CN105024043A - Rapidly-charged graphite lithium ion battery anode material and preparation method thereof - Google Patents
Rapidly-charged graphite lithium ion battery anode material and preparation method thereof Download PDFInfo
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- CN105024043A CN105024043A CN201410784385.5A CN201410784385A CN105024043A CN 105024043 A CN105024043 A CN 105024043A CN 201410784385 A CN201410784385 A CN 201410784385A CN 105024043 A CN105024043 A CN 105024043A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a rapidly-charged graphite lithium ion battery anode material and a preparation method thereof. The preparation method for the rapidly-charged graphite lithium ion battery anode material comprises the following steps of: (1) mixing a mixture containing natural graphite and asphalt, and heating, kneading and smashing the mixture, wherein the average grain size D50 of the natural graphite is 5 to 10 micrometers, and the mass rate of the natural graphite to the asphalt is (50:50) to (90:10); (2) carrying out heat treatment at 300-700 DEG C under the protection of an inert gas; and (3) performing graphitizing. The average grain size D50 of the rapidly-charged graphite lithium ion battery anode material prepared according to the method is ranging from 5 micrometers to 15 micrometers, the specific surface area is less than 2.0 m<2>/g, the initial discharging capacity of the battery prepared from the rapidly-charged graphite lithium ion battery anode material is over 360 mAh/g, the initial charging and discharging efficiency is over 90 percent, the charging rate (1.5C) is over 80 percent, and a product is high in discharging capacity and charging and discharging efficiency and good in rate capability. The invention also relates to a battery, and the battery comprises the rapidly-charged graphite lithium ion battery anode material.
Description
Technical field
The present invention relates to graphite cathode material field, particularly relate to one and fill graphite lithium ion battery negative material and preparation method thereof soon.
Background technology
Lithium ion battery compared with original battery, high with its energy density, have extended cycle life, the feature such as memory-less effect, universal rapidly in mobile phone, notebook computer and electric tool etc.Along with various product is to small-size light-weight and continuous increase that is multi-functional, short time charging requirement, product requires also day by day to improve to the rapid charging performance of lithium ion battery, and the raising of current lithium ion battery rapid charging performance depends on the development and improvement of negative material.Therefore, the low temperature improving lithium ion battery negative material fills characteristic soon, is the focus of future studies exploitation.
The native graphite that ion secondary battery cathode material lithium uses has desirable layer structure, there is very high discharge capacity (close to theoretical capacity 372mAh/g), cost is low but it exists structural instability, in fast charging and discharging process, easily cause graphite synusia to come off, cause cycle performance of battery poor, poor stability.
Therefore, for overcoming the deficiency of native graphite charge-discharge performance, prior art is all carry out modification to native graphite.
It is coated that Japan Patent JP10294111 pitch carries out low temperature to graphite Carbon Materials, must not melt process and Light comminution after coated, and this method is difficult to accomplish evenly coated.
Graphite and hard charcoal particle flood by Japan Patent JP11246209 at 10 ~ 300 DEG C of temperature in pitch or tar, then separated from solvent and heat treatment is carried out, this method is difficult to form the bitumen layer with certain thickness high polymeric at graphite and hard carbon surface, and the raising for native graphite structural stability will be restricted.
Japan Patent JP2000003708 mechanically carries out rounding to graphite material, then floods in heavy oil, tar or pitch, then carries out being separated and washing, close with JP11246209 viewed from method for coating merely.
Japan Patent JP2000182617 adopts native graphite etc. and pitch or resin or its mixture Co carbonization, and this method can reduce graphite material specific area, but is difficult to reach better control on covered effect.
Japan Patent JP2000243398 is that the atmosphere utilizing asphalt pyrolysis to produce carries out surface treatment to graphite material, and this method is unlikely, and make the to be modified form of material is greatly improved, and thus makes the raising of electrical property be restricted.
