CN1624955A - Method for manufacturing carbon nagtive electrode material of lithium ion cell - Google Patents

Method for manufacturing carbon nagtive electrode material of lithium ion cell Download PDF

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Publication number
CN1624955A
CN1624955A CNA2003101089828A CN200310108982A CN1624955A CN 1624955 A CN1624955 A CN 1624955A CN A2003101089828 A CNA2003101089828 A CN A2003101089828A CN 200310108982 A CN200310108982 A CN 200310108982A CN 1624955 A CN1624955 A CN 1624955A
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lithium ion
ion cell
electrode material
negative electrode
carbon negative
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马军旗
王剑桥
付振明
丁晓阳
黎韶明
张殿浩
冯苏宁
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Shanghai Shanshan Technology Co Ltd
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Shanghai Shanshan Technology Co Ltd
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Priority to CNA2003101089828A priority Critical patent/CN1624955A/en
Priority to PCT/CN2004/001297 priority patent/WO2005055346A1/en
Publication of CN1624955A publication Critical patent/CN1624955A/en
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    • C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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    • 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
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Abstract

This invention uses the natural graphite especially the ball-shape natural graphite as raw material A, coal tar/ coal asphalt/ oil asphalt or their mixture as raw material B, mixes the two raw materials according to the proportion A/B=1/0.5-10, carries out polyreaction in the temperature range of 350-500deg.C, the pressure of 0.01-10 MPa, the reaction time is 5-420 minutes, dries after extracting and dispersing, controls the weight adding of dried products is 2-100% of the graphite raw material, and gains a lithium battery carbon negative pole material coasted with natural graphite or artificial graphite through carburization or graphitization. This carbon negative pole material has high specific capacity, long cycling service life.

