CN109449419A - A kind of CNT- graphite composite active material and preparation method thereof for lithium ion battery - Google Patents
A kind of CNT- graphite composite active material and preparation method thereof for lithium ion battery Download PDFInfo
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- CN109449419A CN109449419A CN201811308477.0A CN201811308477A CN109449419A CN 109449419 A CN109449419 A CN 109449419A CN 201811308477 A CN201811308477 A CN 201811308477A CN 109449419 A CN109449419 A CN 109449419A
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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
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- 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
- H01M4/58—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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- 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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The CNT- graphite composite active material and preparation method thereof that the present invention relates to a kind of for lithium ion battery, belongs to lithium electro-technical field.CNT- graphite composite active material of the invention is to have the CNT- graphite material of CNT in graphite surface in-situ authigenic, the preparation method comprises the following steps: at Graphite Coating layer of Ni (OH)2Modified graphite is made in particle；Modified graphite is placed in atmosphere furnace, the CNT- powdered graphite for having CNT in graphite surface growth is made in heating and thermal insulation；CNT- powdered graphite is placed in acid solution and carries out acidic treatment to remove Ni, is then cleaned using deionized water, obtains CNT- graphite composite active material.It is high that CNT- graphite composite active material of the invention is applied to conductivity and charge-discharge magnification when lithium ion battery.
Description
Technical field
The invention belongs to lithium electro-technical field, be related to a kind of CNT- graphite composite active material for lithium ion battery and
Preparation method.
Background technique
Lithium ion battery is being a kind of secondary cell (rechargeable battery), with the development of society, the application of lithium ion battery
Further extensively, the requirement to performance of lithium ion battery is also higher and higher.
Lithium ion battery relies primarily on lithium ion, and movement carrys out work between a positive electrode and a negative electrode.In charge and discharge process, Li+
Insertion and deintercalation back and forth between two electrodes: when charging, Li+ is embedded in cathode from positive deintercalation, by electrolyte, and cathode is in
Lithium-rich state；It is then opposite when electric discharge.Lithium ion battery mainly includes anode pole piece, cathode pole piece, electrolyte and diaphragm, in anode
It is coated with positive active material on pole piece, negative electrode active material, the positive and negative anodes activity of lithium ion battery are coated on cathode pole piece
One of an important factor for material is decision performance of lithium ion battery.Lithium ion battery anode active material is based on graphite at present,
But the charge-discharge magnification that graphite is led as lithium ion battery anode active material is lower, it is to be improved.In order to improve cathode pole
Usually conductive agent, such as CNT will be added in cathode in the electronic conductivity of piece in material.Since the particle of conductive agent is tiny, specific surface
It is actively high, it is easy to reunite in the slurry, is difficult to disperse.And a large amount of additions of conductive agent also improve lithium ion to a certain extent
The cost of battery.
Summary of the invention
The purpose of the present invention is in view of the above-mentioned problems existing in the prior art, propose a kind of graphite surface in-situ authigenic
The CNT- graphite composite active material for lithium ion battery of CNT is applied to conductivity and charge and discharge times when lithium ion battery
Rate is high.
Object of the invention can be realized by the following technical scheme:
A kind of CNT- graphite composite active material for lithium ion battery, the CNT- graphite composite active material be
Graphite surface in-situ authigenic has the CNT- graphite material of CNT.
The present invention has the CNT- graphite material of CNT as negative electrode of lithium ion battery activity material using graphite surface in-situ authigenic
Material can sufficiently improve electronic conductivity of the graphite in charge and discharge process, improve the specific surface area of graphite, improve the charge and discharge of graphite
Electric multiplying power, while the additive amount of cathode conductive agent in lithium ion battery manufacturing process can be reduced and solve traditional directly addition
The difficult problem of conductive agent dispersion.
Preferably, the length of the CNT grown in the CNT- graphite material in graphite surface is 1 μm -3 μm, diameter is
20nm-70nm。
Theoretically, CNT is longer, and diameter is smaller, then the specific gravity of CNT is bigger in CNT- graphite material, specific surface area
It is bigger, be more conducive to the raising of lithium ion battery conductivity.But the specific surface area of CNT- graphite material is consequently increased, and is needed
Increase the usage amount of binder to stablize the service life of cathode, and the excessive use of binder can be to performance of lithium ion battery
Play reaction.Therefore it is electrochemical to comprehensively consider porosity, thickness, the multiplying power of battery and capacity of lithium ion battery negative electrode etc.
