CN108878796A - Graphene modified conductive polymer gel and its preparation method and application - Google Patents
Graphene modified conductive polymer gel and its preparation method and application Download PDFInfo
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- CN108878796A CN108878796A CN201710343106.5A CN201710343106A CN108878796A CN 108878796 A CN108878796 A CN 108878796A CN 201710343106 A CN201710343106 A CN 201710343106A CN 108878796 A CN108878796 A CN 108878796A
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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
- H01M4/364—Composites as mixtures
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/606—Polymers containing aromatic main chain polymers
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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
Abstract
The present invention discloses graphene modified conductive polymer gel and its preparation method and application, and graphene oxide is placed in distilled water, and phytic acid and aniline and evenly dispersed, the first mixed solution of formation is added；Ammonium persulfate is dispersed in distilled water, the second mixed solution is formed；Second mixed solution is added in the first mixed solution after ultrasonic disperse, reaction is stood in ice-water bath, so that aniline polymerization forms polyaniline completely, is reused sodium borohydride and is carried out graphene oxide reduction, in the first mixed solution, Sn nano particle is added as nano-electrode particle.The nanoparticle electrode that three-dimensional conductive macromolecule hydrogel network of the invention does carrier possesses preferable electronic and ionic transmittability and stable structure；In addition, the electrode also has good repeatability and stability, there are extensive Research Prospects in the fields such as high-energy density and slimline battery.
Description
Technical field
The invention belongs to the preparation sides that graphene modified conductive polymer gel is used for new type lithium ion battery cathode
Method.
Background technique
The novel negative electrode active materials such as tinbase, silicon substrate, germanium base have high theoretical capacity, can meet lithium ion battery to big
Power, micromation and high capacity demand for development.But all there is serious volume change in such material charge and discharge process,
This volume change will lead to the dusting of material, destroys the passivating film and consumption electrolyte of electrode surface, seriously affects electrode
Capacity and cycle performance.In order to solve problem above, the unification of novel electrode high capacity and good circulation stability is realized, it is right
Electrode, which is modified, just seems most important with microstructure design.
Conductive polymer gel is the polymer material for having both gel and organic conductor excellent properties simultaneously.Especially nanometer
The conductive polymer gel of structure is substituted in traditional electrode with high surface area and three-dimensional continuous conductive network with it
Binder and conductive agent, electrolyte can enter its internal micro-nano duct, be conducive to filling for active material and electrolyte solution
Tap touching has shorter lithium ion diffusion path relative to traditional two-dimensional film, improves electrode material in high magnification charge and discharge
Chemical property when electric, and the conductive network that is connected to for electronics provides quick transmission channel, it can be achieved that electrode material
Fast charging and discharging performance.In addition, conductive polymer gel has excellent machinability, casting, spraying or printing etc. can be passed through
Film or other desired shape is made in mode, this makes it have huge application value in terms of ultrathin flexible electrode and dive
Power.Although conductive polymer gel has numerous excellent properties, its conductivity and mechanical performance are relatively low, will affect electricity
The transmission of electronics in the material of pole, influences the cycle performance of battery.It based on this, needs to be modified it, to improve its conductance
Rate and mechanical stability.
Representative of the graphene as novel nano carbon material has excellent conductive characteristic, high mechanical strength and two dimension
Flexible structure, it is mutually compound with electrode material, the property such as specific capacity, cycle life and high-multiplying power discharge of active material can be effectively improved
Energy.Based on the above, by graphene be used for modified conductive polymer gel can not only improve simultaneously conducting polymer electric conductivity and
Mechanical strength, and when graphene can also absorb electrode material volume expansion as flexible substrate generated stress, help
In the structure and cyclical stability of enhancing electrode material.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide graphene modified conductive polymer gel and its systems
Preparation Method and application have extensive Research Prospects in fields such as ultra-thin and lithium ion battery with high energy densities.
Technical purpose of the invention is achieved by following technical proposals：
Graphene modified conductive polymer gel and preparation method thereof, carries out as steps described below：
Step 1, graphene oxide is placed in distilled water, phytic acid and aniline and evenly dispersed, the first mixing of formation is added
Solution；Ammonium persulfate is dispersed in distilled water, the second mixed solution is formed；
Step 2, the second mixed solution is added in the first mixed solution after ultrasonic disperse, reaction is stood in ice-water bath,
So that aniline polymerization forms polyaniline completely, polyaniline-graphene oxide plural gel is formed with graphene oxide；
Step 3, polyaniline-graphene oxide plural gel prepared by step 2 is restored using sodium borohydride, with
Graphene oxide is set to be reduced to graphene；
Step 4, the plural gel prepared by step 3 is freeze-dried.
