CN105810947B - A kind of aluminium ion cell positive material, electrode and aluminium ion battery - Google Patents
A kind of aluminium ion cell positive material, electrode and aluminium ion battery Download PDFInfo
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- CN105810947B CN105810947B CN201610281036.0A CN201610281036A CN105810947B CN 105810947 B CN105810947 B CN 105810947B CN 201610281036 A CN201610281036 A CN 201610281036A CN 105810947 B CN105810947 B CN 105810947B
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- aluminium ion
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
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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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 relates to a kind of aluminium ion cell positive material, electrode and aluminium ion batteries, belong to aluminium ion battery technology field.Aluminium ion cell positive material of the invention uses the method included the following steps to prepare: be that the organic carbon source of 1:3-20 and graphite material are added in solvent and carry out solvent thermal reaction by mass ratio, it is dry, be carbonized at 300-2000 DEG C to get；The temperature of the solvent thermal reaction is 120-300 DEG C；The pressure of the solvent thermal reaction is 0.3-3MPa；The organic carbon source is one of phenolic resin, phenolic resin prepolymer, furfural resin, seaweed glue, polyvinyl alcohol, polyacrylic acid, starch, cellulose, cyclodextrin.Aluminium ion cell positive material of the invention has good stability in aluminium ion charge and discharge process, be not in positive electrode structure collapses or deformation and cause the charge-discharge performance of battery to decline.
Description
Technical field
The present invention relates to a kind of aluminium ion cell positive material, electrode and aluminium ion batteries, belong to aluminium ion battery technology
Field.
Background technique
Aluminium ion battery is a kind of novel secondary cell product, is anode with materials such as graphite using aluminium as cathode.Product
In do not include lithium ion and other hold incendive metal.It has a safety feature, and can be fully charged in a short time, recycles
It is almost undamped after 7500 times, it is a kind of new secondary battery of function admirable.
Due to utilizing aluminium ion to carry charge in aluminium ion battery, and much bigger than lithium ion of aluminium ion, thus aluminium from
Sub- battery is higher to the structural requirement of its negative electrode material, using graphite in the prior art as negative electrode material, is difficult completely full
The demand of sufficient aluminium ion battery.Such as application publication number is the Chinese invention patent (application publication number 2014 of CN104241596A
On December 24) a kind of rechargeable aluminium ion battery and preparation method thereof is disclosed, positive electrode uses graphite, carbon paper, carbon
Fibrous paper, expanded graphite and carbon black etc., the electric conductivity and specific surface area of this aluminium ion cell positive material are lower, lead to aluminium
The quick charge of ion battery and cycle performance are restricted.
It is a kind of mode for optimizing graphite material structure that multiple material, which mixes or be made composite material, and application publication number is
The Chinese invention patent (data of publication of application be 2012 on August 29) of CN102651468A discloses a kind of silicon/carbon/graphite in lithium ion batteries
Negative electrode material, after mixing using corresponding method by 100 parts of aggregates and 4-20 parts of additives, by mixture in 2500-
3000 DEG C of progress graphitization processings 1-10 hours or first under protective atmosphere 700-1500 DEG C after roasting 1-10 hours again in 2500-
3000 DEG C graphitization processing 1-10 hours, be made after cooling；Its additive is pitch, phenolic resin, furfural resin, epoxy resin
It is purifying natural graphite Deng, aggregate or is made of purifying natural graphite with clout.Graphite material made from this method and natural stone
Ink is compared, and has good interstitial structure.But the structural stability that composite material is made in this method is poor, if be used as
Aluminium ion cell positive material, then in charge and discharge process, structure is easily deformed, and reduces the efficiency for charge-discharge of battery, therefore not
It is suitable as aluminium ion cell positive material.
Summary of the invention
The purpose of the present invention is to provide a kind of good aluminium ion cell positive materials of stable charge/discharge.Of the invention
Purpose, which also resides in, provides a kind of electrode prepared using above-mentioned aluminium ion cell positive material and the aluminium ion using the electrode
Battery.
In order to achieve the goal above, the technical solution of aluminium ion cell positive material of the invention is as follows:
A kind of aluminium ion cell positive material is prepared using the method included the following steps:
Organic carbon source and graphite material that mass ratio is 1:9 are added in solvent and carry out solvent thermal reaction, it is dry, in 300-
2000 DEG C carbonization to get；
The temperature of the solvent thermal reaction is 120-300 DEG C；The pressure of the solvent thermal reaction is 0.3-3MPa；
The organic carbon source is phenolic resin, phenolic resin prepolymer, furfural resin, seaweed glue, polyvinyl alcohol, polypropylene
One of acid, starch, cellulose, cyclodextrin.
