CN104900878B - Production method of artificial graphite anode material for high-capacity lithium ion battery - Google Patents

Production method of artificial graphite anode material for high-capacity lithium ion battery Download PDF

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CN104900878B
CN104900878B CN201510338421.XA CN201510338421A CN104900878B CN 104900878 B CN104900878 B CN 104900878B CN 201510338421 A CN201510338421 A CN 201510338421A CN 104900878 B CN104900878 B CN 104900878B
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raw material
lithium ion
mixing
production method
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CN104900878A (en
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王丽琼
叶涛
蔡奉翰
韩团辉
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Dalian Hongguang Lithium Industry Co.,Ltd.
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Dalian Hongguan Liye Co Ltd
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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
    • 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/10—Batteries in stationary systems, e.g. emergency power source in plant
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a production method of an artificial graphite anode material for a high-capacity lithium ion battery. Petroleum coke coarse powder is taken as a raw material A, asphalt micro powder is taken as a raw material B, and single transition metal micro powder and multiple transition metal mixed micro powder are taken as a raw material C; the raw materials A and C are mixed in certain weight ratio, graphitized at the temperature of 2,800 DEG C-3,200 DEG C and then smashed; the smashed mixed materials and the raw material B are mixed in a certain weight ratio, modified at the temperature of 300 DEG C-600 DEG C and then carbonized at the temperature of 1,200 DEG C-1,500 DEG C after mixing or are directly carbonized at the temperature of 1,200 DEG C-1,500 DEG C after mixing, and the mixed materials are smashed, subjected to impurity removal and sieved after cooled to the room temperature. The method has the advantages as follows: the degree of graphitization of the material is improved due to adding of metal elements, and the material capacity is improved; the raw material A is graphitized in a coarse powder state, the surface oxidation area and the oxidation degree of particles can be reduced, and the capacity of the material can be improved, and the yield can be increased.

