CN109638239A - A kind of lithium ion battery graphite cathode material and preparation method thereof - Google Patents
A kind of lithium ion battery graphite cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of lithium ion battery graphite cathode materials and preparation method thereof, including following raw material and its weight fraction: graphite powder is 35-50 mass parts；Kamash alloy is 10-15 mass parts；Aqueous adhesive is 2-5 mass parts；Catalyst is 3-4 mass parts；Calcium lignosulfonate pyrolytic carbon is 11-14 mass parts；Surfactant is 3-6 mass parts；Antioxidant is 2-5 mass parts；Dispersing agent is 5-8 mass parts.The addition that the present invention passes through antioxidant, the speed that graphite cathode material is oxidized can effectively have been slowed down, reduce the probability of graphite cathode material damage, extend the service life of graphite cathode material, by the way that kamash alloy is added in graphite cathode material, effectively enhance the toughness and thermal conductivity of graphite cathode material, avoid the phenomenon that graphite cathode material fractures in use, the present invention can greatly improve electronic conductivity, the polarization for reducing graphite cathode material, reduces the internal resistance of material.
Description
Technical field
The present invention relates to technical field of lithium ion, specially a kind of lithium ion battery graphite cathode material and its system
Preparation Method.
Background technique
Development and electric tool, battery-operated motor cycle and electric car with the miniaturization of electronic product with removableization
With the fast development of power battery, high power and high-capacity lithium ion cell have become the hot spot that countries in the world are competitively developed.Make
The negative electrode material of one of the four big main materials for lithium ion battery, and be commercialized and the optimal negative electrode material of using effect at present
It mainly include two class of artificial graphite and natural graphite for graphite Carbon Materials.With the secondary cells such as traditional plumbic acid, ni-Cd, ni-mh
Compare, lithium ion secondary battery have operating voltage is high, small in size, light weight, capacity density height, memory-less effect, it is pollution-free,
The advantages that self discharge is small and has extended cycle life.Since lithium ion battery is successfully realized commercialization by Sony since 1991,
Lithium ion battery has become the leading power supply of mobile phone, laptop and digital product, in the fields such as electric car and energy storage
Using also more and more extensive.Wherein using lithium electricity new energy as the electric car of power, petroleum can not only be replaced with electricity, reduces temperature
The discharge of room gas, can also store electric-net valley-electricity, be the rising industry that developed countries and regions competitively develop.With lithium-ion electric
Pond automobile gradually moves towards market, world's lithium resource use and consume will at geometric growth, thus derived from industry chain (supply chain)
Development prospect is wide, has a high potential.It is contemplated that who seizes the first chance of lithium electricity New Energy Industry, who will just win future
The active of economic development.
Currently, there is also the places of some shortcomings for existing lithium ion battery graphite cathode material, such as；It is existing
Lithium ion battery is oxidized easily in graphite cathode material use process, improves the probability of graphite cathode material damage, contracting
The short service life of graphite cathode material, and the toughness of existing graphite cathode material and thermal conductivity are poor, and graphite is negative
Pole material is easy to appear the phenomenon that fractureing in use, and the polarization of existing lithium ion battery graphite cathode material is compared
Height increases the internal resistance of material, and the high power for reducing lithium ion battery is forthright, cycle performance and charging and discharging capacity.
Summary of the invention
The purpose of the present invention is to provide a kind of lithium ion battery graphite cathode materials and preparation method thereof, solve back
The problem of proposed in scape technology.
To achieve the above object, the invention provides the following technical scheme: a kind of lithium ion battery graphite cathode material and
Preparation method, including following raw material and its weight fraction: graphite powder is 35-50 mass parts；Kamash alloy is 10-15 quality
Part；Aqueous adhesive is 2-5 mass parts；Catalyst is 3-4 mass parts；Calcium lignosulfonate pyrolytic carbon is 11-14 quality
Part；Surfactant is 3-6 mass parts；Antioxidant is 2-5 mass parts；Dispersing agent is 5-8 mass parts.
As a kind of preferred embodiment of the invention, the lithium ion battery graphite cathode material, including it is following
Raw material and its weight fraction: graphite powder is 45 mass parts；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalysis
Agent is 3 mass parts；Surfactant is 5 mass parts；Dispersing agent is 6 mass parts.