Aluminium ion cell positive material of the invention carries out after carrying out solvent thermal reaction using organic carbon source and graphite material
Carbonization, has been made the carbon skeleton of the three-dimensional crosslinking structure filled with graphite material, and the structure is steady in aluminium ion charge and discharge process
It is qualitative very good, be not in positive electrode structure collapses or deformation and cause the charge-discharge performance of battery to decline.
The time of solvent thermal reaction is arranged according to the raw material used, in general, the time of the solvent thermal reaction is 8-
20h.Further preferably 8-12h.
The graphite material is one of natural flake graphite, pyrolytic graphite, hard carbon, expanded graphite, form the few-layer graphene.
The solvent is water or organic solvent, and the organic solvent is one of acetone, methanol, propyl alcohol.
The mass ratio of the organic carbon source and solvent is 1-80:100.
The temperature of solvent thermal reaction can be more preferably 180-220 DEG C according to the type of the raw material and solvent that use.
To avoid high temperature from impacting the structure of solvent thermal reaction product, the drying is vacuum freeze drying.When molten
When agent is water, vacuum freeze drying is directly carried out；When solvent is organic solvent, washing is carried out to organic solvent using water and is set
It changes, carries out vacuum freeze drying again later；Washing displacement method particularly includes: impregnate material in water, when certain
Between (< 1 hour) change a water, allow organic solvent to be diffused into water, 3 times or more repeatedly, remove material in organic solvent simultaneously
Make to be full of water between the gap of material.
It is helium or nitrogen that the carbonization carries out inert atmosphere under vacuum perhaps inert atmosphere.
The technical solution of electrode of the invention is as follows:
A kind of electrode, including above-mentioned aluminium ion cell positive material.
The electrode includes the mixed uniformly binder and the aluminium ion battery of collector and coating on a current collector
Positive electrode.
The amount of binder should not be excessive, and to avoid the conductivity for reducing positive electrode, the amount of binder is also unsuitable very few, with
It avoids positive electrode bonding loosely, is easy to fall off, in general, the mass ratio of the aluminium ion positive electrode and binder is 90-
95:5-10。
In order to further increase the electric conductivity of positive electrode, above-mentioned electrode further includes conductive agent.
The binder is binder commonly used in the art, such as PTFE.
The conductive agent is the common conductive agent of ability, such as carbon black.
The electrode can also be cut and formed to obtain by above-mentioned aluminium ion cell positive material.The aluminium ion battery of cutting
Positive electrode can be the thin slice being pressed into using aluminium ion cell positive material powder, can also be directly blocky aluminium ion electricity
Pond positive electrode.
This electrode suppresses flakiness by aluminium ion cell positive material, is then cut into type, utilizes positive electrode itself
As collector, the energy density of positive plate is improved.
The cutting is cut or is cut by laser using cutter.
The technical solution of aluminium ion battery of the invention is as follows:
A kind of aluminium ion battery, uses above-mentioned electrode.
Aluminium ion battery of the invention uses the complex carbon material with three-dimensional cross-linked carbon backbone structure as anode, improves
The efficiency that aluminium ion is embedded in and is deviate from anode, and then the efficiency for charge-discharge of aluminium ion battery is improved, it is also beneficial to aluminium
Ion battery high rate charge-discharge improves the cycle performance of aluminium ion battery.
Detailed description of the invention
Fig. 1 is the SEM image of the aluminium ion cell positive material of the embodiment of the present invention 1；
Fig. 2 is the SEM image of the aluminium ion cell positive material of the embodiment of the present invention 2；
Fig. 3 is the SEM image of the aluminium ion cell positive material of the embodiment of the present invention 3；
Fig. 4 is the SEM image of the aluminium ion cell positive material of the embodiment of the present invention 4；
Fig. 5 is the charge-discharge test curve of the aluminium ion battery of the embodiment of the present invention 5；
Fig. 6 is the charge-discharge test curve of the aluminium ion battery of the embodiment of the present invention 6；
Fig. 7 is the charge-discharge test curve of the aluminium ion battery of the embodiment of the present invention 7.
Specific embodiment
Technical solution of the present invention is further detailed below by specific embodiment.
Embodiment 1
The aluminium ion cell positive material of the present embodiment is made with the following method: the phenolic aldehyde tree for being 40% by mass fraction
Rouge aqueous solution is uniformly mixed with natural flake graphite, and wherein the mass ratio of phenolic resin and natural flake graphite is 1:9, will be mixed
Mixed liquor afterwards is added in high-pressure reactor, under the pressure of 2MPa, 8h is reacted at a temperature of 180 DEG C, by the mixture after reaction
Taken out from high-pressure reactor, freeze-drying removes water therein, in vacuum atmosphere, at 1000 DEG C carbonization treatment to get.
