CN102117911A - Graphite cathode material for lithium ion battery and preparation method thereof - Google Patents
Graphite cathode material for lithium ion battery and preparation method thereof Download PDFInfo
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- CN102117911A CN102117911A CN2009102477461A CN200910247746A CN102117911A CN 102117911 A CN102117911 A CN 102117911A CN 2009102477461 A CN2009102477461 A CN 2009102477461A CN 200910247746 A CN200910247746 A CN 200910247746A CN 102117911 A CN102117911 A CN 102117911A
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Abstract
The invention discloses a preparation method of a graphite cathode material for lithium ion batteries, which comprises the following steps: (1) mixing natural graphite and amorphous carbon precursor, heating at 400-600 DEG C to perform surface coating treatment of natural graphite; (2) performing carbonization treatment of the material obtained in step (1); (3) mixing the material obtained in step (2) and a conductive agent with a mass ratio of 90:10-99:1 to obtain the finished product; thereinto, the mass ratio of natural graphite and amorphous carbon precursor is 80:20-95:5, and the temperature of the carbonization treatment is 900-1600 DEG C. The graphite cathode material for lithium ion batteries of the invention has high discharge capacity and initial charge-discharge efficiency, and a long cycle life; the initial discharge capacity is above 355 mAh/g; the initial charge-discharge efficiency is above 92%; and the cycle performance is above 80% for 400 weeks. In the preparation method, the process is simple and practical; the source of raw materials is wide; and the cost is low.
Description
Technical field
The present invention is specifically related to a kind of silicon/carbon/graphite in lithium ion batteries negative material and preparation method thereof.
Background technology
Lithium ion battery is compared with original battery, with its energy density height, have extended cycle life, characteristics such as memory-less effect, popularized rapidly at aspects such as mobile phone, notebook computer and electric tools.Along with the requirement of various products to small-sized light weight and multi-functional, long-time drivingization constantly increases, the raising of capacity of lithium ion battery will depend on Development of Materials and perfect.Therefore, for a long time, improve lithium ion battery negative material specific capacity, reduce irreversible capacity first, improve cyclical stability, be the emphasis of research and development always.
Ion secondary battery cathode material lithium is at present mainly based on graphite-like.Comprising Delanium and native graphite class, Delanium is owing to need high temperature graphitization to handle in the course of processing, and cost is higher, and the cost performance that improves material is very difficult; Native graphite has desirable layer structure, has very high capacitance (near theoretical capacity 372mAh/g), and cost is low but there is structural instability in it, easily cause the common insertion of solvent molecule, its synusia in charge and discharge process is come off, cause cycle performance of battery poor, poor stability.
Therefore, for overcoming native graphite and the Delanium deficiency of performance separately, prior art all is that native graphite or Delanium are carried out the modification processing.Japan Patent JP10294111 carries out low temperature with pitch to graphite raw material of wood-charcoal material and coats, and need not melt after the coating to handle and slight the pulverizing, and this method is difficult to accomplish coat evenly.Japan Patent JP11246209 floods graphite and hard charcoal particle under 10～300 ℃ of temperature in pitch or tar, carry out separated from solvent and heat treatment then, this method is difficult to form at graphite and hard carbon surface and has the bitumen layer of certain thickness height polymerization, will be restricted for the raising of native graphite structural stability.Japan Patent JP2000003708 carry out roundingization with mechanical means to graphite material, floods in heavy oil, tar or pitch then, separates and washs, and sees close with JP11246209 merely from method for coating.Japan Patent JP2000182617 adopts native graphite etc. and pitch or resin or the charing altogether of its mixture, and this method can reduce the graphite material specific area, but is difficult to reach preferable control on covered effect.Japan Patent JP2000243398 is that the atmosphere of utilizing asphalt pyrolysis to produce is carried out surface treatment to graphite material, and the unlikely form of the material that is modified that makes of this method is greatly improved, thereby the raising of electrical property is restricted.Japan Patent JP2002042816 is that raw material coats with the CVD method or coats with pitch phenolic resins with aromatic hydrocarbons, and this and JP2000182617 and JP2000283398 have similarity on effect.
