CN108010745B - One kind being based on Ag/PPy/MnO2Stretchable Asymmetric Supercapacitor and preparation method thereof - Google Patents
One kind being based on Ag/PPy/MnO2Stretchable Asymmetric Supercapacitor and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to one kind to be based on Ag/PPy/MnO2The preparation method of the stretchable Asymmetric Supercapacitor of composite nano materials, the Ag/PPy/MnO of preparation2Composite nano materials have the series of advantages such as excellent capacitive property, good flexible, the high and low cost of stability and good printability, super Stretchable fabric substrate flexible are selected, by silver paste, the Ag/PPy/MnO of synthesis by way of silk-screen printing2Composite nano materials, active carbon and PVA-Na2SO4Solid electrolyte is printed as flexible solid Asymmetric Supercapacitor.The energy density of the Asymmetric Supercapacitor of manufacture of the invention is up to 30.9 μ Wh cm‑2, 90.8% capacity retention is possessed after 5000 constant current charge-discharges, 89.2% capacitor is possessed after 40% stretching and is kept.Meanwhile the Asymmetric Supercapacitor of manufacture (stretching distorts, and crimps, bending) under the conditions of different flexibilities remains flexibility and mechanical performance well, and puts the LED light of the 2.8V of shiny red under the above conditions.
Description
Technical field
The present invention relates to one kind to be based on Ag/PPy/MnO2The stretchable Asymmetric Supercapacitor of composite nano materials and its
Preparation method.
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.
The fast development in portable wearable electronic field is accelerated to super flexible, stretchable high-performance super capacitor
Demand.Currently, existing stretchable capacitor is faced with low energy density, tensility energy deficiency and manufacturing process complexity,
Limit its practical application.Therefore, how improving the energy density of existing supercapacitor while simplifying its manufacturing process is
Current key task.
Summary of the invention
The study found that the electric conductivity of active material can have a direct connection to supercapacitor capacitive character, polypyrrole with
Manganese dioxide is widely studied as the active material of two kinds of cheap high theoretical specific capacitances, however it is applied to supercapacitor quilt
Not high electric conductivity itself is limited, and the less flexible of manganese dioxide has obtained very after the silver for introducing high flexibility, polypyrrole
Big improvement, therefore silver, polypyrrole and manganese dioxide are carried out compound being a kind of acquisition high capacitance performance high flexibility active material
Feasible program.Meanwhile the voltage window of supercapacitor largely affects its energy density, asymmetric super capacitor
The preparation of device is the research hotspot in the current field, therefore by the Ag/PPy/MnO of preparation2Composite nano materials and active carbon point
The voltage window of raising supercapacitor that can be very not big as cathode electrode material and anode electrode material, is a kind of acquisition
The feasible program of high-energy density super capacitor.The development of nanosecond science and technology is Ag/PPy/MnO2The preparation of composite nano materials
The technical conditions provided convenience, researcher has prepared that capacitive property is good, stable circulation by the way of silk-screen printing at present
Property strong and excellent mechanical performance flexible extensible Asymmetric Supercapacitor, and be applied to flexibility 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.
The purpose of the invention is to provide to be based on Ag/PPy/MnO2Composite nano materials printing is stretchable asymmetric super
The preparation method of capacitor, to prepare the cheap flexible extensible Asymmetric Supercapacitor haveing excellent performance, realization pair
The substitution and supplement of the high energy storage device of traditional price, and have reaction step simple, the reaction time is short, easy to operate etc.
Advantage can be used for industrial mass preparation and production, and can be applied to flexible energy storage field.