Embodiment 2
The aluminium ion cell positive material of the present embodiment is made with the following method: the phenolic aldehyde tree for being 80% by mass fraction
Rouge aqueous solution is uniformly mixed with expanded graphite, and wherein the mass ratio of phenolic resin and expanded graphite is 1:11, will be mixed mixed
It closes liquid to be added in high-pressure reactor, under the pressure of 2MPa, reacts 15h at a temperature of 180 DEG C, by the mixture after reaction from high pressure
Taken out in reactor, freeze-drying removes water therein, in helium atmosphere, at 1800 DEG C carbonization treatment to get.
Embodiment 3
The aluminium ion cell positive material of the present embodiment is made with the following method: the phenolic aldehyde tree for being 10% by mass fraction
The methanol solution of rouge is uniformly mixed with expanded graphite, and wherein the mass ratio of phenolic resin and expanded graphite is 1:13, after mixing
Mixed liquor be added high-pressure reactor in, under the pressure of 0.3MPa, 20h is reacted at a temperature of 220 DEG C, by the mixture after reaction
It is taken out from high-pressure reactor, washing displacement is to remove wherein remaining organic solvent, then is freeze-dried and removes water therein,
In vacuum atmosphere, at 2000 DEG C carbonization treatment to get.
Embodiment 4
The aluminium ion cell positive material of the present embodiment is made with the following method: the phenolic aldehyde tree for being 10% by mass fraction
The acetone soln of rouge is uniformly mixed with pyrolytic graphite, and wherein the mass ratio of phenolic resin and pyrolytic graphite is 1:15, after mixing
Mixed liquor be added high-pressure reactor in, under the pressure of 3MPa, react 12h at a temperature of 120 DEG C, by the mixture after reaction from
It is taken out in high-pressure reactor, washing displacement is to remove wherein remaining solvent, and freeze-drying removes water therein, in vacuum atmosphere
In, at 800 DEG C carbonization treatment to get.
Embodiment 5
By aluminium ion cell positive material obtained in embodiment 1 and polytetrafluoroethylene (PTFE) (PTFE) according to mass ratio 90:10
Mixed grinding is uniform, is pressed into the uniform sheet with a thickness of 60 μm, cuts into the square pole piece that side length is 20mm with cutter, will
After square pole piece vacuum drying, electrode is formed together with plus plate current-collecting body hot pressing and as aluminium ion anode；With existing
There are the aluminium in technology or the compound containing aluminium to prepare aluminium ion using ionic liquid as electrolyte as aluminium ion battery cathode
Battery.
Embodiment 6
By aluminium ion cell positive material, conductive black obtained in embodiment 2, polytetrafluoroethylene (PTFE) (PTFE) according to quality
It is more uniform than 85:5:10 mixed grinding, be pressed into the uniform sheet with a thickness of 100 μm, with cutter cut into side length be 20mm just
Rectangular pole piece forms electrode and as aluminium ion electricity after the vacuum drying of square pole piece together with plus plate current-collecting body hot pressing
Pond anode；Using aluminium in the prior art or the compound containing aluminium is as aluminium ion battery cathode, using ionic liquid as electrolyte,
Prepare aluminium ion battery.
Embodiment 7
Aluminium ion cell positive material obtained in embodiment 3 and polytetrafluoroethylene (PTFE) (PTFE) is mixed according to mass ratio 95:5
It closes grinding uniformly, is pressed into the uniform sheet with a thickness of 150 μm, the round pole piece that diameter is 18mm is cut into, by round pole piece
After vacuum drying, it is bonded together to form electrode and as aluminium ion anode by conducting resinl and plus plate current-collecting body；With existing
There are the aluminium in technology or the compound containing aluminium to prepare aluminium ion using ionic liquid as electrolyte as aluminium ion battery cathode
Battery.
Embodiment 8
Aluminium ion cell positive material block obtained in embodiment 3 is cut directly into the round pole that diameter is 18mm
Piece is bonded together to form electrode and as aluminium ion after the vacuum drying of round pole piece by conducting resinl and plus plate current-collecting body
Anode；Using aluminium in the prior art or the compound containing aluminium is as aluminium ion battery cathode, is electrolysis with ionic liquid
Liquid prepares aluminium ion battery.
Embodiment 9
Aluminium ion cell positive material obtained in embodiment 4 is pressed into the uniform sheet with a thickness of 120 μm, uses cutter
It is cut into the round pole piece that diameter is 18mm, after the vacuum drying of round pole piece, forms electricity together with plus plate current-collecting body hot pressing
Pole and as aluminium ion anode；Using aluminium in the prior art or the compound containing aluminium is as aluminium ion battery cathode, with
Ionic liquid is electrolyte, prepares aluminium ion battery.
