CN107799325B - A kind of preparation method based on Ag/PPy composite nano materials printing supercapacitor - Google Patents
A kind of preparation method based on Ag/PPy composite nano materials printing supercapacitor Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods based on Ag/PPy composite nano materials printing supercapacitor, acetate is introduced in Ag/PPy composite nano materials preparation process, make the Ag/PPy composite nano materials obtained that there is pod-like core-shell structure, be conducive to the promotion of material capacitive property, different flexible parent metals is selected, by silver paste, the Ag/PPy composite nano materials and PVA-H of synthesis by way of silk-screen printing3PO4Solid electrolyte is printed as flexible solid-state supercapacitor.The energy density of the supercapacitor of manufacture of the invention is up to 4.33 μ Wh cm‑277.6% unit specific capacitance is still maintained after bending 1000 times, and 82.6% unit specific capacitance is still maintained after circulation 10000 times, it is cheap, realize the substitution and supplement of the energy storage device high to traditional price, and the advantages that simple with reaction step, the reaction time is short, easy to operate, it can be used for industrial mass preparation and production, and flexible energy storage field can be applied to, synthetic method cleaning, environmental protection are suitable for promoting and applying.
Description
Technical field
The present invention relates to a kind of preparation methods based on Ag/PPy composite nano materials printing supercapacitor.
Background technique
Supercapacitor (Supercapacitor) is a kind of novel energy storage apparatus, it has, and the charging time is short, uses the longevity
Order length, good temp characteristic, it is energy saving and environmentally protective the features such as, therefore supercapacitor is widely used.Since petroleum provides
Source is increasingly short, and the internal combustion engine tail gas discharge of burning petroleum is increasingly severe to the pollution of environment (especially in big or middle city
City), solia particle increases in air, very big influence is caused to human body, people are in the new energy of research substitution internal combustion engine
Device.Carried out hybrid power, fuel cell, chemical cell product and the research and development of application, achieve it is certain at
Effect.But it is high since their intrinsic service lifes are short, temperature characterisitic is poor, chemical cell pollutes environment, system complex, cost
Etc. deadly defects, never very good solution method.Supercapacitor (Supercapacitor) is raised with its excellent characteristic
It is long to keep away short, traditional chemical cell can be partly or entirely substituted for the traction power source of vehicle and the starting energy, and is had
Purposes more extensive than traditional chemical cell.Just because of this, countries in the world (especially western developed country) is not lost
Research and development are carried out to surplus energy to supercapacitor, however it is good and have how to prepare to large-scale low-cost capacitive property
The main reason for stablizing the supercapacitor of cycle performance but becomes limitation Supercapacitor development.
Currently, the preparation method of supercapacitor mainly has chemical deposition and sputtering, but with this method
Want to be quickly obtained large batch of supercapacitor or a sizable challenge.The study found that the electric conductivity of active material
Can there are direct connection, a kind of active material quilt of the polypyrrole as cheap high theoretical specific capacitance to supercapacitor capacitive character
Research extensively, however it is applied to supercapacitor and is limited by not high electric conductivity itself, therefore silver and polypyrrole are carried out
Compound is a kind of feasible program for obtaining high capacitance performance activity material.And the Ag/PPy (silver/polypyrrole) of structure-controllable is compound
The preparation of nano material is the research hotspot in the field, and different patterns, structure are by the conduction to Ag/PPy composite nano materials
Performance, specific surface area etc. will cause influence, to influence its capacitive property.The development of nanosecond science and technology is Ag/PPy composite Nano
The technical conditions that the preparation of material is provided convenience, researcher has prepared capacitive property by the way of silk-screen printing at present
The flexible super capacitor good, cyclical stability is strong and mechanical performance is excellent, and it is applied to flexible energy storage field.Printed electronic
(Printed Electronics) technology has been caused by the important technology manufactured as a kind of achievable large area and flexible device
Researcher widely pays close attention to, and this method is the manufacturing technology based on print principle, mainly by some good dispersions or
Water-soluble inorganic or organic material carries out printed patterns processing and finally realizes the manufactures of higher order structures.
Summary of the invention
The purpose of the invention is to provide a kind of preparation based on Ag/PPy composite nano materials printing supercapacitor
Method realizes the substitution and benefit of the energy storage device high to traditional price to prepare cheap flexible super capacitor
Fill, and have reaction step it is simple, the reaction time is short, it is easy to operate the advantages that, can be used for industrial mass preparation and production,
And flexible energy storage field can be applied to.