In step 1, the mass ratio of graphene oxide and aniline is (1-8)：(5-10), preferably (3-6)：(8—
10)；The volume ratio of phytic acid and aniline is (1-2)：1.
In step 2, standing the reaction time is 10-30min.
In step 3, relative to graphene oxide, the dosage of sodium borohydride is excessive.
In step 1, in the first mixed solution, Sn nano particle is added as nano-electrode particle, particle size range is
20-50nm, and there is preferable dispersibility；The mass ratio of graphene oxide and aniline is (1-8)：(7-8), preferably (3-
6)：(7—8)；After adding nano-electrode particle, nano-electrode particle-polyaniline-graphene plural gel is formed.
In progress in use, copper foil is polished with abrasive paper for metallograph, rinses, after ultrasound, is dried for standby through distilled water and ethyl alcohol,
By on the sticky pasty solutions of the graphene modified conductive polymer gel-forming copper foil that is uniformly spun on that treated, spontaneously dry
The static pressure 30min under 10MPa pressure afterwards is finally dried in vacuo and electrode is made.
Graphene modified conductive polymer gel cladding novel nano electrode material of the present invention shows good electrochemistry
Behavior has three-dimensional network porous structure, at 25 ± 2 DEG C of room temperature, operating voltage 0.00-3V, current density 0.04mA/cm2It is permanent
Under the conditions of flowing charge and discharge, the novel nano electrode of graphene modified conductive polymer gel cladding shows good stable circulation
Property, capacity is still stable in about 500mAh/g after 400 circulations, which has faster charge-discharge performance, circulation one
The secondary time is about 1h, shows that the nanoparticle electrode that carrier is done using modified three-dimensional conductive macromolecule hydrogel network is possessed
Preferable electronic and ionic transmittability and stable structure；In addition, the electrode also has good repeatability and stability.Cause
This, graphene modified conductive polymer gel encapsulated nanoparticles electrode is expected to become a kind of novel li-ion electrode materials,
There are extensive Research Prospects in the fields such as high-energy density and slimline battery.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of the graphene modified conductive polymer gel of embodiment preparation.
Fig. 2 is the transmission electron microscope photo of the graphene modified conductive polymer gel of embodiment preparation.
Fig. 3 is the stereoscan photograph of the graphene modified conductive polymer gel encapsulated nanoparticles of embodiment preparation.
Fig. 4 is following for the electrode of the graphene modified conductive polymer gel covered stannum rice grain preparation of embodiment preparation
Ring performance map (1).
Fig. 5 is following for the electrode of the graphene modified conductive polymer gel covered stannum rice grain preparation of embodiment preparation
Ring performance map (2).
Fig. 6 is times of the electrode of the graphene modified conductive polymer gel covered stannum rice grain preparation of embodiment preparation
Rate performance test chart.
Fig. 7 is the resistance of the electrode of the graphene modified conductive polymer gel covered stannum rice grain preparation of embodiment preparation
Anti-performance test chart.
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.
10mg graphene oxide is added in 1-2mL distilled water, ultrasound dissolves it sufficiently, is then added 0.1mL's
The aniline solution of phytic acid and 50 μ L, is sufficiently stirred and makes it completely dissolved and be sufficiently mixed, and places it in 0-4 DEG C of ice-water baths；It will
The ammonium persulfate of 0.12g is added in 0.5-1mL distilled water, is then added into the solution of first step configuration, after ultrasonic 30s
Reaction 10min is stood, keeps aniline polymerization complete, is then washed with distilled water 2-3 times；Using sodium borohydride by graphene oxide also
Original, and 2-3 times wash with distilled water；It is freeze-dried the plural gel of above-mentioned preparation to obtain product.Graphene obtained is changed
Property conductive polymer gel do scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis, as illustrated in fig. 1 and 2,
It can be seen that gel is in three-dimensional network porous structure, aperture is 100 ± 10nm.