Japan Patent JP2002042816 is that raw material chemical vapor deposition (CVD) method is carried out coated or carries out coated with pitch phenolic resins with aromatic hydrocarbons, and this and JP2000182617 and JP2000283398 have similarity in effect.
Summary of the invention
Technical problem solved by the invention is the defect that graphite cathode material fast charging and discharging process stability is poor, capacity attenuation is fast in order to overcome existing asphalt modification, provides one and fills graphite lithium ion battery negative material and preparation method thereof soon.
The present invention solves the problems of the technologies described above by the following technical programs.
The invention provides a kind of preparation method filling graphite lithium ion battery negative material soon, it comprises the steps:
(1) mix including native graphite with the mixture of pitch, heat and mediate, pulverize; Wherein, the average grain diameter D50 of described native graphite is 5 ~ 10 μm, and the mass ratio of described native graphite and described pitch is 50:50 ~ 90:10;
(2) under inert gas shielding, heat-treat in 300 ~ 700 DEG C;
(3) graphitization.
In step (1), described native graphite is preferably potato shape and/or spherical.The average grain diameter D50 of described native graphite is preferably 6 ~ 8 μm.
In step (1), described pitch can be the conventional pitch used in this area, and in the present invention, described pitch is preferably petroleum asphalt and/or coal tar pitch.The average grain diameter D50 of described pitch is preferably 2 ~ 10 μm.
In step (1), the mass ratio of described native graphite and described pitch is preferably 60:40 ~ 80:20.
In step (1), described mixture also can include the graphitization catalyst that this area routine uses, and described graphitization catalyst is preferably the carbide of silicon and/or the oxide of iron, and better is carborundum and/or iron oxide.Described graphitization catalyst and the mass ratio of native graphite are preferably 1:50 ~ 7:90, and that better is 3:100 ~ 3:50.
In step (1), native graphite and pitch, preferably for adopting cantilever double-spiral conical mixer to mix, alternately can add by the hybrid mode of described mixture when reinforced, to ensure to mix unanimously; Wherein, the rotating speed of described cantilever double-spiral conical mixer is preferably 35 ~ 37rpm; The time of described mixing is preferably 2 ~ 3 hours.Preferably, after employing cantilever double-spiral conical mixer mixes, then mix in kneading pot.
Described heating kneading process can make graphite granule, and modification is bonding equably, its concrete operation method can adopt the method for this area routine to carry out: by the mixture heat temperature raising of above-mentioned native graphite and pitch, carry out kneading process, such as, in kneading pot, carry out kneading process.
In step (1), the temperature that described heating is mediated is preferably 100 ~ 180 DEG C.The time that described heating is mediated is preferably 1 ~ 10 hour.Heating kneading time short meeting causes material to lump, and mixes uneven, and heating kneading time length can cause binder pitch volatilization loss, affects adhesive effect.
In step (1), described pulverizing is preferably for adopting machine hammer piece type crusher to pulverize.Pulverizing is to ensure that particles stick obtains evenly.
In step (2), described inert gas is preferably nitrogen and/or argon gas.
In step (2), described heat treated temperature is preferably 400 ~ 600 DEG C.The described heat treated time is preferably 12 ~ 24 hours.
In step (3), described graphitizing method can be the method for graphitizing that this area routine uses, and in the present invention, graphited temperature is preferably 2400 ~ 2800 DEG C.The graphited time is preferably 20 ~ 60 hours.
In the present invention, after described graphitization step, also can comprise sieve classification step.
Wherein, the method for described sieve classification can be this area conventional method, preferably for adopting oscillatory type screening machine and/or the classification of ultrasonic type screening machine.Guarantee that the average grain diameter D50 of particle reaches 5 ~ 15 μm by sieve classification, pattern, the high rate performance of product are better.
Present invention also offers a kind of obtained by above-mentioned preparation method fill graphite lithium ion battery negative material soon.The invention still further relates to a kind of battery, it includes and described fills graphite lithium ion battery negative material soon.
