CN110518207A - A kind of flexibility ammonium ion full battery and preparation method thereof - Google Patents
A kind of flexibility ammonium ion full battery and preparation method thereof Download PDFInfo
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- CN110518207A CN110518207A CN201910784541.0A CN201910784541A CN110518207A CN 110518207 A CN110518207 A CN 110518207A CN 201910784541 A CN201910784541 A CN 201910784541A CN 110518207 A CN110518207 A CN 110518207A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/38—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- Y02E60/10—Energy storage using batteries
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a kind of flexible ammonium ion full batteries and preparation method thereof, respectively using carbon fiber loaded ammonium vanadate, conducting polymer as positive and negative anodes active material, the two matches to obtain the flexible water system ammonium ion full battery with excellent electrochemical performance according to appropriate mass the present invention.Carbon fiber is used as collector and conductive additive simultaneously, reduces battery quality and volume, improves the flexibility of battery, and is easy to weave and integrate.The ammonium ion full battery being finally prepared has excellent chemical property, while its light weight, at low cost, flexibility is high, highly-safe and environmental-friendly, to provide possibility applied to wearable electronic devices field.
Description
Technical field
The present invention relates to energy storage device technical fields, and in particular to a kind of flexibility ammonium ion full battery and preparation method thereof.
Background technique
With the development of society, requirement of the mankind to energy storage device is higher and higher, flexible, safety, wearable metal ion
Battery is also widely used for various fields, but traditional secondary cell is mainly using organic solution as electrolyte, these solvents
It is usually toxic and inflammable, therefore there is very big safety problem in use.The appearance of aqueous rechargeable battery is good
Solve these problems, common water-soluble solution battery mainly uses metal ion such as Li+, Na+, K+, Ca2+, Mg2+, Zn2+Equal conducts
Carrier realizes the reversible storage and release of electric energy by the embedding dealkylation reaction of electrochemistry between positive and negative pole material.But it will be non-
Metal ion (NH4 +) as carrier system it is fresh for people pay close attention to, compared with metal ion, non-metal cations are not only showed
Lower molal weight (NH out4 +Only 18g mol-1), but also smaller aquo-ions size (3.31 angstroms) are provided, therefore
It can quickly spread in aqueous solution.Cui Yi seminar compares is inserted into different ions, including Li in prussian blue material+、Na+、K+、NH4 +Effect, find NH4 +There is excellent reaction potentiality and good cycle performance in terms of ion transmission
(J.Electrochem.Soc.2011,159,98).Recently, Ji Xiulei seminar is white as positive electrode using Prussia, and 3,
For 4,9,10- tetracarboxylic acid diimides as cathode, ammonium sulfate solution successfully assembles a kind of " rocking chair type " as electrolyte
The operating voltage of 1.0V, 43Whkg may be implemented in water system ammonium ion full battery, the system-1Energy density and 1000 weeks circulations
Service life (Angew.Chem.2017,56,13026).In spite of these effort, the exploration of water system ammonium ion full battery is still in rising
Step section, and it is far from satisfying practical application.The factor for restricting the development of high-performance ammonium ion full battery mainly has following two
Point: although (1) ammonium ion has the smallest aquo-ions size, NH4 +With Li+、Na+、K+Compared to relatively large ion half
Diameter, the positive electrode of suitable embedding de- ammonium ion stable therefore, it is difficult to find one.(2) performance of full battery is by positive and negative
The mutual restriction at the two poles of the earth, therefore it is critically important to find a matched negative electrode material.
Meanwhile flexible wearable electronic product shows the great demand to flexible battery, especially for high security
Flexible water system battery.However, while the flexible energy storage device qualified as one must have good bendability, it is also necessary to
The integrality and chemical property of retainer member during bending, the conventional batteries energy storage system developed at present, since it is adopted
With the electrode or collector of inflexibility, there is very poor flexibility, when bending inevitably damages battery structure, institute
To select the collector of a high flexibility critically important.Although ammonium ion battery has numerous advantages, almost do not have so far
About the report of flexible ammonium ion full battery.Therefore, energy density height, good rate capability, the flexibility having extended cycle life are developed
Ammonium ion full battery is extremely urgent.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of high securities, the flexible water system ammonium ion of low cost
Full battery and preparation method thereof.The battery has flexibility well, under different degrees of bending, can maintain stable electrification
Performance is learned, is had broad application prospects in wearable electronic field.