Summary of the invention
Technical problem to be solved by this invention is among the preparation method who overcomes existing modified natural graphite or Delanium, inhomogeneous, the difficult raising structural stability of material modified coating, electrical property improve defectives such as limited, and provide a kind of preparation method of silicon/carbon/graphite in lithium ion batteries negative material to reach by its silicon/carbon/graphite in lithium ion batteries negative material that makes.Silicon/carbon/graphite in lithium ion batteries negative material discharge capacity of the present invention and first charge-discharge efficiency height have extended cycle life; Discharge capacity is more than 355mAh/g first for it, and first charge-discharge efficiency is more than 92%, and 400 weeks of cycle performance are more than 80%.In its preparation method, technology is simple and easy to do, and raw material sources are extensive and cost is low.
The present invention relates to a kind of preparation method of silicon/carbon/graphite in lithium ion batteries negative material, it comprises the following step: 1. native graphite and amorphous charcoal predecessor are mixed, the surface of carrying out native graphite 400～600 ℃ of heating coats processing; 2. the material that 1. step is obtained carries out the charing processing; 3. material that 2. step is obtained and conductive agent mix according to 90: 10～99: 1 mass ratio, get final product; Wherein, the mass ratio of native graphite and amorphous charcoal predecessor is 80: 20～95: 5, and the temperature that charing is handled is 900～1600 ℃.
Wherein, what described native graphite was preferable is spherical natural graphite, and as potato shape or spherical, that average grain diameter is preferable is 5～30 μ m, preferred 15～25 μ m; Preferred 90: 10 of the mass ratio of described native graphite and amorphous charcoal predecessor; What described armorphous charcoal predecessor was preferable is petroleum asphalt, coal tar pitch or phenolic resins, preferred petroleum asphalt.Therefore the material that 2. obtains of step coats the native graphite of armorphous charcoal for the surface, and what these armorphous charcoals were preferable be the armorphous charcoal of petroleum asphalt, coal tar pitch or phenolic resins charing gained, preferably the armorphous charcoal of petroleum asphalt charing gained.
Among the present invention, preferred 1000～1250 ℃ of the temperature that described charing is handled.The optional carbon black of described conductive agent, vapor-grown carbon fibers or fine particle Delanium, preferred fine particle Delanium.
Among the preparation method of the present invention, but above-mentioned each optimum condition combination in any without prejudice to the field on the basis of common sense promptly makes each preferred embodiments of the present invention.
The invention further relates to the silicon/carbon/graphite in lithium ion batteries negative material that makes by above-mentioned preparation method.Preferable, its average grain diameter is 5～30 μ m, specific area is below 4.0m2/g.The performance parameter of the preferred silicon/carbon/graphite in lithium ion batteries negative material of the present invention is as shown in table 1.
Table 1
This shows that silicon/carbon/graphite in lithium ion batteries negative material of the present invention has reduced specific area effectively, has improved gram volume and discharging efficiency, the high comprehensive performance of the button cell that it is made.
Except that specified otherwise, raw material that the present invention relates to and reagent are all commercially available to be got.
Positive progressive effect of the present invention is: preparation method of the present invention can obtain adding after the native graphite surface modification treatment negative material of conductive additive again, and it has effectively solved the problem that exists in the current material.Among the preparation method of the present invention, technology is simple and easy to do, and raw material sources are extensive and cost is low.Owing to adopted methods such as surface modification treatment and adding conductive additive, silicon/carbon/graphite in lithium ion batteries negative material discharge capacity of the present invention and efficient height first, good cycle, its first discharge capacity more than 355mAh/g, first charge-discharge efficiency is more than 92%, and cycle performance is in 400 weeks more than 80%.
Description of drawings
The first charge-discharge curve of the graphite cathode material that Fig. 1 makes for embodiments of the invention 4.
The sem photograph of the graphite cathode material that Fig. 2 makes for embodiments of the invention 4.
The cycle performance figure of the graphite cathode material that Fig. 3 makes for embodiments of the invention 4.
Embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.
Raw material among the embodiment is conventional commercially available prod.