Description

A kind of high-capacity lithium ion cell artificial plumbago negative pole material production method
Technical field
The present invention relates to a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, belongs to lithium ion battery Negative material technical field.
Background technology
Lithium ion battery is a kind of preferable green power supply, since coming out from nineteen ninety, because its remarkable performance is obtained Swift and violent development, lithium ion battery has captured rapidly many fields with the incomparable advantage of other batteries, such as known Mobile phone, notebook computer, camera, video camera and electric tool etc., and increasing country by lithium battery applications in electricity Stand, move the purposes such as power vehicle, military affairs.Wherein, negative material is the key factor of lithium ion battery energy storage, and its performance is certain The development level of lithium ion battery is decide in degree.Carbonaceous material is that lithium ion battery is studied and be applied to people's early start The material of negative pole, commercially still occupies an leading position so far.
Although the commercialization of the graphite cathode material of lithium ion battery, also there are some weakness for being difficult to overcome, develop The more excellent negative material of performance remains the important topic of Study on Li-ion batteries.The negative pole of lithium ion battery is by negative pole Active material material with carbon element or non-carbon material, adhesive, additive are mixed and made into pasty state binder and are coated uniformly on Copper Foil, and Jing does Dry, rolling is formed.Make lithium ion battery success, it is critical only that can prepare reversibly take off/embedding lithium ion it is negative Pole material.
In general, a kind of good negative material is selected to follow following principle：Specific energy is high, electrode potential is low, charge and discharge Electricity reaction good reversibility and electrolyte and binding agent it is compatible good.The crystal structure of material is regular, structure in charge and discharge process It is to obtain specific capacity height, the key of the lithium ion battery having extended cycle life that irreversible change does not occur.However, to intercalation materials of li ions Structure is still field link most weak at present with the research of performance.The present invention is ground for the reversibility of carbonaceous material Study carefully improvement, reach higher embedding lithium and cycle performance.
The content of the invention
It is an object of the invention to provide a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, to overcome Delanium raw material degree of oxidation in graphitizing process is too high, causes to lose capacity, Cycle Difference, the low artificial defect of yield.
Technical scheme：A kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, it is concrete raw Production. art is：
A raw material A is ground into the meal that particle diameter is 0.5～5.0mm by () with petroleum coke as raw material A, the raw material A is to prolong Petroleum coke or needle coke after slow petroleum coke, forging；
B () is crushed raw material B with airslide disintegrating mill with pitch as raw material B, be ground into the micro mist of particle diameter≤3 μm, institute Raw material B is stated for asphalt or coal tar pitch；
C (), with single transition metal micro mist or various transition metal admixed finepowders as raw material C, median is≤50nm, The transition metal chooses V, Ni, Co；
The raw material C micro mists that d raw material A meal and (c) step that () obtains (a) step is obtained are by weight A/C=100/ The ratio of (0.2～1) is stirred mixing, and graphitization is carried out at 2800～3200 DEG C after mixing, is crushed after cooling, powder Median is broken into for 12～18 μm, mechanical shaping process is then carried out, makes granule-morphology regular, be close to circle；
The raw material B micro mists that e material and (b) step that () obtains (d) step is obtained, by weight (A+C)/B=100/ The ratio of (2～8) is mixed, and is first modified at 300～600 DEG C after mixing, is then carried out at 1200～1500 DEG C Charing；Or directly carbonized at 1200～1500 DEG C after mixing；
F () is broken up, is sieved, removal of impurities after the material that (e) step is obtained is cooled to room temperature, obtain product.
The stirring mixing is using twin-screw or double ribbon agitating modes.
Beneficial effects of the present invention：
1st, meal is processed into because the present invention carries out mechanical crushing to petroleum coke, graphitization is carried out under meal state, can To reduce the integrated oxidation area of material and the degree of oxidation of individual particles, yield is kept；Jing after fine powder, material fine grained surface It is not oxidized, effective embedding lithium and ion transmission performance can be improved, and contribute to the solid tight of pitch-coating layer cladding, It is difficult for drop-off；
2nd, petroleum coke carries out graphitization under meal state, not only can reduce material oxidation degree, continues after bonding whole The specific surface area of material can be more reduced after shape process, the processing characteristics of raising material, i.e. pole piece compacting bounce-back are little, pole piece compacting is close Degree is high；
3rd, using transient metal doped graphitization, the degree of graphitization of material can be improved, that is, improves the capacity of Delanium； Using mechanical shaping, the uniformity of pitch-coating layer can be improved, so as to improve the uniform densification that SEI films are formed with electrolyte Property, reduce active site, and the tap density for improving material；
In sum, the present invention by using carry out under meal state graphitization, transient metal doped graphitization, thin The treatment technologies such as grain surface shaping can greatly play the reversible capacity and cycle life of material, and its production technology letter Single, production efficiency is high, and low cost, process safety can be used for industrialized production.
Specific embodiment：
Embodiment 1：
Petroleum coke raw material A 100kg after forging is weighed, the meal that particle diameter is about 2mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
The raw material A meal 60kg for crushing is weighed, raw material C micro mist 600g are added, mixing is stirred under normal temperature state 30 minutes, graphitization is then carried out at 3000 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 18 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 600g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1300 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 358.2mAh/g, discharging efficiency is 93.8%, as shown in table 1.
Embodiment 2：
Petroleum coke raw material A 100kg after forging is weighed, the meal that particle diameter is about 4mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 480g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 3000 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 17 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 800g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1400 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 357.8mAh/g, discharging efficiency is 94.3%, as shown in table 1.
Embodiment 3：
Acicular petroleum coke raw material A 100kg is weighed, the meal that particle diameter is about 4mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 540g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 3200 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 15 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 600g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1400 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 352.2mAh/g, discharging efficiency is 94.2%, as shown in table 1.
Embodiment 4：
Retard petroleum coke raw material A 100kg is weighed, the meal that particle diameter is about 5mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 300g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 2800 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 16 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 800g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1300 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 348.6mAh/g, discharging efficiency is 94.3%, as shown in table 1.
Embodiment 5：
Retard petroleum coke raw material A 100kg is weighed, the meal that particle diameter is about 3mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 180g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 3200 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 13 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 1200g are added, mixing 30min is carried out at normal temperatures, so It is modified at 300～600 DEG C afterwards, is and then carbonized at 1400 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 352.1mAh/g, discharging efficiency is 93.6%, as shown in table 1.
Embodiment 6：
Acicular petroleum coke raw material A 100kg is weighed, the meal that particle diameter is about 2mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 120g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 2900 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 14 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 400g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1300 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 343.2mAh/g, discharging efficiency is 94.3%, as shown in table 1.
Embodiment 7：
Acicular petroleum coke raw material A 100kg is weighed, the meal that particle diameter is about 1mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 360g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 3000 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 13 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 400g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1200 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 347.9mAh/g, discharging efficiency is 94.1%, as shown in table 1.
Embodiment 8：
Petroleum coke raw material A 100kg after forging is weighed, the meal that particle diameter is about 0.5mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 420g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 2800 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 12 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 400g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1300 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 349.8mAh/g, discharging efficiency is 94.2%, as shown in table 1.
Embodiment 9：
Retard petroleum coke raw material A 100kg is weighed, the meal that particle diameter is about 1mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 540g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 2800 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 15 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 600g are added, mixing 30min is carried out at normal temperatures, then It is modified at 300～600 DEG C, is and then carbonized at 1400 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 350.6mAh/g, discharging efficiency is 94.5%, as shown in table 1.
Embodiment 10：
Petroleum coke raw material A 100kg after forging is weighed, the meal that particle diameter is about 1mm is ground into.
Asphalt stock B 5kg are weighed, air-flow crushing, powder particle diameter≤3 μm are carried out.
Raw material A 60kg for crushing is weighed, raw material C 180g are added, mixing 30 minutes is stirred under normal temperature state, Then graphitization is carried out at 3200 DEG C.
The mixed material 50kg after graphitization is weighed, finely divided, classification is carried out, classification median is 13 μm, Ran Houjin Row mechanical shaping 30min.
The mixed material 20kg after shaping is weighed, raw material B micro mist 1000g are added, mixing 30min is carried out at normal temperatures, so It is modified at 300～600 DEG C afterwards, is and then carbonized at 1200 DEG C.
Material after carbonizing is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
Done experiment with LIR2430 type button cells, gained negative material discharge capacity is 353.9mAh/g, discharging efficiency is 94.2%, as shown in table 1.
Subordinate list 1
Button cell test data summary sheet