In order to reach above-mentioned technical effect, the present invention provides the following technical scheme that
A kind of preparation method of flexibility ammonium ion full battery, comprising the following steps:
(1) synthesis of carbon fiber loaded ammonium vanadate: carbon fiber is dried after acetone, ethyl alcohol, deionized water supersound washing,
Then acidification is carried out to it, obtains the carbon fiber of surface hydrophilic, vanadic acid is carried out to carbon fiber surface by hydrothermal synthesis method
Ammonium nano material cladding, obtains ammonium vanadate/carbon fibre material；
(2) one layer of cause the synthesis of carbon fiber loaded polyaniline: is deposited in carbon fiber surface by electrochemical cyclic voltammetry
Close Nano particles of polyaniline obtains polyaniline/carbon fibre material；
(3) using carbon fiber loaded ammonium vanadate as positive electrode active materials, carbon fiber loaded conducting polymer is as negative
Pole active material, ammonium sulfate solution are electrolyte, and positive electrode active materials and negative electrode active material are wrapped up diaphragm respectively, will be wrapped
One end of active material after wrapping up in is connected with copper conductor, then penetrates in heat-shrink tube, and one end with copper conductor is exposed at heat respectively
Draw both ends, the other end are placed in inside plastic catheter, finally, electrolyte is added, are purged by heat gun, shrink heat-shrink tube solid
Fixed and packaged device, obtains flexible ammonium ion full battery.
Further technical solution is that the ammonium vanadate is selected from NH4V4O10、(NH4)2V6O16、(NH4)4V6O16、(NH4)0.38V2O5、(NH4)2V3O8In any one or it is several.
Further technical solution is, in the step (2), the circle number of electro-deposition polyaniline is 10-30 circle.
Further, in the step (2), the circle number of electro-deposition polyaniline is 10-20 circle.
Wherein, the circle number of electro-deposition polyaniline encloses from 10 circles, 15 circles, 20 circles, 25, increases to 30 circles always.
Further technical solution is that the electrolyte is in ammonium sulfate, ammonium acetate, ammonium nitrate, ammonium chloride, ammonium carbonate
One or several kinds.
Further technical solution is that the concentration of the electrolyte is 1mol/L-10mol/L.
Further, the concentration of the electrolyte is 1mol/L-3mol/L.
The present invention also provides a kind of flexible ammonium ion full battery prepared by the preparation method, the full batteries
Include anode, cathode and electrolyte, wherein carbon fiber loaded ammonium vanadate is as positive electrode active materials；Carbon fiber loaded
Conducting polymer is as negative electrode active material.
Compared with prior art, the invention has the following beneficial effects: the present invention respectively with carbon fiber loaded ammonium vanadate,
As positive and negative anodes active material, the two matches to obtain the flexibility with excellent electrochemical performance according to appropriate mass conducting polymer
Water system ammonium ion full battery.Carbon fiber is used as collector and conductive additive simultaneously, reduces battery quality and volume, improves
The flexibility of battery, and be easy to weave and integrate, the flexible water system ammonium ion full battery that the present invention is prepared and assembled for the first time has
Excellent chemical property, in current density 100mA g-1When, specific capacity is up to 167mA hg-1, remain to protect after recycling 1000 circles
Hold 66mA h g-1Reversible capacity.Also, used aqueous electrolyte fundamentally solves organic electrolyte bring peace
Full property problem.Meanwhile also there is flexibility well, under different degrees of bending, stable chemical property, In can be maintained
Wearable electronic field has broad application prospects.
Detailed description of the invention
Fig. 1 is (a) ammonium vanadate/carbon fiber, (b) polyaniline/carbon fiber in water system ammonium ion full battery flexible in embodiment 1
The scanning electron microscope diagram piece of electrode；
Fig. 2 is water system ammonium ion full battery flexible in embodiment 1 in 0.1A g-1Charging and discharging curve when current density；
Fig. 3 is the schematic diagram of flexible water system ammonium ion full battery in embodiment 1；
Fig. 4 is flexibility water system ammonium ion full battery in embodiment 1 in the photo of differently curved angle.