With embodiment 2 is that example illustrates lithium ion battery negative composite graphite preparation methods of the present invention:
Take by weighing the 18kg spherical natural graphite, D50 is 20.0 μ m, phosphorus content 99.96%; tap density is 0.98g/cm3, is crushed to the following petroleum asphalt 2kg of 0.1mm, 258 ℃ of the softening points of petroleum asphalt; quinoline insolubles 0.5% stirs alternately to join down and mixes in the reactor, heats to coat at 400～600 ℃ and handles; after coating end; under protection of nitrogen gas, carry out charing and handle, temperature is 1150 ℃ eventually; afterwards product is cooled to room temperature, obtains amorphous charcoal coated natural graphite.Amorphous charcoal coated natural graphite and conductive agent carbon black (the carbon black trade mark is the MA100 of Mitsubishi): the mass ratio by 99: 1 mixes, and makes lithium ion battery negative composite graphite material.Half-cell capacity 356.9mAh/g, efficient 93.8% first.
Table 2
| Embodiment | Pitch | Conductive agent | Spherical graphite particle diameter (μ m) | Spherical graphite/pitch (%) | Coated natural graphite/conductive agent (%) |
| 1 | Petroleum asphalt | Gas-phase growth of |
20 | 90∶10 | 99∶1 |
| 2 | Petroleum asphalt | Carbon black | 20 | 90∶10 | 99∶1 |
| 3 | Petroleum asphalt | The small particle diameter Delanium | 17 | 80∶20 | 92∶8 |
| 4 | Petroleum asphalt | The small |
20 | 90∶10 | 98∶2 |
| 5 | Petroleum asphalt | The small particle diameter Delanium | 23 | 95∶5 | 95∶5 |
| 6 | Coal tar pitch | Carbon black | 20 | 90∶10 | 99∶1 |
| 7 | Coal tar pitch | The small |
20 | 90∶10 | 95∶5 |
| 8 | Phenolic resins | Carbon black | 20 | 90∶10 | 99∶1 |
| 9 | Phenolic resins | The small |
20 | 90∶10 | 95∶5 |
| Comparing |
|
20 | 92/8 | Do not add conductive agent | |
| Comparing embodiment 2 | |
20 | 92/8 | Do not add conductive agent | |
| Comparing embodiment 3 | 20 | 100/0 | Do not add conductive agent |
In the table 2, described percentage is mass percent.
Wherein, the composition of the raw material among each embodiment or originate as follows: spherical graphite: phosphorus content among other embodiment＞99.94%, tap density＞0.96g/cm3, particle diameter is as shown in table 2; Coal tar pitch: 250～270 ℃ of softening points, quinoline insolubles＜2% is crushed to below the 0.1mm; The KS6 that small particle diameter Delanium: Timcal produces; Gas-phase growth of carbon fibre: the VGCF-H that Japan is clear and the electrician produces; Petroleum asphalt: 258 ℃ of softening points, quinoline insolubles 0.5%; Carbon black: the trade mark is the MA100 of Mitsubishi; Phenolic resins: the trade mark is 2130.
The electric performance test of the silicon/carbon/graphite in lithium ion batteries negative material that effect embodiment 1 the present invention and comparing embodiment make (half-cell method of testing)
The used half-cell method of testing of the present invention is: make 2430 type batteries, graphite sample, the N-methyl pyrrolidone that contains 6～7% Kynoar and 2% conductive black mix, be applied on the Copper Foil, it is that 110 ℃ of vacuum drying chamber vacuumizes 4 hours are standby that the pole piece that coats is put into temperature.Simulated battery is assemblied in the German Braun glove box of applying argon gas and carries out, electrolyte is 1M LiPF6+EC: EMC: DMC=1: 1: 1 (volume ratio), metal lithium sheet is to electrode, electrochemical property test carries out on U.S. ArbinBT2000 type cell tester, discharge and recharge system: 1) constant-current discharge (0.6mA, 0.01V); 2) leave standstill (10min); 3) (0.6mA 2.000V), the results are shown in Table 3 to constant current charge.
