CN106784835A - A kind of preparation method of carbon negative electrode material of lithium ion cell - Google Patents
A kind of preparation method of carbon negative electrode material of lithium ion cell Download PDFInfo
- Publication number
- CN106784835A CN106784835A CN201710099746.6A CN201710099746A CN106784835A CN 106784835 A CN106784835 A CN 106784835A CN 201710099746 A CN201710099746 A CN 201710099746A CN 106784835 A CN106784835 A CN 106784835A
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- Prior art keywords
- lithium ion
- negative electrode
- electrode material
- carbon negative
- preparation
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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 a kind of preparation method of carbon negative electrode material of lithium ion cell of technical field of lithium ion, and the preparation method of the carbon negative electrode material of lithium ion cell specifically includes following steps：S1：Raw material is added；S2：Carry out ice-water bath；S3：Form solids；S4：Solids is pyrolyzed；S5：It is cooled to room temperature；S6：Add deionized water；S7：Add hydrogen peroxide；S8：To suspension centrifugal treating；S9：Washed using cleaning solution；S10：Vacuum drying obtains carbon negative pole material, the present invention uses Graphene as the negative material of lithium ion battery, good ion and electronic conduction ability is presented using the self structure characteristic of Graphene, with lithium storage content high and the characteristics of high charge-discharge speed, be conducive to the insertion and deintercalation of lithium ion battery, its cyclical stability is high.
Description
Technical field
The present invention relates to technical field of lithium ion, specially a kind of preparation side of carbon negative electrode material of lithium ion cell
Method.
Background technology
Lithium ion battery, also known as " rocking chair batteries ", referring to being capable of reversible insertion and the change of deintercalate lithium ions with both positive and negative polarity use
Compound constitutes secondary cell.Present commercialized lithium ion battery makees positive pole with graphite as negative pole with the compound containing lithium, is filling
In discharge process, there is no the presence of lithium metal, only lithium ion comes and goes intercalation/deintercalation between both positive and negative polarity.Battery charge when,
Lithium ion is deviate from from positive pole, by electrolyte and barrier film, is embedded into negative pole, conversely, battery is in electric discharge, lithium ion is by bearing
Extremely middle deintercalation, by electrolyte and barrier film, is embedded into positive pole again, and interior circuit does not have electron shuttle, with the electric charge such as lithium ion
The electronics of equivalent is transmitted in external circuit.
The negative pole majority of traditional lithium ion battery uses lithium metal, and branch is easily produced in the charge and discharge process of battery
The crystallization of shape, when crystalline solid develops to a certain extent, on the one hand can fracture and cause the loss of lithium, on the other hand even more serious
It is that crystalline solid can puncture barrier film, and positive pole is coupled together with negative pole, produces short circuit, very big potential safety hazard is brought to battery, is
This, comes into operation, we have proposed a kind of preparation method of carbon negative electrode material of lithium ion cell to solve the above problems.
The content of the invention
It is an object of the invention to provide a kind of preparation method of carbon negative electrode material of lithium ion cell, to solve above-mentioned background
What is proposed in technology easily produces dendritic crystallization in the charge and discharge process of battery, when crystalline solid develops to a certain extent
When, on the one hand can fracture and cause the loss of lithium, on the other hand more seriously, crystalline solid can puncture barrier film, positive pole with bear
Pole is coupled together, and produces short circuit, and the problem of very big potential safety hazard is brought to battery.
To achieve the above object, the present invention provides following technical scheme：A kind of preparation of carbon negative electrode material of lithium ion cell
Method, the preparation method of the carbon negative electrode material of lithium ion cell specifically includes following steps：
S1：The graphite powder and 5~7g sodium nitrate for weighing 3~7g are put into flask, and add 75~90ml's in flask
Concentrated sulfuric acid solution is reacted；
S2：Flask is placed in ice-water bath, under agitation being slowly added in batches by the potassium permanganate of 9~12g
To in flask；
S3：Flask in ice-water bath in moving to tepidarium after magnetic agitation 15min, and argon gas protection under continue to stir
9~12h of reaction is mixed, solid is formed；
S4：Material after solidification is put into porcelain boat and is moved into quartz ampoule, it is pyrolyzed using tube furnace, 900
DEG C constant temperature 3h；
S5：After pyrolytic reaction terminates, room temperature is naturally cooled under argon gas protection, during material moved into beaker；
S6：It is in batches slow in beaker to add the deionized water of 300ml, and general after heating stirring 15min is carried out again
Mixture is cooled to room temperature；
S7：The hydrogen peroxide of 10~13ml 30% is added in beaker, 20~23min is stirred, and stand 2h；
S8：By suspension in step S7 by centrifugal treating, and supernatant is abandoned, sediment is scattered in dispersion soln,
And centrifugation 10min is carried out again, abandon supernatant；
S9：The sediment obtained in step S8 is dispersed in the hydrochloric acid solution of 200ml0.5N, is centrifuged under 9500rpm
10min, abandons supernatant, the product for obtaining cleaning solution repeated washing 3~5 times；
S10：The product obtained in step S9 is vacuum dried 3h under conditions of 75~85 DEG C, the product mortar for obtaining
Grinding, crosses 320 mesh standard sieves, obtains carbon negative electrode material of lithium ion cell.