As a kind of preferred embodiment of the invention, the lithium ion battery graphite cathode material, including it is following
Raw material and its weight fraction: graphite powder is 45 mass parts；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalysis
Agent is 3 mass parts；Calcium lignosulfonate pyrolytic carbon is 13 mass parts；Surfactant is 5 mass parts；Antioxidant is 3 mass
Part；Dispersing agent is 6 mass parts.
As a kind of preferred embodiment of the invention, the preparation side of the lithium ion battery graphite cathode material
Method, preparation step are as follows:
A. above-mentioned raw materials are weighed according to parts by weight；
B. after the completion of step a, first graphite powder and calcium lignosulfonate pyrolytic carbon are put into be added in mixer and are fitted
The deionized water of amount is mixed, and temperature when mixing is 25-30 DEG C, and the mixed time is 5-10min, then again to mixing
Dispersing agent and catalyst are added in device to be mixed, temperature when mixing is 40-50 DEG C, and the mixed time is 20-30min,
Revolving speed when mixing is 800-1200r/min, and mixture A is made；
C. after the completion of step b, then kamash alloy, aqueous adhesive and surfactant is added into mixture A and carries out
Mixing, temperature when mixing are 35-45 DEG C, and the mixed time is 15-25min, and revolving speed when mixing is 1100-1500r/
Mixture B is made in min；
D. after the completion of step c, the surface of mixture B is then sprayed into one layer of antioxidant again, then again by mixture B
It is put into vacuum oven and is dried, temperature when dry is 80-90 DEG C, and the dry time is 15-20min；
E. after the completion of step d, then the mixture B after drying is put into sintering furnace, and in inert atmosphere or also
In former mixed atmosphere, with the heating of 10~20 DEG C/min rate of heat addition, constant temperature calcining 4~7 hours at 400~750 DEG C, then with 10
The heating of~20 DEG C/min rate of heat addition, constant temperature calcining 10~15 hours at 850~1200 DEG C, then with 10~20 DEG C/min drop
Warm speed is cooled to room temperature, and obtains graphite cathode material.
As a kind of preferred embodiment of the invention, the aqueous binders are polyethylene nitrile, polyvinyl chloride, poly- second
One of vinyl acetate, polyacrylic acid glycol ester and polymethyl methacrylate or arbitrary proportion it is a variety of.
As a kind of preferred embodiment of the invention, the catalyst is in the oxide or nitride of silicon, iron, boron
It is one or more, additional amount be graphite powder primary particle quality 1-10wt%.
As a kind of preferred embodiment of the invention, the surfactant be dodecyl sodium sulfate, stearic acid,
Any a kind or at least two kinds of of combination in PVA.
As a kind of preferred embodiment of the invention, the dispersing agent is water, methanol, ethyl alcohol, benzene, toluene, acetone, has
One or more of machine acid and organic ester.
As a kind of preferred embodiment of the invention, the antioxidant is the mixture of ceramic powder in aqueous solution
Coating.
Compared with prior art, beneficial effects of the present invention are as follows:
The present invention can effectively slow down the speed that graphite cathode material is oxidized by the addition of antioxidant, reduce
The probability of graphite cathode material damage, extends the service life of graphite cathode material, by graphite cathode material plus
Enter kamash alloy, effectively enhance the toughness and thermal conductivity of graphite cathode material, avoids graphite cathode material and using
The phenomenon that fractureing in journey, the present invention can greatly improve electronic conductivity, reduce the polarization of graphite cathode material, reduce
The internal resistance of material, the high power for improving lithium ion battery is forthright, cycle performance and charging and discharging capacity.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is a kind of flow chart of lithium ion battery graphite cathode material of the present invention and preparation method thereof.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of lithium ion battery graphite cathode material and its preparation
Method, including following raw material and its weight fraction: graphite powder is 35-50 mass parts；Kamash alloy is 10-15 mass parts；It is aqueous
Bonding agent is 2-5 mass parts；Catalyst is 3-4 mass parts；Calcium lignosulfonate pyrolytic carbon is 11-14 mass parts；Surface is living
Property agent be 3-6 mass parts；Antioxidant is 2-5 mass parts；Dispersing agent is 5-8 mass parts.
