CN103618088B - A kind of preparation method of graphite material of lithium ion battery - Google Patents
A kind of preparation method of graphite material of lithium ion battery Download PDFInfo
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- CN103618088B CN103618088B CN201310589619.6A CN201310589619A CN103618088B CN 103618088 B CN103618088 B CN 103618088B CN 201310589619 A CN201310589619 A CN 201310589619A CN 103618088 B CN103618088 B CN 103618088B
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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
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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 invention belongs to technical field of lithium ion, particularly relate to a kind of preparation method of graphite material of lithium ion battery, comprise the following steps: under atmosphere of inert gases, active carbon is added in high temperature carbonization furnace, be heated to 900 ~ 1100 DEG C and make active carbon carbonization, vacuumize simultaneously, after cooling, obtain the active carbon after carbonization; Under atmosphere of inert gases, the active carbon after carbonization step one obtained adds in graphitizing furnace, then injects pitch, fully stirs, and vacuumizes, and then at 2500 ~ 2700 DEG C, carries out graphitization, obtains graphite after cooling.Relative to prior art, the present invention is first by active carbon carbonization in high temperature and high pressure kettle, and then inject pitch, liquid pitch can fill the hole on the active carbon after carbonization, again after the graphitization processing of subsequent high temperature high pressure, just can obtain the higher graphite of real density, thus improve the discharging efficiency first of the gram volume using this graphite and the lithium ion battery using this graphite.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of preparation method of graphite material of lithium ion battery.
Background technology
In graphite crystal, the carbon atom with layer forms covalent bond with sp2 hydridization, and each carbon atom is connected with other three atoms with three covalent bonds.Six carbon atom defines hexagonal ring in same plane, is extended into laminated structure, and the spacing distance between layers of graphite is comparatively large, is generally 340pm, and between carbon atom on same layer, adhesion is very strong, extremely difficultly destroys.Due to the above design feature of graphite, it has heat-resisting quantity, electrical and thermal conductivity, lubrification and chemical stability etc., is therefore widely used as refractory material (as graphite crucible), electric conducting material (as carbon-point, graphite gasket etc.), wear-resisting lubriation material (as lubricant) and lithium ion battery negative material etc.It is wherein an extremely important application of graphite as lithium ion battery negative material.
In recent years, lithium ion battery, owing to having the advantage of high voltage, high-energy-density and long circulation life, has become one of the widest secondary cell of range of application.But, along with the day by day miniaturized, microminiaturized of electronic product (as mobile phone, notebook computer and panel computer) etc. and long standbyization, the requirement of people to the lithium ion battery of the energy source as these electronic products is more and more higher, wish its reduced volume when ensureing energy supply, so, the volume energy density improving battery is just needed.
Volume energy density=energy/volume=(voltage × electric current × time)/volume, when voltage, electric current and time are certain, in order to improve the volume energy density of battery, just needs the volume reducing lithium ion battery.The electrolyte etc. that lithium ion battery generally comprises positive plate, negative plate, barrier film, packaging film and is filled in packaging film, the thickness of positive plate wherein, negative plate, barrier film and packaging film all can have influence on the volume of battery.If their thickness can be reduced, contribute to the volume energy density improving battery undoubtedly.Wherein, in order to reduce the thickness of negative plate, can be realized by the amount reducing active material, bonding agent etc., being realized by the compacted density improving negative pole; But the former, while minimizing thickness, also can cause the reduction of energy, therefore, there is no benifit to the raising of the volume energy density of battery; And the raising of the latter to the volume energy density of battery is limited, because graphite cathode exists the problem of bounce-back, compacted density is larger, and the bounce-back of battery in cyclic process is larger, thus greatly reduces the security performance of battery.
But, if the real density (but not compacted density) of graphite can be improved, then effectively can improve the volume energy density of battery undoubtedly.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, and provide a kind of preparation method of graphite material of lithium ion battery, the graphite adopting the method to prepare has higher real density, and low raw-material cost, simple and easy to get, easily realizes.
To achieve these goals, the present invention adopt following technical scheme: a kind of preparation method of graphite material of lithium ion battery, comprises the following steps:
Step one, under atmosphere of inert gases, adds active carbon in high temperature carbonization furnace, is heated to 900 ~ 1100 DEG C and makes active carbon carbonization, vacuumize simultaneously, after cooling, obtains the active carbon after carbonization.
