CN109256530A - A kind of high performance lithium ion battery carbon cathode material and preparation method thereof - Google Patents
A kind of high performance lithium ion battery carbon cathode material and preparation method thereof Download PDFInfo
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- CN109256530A CN109256530A CN201710574142.2A CN201710574142A CN109256530A CN 109256530 A CN109256530 A CN 109256530A CN 201710574142 A CN201710574142 A CN 201710574142A CN 109256530 A CN109256530 A CN 109256530A
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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
- H01M4/366—Composites as layered products
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
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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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- 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 present invention relates to technical field of lithium ion, specifically a kind of high performance lithium ion battery carbon cathode material and preparation method thereof, it is characterized by comprising layer of charcoal and the inorganic, ceramic layers being coated on outside layer of charcoal, or the mixed layer mixed including charcoal and inorganic ceramic.The present invention is compared with the existing technology, charcoal/inorganic, ceramic layer in material can reach double effects simultaneously, wherein layer of charcoal can increase the diffusion admittance of lithium ion during charge and discharge, lithium ion is quickly to spreading inside particle when big multiplying power charging, the enrichment in particle surface lithium ion is avoided, while reaching fast charge effect；And inorganic, ceramic layer can be with HF, H in electrolyte2The harmful constituents such as O are reacted in time, are increased the stability of electrolyte and negative terminal surface, while can be effectively heat-insulated, are improved heat resistance, achieve the effect that security performance improves；Preparation process is carried out in aqueous solvent, and raw material sources are extensive, simple process, economic and environment-friendly.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically a kind of high performance lithium ion battery carbon cathode material
And preparation method thereof.
Background technique
Since lithium ion battery is commercialized since 1991, because of its high-energy density, long circulation life, high working voltage, good
The advantages that good multiplying power charge and discharge performance and be widely used in consumer electronics field, meanwhile, also become electric car etc. in recent years
The preferred battery system in field.
With the sustainable development in electric car field, market application problem is also increasingly prominent, especially safety problem by
Market concern.The safety issue of lithium ion battery is mostly derived from two aspects: first is that when the embedding lithium of lithium ion battery negative material
Voltage platform is at 0.01~0.2V (Vs Li+/Li), if Li+ is enriched on the surface of the material, Li dendrite easy to form pierces through diaphragm,
Cause internal short-circuit of battery that thermal runaway occurs, internal temperature of battery increases, and the vigorous reaction of negative electrode material and electrolyte is caused to reach
To embedding lithium state cathode burning point and it is on fire or explosion；Second is that lithium ion anode material under high voltages with electrolyte vigorous reaction,
And then heat and oxygen are discharged, cause more exothermic reactions and on fire or explosion.
For the security performance for solving lithium ion battery, the work of researcher is related to each component part of lithium ion battery,
But to the work and few that negative electrode material security performance itself improves.Patent CN106486651A uses silicon powder and graphite mixture
Mechanical ball mill, after in organic system solvent and pitch-coating heat treatment, dry, cooling obtained cathode pole piece, in the cathode pole piece
Upper coating lithium metaaluminate slurry drying forms pole coating.This method puts forth effort on the conduction of velocity for improving lithium battery, inhibits lithium branch
Brilliant generation, but integrated artistic is complex, higher cost, and it is limited that the safety is improved.
Summary of the invention
Being able to achieve fast charge again the purpose of the present invention is overcoming the deficiencies of the prior art and provide one kind can improve to the maximum extent
The negative electrode material and simple process of lithium ion battery safety performance.
To achieve the above object, a kind of high performance lithium ion battery carbon cathode material is designed, it is characterised in that: including layer of charcoal
And it is coated on the inorganic, ceramic layer outside layer of charcoal, or the mixed layer mixed including charcoal and inorganic ceramic.
The inorganic ceramic is one of Al, Si or Mg element or more than one oxide ceramics.
The charcoal be one of hard charcoal or soft charcoal or more than one.
