CN109524667A - A kind of preparation method of combined conductive agent and preparation method thereof, carbon nanotube - Google Patents
A kind of preparation method of combined conductive agent and preparation method thereof, carbon nanotube Download PDFInfo
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Abstract
The invention discloses a kind of combined conductive agent and preparation method thereof, the preparation method of carbon nanotube, the combined conductive agent, each components including following mass percent: carbon nanotube 0.25~0.35%；One-dimensional electric agent 1~2%；Dispersing agent 0.5~1%；Solvent 96.65~98.25%；A kind of preparation method of combined conductive agent, comprising the following steps: 1) according to formula ratio, the composite powder of carbon nanotube and one-dimensional electric agent is made of hydro-thermal method；2) composite powder is added in solvent, after dispersing agent is added in solvent, obtain mixture；3) mixture is subjected to ultrasonic disperse.It is an advantage of the invention that dotted one-dimensional electric agent is combined closely with linear carbon nanotube, form the two-dimentional conductive network of Joint of Line and Dot, when combined conductive agent is added in lithium ion cell electrode, carbon nanotube forms effective line-shaped conductive network, can significantly improve the high rate performance and cycle performance of lithium ion battery.
Description
Technical field
The present invention relates to combined conductive agent fields, more particularly to a kind of combined conductive agent and preparation method thereof, carbon nanometer
The preparation method of pipe.
Background technique
Quick with electric car is popularized, and increases dynamic to the lithium ion of high-power, high-energy density, thermal safety
The demand of power battery, lithium-ion-power cell industry have welcome new challenge.As lithium-ion-power cell important component
Conductive agent plays an important role to lithium-ion-power cell performance is improved.Therefore the promotion of energy density and cycle life is compeled instantly
The further improvement for the material system being essential including conductive agent to be included.
Summary of the invention
Goal of the invention: in view of the above-mentioned problems, an object of the present invention is to provide a kind of combined conductive agent, to solve energy
The technical issues of promotion demand of density and cycle life.
The second object of the present invention is to provide a kind of preparation method of combined conductive agent.
The third object of the present invention is to provide a kind of preparation method of carbon nanotube.
Technical solution:
A kind of combined conductive agent, each component including following mass percent:
Due to including carbon nanotube and one-dimensional electric agent, the carbon nanotube of dotted one-dimensional electric agent and threadiness is combined closely,
The two-dimentional conductive network of Joint of Line and Dot is formed, one-dimensional electric agent porosity is very high, has excellent imbibition and water retainability, and carbon is received
Mitron has excellent electric conductivity, and graphitization is with high purity, when combined conductive agent is added in lithium ion cell electrode, carbon
Nanotube forms effective line-shaped conductive network, can greatly reduce the dosage of combined conductive agent, carbon nanotube and one-dimensional electric agent
Collaboration use, the high rate performance and cycle performance of lithium ion battery can be significantly improved.
The dispersing agent is polyvinylpyrrolidone in one of the embodiments,.
The solvent is N-Methyl pyrrolidone in one of the embodiments,.
The carbon nanotube is made by following preparation method in one of the embodiments: carbon is made with catalystic pyrolysis
Nanotube crude samples, with the HNO of 0.8~1.5mol/L3Solution to carbon nanotube crude samples carry out pickling, after use high-temperature roasting furnace
High-temperature process is carried out to the carbon nanotube crude samples after pickling, obtains carbon nanotube.Since carbon nanotube crude samples first pass through acid
It washes, carries out high-temperature process afterwards, the degree of graphitization of carbon nanotube can be effectively improved, improve the purity of carbon nanotube, effectively drop
Low DC internal resistance improves the high temperature cyclic performance of lithium ion battery.
The one-dimensional electric agent is Ketjen black, conductive black or electrically conductive graphite in one of the embodiments,.One-dimensional electric
Agent has high porosity with active material in lithium ion cell electrode with dotted combination, especially Ketjen black, has very
Strong imbibition and water retainability.
A kind of preparation method of combined conductive agent, comprising the following steps:
1) according to formula ratio, the composite powder of carbon nanotube and one-dimensional electric agent is made of hydro-thermal method；
2) composite powder is added in solvent, after dispersing agent is added in solvent, obtain mixture；
3) mixture is subjected to ultrasonic disperse, combined conductive agent can be obtained.
