CN106299281A - A kind of negative material of low temperature lithium battery and preparation method thereof - Google Patents
A kind of negative material of low temperature lithium battery and preparation method thereof Download PDFInfo
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- CN106299281A CN106299281A CN201610790734.3A CN201610790734A CN106299281A CN 106299281 A CN106299281 A CN 106299281A CN 201610790734 A CN201610790734 A CN 201610790734A CN 106299281 A CN106299281 A CN 106299281A
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- coke
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
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Abstract
The invention discloses negative material of a kind of low temperature lithium battery and preparation method thereof, it is prepared from by petroleum coke 30 40 parts, needle coke 5 15 parts, carbonaceous mesophase spherules 20 30 parts, agraphitic carbon 5 10 parts, isotropic coke 20 30 parts.In the present invention, amorphous carbon, carbonaceous mesophase spherules, isotropic coke are isotropic materials, and with Delanium is compared, it is very fast, so the conductive effect of material is more preferable for the diffusion velocity of lithium ion；But owing to gram volume is on the low side, so adding again a certain proportion of needle coke and petroleum coke, to meet gram volume requirement.
Description
Technical field
The present invention relates to field of lithium, negative material of a kind of low temperature lithium battery and preparation method thereof.
Background technology
The features such as lithium battery has that nominal voltage is high, specific energy high, has extended cycle life, memory-less effect, and green ring
Protect, pollution-free, therefore it is widely used in the digital products such as mobile phone, notebook computer and MP3, simultaneously at electric automobile, electricity
The dynamic industry such as bicycle, defence equipment is also used widely.In recent years, lithium battery was more and more wider in the application of every field
General, that battery uses circumstance complication, the highest to the performance requirement of battery, such as rate battery, is applied on starting device
Time, it is desirable at-40 DEG C of even lower temperature, also can quickly equipment be started.But the cryogenic property of lithium-ions battery at present
Relatively poor, the particularly service behaviour in the low temperature environment below-30 DEG C is poor.The master of existing lithium cell cathode material
Wanting composition is Delanium, and its conductive effect is poor, and the most at low ambient temperatures, its electric conductivity is worse.
Summary of the invention
The technical problem to be solved in the present invention is to provide the negative material of a kind of low temperature lithium battery, it is ensured that negative material exists
There is under low temperature environment good conductive effect, and there is higher gram volume and cycle performance.
The technical scheme is that
A kind of negative material of low temperature lithium battery, it is prepared from by weight by following component:
Petroleum coke 30-40 part,
Needle coke 5-15 part,
Carbonaceous mesophase spherules 20-30 part,
Agraphitic carbon 5-10 part,
Isotropic coke 20-30 part.
Scheme further, described petroleum coke is the spherical graphite of purity C >=99.5%, and its granularity D50 is 15-20um.
Scheme further, described carbonaceous mesophase spherules is mesophase pitch carbosphere；Described isotropic Jiao is by Colophonium
Delayed coking prepares.
Another goal of the invention of the present invention is to provide the preparation method of the negative material of above-mentioned a kind of low temperature lithium battery, its
Step is as follows:
(1) shaping is pulverized
By proportioning, petroleum coke, needle coke, carbonaceous mesophase spherules, isotropic coke are together joined in pulverizer and carries out
Agitating ball mill, uses wet method stirring ball-milling shaping, obtains mixed-powder；
(2) intercalation is micro-swollen
Mixed-powder and concentrated acid are together added employing ultrasonic agitation 0.5-1h in mixer, then is isolated by centrifuge
Powder body, and be 6-8 to powder body washing to its pH value respectively with pure water and ethanol；Then, after powder body being dried, it is placed in protection
Atmosphere, the temperature of 500-900 DEG C are incubated 1-10h；It is finally cooled to room temperature, obtains microdilatancy graphite；
(3) agglomeration granulation
Microdilatancy graphite is added together with carbon source, solvent stirring 1-4h in homogenizer；Described carbon source accounts for microdilatancy
The mass ratio of graphite is 1～10%；
(4) carbonization sintering
The agglomeration granulation thing being coated with carbon source is placed in protective atmosphere and carries out carbonization sintering processes in 1000-1500 DEG C
10-48h；
(5) graphitization sintering
Powder after step (4) carbonization sintering processes is placed in protective atmosphere, carries out graphitization in 2000-3000 DEG C
Sintering processes 48-72h；
(6) mixing
Powder after step (5) graphitization sintering processes is added together with agraphitic carbon stirring 1-in homogenizer
4h, obtains the negative material of low temperature lithium battery.
