CN109786725A - Independent self-supporting positive electrode and preparation method thereof and aluminium ion battery and preparation method thereof - Google Patents
Independent self-supporting positive electrode and preparation method thereof and aluminium ion battery and preparation method thereof Download PDFInfo
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- CN109786725A CN109786725A CN201910225179.3A CN201910225179A CN109786725A CN 109786725 A CN109786725 A CN 109786725A CN 201910225179 A CN201910225179 A CN 201910225179A CN 109786725 A CN109786725 A CN 109786725A
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- positive electrode
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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
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to aluminium ion field of batteries, a kind of independent self-supporting positive electrode and preparation method thereof and aluminium ion battery and preparation method thereof are disclosed, this aluminium ion battery includes anode, cathode, diaphragm and ionic liquid electrolyte；Wherein anode is that cobalt sulfide is grown in the adhesive-free material made in conductive carbon matrix.The battery is characterized in: anode is the compound of cobalt sulfide and conductive carbon matrix, is a kind of independent self-supporting formula material without bonding agent, internal resistance of cell problem caused by avoiding because of bonding agent.This aluminium ion battery has that price is low, stable circulation, voltage window mouth width, clean and environmental protection, it is highly-safe many advantages, such as, electronics industry, communication industry, the various fields such as energy reserves can be used in.
Description
Technical field
The present invention relates to energy-storage battery technical field, in particular to a kind of aluminium ion battery independent self-supporting positive electrode
And preparation method thereof and using the positive electrode aluminium ion battery and preparation method thereof.
Background technique
In recent years, as petering out for traditional energy is increasingly serious with environmental problem, New Energy Industry increasingly by
To attention.Wherein quickly, but its safety issue and higher cost limit its development to lithium ion battery development speed.Aluminium
Ion battery is expected to make up this disadvantage, is just attract the sight of people.
Rechargeable aluminium ion battery (AIB) is due to silicon source abundant, the attraction of height ratio capacity and high-energy density
Characteristic, it is considered to be a new generation's large size energy storage device.However, AIB lack have required capacity and long-time stability it is suitable just
Pole material, this severely limits the practical applications of AIB.Relative to the aluminium ion cell positive material having been reported that, including graphite
Class (natural graphite, artificial graphite, graphene, graphene oxide etc.), polymerization species (polyaniline, polythiophene, polypyrrole etc.), gold
Belong to oxide-based (VO2, V2O5, TiO2Deng) etc., transient metal sulfide shows outstanding chemical property.Such as
The Mo of Cheverel phase structure6S8Positive active material can be good at reversible embedding dealuminzation, and first circle specific discharge capacity reaches
148mAh·g-1.It is for another example a kind of disclosed in Chinese invention patent (CN104393290) to use MoS2For the aluminium ion of positive electrode
Battery and preparation method thereof, battery first circle discharge capacity is up to 220mAhg-1.However, due to lacking reasonable electrode knot
Structure, battery show poor cycle performance.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the present invention provides a kind of positive electrode and preparation method thereof
And aluminium ion battery and preparation method thereof, realize the high capacity charge and discharge of rechargeable aluminium ion battery, and good cycle,
It is highly-safe.
Technical solution: the present invention provides a kind of independent self-supporting positive electrode, the positive electrode be by cobalt sulfide and
Adhesive-free material made of conductive carbon matrix composite, the cobalt sulfide be evenly distributed in the conductive carbon matrix gap or
Surface.
Preferably, the cobalt sulfide be it is following any one or combinations thereof: CoS2、CoS、Co3S4、Co9S8。
Preferably, mass percent of the cobalt sulfide in the positive electrode is 20%-45%.
Preferably, the conductive carbon matrix be have from group, the carbon nanotube of intertexture or lamination ability, carbon nano-fiber,
Conductive aeroge, graphite-like or graphite alkenes carbon material.