A kind of preparation method of high performance lithium ion battery carbon cathode material, which comprises the steps of:
A, surfactant, the weight ratio of the surfactant and aqueous solvent are added in water are as follows: 1~20: 100,
It is sufficiently stirred and dissolves to obtain surfactant solution；
B, graphite powder is put into surfactant solution or coke micro mist, surfactant solution and graphite or coke are micro-
The weight ratio of powder is 500~2000: 100, and 0.5~5h of ultrasonic disperse obtains suspension；
C, while mechanical stirring, inorganic salt solution is added into suspension；
D, it is spray-dried, obtains dry powder；
E, by dry powder with 300 DEG C~1300 DEG C 5~15h of vacuum heat treatment, cooling discharge is up to the high-performance
Carbon negative electrode material of lithium ion cell；
The hydrophilic radical of the surfactant be one of carboxylate, sulfonate or sulfate or more than one,
Hydrophobic group is the hydrocarbon chain containing one or more phenyl ring of 20 or more carbon atom number；
The inorganic salt solution is that chloride, the ammonium salt solution containing Al, the chloride of Mg, the ammonium salt containing Mg of Al is molten
One of liquid, aluminate solution or silicate solutions or more than one.
The aluminate is sodium aluminate, potassium aluminate, lithium aluminate；The silicate is sodium metasilicate, potassium silicate.
The inorganic salt solution uses concentration for the inorganic salt solution of 1~20wt%；The inorganic salt solution and outstanding
The weight ratio of supernatant liquid are as follows: 1~50: 100.
The graphite microparticles be one of artificial graphite, natural graphite, mesocarbon microspheres or more than one.
The coke micro mist be the petroleum coke of charing, coal tar pitch be burnt, one of interphase microballoon or more than one.
The temperature of the spray drying is 200 DEG C~400 DEG C.
Vacuum degree >=0.01MPa of the vacuum heat treatment.
Compared with the existing technology, charcoal/inorganic, ceramic layer in material can reach double effects to the present invention simultaneously, wherein charcoal
Layer can increase the diffusion admittance of lithium ion during charge and discharge, and lithium ion is kept away quickly to spreading inside particle when big multiplying power charges
Exempt from the enrichment in particle surface lithium ion, while reaching fast charge effect；And inorganic, ceramic layer can be with HF, H in electrolyte2O
Etc. harmful constituents react in time, increase electrolyte and negative terminal surface stability, while can effectively it is heat-insulated, improve heat resistance,
Achieve the effect that security performance improves；Preparation process is carried out in aqueous solvent, and raw material sources are extensive, simple process,
It is economic and environment-friendly.
Specific embodiment
The present invention is further described now in conjunction with embodiment.Obviously, embodiments described below is only the present invention
In a part, embodiment is not all of embodiment.Based on the embodiments of the present invention, those skilled in the art is not doing
Other all embodiments under the premise of creative achievement out, belong to protection scope of the present invention.
Embodiment 1
10g cetyl benzene carboxylic acid sodium is added in 100g water under stirring, partial size D50 is added after completely dissolution
The AlCl that concentration is 5wt% is added while mechanical stirring in artificial graphite micro mist 10g, the ultrasonic disperse 30min of 10.0um3
Then the suspension is spray-dried by solution 10g at 200 DEG C, dried powder is in the lower 1000 DEG C of heat treatment of 0.01Mpa vacuum degree
High performance lithium ion battery carbon cathode material is made in 10h, cooling discharge.
Embodiment 2
20g cetyl benzenesulfonic acid sodium is added in 100g water under stirring, partial size D50 is added after completely dissolution
The AlCl of concentration 20wt% is added while mechanical stirring in artificial graphite micro mist 10g, the ultrasonic disperse 30min of 10.0um3
Then the suspension is spray-dried by solution 10g at 200 DEG C, dried powder is in the lower 1300 DEG C of heat treatment of 0.01Mpa vacuum degree
High performance lithium ion battery carbon cathode material is made in 5h, cooling discharge.