Preferably, in the step S2, the raw material in flask is stirred using magnetic agitation, the addition of potassium permanganate
Added in 6min in batches and finished.
Preferably, in the step S4, before pyrolysis, after being first passed through argon gas protection 10min, the air in quartz ampoule is complete
Discharge and full of argon gas, start to warm up.
Preferably, in the step S8, the rotating speed 9500rpm of centrifugal treating, dispersion soln for 3wt% sulfuric acid and
The mixed liquor of the hydrogen peroxide of 0.5wt%.
Preferably, in the step S9, cleaning solution is the mixed liquor of the ether of the ethanol and 200ml of 200ml.
Preferably, in the step S10, vacuum drying reaction is carried out in vacuum drying chamber.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is using Graphene as the negative of lithium ion battery
Pole material, presents good ion and electronic conduction ability, with lithium storage content high using the self structure characteristic of Graphene
The characteristics of with high charge-discharge speed, be conducive to the insertion and deintercalation of lithium ion battery, its cyclical stability is high.
Brief description of the drawings
Fig. 1 is workflow diagram of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Fig. 1 is referred to, the present invention provides a kind of technical scheme：A kind of preparation method of carbon negative electrode material of lithium ion cell,
The preparation method of the carbon negative electrode material of lithium ion cell specifically includes following steps：
S1：The graphite powder and 5~7g sodium nitrate for weighing 3~7g are put into flask, and add 75~90ml's in flask
Concentrated sulfuric acid solution is reacted；
S2：Flask is placed in ice-water bath, under agitation being slowly added in batches by the potassium permanganate of 9~12g
To in flask, the raw material in flask is stirred using magnetic agitation, the addition of potassium permanganate is added in 6min in batches
Finish；
S3：Flask in ice-water bath in moving to tepidarium after magnetic agitation 15min, and argon gas protection under continue to stir
9~12h of reaction is mixed, solid is formed；
S4：Material after solidification is put into porcelain boat and is moved into quartz ampoule, it is pyrolyzed using tube furnace, 900
DEG C constant temperature 3h, before pyrolysis, after being first passed through argon gas protection 10min, the air in quartz ampoule is completely exhausted out and full of argon gas, starts
Heat up；
S5：After pyrolytic reaction terminates, room temperature is naturally cooled under argon gas protection, during material moved into beaker；
S6：It is in batches slow in beaker to add the deionized water of 300ml, and general after heating stirring 15min is carried out again
Mixture is cooled to room temperature；
S7：The hydrogen peroxide of 10~13ml 30% is added in beaker, 20~23min is stirred, and stand 2h；
S8：By suspension in step S7 by centrifugal treating, and supernatant is abandoned, sediment is scattered in dispersion soln,
And carry out centrifugation 10min again, abandon supernatant, the rotating speed 9500rpm of centrifugal treating, dispersion soln for 3wt% sulfuric acid and
The mixed liquor of the hydrogen peroxide of 0.5wt%；
S9：The sediment obtained in step S8 is dispersed in the hydrochloric acid solution of 200ml0.5N, is centrifuged under 9500rpm
10min, abandons supernatant, the product for obtaining cleaning solution repeated washing 3~5 times, and cleaning solution is the ethanol and 200ml of 200ml
The mixed liquor of ether；
S10：The product obtained in step S9 is vacuum dried 3h under conditions of 75~85 DEG C, the product mortar for obtaining
Grinding, crosses 320 mesh standard sieves, obtains carbon negative electrode material of lithium ion cell, and vacuum drying reaction is carried out in vacuum drying chamber.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (6)
1. a kind of preparation method of carbon negative electrode material of lithium ion cell, it is characterised in that：The carbon negative electrode material of lithium ion cell
Preparation method specifically includes following steps：
S1：The graphite powder and 5~7g sodium nitrate for weighing 3~7g are put into flask, and the dense sulphur of 75~90ml is added in flask
Acid solution is reacted；
S2：Flask is placed in ice-water bath, under agitation by the potassium permanganate of 9~12g in batches be slowly added into burning
