CN110224121A - A kind of preparation method of anode sizing agent - Google Patents
A kind of preparation method of anode sizing agent Download PDFInfo
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- CN110224121A CN110224121A CN201910497120.XA CN201910497120A CN110224121A CN 110224121 A CN110224121 A CN 110224121A CN 201910497120 A CN201910497120 A CN 201910497120A CN 110224121 A CN110224121 A CN 110224121A
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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
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- 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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- H—ELECTRICITY
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- 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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- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- H—ELECTRICITY
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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
- H01M2004/028—Positive electrodes
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Abstract
The invention discloses a kind of preparation methods of anode sizing agent, include the following steps: the first step, Kynoar powder is put into blender, and N-Methyl pyrrolidone is added and is infiltrated；Combined conductive agent slurry is added in blender second step；Positive active material is added in third step；4th step adds N-Methyl pyrrolidone dilution mixing, ball milling, vacuum defoamation into mixture.Kynoar is soaked by existing, obtain wetting glue, pass through the addition of combined conductive agent slurry again, the addition of combined conductive agent slurry can effectively avoid conductive agent from reuniting with remaining substance, can effectively disperse each composition of slurry containing combined conductive agent and other positive materials；The auxiliary agent for not using any help combined conductive agent to disperse, reduces influence of the substance to battery performance of this analog assistant class；Meanwhile traditional carbon nanotube is replaced by using combined conductive agent, the electric conductivity of anode sizing agent can be effectively improved.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular, to a kind of preparation method of anode sizing agent.
Background technique
The preparation of slurry is the critical process of lithium ion battery production link, and the performance of electrode slurry is to lithium ion battery
Performance has important influence.Each component disperses to obtain uniformity in electrode slurry, directly affects the processing performance of pole piece, wherein mixing
Expect that technique is greater than 30% to the qualitative effects degree of product in the entire production technology of lithium ion battery, is in entire production technology
Most important link.In the electrode manufacture of lithium ion battery, anode and cathode slurry is essentially all by active material, polymer bonding
The composition such as agent, conductive agent.The mixing procedure of electrode slurry is probably divided into two kinds of (1) material by wet type mixing techniques, and basic process is first will
The substances such as binder, conductive agent are mixed, and active material is then added and is adequately dispersed with stirring, is eventually adding suitable
The adjustment that solvent carries out viscosity is measured, to be suitble to coating.This is current domestic prevailing technology.(2) dry mixing technique, basic mistake
Journey is active material, conductive agent and binder dry powder blend, and appropriate wet with solvent is added, and solvent high speed dispersion is added and is crushed, dilution
Adjust viscosity.
Currently, pulp of lithium ion battery can add dispersing aid in dispersion process, but the introducing of this kind of dispersing aid
Unpredictable negative effect may be brought to the performance of manufactured battery；Meanwhile the conductive agent base used in the prior art
This is common carbon nanotube, and the contact, the performance of formation conductive network with positive active material are strong not enough, and then reduce just
The electric conductivity of pole slurry.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of anode sizing agent, are moistened Kynoar by existing
It is wet, wetting glue is obtained, then pass through the addition of combined conductive agent slurry, the addition of combined conductive agent slurry can effectively avoid conductive agent
Reunite with remaining substance, can effectively disperse each composition of slurry containing combined conductive agent and other positive materials；It does not adopt
With the auxiliary agent of any help combined conductive agent dispersion, influence of the substance to battery performance of this analog assistant class is reduced；Meanwhile it is multiple
The electric conductivity of anode sizing agent can be effectively improved by closing conductive agent.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of anode sizing agent, includes the following steps:
Kynoar powder is put into blender by the first step, and N-Methyl pyrrolidone is added and is infiltrated, with 500-
The speed of 600r/min stirs 5-15min, the Kynoar powder soaked；
Combined conductive agent slurry is added in blender second step, stirs 5-10min with the speed of 150-200r/min；
Positive active material is added in third step, and first 300r/min stirs 30min, is then turned on blender kneading at this time pre-
Mixing stirs kneading 1-3h, stops stirring when there is the phenomenon that pole-climbing with mixing, obtains finely dispersed mixture；
4th step adds N-Methyl pyrrolidone dilution mixing into mixture, makes the solid content 66- of mixture
68%, be stirred 40min, then ultrasonic disperse 10min, be put into ball grinder, ball milling 3h, vacuum defoamation, obtain it is described just
Pole slurry.
