CN109859961A - A kind of preparation method of the flexible super capacitor electrode based on chemical & blended fabric - Google Patents
A kind of preparation method of the flexible super capacitor electrode based on chemical & blended fabric Download PDFInfo
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- CN109859961A CN109859961A CN201811267295.3A CN201811267295A CN109859961A CN 109859961 A CN109859961 A CN 109859961A CN 201811267295 A CN201811267295 A CN 201811267295A CN 109859961 A CN109859961 A CN 109859961A
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- 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
Abstract
The invention belongs to supercapacitor technologies fields, provide a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric, it is therefore an objective to prepare a kind of electrode material with superhigh-flexibility and excellent mechanical performance.A kind of its method specifically: using the chemical method for being similar to " silver mirror reaction " one layer of nano nickel conductive layer of homoepitaxial on chemical & blended fabric, in this, as electrode basement and collector.Hydro-thermal method growth in situ MnO in substrate is used again2Etc electrode active material, obtain the electrode with high specific capacitance and superhigh-flexibility.The invention belongs to supercapacitor technologies fields, and preparation process is simple, at low cost, have good application value in flexible electronic field.
Description
Technical field:
The invention belongs to supercapacitor technologies fields, and in particular, to a kind of flexible electrode based on chemical & blended fabric
Preparation method.
Background technique
Supercapacitor is a kind of novel energy storage apparatus between traditional capacitor and battery, it has power close
Degree is big, capacity is big, long service life, it is non-maintaining, economic and environment-friendly the advantages that.In recent years, people require electronic equipment to become small,
But do not want that allowing integrated bring power consumption to increase influences power and stand-by time.Traditional battery is not able to satisfy these gradually
It is required that this has pushed the development of supercapacitor.In addition, with the development of wearable, foldable flexible portable electronics, energy
The flexible super capacitor for being provided energy is increasingly becoming research hotspot.
The electrode material of flexible super capacitor mainly has carbon material, conducting polymer, metal oxide and hydroxide.
Wherein metal oxide has been demonstrated there is very high specific capacitance, such as MnO2Theoretical capacitance be 1370Fg-1.Super electricity
The electrode material of container usually require to be attached to high conductivity, high-specific surface area conducting base on, which claims
For collector.The common collector of flexible super capacitor can be divided into metal, carbon material, macromolecule three categories at present.
Common stainless (steel) wire, nickel foam and porous nano-Au as conductive substrates, above settling electrode active material, lead
The mixture of electric additive and adhesive.For example, Chinese invention document CN108538616A discloses a kind of nickel foam self-supporting
The plate-like MnO that nanometer sheet stacks2The preparation method of electrode of super capacitor first grows nanometer in foam nickel surface using hydro-thermal method
The plate-like MnO that piece stacks2Presoma, then presoma is calcined to the plate-like MnO for generating nanometer sheet and stacking2, obtain that there is excellent electrification
Learn the electrode of performance.However, they do not have real flexibility, easily corroded in aqueous electrolyte, and metal collector
Cause power density and energy density lower with the weight of additive.
Carbon cloth has preferable flexible and light, environmental protection, with three-dimensional porous structure, is conducive to ion diffusion and charge
Transmission, therefore it is often used as flexible electrode substrate.For example, Chinese invention document CN105810883A, which discloses a kind of flexibility, to be worn
The preparation method for wearing electrode is chemically treated and is loaded to it graphene and metal oxide using carbon cloth as matrix, obtained
Lesser internal resistance and higher energy density may be implemented in flexible electrode.But the price of carbon cloth is higher in the market, cause electrode at
This increase.
By weaving, knitting or obtained fabric is squeezed with biological fiber or chemical fibre, due to light weight, flexibility
Good, property at low cost, is chosen as optimal flexible super capacitor substrate.These fabrics equally have abundant three-dimensional porous
Structure facilitates the load for increasing active material.But it needs on surface to do conductive layer, and solves asking for binding force between interface
Topic.For example, Chinese invention document CN102779648B discloses a kind of preparation method of supercapacitor flexible electrode, pass through
Magnetron sputtering does conductive gold plating on the fabric, then loads conducting polymer PPy and be made into flexible compound electrode, can be realized simultaneously
Good chemical property and flexible, stretchable characteristic.Though this technique uses fabric, magnetron sputtering Au undoubtedly increases preparation
Cost.