What obtain by above-mentioned preparation method fills graphite lithium ion battery negative material soon, and its average grain diameter D50 can between 5 ~ 15 μm, and specific area can at 2.0m
2/ below g.In the present invention, carry out performance test preferably filling soon in the button cell that graphite lithium ion battery negative material makes, discharge capacity is at more than 360mAh/g first, first charge-discharge efficiency is more than 90%, quick charge (1.5C) can reach more than 80% in 45 minutes, product discharge capacity and efficiency for charge-discharge high, good rate capability, its performance parameter is as shown in table 1.
Watch 1 fills the performance parameter of graphite lithium ion battery negative material soon
As seen from the above table, the graphite lithium ion battery negative material that fills soon of the present invention significantly reduces specific area, improves rate of charge, the high comprehensive performance of its button cell made.
On the basis meeting this area general knowledge, above-mentioned each optimum condition can combination in any, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially.
Positive progressive effect of the present invention is:
(1) preparation method's simple process of the present invention is easy, and raw material sources are extensive and cost is low.
(2) the graphite lithium ion battery negative material that fills soon of the present invention have employed the methods such as asphalt modification granulation process, graphitization, and productive rate is high, and operation is simple, obtained product discharge capacity and efficiency for charge-discharge high, good rate capability.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph filling graphite cathode material soon of the embodiment of the present invention 2.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or selects according to catalogue.
Native graphite is the QDC-80 native graphite that Qingdao Tai Neng graphite Co., Ltd produces.
Petroleum asphalt is the MQ-260 oil hard pitch that Dalian bright strengthening work Materials Co., Ltd produces.
Coal tar pitch is the modified coal tar pitch that Henan Bo Hai Chemical Co., Ltd. produces.
SiC is the GCF carborundum that Linyi Jin Meng carborundum Co., Ltd produces.
Embodiment 1
Native graphite (D50 is 6.0 μm) 16kg, petroleum asphalt (D50 is 4.0 μm) 4kg and graphitization catalyst (SiC) 0.8kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 160 DEG C and carry out kneading process 3 hours, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 500 DEG C, heat treatment granulation time 12 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 48 hours in 2400 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 364.9mAh/g, and efficiency is 91.8% first, and rate of charge (1.5C) is 82.8%.
Embodiment 2
Native graphite (D50 is 6.0 μm) 16kg, coal tar pitch (D50 is 6.4 μm) 4kg and graphitization catalyst (SiC) 0.8kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 160 DEG C and carry out kneading process 5 hours, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 500 DEG C, heat treatment granulation time 18 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 48 hours in 2400 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 363.7mAh/g, and efficiency is 90.8% first, and rate of charge (1.5C) is 84.0%.
Embodiment 3
Native graphite (D50 is 5.0 μm) 10kg, petroleum asphalt (D50 is 4.0 μm) 10kg and graphitization catalyst (SiC) 0.5kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 100 DEG C and carry out kneading process 10 hours, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 700 DEG C, heat treatment granulation time 18 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 20 hours in 2500 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 360.2mAh/g, and efficiency is 91.3% first, and rate of charge (1.5C) is 82.1%.
Embodiment 4
By native graphite (D50 is 7.5 μm) 14kg, petroleum asphalt (D50 is 4.0 μm) 6kg and graphitization catalyst (Fe
2o
3) 0.7kg alternately add in cantilever double-spiral conical mixer mix 2 hours, be added under stirring in kneading pot and mix, be heated to 140 DEG C and carry out kneadings process 5 hours, mediate terminate after, in tablet press machine, be pressed into sheet, beater disintegrating machine pulverizing.Under the protection of nitrogen, and heat-treat granulation at 600 DEG C, heat treatment granulation time 15 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 60 hours in 2800 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 360.5mAh/g, and efficiency is 91.2% first, and rate of charge (1.5C) is 83.2%.
