CN105024075A - Negative electrode material for quickly rechargeable graphite lithium-ion battery and preparation method of negative electrode material - Google Patents
Negative electrode material for quickly rechargeable graphite lithium-ion battery and preparation method of negative electrode material Download PDFInfo
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Abstract
The invention discloses a negative electrode material for a quickly rechargeable graphite lithium-ion battery and a preparation method of the negative electrode material. The preparation method of the negative electrode material for the quickly rechargeable graphite lithium-ion battery comprises the following steps: (1) mixing a mixture containing a graphite precursor and bitumen and heating the mixture for kneading and crushing, wherein the mean grain size D50 of the graphite precursor ranges from 5 to 10 microns, and the mass ratio of the graphite precursor to the bitumen ranges from 50:50 to 90:10; (2) performing heat treatment at a temperature within the range of 300-700 DEG C under the protection of an inert gas; and (3) carrying out graphitizing. The mean grain size D50 of the negative electrode material prepared by use of the preparation method for the quickly rechargeable graphite lithium-ion battery is within the range of 5-15 microns and the specific surface area of the negative electrode material is below 2.0m2/g; the first discharge capacity of a negative electrode, manufactured by use of the negative electrode material for the quickly rechargeable graphite lithium-ion battery, is more than 355mAh/g, and the initial charge-discharge efficiency of the battery is above 90%; if the battery is quickly charged (1.5C) for 45 minutes, the capacity of the battery can be above 80%; in short, the product is high in discharge capacity and charge/discharge efficiency, and good in rate capability. The invention also relates to a battery comprising the negative electrode material for the quickly rechargeable graphite lithium-ion battery.
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 constantly increases small-size light-weight and requirement that is multi-functional, short time charging, 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.
Lithium rechargeable battery graphite cathode material, has very high discharge capacity, easily causes graphite synusia to come off, cause cycle performance of battery poor, poor stability in fast charging and discharging process.
Summary of the invention
Technical problem solved by the invention is, in order to overcome the defect that existing graphite cathode material fast charging and discharging process stability is poor, capacity attenuation is fast, to provide one and fill 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 graphite presoma with the mixture of pitch, heat and mediate, pulverize; Wherein, the average grain diameter D50 of described graphite presoma is 5 ~ 10 μm, and described graphite presoma and the mass ratio of described pitch are 50:50 ~ 90:10;
(2) under inert gas shielding, heat-treat in 300 ~ 700 DEG C;
(3) graphitization.
In step (1), described graphite presoma is petroleum coke and/or pitch coke.The average grain diameter D50 of described graphite presoma 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), described graphite presoma and the mass ratio of described pitch are 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.The mass ratio of described graphitization catalyst and graphite presoma is preferably 1:50 ~ 7:90, and that better is 3:100 ~ 3:50.
In step (1), graphite presoma 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 graphite presoma 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 graphite negative material of lithium ion battery obtained by above-mentioned preparation method.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 355mAh/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 of the graphite cathode material 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.
Petroleum coke is the CG-06 calcined petroleum coke that field refractory Company production is won in Yingkou.
Pitch coke is the calcining pitch coke that species abundance in Baosteel in Shanghai coke-oven plant 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
Petroleum coke (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 358.9mAh/g, and efficiency is 91.8% first, and rate of charge (1.5C) is 82.8%.
Embodiment 2
Petroleum coke (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 356.7mAh/g, and efficiency is 90.8% first, and rate of charge (1.5C) is 84.0%.
Embodiment 3
Pitch coke (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 357.2mAh/g, and efficiency is 91.3% first, and rate of charge (1.5C) is 82.1%.
Embodiment 4
By pitch coke (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 356.5mAh/g, and efficiency is 91.2% first, and rate of charge (1.5C) is 83.2%.
Embodiment 5
Petroleum coke (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 355.2mAh/g, and efficiency is 91.8% first, and rate of charge (1.5C) is 83.0%.
Embodiment 6
Petroleum coke (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 355.8mAh/g, and efficiency is 90.5% first, and rate of charge (1.5C) is 82.0%.
Embodiment 7
Pitch coke (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 356.2mAh/g, and efficiency is 91.0% first, and rate of charge (1.5C) is 83.8%.
Embodiment 8
Pitch coke (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 355.9mAh/g, and efficiency is 90.5% first, and rate of charge (1.5C) is 80.7%.
Comparative example 1
Petroleum coke (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 rate of charge.
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, after the forging that the coated heating of non-bituminous is mediated, the efficiency for charge-discharge of product is only 87.2% after petroleum coke graphitization, and rate of charge (1.5C) only reaches 70.8%.Adopt negative material prepared by the method for the invention, specific area reduces greatly, is less than 2.0m
2/ g, discharge capacity is all greater than 355mAh/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 the preparation method of graphite lithium ion battery negative material soon, it is characterized in that, it comprises the steps:
(1) mix including graphite presoma with the mixture of pitch, heat and mediate, pulverize; Wherein, the average grain diameter D50 of described graphite presoma is 5 ~ 10 μm, and described graphite presoma and the mass ratio of described pitch are 50:50 ~ 90:10;
(2) under inert gas shielding, heat-treat in 300 ~ 700 DEG C;
(3) graphitization.
2. 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 graphite presoma is petroleum coke and/or pitch coke.
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 graphite presoma 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 lithium ion battery negative material as claimed in claim 1 soon, it is characterized in that, in step (1), described graphite presoma and the mass ratio of described pitch are 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 the mass ratio of described graphitization catalyst and graphite presoma is 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 the mass ratio of described graphitization catalyst and graphite presoma is 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, graphite presoma 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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