In one of the embodiments, in step 1), hydro-thermal method specifically: one-dimensional electric agent is added in water heating kettle and goes
Ionized water, at room temperature stir 10~20min, be added carbon nanotube after continue that 20~30min is stirred at room temperature, after at 180~200 DEG C
3~4h of lower stirring, obtained product cooled to room temperature is put into tube furnace after being filtered, washed, drying, in nitrogen
500~600 DEG C, 2~3h of constant temperature are warming up under atmosphere, after be cooled to room temperature, composite powder can be obtained.Due to first using hydro-thermal
Method mixes carbon nanotube and one-dimensional electric agent, and dotted one-dimensional electric agent is combined closely with linear carbon nanotube, forms point
The two-dimentional conductive network that knot is closed makes to be uniformly mixed afterwards and dispersant, it is rear solvent is added after carry out ultrasonic disperse, make carbon
Nanotube and one-dimensional electric agent obtain being sufficiently mixed dispersion, obtain the stable combined conductive agent of performance.
In one of the embodiments, in step 3), the dispersion frequency of ultrasonic disperse is 40~50Hz, jitter time 1
~1.5h.
Dispersing agent is polyvinylpyrrolidone in one of the embodiments, and solvent is N-Methyl pyrrolidone.
A kind of preparation method of carbon nanotube, comprising the following steps:
1) carbon nanotube crude samples are made with catalystic pyrolysis；
2) with the HNO of 0.8~1.5mol/L3Solution carries out pickling to carbon nanotube crude samples；
3) high-temperature process is carried out to the carbon nanotube crude samples after pickling with high-temperature roasting furnace, obtains carbon nanotube.Due to
Carbon nanotube crude samples first pass through pickling, carry out high-temperature process afterwards, can effectively improve the degree of graphitization of carbon nanotube, improve
The purity of carbon nanotube, is effectively reduced DC internal resistance, improves the high temperature cyclic performance of lithium ion battery.
The utility model has the advantages that compared with prior art, the invention has the advantages that combined conductive agent of the invention, due to including
Carbon nanotube and one-dimensional electric agent, dotted one-dimensional electric agent are combined closely with linear carbon nanotube, form Joint of Line and Dot
Two-dimentional conductive network, one-dimensional electric agent porosity is very high, has excellent imbibition and water retainability, and carbon nanotube has excellent
Electric conductivity, graphitization purity is high, when combined conductive agent is added in lithium ion cell electrode, carbon nanotube is formed effectively
Line-shaped conductive network, the dosage of combined conductive agent can be greatly reduced, the collaboration of carbon nanotube and one-dimensional electric agent uses, can be with
Significantly improve the high rate performance and cycle performance of lithium ion battery.
The preparation method of combined conductive agent of the invention, due to first hydro-thermal method being used to mix carbon nanotube and one-dimensional electric agent
Close, dotted one-dimensional electric agent and linear carbon nanotube are combined closely, form the two-dimentional conductive network of Joint of Line and Dot, afterwards with divide
Powder mixing, makes to be uniformly mixed, and carries out ultrasonic disperse after rear addition solvent, mixes carbon nanotube and one-dimensional electric agent sufficiently
Dispersion is closed, the stable combined conductive agent of performance is obtained.
The preparation method of carbon nanotube of the invention, it is rear to carry out at high temperature since carbon nanotube crude samples first pass through pickling
Reason, can effectively improve the degree of graphitization of carbon nanotube, improve the purity of carbon nanotube, DC internal resistance is effectively reduced, and improve
The high temperature cyclic performance of lithium ion battery.
Detailed description of the invention
Fig. 1 is embodiment 4 and the cycle-index-capacity retention ratio contrast curve chart at 45 DEG C of comparative example 1；
Fig. 2 is embodiment 5 and SOC-DCR (state-of-charge-DC internal resistance) contrast curve chart at 25 DEG C of comparative example 2；
Fig. 3 is embodiment 6 and the difference discharge-rate-capacity retention ratio contrast curve chart at 25 DEG C of comparative example 3.
Specific embodiment
Embodiment 1
A kind of preparation method of carbon nanotube, comprising the following steps:
1) carbon nanotube crude samples are made with catalystic pyrolysis.