Further, the lithium ion battery graphite cathode material, including following raw material and its weight fraction: graphite powder
For 45 mass parts；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalyst is 3 mass parts；Surfactant
For 5 mass parts；Dispersing agent is 6 mass parts.
Further, the lithium ion battery graphite cathode material, including following raw material and its weight fraction: graphite powder
For 45 mass parts；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalyst is 3 mass parts；Lignin sulfonic acid
Calcium pyrolytic carbon is 13 mass parts；Surfactant is 5 mass parts；Antioxidant is 3 mass parts；Dispersing agent is 6 mass parts.
Further, the preparation method of the lithium ion battery graphite cathode material, preparation step are as follows:
A. above-mentioned raw materials are weighed according to parts by weight；
B. after the completion of step a, first graphite powder and calcium lignosulfonate pyrolytic carbon are put into be added in mixer and are fitted
The deionized water of amount is mixed, and temperature when mixing is 25-30 DEG C, and the mixed time is 5-10min, then again to mixing
Dispersing agent and catalyst are added in device to be mixed, temperature when mixing is 40-50 DEG C, and the mixed time is 20-30min,
Revolving speed when mixing is 800-1200r/min, and mixture A is made；
C. after the completion of step b, then kamash alloy, aqueous adhesive and surfactant is added into mixture A and carries out
Mixing, temperature when mixing are 35-45 DEG C, and the mixed time is 15-25min, and revolving speed when mixing is 1100-1500r/
Mixture B is made in min；
D. after the completion of step c, the surface of mixture B is then sprayed into one layer of antioxidant again, then again by mixture B
It is put into vacuum oven and is dried, temperature when dry is 80-90 DEG C, and the dry time is 15-20min；
E. after the completion of step d, then the mixture B after drying is put into sintering furnace, and in inert atmosphere or also
In former mixed atmosphere, with the heating of 10~20 DEG C/min rate of heat addition, constant temperature calcining 4~7 hours at 400~750 DEG C, then with 10
The heating of~20 DEG C/min rate of heat addition, constant temperature calcining 10~15 hours at 850~1200 DEG C, then with 10~20 DEG C/min drop
Warm speed is cooled to room temperature, and obtains graphite cathode material.
Further, the aqueous binders are polyethylene nitrile, polyvinyl chloride, polyvinyl acetate, polyacrylic acid second two
One of alcohol ester and polymethyl methacrylate or arbitrary proportion it is a variety of.
Further, the catalyst is one of silicon, iron, the oxide of boron or nitride or a variety of, additional amount
For the 1-10wt% of graphite powder primary particle quality.
Further, the surfactant is dodecyl sodium sulfate, stearic acid, any a kind or at least two kinds of in PVA
Combination.
Further, the dispersing agent be one of water, methanol, ethyl alcohol, benzene, toluene, acetone, organic acid and organic ester or
It is several.
Further, the antioxidant is the mixture coating of ceramic powder in aqueous solution.
Embodiment one
The lithium ion battery graphite cathode material, including following raw material and its weight fraction: graphite powder is 45 matter
Measure part；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalyst is 3 mass parts；Surfactant is 5 mass
Part；Dispersing agent is 6 mass parts.
Preparation step is as follows:
A. above-mentioned raw materials are weighed according to parts by weight；
B. after the completion of step a, first graphite powder and calcium lignosulfonate pyrolytic carbon are put into be added in mixer and are fitted
The deionized water of amount is mixed, and temperature when mixing is 25-30 DEG C, and the mixed time is 5-10min, then again to mixing
Dispersing agent and catalyst are added in device to be mixed, temperature when mixing is 40-50 DEG C, and the mixed time is 20-30min,
Revolving speed when mixing is 800-1200r/min, and mixture A is made；
C. after the completion of step b, then kamash alloy, aqueous adhesive and surfactant is added into mixture A and carries out
Mixing, temperature when mixing are 35-45 DEG C, and the mixed time is 15-25min, and revolving speed when mixing is 1100-1500r/
Mixture B is made in min；
D. after the completion of step c, the surface of mixture B is then sprayed into one layer of antioxidant again, then again by mixture B
It is put into vacuum oven and is dried, temperature when dry is 80-90 DEG C, and the dry time is 15-20min；
E. after the completion of step d, then the mixture B after drying is put into sintering furnace, and in inert atmosphere or also
In former mixed atmosphere, with the heating of 10~20 DEG C/min rate of heat addition, constant temperature calcining 4~7 hours at 400~750 DEG C, then with 10
The heating of~20 DEG C/min rate of heat addition, constant temperature calcining 10~15 hours at 850~1200 DEG C, then with 10~20 DEG C/min drop
Warm speed is cooled to room temperature, and obtains graphite cathode material.