In view of the above problems, the present invention proposes a kind of preparation side of flexible super capacitor electrode based on chemical & blended fabric
Method, it is easy to operate, at low cost, it is of great significance to the application field of flexible super capacitor.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of, and the flexible super capacitor based on chemical & blended fabric is electric
The preparation method of pole, it is intended to guarantee to improve its flexibility while electrode high specific capacitance energetically.
In order to achieve the above object, the invention adopts the following technical scheme: preparing a kind of chemical & blended fabric compliant conductive first
Substrate, then growth in situ MnO2Etc electrode active material.
The present invention is achieved through the following technical solutions, a kind of preparation method of the flexible electrode based on chemical & blended fabric, tool
Body the following steps are included:
Step S1: preparing one piece of chemical & blended fabric for being cut into suitable dimension, successively washed with dehydrated alcohol and deionized water,
Drying.
Step S2: preparation contains Ni2+Precursor liquid-A liquid, specially Ni2+, trisodium citrate or ascorbic acid, chloroplatinic acid
Or the mixed aqueous solution of gold chloride, it is uniformly mixed, and adjust pH value with NaOH；
Step S3: reducing solution-B liquid, i.e. hydrazine hydrate (NH are prepared4·H2O) aqueous solution, and pH value is adjusted with NaOH；
Step S4: ready chemical & blended fabric being attached in the walls of beaker equipped with A liquid, then pours into B liquid, then in certain temperature
Spend lower heating water bath for a period of time；
Step S5: to cool down after reaction, taking out the fabric that is attached in walls of beaker, successively with dehydrated alcohol and go from
Sub- water washing, drying, obtains flexible conducting substrate；
Step S6: preparing liquor potassic permanganate, and trace catalyst is added, is then transferred in ptfe autoclave, puts
Enter flexible conducting substrate after cropped, a period of time is reacted in air dry oven；
Step S7: to cool down after reaction, substrate is taken out, is successively washed with dehydrated alcohol and deionized water, dried, i.e.,
Flexible super capacitor electrode can be obtained.
Preferably, the cut size of the chemical & blended fabric can be 10 × 20cm.This can preferably guarantee that conductive layer is equal
Preparation section and cost are reduced to the greatest extent while even property.
Preferably, described to contain Ni2+Precursor liquid in, Ni2+Concentration range be 0.01~2M, trisodium citrate or anti-
The concentration range of bad hematic acid is 0.01~2M, and the concentration range of chloroplatinic acid or gold chloride is 0.01~5mM.Each material concentration range
Selection be according to the amount and crystal seed growing principle of substance each in redox reaction combine a large amount of experimentation obtain.
Preferably, in the reducing solution, the concentration range of hydrazine hydrate is 0.01~1M.It should be preferably according to reducing agent excess
What principle obtained, guarantee that material is not wasted and reacted and can sufficiently carry out.
Preferably, the pH value is about 12, and naoh concentration range is 0.01~1M.This preferably facilitates hydrazine hydrate hair
Its reproducibility is waved, preferably progress redox reaction.
Preferably, the reaction temperature of the flexible conducting substrate is 40~160 DEG C, and the reaction time is 30min~5h.This is excellent
Selecting can guarantee to react abundant progress, obtain ideal flexible conducting substrate.
Preferably, the growth in situ MnO2During, KMnO4Concentration range be 0.005~1M, NH4The concentration of Cl
Range is 0.01~5mM.This preferably obtains according to reactant excess principle, guarantee material do not waste and react can sufficiently into
Row.
Preferably, the growth in situ MnO2During, oven temperature is 50~150 DEG C, and the reaction time is 6~48h.
When reaction time is shorter, the short and quality specific capacitance of the electrode obtained time-consuming is higher；When reaction time is longer, active material on electrode
Load capacity is larger, and area specific capacitance is higher.
Preferably, in the step S6 react a period of time after in substrate growth in situ active material, it is described activity material
Material removes MnO2Outside also alternatively at other systems, such as NiO, Ni (OH)2、MoO3、MoS2、Co3O4、TiO2、ZnO、Fe3O4、NaxWO3、
LiCoO2Deng.
