CN103682347B - Composite lithium ion battery cathode material - Google Patents

Composite lithium ion battery cathode material Download PDF

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Publication number
CN103682347B
CN103682347B CN201310491729.9A CN201310491729A CN103682347B CN 103682347 B CN103682347 B CN 103682347B CN 201310491729 A CN201310491729 A CN 201310491729A CN 103682347 B CN103682347 B CN 103682347B
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lithium ion
ion battery
cathode material
battery cathode
percentage
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CN103682347A (en
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罗建伟
黄雨生
吴壮雄
杨建锋
周新
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JIANGXI ZHENGTUO NEW ENERGY TECHNOLOGY POLYTRON Co Ltd
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JIANGXI ZHENGTUO NEW ENERGY TECHNOLOGY POLYTRON 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • 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

Abstract

The invention relates to a kind of composite lithium ion battery cathode material, this composite lithium ion battery cathode material is mainly composed of the following components: needle-like coke powder, and percentage by weight is 30%-50%; Natural spherical plumbago powder, percentage by weight is 20%-30%; Isotropism coke powder, percentage by weight is 15%-25%; Pitch coke powder, percentage by weight is 10%-20%.Present invention also offers a kind of preparation method of composite lithium ion battery cathode material.Composite lithium ion battery cathode material of the present invention has good imbibition ability, liquid-keeping property, cycle performance, cryogenic property, energy density and power density, and has the feature of security performance excellence.