The present invention also provides a kind of preparation methods of aluminium ion battery independent self-supporting positive electrode, by cobalt sulfide
It grows into conductive carbon matrix and obtains compound, then disperse compound in water or ethanol solution again, taken out by vacuum
Filter forms a film and obtains the positive electrode.
Preferably, the synthetic method of the cobalt sulfide is hydro-thermal method, solvent-thermal method, high temperature vulcanized method, microwave assisting method
Or spray pyrolysis.
The present invention also provides a kind of aluminium ion battery, positive electrode is aluminium ion battery independent self-supporting anode material
Material.
The present invention also provides a kind of preparation method of aluminium ion battery, using containing the AlCl that can move freely4 -Or
Al2Cl7 -The independent self-supporting positive electrode is uniformly fixed on by the imidazole ion liquid of ion as il electrolyte
As anode on the collector of inert metal paillon, the aluminium flake cleaning by purity greater than 97%, which is cut, is used as cathode, between positive and negative anodes
It is separated using diaphragm, the aluminium ion battery is assembled into glove box.It is specifically implemented according to the following steps:
Step 1, it cuts high-purity aluminium flake or aluminum alloy sheet is that suitable dimension obtains cathode after washes of absolute alcohol；Step 2, lead to
It crosses hydro-thermal method and cobalt sulfide is grown in formation independent self-supporting positive electrode on conductive carbon matrix material, it then will be independent from branch
Support positive electrode forms film as anode on inert metal paillon collector；Step 3, by anhydrous aluminum chloride and 1- ethyl-
3- methylimidazolium chloride is mixed to get electrolyte in applying argon gas glove box；Step 4, by step 1, component obtained in 2,3
It is equipped with diaphragm to be encapsulated in glove box with aluminum plastic film, becomes battery；Step 5,4-6 hours after battery assembly, charge and discharge electrical measurement is carried out
Examination.Above-mentioned diaphragm preferably uses fibreglass diaphragm, and above-mentioned aluminium alloy is metallic aluminium and the conjunction in copper, silver, nickel, lead, tin, bismuth, iron
Gold.
The method specific implementation step of cathode is handled in above-mentioned steps 1: step 1.1, aluminium flake or aluminum alloy sheet are in cutting
After need to polish using sand paper；Step 1.2, the aluminium flake dehydrated alcohol or acetone soak and ultrasonic vibration polished, then exist
It is dried in 60-80 DEG C of baking oven；The hydro-thermal reaction specific implementation step being previously mentioned in above-mentioned steps 2: it step 2.1, will first lead
Electrical carbon matrix (by taking carbon nanotube as an example) acidification, is put into the mixing of the 80ml concentrated sulfuric acid/concentrated nitric acid (v/v:3/1) for 1g carbon nanotube
80 DEG C of 1 hours of reflux in liquid.Step 2.2,1g urea is weighed, 3g cobalt chloride is added in 160ml water, stirs 1 hour, is put into
In hydrothermal reaction kettle, 120 degree of hydro-thermal reactions obtain 60 DEG C drying 12 hours after product.Step 2.3, product in step 2.2 is weighed
0.2 gram, then the vulcanized sodium of the carbon nanotube and 0.8g that have been acidified in 0.3g step 2.1 is weighed, it is added in 60ml water, stirring
It 30 minutes, is put into hydrothermal reaction kettle and reacts 24 hours for 160 DEG C.Obtain 80 DEG C drying 12 hours after product.Step 2.3, claim
The product in 0.06g step 2.2 is measured, is added in 50ml water, ultrasonic disperse 15 minutes.Then dispersion liquid is filtered by polypropylene
Film filters film forming, takes material from filter membrane off after dry, and positive electrode is obtained after cutting, and subsequent 80 DEG C of vacuum drying 12 are small
When.
Preferably, the inert metal paillon is molybdenum sheet, titanium sheet, tantalum piece, gold or platinum group metal.