Performance is learned, the present invention controls the length of CNT in 1-3 μm.
Another object of the present invention is to provide a kind of systems of CNT- graphite composite active material for lithium ion battery
Preparation Method, the preparation method comprises the following steps,
S1, at Graphite Coating layer of Ni (OH)2Modified graphite is made in particle；
S2, modified graphite is placed in atmosphere furnace, the CNT- graphite powder for having CNT in graphite surface growth is made in heating and thermal insulation
End；
S3, by CNT- powdered graphite be placed in acid solution carry out acidic treatment to remove Ni, then using deionized water clean,
Obtain CNT- graphite composite active material.
The present invention passes through at graphite surface Ni (OH)2The cladding of particle, so that the growth of catalytic graphite surface C NT, is adding
Ni (OH) in thermal process2It resolves into NiO and is reacted again with carbon atom and be reduced into W metal, using solid graphite as carbon source, in stone
Black surface directly grows CNT.
Preferably, in the step S1 then graphite is filtered off prior to being cleaned by ultrasonic 20min-40min in dehydrated alcohol
Except dehydrated alcohol.Purpose is the affinity in order to remove the impurity in graphite, improve graphite and aqueous solution.
Preferably, Ni (OH) in the step S12The partial size of particle is 20nm-70nm.
The present invention passes through control Ni (OH)2Particle size and then the diameter for controlling CNT.W metal being capable of catalytic graphite surface
The growth of CNT, the size of W metal determine the diameter of CNT, and Ni (OH)2As the presoma of W metal, partial size
Size determines the size of Ni particle.
Preferably, in the step S1 modified graphite preparation method be by coprecipitation graphite surface with packet
Cover layer of Ni (OH)2Particle.
Preferably, the preparation method of modified graphite is specifically, by graphite and Ni (NO in the step S13)2Solution according to
Suspension is made in the ratio of 4.5g/L-5.5g/L, and it is 7.5-8.0 that NaOH solution to pH value, which is added, and removal supernatant is used after standing
Washes of absolute alcohol obtains Ni (OH)2The turbid body of graphite, then be dried in vacuo and obtain Ni nanoparticle (OH)2Particles coat changes
Property graphite particle.
Preferably, Ni (the NO3)2The concentration of solution is 0.03mol/L-0.6mol/L.
Preferably, the time of the standing is 22-26h.
Preferably, the concentration of the NaOH solution is 0.4mol/L-0.5mol/L.
Preferably, the adding manner of the NaOH solution is to be added dropwise.
Preferably, washes of absolute alcohol number is three times.
Ni(NO3)2The molar concentration of solution influences final Ni (OH)2Particle size, the present invention pass through control Ni (NO3)2It is molten
The molar concentration of liquid is by Ni (OH)2The size controlling of particle is in 20nm-70nm.
Preferably, the process of heating and thermal insulation is in the step S2, under inert gas atmosphere protection, with 14 DEG C/
The heating speed of min-16 DEG C/min is heated to 600 DEG C -850 DEG C, keeps the temperature 1h-2h.
The present invention is controlled the length of CNT in 1 μ by heating speed, temperature and soaking time in control insulating process
m-3μm。
Preferably, the inert gas is argon gas.
Preferably, acid solution is the HCl solution of 4.5wt.%-5.5wt.% in the step S3.
Preferably, acidic treatment is to carry out ultrasonic treatment 2.5-3.5h in acid solution in the step S3.