The nano-electrode particle of 70-80mg is added in 1-2mL graphene oxide water solution, ultrasound keeps its dispersion equal
It is even.Then, the phytic acid of 0.1mL and the aniline solution of 50 μ L is added, stirs and ultrasound makes it be uniformly dispersed.Finally, by 0.12g's
Ammonium persulfate is added in 0.5-1mL distilled water, is then added into the solution of previous step configuration, is stood after ultrasonic 30s anti-
10min is answered, keeps aniline polymerization complete, is then restored graphene oxide with sodium borohydride, then be washed with distilled water 2-3 times, shape
At the composite material of graphene modified conductive polymer gel covered stannum rice grain.Graphene denatured conductive obtained is polymerize
Object gel covered stannum rice grain does scanning electron microscope (SEM) analysis, as shown in Figure 2, it can be seen that material is in three-dimensional more
Pore structure, particle are uniformly distributed in graphene film and gel, and polyaniline gel is closely connect with graphene film.
Nano-electrode particle is grey Sn nano particle：Weigh 2.0g stannous sulfate (SnSO4) and 0.1g polyvinyl pyrrole
Alkanone (PVP) is dissolved in the dilution heat of sulfuric acid of 60mL 0.1mol/L, forms solution A after being completely dissolved.Weigh 1.28g hydroboration
Sodium (NaBH4) NaOH solution for forming solution B, and 1mol/L being added dropwise under agitation is dissolved in 160mL deionized water,
PH value is adjusted to 12-14.It will be dissolved with SnSO4Solution A be added drop-wise to dropwise dissolved with NaBH4Solution B in, held under normal temperature condition
It is continuous to be stirred to react 3h.To after reaction, be centrifugated under the revolving speed of 8000r/min using centrifuge, and respectively with distillation
Water and dehydrated alcohol respectively clean 3-5 times, and vacuum drying obtains for 24 hours.In the synthesis of Sn nano particle, PVP is in aqueous solution first
Middle formation spherical micelle, then its electronegative group is by Sn2+At Electrostatic Absorption to spherical micelle, finally by addition NaBH4
By Sn2+Ion reduction generates Sn nano particle, particle size range 20-50nm, and has preferable dispersibility.
Copper foil is polished with abrasive paper for metallograph, rinses, after ultrasound, is dried for standby through distilled water and ethyl alcohol.Preparation will be contained
The sticky pasty solutions of the composite material of graphene modified conductive polymer gel covered stannum rice grain are uniformly spun on processing
On copper foil afterwards, electrode is made in static pressure 30min, finally vacuum drying under 10MPa pressure after natural drying, i.e. graphene is modified
Application of the composite material of conductive polymer gel covered stannum rice grain as positive electrode.Active material electrode will be prepared
Piece is put into anode cover, and active material electrode slice is in anode cover center position as far as possible；Two drop electrolyte are added dropwise in active material
On electrode slice, electrolyte is allowed sufficiently to invade profit electrode slice, the group of electrolyte becomes the LiPF of 1mol/L6/ EC+DMC+EMC (volume ratio
1:1:1)；Diaphragm is placed on active material electrode slice, and electrolyte is made sufficiently to infiltrate diaphragm, diaphragm is that polypropylene microporous is compound
Film (Celgard 2400)；Lithium piece is placed on diaphragm, convex surface is downward；Gasket is placed on lithium piece, convex surface downward, lithium piece
For to electrode；Spring leaf is placed on gasket；Finally by cathode cap on anode cover, pressurization to get arrive knob
Detain half-cell.
Button half-cell obtained is subjected to charge-discharge performance test using LAND battery test system (CT2001A), is filled
Discharge test voltage range is 0.002-3V, current density 50-1000mAg-1.Assembled button half-cell is existed
Electrochemical impedance spectroscopy test is carried out on the comprehensive electrochemical test of PARSTAT 2263.It is just extremely worked electricity with button half-cell
Pole, lithium piece are to electrode and reference electrode, frequency range 105~10-2Hz.Battery is before testing with 100mAg-1Current density
It recycles and discharges into platform voltage 0.4V again after making within 5 weeks electrode activation, 5h is balanced under the current potential makes the Li in solid phase+Concentration reaches
Balance.
It is followed the result shows that the electrode of graphene modified conductive polymer gel covered stannum rice grain preparation is with higher
Ring stability, the long-life, 400 times circulation after capacity be still up to 500mAh/g, this shows that conductive polymer gel can significantly change
The problem of kind tin nanoparticles volume expansion causes capacity to decline, the addition of graphene improves the conduction of conductive polymer gel
Property, improve the multiplying power discharging property of tin nanoparticles.The result illustrates that graphene modified conductive polymer gel can be used for it
The novel nano electrode material that he causes capacity sharply to decline because of charge and discharge volume change.This is for novel high-capacity, Gao Wen
Qualitative and extended-life lithium ion battery electrode material research has important value and significance.