Embodiment 5
Native graphite (D50 is 6.0 μm) 14kg, petroleum asphalt (D50 is 2.1 μm) 6kg and graphitization catalyst (SiC) 0.3kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 180 DEG C and carry out kneading process 1 hour, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 300 DEG C, heat treatment granulation time 24 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 48 hours in 2400 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 362.2mAh/g, and efficiency is 91.8% first, and rate of charge (1.5C) is 83.0%.
Embodiment 6
Native graphite (D50 is 10.0 μm) 18kg, coal tar pitch (D50 is 6.4 μm) 2kg and graphitization catalyst (SiC) 0.9kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 160 DEG C and carry out kneading process 2 hours, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 500 DEG C, heat treatment granulation time 20 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 48 hours in 2600 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 360.8mAh/g, and efficiency is 90.5% first, and rate of charge (1.5C) is 82.0%.
Embodiment 7
Native graphite (D50 is 6.0 μm) 14kg, coal tar pitch (D50 is 9.9 μm) 6kg and graphitization catalyst (SiC) 1.1kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 160 DEG C and carry out kneading process 2 hours, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 400 DEG C, heat treatment granulation time 24 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 40 hours in 2400 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 361.2mAh/g, and efficiency is 91.0% first, and rate of charge (1.5C) is 83.8%.
Embodiment 8
Native graphite (D50 is 6.0 μm) 14kg, petroleum asphalt (D50 is 4.0 μm) 6kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours, be added under stirring in kneading pot and mix, be heated to 160 DEG C and carry out kneading process 2 hours, after kneading terminates, in tablet press machine, be pressed into sheet, beater disintegrating machine is pulverized.Under the protection of nitrogen, and heat-treat granulation at 500 DEG C, heat treatment granulation time 18 hours, is cooled to room temperature by product afterwards, then carries out 48 hours graphitization processing in 2800 DEG C, obtains and fills graphite lithium ion battery negative material soon.Its button cell capacity is 365.9mAh/g, and efficiency is 90.5% first, and rate of charge (1.5C) is 80.7%.
Comparative example 1
Native graphite (D50 is 9.8 μm) 14kg, graphitization catalyst (SiC) 0.7kg are alternately added in cantilever double-spiral conical mixer and mix 2 hours.Under the protection of nitrogen, and heat-treat at 500 DEG C, heat treatment time 18 hours, is cooled to room temperature by product afterwards, then carries out catalyzed graphitization process in 48 hours in 2400 DEG C, obtained graphite negative material of lithium ion battery.Its button cell capacity is 354.1mAh/g, and efficiency is 87.2% first, and rate of charge (1.5C) is 70.8%.
Effect example
(1) graphite cathode material in embodiment 1 ~ 8 and comparative example 1 is carried out the item such as particle diameter, specific area index test respectively, the results are shown in Table 2.The instrument title that test uses and model are: particle diameter, laser fineness gage MS2000; Specific area, specific surface area measuring instrument NOVA2000.
(2) adopt button cell method of testing to carry out the test of discharge capacity and efficiency first to the graphite cathode material in embodiment 1 ~ 8 and comparative example 1, the results are shown in table 2.
The present invention's button cell method of testing used is: in carboxymethyl cellulose (CMC) aqueous solution, add conductive black, then graphite sample is added, finally add butadiene-styrene rubber (SBR), stir, slurry is coated on Copper Foil by coating machine uniformly and makes pole piece.The pole piece coated being put into temperature is 110 DEG C of vacuum drying chamber vacuumizes 4 hours, takes out pole piece roll extrusion on roll squeezer, for subsequent use.Simulated battery is assemblied in the German Braun glove box of applying argon gas and carries out, and electrolyte is 1MLiPF6EC:DEC:DMC=1:1:1(volume ratio), metal lithium sheet is to electrode.Volume test is carried out on U.S. ArbinBT2000 type cell tester, and charging/discharging voltage scope is 0.005 to 2.0V, and charge-discharge velocity is 0.1C.