Chemical & blended fabric surface homoepitaxial is shown as by the flexible conducting substrate that aforementioned preparation process is prepared
One layer of nano nickel conductive layer, pattern are thorniness ball or pointed cone array, and thickness is about 500nm；Base conductive is good, through four probes
Method tests its surface resistance < 1 Ω；With good bend resistance and anti-washing performance, bent 100000 times using bar folder or in water
Performance does not have significant change after more days of middle soaking and stirring.
Another object of the present invention is the provision of a kind of flexible super capacitor electrode based on chemical & blended fabric, the flexibility
Electrode of super capacitor is prepared by preparation method above-mentioned；The flexible electrode has fabric fibre-nano nickel conductive
The composite construction of layer-manganese dioxide nano-plates, integral thickness is between 0.1~2mm；It is flexible, it can bend resistance and washing；0
Carry out charge and discharge cycles can be stablized under the voltage window of~1V, quality specific capacitance is about 80~200Fg-1；After circulation 1000 times,
Capacity retention is 82.6%.
When the electrode is tested in aqueous electrolyte, Na is may be selected in electrolyte2SO4、K2SO4、Li2SO4、NaCl、
KCl、LiCl、NaNO3、KNO3、LiNO3Deng.
Another object of the present invention be it is subsequent be assembled into all-solid-state flexible supercapacitor, be applied to flexible electronic lead
Domain.
Specifically, the electrode can be used for subsequent all-solid-state flexible supercapacitor assembling, by two plate electrodes to folded, centre
The gel electrolyte that different systems can be used is assembled, including polyvinyl alcohol (PVA)/LiCl, PVA/H3PO4, polyacrylic acid
(PAA), Sodium Polyacrylate (PAAS) etc., finally obtains the all-solid-state supercapacitor with superhigh-flexibility.
Detailed description of the invention:
Fig. 1 is the both macro and micro shape appearance figure of flexible conducting substrate in the present invention.Wherein, (1b), (1c), (1d) are respectively
The scanning electron microscope image of (1a) under different amplification.
Fig. 2 is flexible conducting substrate different location (being detailed in (2a), (2b), (2c)) multimeter visual representation in the present invention
Resistance situation.
Fig. 3 is the situation of change of flexible conducting substrate surface resistance in bending and water-washing process in the present invention.Wherein, (3a)
Influence for bending number to surface resistance, (3b) are the influence for impregnating number of days opposite resistance in water.
Fig. 4 is flexibility MnO in the present invention2The scanning electron microscope image of electrode.
Fig. 5 is flexibility MnO in the present invention2Electrode sweeps the cyclic voltammogram under speed in difference.Wherein, abscissa represents work
Current potential (V), ordinate represent operating current (A), and electrolyte is 1M Na2SO4Solution.
Fig. 6 is flexibility MnO in the present invention2Electrode is in 1Ag-1Cycle performance figure under current density.Wherein, abscissa is
Cycle-index, ordinate are capacity retention ratio, and electrolyte is 1M Na2SO4Solution.
Wherein:
As shown in Figure 1, the fabric fibre marshalling of flexible conducting substrate, one layer of partial size of surface homoepitaxial are about
The nano nickel pointed cone array of 50nm.
As shown in Figure 2, the electric conductivity of flexible conducting substrate is uniformly and good.
From the figure 3, it may be seen that flexible conducting substrate has excellent bend resistance and anti-washing performance.
As shown in Figure 4, flexible electrode upper surface is the MnO of sheet2, there is big specific surface area.
As shown in Figure 5, flexible electrode can be assembled into fake capacitance supercapacitor, and quality specific capacitance is about 80~200Fg-1。
It will be appreciated from fig. 6 that flexible electrode can stablize carry out charge and discharge cycles under the voltage window of 0~1V, work as current density
For 1Ag-1When, recycling 1000 capacity retentions is 82.6%.
Specific embodiment:
With embodiment and attached drawing, the invention will be further described below, and however, it is not limited to this.