Embodiment 3
5g cetyl phenyl-hydrogen-sulfate sodium is added in 100g water under stirring, partial size D50 is added after completely dissolution
The AlCl of concentration 10wt% is added while mechanical stirring in artificial graphite micro mist 20g, the ultrasonic disperse 4h of 10.0um3Solution
Then the suspension is spray-dried by 10g at 400 DEG C, dried powder in the lower 600 DEG C of heat treatment 15h of 0.01Mpa vacuum degree,
High performance lithium ion battery carbon cathode material is made in cooling discharge.
Embodiment 4
5g cetyl benzenesulfonic acid sodium is added in 100g water under stirring, partial size D50 is added after completely dissolution
Concentration 10wt%MgCl is added while mechanical stirring in artificial graphite micro mist 10g, the ultrasonic disperse 2h of 10.0um2Solution
Then the suspension is spray-dried by 30g at 400 DEG C, dried powder in the lower 1000 DEG C of heat treatment 5h of 0.01Mpa vacuum degree,
High performance lithium ion battery carbon cathode material is made in cooling discharge.
Embodiment 5
10g eicosyl benzene carboxylic acid sodium is added in 100g water under stirring, partial size D50 is added after completely dissolution
Concentration 5wt% sodium aluminate solution is added while mechanical stirring in natural graphite micro mist 10g, the ultrasonic disperse 1h of 10.0um
Then the suspension is spray-dried by 30g at 200 DEG C, dried powder in the lower 1000 DEG C of heat treatment 5h of 0.01Mpa vacuum degree,
High performance lithium ion battery carbon cathode material is made in cooling discharge.
Embodiment 6
10g eicosyl benzene carboxylic acid sodium is added in 100g water under stirring, partial size D50 is added after completely dissolution
Charing petroleum coke micro mist 15g, the ultrasonic disperse 1h of 10.0um, while mechanical stirring, the sodium metasilicate that concentration 5wt% is added is molten
Then the suspension is spray-dried by liquid 50g at 200 DEG C, dried powder is in the lower 1300 DEG C of heat treatment of 0.01Mpa vacuum degree
High performance lithium ion battery carbon cathode material is made in 5h, cooling discharge.
Effect example
(1) to artificial stone used in high performance lithium ion battery carbon cathode material made from Examples 1 to 2 and embodiment
Black micro mist carries out indicator powder test, and index is listed in table 1.
Table 1
(2) the high performance lithium ion battery carbon cathode material of the embodiment of the present invention is filled using full battery test method
Electric high rate performance test and security performance test.Full battery test method are as follows: with the high-performance lithium ion electricity of the embodiment of the present invention
Pond carbon cathode material is cathode, is anode, 1MLiPF6+EC: DMC: EMC=1: 1: 1 (volume with 4.35V lithium cobaltate cathode material
Than) solution be electrolyte.Lithium ion battery, battery design capacity are made according to Soft Roll coiled lithium ion battery basic technology
800mAh.Artificial graphite micro mist used in the contrast test embodiment of the present invention.Wherein, rate of charge performance test are as follows: room temperature
Under, 0.2C/0.5C/1C/2.0C/3.0C constant-current charge to 4.35V, 4.35V constant-voltage charge to cut-off current 0.02C is stood
15min, 0.5C are discharged to 3.2V, and using the discharge capacity of 0.2C/0.5C charge and discharge system as benchmark, test result is shown in Table
2.Security performance test are as follows: heavy impact, thermal shock, short-circuit test, test condition is with reference to national lithium ion battery standard GB/T
18287-2000.Test result is shown in Table 3.
Table 2
| Embodiment | 0.2C(mAh) | 0.5C (%) | 1.0C (%) | 2.0C (%) | 3.0C (%) |
| 1 | 810.2 | 99.8 | 99.1 | 90.5 | 76.3 |
| 2 | 812.3 | 99.8 | 99.3 | 91.2 | 80.9 |
| 3 | 815.3 | 99.8 | 99.1 | 90.6 | 78.2 |
| 4 | 810.2 | 99.8 | 99.2 | 92.1 | 80.5 |
| 5 | 809.3 | 99.8 | 99.1 | 90.8 | 79.2 |
| 6 | 800.5 | 99.9 | 99.5 | 95.6 | 85.5 |
| Artificial graphite micro mist | 810.5 | 99.6 | 98.2 | 85.7 | 64.7 |
| Natural graphite micro mist | 808.2 | 99.2 | 97.4 | 84.3 | 63.3 |
| Carbonize petroleum coke micro mist | 801.6 | 99.9 | 98.7 | 91.2 | 73.2 |
Table 3
Claims (10)
1. a kind of high performance lithium ion battery carbon cathode material, it is characterised in that: including layer of charcoal and be coated on inorganic outside layer of charcoal
Ceramic layer, or the mixed layer mixed including charcoal and inorganic ceramic.
