CN104779396A - Production method of lithium ion composite graphite cathode material - Google Patents
Production method of lithium ion composite graphite cathode material Download PDFInfo
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- CN104779396A CN104779396A CN201510193491.0A CN201510193491A CN104779396A CN 104779396 A CN104779396 A CN 104779396A CN 201510193491 A CN201510193491 A CN 201510193491A CN 104779396 A CN104779396 A CN 104779396A
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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
- H01M4/5835—Comprising fluorine or fluoride salts
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- 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 provides a production method of a lithium ion composite graphite cathode material. The production method comprises the following steps: by taking one or the mixture of two of calcined coke and natural graphite as the raw material A, delay coke as the raw material B and pitch micro-powder as the raw material C, modifying the micro-powder B and then grading, and controlling the minimum grain size after grading to be above 2 microns; proportionally mixing the micro-powder B with the micro-powder A, and mixing the mixture with the raw material C proportionally by use of airflow; finally, carbonizing at a temperature ranging from 1200 to 1500 DEG C or graphitizing at a temperature ranging from 2800 to 3200 DEG C, or graphitizing at the temperature ranging from 2800 to 3200 DEG C after carbonizing at the temperature ranging from 1200 to 1500 DEG C. The production method has the advantages that the problem of poor cyclic performance of a large-grain diameter material is solved, and meanwhile, relatively high capacity and efficiency are maintained; the granularity of the material produced by use of the production method is in abnormal distribution, and the material has unique processing adaptability and good safety performance, and can be applied to lithium ion batteries in different fields.
Description
Technical field
The present invention relates to a kind of lithium ion composite graphite negative electrode material production method, belong to technical field of lithium ion battery negative.
Background technology
Along with low-carbon (LC), green, recycling economy in the urgent need to, the research of new forms of energy battery obtains and develops rapidly, development as the lithium ion battery of energy-conserving and environment-protective receives much concern especially, and cell negative electrode material is the key factor of battery energy storage, the performance of negative material decides the development level of lithium ion battery.Carbonaceous material is that people's early start is studied and is applied to the material of lithium ion battery negative, so far market still can occupy the leading position of carbonaceous material as lithium ion battery negative material without other material.
Carbonaceous negative material mainly has the advantages such as specific capacity is high, electrode potential is low, cycle efficieny is high, have extended cycle life, but because raw material sources are different, the application performance of the negative material that various different carbon raw material is produced respectively has its pluses and minuses, so the exploitation of carbonaceous material is still the focus of current research.And, along with the development of science and technology and the demand in market, the demand of lithium ion battery will constantly increase from now on, not only be widely used in the compact battery fields such as mobile phone, notebook, digital product and electric tool, also will be widely used in electric automobile, the electrically field such as hybrid vehicle, aviation.Present invention employs the raw material of unlike material, and for the different qualities of material, different processing modes is used to design such as its granularity, structure etc., plays material advantage separately, to reach integrated application effect.
Summary of the invention
The object of this invention is to provide a kind of lithium ion composite graphite negative electrode material production method, to solve the problem of large grain through the cycle performance difference of material, keep higher capacity and efficiency simultaneously, improve the natural flaws such as the poorly conductive of Large stone capacity type material, cycle life is short simultaneously.
Technical scheme of the present invention: a kind of lithium ion composite graphite negative electrode material production method, concrete production technology is:
A () is to forge one or both mixtures in rear Jiao and native graphite for raw material A;
B () take delay coke as raw material B;
C () take particle diameter as the pitch micro mist of≤3 μm is raw material C;
D the raw material A of (a) step is pulverized by (), be classified into the micro mist A that median is 18 ~ 21 μm;
E the raw material B of (b) step pulverizes by (), be classified into the micro mist B that median is 8 ~ 10 μm;
F micro mist B that (e) step obtains by () first carries out modification, then classification at 300 ~ 600 DEG C, and the minimum grain size after classification controls more than 2 μm, and the micro mist A and then obtained with (d) step is in A/B=100/(30 ~ 100) ratio mix;
The raw material C of g mixed material that (f) step obtains by () and (c) step is in (A+B)/C=100/(2 ~ 8) ratio carry out air-flow and mix, then select to carbonize at 1200 ~ 1500 DEG C, or at 2800 ~ 3200 DEG C, carry out graphitization, or at 2800 ~ 3200 DEG C, carry out graphitization after first carbonizing at 1200 ~ 1500 DEG C;
H (), after the material that (g) step obtains is cooled to room temperature, carries out breaing up, sieving.