Description

A kind of manufacture method of carbon negative electrode material of lithium ion cell
Technical field
The present invention relates to the manufacture method of cell negative electrode material, relate in particular to a kind of manufacture method of carbon negative electrode material of lithium ion cell.
Background technology
Lithium ion battery negative material mainly contains two kinds of Delanium and native graphites based on the raw material of wood-charcoal material.Delanium has MCMB such as CMS and MCMB, phase charcoal fiber MCF and graphous graphite powder in the middle of also having.Preceding two kinds of Delaniums are the negative materials that are widely adopted, has the advantage that particle shape is good, irreversible capacity loss is low, cycle life is stable, but also have production cost height, deficiency that discharge capacity is low, the discharge capacity of MCMB is generally about 320mAh/g.Irregular form graphous graphite powder is owing to exist the shortcoming that tap density is low, specific area is high to be not suitable for directly using as negative material.The native graphite cost of material is low, and its higher degree of graphitization makes it have higher embedding lithium ability, but there is the shortcoming that tap density is low, specific area is high equally in the native graphite of sheet, is not suitable for directly using as negative material.Irreversible capacity loss is very high first not pass through the natural graphite negative electrode material of modification, generally can reach 10%, owing to solvent takes place embed altogether, causes problems such as capacity attenuation is fast at circulation time.
For a long time, the irreversible capacity loss first of the capacitance of raising Delanium, minimizing native graphite improves the emphasis that its cycle performance is research and development always.Particularly the modification for native graphite has proposed a lot of methods.
Japan Patent JP10294111 carries out low temperature with pitch to graphite raw material of wood-charcoal material and coats, and must not melt after the coating to handle and slight the pulverizing, and this method is wanted strict control covering amount.If lower to native graphite class negative material covering amount, cyclical stability just is difficult to be greatly improved.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 covering amount and 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
Purpose of the present invention is exactly to provide a kind of technology simple in order to overcome the defective that above-mentioned prior art exists, and product is the also manufacture method of improved carbon negative electrode material of lithium ion cell of cycle performance when obtaining high power capacity.
Purpose of the present invention can be achieved through the following technical solutions: a kind of manufacture method of carbon negative electrode material of lithium ion cell is characterized in that this method comprises following processing step:
(1) with the native graphite being clad material (A), is clad material (B) with heavy arene or its mixture, weight ratio (A): (B)=1: 0.5～10;
(2) raw material that will satisfy step (1) requirement is consolidated-the liquid mixing, in 350～500 ℃ temperature range, carries out polymerization reaction under 0.01～10MPa pressure condition, and in 5～450 minutes reaction time, the native graphite surface obtains the coating layer of microencapsulation;
(3) from reaction system, isolate solid phase particles with separation method;
(4) remove light component in the solid phase particles with drying means, the control dried product exhibited with respect to the weightening finish of graphite raw material 2～100%;
(5) obtain the carbon cathode material that the surface coats the charcoal layer by charing, carbonization temperature is 800～2200 ℃, perhaps obtains the carbon cathode material that expression coats the Delanium layer by graphitization, and graphitization temperature is 2400～3000 ℃.
Described native graphite is sphere or sheet native graphite.
Described heavy arene or its mixture are selected from coal tar, coal tar pitch, petroleum asphalt or its mixture.
Described separation method adopts a kind of in solvent segregation, centrifugal separation, the separation by precipitation.
The solvent that described solvent segregation adopted is selected from a kind of in carbolineum, washing oil, diesel oil, pyridine, quinoline, dimethylbenzene, the toluene; The weight ratio of this solvent and product is 0.5～5: 1.
The baking temperature of described drying means is 200～500 ℃.
Described graphitization temperature is 2800～3000 ℃.
The present invention is a kind of new method of producing negative material that puts forward on the basis of pluses and minuses separately at research various Delaniums and modified natural graphite negative material, it is to coat raw material with the heavy arene, under hot conditions, consolidating-liquid interface polymerization reaction take place, utilize product that solid phase particles is coated, after separating, obtain the micron particles of microencapsulation, obtain carbon cathode material by the heat treatment means again.
The carbon negative pole material that obtains with the present invention has the following advantages:
(1) raw material obtains easily;
(2) reparation technology is simple, especially is fit to large-scale production, constant product quality;
(3) product form is improved significantly, and processing characteristics improves;
(4) be greatly improved with respect to Delanium and native graphite properties of product, when obtaining high power capacity, the cycle performance of product also improves.
Embodiment
1 is encapsulated material with the especially spherical native graphite of native graphite, graphite granule D 50Between 5～45 μ m, the carbon content of graphite raw material should be more than 99%.The tap density of spherical native graphite preferably reaches 0.90g/cm 3More than.
2 serves as to coat the material raw material with coal tar/coal tar pitch/petroleum asphalt or its mixture, also can be with the by-product pitch of production MCMB as clad material.The ratio of clad material and encapsulated material is 1/0.5～10.
3 pairs are satisfied the above raw material that requires and consolidate-the liquid mixing, be warmed up in 350～500 ℃ the temperature range and carry out thermal polymerization, polymerization pressure is 5～420 minutes at 0.01～10MPa in the reaction time of control temperature, and the native graphite surface obtains the coating layer of microencapsulation.
4 usefulness separated from solvent/centrifugation/methods such as precipitate and separate are isolated solid phase particles from reaction system.Solvent can be the solvents stronger to the pitch solvability such as carbolineum, washing oil, diesel oil, pyridine, quinoline, dimethylbenzene, toluene.The ratio of solvent and product is 0.5～5/1.
5 can with filter, method such as centrifugal, precipitation isolates solid phase particles from solution.
6 usefulness drying means are removed the light component in the solid phase particles, 200～500 ℃ of baking temperatures, and dry back is controlled at 2～100% with respect to the weightening finish of graphite raw material.
7 carbon cathode materials by charing acquisition surface coating charcoal layer, carbonization temperature is 800～2200 ℃; Perhaps obtain the carbon cathode material that the surface coats the Delanium layer by graphitization, 2400～3000 ℃ of graphitization temperatures are preferably in more than 2800 ℃.
Embodiment 1～13
Embodiment Graphite (A) Clad material (B) Ratio A/B Reaction temperature ℃ Reaction pressure MPa Reaction time min Charing ℃ Graphitization ℃
????1 Spherical Coal tar pitch ??1/1 ??400 ??0.10 ??60 ?1000
????2 Spherical Coal tar pitch ??1/2 ??420 ??0.10 ??120 ?＞2600
????3 Spherical Coal tar pitch ??1/4 ??450 ??0.01 ??180 ?＞2800
????4 Sheet Coal tar pitch ??1/6 ??450 ??0.10 ??180 ?＞2800
????5 Sheet Coal tar pitch ??1/10 ??450 ??0.50 ??180 ?＞2800
????6 Spherical Coal tar ??1/0.8 ??350 ??0.10 ??30 ?2000
????7 Spherical Coal tar ??1/1 ??420 ??0.10 ??120 ?＞2800
????8 Spherical By-product pitch ??1/0.5 ??400 ??0.10 ??5 ?900
????9 Spherical By-product pitch ??1/2 ??420 ??0.10 ??120 ?＞2400
????10 Spherical Petroleum asphalt ??1/3 ??450 ??0.50 ??450 ?＞2800
????11 Sheet Petroleum asphalt ??1/4 ??450 ??0.01 ??450 ?＞2800
????12 Spherical Coal tar pitch+petroleum asphalt ??1/3 ??450 ??0.10 ??450 ?＞2800
????13 Spherical Coal tar pitch+petroleum asphalt ??1/4 ??500 ??10.00 ??450 ?＞3000
The performance parameter of embodiment 1～13
Embodiment ??D 50??μm Weightening finish % Real density g/cm 3 Tap density g/cm 3 Specific area m 2/g Discharge capacity mAh/g first Discharging efficiency % first Keep 90% capacity cycle-index
????1 ??20.1 ??6.2 ????2.18 ????1.25 ????2.6 ??354 ??94.3
????2 ??21.0 ??10.0 ????2.20 ????1.27 ????2.3 ??351 ??94.6
????3 ??21.5 ??21.3 ????2.21 ????1.28 ????1.7 ??355 ??95.3 ??450
????4 ??23.1 ??74.3 ????2.19 ????1.17 ????1.6 ??341 ??95.6
????5 ??25.3 ??103.0 ????2.22 ????1.19 ????1.4 ??338 ??94.9
????6 ??13.1 ??5.6 ????2.18 ????1.21 ????2.2 ??349 ??94.7
????7 ??14.5 ??12.0 ????2.10 ????1.22 ????2.0 ??350.0 ??95.8
????8 ??13.6 ??2.4 ????2.19 ????1.20 ????2.4 ??355.2 ??93.7
????9 ??13.9 ??10.2 ????2.21 ????1.22 ????2.3 ??346.0 ??94.6
????10 ??25.6 ??15.4 ????2.20 ????1.31 ????1.8 ??352.1 ??95.8 ??500
????11 ??26.3 ??25.1 ????2.23 ????1.13 ????1.6 ??354.0 ??95.7
????12 ??27.4 ??30.0 ????2.20 ????1.35 ????1.5 ??359.0 ??95.3 ??450
????13 ??28.0 ??38.9 ????2.19 ????1.39 ????1.5 ??357.6 ??94.9