In order to achieve the above object, present invention provide the technical scheme that a kind of be based on Ag/PPy/MnO2Composite Nano material
The preparation method of the stretchable Asymmetric Supercapacitor of material, includes the following steps:
1)Ag/PPy/MnO2The synthesis of composite nano materials, method particularly includes: nitre is sequentially added in mass ratio for 5:20:2
Sour silver, polyvinylpyrrolidone and acetate stir to get mixed solution, then, by the mixed solution room into a certain amount of water
The pyrrole monomer and ferric trichloride that mass ratio is 1:2 is added by peristaltic pump in temperature stirring 30-40min, and the reaction was continued 2-3h will
It is added in a certain amount of certain density liquor potassic permanganate after obtained product cleaning 3 times or more, is reacted under the conditions of 120 DEG C
2-3h；
2)Ag/PPy/MnO2The cleaning of composite nano materials and Ag/PPy/MnO2The preparation of particle, method particularly includes: pass through
Ethyl alcohol is by the obtained Ag/PPy/MnO of step 1)2Composite nano materials are by being centrifuged cleaning in 10 minutes 3 times or more, then by it
It is distributed in dehydrated alcohol, and its mass fraction is made to reach 60%, 6-8h is dried under conditions of 60 DEG C by baking oven；
3) Ag/PPy/MnO is prepared2Ink, active carbon ink, method particularly includes: it according to mass ratio is 8:1:1 by Ag/
PPy/MnO2Particle, conductive black and epoxy resin be added in a certain amount of water configure be suitble to silk-screen printing viscosity be
The Ag/PPy/MnO of 0.2Pas2Ink adds active carbon particle, conductive black and epoxy resin for 6:1:1 according to mass ratio
The active carbon ink for being suitble to that the viscosity of silk-screen printing is 0.2Pas is configured into a certain amount of water；
4) preparation of Asymmetric Supercapacitor, method particularly includes: by the silk screen plate of 300-400 mesh by silver paste, step
3) Ag/PPy/MnO prepared2Ink, active carbon ink and PVA-Na2SO4Solid electrolyte, which is sequentially overlapped, is printed on printing
On object, various supercapacitor patterns are formed, are then drying to obtain.
Further, the molar concentration of the step 1) liquor potassic permanganate is 0.6mmol/L.
Further, the step 4) stock is flexible fabric, and drying temperature is no more than 80 DEG C.
The present invention also provides a kind of stretchable Asymmetric Supercapacitor based on Ag/PPy/MnO2 composite nano materials,
It is prepared by any claim the method for claims 1 to 3.
Further, the energy density of the Asymmetric Supercapacitor is 30.9 μ Wh cm-2, after 5000 constant current charge-discharges
Possess 90.8% capacity retention, 89.2% capacity retention is possessed after 40% stretching.
Compared with prior art, the advantages of the present invention:
1, the Ag/PPy/MnO of the method for the present invention preparation2Composite nano materials have excellent capacitive property, good soft
Property, the series of advantages such as the high and low cost of stability and good printability, be conducive to flexible supercapacitor, stability and
The promotion of electric property substantially increases the practicability 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.By controlling the stock of silk-screen printing, the asymmetric super capacitor of flexible extensible can be prepared on super flexible fabric
Device.
3, the Ag/PPy/MnO of the invention by preparation2Composite nano materials and active carbon respectively as cathode electrode material with
Anode electrode material, the voltage window of raising supercapacitor that can be very big, to greatly enhance super capacitor
The energy density of device.
3, the energy density of the Asymmetric Supercapacitor prepared is up to 30.9 μ Wh cm-2, after 5000 constant current charge-discharges
Possess 90.8% capacity retention, 89.2% capacity retention is possessed after 40% stretching.Meanwhile it is produced by the present invention non-
Symmetrical supercapacitor (stretches, distortion crimps, bending) under the conditions of different flexibilities remains flexible well and machinery
Performance, and the LED light of the 2.8V of shiny red is put under the above conditions.
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.It will
It is anti-under the conditions of 120 DEG C in the liquor potassic permanganate for the 0.6mmol/L for being added to 20mL after obtained product cleaning 3 times or more
Answer 2h.2) by synthesized Ag/PPy/MnO2Composite nano materials carry out cleaning and Ag/PPy/MnO2The preparation of particle, specific side
Method are as follows: be then dispersed in product obtained by being centrifuged at 10000 turns cleaning in 10 minutes 3 times or more by ethyl alcohol
In dehydrated alcohol, and its mass fraction is made to reach 60%, 6h is dried under conditions of 60 DEG C by baking oven.3) Ag/PPy/ is prepared
MnO2Ink, active carbon ink, method particularly includes: 0.8g Ag/PPy/MnO is added for 8:1:1 according to mass ratio2Composite Nano
It is 0.2Pas that particle, 0.1g conductive black and 0.1g epoxy resin, which are added to and configure the viscosity for being suitble to silk-screen printing in the water of 5mL,
Ag/PPy/MnO2Ink is that 0.6g active carbon particle, 0.1g conductive black and 0.1g epoxy is added in 6:1:1 according to mass ratio
Resin is added to and configures the active carbon ink that the viscosity for being suitble to silk-screen printing is 0.2Pas in the water of 6mL.4) asymmetric super electricity
The preparation of container, method particularly includes: the Ag/PPy/MnO for being prepared silver paste, above-mentioned steps by the silk screen plate of 400 mesh2Ink,
Active carbon ink and PVA-Na2SO4Solid electrolyte, which is sequentially overlapped, is printed as various supercapacitor patterns.5) pass through baking oven
The Asymmetric Supercapacitor that silk-screen printing is obtained is dry, and drying temperature should not be greater than 80 DEG C.What is prepared is asymmetric super
The energy density of capacitor is up to 30.9 μ Wh cm-2, possess 90.8% capacity retention after 5000 constant current charge-discharges, 40%
Stretching after possess 89.2% capacitor keep.Meanwhile the Asymmetric Supercapacitor that the embodiment of the present invention 1 manufactures is different
(stretching, distort, crimp, bending) under the conditions of flexibility remains flexible and mechanical performance, and point under the above conditions well
The LED light of the 2.8V of shiny red.