Described raw material C is coal tar pitch or petroleum asphalt.
G air-flow described in () step is mixed into and uses airflow mixer to mix.
F mixing described in () step adopts double-cone mixer mixing.
The median of described native graphite is 12 μm-18 μm.
Beneficial effect of the present invention:
Does 1, the present invention (represent calcined coke and delay coke in this application to petroleum coke powder? petroleum coke is burnt and delay coke after comprising forging) carry out the mixed processing of two kinds of size specification, utilize Non-Gaussian Distribution particle size distribution characteristics, play the conduction of its small particle diameter and circulation advantage to make up the defect of Large stone, ensure the energy storage advantage of Large stone material simultaneously;
2, adopt the mixture of two kinds of burnt classes as primary raw material, the electrochemical effects that they are different can be played, ensure better flexibility (adaptability) of operation;
3, delay coke through modified with forging after burnt compound, and covered composite yarn before the heat treatment, can strengthen composite effect, can not produce the rejections such as uneven, difficult dispersion;
4, in sum, the present invention is by utilizing the different qualities of granularity Non-Gaussian Distribution, two kinds of burnt class raw materials of material and carry out compound between modification and graphitization, the composite characteristic of material can be played greatly, and its production technology is simple, production efficiency is high, cost is low, and course of processing safety, can be used for suitability for industrialized production.
embodiment:
embodiment 1:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist A that median is 18 μm.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 4kg, add above-mentioned modified micro mist B 2kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of above-mentioned micro mist A and micro mist B, add raw material C 100g, carry out air-flow mixing, then carry out graphitization at 3000 DEG C.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 350.6mAh/g, and discharging efficiency is 94.6%, as shown in table 1.
embodiment 2:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist A that median is 19 μm.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 8 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 3kg, add above-mentioned modified micro mist B 3kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of above-mentioned micro mist A and micro mist B, add raw material C 150g, carry out air-flow mixing, then carry out graphitization at 2800 DEG C.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 353.8mAh/g, and discharging efficiency is 94.8%, as shown in table 1.
embodiment 3:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist that median is 20 μm.Take burnt micro mist 5kg after forging, adding median is that the native graphite 2kg of 12 μm mixes, and obtains admixed finepowder A.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take admixed finepowder A 4kg, add above-mentioned modified micro mist B 3kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of admixed finepowder A and micro mist B, add raw material C 150g, carry out air-flow mixing, then carry out graphitization at 3200 DEG C.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 360.2mAh/g, and discharging efficiency is 94.4%, as shown in table 1.
embodiment 4:
Take burnt raw material 50kg after forging, carry out crushing and classification and become median to be the micro mist of 18 μm.Take burnt micro mist 5kg after forging, adding median is that the native graphite 5kg of 18 μm mixes, and obtains admixed finepowder A.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 5kg, add above-mentioned modified micro mist B 1.5kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of admixed finepowder A and micro mist B, add raw material C 150g, carry out air-flow mixing, then carry out graphitization at 3000 DEG C.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 362.6mAh/g, and discharging efficiency is 94.6%, as shown in table 1.
embodiment 5:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist A that median is 21 μm.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 4kg, add above-mentioned modified micro mist B 3kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of micro mist A and micro mist B, add raw material C 200g, carry out air-flow mixing, first carbonize at 1300 DEG C after mixing, then at 2800 DEG C, carry out graphitization.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 351.6mAh/g, and discharging efficiency is 94.9%, as shown in table 1.
embodiment 6:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist A that median is 18 μm.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 4kg, add above-mentioned modified micro mist B 2.8kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of micro mist A and micro mist B, add raw material C 100g, carry out air-flow mixing, then carry out graphitization at 3000 DEG C.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 345.8mAh/g, and discharging efficiency is 95.0%, as shown in table 1.
embodiment 7:
Take the rear burnt raw material 50kg of forging, carry out pulverizing and be classified into the micro mist that median is 18 μm.Take burnt micro mist 5kg after forging, adding median is that the native graphite 3kg of 18 μm mixes, and obtains admixed finepowder A.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take admixed finepowder A 4kg, add above-mentioned modified micro mist B 1.2kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 4kg of admixed finepowder A and micro mist B, add raw material C 120g, carry out air-flow mixing, first carbonize at 1300 DEG C after mixing, then at 3000 DEG C, carry out graphitization.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 351.2mAh/g, and discharging efficiency is 94.2%, as shown in table 1.
embodiment 8:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist A that median is 18 μm.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 5kg, add above-mentioned modified micro mist B 1.5kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of micro mist A and micro mist B, add raw material C 300g, carry out air-flow mixing, first carbonize at 1300 DEG C after mixing, then at 3200 DEG C, carry out graphitization.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 349.6mAh/g, and discharging efficiency is 94.8%, as shown in table 1.
embodiment 9:
Take the rear burnt raw material A 50kg of forging, carry out pulverizing and be classified into the micro mist A that median is 18 μm.