Further, the mass ratio of the N-Methyl pyrrolidone and Kynoar that are added in the first step is 0.5-0.6:
1。
Further, the ratio between dosage of composite conducting slurry and Kynoar is 8-10mL:1g in second step.
Further, positive active material is LiMn2O4 in third step, and the additional amount of positive active material is polyvinylidene fluoride
7-9 times of alkene quality.
Further, the combined conductive agent slurry is made by the following method:
(1) it weighs 180mg silver nitrate and is mixed with 120mg graphene oxide and is dispersed in 240-260mL deionized water, ultrasound
2h, then weigh 90mg polyvinylpyrrolidone and be added in scattered graphene oxide-silver nitrate mixed solution, with ammonium hydroxide tune
The pH value of section system stirs evenly to 6-6.5, obtains premixed liquid；
(2) hydrazine hydrate is dissolved in 240-260mL deionized water, obtains reducing solution；
Wherein, the ratio between amount of substance of hydrazine hydrate and silver nitrate is 1.2-1.3:4；
It (3), will be also in 62-65 DEG C of water-bath after premixed liquid and reducing solution being separately heated to constant 62-65 DEG C of temperature
Stoste is slowly dropped in premixed liquid, after being added dropwise, is stirred to react 115-120min, is obtained suspension；
(4) suspension is stood into 50-60min, is centrifugated 15min under 8000r/min revolving speed, removes supernatant liquid,
Then it is respectively washed 3 times with deionized water and dehydrated alcohol again, is dried in vacuo 12h at 60 DEG C, obtains combined conductive agent；
(5) it disperses combined conductive agent in N-Methyl pyrrolidone, being configured to mass fraction is the compound of 4.5%-8%
Conductive agent slurry.
Beneficial effects of the present invention:
The present invention is soaked Kynoar by existing, obtains wetting glue, then adding by combined conductive agent slurry
Enter, the addition of combined conductive agent slurry can effectively avoid conductive agent from reuniting with remaining substance, can effectively disperse containing multiple
Close each composition of conductive agent slurry and other positive materials；The auxiliary agent for not using any help combined conductive agent to disperse, reduces
Influence of the substance of this analog assistant class to battery performance；
The combined conductive agent that the present invention uses, under the reduction of hydrazine hydrate, silver nitrate reduction at Ag nano particles simultaneously
It is deposited on graphene sheet layer, obtains nanometer Ag-graphene combined conductive agent；Meanwhile graphene oxide going back in hydrazine hydrate
Under original work are used, the oxygen-containing group in lamella is reduced, and a large amount of oxygen-containing functional group in surface is removed, and obtains the graphite of sheet
Alkene, flake graphite alkene are conducive to its coming into full contact with nano Ag particles；When combined conductive agent is filled into matrix, a side
Face, the graphene base body of lamellar structure can guarantee the face contact between combined conductive agent powder and positive active material；Another party
Face, the nano silver particles in composite powder can be filled the gap between positive active material, increase the contact between conductive phase, make
It obtains and forms more perfect conductive network between conductive phase, the conduction efficiency of electronics is increased, to improve leading for anode sizing agent
Electrical property.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiment obtained without creative efforts belongs to what the present invention protected
Range.