Preferably, the il electrolyte is anhydrous aluminum chloride (AlCl3) and 1- ethyl-3-methylimidazole salt
(MEICl), 1- methyl -3- ethyl imidazol(e) salt (MEICl), 1,2- dimethyl -3- propyl imidazole salt (DMPrICl) or 1- butyl -
The mixture of 3- methylimidazole salt (BMICl).Anhydrous aluminum chloride (AlCl3) and 1- ethyl-3-methylimidazole salt (MEICl), 1-
Methyl -3- ethyl imidazol(e) salt (MEICl), 1,2- dimethyl -3- propyl imidazole salt (DMPrICl) or 1- butyl -3- methylimidazole
The molar ratio of salt (BMICl) is 1.1-1.6:1；It is preferably in a proportion of 1.3:1.
The utility model has the advantages that the positive electrode in the present invention is the cobalt sulfide and conductive carbon matrix material of a kind of self-support type
Compound is used as the novel cathode material of AIB, and cobalt sulfide is positive active material, and conductive carbon matrix material is handed over from made of group
Mutual network provides ion abundant and electron transfer channel, and adhesive-free electrode avoids bonding agent bring internal resistance of cell shadow
It rings, eliminates influence of the bonding agent to battery itself, while also saving the processes such as coating, roll-in, keep fabrication more simple；
The suction filtration technique used, the thickness and unit area active matter quality of the accurate coordination electrode of energy, improves efficiency；Matrix is loose more
Hole, carbon nanotubes are interweaved, and provide channel abundant for the migration of ion and electronics.Aluminium ion electricity provided by the present invention
Pond, anode be cobalt sulfide be attached to carbon matrix material interleaving network adhesive-free and independent self-supporting material, production
Simplicity, it is cheap, it is suitable for industrialized production, can be widely applied to technical field of energy storage.It is had not been reported so far about cobalt
Sulfide and conductive carbon matrix composite make the patent of aluminium ion anode.
Detailed description of the invention
Fig. 1 is the SEM picture of positive electrode prepared by embodiment 1；
Fig. 2 is aluminium ion battery first circle charge-discharge performance test curve prepared by embodiment 1；
Fig. 3 is aluminium ion cycle performance of battery figure prepared by embodiment 1.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
Embodiment 1:
Present embodiments provide for a kind of aluminium ion battery independent self-supporting positive electrodes, which is by Co3S4With
The adhesive-free material that carbon nanotube is combined, Co3S4It is evenly distributed in carbon nanotube gap or surface, Co3S4This just
Mass percent in the material of pole is 30%.
Above-mentioned independent self-supporting positive electrode the preparation method is as follows:
The acidification of carbon nanotube: 1g carbon nanotube is weighed, takes 60ml sulfuric acid and 20ml nitric acid to be put into beaker and mix with graduated cylinder, so
Carbon nanotube and mixed acid are poured into afterwards and carry out reflow treatment in three-necked flask, when reflux is put into magnetic rotor stirring, reflux temperature
80 DEG C, return time 1 hour of degree.It is taken out after the completion of reflux, filters and clean after distilled water dilution is added, be put into baking oven later
70 DEG C are dried overnight, and obtain the carbon nanotube being acidified.
Cobalt sulfide is compound with acidification carbon nanotube: 1g urea is weighed, 3g cobalt chloride hexahydrate is added in 160ml water,
Stirring 1 hour, be put into hydrothermal reaction kettle, 120 DEG C hydro-thermal reaction 12 hours, obtain pink product, wash with distilled water after
60 DEG C drying 12 hours.It weighs the above-mentioned pink material of 0.2g, 0.8g vulcanized sodium and 0.3g and is acidified carbon nanotube, be successively put into
It is stirred 30 minutes in 60ml water, then ultrasound 15 minutes, is put into hydrothermal reaction kettle and reacts 24 hours for 160 DEG C, obtain black product
Later, it is respectively washed 3 times with distilled water and ethyl alcohol, 80 DEG C drying 12 hours after filtering, obtains cobalt sulfide and acidification carbon nanometer
The composite material of pipe, the composite material are independent self-supporting positive electrode.