Wherein, active carbon, also known as activated carbon black, is black powder or granular amorphous carbon.Active carbon principal component goes back the element such as aerobic, hydrogen in addition to carbon.Active carbon is structurally irregular alignment due to microcrystalline carbon, and between interconnection, have pore, be a kind of porous carbon, bulk density is low, and specific area is large.
Carbonization also claims pyrolysis, is to heat raw material under the condition of isolated air.Active carbon raw material, after carbonization, can go out the gases such as aqueous vapor, carbon monoxide, carbon dioxide and hydrogen by decomposing; Feed material degradation fragmentates, and recombines into stable structure.These fragments may be made up of some microcrystals.Microcrystal by more than two panels, the laminated structure that has carbon atom to arrange with hexagonal lattice piles up and forms, but pile up without fixing crystal formation, the size of microcrystal is relevant with structure with raw-material composition, and is subject to the impact of carburizing temperature, and the rising roughly with carburizing temperature increases.Therefore, the present invention adopts 900 ~ 1100 DEG C to carry out carbonization to active carbon, can obtain larger microcrystal.But the bulk density of the active carbon after carbonization is still not high, structure is still comparatively loose, there is more hole.
The effect vacuumized in step one is the gases such as aqueous vapor, carbon monoxide, carbon dioxide and the hydrogen produced in removing carbonisation.
Step 2, under atmosphere of inert gases, the active carbon after carbonization step one obtained adds in graphitizing furnace, then injects pitch, fully stirs, and vacuumizes simultaneously, then at 2500 ~ 2700 DEG C, carries out graphitization, obtains graphite after cooling.
Wherein, the pitchy complex mixture that pitch is made up of hydrocarbon and the nonmetal derivative thereof of different molecular weight, being in a liquid state, when being injected in the active carbon after carbonization, can being full of the hole of the active carbon after carbonization.
Graphitization utilizes thermal activation by the charcoal atoms at suitable temperatures of thermodynamic instability by the transform in order of Turbostratic to crystal structure of graphite, therefore, in graphitizing process, high-temperature heat treatment is used to provide energy to atomic rearrangement and Structure Transformation, the invention provides the graphitization that 2500 ~ 2700 DEG C realize pitch and active carbon, carry out graphitization at such a temperature and can greatly reduce the impurity existed in product.
The serviceability temperature of graphitizing furnace is up to 2800 DEG C, and production efficiency is high, energy saving, and with temperature measurement on-line and temperature-controlling system, can monitor the temperature in stove in real time, and regulate automatically.And furnace sealing is good, protective gas loss is little, and the heating-up time is short, can reach 200 DEG C/time.
The effect vacuumized in step 2 is the gases such as aqueous vapor, carbon monoxide, carbon dioxide and the hydrogen produced in removing graphitizing process, to prevent the quality of these gases to the graphite generated in follow-up graphitizing process from having an impact, graphite is made to produce unnecessary fault of construction (as formed bubble eye).
Cooling in step one and step 2 is nature cooling.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and the dynamic viscosity of pitch described in step 2 60 DEG C time is 60 ~ 120Pas, and the viscosity of pitch is too large, then its poor fluidity, be unfavorable for that it is filled in the hole of active carbon, viscosity is too little, and carbon source can be made inadequate.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and active carbon described in step one is coconut husk charcoal, fruit shell carbon, carbo lignius or ature of coal charcoal, and these active carbons are cheap and easy to get, greatly can reduce production cost.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and pitch described in step 2 is coal tar pitch, petroleum asphalt or bitumen, and these pitches are cheap and easy to get, greatly can reduce production cost.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, the mass ratio of described active carbon and described pitch is (5 ~ 10): 1, pitch is mainly used for the hole on the active carbon after filling carbonization, therefore, its ratio is unsuitable too high, but the ratio of pitch can not be too low, otherwise do not have the effect of the real density improving graphite.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and the pressure vacuumizing front high temperature carbonization furnace in step one is 0.1 ~ 1MPa, and the pressure within the scope of this can impel the graphite-structure of formation compacter, has higher real density.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and the vacuum degree vacuumized in step one in rear carbide furnace is-99KPa ~-1KPa; The vacuum degree vacuumized in step 2 in rear graphitizing furnace is-99KPa ~-1KPa.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and the duration of carbonization described in step one is 30min ~ 24h.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and the graphited duration described in step 2 is 30min ~ 24h.