Specific embodiment
The present invention is further explained and is illustrated combined with specific embodiments below.
Embodiment 1
A kind of preparation method of flexibility ammonium ion full battery, comprising the following steps:
(1) carbon fiber is dried after acetone, ethyl alcohol, deionized water supersound washing, is then dipped into 10% nitre
In acid solution, handled 5 hours in 70 DEG C, the carbon fiber for obtaining surface hydrophilic is spare.Weigh 0.56g ammonium metavanadate and 0.68g β-
Cyclodextrin, stirring be dissolved in the deionized water of 60mL, it is to be dissolved completely after, be added 0.65g oxalic acid；The carbon fiber handled well is set
In 100 milliliters of high pressure water heating kettles, above-mentioned mixed solution is then added, is reacted 20 hours in 120 DEG C.To take out carbon after reaction
Fiber is dried after cleaning, obtains carbon fiber loaded ammonium vanadate (CF@NH4V4O10)。
(1) by 0.1mol L-1Aniline and 0.5mol L-1Sulfuric acid dissolution is in 100mL deionized water.Using three electrodes into
Row cyclic voltammetry is deposited, and carbon fiber is saturated calomel and platinized platinum respectively as reference electrode and to electricity as working electrode
Pole, 20 circle of deposition in the voltage range of -0.2V to 0.9V.After the reaction was completed, carbon fiber electrode is taken out, ultrasound is washed in ethanol
Drying obtains carbon fiber loaded polyaniline (CF@PANI) after washing.
(3) above-mentioned CF@NH is taken4V4O10Fiber is with CF@PANI fiber respectively as the positive and negative anodes material of ammonium ion full battery
Material, 1M ammonium sulfate use diameter to encapsulate for the heat-shrink tube of 2mm, obtain flexible fiber shape ammonium ion full battery as electrolyte.
Embodiment 2
A kind of preparation method of flexibility ammonium ion full battery, comprising the following steps:
(1) carbon fiber is dried after acetone, ethyl alcohol, deionized water supersound washing, is then dipped into 10% nitre
In acid solution, handled 5 hours in 70 DEG C, the carbon fiber for obtaining surface hydrophilic is spare.Weigh 1.27g ammonium metavanadate and 0.68g grass
Acid, stirring be dissolved in the deionized water of 60mL, it is to be dissolved completely after, the carbon fiber handled well is placed in 100mL high pressure water heating kettle,
Then above-mentioned mixed solution is added, is reacted 20 hours in 180 DEG C.To take out carbon fiber after reaction, dries, obtain after cleaning
Carbon fiber loaded ammonium vanadate (CF@(NH4)2V3O8)。
(2) by 0.1mol L-1Aniline and 0.5mol L-1Sulfuric acid dissolution is in 100mL deionized water.Using three electrodes into
Row cyclic voltammetry is deposited, and carbon fiber is saturated calomel and platinized platinum respectively as reference electrode and to electricity as working electrode
Pole, 25 circle of deposition in the voltage range of -0.2V to 0.9V.After the reaction was completed, carbon fiber electrode is taken out, ultrasound is washed in ethanol
It is dried after washing, obtains carbon fiber loaded polyaniline (CF@PANI).
(3) above-mentioned CF@(NH is taken4)2V3O8Fiber is with CF@PANI fiber respectively as the positive and negative anodes material of ammonium ion battery
Material, 1M ammonium sulfate use diameter to encapsulate for the heat-shrink tube of 2mm, obtain flexible fiber shape ammonium ion full battery as electrolyte.