2. a kind of high performance lithium ion battery carbon cathode material as described in claim 1, it is characterised in that: the inorganic pottery
Porcelain is one of Al, Si or Mg element or more than one oxide ceramics.
3. a kind of high performance lithium ion battery carbon cathode material as described in claim 1, it is characterised in that: the charcoal is hard
One of charcoal or soft charcoal or more than one.
4. a kind of preparation method of high performance lithium ion battery carbon cathode material as claimed in any one of claims 1 to 3, special
Sign is, includes the following steps:
A, surfactant, the weight ratio of the surfactant and aqueous solvent are added in water are as follows: 1~20: 100, sufficiently
Stirring and dissolving obtains surfactant solution；
B, graphite powder or coke micro mist are put into surfactant solution, surfactant solution and graphite or coke micro mist
Weight ratio is 500~2000: 100, and 0.5~5h of ultrasonic disperse obtains suspension；
C, while mechanical stirring, inorganic salt solution is added into suspension；
D, it is spray-dried, obtains dry powder；
E, by dry powder with 300 DEG C~1300 DEG C 5~15h of vacuum heat treatment, cooling discharge up to the high-performance lithium from
Sub- battery carbon cathode material；
The hydrophilic radical of the surfactant be one of carboxylate, sulfonate or sulfate or more than one, hydrophobic
Group is the hydrocarbon chain containing one or more phenyl ring of 20 or more carbon atom number；
The inorganic salt solution is chloride, the ammonium salt solution containing Al, the chloride of Mg, the ammonium salt solution containing Mg, aluminium of Al
One of acid salt solution or silicate solutions or more than one.
5. method as claimed in claim 4, it is characterised in that: the aluminate is sodium aluminate, potassium aluminate, lithium aluminate；It is described
Silicate is sodium metasilicate, potassium silicate.
6. method as claimed in claim 4, it is characterised in that: the inorganic salt solution uses concentration for the nothing of 1~20wt%
Machine salting liquid；The weight ratio of the inorganic salt solution and suspension are as follows: 1~50: 100.
7. method as claimed in claim 4, it is characterised in that: the graphite microparticles are artificial graphite, natural graphite, interphase
One of carbon microspheres or more than one.
8. method as claimed in claim 4, it is characterised in that: the coke micro mist be the petroleum coke of charing, coal tar pitch it is burnt, in
Between one of phase microballoon or more than one.
9. method as claimed in claim 4, it is characterised in that: the temperature of the spray drying is 200 DEG C~400 DEG C.
10. method as claimed in claim 4, it is characterised in that: vacuum degree >=0.01MPa of the vacuum heat treatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110400904A (en) * | 2019-06-04 | 2019-11-01 | 江西力能新能源科技有限公司 | A kind of composite ceramic coat lithium battery positive-negative plate and lithium battery |
| CN115872744A (en) * | 2022-12-14 | 2023-03-31 | 湖南大学 | Method for preparing high-performance binder-free carbon graphite material by solid-phase densification |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110400904A (en) * | 2019-06-04 | 2019-11-01 | 江西力能新能源科技有限公司 | A kind of composite ceramic coat lithium battery positive-negative plate and lithium battery |
| CN115872744A (en) * | 2022-12-14 | 2023-03-31 | 湖南大学 | Method for preparing high-performance binder-free carbon graphite material by solid-phase densification |
| CN115872744B (en) * | 2022-12-14 | 2023-08-08 | 湖南大学 | Method for preparing high-performance binder-free carbon graphite material by solid-phase densification |
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Application publication date: 20190122 |