A kind of preparation method of anode sizing agent, includes the following steps:
Kynoar powder is put into blender by the first step, and N-Methyl pyrrolidone is added and is infiltrated, with 500-
The speed of 600r/min stirs 5-15min, the Kynoar powder soaked；
Wherein, the mass ratio of the N-Methyl pyrrolidone and Kynoar of addition is 0.5-0.6:1；
Combined conductive agent slurry is added in blender second step, stirs 5-10min with the speed of 150-200r/min；
The ratio between dosage of composite conducting slurry and Kynoar is 8-10mL:1g；
Positive active material is added in third step, and first 300r/min stirs 30min, is then turned on blender kneading at this time pre-
Mixing stirs kneading 1-3h, stops stirring when there is the phenomenon that pole-climbing with mixing, obtains finely dispersed mixture；
Positive active material is LiMn2O4, and the additional amount of positive active material is 7-9 times of Kynoar quality；
4th step adds N-Methyl pyrrolidone dilution mixing into mixture, makes the solid content 66- of mixture
68%, be stirred 40min, then ultrasonic disperse 10min, be put into ball grinder, ball milling 3h, vacuum defoamation, obtain it is described just
Pole slurry；
The combined conductive agent slurry is made by the following method:
(1) it weighs 180mg silver nitrate and is mixed with 120mg graphene oxide and is dispersed in 240-260mL deionized water, ultrasound
2h, then weigh 90mg polyvinylpyrrolidone and be added in scattered graphene oxide/silver nitrate mixed solution, with ammonium hydroxide tune
The pH value of section system stirs evenly to 6-6.5, obtains premixed liquid；
(2) hydrazine hydrate (wherein, the ratio between amount of substance of hydrazine hydrate and silver nitrate is 1.2-1.3:4, slightly excessively) is molten
Solution obtains reducing solution in 240-260mL deionized water；
It (3), will be also in 62-65 DEG C of water-bath after premixed liquid and reducing solution being separately heated to constant 62-65 DEG C of temperature
Stoste is slowly dropped in premixed liquid, after being added dropwise, is stirred to react 115-120min, is obtained suspension；
(4) suspension is stood into 50-60min, is centrifugated 15min under 8000r/min revolving speed, removes supernatant liquid,
Then it is respectively washed 3 times with deionized water and dehydrated alcohol again, is dried in vacuo 12h at 60 DEG C, obtains combined conductive agent；
(5) it disperses combined conductive agent in N-Methyl pyrrolidone, being configured to mass fraction is the compound of 4.5%-8%
Conductive agent slurry；
Under the reduction of hydrazine hydrate, silver nitrate reduction is at Ag nano particles and is deposited on graphene sheet layer, obtains
Nanometer Ag-graphene combined conductive agent；Meanwhile oxygen-containing group of the graphene oxide under the reduction of hydrazine hydrate, in lamella
Group is reduced, and a large amount of oxygen-containing functional group in surface is removed, and obtains the graphene of sheet, flake graphite alkene is conducive to it and receives
Rice Ag particle comes into full contact with；When combined conductive agent is filled into matrix, on the one hand, the graphene base body of lamellar structure can protect
Demonstrate,prove the face contact between combined conductive agent powder and positive active material；On the other hand, the nano silver particles in composite powder can
The gap between positive active material is filled, increases the contact between conductive phase, so that being formed between conductive phase more perfect
Conductive network, increases the conduction efficiency of electronics, to improve the electric conductivity of anode sizing agent.
Embodiment 1
Combined conductive agent slurry is made by the following method:
(1) it weighs 180mg silver nitrate and is mixed with 120mg graphene oxide and is dispersed in 240mL deionized water, ultrasonic 2h,
90mg polyvinylpyrrolidone is weighed again to be added in scattered graphene oxide/silver nitrate mixed solution, is adjusted with ammonium hydroxide
The pH value of system stirs evenly to 6, obtains premixed liquid；
(2) hydrazine hydrate (wherein, the ratio between amount of substance of hydrazine hydrate and silver nitrate is 1.2:4, slightly excessively) is dissolved in
In 240mL deionized water, reducing solution is obtained；
(3) after premixed liquid and reducing solution being separately heated to constant 62 DEG C of temperature, reducing solution is delayed in 62 DEG C of water-baths
Slowly it is added drop-wise in premixed liquid, after being added dropwise, is stirred to react 115min, obtains suspension；
(4) suspension is stood into 50min, is centrifugated 15min under 8000r/min revolving speed, remove supernatant liquid, then
It is respectively washed 3 times with deionized water and dehydrated alcohol again, is dried in vacuo 12h at 60 DEG C, obtains combined conductive agent；
(5) it disperses combined conductive agent in N-Methyl pyrrolidone, is configured to the composite conducting that mass fraction is 4.5%
Agent slurry.