Claims (6)

1. a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, concrete production technology is：
（a）With petroleum coke as raw material A, raw material A is ground into into the meal that particle diameter is 0.5 ~ 5.0mm；
（b）With pitch as raw material B, raw material B is crushed with airslide disintegrating mill, be ground into the micro mist of particle diameter≤3 m；
（c）With single transition metal micro mist or various transition metal admixed finepowders as raw material C, median is≤50nm；
（d）Will（a）Raw material A meal that step is obtained and（c）The raw material C micro mists that step is obtained are by weight A/C=100/（0.2~ 1）Ratio be stirred mixing, carry out graphitization at 2800 ~ 3200 DEG C after mixing, crushed after cooling, in being ground into Position particle diameter is 12 ~ 18 m, then carries out mechanical shaping process；
（e）Will（d）Material that step is obtained and（b）The raw material B micro mists that step is obtained, by weight（A+C）/B=100/（2~8） Ratio mixed, be first modified at 300 ~ 600 DEG C after mixing, then carbonized at 1200 ~ 1500 DEG C；Or Directly carbonized at 1200 ~ 1500 DEG C after mixing；
（f）Treat（e）The material that step is obtained is cooled to after room temperature, is broken up, is sieved, removal of impurities, obtains product.
2. a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method as claimed in claim 1, its feature exists In：The raw material A is petroleum coke or needle coke after retard petroleum coke, forging.
3. a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method as claimed in claim 1, its feature exists In：The raw material B is asphalt or coal tar pitch.
4. a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method as claimed in claim 1, its feature exists In：The transition metal chooses V, Ni, Co.
5. a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method as claimed in claim 1, its feature exists In：Step（d）The material for obtaining carries out mechanical shaping process Jing after graphitization and crushing, makes granule-morphology regular, is close to circle Shape.
6. a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method as claimed in claim 1, its feature exists In：The stirring mixing is using twin-screw or double ribbon agitating modes.
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CN105272255A (en) * 2015-10-23 2016-01-27 广西兴安县桂兴矿粉厂 Manufacturing method of graphite electrode
CN109244392A (en) * 2018-08-23 2019-01-18 武汉艾特米克超能新材料科技有限公司 A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery
CN111048749B (en) * 2019-10-30 2022-01-14 深圳市卓能新能源股份有限公司 Negative pole piece, lithium ion battery and manufacturing method thereof
CN114725377B (en) * 2022-04-20 2024-04-19 太原理工大学 Needle coke regulated by transition metal and preparation and application thereof
CN114927685A (en) * 2022-06-28 2022-08-19 山西沁新能源集团股份有限公司 Catalytic graphitization coal-based negative electrode material and preparation method thereof

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CN102195036A (en) * 2010-03-05 2011-09-21 宁波杉杉新材料科技有限公司 Surface modified graphitized interphase carbon micro-powder and preparation method thereof
CN103066243A (en) * 2012-12-06 2013-04-24 中南大学 Coke powder-based cathode material of lithium ion power battery and preparation method thereof

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KR20130056668A (en) * 2011-11-22 2013-05-30 삼성전자주식회사 Composite negative active material, method of preparing the same and lithium secondary battery comprising the same

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CN103066243A (en) * 2012-12-06 2013-04-24 中南大学 Coke powder-based cathode material of lithium ion power battery and preparation method thereof

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