One as the preparation method of graphite material of lithium ion battery of the present invention is improved, and described in step one and step 2, atmosphere of inert gases is argon atmosphere or nitrogen atmosphere.
Relative to prior art, the present invention is first by active carbon carbonization in high temperature and high pressure kettle, formed by more than two panels, the microcrystal of the laminated structure accumulation that has carbon atom arrange with hexagonal lattice, and remain containing the open structure compared with porous, and then injecting pitch, liquid pitch can fill the hole on the active carbon after carbonization, then after the graphitization processing of subsequent high temperature high pressure, just can obtain the higher graphite of real density, thus improve the gram volume using this graphite; And due to the real density of graphite higher, its specific area is little, active large, therefore can improve the discharging efficiency first of the lithium ion battery using this graphite.In addition, whole technological process is simple, and raw material is cheap and easy to get, thus greatly reduces production cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation method of a kind of graphite material of lithium ion battery that the present embodiment provides, comprises the following steps:
Step one, under argon gas atmosphere, coconut husk charcoal being added pressure is in the high temperature carbonization furnace of 0.5MPa, be heated to 1000 DEG C and continue 5h at such a temperature, making the carbonization of coconut husk charcoal, vacuumize simultaneously, make the vacuum degree in carbide furnace be-20KPa, after cooling, obtain the coconut husk charcoal after carbonization;
Step 2, under argon atmosphere, coconut husk charcoal after carbonization step one obtained adds in graphitizing furnace, then injects coal tar pitch, and the dynamic viscosity of this coal tar pitch 60 DEG C time is 90Pas, abundant stirring, vacuumize simultaneously, make the vacuum degree in graphitizing furnace be-10KPa, at 2600 DEG C, then carry out graphitization, the graphited duration is 5h, obtains graphite after cooling.
Wherein, the mass ratio of coconut husk charcoal and coal tar pitch is 7:1.
Embodiment 2
The preparation method of a kind of graphite material of lithium ion battery that the present embodiment provides, comprises the following steps:
Step one, under nitrogen gas atmosphere, fruit shell carbon being added pressure is in the high temperature carbonization furnace of 0.8MPa, be heated to 1100 DEG C and continue 10h at such a temperature, making fruit shell carbon carbonization, vacuumize simultaneously, make the vacuum degree in carbide furnace be-30KPa, after cooling, obtain the fruit shell carbon after carbonization;
Step 2, under nitrogen gas atmosphere, coconut husk charcoal after carbonization step one obtained adds in graphitizing furnace, then injects petroleum asphalt, and the dynamic viscosity of this petroleum asphalt 60 DEG C time is 70Pas, abundant stirring, vacuumize simultaneously, make the vacuum degree in graphitizing furnace be-1KPa, at 2500 DEG C, then carry out graphitization, the graphited duration is 10h, obtains graphite after cooling.
Wherein, the mass ratio of fruit shell carbon and petroleum asphalt is 5:1.
Embodiment 3
The preparation method of a kind of graphite material of lithium ion battery that the present embodiment provides, comprises the following steps:
Step one, under nitrogen gas atmosphere, carbo lignius being added pressure is in the high temperature carbonization furnace of 1MPa, be heated to 1000 DEG C and continue 15h at such a temperature, making carbo lignius carbonization, vacuumize simultaneously, make the vacuum degree in carbide furnace be-1KPa, after cooling, obtain the carbo lignius after carbonization;
Step 2, under nitrogen gas atmosphere, carbo lignius after carbonization step one obtained adds in graphitizing furnace, then injects bitumen, and the dynamic viscosity of this bitumen 60 DEG C time is 60Pas, abundant stirring, vacuumize simultaneously, make the vacuum degree in graphitizing furnace be-80KPa, at 2700 DEG C, then carry out graphitization, the graphited duration is 1h, obtains graphite after cooling.
Wherein, the mass ratio of carbo lignius and bitumen is 10:1.