Embodiment 1:
The preparation method of flexible conducting substrate, comprises the following steps:
Step S1 prepares one piece of chemical & blended fabric for being cut into 10 × 20cm, is successively washed with dehydrated alcohol and deionized water,
Drying.
Step S2, preparation contain Ni2+Precursor liquid-A liquid: weigh 1.1g nickel chloride, 5.6mg chloroplatinic acid and 1.8g citric acid
Trisodium is added in 30mL deionized water, is uniformly mixed.
Step S3 prepares reducing solution-B liquid: measuring 4mL hydrazine hydrate (40~50%) and is added in 26mL deionized water, stirs
It mixes uniformly mixed.
Step S4 prepares sodium hydrate aqueous solution: weighing 0.4g NaOH and is added in 40mL deionized water, is stirred
Uniformly, 20mL sodium hydrate aqueous solution is separately added into A liquid and B liquid.
Ready chemical & blended fabric is attached in the walls of beaker equipped with A liquid, then pours into B liquid by step S5, then at 80 DEG C
Heating water bath 1h；To cool down after reaction, the fabric being attached in walls of beaker is taken out, successively uses dehydrated alcohol and deionized water
Washing, drying, obtains flexible conducting substrate.
The flexible conducting substrate that the present embodiment obtains, surface smooth pieces have metallic luster, nano nickel pointed cone array partial size
About 50nm, it is shown referring to Fig.1；Good conductivity, surface resistance < 1 Ω, referring to shown in Fig. 2；It is washed with good bend resistance and water resistant
Performance, referring to shown in Fig. 3, (3a) is the influence for bending number to surface resistance, and (3b) is to impregnate number of days opposite resistance in water
It influences.
Embodiment 2:
Flexible MnO based on chemical & blended fabric2The preparation method of electrode, comprises the following steps:
Prepare flexible conducting substrate: with embodiment 1；Further comprise:
Step S6 prepares liquor potassic permanganate: weighing 0.0316g KMnO4It is added in 10mL deionized water, adds
0.001g NH4Cl catalyst is then transferred into the ptfe autoclave that capacity is 50mL；Flexible conducting substrate is cut out
It is cut to the size of 1 × 2cm, is put into reaction kettle, then reacts 6h in 90 DEG C of baking ovens；
Step S7 takes out electrode, is successively washed with dehydrated alcohol and deionized water to cool down after reaction, dries, i.e.,
Flexible MnO can be obtained2Electrode.
The flexible MnO based on chemical & blended fabric that the present embodiment obtains2Electrode referring to shown in Fig. 4 there is fabric fibre-to receive
Rice nickel pointed cone array-manganese dioxide nano-plates composite construction, integral thickness is flexible between 0.1~2mm, can bend resistance
And washing.
Embodiment 3:
Electrochemical property test comprises the following steps:
In the present embodiment, by flexibility MnO made from embodiment 22Electrode is made into electrode of super capacitor and carries out electrochemistry
It can test.Test results are shown in figure 5, when electrolyte is 1M Na2SO4When solution, the quality specific capacitance of electrode is about 80~
200F·g-1.It will be appreciated from fig. 6 that when current density is 1Ag-1When, recycling 1000 capacity retentions is 82.6%.
It can illustrate the flexible super capacitor electrode based on chemical & blended fabric that present invention production obtains from the above, no
Only there is excellent mechanical property and superhigh-flexibility, specific capacitance also with higher and cyclical stability, and preparation process is simple,
It is at low cost, there is good application value in flexible super capacitor and flexible electronic field.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the flexible super capacitor electrode based on chemical & blended fabric, which is characterized in that comprise the steps of:
Step S1: prepare one piece of chemical & blended fabric for being cut into suitable dimension, successively washed with dehydrated alcohol and deionized water, dried
It is dry；
Step S2: preparation contains Ni2+Precursor liquid-A liquid, specially Ni2+, trisodium citrate or ascorbic acid, chloroplatinic acid or chlorine
The mixed aqueous solution of auric acid, is uniformly mixed, and adjusts pH value with NaOH；
Step S3: reducing solution-B liquid, i.e. hydrazine hydrate (NH are prepared4·H2O) aqueous solution, and pH value is adjusted with NaOH；
Step S4: ready chemical & blended fabric is attached in the walls of beaker equipped with A liquid, then pours into B liquid, then at a certain temperature
Heating water bath is for a period of time；
Step S5: to cool down after reaction, the fabric being attached in walls of beaker is taken out, successively uses dehydrated alcohol and deionized water
Washing, drying, obtains flexible conducting substrate；
Step S6: preparing liquor potassic permanganate, and trace catalyst is added, is then transferred in ptfe autoclave, be put into through
Flexible conducting substrate after cutting reacts a period of time in air dry oven；
Step S7: to cool down after reaction, substrate is taken out, is successively washed with dehydrated alcohol and deionized water, dried, can obtain
To flexible super capacitor electrode.