Table 3
| Embodiment | Particle diameter (μ m) | Specific area (m 2/g) | Discharge capacity (mAh/g) | Efficient (%) first | Circulate 400 weeks (%) |
| 1 | 21.2 | 3.6 | 356.9 | 92.8 | 84.0 |
| 2 | 21.3 | 3.8 | 357.0 | 92.6 | 83.9 |
| 3 | 17.6 | 3.2 | 358.2 | 92.3 | 85.8 |
| 4 | 21.7 | 2.5 | 360.5 | 93.2 | 86.8 |
| 5 | 23.0 | 3.4 | 357.2 | 91.8 | 83.8 |
| 6 | 20.8 | 3.0 | 357.8 | 92.5 | 85.0 |
| 7 | 20.1 | 3.4 | 356.2 | 92.0 | 84.8 |
| 8 | 20.6 | 3.8 | 359.0 | 92.0 | 84.5 |
| 9 | 19.3 | 3.7 | 358.2 | 91.8 | 83.2 |
| |
20.5 | 2.6 | 359.1 | 90.2 | 76 |
| Comparing embodiment 2 | 20.4 | 2.8 | 357.6 | 90.8 | 78 |
| Comparing embodiment 3 | 20 | 6.0 | 354.1 | 89.2 | 60 |
From top data as can be seen, the comparative example 3 spherical natural graphite specific area that is untreated is big, is 6.0m
2/ g, efficient is low first only 90.2%; The amorphous charcoal coats the minimum 356.2mAh/g of being of spherical graphic discharge capacity; Adopt the negative material of the described method preparation of patent, specific area reduces greatly less than 4.0m
2/ g, capacity are greater than 355mAh/g, and efficient is greater than 92%, and 400 weeks of circulating are all more than 80%.
The electric performance test of the silicon/carbon/graphite in lithium ion batteries negative material that effect embodiment 2 the present invention make (full battery testing method)
The used full battery testing method of the present invention is: make negative pole with the graphite material that the embodiment of the invention 4 makes, cobalt acid lithium is done anodal, 1M-LiPF6EC: EMC: DMC=1: 1: 1 (volume ratio) solution is done the electrolyte assembling and is helped battery, test 1C charges and discharge 400 all capability retentions more than 85.0%, as shown in Figure 3.
Claims (9)
1. the preparation method of a silicon/carbon/graphite in lithium ion batteries negative material is characterized in that comprising the following step: 1. native graphite and amorphous charcoal predecessor are mixed, carry out the surface coating of native graphite 400～600 ℃ of heating and handle; 2. the material that 1. step is obtained carries out the charing processing; 3. material that 2. step is obtained and conductive agent mix according to 90: 10～99: 1 mass ratio, get final product; Wherein, the mass ratio of native graphite and amorphous charcoal predecessor is 80: 20～95: 5, and the temperature that charing is handled is 900～1600 ℃.
2. preparation method as claimed in claim 1 is characterized in that: described native graphite is a spherical natural graphite, and average grain diameter is 5～30 μ m.
3. preparation method as claimed in claim 2 is characterized in that: the average grain diameter of described native graphite is 15～25 μ m.
4. preparation method as claimed in claim 1 is characterized in that: the mass ratio of described native graphite and amorphous charcoal predecessor is 90: 10.
5. preparation method as claimed in claim 1 is characterized in that: described armorphous charcoal predecessor is any one in petroleum asphalt, coal tar pitch or the phenolic resins.
6. preparation method as claimed in claim 1 is characterized in that: the temperature that described charing is handled is 1000～1250 ℃.
7. preparation method as claimed in claim 1 is characterized in that: described conductive agent be in carbon black, vapor-grown carbon fibers or the fine particle Delanium any one.
8. the silicon/carbon/graphite in lithium ion batteries negative material that makes as each described preparation method of claim 1～7.
9. silicon/carbon/graphite in lithium ion batteries negative material as claimed in claim 8 is characterized in that: its average grain diameter is 5～30 μ m, and specific area is at 4.0m
2Below/the g.
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| CN106252625A (en) * | 2016-08-26 | 2016-12-21 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of EV graphite negative material of lithium ion battery |
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