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.It will
It is anti-under the conditions of 120 DEG C in the liquor potassic permanganate for the 0.6mmol/L for being added to 200mL after obtained product cleaning 3 times or more
Answer 2h.2) by synthesized Ag/PPy/MnO2Composite nano materials carry out cleaning and Ag/PPy/MnO2The preparation of particle, specific side
Method are as follows: be then dispersed in product obtained by being centrifuged at 10000 turns cleaning in 10 minutes 3 times or more by ethyl alcohol
In dehydrated alcohol, and its mass fraction is made to reach 60%, 6h is dried under conditions of 60 DEG C by baking oven.3) Ag/PPy/ is prepared
MnO2Ink, active carbon ink, method particularly includes: 0.8 g Ag/PPy/MnO is added for 8:1:1 according to mass ratio2Composite Nano
It is 0.2Pas that particle, 0.1g conductive black and 0.1g epoxy resin, which are added to and configure the viscosity for being suitble to silk-screen printing in the water of 5mL,
Ag/PPy/MnO2Ink is that 0.6 g active carbon particle, 0.1g conductive black and 0.1g epoxy is added in 6:1:1 according to mass ratio
Resin is added to and configures the active carbon ink that the viscosity for being suitble to silk-screen printing is 0.2Pas in the water of 6mL.4) asymmetric super electricity
The preparation of container, method particularly includes: the Ag/PPy/MnO for being prepared silver paste, above-mentioned steps by the silk screen plate of 400 mesh2Ink,
Active carbon ink and PVA-Na2SO4Solid electrolyte, which is sequentially overlapped, is printed as various supercapacitor patterns.5) pass through baking oven
The Asymmetric Supercapacitor that silk-screen printing is obtained is dry, and drying temperature should not be greater than 80 DEG C.What is prepared is asymmetric super
The energy density of capacitor is up to 30.9 μ Wh cm-2, possess 90.8% capacity retention after 5000 constant current charge-discharges, 40%
Stretching after possess 89.2% capacitor keep.Meanwhile the Asymmetric Supercapacitor that the embodiment of the present invention 2 manufactures is in difference
Flexibility under the conditions of (stretch, distort, crimp, bending) and remain flexible well and mechanical performance, and under the above conditions
The LED light of the 2.8V of point shiny red.
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.
In the liquor potassic permanganate for the 0.6mmol/L for being added to 32mL later for product cleaning 3 times or more obtained, under the conditions of 120 DEG C
React 2h.2) by synthesized Ag/PPy/MnO2Composite nano materials carry out cleaning and Ag/PPy/MnO2The preparation of particle, specifically
Method are as follows: then dispersed product obtained by being centrifuged at 10000 turns cleaning in 10 minutes 3 times or more by ethyl alcohol
Into dehydrated alcohol, and its mass fraction is made to reach 60%, 6h is dried under conditions of 60 DEG C by baking oven.3) Ag/ is prepared
PPy/MnO2Ink, active carbon ink, method particularly includes: 0.8g Ag/PPy/MnO is added for 8:1:1 according to mass ratio2It is compound
Nano particle, 0.1g conductive black and 0.1g epoxy resin be added in the water of 5mL configure be suitble to silk-screen printing viscosity be
The Ag/PPy/MnO of 0.2Pas2Ink, according to mass ratio be 6:1:1 be added 0.6g active carbon particle, 0.1g conductive black and
0.1g epoxy resin is added to and configures the active carbon ink that the viscosity for being suitble to silk-screen printing is 0.2Pas in the water of 6mL.4) non-right
Claim the preparation of supercapacitor, method particularly includes: the Ag/PPy/ for being prepared silver paste, above-mentioned steps by the silk screen plate of 400 mesh
MnO2Ink, active carbon ink and PVA-Na2SO4Solid electrolyte, which is sequentially overlapped, is printed as various supercapacitor patterns.