In order to achieve the above object, present invention provide the technical scheme that a kind of printed based on Ag/PPy composite nano materials
The preparation method of supercapacitor processed, includes the following steps:
1) acetate regulates and controls the synthesis of lower Ag/PPy composite nano materials, method particularly includes: in mass ratio for 5:20:2 according to
Secondary addition silver nitrate, polyvinylpyrrolidone and acetate stir to get mixed solution, then, this are mixed into a certain amount of water
It closes solution and 30-40min is stirred at room temperature, the pyrrole monomer and ferric trichloride that mass ratio is 1:2 are added by peristaltic pump, the reaction was continued
2-3h；
2) cleaning of Ag/PPy composite nano materials and the preparation of Ag/PPy particle, method particularly includes: it will be walked by ethyl alcohol
Rapid 1) obtained Ag/PPy composite nano materials are by being then dispersed in anhydrous second at centrifugation cleaning in 10 minutes 3 times or more
In alcohol, and its mass fraction is made to reach 60%, 6-8h is dried under conditions of 60 DEG C by baking oven；
3) the Ag/PPy ink prepared, method particularly includes: it according to mass ratio is 8:1:1 by Ag/PPy particle, conductive black
The Ag/PPy ink for configuring that the viscosity for being suitble to silk-screen printing is 0.2Pas in a certain amount of water is added to epoxy resin；
4) preparation of supercapacitor, method particularly includes: by the silk screen plate of 300-400 mesh prepared by silver paste, step 3)
Ag/PPy ink and PVA-H3PO4Solid electrolyte is sequentially overlapped printing on the substrate, forms supercapacitor pattern,
Then it is drying to obtain.
Preferably, it is dried in the step 4) by baking oven, if stock is polyester, drying temperature be should not be greater than
120 DEG C, if stock is paper, drying temperature should not be greater than 100 DEG C, if stock is cotton, drying temperature does not answer height
In 80 DEG C.
Preferably, the supercapacitor pattern is pectination solid pattern.
Compared with prior art, the advantages of the present invention:
1, the method for the present invention introduces acetate into the preparation of Ag/PPy composite nano materials, keeps the Ag/PPy obtained multiple
Nano material electric conductivity with higher and capacitive property are closed, is conducive to the promotion of supercapacitor electricity performance, significantly
Improve the capacitive property of supercapacitor.
2, the method for the present invention without product purification, quickly, it is intuitive, be a kind of easy to operate, quick, high yield novel conjunction
At method.It, can be on different stocks (PET, common A4 paper and common cotton) by controlling the stock of silk-screen printing
Prepare flexible super capacitor.
3, the energy density of the supercapacitor prepared is up to 4.33 μ Wh cm-2, still maintained after bending 1000 times
77.6% unit specific capacitance still maintains 82.6% unit specific capacitance after recycling 10000 times.
Specific embodiment
Embodiment 1:
Specific preparation process is as follows: 1) 0.05g silver nitrate, 0.2g polyvinylpyrrolidone (PVP) and 0.02g acetate,
It is added in 20mL water and stirs in order.Then, which is stirred at room temperature 30min, by peristaltic pump with 600 μ L/
Min speed is separately added into the ferric chloride aqueous solutions of the pyrrole monomer of 0.25mL and the 0.3mol/L of 10mL, the reaction was continued 2h.2)
Synthesized Ag/PPy composite nano materials are subjected to cleaning and the preparation of Ag/PPy particle, method particularly includes: it will by ethyl alcohol
Product obtained is then dispersed in dehydrated alcohol, and make by being centrifuged at 10000 turns cleaning in 10 minutes 3 times or more
Its mass fraction reaches 60%, and 6h is dried under conditions of 60 DEG C by baking oven.3) Ag/PPy ink is prepared, method particularly includes:
It is that 8:1:1 addition 0.8g Ag/PPy composite nanometer particle, 0.1g conductive black and 0.1g epoxy resin are added to according to mass ratio
The Ag/PPy ink for being suitble to that the viscosity of silk-screen printing is 0.2Pas is configured in the water of 5mL.4) preparation of supercapacitor is printed,
Method particularly includes: the Ag/PPy ink and PVA-H for being prepared silver paste, above-mentioned steps by the silk screen plate of 400 mesh3PO4Solid-state electricity
Solution matter, which is sequentially overlapped, is printed as various supercapacitor patterns, such as pectination solid pattern.5) silk-screen printing is obtained by baking oven
Supercapacitor it is dry, if stock is polyester (PET), drying temperature should not be greater than 120 DEG C, if stock is common A4
Paper, drying temperature should not be greater than 100 DEG C, if stock is common cotton, drying temperature should not be greater than 80 DEG C.Preparation
The energy density of supercapacitor is up to 4.33 μ Wh cm-2, 77.6% unit specific capacitance is still maintained after bending 1000 times,
82.6% unit specific capacitance is still maintained after circulation 10000 times.