Description

Composite lithium ion battery cathode material
Technical field
The present invention relates to a kind of negative material of field of batteries, particularly relate to a kind of composite lithium ion battery cathode material.
Background technology
Compared with lithium ion battery miscellaneous part, the development of lithium ion battery negative material is comparatively ripe.In commercial applications, graphite-like material with carbon element technology is comparatively ripe, the market price is also more stable, but constantly promotes along with the requirement of lithium-ion-power cell to performances such as energy density, power density, safety, and existing negative material more and more can not meet current demand.
Lithium ion battery negative material requires to possess following feature: 1. alap electrode potential; 2. ion has higher diffusivity in negative pole solid-state structure; 3. the deintercalation invertibity of height; 4. good conductivity and thermodynamic stability; 5. security performance is good; 6. good with electrolyte solvent compatibility; 7. aboundresources, cheap; 8. safe, pollution-free.
At present, have the research of lithium ion battery negative material is more: material with carbon element, silica-base material, tin-based material, lithium titanate, transition metal oxide etc.
Graphite-like material with carbon element Technical comparing is ripe, better performances in safety and cycle life, and cheap, nontoxic, is comparatively common negative material.Traditional lithium-ion battery negative material comprises native graphite, modifying natural graphite material, MCMB and petroleum coke class Delanium.Native graphite and modifying natural graphite material price lower, but at efficiency for charge-discharge with need in useful life to be improved further.The product of petroleum coke class is more outstanding in discharging efficiency and cycle life, but there is the problem of high cost and complicated process of preparation.
In recent years, along with deepening continuously of research work, researcher finds by carrying out surface modification and structural adjustment to graphite and all kinds of material with carbon element, or makes graphite part disordering, or the structures such as nano level hole, hole and passage are formed in all kinds of material with carbon element, be conducive to lithium embedding-deintercalation wherein.At present, owing to there is the problems such as first effect is low, compacted density is low, technique is immature in hard carbon material, therefore, also do not enter the large-scale commercial stage, domestic association area is still under test, and pertinent literature report seldom.
Electrokinetic cell market demands lithium ion battery has high-rate discharge ability, high safety performance, high efficiency, high cycle life.Meanwhile, for the industrialization prospect of electric automobile, material leaved for development should have the feature of low cost.
Because the defect that above-mentioned existing lithium ion battery negative material exists, the present inventor is based on being engaged in the practical experience and professional knowledge that this type of product design manufacture enriches for many years, and coordinate the utilization of scientific principle, actively in addition research and innovation, to founding a kind of new composite lithium ion battery cathode material, can improve general existing lithium ion battery negative material, make its performance more excellent, cost is cheaper.Through constantly research, design, and after repeatedly studying and improving, finally create the present invention had practical value.
Summary of the invention
Main purpose of the present invention is, overcome the defect that existing lithium ion battery negative material exists, and a kind of new composite lithium ion battery cathode material is provided, technical problem to be solved is the improvement by lithium ion battery negative material performance, thus improves specific capacity, the first coulombic efficiency of lithium ion battery.
Another object of the present invention is by NEW TYPE OF COMPOSITE lithium ion battery negative material, thus the defect that the useful life overcoming existing lithium-ion-power cell is shorter, cryogenic property is poor.
Another object of the present invention is, provides a kind of method preparing composite lithium ion battery cathode material, and the method step is relatively simple, thus is more suitable for practicality.
The object of the invention to solve the technical problems realizes by the following technical solutions.According to a kind of composite lithium ion battery cathode material that the present invention proposes, it is mainly composed of the following components: needle-like coke powder, and percentage by weight is 30%-50%; Natural spherical plumbago powder, percentage by weight is 20%-30%; Isotropism coke powder, percentage by weight is 15%-25%; Pitch coke powder, percentage by weight is 10%-20%.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid composite lithium ion battery cathode material, it contains percentage by weight is further the isotope of 1%-5%.
Aforesaid composite lithium ion battery cathode material, the calcining heat of wherein said needle-like coke powder is 1400 DEG C-1600 DEG C, bulk density is 0.7-0.8 gram/cc, particle diameter is 10 nanometer-300 nanometers, the particle diameter of described natural spherical plumbago powder is 10 nanometer-800 nanometers, and phosphorus content is 99.93%-99.99%, and the particle diameter of described isotropism coke powder is 100 nanometer-300 nanometers, the particle diameter of described pitch coke powder is 100 nanometer-500 nanometers, and ash content is less than 0.05%.
Aforesaid composite lithium ion battery cathode material, isotope choosing is made up of isotope crystal, isotope alloy crystal or its compound crystal, and described isotope is selected from 12c or 59co.
Aforesaid composite lithium ion battery cathode material, its average grain diameter D 50be 200 nanometer-600 nanometers, specific area is 7.0-12.0m 2/ g, average pore size 2 nanometer-10 nanometer.
The object of the invention to solve the technical problems also adopts following technical scheme to realize.According to a kind of method preparing composite lithium ion battery cathode material that the present invention proposes, it comprises the following steps: blend step, and it is even powder to be pressed constant weight percentage mix; Graphitization step, is placed in graphitizing furnace by mixture material and carries out graphitization purification process, finally obtained ion secondary battery cathode material lithium, and graphitization processing temperature is within the scope of 2500-3000 DEG C; Shaping process, carries out shaping, classification, screening to the powder after graphitization further, obtains composite lithium ion battery cathode material.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
The aforesaid method preparing composite lithium ion battery cathode material, wherein said powder comprises needle-like coke powder, natural spherical plumbago powder, isotropism coke powder and pitch coke powder, the percentage by weight of described needle-like coke powder is 30%-50%, the percentage by weight of natural spherical plumbago powder is 20%-30%, the percentage by weight of isotropism coke powder is 15%-25%, and the percentage by weight of pitch coke powder is 10%-20%.
The aforesaid method preparing composite lithium ion battery cathode material, it is the isotope of 1%-5% that wherein said powder contains percentage by weight further, described isotope is made up of isotope crystal, isotope alloy crystal or its compound crystal, and described isotope is selected from 12c or 59co.