Embodiment 4
The preparation method of a kind of graphite material of lithium ion battery that the present embodiment provides, comprises the following steps:
Step one, under argon gas atmosphere, it is in the high temperature carbonization furnace of 0.1MPa that carbo lignius and ature of coal charcoal are added pressure, be heated to 1200 DEG C and continue 1h at such a temperature, make carbo lignius and the carbonization of ature of coal charcoal, vacuumize simultaneously, make the vacuum degree in carbide furnace be-99KPa, after cooling, obtain the carbo lignius after carbonization and ature of coal carbon mixture;
Step 2, under argon gas atmosphere, the carbo lignius after carbonization step one obtained and ature of coal charcoal add in graphitizing furnace, then inject petroleum asphalt and natural mixture of asphalt, the dynamic viscosity of this petroleum asphalt 60 DEG C time is 60Pas, the dynamic viscosity of this bitumen 60 DEG C time is 120Pas, fully stirs, vacuumizes simultaneously, the vacuum degree in graphitizing furnace is made to be-99KPa, then at 2650 DEG C, carry out graphitization, the graphited duration is 24h, obtains graphite after cooling.
Wherein, the mass ratio of carbo lignius, ature of coal charcoal, petroleum asphalt and bitumen is 4:4:1:1.
The graphite adopting the method for embodiment 1-4 to obtain is numbered S1-S4 respectively, as a comparison, commercially available native graphite is numbered D1, then use lithium sheet as negative pole, graphite is assembled into button cell as positive pole, arranges barrier film therebetween, perfusion electrolyte after ageing, first discharge with the electric current of 0.2mA, be discharged to 0.005V, allow the embedding lithium of graphite, after leaving standstill 10min, again with the current charges of 0.2mA to 2.000V, the gram volume of test graphite and discharging efficiency first, acquired results is in table 1.
Table 1: the gram volume recorded after the graphite being numbered S1-S4 and D1 is assembled into button cell and first discharging efficiency.
As can be seen from Table 1, the graphite adopting method of the present invention to prepare has the discharging efficiency first of higher gram volume and Geng Gao, this is because after injecting liquid bitumen between active carbon in the carbonized, the hole that active carbon after liquid bitumen can be full of carbonization exists, again through follow-up graphitization processing, the real density of graphite can be increased, and then improve its gram volume and discharging efficiency first.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-mentioned execution mode and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection range of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (9)
1. a preparation method for graphite material of lithium ion battery, is characterized in that, comprises the following steps:
Step one, under atmosphere of inert gases, adds active carbon in high temperature carbonization furnace, is heated to 900 ~ 1100 DEG C and makes active carbon carbonization, vacuumize simultaneously, after cooling, obtains the active carbon after carbonization;
Step 2, under atmosphere of inert gases, the active carbon after carbonization step one obtained adds in graphitizing furnace, then injects pitch, fully stirs, and vacuumizes simultaneously, then at 2500 ~ 2700 DEG C, carries out graphitization, obtains graphite after cooling;
The dynamic viscosity of pitch described in step 2 60 DEG C time is 60 ~ 120Pas.
2. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: active carbon described in step one is at least one in coconut husk charcoal, fruit shell carbon, carbo lignius and ature of coal charcoal.
3. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: pitch described in step 2 is at least one in coal tar pitch, petroleum asphalt and bitumen.
4. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: the mass ratio of described active carbon and described pitch is (5 ~ 10): 1.
5. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: the pressure vacuumizing front high temperature carbonization furnace in step one is 0.1 ~ 1MPa.
6. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: the vacuum degree vacuumized in step one in rear carbide furnace is-99KPa ~-1KPa; The vacuum degree vacuumized in step 2 in rear graphitizing furnace is-99KPa ~-1KPa.
7. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: the duration of carbonization described in step one is 30min ~ 24h.
8. the preparation method of graphite material of lithium ion battery according to claim 1, is characterized in that: the graphited duration described in step 2 is 30min ~ 24h.
9. the preparation method of the graphite material of lithium ion battery according to any one of claim 1 to 8, is characterized in that: described in step one and step 2, atmosphere of inert gases is argon atmosphere or nitrogen atmosphere.
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| CN106299240A (en) * | 2015-06-05 | 2017-01-04 | 东莞市亿顺新材料有限公司 | The preparation method of stabilized lithium metal |
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| CN101855757A (en) * | 2007-11-16 | 2010-10-06 | 旭化成株式会社 | Nonaqueous lithium-type storage element |
| CN102502594A (en) * | 2011-10-14 | 2012-06-20 | 上海理工大学 | Method for preparing isotropic graphite containing coal-based needle coke as aggregate |
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| CN101855757A (en) * | 2007-11-16 | 2010-10-06 | 旭化成株式会社 | Nonaqueous lithium-type storage element |
| CN102502594A (en) * | 2011-10-14 | 2012-06-20 | 上海理工大学 | Method for preparing isotropic graphite containing coal-based needle coke as aggregate |
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