Embodiment 2:
Specific preparation process is as follows: 1) 0.5g silver nitrate, 2.0g polyvinylpyrrolidone (PVP) and 0.2g acetate are pressed
Order is added in 200mL water and stirs.Then, which is stirred at room temperature 30min, by peristaltic pump with 600 μ L/
Min speed is separately added into the ferric chloride aqueous solutions of the pyrrole monomer of 2.5mL and the 0.3mol/L of 100mL, the reaction was continued 2h.2)
Synthesized Ag/PPy composite nano materials are subjected to cleaning and the preparation of Ag/PPy particle, method particularly includes: it will by ethyl alcohol
Product obtained is then dispersed in dehydrated alcohol, and make by being centrifuged at 10000 turns cleaning in 10 minutes 3 times or more
Its mass fraction reaches 60%, and 6h is dried under conditions of 60 DEG C by baking oven.It 3) is that 8g Ag/ is added in 8:1:1 according to mass ratio
PPy composite nanometer particle, 1g conductive black and 1g epoxy resin be added in the water of 50mL configure be suitble to silk-screen printing viscosity be
The Ag/PPy ink of 0.2Pas.4) preparation of supercapacitor is printed, method particularly includes: it will be silver-colored by the silk screen plate of 400 mesh
Ag/PPy ink and PVA-H prepared by slurry, above-mentioned steps3PO4Solid electrolyte, which is sequentially overlapped, is printed as various supercapacitors
Pattern, such as pectination solid pattern.5) supercapacitor obtained silk-screen printing by baking oven is dry, if stock is polyester
(PET), drying temperature should not be greater than 120 DEG C, if stock is common A4 paper, drying temperature should not be greater than 100 DEG C, if
Stock is common cotton, and drying temperature should not be greater than 80 DEG C.The energy density of the supercapacitor of preparation is up to 4.33 μ Wh
cm-2, 77.6% unit specific capacitance is still maintained after bending 1000 times, still maintains 82.6% after circulation 10000 times
Unit specific capacitance.
Embodiment 3:
Specific preparation process is as follows: 1) 0.08g silver nitrate, 0.32g polyvinylpyrrolidone (PVP) and 0.032g acetic acid
Salt is added in 30mL water in order and stirs.Then, which is stirred at room temperature 30min, by peristaltic pump with 600 μ
L/min speed is separately added into the ferric chloride aqueous solutions of the pyrrole monomer of 0.4mL and the 0.3mol/L of 16mL, the reaction was continued 2h.
2) synthesized Ag/PPy composite nano materials are subjected to cleaning and the preparation of Ag/PPy particle, method particularly includes: pass through ethyl alcohol
By product obtained by being then dispersed in dehydrated alcohol at 10000 turns of centrifugations cleaning in 10 minutes 3 times or more, and
So that its mass fraction is reached 60%, 6h is dried under conditions of 60 DEG C by baking oven.It 3) is that 1.6g is added in 8:1:1 according to mass ratio
Ag/PPy composite nanometer particle, 0.2g conductive black and 0.2g epoxy resin, which are added to configure in the water of 10mL, is suitble to silk-screen printing
Viscosity is the Ag/PPy ink of 0.2Pas.4) preparation of supercapacitor is printed, method particularly includes: pass through the silk screen of 400 mesh
The Ag/PPy ink and PVA-H that plate prepares silver paste, above-mentioned steps3PO4Solid electrolyte be sequentially overlapped be printed as it is various super
Capacitor pattern, such as pectination solid pattern.5) supercapacitor obtained silk-screen printing by baking oven is dry, if stock is
Polyester (PET), drying temperature should not be greater than 120 DEG C, if stock is common A4 paper, drying temperature should not be greater than 100
DEG C, if stock is common cotton, drying temperature should not be greater than 80 DEG C.The energy density of the supercapacitor of preparation is reachable
4.33μWh cm-2, 77.6% unit specific capacitance is still maintained after bending 1000 times, is still maintained after circulation 10000 times
82.6% unit specific capacitance.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (3)
1. a kind of preparation method based on Ag/PPy composite nano materials printing supercapacitor, which is characterized in that including as follows
