CN108550903A - A kind of aluminium ion battery - Google Patents
A kind of aluminium ion battery Download PDFInfo
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- CN108550903A CN108550903A CN201810426203.5A CN201810426203A CN108550903A CN 108550903 A CN108550903 A CN 108550903A CN 201810426203 A CN201810426203 A CN 201810426203A CN 108550903 A CN108550903 A CN 108550903A
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- film
- graphene
- salt
- graphene oxide
- ion battery
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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 invention discloses a kind of aluminium ion batteries, using porous graphene film as positive electrode, have uniform bubble structure inside the porous graphene film;It is 100~150nm that walls, which have uniform venthole, aperture, and porosity is more than 5%.Graphene film is by 3000 degree of processing, and without defect, interlayer AB perfect structures stack, thus have fabulous electric conductivity (0.8 1.2MS/m);Porous structure on interlayer air hole structure and gas wall so that electrolysis mass transter is rapid, thus assembled battery has higher battery capacity and coulombic efficiency.
Description
Technical field
The present invention relates to a kind of aluminium ion batteries.
Background technology
Aluminium ion battery becomes because its aluminum metal cathode has the advantages that the specific capacity, low cost and safety of superelevation
Very promising next-generation energy storage mode.However it finds a kind of forthright with higher capacity, high discharge platform and high power
The positive electrode of energy is always the Main way of aluminium ion battery research.
Graphene is the ultra-thin two-dimension nano material that a kind of thickness only has 0.34nm, electric conductivity and current-carrying with superelevation
Transport factor has great application value in various battery material fields.Graphene by self assembly can get it is continuous and from
The graphene macroform material of support, to can get chemical property more better than graphite material.Such as application publication number is
The Chinese invention patent (application publication number on December 24th, 2014) of CN104241596A discloses a kind of positive electrode and uses stone
The rechargeable aluminium ion battery and preparation method thereof of ink, due to the height of this rechargeable aluminium ion battery of the high stacked structure of graphite
High rate performance is just restricted.
Graphene oxide is a kind of important source material of grapheme material, and yield height is at low cost, has extraordinary industrialization
Foreground, however the method for preparing graphene oxide on a large scale at present can carry out the structure of graphene mainly by oxidizing process
It destroys and then reduces its conductivity and chemical property, the highly conductive graphene without defect is mainly obtained with vapour deposition process
, it can not mass produce.
It is generally acknowledged that the mentality of designing of carbon material is all based on the defect for improving carbon material to improve electricity in lithium ion battery
The migration velocity of pole material intermediate ion, and increase the load capacity of active material.Therefore, the defect density of carbon material is improved to improve
The performance of battery is the focus on research direction of those skilled in the art.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to overcome the technology prejudice of this field, provide a kind of aluminium from
Sub- battery.
The purpose of the present invention is what is be achieved through the following technical solutions:A kind of aluminium ion battery is with porous graphene film
Positive electrode, the porous graphene film inside have uniform bubble structure;Walls have uniform venthole, and aperture is
100~150nm, porosity are more than 5%.
Further, the graphene number of plies of the graphene film thickness direction is not more than 20000 layers.
Further, it is prepared by the following method to obtain:
(1) graphene oxide being configured to a concentration of 5-10mg/mL graphene oxide water solutions, scraper coating forms a film, from
It so dries, the thickness of film is not more than 20 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1-2 centigrade per minutes, temperature
Degree is 1300-1800 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10-20 centigrade per minutes;2000 degrees Celsius with
On, 2-5 centigrade per minutes.
Further, the graphene number of plies 2 × 10 of the graphene film thickness direction4~10 × 104Between.
Further, the graphene film is prepared by the following method to obtain:
(1) graphene oxide is configured to a concentration of 5-10mg/mL graphene oxide water solutions, water soluble salt is added, obtains
To film forming precursor solution, the wherein content of salt is the 1~5% of graphene oxide quality;Or use Nitric acid etching graphite oxide
Then alkene is configured to the film forming precursor solution of 5-10mg/mL;Film forming precursor solution scraper coating is formed a film, naturally dry,
The thickness of film is 20-100 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1-2 centigrade per minutes, temperature
Degree is 1300-1800 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10-20 centigrade per minutes;2000 degrees Celsius with
On, 2-5 centigrade per minutes.
Further, the salt is selected from:Magnesium salts, calcium salt, titanium salt, silicon salt, boron salt, molysite, aluminium salt, zinc salt, mantoquita, nickel salt
Etc..
Further, the battery cathode is aluminum metal or aluminium alloy;Diaphragm is selected from glass fibre, polypropylene diaphragm, gathers
Tetrafluoroethene diaphragm or polyethylene diagrams.
The beneficial effects of the present invention are:The present invention is extended by high temperature defect, is prepared for the unique multidimensional gas of graphene
Pore structure:Graphene film is by 3000 degree of processing, and without defect, interlayer AB perfect structures stack, height-oriented continuous in film
In the case of, there is fabulous electric conductivity (0.8-1.2MS/m), efficiency for charge-discharge is high, and discharge voltage is high;Interlayer air hole structure with
And porous structure on gas wall, channel is more, and ion transmission is fast so that electrolysis mass transter is rapid, thus assembled battery is with higher
Coulombic efficiency performance;It is too many that nano level duct will not cause density to reduce again, and load capacity is big, and battery capacity is high.