Compared with prior art, the invention has the following advantages:
There is the CNT- graphite material of CNT as lithium ion battery anode active material using graphite surface in-situ authigenic, fills
Point improve electronic conductivity of the graphite in charge and discharge process, improve the charge-discharge magnification of graphite, at the same can reduce lithium from
The additive amount of cathode conductive agent in sub- battery manufacturing process avoids the difficult problem of traditional directly addition conductive agent dispersion.Pass through
Layer of Ni (OH) is first generated in graphite surface2, and by specifically heat preservation calcination technique, the size for generating CNT is effectively controlled,
To control the performance for generating negative electrode active material.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
CNT- graphite composite active material in the present embodiment for lithium ion battery is made according to the following steps:
(1) 2.5g graphite is cleaned by ultrasonic 30min in dehydrated alcohol, then filtering removal dehydrated alcohol, after cleaning
Graphite be added to the Ni (NO of 500mL 0.03mol/L3)2In solution, magnetic agitation 10min forms suspension, then proceedes to
It stirs and NaOH solution to the pH value that 0.45mol/L is added dropwise is 7.8 end, stand and remove the anhydrous second of supernatant afterwards for 24 hours
Alcohol cleans three times, obtains stable Ni (OH)2The turbid body of graphite, then be dried in vacuo and obtain Ni nanoparticle (OH)2Particles coat
Modified graphite particle, Ni nanoparticle (OH)2The partial size of particle is 20nm-30nm；
(2) modified graphite is placed in atmosphere furnace, under protection of argon gas, with the heating speed of 15 DEG C/min, is heated to 730
DEG C, 1.6h is kept the temperature, graphite surface is made to grow CNT, CNT- powdered graphite is made, the length of CNT is 1.8 μm -2.3 μm, and diameter is
20nm-30nm；
(3) CNT- powdered graphite is placed in the HCl solution of 5.0wt.% and carries out ultrasonic treatment 3h removal Ni, then used
Deionized water is cleaned three times, and CNT- graphite composite active material is obtained.
Embodiment 2
Unlike the first embodiment, quantity of graphite used in step (1) is 2.8g, Ni (NO3)2The concentration of solution is
0.45mol/L, other are same as Example 1.
Ni nanoparticle (OH) obtained2In the modified graphite particle of particles coat, Ni nanoparticle (OH)2The partial size of particle is 40nm-
60nm；In CNT- powdered graphite obtained, the length of CNT is 1.8 μm -2.5 μm, diameter 40nm-60nm；
Embodiment 3
Unlike the first embodiment, quantity of graphite used in step (1) is 3.0g, Ni (NO3)2The concentration of solution is
0.6mol/L, other are same as Example 1.
Ni nanoparticle (OH) obtained2In the modified graphite particle of particles coat, Ni nanoparticle (OH)2The partial size of particle is 50nm-
70nm；In CNT- powdered graphite obtained, the length of CNT is 1.9 μm -2.6 μm, diameter 50nm-70nm；
Embodiment 4
Unlike the first embodiment, heating speed of the modified graphite in atmosphere furnace is 14 DEG C/min in step (2),
He is same as Example 1.
The length of CNT is 2.0 μm -3.0 μm in CNT- graphite material obtained, diameter 20nm-30nm.
Embodiment 5
Unlike the first embodiment, heating speed of the modified graphite in atmosphere furnace is 16 DEG C/min in step (2),
He is same as Example 1.
The length of CNT is 1.2 μm -2.0 μm in CNT- graphite material obtained, diameter 20nm-30nm.
Embodiment 6
Unlike the first embodiment, holding temperature of the modified graphite in atmosphere furnace is 600 DEG C in step (2), other are
It is same as Example 1.
The length of CNT is 1.5 μm -2.2 μm in CNT- graphite material obtained, diameter 20nm-30nm.
Embodiment 7
Unlike the first embodiment, holding temperature of the modified graphite in atmosphere furnace is 850 DEG C in step (2), other are
It is same as Example 1.
The length of CNT is 2.0-2.6 μm in CNT- graphite material obtained, diameter 20nm-30nm.
Comparative example 1
In step (2) holding temperature of the modified graphite in atmosphere furnace be 590 DEG C, soaking time 50min, other with
Embodiment 1 is identical.
CNT lacks orientation in CNT- graphite material obtained, of poor quality, there is impurity.
Comparative example 2
In step (2) holding temperature of the modified graphite in atmosphere furnace be 870 DEG C, soaking time 2h, other with reality
It is identical to apply example 1.
CNT impurity is more in CNT- graphite material obtained.
Comparative example 3
In the prior art using ordinary graphite, addition conductive agent CNT as negative electrode active material.
Using in 1-7 of the embodiment of the present invention, comparative example 1-3 negative electrode active material preparation lithium ion battery performance into
Row compares, and comparison result is as shown in table 1.