It is adjusted according to the parameter that the content of present invention is recorded, the preparation of material of the present invention can be achieved, and show base
This consistent electric property.Illustrative description is done to the present invention above, it should which explanation is not departing from core of the invention
In the case where the heart, it is any it is simple deformation, modification or other skilled in the art can not spend creative work etc.
Protection scope of the present invention is each fallen with replacement.
Claims (10)
1. graphene modified conductive polymer gel, which is characterized in that carry out as steps described below：
Step 1, graphene oxide is placed in distilled water, phytic acid and aniline and evenly dispersed, the first mixed solution of formation is added；
Ammonium persulfate is dispersed in distilled water, the second mixed solution is formed；
Step 2, the second mixed solution is added in the first mixed solution after ultrasonic disperse, reaction is stood in ice-water bath, so that
Aniline polymerization forms polyaniline completely, forms polyaniline-graphene oxide plural gel with graphene oxide；
Step 3, polyaniline-graphene oxide plural gel prepared by step 2 is restored using sodium borohydride, so that oxygen
Graphite alkene is reduced to graphene；
Step 4, the plural gel prepared by step 3 is freeze-dried.
2. graphene modified conductive polymer gel according to claim 1, which is characterized in that graphene oxide and aniline
Mass ratio be (1-8)：(5-10), preferably (3-6)：(8—10)；The volume ratio of phytic acid and aniline is (1-2)：1.
3. graphene modified conductive polymer gel according to claim 1, which is characterized in that in step 2, stand anti-
It is 10-30min between seasonable.
4. graphene modified conductive polymer gel described according to claim 1-one of 3, which is characterized in that in step 1
In, in the first mixed solution, addition Sn nano particle be used as nano-electrode particle, particle size range 20-50nm, and with compared with
Good dispersibility；The mass ratio of graphene oxide and aniline is (1-8)：(7-8), preferably (3-6)：(7—8)；It is received in addition
After rice electrode particle, nano-electrode particle-polyaniline-graphene plural gel is formed.
5. the preparation method of graphene modified conductive polymer gel, which is characterized in that carry out as steps described below：
Step 1, graphene oxide is placed in distilled water, phytic acid and aniline and evenly dispersed, the first mixed solution of formation is added；
Ammonium persulfate is dispersed in distilled water, the second mixed solution is formed；
Step 2, the second mixed solution is added in the first mixed solution after ultrasonic disperse, reaction is stood in ice-water bath, so that
Aniline polymerization forms polyaniline completely, forms polyaniline-graphene oxide plural gel with graphene oxide；
Step 3, polyaniline-graphene oxide plural gel prepared by step 2 is restored using sodium borohydride, so that oxygen
Graphite alkene is reduced to graphene；
Step 4, the plural gel prepared by step 3 is freeze-dried.
6. the preparation method of graphene modified conductive polymer gel according to claim 5, which is characterized in that oxidation stone
The mass ratio of black alkene and aniline is (1-8)：(5-10), preferably (3-6)：(8—10)；The volume ratio of phytic acid and aniline is
(1—2)：1.
7. the preparation method of graphene modified conductive polymer gel according to claim 5, which is characterized in that in step
In 2, the standing reaction time is 10-30min.
8. the preparation method of graphene modified conductive polymer gel, feature according to one of claim 5-7 exist
In in step 1, in the first mixed solution, addition Sn nano particle is as nano-electrode particle, particle size range 20-
50nm, and there is preferable dispersibility；The mass ratio of graphene oxide and aniline is (1-8)：(7-8), preferably (3-6)：
(7—8)；After adding nano-electrode particle, nano-electrode particle-polyaniline-graphene plural gel is formed.
9. application of the graphene modified conductive polymer gel as described in claim 1 as positive electrode.
10. application of the graphene modified conductive polymer gel as claimed in claim 4 as positive electrode.
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| CN115304323A (en) * | 2022-07-21 | 2022-11-08 | 中交四航工程研究院有限公司 | Conductive mortar and preparation method and application thereof |
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Application publication date: 20181123 |