Catalystic pyrolysis specifically: carbon source material propylene diluted by nitrogen after [with n (N2):(C3H6)=6:1 carries out dilute
Release], mixed gas enters reactor with the flow velocity of 0.09mL/s, makes Fe-Mo-Al at 700 DEG C2O3Catalyst is in troupe's stream
Change state, mixed gas come into full contact with catalyst, and propylene cracks the carbon deposited on a catalyst, and to be grown to carbon nanotube thick
Sample.
2) with the HNO of 0.8~1.5mol/L3Solution carries out pickling to carbon nanotube crude samples.
In the present embodiment, with the HNO of 1mol/L3Solution carries out pickling to carbon nanotube crude samples, can be by carbon nanotube
Fe-Mo-Al on crude samples2O3Metallic catalyst removal.
3) high-temperature process is carried out to the carbon nanotube crude samples after pickling with high-temperature roasting furnace, obtains carbon nanotube.
Wherein, high-temperature temperature is 1900 DEG C, calcining time 2.5h, and vacuum degree is 90Pa in the furnace of high-temperature roasting furnace, from
And guarantee that carbon nanotube will not be oxidized and lose.
A kind of combined conductive agent, each component including following mass percent:
Carbon nanotube 0.3%；Ketjen black 1%；Dispersing agent 0.7%；Solvent 98%.Wherein, carbon nanotube is the above method
The carbon nanotube of preparation, dispersing agent are polyvinylpyrrolidone, and solvent is N-Methyl pyrrolidone.
A kind of preparation method of combined conductive agent, comprising the following steps:
1) according to formula ratio, the composite powder of carbon nanotube and one-dimensional electric agent is made of hydro-thermal method.
Wherein, hydro-thermal method specifically: one-dimensional electric agent and deionized water are added in water heating kettle, stirs 15min at room temperature,
Be added carbon nanotube after continue that 20min is stirred at room temperature, after stir 3h at 180 DEG C, obtained product cooled to room temperature, warp
After being filtered, washed, drying, be put into tube furnace, be warming up to 500 DEG C, constant temperature 2.5h in a nitrogen atmosphere, after be cooled to room
Composite powder can be obtained in temperature.
2) composite powder is added in solvent, after dispersing agent is added in solvent, obtain mixture.
3) mixture is subjected to ultrasonic disperse, combined conductive agent can be obtained.
Wherein, the dispersion frequency of ultrasonic disperse is 40~50Hz, and jitter time is 1~1.5h.In the present embodiment, dispersion frequency
Rate is 40Hz, jitter time 1h.
Embodiment 2
A kind of preparation method of carbon nanotube, comprising the following steps:
1) carbon nanotube crude samples are made with catalystic pyrolysis.
Catalystic pyrolysis specifically: [n (N after carbon source material propylene is diluted by nitrogen2):(C3H6)=6:1], mixed gas
Enter reactor with the flow velocity of 0.09mL/s, makes Fe-Mo-Al at 700 DEG C2O3Catalyst is in troupe's fluidized state, gaseous mixture
Body comes into full contact with catalyst, and propylene cracks the carbon deposited on a catalyst and is grown to carbon nanotube crude samples.
2) HNO of 1.2mol/L is used3Solution carries out pickling to carbon nanotube crude samples.
3) high-temperature process is carried out to the carbon nanotube crude samples after pickling with high-temperature roasting furnace, obtains carbon nanotube.
Wherein, high-temperature temperature is 1800 DEG C, calcining time 3h, and vacuum degree is 80Pa in the furnace of high-temperature roasting furnace, thus
Guarantee that carbon nanotube will not be oxidized and lose.
A kind of combined conductive agent, each component including following mass percent:
Carbon nanotube 0.25%；Conductive black 1.5%；Dispersing agent 0.8%；Solvent 97.45%.Wherein, carbon nanotube is
The carbon nanotube of above method preparation, dispersing agent is polyvinylpyrrolidone, and solvent is N-Methyl pyrrolidone.
A kind of preparation method of combined conductive agent, comprising the following steps:
1) according to formula ratio, the composite powder of carbon nanotube and one-dimensional electric agent is made of hydro-thermal method.