Embodiment 3
(1) carbon fiber is dried after acetone, ethyl alcohol, deionized water supersound washing, is then dipped into 10% nitre
In acid solution, handled 5 hours in 70 DEG C, the carbon fiber for obtaining surface hydrophilic is spare.Weigh 0.56g ammonium metavanadate and 0.68g β-
Cyclodextrin, stirring be dissolved in the deionized water of 60mL, it is to be dissolved completely after, be added 0.65g oxalic acid；The carbon fiber handled well is set
In 100 milliliters of high pressure water heating kettles, above-mentioned mixed solution is then added, is reacted 20 hours in 120 DEG C.To take out carbon after reaction
Fiber is dried after cleaning, obtains carbon fiber loaded ammonium vanadate (CF@NH4V4O10)。
(1) by 0.1mol L-1Aniline and 0.5mol L-1Sulfuric acid dissolution is in 100mL deionized water.Using three electrodes into
Row cyclic voltammetry is deposited, and carbon fiber is saturated calomel and platinized platinum respectively as reference electrode and to electricity as working electrode
Pole, 20 circle of deposition in the voltage range of -0.2V to 0.9V.After the reaction was completed, carbon fiber electrode is taken out, ultrasound is washed in ethanol
Drying obtains carbon fiber loaded polyaniline (CF@PANI) after washing.
(3) above-mentioned CF@NH is taken4V4O10Fiber is with CF@PANI fiber respectively as the positive and negative anodes material of ammonium ion full battery
Material, 1M ammonium acetate solution use diameter to encapsulate for the heat-shrink tube of 2mm, it is entirely electric to obtain flexible fiber shape ammonium ion as electrolyte
Pond.
The flexible water system ammonium ion full battery that the present invention is prepared and assembled for the first time has excellent chemical property, in electric current
Density 100mA g-1When, specific capacity is up to 167mA hg-1, 66mA h g is still able to maintain after recycling 1000 circles-1Reversible capacity.
Also, used aqueous electrolyte fundamentally solves organic electrolyte bring safety issue.Meanwhile also having very
Good flexibility can maintain stable chemical property under different degrees of bending, have in wearable electronic field wide
Application prospect.
Claims (6)
1. a kind of preparation method of flexibility ammonium ion full battery, which comprises the following steps: (1) carbon fiber loaded vanadium
The synthesis of sour ammonium: carbon fiber is dried after acetone, ethyl alcohol, deionized water supersound washing, acidification then is carried out to it, is obtained
To the carbon fiber of surface hydrophilic, ammonium vanadate nano material cladding is carried out to carbon fiber surface by hydrothermal synthesis method, obtains vanadic acid
Ammonium/carbon fibre material；(2) it the synthesis of carbon fiber loaded polyaniline: is deposited by electrochemical cyclic voltammetry in carbon fiber surface
One layer of fine and close Nano particles of polyaniline, obtains polyaniline/carbon fibre material；(3) using carbon fiber loaded ammonium vanadate as just
Pole active material, for carbon fiber loaded conducting polymer as negative electrode active material, ammonium sulfate solution is electrolyte, will be positive
Active material and negative electrode active material wrap up diaphragm respectively, one end of the active material after package are connected with copper conductor, then
It penetrating in heat-shrink tube, one end with copper conductor is exposed at heat-shrink tube both ends respectively, and the other end is placed in inside plastic catheter, finally,
Electrolyte is added, is purged by heat gun, so that heat-shrink tube is shunk fixed and packaged device, obtains flexible ammonium ion full battery.
2. the preparation method of flexibility ammonium ion full battery according to claim 1, which is characterized in that the ammonium vanadate is selected from
NH4V4O10、(NH4)2V6O16、(NH4)4V6O16、(NH4)0.38V2O5、(NH4)2V3O8In any one or it is several.
3. the preparation method of flexibility ammonium ion full battery according to claim 1, which is characterized in that in the step (2),
The circle number of electro-deposition polyaniline is 10-30 circle.
4. the preparation method of flexibility ammonium ion full battery according to claim 1, which is characterized in that the electrolyte is selected from
One of ammonium sulfate, ammonium acetate, ammonium nitrate, ammonium chloride, ammonium carbonate are several.
5. the preparation method of flexibility ammonium ion full battery according to claim 1, which is characterized in that the electrolyte it is dense
Degree is 1mol/L-10mol/L.
6. a kind of flexible ammonium ion that the preparation method as described in claim 1-5 any one claim is prepared is entirely electric
Pond.
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| CN111599978A (en) * | 2020-05-18 | 2020-08-28 | 西北工业大学 | Water system ammonium ion battery electrode based on pyrazine condensed ring semiconductor |
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