Embodiment two
The lithium ion battery graphite cathode material, including following raw material and its weight fraction: graphite powder is 45 matter
Measure part；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalyst is 3 mass parts；Calcium lignosulfonate pyrolysis
Carbon is 13 mass parts；Surfactant is 5 mass parts；Antioxidant is 3 mass parts；Dispersing agent is 6 mass parts.
Preparation step is as follows:
A. above-mentioned raw materials are weighed according to parts by weight；
B. after the completion of step a, first graphite powder and calcium lignosulfonate pyrolytic carbon are put into be added in mixer and are fitted
The deionized water of amount is mixed, and temperature when mixing is 25-30 DEG C, and the mixed time is 5-10min, then again to mixing
Dispersing agent and catalyst are added in device to be mixed, temperature when mixing is 40-50 DEG C, and the mixed time is 20-30min,
Revolving speed when mixing is 800-1200r/min, and mixture A is made；
C. after the completion of step b, then kamash alloy, aqueous adhesive and surfactant is added into mixture A and carries out
Mixing, temperature when mixing are 35-45 DEG C, and the mixed time is 15-25min, and revolving speed when mixing is 1100-1500r/
Mixture B is made in min；
D. after the completion of step c, the surface of mixture B is then sprayed into one layer of antioxidant again, then again by mixture B
It is put into vacuum oven and is dried, temperature when dry is 80-90 DEG C, and the dry time is 15-20min；
E. after the completion of step d, then the mixture B after drying is put into sintering furnace, and in inert atmosphere or also
In former mixed atmosphere, with the heating of 10~20 DEG C/min rate of heat addition, constant temperature calcining 4~7 hours at 400~750 DEG C, then with 10
The heating of~20 DEG C/min rate of heat addition, constant temperature calcining 10~15 hours at 850~1200 DEG C, then with 10~20 DEG C/min drop
Warm speed is cooled to room temperature, and obtains graphite cathode material.
Conventional graphite negative material data parameters table 1 is as follows:
| Test item | Antioxidant effect | Toughness and thermal conductivity | Polarization effect | Charging and discharging capacity |
| Parameter index | Difference | It is weak | It is high | It is lower |
One graphite cathode material data parameters table 2 of embodiment is as follows:
| Test item | Antioxidant effect | Toughness and thermal conductivity | Polarization effect | Charging and discharging capacity |
| Parameter index | Generally | It is relatively strong | In | Generally |
Two graphite cathode material data parameters table 3 of embodiment is as follows:
| Test item | Antioxidant effect | Toughness and thermal conductivity | Polarization effect | Charging and discharging capacity |
| Parameter index | Well | By force | It is low | It is higher |
It to sum up states, is obtained referring to the data comparison of table 1, table 2 and table 3, the present invention, can be effective by the addition of antioxidant
The speed for having slowed down graphite cathode material and being oxidized, reduce graphite cathode material damage probability, extend graphite cathode
The service life of material effectively enhances the tough of graphite cathode material by the way that kamash alloy is added in graphite cathode material
Property and thermal conductivity, avoid the phenomenon that graphite cathode material fractures in use, the present invention can greatly improve
Electronic conductivity reduces the polarization of graphite cathode material, reduces the internal resistance of material, and the high power for improving lithium ion battery is forthright, follows
Ring performance and charging and discharging capacity.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for this field skill
For art personnel, it is clear that invention is not limited to the details of the above exemplary embodiments, and without departing substantially from spirit of the invention or
In the case where essential characteristic, the present invention can be realized in other specific forms.Therefore, in all respects, should all incite somebody to action
Embodiment regards exemplary as, and is non-limiting, the scope of the present invention by appended claims rather than on state
Bright restriction, it is intended that including all changes that fall within the meaning and scope of the equivalent elements of the claims in the present invention
It is interior.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of lithium ion battery graphite cathode material, it is characterised in that: including following raw material and its weight fraction: graphite powder
For 35-50 mass parts；Kamash alloy is 10-15 mass parts；Aqueous adhesive is 2-5 mass parts；Catalyst is 3-4 quality
Part；Calcium lignosulfonate pyrolytic carbon is 11-14 mass parts；Surfactant is 3-6 mass parts；Antioxidant is 2-5 quality
Part；Dispersing agent is 5-8 mass parts.