The aforesaid method preparing composite lithium ion battery cathode material, the average grain diameter D of wherein said composite lithium ion battery cathode material 50be 200 nanometer-600 nanometers, specific area is 7.0-12.0m 2/ g, average pore size 2 nanometer-10 nanometer.
The present invention compared with prior art has obvious advantage and beneficial effect.From above technical scheme, in order to reach aforementioned invention object, main technical content of the present invention is as follows:
The present invention proposes a kind of composite lithium ion battery cathode material, and adopt the form of soft or hard carbon compound, tool has the following advantages: improve the bulk density (being greater than 2.0g/ml) of material and the isotropism (improving the cycle performance of material) of material; Imbibition ability and liquid-keeping property excellence, still can keep more than 92% of initial ion conductivity at 30 days, embody extremely strong imbibition liquid-keeping property; Cycle performance is excellent, and within 1000 weeks, circulation volume keeps more than 95%; Coulombic efficiency more than 93% first, low temperature performance excellent, relative to common negative material, the discharge voltage plateau at-40 DEG C improves 0.17V, and low temperature discharge capacity improves 7.5%; Specific capacity can reach more than 400mAh/g.
In the present invention, the technical advantage of soft or hard carbon compound reduces respective shortcoming: the shortcomings such as such as soft carbon capacity is lower, circulates poor, and hard charcoal coulombic efficiency is low, good combination property.Anion S, P etc. can with S, P-compound such as yellow phosphorus etc., N such as urea etc. can also be mixed join with the form of additive, the capacity of material, absorbent, high rate performance and cycle performance etc. can be improved.
In sum, the composite lithium ion battery cathode material that the present invention is special, it has above-mentioned many advantages and practical value, and publish there are no similar design or use in like product and really belong to innovation, no matter it is at product, preparation method or functionally all have larger improvement, have large improvement technically, and create handy and practical effect, and more existing lithium ion battery negative material has multinomial effect of enhancement, thus be more suitable for practicality, and there is the extensive value of industry, it is really a novelty, progressive, practical new design.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of specification, be described in detail as follows below with preferred embodiment of the present invention.
Embodiment
For further setting forth the present invention for the technological means reaching predetermined goal of the invention and take and effect, below in conjunction with preferred embodiment, its embodiment of composite lithium ion battery cathode material proposed according to the present invention is described in detail as follows.
Embodiment 1-5
The present invention illustrates the composition of composite lithium ion battery cathode material of the present invention, performance and preparation method by example 1-5.
Preparation process comprises:
Blend step, it is even powder to be pressed constant weight percentage mix;
Graphitization step, is placed in graphitizing furnace by mixture material and carries out graphitization purification process, finally obtained ion secondary battery cathode material lithium, and graphitization processing temperature is within the scope of 2500-3000 DEG C;
Shaping process, carries out shaping, classification, screening to the powder after graphitization further, obtains composite lithium ion battery cathode material.
In addition, can further include briquetting technique and impregnating pitch technique in the preferred embodiment of the present invention.Briquetting technique and impregnating pitch technique mainly improve the bulk density of material, and material is better merged, and can improve material compacted density, improve the cycle performance of material.
Table 1 lists composition and the physical property of each preferred embodiment composite lithium ion battery cathode material, and the composition of case of comparative examples and physical property.The performance of the lithium ion battery that table 2 lists case of comparative examples, corresponding embodiment composite lithium ion battery cathode material forms.
Table 1
Table 2
Numbering Specific capacity (mAh/g) Coulombic efficiency first Ionic conductivity Cryogenic property (-15 DEG C)
Reference examples 318 85% 82% 79%
Example 1 380 89% 87% 91%
Example 2 410 91% 91% 90%
Example 3 415 93% 89% 93%
Example 4 438 95% 94% 95%
Can be found out by the Data Comparison of table 1 and table 2, the performance of preferred embodiment of the present invention lithium ion battery negative material will be better than lithium ion battery negative material conventional in prior art far away.
For improving the multiplying power discharging property of negative material, reducing the lithium ion path of deviating from negative material or embedding, pulverizing shaping need be carried out to graphite, Control granularity at D 50for in the scope of 200nm-600 μm, reach the object of shaping.
For improving absorbent and the low temperature energy-absorbing of negative material, and improving the high rate performance of negative material further, need graphitization processing be carried out.
Cathode material for lithium-ion power battery prepared by method of the present invention, specific area adopts health tower specific surface instrument to measure.
Cathode material for lithium-ion power battery prepared by method of the present invention, its electrochemical property test method is: cathode material for lithium-ion power battery: binding agent Kynoar PVDF=98:2, first dissolve with 1-METHYLPYRROLIDONE NMP the solution that PVDF becomes 10%, then add cathode material for lithium-ion power battery and stir into uniform slurry, then be coated on the Copper Foil of 10 μm, tabletted, then the disk of diameter 10mm is made, 120 DEG C of dry for standby, by the negative plate of drying, metal lithium sheet, barrier film, button cell both positive and negative polarity shell, the glove box that argon shield put into by electrolyte carries out assembling button cell, then test, charging/discharging voltage scope: 0.001V-2.0V, electric current is 0.2C, the capacity of test material and efficiency.
Resultant battery preparation and high rate performance, cryogenic property test: cathode material for lithium-ion power battery, binding agent styrene butadiene rubber sbr, suspending agent carboxyl methyl cellulose mass ratio be 98:1:1 mixing, add appropriate deionized water to size mixing as dispersant, evenly be coated on Copper Foil, vacuum drying, is rolled into negative plate for subsequent use.LiCoO 2: PVDF: conductive agent Super-P mass ratio is 94:3:3 mixing, and adding appropriate NMP is that dispersant is sized mixing, and is evenly coated on aluminium foil, vacuum drying, is rolled into positive plate for subsequent use.Positive/negative plate and membrane coil wind, and seal in the glove box sending into argon shield and inject electrolyte, then seal with aluminum plastic film, take out after shelving 24h and carry out Performance Detection.Cycle performance test uses 1C to carry out constant current charge-discharge test, and charging/discharging voltage is limited in 4.2-3.0V.The electric current of rate charge-discharge test 15C carries out, and characterizes high rate performance with the capability retention of 15V/1C.Cryogenic property test adopts-15 DEG C of circulations 30 weeks, and 0.2C charges, and the electric discharge ratio of 0.5C/1C characterizes.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, when the method and technology contents that can utilize above-mentioned announcement are made a little change or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.