Wherein, hydro-thermal method specifically: one-dimensional electric agent and deionized water are added in water heating kettle, stirs 20min at room temperature,
Be added carbon nanotube after continue that 25min is stirred at room temperature, after stir 3.5h at 190 DEG C, obtained product cooled to room temperature,
After being filtered, washed, drying, be put into tube furnace, be warming up to 600 DEG C, constant temperature 2h in a nitrogen atmosphere, after be cooled to room
Composite powder can be obtained in temperature.
2) composite powder is added in solvent, after dispersing agent is added in solvent, obtain mixture.
3) mixture is subjected to ultrasonic disperse, combined conductive agent can be obtained.
Wherein, the dispersion frequency of ultrasonic disperse is 40~50Hz, and jitter time is 1~1.5h.In the present embodiment, dispersion frequency
Rate is 50Hz, jitter time 1.5h.
Embodiment 3
A kind of preparation method of carbon nanotube, comprising the following steps:
1) carbon nanotube crude samples are made with catalystic pyrolysis.
Catalystic pyrolysis specifically: [n (N after carbon source material propylene is diluted by nitrogen2):(C3H6)=6:1], mixed gas
Enter reactor with the flow velocity of 0.09mL/s, makes Fe-Mo-Al at 700 DEG C2O3Catalyst is in troupe's fluidized state, gaseous mixture
Body comes into full contact with catalyst, and propylene cracks the carbon deposited on a catalyst and is grown to carbon nanotube crude samples.
2) HNO of 1.5mol/L is used3Solution carries out pickling to carbon nanotube crude samples.
3) high-temperature process is carried out to the carbon nanotube crude samples after pickling with high-temperature roasting furnace, obtains carbon nanotube.
Wherein, high-temperature temperature is 1900 DEG C, calcining time 3h, and vacuum degree is 85Pa in the furnace of high-temperature roasting furnace, thus
Guarantee that carbon nanotube will not be oxidized and lose.
A kind of combined conductive agent, each component including following mass percent:
Carbon nanotube 0.35%；Electrically conductive graphite 1.5%；Dispersing agent 0.9%；Solvent 97.25%.Wherein, carbon nanotube is
The carbon nanotube of above method preparation, dispersing agent is polyvinylpyrrolidone, and solvent is N-Methyl pyrrolidone.
A kind of preparation method of combined conductive agent, comprising the following steps:
1) according to formula ratio, the composite powder of carbon nanotube and one-dimensional electric agent is made of hydro-thermal method.
Wherein, hydro-thermal method specifically: one-dimensional electric agent and deionized water are added in water heating kettle, stirs 20min at room temperature,
Be added carbon nanotube after continue that 25min is stirred at room temperature, after stir 3.5h at 185 DEG C, obtained product cooled to room temperature,
After being filtered, washed, drying, be put into tube furnace, be warming up to 500 DEG C, constant temperature 3h in a nitrogen atmosphere, after be cooled to room
Composite powder can be obtained in temperature.
2) composite powder is added in solvent, after dispersing agent is added in solvent, obtain mixture.
3) mixture is subjected to ultrasonic disperse, combined conductive agent can be obtained.
Wherein, the dispersion frequency of ultrasonic disperse is 40~50Hz, and jitter time is 1~1.5h.In the present embodiment, dispersion frequency
Rate is 40Hz, jitter time 1.2h.
Embodiment 4
The combined conductive agent that embodiment 1 is obtained, using anode formula, ternary material NCM523:PVDF: combined conductive agent
Three's mass percent is 98.3%:1%:0.7%, and soft-package battery is made.
Embodiment 5
The combined conductive agent that embodiment 2 is obtained, using anode formula, ternary material NCM811:PVDF: combined conductive agent
Three's mass percent is 98.4%:1%:0.6%, and soft-package battery is made.
Embodiment 6
The combined conductive agent that embodiment 1 is obtained, using anode formula, LiFePO4: PVDF: combined conductive agent three's matter
Amount percentage is 98%:1%:1%, and soft-package battery is made.
Comparative example 1
By commercially available Shenzhen three along CNTs10 (N) carbon nanotube of nanometer company, new material limited liability company, using just
Pole formula, ternary material NCM523:PVDF:CNTs10 (N) three's mass percent are 98.3%:1%:0.7%, and Soft Roll is made
Battery.