Step:
1) acetate regulates and controls the synthesis of lower Ag/PPy composite nano materials, method particularly includes: successively add for 5:20:2 in mass ratio
Enter silver nitrate, polyvinylpyrrolidone and acetate into a certain amount of water, stirs to get mixed solution, it is then, the mixing is molten
30-40min is stirred at room temperature in liquid, and the pyrrole monomer and ferric trichloride that mass ratio is 1:2, the reaction was continued 2- is added by peristaltic pump
3h；
2) cleaning of Ag/PPy composite nano materials and the preparation of Ag/PPy particle, method particularly includes: by ethyl alcohol by step 1)
Obtained Ag/PPy composite nano materials by being then dispersed in dehydrated alcohol in centrifugation cleaning 3 times or more in 10 minutes,
And its mass fraction is made to reach 60%, 6-8h is dried under conditions of 60 DEG C by baking oven；
3) the Ag/PPy ink prepared, method particularly includes: it according to mass ratio is 8:1:1 by Ag/PPy particle, conductive black and ring
Oxygen resin is added to and configures the Ag/PPy ink that the viscosity for being suitble to silk-screen printing is 0.2Pas in a certain amount of water；
4) preparation of supercapacitor, method particularly includes: the Ag/ for being prepared silver paste, step 3) by the silk screen plate of 300-400 mesh
PPy ink and PVA-H3PO4Solid electrolyte is sequentially overlapped printing on the substrate, forms supercapacitor pattern, then does
It is dry to obtain the final product.
2. a kind of preparation method based on Ag/PPy composite nano materials printing supercapacitor as described in claim 1,
It is characterized in that: being dried in the step 4) by baking oven, if stock is polyester, drying temperature should not be greater than 120 DEG C,
If stock is paper, drying temperature should not be greater than 100 DEG C, if stock is cotton, drying temperature should not be greater than 80 DEG C.
3. a kind of preparation method based on Ag/PPy composite nano materials printing supercapacitor as described in claim 1,
Be characterized in that: the supercapacitor pattern is pectination solid pattern.
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| CN109659164B (en) * | 2019-01-04 | 2021-01-05 | 西北工业大学 | Manufacturing method of planar comb tooth type super capacitor |
| US10526441B1 (en) | 2019-01-23 | 2020-01-07 | King Fahd University Of Petroleum And Minerals | Polypyrrole-coated silver particles for surface enhanced Raman scattering |
| CN112940690B (en) * | 2021-02-05 | 2021-11-02 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Phase change energy storage material with pod structure and preparation method and application thereof |
| CN116334948B (en) * | 2023-03-03 | 2024-04-19 | 金陵科技学院 | Polypyrrole/silver/cellulose composite paper-based material, and preparation method and application thereof |
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| CN103408933A (en) * | 2013-06-24 | 2013-11-27 | 金陵科技学院 | Preparation method of hollow high-electroactivity nano-silver/ polypyrrole composite material |
| CN104599862A (en) * | 2015-01-09 | 2015-05-06 | 上海应用技术学院 | Method for preparing polypyrrole/sliver nano composite material |
| CN104813425A (en) * | 2012-10-17 | 2015-07-29 | 新加坡科技设计大学 | High specific capacitance and high power density of printed flexible micro-supercapacitors |
| CN106783220A (en) * | 2016-12-19 | 2017-05-31 | 北京印刷学院 | A kind of preparation method of flexible all-solid-state supercapacitor |
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| CN104813425A (en) * | 2012-10-17 | 2015-07-29 | 新加坡科技设计大学 | High specific capacitance and high power density of printed flexible micro-supercapacitors |
| CN103408933A (en) * | 2013-06-24 | 2013-11-27 | 金陵科技学院 | Preparation method of hollow high-electroactivity nano-silver/ polypyrrole composite material |
| CN104599862A (en) * | 2015-01-09 | 2015-05-06 | 上海应用技术学院 | Method for preparing polypyrrole/sliver nano composite material |
| CN106783220A (en) * | 2016-12-19 | 2017-05-31 | 北京印刷学院 | A kind of preparation method of flexible all-solid-state supercapacitor |
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