Take delay coke raw material B 50kg, carry out pulverizing and be classified into the micro mist B that median is 10 μm.
Take micro mist B 5kg, carry out modification, then classification at 300 ~ 600 DEG C, the minimum grain size after classification controls more than 2 μm.
Take micro mist A 4kg, add above-mentioned modified micro mist B 2kg, under normal temperature state, carry out mixing 30min.
Take the mixed material 5kg of micro mist A and micro mist B, add raw material C 200g, carry out air-flow mixing, carbonize at 1400 DEG C after mixing.
After material cooling after graphitization, carry out breaing up, sieving process, obtain final products.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 345.4mAh/g, and discharging efficiency is 94.6%, as shown in table 1.
subordinate list 1
button cell test data summary sheet
Claims (5)
1. a lithium ion composite graphite negative electrode material production method, is characterized in that concrete production technology is:
To forge one or both mixtures in rear Jiao and native graphite for raw material A;
Take delay coke as raw material B;
C () take particle diameter as the pitch micro mist of≤3 μm is raw material C;
D the raw material A of (a) step is pulverized by (), be classified into the micro mist A that median is 18 ~ 21 μm;
E the raw material B of (b) step pulverizes by (), be classified into the micro mist B that median is 8 ~ 10 μm;
F micro mist B that (e) step obtains by () first carries out modification, then classification at 300 ~ 600 DEG C, and the minimum grain size after classification controls more than 2 μm, and the micro mist A and then obtained with (d) step is in A/B=100/(30 ~ 100) ratio mix;
The raw material C of g mixed material that (f) step obtains by () and (c) step is in (A+B)/C=100/(2 ~ 8) ratio carry out air-flow and mix, then select to carbonize at 1200 ~ 1500 DEG C, or at 2800 ~ 3200 DEG C, carry out graphitization, or at 2800 ~ 3200 DEG C, carry out graphitization after first carbonizing at 1200 ~ 1500 DEG C;
H (), after the material that (g) step obtains is cooled to room temperature, carries out breaing up, sieving.
2. a kind of lithium ion composite graphite negative electrode material production method as claimed in claim 1, is characterized in that: described raw material C is coal tar pitch or petroleum asphalt.
3. a kind of lithium ion composite graphite negative electrode material production method as claimed in claim 1, is characterized in that: air-flow described in (g) step is mixed into and uses airflow mixer to mix.
4. a kind of lithium ion composite graphite negative electrode material production method as claimed in claim 1, is characterized in that: mixing described in (f) step adopts double-cone mixer mixing.
5. a kind of lithium ion composite graphite negative electrode material production method as claimed in claim 1, is characterized in that: the median of described native graphite is 12 μm ~ 18 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105118960A (en) * | 2015-07-17 | 2015-12-02 | 大连宏光锂业股份有限公司 | Production method of high-capacity lithium ion battery composite graphite negative electrode material |
| CN105428615A (en) * | 2015-11-09 | 2016-03-23 | 大连宏光锂业股份有限公司 | Production method for modified artificial graphite negative electrode material |
| CN112978725A (en) * | 2021-02-07 | 2021-06-18 | 大连宏光锂业股份有限公司 | Modified artificial graphite cathode material of power lithium ion battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105118960A (en) * | 2015-07-17 | 2015-12-02 | 大连宏光锂业股份有限公司 | Production method of high-capacity lithium ion battery composite graphite negative electrode material |
| CN105428615A (en) * | 2015-11-09 | 2016-03-23 | 大连宏光锂业股份有限公司 | Production method for modified artificial graphite negative electrode material |
| CN105428615B (en) * | 2015-11-09 | 2017-08-08 | 大连宏光锂业股份有限公司 | A kind of modified artificial graphite cathode material production method |
| CN112978725A (en) * | 2021-02-07 | 2021-06-18 | 大连宏光锂业股份有限公司 | Modified artificial graphite cathode material of power lithium ion battery and preparation method thereof |
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