Claims (7)

1. the manufacture method of a carbon negative electrode material of lithium ion cell is characterized in that, this method comprises following processing step:
(1) with the native graphite being clad material (A), is clad material (B) with heavy arene or its mixture, weight ratio (A): (B)=1: 0.5～10;
(2) raw material that will satisfy step (1) requirement is consolidated-the liquid mixing, in 350～500 ℃ temperature range, carries out polymerization reaction under 0.01～10MPa pressure condition, and in 5～450 minutes reaction time, the native graphite surface obtains the coating layer of microencapsulation;
(3) from reaction system, isolate solid phase particles with separation method;
(4) remove light component in the solid phase particles with drying means, the control dried product exhibited with respect to the weightening finish of graphite raw material 2～100%;
(5) obtain the carbon cathode material that the surface coats the charcoal layer by charing, carbonization temperature is 800～2200 ℃, perhaps obtains the carbon cathode material that expression coats the Delanium layer by graphitization, and graphitization temperature is 2400～3000 ℃.
2. the manufacture method of a kind of carbon negative electrode material of lithium ion cell according to claim 1 is characterized in that, described native graphite is sphere or sheet native graphite.
3. the manufacture method of a kind of carbon negative electrode material of lithium ion cell according to claim 1 is characterized in that, described heavy arene or its mixture are selected from coal tar, coal tar pitch, petroleum asphalt or its mixture.
4. the manufacture method of a kind of carbon negative electrode material of lithium ion cell according to claim 1 is characterized in that, described separation method adopts a kind of in solvent segregation, centrifugal separation, the separation by precipitation.
5. the manufacture method of a kind of carbon negative electrode material of lithium ion cell according to claim 4 is characterized in that, the solvent that described solvent segregation adopted is selected from a kind of in carbolineum, washing oil, diesel oil, pyridine, quinoline, dimethylbenzene, the toluene; The weight ratio of this solvent and product is 0.5～5: 1.
6. the manufacture method of a kind of carbon negative electrode material of lithium ion cell according to claim 1 is characterized in that, the baking temperature of described drying means is 200～500 ℃.
7. the manufacture method of a kind of carbon negative electrode material of lithium ion cell according to claim 1 is characterized in that, described graphitization temperature is 2800～3000 ℃.
CNA2003101089828A 2003-12-01 2003-12-01 Method for manufacturing carbon nagtive electrode material of lithium ion cell Pending CN1624955A (en)

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PCT/CN2004/001297 WO2005055346A1 (en) 2003-12-01 2004-11-15 A process of production of carbon negative electrode material for lithium ion battery

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Cited By (19)

* Cited by examiner, † Cited by third party
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CN101186292A (en) * 2006-11-22 2008-05-28 辽宁工程技术大学 Method for preparing carbon cathode material and lithium iron battery using the material
CN100420627C (en) * 2006-08-14 2008-09-24 长沙市海容电子材料有限公司 Graphite material with shell-core structure and preparation method thereof
CN1907848B (en) * 2005-08-04 2010-11-10 中央电气工业株式会社 Carbon powder for use in cathode materials of non-aqueous secondary battery
CN101986392A (en) * 2010-05-25 2011-03-16 华东理工大学 A conducting material and preparation method and use thereof
CN102485648A (en) * 2010-12-03 2012-06-06 上海杉杉科技有限公司 Modified graphite, composite graphite material containing the modified graphite and their preparation methods and application
CN102557015A (en) * 2010-12-31 2012-07-11 上海杉杉科技有限公司 Carbon material with isotropic fine structure and preparation method for same
CN103311521A (en) * 2012-03-07 2013-09-18 上海杉杉科技有限公司 Surface-modified graphite negative electrode material, and preparation method and application thereof
CN103346326A (en) * 2013-07-08 2013-10-09 辽宁弘光科技(集团)有限公司 Preparation method for carbon cathode material of lithium ion battery
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CN103626147A (en) * 2012-08-23 2014-03-12 上海杉杉科技有限公司 Lithium ion battery cathode composite material and preparation method thereof
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