5) Asymmetric Supercapacitor obtained silk-screen printing by baking oven is dry, and drying temperature should not be greater than 80 DEG C.Preparation
The energy density of Asymmetric Supercapacitor is up to 30.9 μ Wh cm-2, 90.8% capacitor is possessed after 5000 constant current charge-discharges
Conservation rate possesses 89.2% capacitor holding after 40% stretching.Meanwhile the asymmetric super electricity that the embodiment of the present invention 1 manufactures
Container (stretches, distortion crimps, bending) under the conditions of different flexibilities remains flexible and mechanical performance well, and
The LED light of the 2.8V of shiny red is put under above-mentioned condition.
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 (5)
1. a kind of preparation method of the stretchable Asymmetric Supercapacitor based on Ag/PPy/MnO2, which is characterized in that including such as
Lower step:
1)Ag/PPy/MnO2The synthesis of composite nano materials, method particularly includes: in mass ratio for 5:20:2 sequentially add silver nitrate,
Polyvinylpyrrolidone and acetate stir to get mixed solution into a certain amount of water, and then, which is stirred at room temperature
The pyrrole monomer and ferric trichloride that mass ratio is 1:2, the reaction was continued 2-3h, by what is obtained is added by peristaltic pump in 30-40min
It is added in a certain amount of certain density liquor potassic permanganate after product cleaning 3 times or more, reacts 2-3h under the conditions of 120 DEG C；
2)Ag/PPy/MnO2The cleaning of composite nano materials and Ag/PPy/MnO2The preparation of particle, method particularly includes: pass through ethyl alcohol
By the obtained Ag/PPy/MnO of step 1)2Then composite nano materials are by being dispersed at centrifugation cleaning in 10 minutes 3 times or more
Into dehydrated alcohol, and its mass fraction is made to reach 60%, 6-8h is dried under conditions of 60 DEG C by baking oven；
3) Ag/PPy/MnO is prepared2Ink, active carbon ink, method particularly includes: it according to mass ratio is 8:1:1 by Ag/PPy/MnO2
Particle, conductive black and epoxy resin are added to and configure the Ag/ that the viscosity for being suitble to silk-screen printing is 0.2Pas in a certain amount of water
PPy/MnO2Active carbon particle, conductive black and epoxy resin are added in a certain amount of water according to mass ratio for 6:1:1 by ink
Configure the active carbon ink for being suitble to that the viscosity of silk-screen printing is 0.2Pas；
4) preparation of Asymmetric Supercapacitor, method particularly includes: silver paste, step 3) are made by the silk screen plate of 300-400 mesh
Standby Ag/PPy/MnO2Ink, active carbon ink and PVA-Na2SO4Solid electrolyte is sequentially overlapped printing on the substrate,
Various supercapacitor patterns are formed, are then drying to obtain；The stock is flexible fabric.
2. a kind of preparation method of the stretchable Asymmetric Supercapacitor based on Ag/PPy/MnO2 as described in claim 1,
It is characterized by: the molar concentration of the step 1) liquor potassic permanganate is 0.6mmol/L.
3. a kind of preparation method of the stretchable Asymmetric Supercapacitor based on Ag/PPy/MnO2 as described in claim 1,
It is characterized by: the drying temperature in step 4) is no more than 80 DEG C.
4. a kind of stretchable Asymmetric Supercapacitor based on Ag/PPy/MnO2, it is characterised in that: appointed by claims 1 to 3
Meaning claim the method is prepared.
5. a kind of stretchable Asymmetric Supercapacitor based on Ag/PPy/MnO2 as claimed in claim 4, it is characterised in that:
The energy density of the Asymmetric Supercapacitor is 30.9 μ Wh cm-2, 90.8% capacitor is possessed after 5000 constant current charge-discharges
Conservation rate possesses 89.2% capacity retention after 40% stretching.
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| CN110144137B (en) * | 2019-05-06 | 2020-05-22 | 武汉大学 | CoHCF-based nanocube ink, and preparation method and application thereof |
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