2. a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric according to claim 1, special
Sign is, the Ni in the step S22+Selected from one or more of nickel chloride, nickel sulfate, nickel nitrate, nickel acetate；In solution
Ni2+Concentration range be 0.01~2M, the concentration range of trisodium citrate or ascorbic acid is 0.01~2M, chloroplatinic acid or chlorine gold
The concentration range of acid is 0.01~5mM, and the concentration range of sodium hydroxide is 0.01~1M, and adjusting PH is about 12.
3. a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric according to claim 1, special
Sign is that the concentration range of the hydrazine hydrate in the step S3 is 0.01~1M, and the concentration range of sodium hydroxide is 0.01~1M,
Adjusting PH is about 12.
4. a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric according to claim 1, special
Sign is, the heating in water bath for reaction condition at a certain temperature in the step S4 specifically: reaction temperature is 40~160 DEG C,
Reaction time is 30min~5h.
5. a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric according to claim 1, special
Sign is, the flexible conducting substrate in the step S5 shows themselves in that fabric fibre marshalling, and one layer of surface homoepitaxial is received
Rice nickel conductive layer, pattern are thorniness ball or pointed cone array, and substrate surface resistance < 1 Ω can bend resistance and washing.
6. a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric according to claim 1, special
Sign is that the concentration range of the potassium permanganate in the step S6 is 0.005~1M, catalyst NH4Cl, concentration range are
0.01~5mM；Reaction temperature is 50~150 DEG C, and the reaction time is 6~48h.
7. a kind of preparation method of flexible super capacitor electrode based on chemical & blended fabric according to claim 1, special
Sign is that growth in situ active material, the active material remove MnO in substrate after reaction a period of time in the step S62
Outside also alternatively at other systems, such as NiO, Ni (OH)2、MoO3、MoS2、Co3O4、TiO2、ZnO、Fe3O4、NaxWO3、LiCoO2
Deng.
8. a kind of flexible super capacitor electrode based on chemical & blended fabric, which is characterized in that the flexible super capacitor electrode
It is prepared by any one of claim 1-7 preparation method, there is fabric fibre-nano nickel conductive layer-manganese dioxide nano
The composite construction of piece, integral thickness is flexible between 0.1~2mm, can stablize carry out charge and discharge under the voltage window of 0~1V
Electricity circulation, quality specific capacitance is about 80~200Fg-1。
9. a kind of flexible super capacitor electrode based on chemical & blended fabric according to claim 8, which is characterized in that described
When electrode is tested in aqueous electrolyte, Na is may be selected in electrolyte2SO4、K2SO4、Li2SO4、NaCl、KCl、LiCl、
NaNO3、KNO3、LiNO3Deng.
10. a kind of flexible super capacitor electrode based on chemical & blended fabric according to claim 8, which is characterized in that institute
Stating electrode can be used for subsequent all-solid-state flexible supercapacitor assembling, and by two plate electrodes to folding, different systems are can be used in centre
Gel electrolyte is assembled, including polyvinyl alcohol (PVA)/LiCl, PVA/H3PO4, polyacrylic acid (PAA), Sodium Polyacrylate
(PAAS) etc., the all-solid-state supercapacitor with superhigh-flexibility is finally obtained, flexible electronic field is applied to.
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| RU2807173C1 (en) * | 2023-04-18 | 2023-11-10 | Общество с ограниченной ответственностью "КАРБОКС-ЭЛЕКТРОД" (ООО "КАРБОКС-ЭЛЕКТРОД") | Method for producing flexible electrode material |
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