gel: preparing graphene oxide by using a Hummers method, magnetically stirring the prepared graphene oxide dispersion liquid with the mass fraction of 1-5 mg/mL at 40 ℃, concentrating to form gel, and transferring to a 60mm culture dish for later use.
Self-assembly: winding the viscose yarn on a self-made hollow rectangular support in an S shape, wherein the width of the support is 5mm, the lower end of the support is immersed into the concentrated graphene oxide for 2mm, taking out the support after 30 minutes, washing the support with deionized water, and drying the support in a drying oven at 40 ℃. Repeating for 4 times to ensure that the graphene oxide is fully and uniformly attached to the surface of the viscose yarn.
Reduction: the prepared yarn was suspended in a 300mL beaker of 2mL of acid and 5mL of glacial acetic acid and was subjected to a sealing treatment. And (3) putting the beaker into a 40 ℃ oil bath pot for reaction for 24 hours, cooling, taking out, washing with deionized water and ethanol, and drying to obtain the continuous insulating-conductive spacing yarn.
Assembling and testing the super capacitor: and (3) coating the prepared colloid electrolyte on the insulation part of the continuous insulation-conduction spacing yarn, standing for 12-24 hours, airing, preparing the ultra-high output voltage linear supercapacitor, and testing, wherein the test result is shown in figure 1.
As can be seen from fig. 1, as the number of the super capacitors connected in series increases, the overall output voltage of the assembled device increases, which indicates that the series super capacitor obtained by the method has good integrity and can achieve the purpose of outputting high voltage by increasing the number of the super capacitors connected in series.
Example 2
A preparation method of an ultra-high output voltage linear super capacitor comprises the following steps:
preparation: graphene oxide is prepared by a Hummers method, and the prepared graphene oxide dispersion liquid with the mass fraction of 2mg/ml is transferred to a 60mm culture dish for later use. And preparing the graphene oxide dispersion liquid into filaments by a wet spinning method, and drying at a low temperature (40-60 ℃) to obtain the continuous pure graphene oxide filaments.
Reduction: and locally reducing the prepared graphene oxide filament by using laser to prepare the continuous conductive-insulating spaced graphene yarn.
Assembling and testing the super capacitor: and coating the prepared insulation position of the continuous conductive-insulation spacing yarn with colloid electrolyte, standing for 12-24 hours, airing, and preparing the ultra-high output voltage linear supercapacitor and testing.
The test results are the same as in example 1, and as the number of supercapacitors connected in series increases, the overall output voltage of the assembled device increases.
Claims (9)
1. A preparation method of a graphene-based series linear supercapacitor is characterized in that discontinuous composite conductive active materials are utilized to enable yarns to be locally conductive, so that continuous insulating and conductive yarns arranged at intervals are formed, and a plurality of supercapacitor series devices can be directly assembled by coating colloid electrolyte on the insulating yarns; the preparation method of the graphene-based series linear supercapacitor comprises the following steps:
step 1): preparing graphene oxide by using a Hummers method, magnetically stirring and concentrating the prepared graphene oxide dispersion liquid to be in a gel state, and transferring the gel state to a culture dish for later use;
step 2): winding the insulating yarn on a hollow rectangular support in an S shape, immersing the lower end of the support into graphene oxide, taking out after 30-60 minutes, washing with deionized water to remove the graphene oxide floating on the surface, and drying in a drying oven at 30-50 ℃; repeating for 2-10 times to ensure that the graphene oxide is fully and uniformly attached to the surface of the insulating yarn;
step 3): locally reducing the prepared graphene oxide filament to prepare continuous insulated and conductive yarn arranged at intervals;
step 4): and coating the insulating part of the continuous insulating and conducting yarns which are arranged at intervals with colloid electrolyte, standing for 12-24 hours, and airing to prepare the graphene-based series linear supercapacitor.
2. The method for preparing the graphene-based series linear supercapacitor according to claim 1, wherein the temperature of the magnetic stirring in the step 1) is 40 ℃.
3. The method for preparing the graphene-based series linear supercapacitor as claimed in claim 1, wherein the support in the step 2) is made of metal wires, and insulating yarns are wound after a preservative film is wrapped on the surface of the metal wires; the insulating yarn is made of natural fibers or synthetic fibers.
4. The method of manufacturing a graphene-based series wire-like supercapacitor of claim 3, wherein the natural fiber is cotton, wool or silk; the synthetic fiber is terylene, chinlon or acrylon.
5. The method for preparing the graphene-based series wire-like supercapacitor according to claim 1, wherein the stent in step 2) has a width of 3-5mm and a length of 1-2mm at its end immersed in the conductive active material.
6. The method for preparing the graphene-based series linear supercapacitor according to claim 1, wherein in the step 3), the graphene oxide is reduced by using a laser or a direct reduction method.
7. The method for preparing the graphene-based series wire-like supercapacitor according to claim 6, wherein the reducing agent adopted by the direct reduction method is hydrazine hydrate, phenols, dimethylhydrazine or a sulfur-containing compound.
8. The method for manufacturing the graphene-based series linear supercapacitor according to claim 6, wherein the reduction method specifically comprises: suspending the insulated yarn in HI acid and glacial acetic acid, and sealing; and (3) putting the beaker into an oil bath kettle at the temperature of 40 ℃ for reaction for 24-48 hours, cooling, taking out, washing with deionized water and ethanol, and drying.
9. The method for preparing the graphene-based series linear supercapacitor according to claim 1, wherein the colloidal electrolyte in the step 4) is a polyvinyl alcohol aqueous solution of one or more of potassium hydroxide, sodium chloride, potassium chloride, ammonium sulfate, sodium sulfate, potassium sulfate, ammonium nitrate, sodium nitrate, potassium nitrate, sulfuric acid, phosphoric acid, hydrochloric acid and lithium chlorate; the prepared graphene-based series linear super capacitor is subjected to electrochemical test, specifically to a cyclic voltammetry method or a constant current charging and discharging method; wherein the scanning speed in the cyclic voltammetry is 0.005-100V/s, and the current density in the constant current charging and discharging method is 0.1-1000 mA/cm2。
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