Scheme further, is dried in described step (2) and refers at 85-50 DEG C of dry 10-24h；Described concentrated acid be concentrated nitric acid,
At least one in perchloric acid or concentrated sulphuric acid.
Scheme further, in described step (3), carbon source is at least one in asphalt, coal tar pitch, coal tar；Described
Solvent is at least one in toluene, benzene, oxolane.
Scheme further, the stirring frequency of the homogenizer in described step (3), (6) is 50-70HZ.
Advantages of the present invention:
1, the present invention is jointly to be composited by various raw materials, due to amorphous carbon, carbonaceous mesophase spherules, isotropism
Jiao is isotropic material, and with Delanium is compared, it is very fast for the diffusion velocity of lithium ion, so the conductive effect of material
More preferably；But owing to gram volume is on the low side, so adding again a certain proportion of needle coke and petroleum coke, with meet gram volume want
Ask.
2, the present invention uses petroleum coke, needle coke graphitization, carbonaceous mesophase spherules, agraphitic carbon, isotropic Jiao by one
The mixing of fixed ratio just supplements the shortcoming of other kind of material, reaches complementary effect.
3, owing to the little granule of schungite porous carbon matrix in core being agglomerated into second particle, its degree of isotropy
Height, unidirectional breathing that discharge and recharge causes is little, thus substantially increases the embedding lithium of low temperature of low temperature high magnification graphite cathode material
Performance.
Accompanying drawing explanation
Fig. 1 is the graphite cathode material electron-microscope scanning figure obtained by the embodiment of the present invention 3.
Detailed description of the invention
In example below, petroleum coke selects purity C >=99.5%, granularity D50 to be the spherical graphite of 15-20um；Mesophase
Carbosphere is mesophase pitch carbosphere；Described isotropic Jiao is to be prepared by the delayed coking of Colophonium.
Embodiment 1:
A kind of preparation method of the negative material of low temperature lithium battery, its step is as follows:
(1) shaping is pulverized
30 parts of petroleum cokes, 5 parts of needle cokes, 30 parts of carbonaceous mesophase spherules, 30 parts of isotropic coke are together joined pulverizing
Machine is stirred ball mill, uses wet method stirring ball-milling shaping, obtain mixed-powder；
(2) intercalation is micro-swollen
Mixed-powder and concentrated nitric acid are together added employing ultrasonic agitation 0.5h in mixer, then is isolated by centrifuge
Powder body, and be 6 to powder body washing to its pH value respectively with pure water and ethanol；Then powder body is carried out 85 DEG C of dry 10h dried,
It is placed in protective atmosphere, the temperature of 500 DEG C and is incubated 10h；It is finally cooled to room temperature, obtains microdilatancy graphite；
(3) agglomeration granulation
Microdilatancy graphite is added together with asphalt, toluene in homogenizer and stir for 50HZ with stirring frequency
4h；It is 1% that described carbon source accounts for the mass ratio of microdilatancy graphite；
(4) carbonization sintering
The agglomeration granulation thing being coated with carbon source is placed in protective atmosphere and carries out carbonization sintering processes 48h in 1000 DEG C；
(5) graphitization sintering
Powder after step (4) carbonization sintering processes is placed in protective atmosphere, carries out graphitization sintering in 2000 DEG C
Process 72h；
(6) mixing
Powder after step (5) graphitization sintering processes is added together with 5 parts of agraphitic carbons in homogenizer with
Stirring frequency is that 50HZ stirs 4h, obtains the negative material of low temperature lithium battery.