The present invention's rate of charge method of testing used is: the graphite of the embodiment of the present invention or comparative example makes negative pole, and cobalt acid lithium makes positive pole, 1MLiPF6EC:DMC:EMC=1:1:1(volume ratio) solution does electrolyte assembling and helps battery, test 1.5C ~ 2.0C discharge-rate.
The performance parameter of table 2 embodiment and comparative example
Data as can be seen from table 2, the discharge capacity in comparative example 1 and efficiency for charge-discharge low, the efficiency for charge-discharge of native graphite that the coated heating of non-bituminous is mediated is only 87.2%, and rate of charge (1.5C) only reaches 70.8%.And the negative material adopting the method for the invention to prepare, specific area reduces greatly, is all less than 2.0m
2/ g, equal discharge capacity is greater than 360mAh/g, and efficiency for charge-discharge is all greater than 90%, and rate of charge (1.5C) is all more than 80%.
Claims (16)
1. fill a preparation method for graphite lithium ion battery negative material soon, it is characterized in that, it comprises the steps:
(1) mix including native graphite with the mixture of pitch, heat and mediate, pulverize; Wherein, the average grain diameter D50 of described native graphite is 5 ~ 10 μm, and the mass ratio of described native graphite and described pitch is 50:50 ~ 90:10;
(2) under inert gas shielding, heat-treat in 300 ~ 700 DEG C;
(3) graphitization.
2. fill as claimed in claim 1 the preparation method of graphite lithium ion battery negative material soon, it is characterized in that, in step (1), described native graphite is potato shape and/or spherical.
3. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), the average grain diameter D50 of described native graphite is 6 ~ 8 μm.
4. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), described pitch is petroleum asphalt and/or coal tar pitch, and the average grain diameter D50 of described pitch is 2 ~ 10 μm.
5. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), the mass ratio of described native graphite and described pitch is 60:40 ~ 80:20.
6. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), described mixture also comprises graphitization catalyst.
7. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 6 soon, it is characterized in that, described graphitization catalyst is the carbide of silicon and/or the oxide of iron, and described graphitization catalyst and the mass ratio of native graphite are 1:50 ~ 7:90.
8. the preparation method filling graphite lithium ion battery negative material soon as claimed in claims 6 or 7, it is characterized in that, described graphitization catalyst is carborundum and/or iron oxide, and described graphitization catalyst and the mass ratio of native graphite are 3:100 ~ 3:50.
9. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), the mode of the mixing of mixture mixes for adopting cantilever double-spiral conical mixer, native graphite and pitch is alternately added time reinforced; The rotating speed of described cantilever double-spiral conical mixer is 35 ~ 37rpm; The time of described mixing is 2 ~ 3 hours.
10. fill the preparation method of graphite lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), described heating is mediated and is carried out in kneading pot, the temperature that described heating is mediated is 100 ~ 180 DEG C, and the time that described heating is mediated is 1 ~ 10 hour.
11. preparation methods filling graphite lithium ion battery negative material soon as claimed in claim 1, it is characterized in that, in step (2), described heat treated temperature is 400 ~ 600 DEG C, and the described heat treated time is 12 ~ 24 hours.
12. preparation methods filling graphite lithium ion battery negative material soon as claimed in claim 1, it is characterized in that, in step (3), described graphited temperature is 2400 ~ 2800 DEG C, and the described graphited time is 20 ~ 60 hours.
13. preparation methods filling graphite lithium ion battery negative material soon as claimed in claim 1, is characterized in that, also comprise sieve classification step after described graphitization step.
14. fill graphite lithium ion battery negative material soon, and it is obtained by such as the preparation method in claim 1 ~ 13 as described in any one.
15. fill graphite lithium ion battery negative material as claimed in claim 14 soon, and its average grain diameter D50 is between 5 ~ 15 μm, and specific area is at 2.0m
2/ below g.
16. 1 kinds of batteries, it comprises fill graphite lithium ion battery negative material soon as described in claims 14 or 15.
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