Use above-mentioned independent self-supporting positive electrode as the preparation of the aluminium ion battery of positive electrode:
The preparation of anode: the above-mentioned positive electrode of 0.06g is weighed, is put into 50ml water, ultrasonic disperse 15 minutes.Then by dispersion liquid
It is slowly added in funnel using glass bar, is filtered and formed a film by polypropylene filter, material is taken off from filter membrane after dry, is obtained
Film after 60 μm obtains positive electrode after cutting, subsequent 80 DEG C are dried in vacuo 12 hours.Dried anode is attached to
1.5cm × 5cm size, 100 μ m-thicks molybdenum sheet collector on, obtain anode.
High-purity aluminium flake of 100 μ m-thicks: being cut into 1.5cm × 5cm size by the preparation of cathode, needed after cutting using
Sand paper polishing, then is cleaned, wherein the method cleaned is, with dehydrated alcohol or acetone soak and ultrasonic vibration, then
It is dried in 60-80 DEG C of baking oven, is used as cathode.
The preparation of il electrolyte: under anhydrous and oxygen-free environment, by anhydrous aluminum chloride and -3 methyl-imidazoles of 1- ethyl
Chlorate obtains il electrolyte with molar ratio 1.3:1 mixing.
Assembling: anode, fibreglass diaphragm, cathode and il electrolyte with aluminum plastic film in glove box, utilize
Edge banding machine encapsulating, is finally fabricated to Soft Roll aluminium ion battery.
Charge-discharge test: after aluminium ion battery standing 4 hours, between 0.1 ~ 1.8V voltage, with the current density of 100mA/g
Lower carry out charge-discharge test.If Fig. 2 is aluminium ion battery first circle charge-discharge performance test curve, it is seen then that use Co3S4It is received with carbon
Mitron composite material is that the aluminium ion battery first circle specific discharge capacity of anode is about 100mAhg-1, which puts with about 0.8V
Piezoelectric voltage.If Fig. 3 is aluminium ion cycle performance of battery figure, it is seen that the aluminium ion battery can continuous charge and discharge up to more than 200 circulations,
Circulating still there is 70mAhg at 200 times-1Capacity keep.
Embodiment 2:
Present embodiments provide for a kind of aluminium ion battery independent self-supporting positive electrodes, which is by CoS2And carbon
The adhesive-free material that nanotube is combined, CoS2It is evenly distributed in carbon nanotube gap or surface, CoS2In the anode material
Mass percent in material is 35%.
Above-mentioned independent self-supporting positive electrode the preparation method is as follows:
The acidification of carbon nanotube: identical with embodiment 1.
Cobalt sulfide is compound with acidification carbon nanotube: weighing 0.4g cobalt chloride hexahydrate, 0.6g cysteine and 0.3g
It is acidified carbon nanotube, is successively put into 60ml distilled water in water and stirs 30 minutes, then ultrasound 15 minutes, is put into hydrothermal reaction kettle
160 DEG C are reacted 20 hours, after obtaining black product, are respectively washed 3 times with distilled water and ethyl alcohol, 80 DEG C of dryings 12 after filtering
Hour, it obtains cobalt sulfide and is acidified the composite material of carbon nanotube, which is independent self-supporting positive electrode.
Use above-mentioned independent self-supporting positive electrode as the preparation of the aluminium ion battery of positive electrode: with embodiment 1
Roughly the same, difference, which is only that after aluminium ion battery standing 5 hours, carries out charge-discharge test.
Embodiment 3:
Present embodiments provide for a kind of aluminium ion battery independent self-supporting positive electrodes, which is by CoS and carbon
The adhesive-free material that nanotube is combined, CoS is evenly distributed in carbon nanotube gap or surface, and CoS is in the anode material
Mass percent in material is 27%.
Above-mentioned independent self-supporting positive electrode the preparation method is as follows:
The acidification of carbon nanotube: identical with embodiment 1.