Embodiment 2:
A kind of preparation method of the negative material of low temperature lithium battery, its step is as follows:
(1) shaping is pulverized
40 parts of petroleum cokes, 15 parts of needle cokes, 20 parts of carbonaceous mesophase spherules, 20 parts of isotropic coke are together joined pulverizing
Machine is stirred ball mill, uses wet method stirring ball-milling shaping, obtain mixed-powder；
(2) intercalation is micro-swollen
Mixed-powder and perchloric acid are together added employing ultrasonic agitation 1h in mixer, then by centrifuge separation powder delivery
Body, and be 8 to powder body washing to its pH value respectively with pure water and ethanol；Then powder body is carried out 50 DEG C of dry 24h dried, put
1h it is incubated in protective atmosphere, the temperature of 900 DEG C；It is finally cooled to room temperature, obtains microdilatancy graphite；
(3) agglomeration granulation
Microdilatancy graphite is added together with coal tar, oxolane in homogenizer and stir for 70HZ with stirring frequency
1h；It is 10% that described carbon source accounts for the mass ratio of microdilatancy graphite；
(4) carbonization sintering
The agglomeration granulation thing being coated with carbon source is placed in protective atmosphere and carries out carbonization sintering processes 10h in 1500 DEG C；
(5) graphitization sintering
Powder after step (4) carbonization sintering processes is placed in protective atmosphere, carries out graphitization sintering in 3000 DEG C
Process 48h；
(6) mixing
Powder after step (5) graphitization sintering processes is added together with 5 parts of agraphitic carbons in homogenizer with
Stirring frequency is that 70HZ stirs 1h, obtains the negative material of low temperature lithium battery.
Embodiment 3:
A kind of preparation method of the negative material of low temperature lithium battery, its step is as follows:
(1) shaping is pulverized
35 parts of petroleum cokes, 10 parts of needle cokes, 25 parts of carbonaceous mesophase spherules, 25 parts of isotropic coke are together joined pulverizing
Machine is stirred ball mill, uses wet method stirring ball-milling shaping, obtain mixed-powder；
(2) intercalation is micro-swollen
Mixed-powder and concentrated sulphuric acid are together added employing ultrasonic agitation 0.5h in mixer, then is isolated by centrifuge
Powder body, and be 7 to powder body washing to its pH value respectively with pure water and ethanol；Then powder body is carried out 75 DEG C of dry 20h dried,
It is placed in protective atmosphere, the temperature of 700 DEG C and is incubated 5h；It is finally cooled to room temperature, obtains microdilatancy graphite；
(3) agglomeration granulation
Microdilatancy graphite is added in homogenizer together with coal tar pitch, benzene and stirs 3h with stirring frequency for 60HZ；Institute
Stating carbon source and accounting for the mass ratio of microdilatancy graphite is 5%；
(4) carbonization sintering
The agglomeration granulation thing being coated with carbon source is placed in protective atmosphere and carries out carbonization sintering processes 30h in 1200 DEG C；
(5) graphitization sintering
Powder after step (4) carbonization sintering processes is placed in protective atmosphere, carries out graphitization sintering in 2500 DEG C
Process 60h；
(6) mixing
Powder after step (5) graphitization sintering processes is added together with 8 parts of agraphitic carbons in homogenizer with
Stirring frequency is that 60HZ stirs 3h, obtains the negative material of low temperature lithium battery.
It is illustrated in figure 1 the graphite cathode material electron-microscope scanning figure that the present embodiment prepares, from figure 1 it appears that negative pole
The composite that material is mixed to form by petroleum coke, needle coke graphitization, carbonaceous mesophase spherules, agraphitic carbon, isotropic Jiao.
Comparative example:
The preparation method using embodiment 3 prepares comparative example, 95 parts of Delaniums of raw material selection and 5 parts of nothings in comparative example
Sizing carbon.
Negative material prepared by above-described embodiment 3 and comparative example and positive pole, barrier film, electrolyte make battery capacity,
Charge-discharge performance, wherein cell capacity testing standard: at temperature 25 ± 2 °, relative humidity 15%～90% environment, electricity
Pond discharges into 2.5v with 1I, stands 1h；With 1I constant-current charge to 3.65v, transfer constant voltage 3.65v to, reach 0.05I to cut-off current
Time stop charging, after charging stand 1h；Discharge with 1I, discharge into 2.5v and stop.Concrete data such as following table:
Can be seen that from upper table 1, the negative material that the present invention prepares be applied in electrokinetic cell to have higher gram volume and
Cryogenic property.
It should be pointed out that, the professional and technical personnel for making the art, in the premise without departing from the technology of the present invention principle
Under, it is that by the multiple amendment to these embodiments, and these amendments also should be regarded as the scope that the present invention should protect
In.
Claims (7)
1. the negative material of a low temperature lithium battery, it is characterised in that: it is prepared from by weight by following component:
Petroleum coke 30-40 part,
Needle coke 5-15 part,
Carbonaceous mesophase spherules 20-30 part,
Agraphitic carbon 5-10 part,
Isotropic coke 20-30 part.