Embodiment 2
Combined conductive agent slurry is made by the following method:
(1) it weighs 180mg silver nitrate and is mixed with 120mg graphene oxide and is dispersed in 260mL deionized water, ultrasonic 2h,
90mg polyvinylpyrrolidone is weighed again to be added in scattered graphene oxide/silver nitrate mixed solution, is adjusted with ammonium hydroxide
The pH value of system stirs evenly to 6.5, obtains premixed liquid；
(2) hydrazine hydrate (wherein, the ratio between amount of substance of hydrazine hydrate and silver nitrate is 1.3:4, slightly excessively) is dissolved in
In 260mL deionized water, reducing solution is obtained；
(3) after premixed liquid and reducing solution being separately heated to constant 65 DEG C of temperature, reducing solution is delayed in 65 DEG C of water-baths
Slowly it is added drop-wise in premixed liquid, after being added dropwise, is stirred to react 120min, obtains suspension；
(4) suspension is stood into 60min, is centrifugated 15min under 8000r/min revolving speed, remove supernatant liquid, then
It is respectively washed 3 times with deionized water and dehydrated alcohol again, is dried in vacuo 12h at 60 DEG C, obtains combined conductive agent；
(5) it disperses combined conductive agent in N-Methyl pyrrolidone, is configured to the combined conductive agent that mass fraction is 8%
Slurry.
Comparative example 1
It disperses carbon nanotube in N-Methyl pyrrolidone, is configured to the carbon nano tube paste that mass fraction is 8%.
Embodiment 3
A kind of preparation method of anode sizing agent, includes the following steps:
Kynoar powder is put into blender by the first step, and N-Methyl pyrrolidone is added and is infiltrated, with
The speed of 500r/min stirs 5min, the Kynoar powder soaked；
Wherein, the mass ratio of the N-Methyl pyrrolidone and Kynoar of addition is 0.5:1；
Combined conductive agent slurry is added in blender second step, stirs 5min with the speed of 150r/min；
The ratio between dosage of composite conducting slurry and Kynoar is 8mL:1g；
Positive active material is added in third step, and first 300r/min stirs 30min, is then turned on blender kneading at this time pre-
Mixing stirs kneading 1h, stops stirring when there is the phenomenon that pole-climbing with mixing, obtains finely dispersed mixture；
Positive active material is LiMn2O4, and the additional amount of positive active material is 7 times of Kynoar quality；
4th step adds N-Methyl pyrrolidone dilution mixing into mixture, makes the solid content 66% of mixture, stirs
Mixing 40min is mixed, then ultrasonic disperse 10min, is put into ball grinder, ball milling 3h, and vacuum defoamation obtains the anode sizing agent.
Embodiment 4
A kind of preparation method of anode sizing agent, includes the following steps:
Kynoar powder is put into blender by the first step, and N-Methyl pyrrolidone is added and is infiltrated, with
The speed of 550r/min stirs 10min, the Kynoar powder soaked；
Wherein, the mass ratio of the N-Methyl pyrrolidone and Kynoar of addition is 0.55:1；
Combined conductive agent slurry is added in blender second step, stirs 8min with the speed of 180r/min；
The ratio between dosage of composite conducting slurry and Kynoar is 9mL:1g；
Positive active material is added in third step, and first 300r/min stirs 30min, is then turned on blender kneading at this time pre-
Mixing stirs kneading 2h, stops stirring when there is the phenomenon that pole-climbing with mixing, obtains finely dispersed mixture；
Positive active material is LiMn2O4, and the additional amount of positive active material is 8 times of Kynoar quality；
4th step adds N-Methyl pyrrolidone dilution mixing into mixture, makes the solid content 67% of mixture, stirs
Mixing 40min is mixed, then ultrasonic disperse 10min, is put into ball grinder, ball milling 3h, and vacuum defoamation obtains the anode sizing agent.