Cobalt sulfide with acidification carbon nanotube it is compound: weigh 0.4g cobalt chloride hexahydrate, 0.35g sodium thiosulfate and
0.3g acidification carbon nanotube, which is successively put into 60ml distilled water in water, to be stirred 30 minutes, then ultrasound 15 minutes, is put into hydro-thermal reaction
It reacts 20 hours for 160 DEG C in kettle, after obtaining black product, is respectively washed 3 times with distilled water and ethyl alcohol, done for 80 DEG C after filtering
It dry 12 hours, obtains cobalt sulfide and is acidified the composite material of carbon nanotube, which is independent self-supporting positive electrode.
Use above-mentioned independent self-supporting positive electrode as the preparation of the aluminium ion battery of positive electrode: with embodiment 1
Roughly the same, difference, which is only that after aluminium ion battery standing 6 hours, carries out charge-discharge test.
The technical concepts and features of above embodiment only to illustrate the invention, its object is to allow be familiar with technique
People cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of independent self-supporting positive electrode, which is characterized in that the positive electrode is answered by cobalt sulfide and conductive carbon matrix
Adhesive-free material made of conjunction, the cobalt sulfide is evenly distributed in the conductive carbon matrix gap or surface.
2. independent self-supporting positive electrode according to claim 1, which is characterized in that the cobalt sulfide is following any
One kind or combinations thereof: CoS2、CoS、Co3S4、Co9S8。
3. independent self-supporting positive electrode according to claim 1, which is characterized in that the cobalt sulfide is in the anode
Mass percent in material is 20%-45%.
4. independent self-supporting positive electrode according to any one of claim 1 to 3, which is characterized in that the conductive carbon
Matrix is to have from group, the carbon nanotube of intertexture or lamination ability, carbon nano-fiber, conductive aeroge, graphite-like or graphene
Class carbon material.
5. a kind of preparation method of independent self-supporting positive electrode according to any one of claims 1 to 4, feature exist
In cobalt sulfide is grown into conductive carbon matrix and obtains compound, then disperses compound in again water or ethanol solution
In, it forms a film by vacuum filtration and obtains the positive electrode.
6. independent self-supporting positive electrode according to claim 5, which is characterized in that the synthetic method of the cobalt sulfide
It is hydro-thermal method, solvent-thermal method, high temperature vulcanized method, microwave assisting method or spray pyrolysis.
7. a kind of aluminium ion battery, which is characterized in that its positive electrode is aluminium ion described in any one of Claims 1-4
Battery independent self-supporting positive electrode.
8. a kind of preparation method of aluminium ion battery as claimed in claim 7, which is characterized in that can move freely using containing
AlCl4 -Or Al2Cl7 -The imidazole ion liquid of ion is as il electrolyte, by the independent self-supporting positive electrode
The metal aluminum or aluminum alloy cleaning as anode, with purity greater than 97% is uniformly fixed on inert metal paillon collector to cut
It as cathode, is separated between positive and negative anodes using diaphragm, is assembled into the aluminium ion battery using aluminum plastic film encapsulating in glove box.
9. the preparation method of aluminium ion battery according to claim 8, which is characterized in that the inert metal paillon is molybdenum
Piece, titanium sheet, tantalum piece, gold or platinum group metal.
10. the preparation method of aluminium ion battery according to claim 8, which is characterized in that the imidazole ion liquid is
Anhydrous aluminum chloride and 1- ethyl-3-methylimidazole salt, 1- methyl -3- ethyl imidazol(e) salt, 1,2- dimethyl -3- propyl imidazole salt or
The mixture of 1- butyl -3- methylimidazole salt.
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| CN110723757A (en) * | 2019-07-31 | 2020-01-24 | 青岛大学 | Nine-cobalt octasulfide porous nanosheet, positive electrode material, battery and preparation method |
| CN112599769A (en) * | 2020-12-28 | 2021-04-02 | 江苏大学 | Aluminum ion battery and positive electrode material Co thereofxSy@MXene |
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