Table 1: the comparison of battery performance in embodiment 1-7, comparative example 1-3
In conclusion the present invention is a kind of for lithium-ion electric by being prepared in the method for graphite surface growth in situ CNT
The CNT- graphite composite active material in pond, effectively increases the specific surface area of graphite, improves the electronic conductivity of graphite and fills
Discharge-rate.
Quantity of graphite in the embodiment of the present invention 1 can also be 2.25g (i.e. graphite and Ni (NO3)2The ratio of solution is 4.5g/
L), 2.75g (i.e. graphite and Ni (NO3)2The ratio of solution is 5.5g/L) and 2.25g to any value between 2.75g；NaOH is molten
The concentration of liquid can also be 0.4mol/L, 0.5mol/L and 0.4mol/L to any value between 0.5mol/L；It is molten that NaOH is added
The pH value adjusted after liquid can also be any value between 7.5,8.0 and 7.5 to 8.0；Guarantor of the modified graphite in atmosphere furnace
The warm time can also be 1h, 2h and 1h to any value between 2h；Final Ni nanoparticle (OH) obtained2The modification stone of particles coat
In black particle, Ni nanoparticle (OH)2The partial size of particle is between 20nm-70nm, and the length of CNT is equal in CNT- graphite material obtained
Between 2.0 μm -2.6 μm, diameter is between 20nm-70nm, to the lithium-ion electric using the preparation of above-mentioned negative electrode active material
The performance in pond is detected, capacity between 3.8Ah-4.1Ah, energy density between 146Wh/kg-151Wh/kg,
Internal resistance is between 28m Ω -32m Ω, and discharge capacitance is between 83.5%-86.0% after 1C/1C is recycled 1000 times.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (10)
1. a kind of CNT- graphite composite active material for lithium ion battery, which is characterized in that the compound work of CNT- graphite
Property material be in graphite surface in-situ authigenic to have the CNT- graphite material of CNT.
2. the CNT- graphite composite active material according to claim 1 for lithium ion battery, which is characterized in that described
Length in CNT- graphite material in the CNT of graphite surface growth is 1 μm -3 μm, diameter 20nm-70nm.
3. a kind of preparation method for the CNT- graphite composite active material of lithium ion battery as claimed in claim 1 or 2,
It is characterized in that, the preparation method comprises the following steps,
S1, at Graphite Coating layer of Ni (OH)2Modified graphite is made in particle；
S2, modified graphite is placed in atmosphere furnace, the CNT- powdered graphite for having CNT in graphite surface growth is made in heating and thermal insulation；
S3, by CNT- powdered graphite be placed in acid solution carry out acidic treatment to remove Ni, then using deionized water clean, that is, make
Obtain CNT- graphite composite active material.
4. preparation method according to claim 3, which is characterized in that Ni (OH) in the step S12The partial size of particle is
20nm-70nm。
5. preparation method according to claim 3 or 4, which is characterized in that the preparation side of modified graphite in the step S1
Method be by coprecipitation graphite surface with cladding layer of Ni (OH)2Particle.
6. preparation method according to claim 3 or 4, which is characterized in that the preparation side of modified graphite in the step S1
Method is specifically, by graphite and Ni (NO3)2Suspension is made according to the ratio of 4.5g/L-5.5g/L in solution, and NaOH solution is added extremely
PH value is 7.5-8.0, removes supernatant washes of absolute alcohol after standing, obtains Ni (OH)2The turbid body of graphite, then carry out vacuum
Drying to obtain Ni nanoparticle (OH)2The modified graphite particle of particles coat.
7. preparation method according to claim 6, which is characterized in that the Ni (NO3)2The concentration of solution is 0.03mol/
L-0.6mol/L。
8. preparation method according to claim 3, which is characterized in that the process of heating and thermal insulation is in the step S2,
Under inert gas atmosphere protection, with the heating speed of 14 DEG C/min-16 DEG C/min, 600 DEG C -850 DEG C are heated to, keeps the temperature 1h-2h.
9. preparation method according to claim 3, which is characterized in that acid solution is 4.5wt.%- in the step S3
The HCl solution of 5.5wt.%.
10. preparation method according to claim 3, which is characterized in that acidic treatment is in acid solution in the step S3
Carry out ultrasonic treatment 2.5-3.5h.
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