In bottle；
S3：Flask in moving to tepidarium after magnetic agitation 15min, and continues to stir anti-in ice-water bath under argon gas protection
9~12h is answered, solid is formed；
S4：Material after solidification is put into porcelain boat and is moved into quartz ampoule, it is pyrolyzed using tube furnace, in 900 DEG C of perseverances
Warm 3h；
S5：After pyrolytic reaction terminates, room temperature is naturally cooled under argon gas protection, during material moved into beaker；
S6：It is in batches slow in beaker to add the deionized water of 300ml, and carry out again will mixing after heating stirring 15min
Thing is cooled to room temperature；
S7：The hydrogen peroxide of 10~13ml 30% is added in beaker, 20~23min is stirred, and stand 2h；
S8：By suspension in step S7 by centrifugal treating, and supernatant is abandoned, sediment is scattered in dispersion soln, and again
It is secondary to carry out centrifugation 10min, abandon supernatant；
S9：The sediment obtained in step S8 is dispersed in the hydrochloric acid solution of 200ml0.5N, is centrifuged under 9500rpm
10min, abandons supernatant, the product for obtaining cleaning solution repeated washing 3~5 times；
S10：The product obtained in step S9 is vacuum dried 3h under conditions of 75~85 DEG C, the product for obtaining is ground with mortar
Mill, crosses 320 mesh standard sieves, obtains carbon negative electrode material of lithium ion cell.
2. the preparation method of a kind of carbon negative electrode material of lithium ion cell according to claim 1, it is characterised in that：The step
In rapid S2, the raw material in flask is stirred using magnetic agitation, the addition of potassium permanganate has been added in 6min in batches
Finish.
3. the preparation method of a kind of carbon negative electrode material of lithium ion cell according to claim 1, it is characterised in that：The step
In rapid S4, before pyrolysis, after being first passed through argon gas protection 10min, the air in quartz ampoule is completely exhausted out and full of argon gas, starts to rise
Temperature.
4. the preparation method of a kind of carbon negative electrode material of lithium ion cell according to claim 1, it is characterised in that：The step
In rapid S8, the rotating speed 9500rpm of centrifugal treating, dispersion soln is the mixed liquor of the hydrogen peroxide of the sulfuric acid and 0.5wt% of 3wt%.
5. the preparation method of a kind of carbon negative electrode material of lithium ion cell according to claim 1, it is characterised in that：The step
In rapid S9, cleaning solution is the mixed liquor of the ether of the ethanol and 200ml of 200ml.
6. the preparation method of a kind of carbon negative electrode material of lithium ion cell according to claim 1, it is characterised in that：The step
In rapid S10, vacuum drying reaction is carried out in vacuum drying chamber.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604750A (en) * | 2009-07-09 | 2009-12-16 | 上海交通大学 | A kind of preparation method of lithium ion battery negative material |
| CN102275908A (en) * | 2011-07-07 | 2011-12-14 | 中南大学 | Preparation method of graphene material |
| CN103663432A (en) * | 2012-09-26 | 2014-03-26 | 海洋王照明科技股份有限公司 | Graphene and preparation method thereof and lithium ion battery |
| CN104671232A (en) * | 2013-11-29 | 2015-06-03 | 上海悦达墨特瑞新材料科技有限公司 | Preparation method of graphene and application of prepared graphene |
| CN105439128A (en) * | 2015-11-09 | 2016-03-30 | 国网智能电网研究院 | Preparation method for porous graphene lithium ion battery positive electrode material |
-
2017
- 2017-02-23 CN CN201710099746.6A patent/CN106784835A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101604750A (en) * | 2009-07-09 | 2009-12-16 | 上海交通大学 | A kind of preparation method of lithium ion battery negative material |
| CN102275908A (en) * | 2011-07-07 | 2011-12-14 | 中南大学 | Preparation method of graphene material |
| CN103663432A (en) * | 2012-09-26 | 2014-03-26 | 海洋王照明科技股份有限公司 | Graphene and preparation method thereof and lithium ion battery |
| CN104671232A (en) * | 2013-11-29 | 2015-06-03 | 上海悦达墨特瑞新材料科技有限公司 | Preparation method of graphene and application of prepared graphene |
| CN105439128A (en) * | 2015-11-09 | 2016-03-30 | 国网智能电网研究院 | Preparation method for porous graphene lithium ion battery positive electrode material |
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