Description of the drawings
Fig. 1 is the electron microscope of porous graphene film prepared by embodiment 1, and b figures are the partial enlargement of a figures;
Fig. 2 is the electron microscope of porous graphene film prepared by embodiment 2, and b figures are the partial enlargement of a figures;
Fig. 3 is the electron microscope of porous graphene thick film prepared by embodiment 4, and b figures are the partial enlargement of a figures;
Figure 4 and 5 are the aluminium ion batteries that prepare of embodiment 1 in cycle performance curve under the conditions of 50C constant current charge-discharges,
Wherein Fig. 4 is capacity retention curve, and Fig. 5 is coulombic efficiency curve.
Specific implementation mode
Embodiment 1
(1) graphene oxide is configured to a concentration of 10mg/mL graphene oxide water solutions, scraper coating film forming is natural
It dries, the thickness of film is 20 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 2 centigrade per minutes, temperature
It is 1800 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film, as shown in Figure 1.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 20 centigrade per minutes;2000
Degree Celsius or more, 5 centigrade per minutes.It will be seen from figure 1 that having uniform bubble structure, walls inside graphene film
With uniform venthole, aperture is 100~150nm, and porosity is more than 5%.After being compacted into, through micrometer caliper thickness measuring
Degree, between the graphene number of plies for calculating the graphene film thickness direction is 19100~19600 layers.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;Fig. 4 is the aluminium ion battery in cyclicity under the conditions of 50C constant current charge-discharges
It can curve.It can be seen from the figure that the stabilization specific capacity that the battery can be kept at the current density 100mAh/g of superelevation continues
25000 circles, coulombic efficiency are maintained at 95 or more.
Embodiment 2
(1) graphene oxide is configured to a concentration of 5mg/mL graphene oxide water solutions, scraper coating film forming is dried in the air naturally
Dry, the thickness of film is 5 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1 centigrade per minute, temperature
It is 1300 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film, as shown in Figure 2.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10 centigrade per minutes;2000
Degree Celsius or more, 2 centigrade per minutes.Figure it is seen that having uniform bubble structure, walls inside graphene film
With uniform venthole, aperture is 100~150nm, and porosity is more than 5%.After being compacted into, through micrometer caliper thickness measuring
Degree, between the graphene number of plies for calculating the graphene film thickness direction is 4700~5000 layers.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;The stabilization specific volume that the battery can be kept at the current density 100mAh/g of superelevation
Amount continues 25000 circles, and coulombic efficiency is maintained at 95 or more.
Embodiment 3
(1) graphene oxide is configured to a concentration of 8mg/mL graphene oxide water solutions, scraper coating film forming is dried in the air naturally
Dry, the thickness of film is 1 micron.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1 centigrade per minute, temperature
It is 1500 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10 centigrade per minutes;2000 degrees Celsius or more,
5 centigrade per minutes.There is uniform bubble structure, walls to have uniform ventilation inside the graphene film being prepared
Hole, aperture are 100~150nm, and porosity is more than 5%.After being compacted into, through micrometer caliper Thickness Measurement by Microwave, the graphite is calculated
The graphene number of plies of alkene film thickness direction is 1000 layers or so.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;The stabilization specific volume that the battery can be kept at the current density 100mAh/g of superelevation
Amount continues 25000 circles, and coulombic efficiency is maintained at 95 or more.
Embodiment 4
(1) graphene oxide is configured to a concentration of 10mg/mL graphene oxide water solutions, zinc sulfate, zinc sulfate is added
Content be the 5% of graphene oxide quality, scraper coating film forming, naturally dry, the thickness of film is 100 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 2 centigrade per minutes, temperature
It is 1800 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film, as shown in Figure 3.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 20 centigrade per minutes;2000
Degree Celsius or more, 5 centigrade per minutes.From figure 3, it can be seen that having uniform bubble structure, walls inside graphene film
With uniform venthole, aperture is 100~150nm, and porosity is more than 5%.After being compacted into, through micrometer caliper thickness measuring
Degree, the graphene number of plies for calculating the graphene film thickness direction are 100000 layers or so.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;The stabilization specific volume that the battery can be kept at the current density 100mAh/g of superelevation
Amount continues 25000 circles, and coulombic efficiency is maintained at 95 or more.