The negative material of a kind of low temperature lithium battery the most according to claim 1, it is characterised in that: described petroleum coke is purity
The spherical graphite of C >=99.5%, its granularity D50 is 15-20um.
The negative material of a kind of low temperature lithium battery the most according to claim 1, it is characterised in that: described carbonaceous mesophase spherules
For mesophase pitch carbosphere；Described isotropic Jiao is to be prepared by the delayed coking of Colophonium.
4. the preparation method of the negative material of an a kind of low temperature lithium battery as claimed in claim 1, it is characterised in that: step
As follows:
(1) shaping is pulverized
By proportioning, petroleum coke, needle coke, carbonaceous mesophase spherules, isotropic coke are together joined in pulverizer and is stirred
Ball mill, uses wet method stirring ball-milling shaping, obtains mixed-powder；
(2) intercalation is micro-swollen
Mixed-powder and concentrated acid are together added employing ultrasonic agitation 0.5-1h in mixer, then by centrifuge separation powder delivery
Body, and be 6-8 to powder body washing to its pH value respectively with pure water and ethanol；Then, after powder body being dried, it is placed in protection gas
Atmosphere, the temperature of 500-900 DEG C are incubated 1-10h；It is finally cooled to room temperature, obtains microdilatancy graphite；
(3) agglomeration granulation
Microdilatancy graphite is added together with carbon source, solvent stirring 1-4h in homogenizer；Described carbon source accounts for microdilatancy graphite
Mass ratio be 1～10%；
(4) carbonization sintering
The agglomeration granulation thing being coated with carbon source is placed in protective atmosphere and carries out carbonization sintering processes 10-in 1000-1500 DEG C
48h；
(5) graphitization sintering
Powder after step (4) carbonization sintering processes is placed in protective atmosphere, carries out graphitization burning in 2000-3000 DEG C
Knot processes 48-72h；
(6) mixing
Powder after step (5) graphitization sintering processes is added together with agraphitic carbon stirring 1-4h in homogenizer,
Obtain the negative material of low temperature lithium battery.
Preparation method the most according to claim 4, it is characterised in that: described step (2) is dried and refers to do at 85-50 DEG C
Dry 10-24h；Described concentrated acid is at least one in concentrated nitric acid, perchloric acid or concentrated sulphuric acid.
Preparation method the most according to claim 4, it is characterised in that: in described step (3), carbon source is asphalt, coal drip
At least one in green grass or young crops, coal tar；Described solvent is at least one in toluene, benzene, oxolane.
Preparation method the most according to claim 4, it is characterised in that: the homogenizer in described step (3), (6)
Stirring frequency is 50-70HZ.
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| CN201610790734.3A CN106299281B (en) | 2016-08-30 | 2016-08-30 | A kind of negative electrode material and preparation method thereof of low temperature lithium battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112670459A (en) * | 2019-12-09 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Graphite negative electrode material and preparation and application thereof |
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| CN104779413A (en) * | 2015-04-09 | 2015-07-15 | 深圳市美拜电子有限公司 | Lithium ion battery |
| CN105375030A (en) * | 2015-10-30 | 2016-03-02 | 福建翔丰华新能源材料有限公司 | Preparation method of low-temperature and high-rate graphite anode material for power battery |
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2016
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Patent Citations (5)
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| CN101017890A (en) * | 2005-02-09 | 2007-08-15 | 索尼株式会社 | Anode and battery using same |
| CN101529624A (en) * | 2006-11-10 | 2009-09-09 | 东海碳素株式会社 | Negative electrode material for lithium ion secondary battery and method for producing the same |
| CN102956889A (en) * | 2012-11-05 | 2013-03-06 | 江西正拓新能源科技有限公司 | Lithium ion battery composite negative electrode material and preparation method thereof |
| CN104779413A (en) * | 2015-04-09 | 2015-07-15 | 深圳市美拜电子有限公司 | Lithium ion battery |
| CN105375030A (en) * | 2015-10-30 | 2016-03-02 | 福建翔丰华新能源材料有限公司 | Preparation method of low-temperature and high-rate graphite anode material for power battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112670459A (en) * | 2019-12-09 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Graphite negative electrode material and preparation and application thereof |
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