2. a kind of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: including following raw material
And its weight fraction: graphite powder is 45 mass parts；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalyst is
3 mass parts；Surfactant is 5 mass parts；Dispersing agent is 6 mass parts.
3. a kind of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: including following raw material
And its weight fraction: graphite powder is 45 mass parts；Kamash alloy is 12 mass parts；Aqueous adhesive is 4 mass parts；Catalyst is
3 mass parts；Calcium lignosulfonate pyrolytic carbon is 13 mass parts；Surfactant is 5 mass parts；Antioxidant is 3 mass parts；Point
Powder is 6 mass parts.
4. a kind of preparation method of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: system
It is standby that steps are as follows:
A. above-mentioned raw materials are weighed according to parts by weight；
B. after the completion of step a, graphite powder and calcium lignosulfonate pyrolytic carbon are put into mixer first be added it is suitable
Deionized water is mixed, and temperature when mixing is 25-30 DEG C, and the mixed time is 5-10min, then again into mixer
Dispersing agent and catalyst is added to be mixed, temperature when mixing is 40-50 DEG C, and the mixed time is 20-30min, mixing
When revolving speed be 800-1200r/min, be made mixture A；
C. after the completion of step b, then kamash alloy, aqueous adhesive and surfactant is added into mixture A and is mixed,
Temperature when mixing is 35-45 DEG C, and the mixed time is 15-25min, and revolving speed when mixing is 1100-1500r/min, system
Obtain mixture B；
D. after the completion of step c, the surface of mixture B is then sprayed into one layer of antioxidant again, is then again put into mixture B
It is dried in vacuum oven, temperature when dry is 80-90 DEG C, and the dry time is 15-20min；
E. after the completion of step d, then the mixture B after drying is put into sintering furnace, and mixed in inert atmosphere or reduction
It closes in atmosphere, with the heating of 10~20 DEG C/min rate of heat addition, constant temperature calcining 4~7 hours at 400~750 DEG C, then with 10~20
DEG C/heating of the min rate of heat addition, then constant temperature calcining 10~15 hours at 850~1200 DEG C are cooled down fast with 10~20 DEG C/min
Degree is cooled to room temperature, and obtains graphite cathode material.
5. a kind of preparation method of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: institute
The aqueous binders stated are polyethylene nitrile, polyvinyl chloride, polyvinyl acetate, polyacrylic acid glycol ester and polymethylacrylic acid
One of methyl esters or arbitrary proportion it is a variety of.
6. a kind of preparation method of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: institute
Stating catalyst is one of silicon, iron, the oxide of boron or nitride or a variety of, and additional amount is graphite powder primary particle matter
The 1-10wt% of amount.
7. a kind of preparation method of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: institute
Surfactant is stated as any a kind or at least two kinds of of combination in dodecyl sodium sulfate, stearic acid, PVA.
8. a kind of preparation method of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: institute
Stating dispersing agent is one or more of water, methanol, ethyl alcohol, benzene, toluene, acetone, organic acid and organic ester.
9. a kind of preparation method of lithium ion battery graphite cathode material according to claim 1, it is characterised in that: institute
Stating antioxidant is the mixture coating of ceramic powder in aqueous solution.
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| CN102464883A (en) * | 2010-11-16 | 2012-05-23 | 比亚迪股份有限公司 | Heat-conducting resin composition and preparation method thereof |
| CN104124431A (en) * | 2014-08-12 | 2014-10-29 | 湖南元素密码石墨烯研究院（有限合伙） | Graphite negative electrode material for lithium ion battery and preparation method of graphite negative electrode material |
| CN104609400A (en) * | 2014-12-30 | 2015-05-13 | 东莞市凯金新能源科技有限公司 | Composite graphite cathode material and preparation method thereof |
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