Comparative example 2
By commercially available Shenzhen three along CNTs10 (N) carbon nanotube of nanometer company, new material limited liability company, using just
Pole formula, ternary material NCM811:PVDF:CNTs10 (N) three's mass percent are 98.3%:1%:0.7%, and Soft Roll is made
Battery.Comparative example of this comparative example as embodiment 5.
Comparative example 3
By commercially available Shenzhen three along CNTs10 (N) carbon nanotube of nanometer company, new material limited liability company, using just
Pole formula, LiFePO4: PVDF:CNTs10 (N) three's mass percent is 98%:1%:1%, and soft-package battery is made.This is right
Comparative example of the ratio as embodiment 6.
Performance test
The soft-package battery that embodiment 4~6 and comparative example 1~3 are obtained carries out long-term loop test, at 25 DEG C respectively
HPPC (hybrid power pulse ability characteristics) test and multiplying power discharging property test, comparative example 4 are followed for a long time with comparative example 1
Ring test, embodiment 5 and the DC internal resistance of comparative example 2 and the multiplying power discharging property test result of embodiment 6 and comparative example 3,
Test result is as shown in FIG. 1 to 3.
By FIG. 1 to FIG. 3 it is found that combined conductive agent produced by the present invention, after being added in lithium ion cell electrode, Neng Gouming
The aobvious high temperature cyclic performance for improving battery, this is because carbon nanotube and one-dimensional electric agent are covered on positive electrode with reticular structure
On surface, the internal resistance of cell is can be significantly reduced in the Joint of Line and Dot of combined conductive agent and positive electrode, can be obviously improved charge and discharge
High rate performance enhances lithium ion battery service life cycle.
Claims (10)
1. a kind of combined conductive agent, which is characterized in that each component including following mass percent:
2. a kind of combined conductive agent according to claim 1, which is characterized in that the dispersing agent is polyvinylpyrrolidine
Ketone.
3. a kind of combined conductive agent according to claim 1, which is characterized in that the solvent is N-Methyl pyrrolidone.
4. a kind of combined conductive agent according to claim 1, which is characterized in that the carbon nanotube is by following preparation method
It is made: carbon nanotube crude samples is made with catalystic pyrolysis, with the HNO of 0.8~1.5mol/L3Solution is to carbon nanotube crude samples
Carry out pickling, after with high-temperature roasting furnace high-temperature process is carried out to the carbon nanotube crude samples after pickling, obtain carbon nanotube.
5. a kind of combined conductive agent according to claim 1, which is characterized in that the one-dimensional electric agent is Ketjen black, leads
Electric carbon black or electrically conductive graphite.
6. a kind of preparation method of combined conductive agent described in claim 1, which comprises the following steps:
1) according to formula ratio, the composite powder of carbon nanotube and one-dimensional electric agent is made of hydro-thermal method；
2) composite powder is added in solvent, after dispersing agent is added in solvent, obtain mixture；
3) mixture is subjected to ultrasonic disperse, combined conductive agent can be obtained.
7. a kind of preparation method of combined conductive agent according to claim 6, which is characterized in that in step 1), hydro-thermal method
Specifically: one-dimensional electric agent and deionized water are added in water heating kettle, stirs 10~20min at room temperature, after carbon nanotube is added
Continue that 20~30min is stirred at room temperature, after 3~4h is stirred at 180~200 DEG C, obtained product is cooled to room temperature, passed through
Filter, washing, it is dry after, be put into tube furnace, be warming up to 500~600 DEG C, 2~3h of constant temperature in a nitrogen atmosphere, after be cooled to room
Composite powder can be obtained in temperature.
8. a kind of preparation method of combined conductive agent according to claim 6, which is characterized in that in step 3), ultrasound point
Scattered dispersion frequency is 40~50Hz, and jitter time is 1~1.5h.
9. a kind of preparation method of combined conductive agent according to claim 6, which is characterized in that dispersing agent is polyethylene pyrrole
Pyrrolidone, solvent are N-Methyl pyrrolidone.
10. a kind of preparation method of carbon nanotube, which comprises the following steps:
1) carbon nanotube crude samples are made with catalystic pyrolysis；
2) with the HNO of 0.8~1.5mol/L3Solution carries out pickling to carbon nanotube crude samples；
3) high-temperature process is carried out to the carbon nanotube crude samples after pickling with high-temperature roasting furnace, obtains carbon nanotube.
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