Claims (8)

1. a composite lithium ion battery cathode material, it is made primarily of following component:
Needle-like coke powder, percentage by weight is 30%-50%; Natural spherical plumbago powder, percentage by weight is 20%-30%; Isotropism coke powder, percentage by weight is 15%-25%; Pitch coke powder, percentage by weight is 10%-20%.
2. composite lithium ion battery cathode material according to claim 1, it contains percentage by weight is further 1%-5%'s 12c or 59co.
3. composite lithium ion battery cathode material according to claim 1, the calcining heat of wherein said needle-like coke powder is 1400 DEG C-1600 DEG C, bulk density is 0.7-0.8 gram/cc, particle diameter is 10 nanometer-300 nanometers, the particle diameter of described natural spherical plumbago powder is 10 nanometer-800 nanometers, and phosphorus content is 99.93%-99.99%, and the particle diameter of described isotropism coke powder is 100 nanometer-300 nanometers, the particle diameter of described pitch coke powder is 100 nanometer-500 nanometers, and ash content is less than 0.05%.
4. composite lithium ion battery cathode material according to claim 2, wherein said 12c or 59co comprises isotope crystal, isotope alloy crystal or its compound crystal.
5. the composite lithium ion battery cathode material according to claim arbitrary in claim 1-4, its average grain diameter D 50be 200 nanometer-600 nanometers, specific area is 7.0-12.0m 2/ g, average pore size is 2 nanometer-10 nanometers.
6. prepare a method for composite lithium ion battery cathode material, it comprises the following steps:
Blend step, it is even powder to be pressed constant weight percentage mix;
Graphitization step, is placed in graphitizing furnace by mixture material and carries out graphitization purification process, finally obtained ion secondary battery cathode material lithium, and graphitization processing temperature is within the scope of 2500-3000 DEG C;
Shaping process, carries out shaping, classification, screening to the powder after graphitization further, obtains composite lithium ion battery cathode material; Wherein, described powder comprises needle-like coke powder, natural spherical plumbago powder, isotropism coke powder and pitch coke powder, the percentage by weight of described needle-like coke powder is 30%-50%, the percentage by weight of natural spherical plumbago powder is 20%-30%, the percentage by weight of isotropism coke powder is 15%-25%, and the percentage by weight of pitch coke powder is 10%-20%.
7. the method preparing composite lithium ion battery cathode material according to claim 6, it is 1%-5%'s that described powder contains percentage by weight further 12c or 59co, described 12c or 59co is made up of isotope crystal, isotope alloy crystal or its compound crystal.
8. the method preparing composite lithium ion battery cathode material according to claim arbitrary in claim 6-7, the average grain diameter D of wherein said composite lithium ion battery cathode material 50be 200 nanometer-600 nanometers, specific area is 7.0-12.0m 2/ g, average pore size 2 nanometer-10 nanometer.
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CN104821396A (en) * 2015-04-03 2015-08-05 安徽江威精密制造有限公司 Porous active carbon/aluminum oxide composite electrode material and preparation method
CN107845810A (en) * 2017-10-26 2018-03-27 深圳市斯诺实业发展股份有限公司 A kind of soft or hard carbon of lithium ion battery is modified the preparation method of negative material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1481041A (en) * 2002-07-31 2004-03-10 ���µ�����ҵ��ʽ���� Lithium secondary cell
CN102299340A (en) * 2011-08-05 2011-12-28 江西正拓新能源科技有限公司 Conductive graphite additive for lithium ion battery and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1481041A (en) * 2002-07-31 2004-03-10 ���µ�����ҵ��ʽ���� Lithium secondary cell
CN102299340A (en) * 2011-08-05 2011-12-28 江西正拓新能源科技有限公司 Conductive graphite additive for lithium ion battery and preparation method thereof

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