Embodiment 5
(1) graphene oxide is configured to a concentration of 5mg/mL graphene oxide water solutions, magnesium chloride is added, magnesium chloride
Content is the 1% of graphene oxide quality, and the thickness of scraper coating film forming, naturally dry, film is 20 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1 centigrade per minute, temperature
It is 1300 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10 centigrade per minutes;2000 degrees Celsius or more,
2 centigrade per minutes.There is uniform bubble structure, walls to have uniform ventilation inside the graphene film being prepared
Hole, aperture are 100~150nm, and porosity is more than 5%.After being compacted into, through micrometer caliper Thickness Measurement by Microwave, the graphite is calculated
The graphene number of plies of alkene film thickness direction is 20000 layers or so.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;The stabilization specific volume that the battery can be kept at the current density 100mAh/g of superelevation
Amount continues 25000 circles, and coulombic efficiency is maintained at 95 or more.
Embodiment 6
(1) graphene oxide is configured to a concentration of 8mg/mL graphene oxide water solutions, nickel chloride is added, nickel chloride
Content is the 2% of graphene oxide quality, and the thickness of scraper coating film forming, naturally dry, film is 80 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 2 centigrade per minutes, temperature
It is 1600 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 20 centigrade per minutes;2000 degrees Celsius or more,
5 centigrade per minutes.There is uniform bubble structure, walls to have uniform ventilation inside the graphene film being prepared
Hole, aperture are 100~150nm, and porosity is more than 5%.After being compacted into, through micrometer caliper Thickness Measurement by Microwave, the graphite is calculated
The graphene number of plies of alkene film thickness direction is 80000 layers or so.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;The stabilization specific volume that the battery can be kept at the current density 100mAh/g of superelevation
Amount continues 25000 circles, and coulombic efficiency is maintained at 95 or more.
Embodiment 7
(1) Nitric acid etching graphene oxide is used, the film forming precursor solution of 7mg/mL is then configured to;It will be at membrane precursor
The thickness of liquid solution scraper coating film forming, naturally dry, film is 40 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 2 centigrade per minutes, temperature
It is 1300 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtained with secondary gas-pore structure
Graphene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10 centigrade per minutes;2000 degrees Celsius or more,
5 centigrade per minutes.
(4) graphene film that step 3 is prepared is as anode, and aluminium foil is cathode, and ionic liquid is electrolyte, glass
Fiber is diaphragm, is assembled into aluminium ion battery;The stabilization specific volume that the battery can be kept at the current density 100mAh/g of superelevation
Amount continues 20000 circles, and coulombic efficiency is maintained at 95 or more.
Claims (7)
1. a kind of aluminium ion battery, which is characterized in that using porous graphene film as positive electrode, inside the porous graphene film
With uniform bubble structure;It is 100~150nm that walls, which have uniform venthole, aperture, and porosity is more than 5%.
2. aluminium ion battery according to claim 1, which is characterized in that the graphite of the porous graphene film thickness direction
The alkene number of plies is not more than 20000 layers.
3. aluminium ion battery according to claim 2, which is characterized in that porous graphene film is prepared by the following method
It arrives:
(1) graphene oxide is configured to a concentration of 5-10mg/mL graphene oxide water solutions, scraper coating film forming is dried in the air naturally
Dry, the thickness of film is not more than 20 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1-2 centigrade per minutes, and temperature is
1300-1800 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtains the stone with secondary gas-pore structure
Black alkene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10-20 centigrade per minutes;2000 degrees Celsius or more,
2-5 centigrade per minutes.
4. aluminium ion battery according to claim 1, which is characterized in that the graphite of the porous graphene film thickness direction
The alkene number of plies 2 × 104~10 × 104Between.
5. aluminium ion battery according to claim 4, which is characterized in that the porous graphene film is made by the following method
It is standby to obtain:
(1) graphene oxide is configured to a concentration of 5-10mg/mL graphene oxide water solutions, water soluble salt is added, obtains into
Film precursor solution, the wherein content of salt are the 1~5% of graphene oxide quality;Or Nitric acid etching graphene oxide is used, so
It is configured to the film forming precursor solution of 5-10mg/mL afterwards;Film forming precursor solution scraper coating is formed a film, naturally dry, film
Thickness is 20-100 microns.
(2) graphene oxide membrane is placed in moderate oven slowly heating sintering, and heating rate is 1-2 centigrade per minutes, and temperature is
1300-1800 degrees Celsius.
(3) graphene film that intermediate sintering temperature is crossed is placed in 3000 degree of annealing in high temperature furnace, obtains the stone with secondary gas-pore structure
Black alkene film.The heating rate of high temperature furnace is as follows:2000 degrees Celsius hereinafter, 10-20 centigrade per minutes;2000 degrees Celsius or more,
2-5 centigrade per minutes.
6. aluminium ion battery according to claim 5, which is characterized in that the salt is selected from:Magnesium salts, calcium salt, titanium salt, silicon
Salt, boron salt, molysite, aluminium salt, zinc salt, mantoquita, nickel salt etc..
7. aluminium ion battery according to claim 1, which is characterized in that the battery cathode is aluminum metal or aluminium alloy;
Diaphragm is selected from glass fibre, polypropylene diaphragm, Teflon septum or polyethylene diagrams.
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CN103387229A (en) * | 2013-07-23 | 2013-11-13 | 哈尔滨工业大学 | A preparation method for porous graphene and a preparation method for a graphene-based aluminium-air cell |
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