Experimental example
1) physical and chemical performance is tested.
Aluminium ion cell positive material obtained in embodiment 1-4 is utilized respectively SEM and tests its SEM photograph, respectively such as
Shown in Fig. 1-4.
2) electrochemical property test.
Aluminium ion battery obtained in embodiment 5 is subjected to charge-discharge test under the multiplying power of 2C, 5C, 10C respectively, is tested
As a result as shown in Figure 5 respectively；
Aluminium ion battery obtained in embodiment 6 is subjected to charge-discharge test, test result such as Fig. 6 under the multiplying power of 100C
It is shown；
Aluminium ion battery obtained in embodiment 7 is subjected to charge-discharge test, test result such as Fig. 7 under the multiplying power of 50C
It is shown.
Aluminium ion cell positive material of the invention has uniform appearance structure, graphite material it can be seen from Fig. 1-4
It is evenly distributed in three-dimensional cross-linked carbon skeleton.It can be seen from Fig. 5-7 using aluminium made from the aluminium ion cell positive material from
Sub- battery multiplying power discharging property is excellent.
Claims (7)
1. a kind of aluminium ion cell positive material, which is characterized in that using the method preparation included the following steps:
Organic carbon source and graphite material that mass ratio is 1:3-15 are added in solvent and carry out solvent thermal reaction, vacuum refrigeration is dry
It is dry, 800-2000 DEG C carbonization to get；The mass ratio of the organic carbon source and solvent is 1-80:100；
The temperature of the solvent thermal reaction is 120-300 DEG C；The pressure of the solvent thermal reaction is 0.3-3MPa；The solvent heat
The time of reaction is 8-20h；
The organic carbon source is one of phenolic resin, phenolic resin prepolymer, furfural resin；The solvent be water, acetone,
One of methanol, propyl alcohol.
2. aluminium ion cell positive material as described in claim 1, which is characterized in that the graphite material is natural scale stone
One of ink, pyrolytic graphite, expanded graphite, form the few-layer graphene.
3. a kind of electrode, which is characterized in that including aluminium ion cell positive material as described in claim 1.
4. electrode as claimed in claim 3, which is characterized in that including collector and coating on a current collector mixed uniformly
Binder and the aluminium ion cell positive material.
5. electrode as claimed in claim 4, which is characterized in that the mass ratio of the aluminium ion positive electrode and binder is
90-95:5-10。
6. electrode as claimed in claim 3, which is characterized in that be cut and formed to obtain by the aluminium ion cell positive material.
7. a kind of aluminium ion battery, which is characterized in that use electrode as claimed in claim 3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107342434B (en) * | 2017-07-17 | 2019-07-05 | 济南大学 | Rechargeable aluminium battery using ordered mesopore carbon as positive electrode and preparation method thereof |
| WO2019029192A1 (en) * | 2017-08-11 | 2019-02-14 | 杭州高烯科技有限公司 | Aluminum battery |
| CN107482219A (en) * | 2017-08-11 | 2017-12-15 | 杭州高烯科技有限公司 | A kind of high-performance aluminum ion battery |
| CN107546390A (en) * | 2017-08-11 | 2018-01-05 | 杭州高烯科技有限公司 | A kind of aluminium ion battery of high graphitization degree positive pole |
| CN110391419B (en) * | 2019-07-26 | 2022-07-05 | 广东工业大学 | Porous carbon and application thereof in lithium-sulfur battery anode |
| CN113036122B (en) * | 2021-03-09 | 2022-05-24 | 中南大学 | Expanded graphite cathode material, preparation method thereof, electrode and aluminum ion battery |
| CN114335484A (en) * | 2022-01-05 | 2022-04-12 | 徐州博磊达新能源科技有限公司 | Negative electrode composite material for alkali metal ion battery, preparation method of negative electrode composite material and alkali metal ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102050437A (en) * | 2009-10-29 | 2011-05-11 | 上海比亚迪有限公司 | Carbon composite material, and preparation method and application thereof |
| CN104241596A (en) * | 2014-08-22 | 2014-12-24 | 北京科技大学 | Rechargeable aluminum ion cell and preparation method thereof |
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| JP6332031B2 (en) * | 2012-10-30 | 2018-05-30 | 株式会社村田製作所 | Aluminum secondary battery and electronic device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102050437A (en) * | 2009-10-29 | 2011-05-11 | 上海比亚迪有限公司 | Carbon composite material, and preparation method and application thereof |
| CN104241596A (en) * | 2014-08-22 | 2014-12-24 | 北京科技大学 | Rechargeable aluminum ion cell and preparation method thereof |
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