Embodiment 5
A kind of preparation method of anode sizing agent, includes the following steps:
Kynoar powder is put into blender by the first step, and N-Methyl pyrrolidone is added and is infiltrated, with
The speed of 600r/min stirs 15min, the Kynoar powder soaked；
Wherein, the mass ratio of the N-Methyl pyrrolidone and Kynoar of addition is 0.6:1；
Combined conductive agent slurry is added in blender second step, stirs 10min with the speed of 200r/min；
The ratio between dosage of composite conducting slurry and Kynoar is 10mL:1g；
Positive active material is added in third step, and first 300r/min stirs 30min, is then turned on blender kneading at this time pre-
Mixing stirs kneading 3h, stops stirring when there is the phenomenon that pole-climbing with mixing, obtains finely dispersed mixture；
Positive active material is LiMn2O4, and the additional amount of positive active material is 9 times of Kynoar quality；
4th step adds N-Methyl pyrrolidone dilution mixing into mixture, makes the solid content 68% of mixture, stirs
Mixing 40min is mixed, then ultrasonic disperse 10min, is put into ball grinder, ball milling 3h, and vacuum defoamation obtains the anode sizing agent.
Comparative example 2
Combined conductive agent in embodiment 3 is changed to carbon nano tube paste made from comparative example 1, remaining step is constant.
Following performance test is done to slurry made from embodiment 1-2 and comparative example 1:
Measure volume resistivity (10-5Ω·cm)；
It is found that the volume resistivity of slurry made from embodiment 1-2 is 1.82-1.85x10-5Ω·cm；Compared to comparison
Example 1, the combined conductive agent that the present invention uses have good conductive property.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (5)
1. a kind of preparation method of anode sizing agent, which comprises the steps of:
Kynoar powder is put into blender by the first step, and N-Methyl pyrrolidone is added and is infiltrated, with 500-
The speed of 600r/min stirs 5-15min, the Kynoar powder soaked；
Combined conductive agent slurry is added in blender second step, stirs 5-10min with the speed of 150-200r/min；
Positive active material is added in third step, and first 300r/min stirs 30min, is then turned on the premix of blender kneading at this time,
Kneading 1-3h is stirred, stops stirring when there is the phenomenon that pole-climbing with mixing, obtains finely dispersed mixture；
4th step adds N-Methyl pyrrolidone dilution mixing into mixture, makes the solid content 66-68% of mixture, stirs
Mixing 40min is mixed, then ultrasonic disperse 10min, is put into ball grinder, ball milling 3h, and vacuum defoamation obtains the anode sizing agent.
2. a kind of preparation method of anode sizing agent according to claim 1, which is characterized in that the N- first being added in the first step
The mass ratio of base pyrrolidones and Kynoar is 0.5-0.6:1.
3. a kind of preparation method of anode sizing agent according to claim 1, which is characterized in that composite guide plasma-based in second step
The ratio between material and the dosage of Kynoar are 8-10mL:1g.
4. a kind of preparation method of anode sizing agent according to claim 1, which is characterized in that positive electrode active material in third step
Matter is LiMn2O4, and the additional amount of positive active material is 7-9 times of Kynoar quality.
5. a kind of preparation method of anode sizing agent according to claim 1, which is characterized in that the combined conductive agent slurry
It is made by the following method:
(1) it weighs 180mg silver nitrate and is mixed with 120mg graphene oxide and is dispersed in 240-260mL deionized water, ultrasonic 2h,
90mg polyvinylpyrrolidone is weighed again to be added in scattered graphene oxide-silver nitrate mixed solution, is adjusted with ammonium hydroxide
The pH value of system stirs evenly to 6-6.5, obtains premixed liquid；
(2) hydrazine hydrate is dissolved in 240-260mL deionized water, obtains reducing solution；
Wherein, the ratio between amount of substance of hydrazine hydrate and silver nitrate is 1.2-1.3:4；
(3) after premixed liquid and reducing solution being separately heated to constant 62-65 DEG C of temperature, by reducing solution in 62-65 DEG C of water-bath
It is slowly dropped in premixed liquid, after being added dropwise, is stirred to react 115-120min, obtains suspension；
(4) suspension is stood into 50-60min, is centrifugated 15min under 8000r/min revolving speed, remove supernatant liquid, then
It is respectively washed 3 times with deionized water and dehydrated alcohol again, is dried in vacuo 12h at 60 DEG C, obtains combined conductive agent；
(5) it disperses combined conductive agent in N-Methyl pyrrolidone, is configured to the composite conducting that mass fraction is 4.5%-8%
Agent slurry.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111081984A (en) * | 2019-12-31 | 2020-04-28 | 东莞市沃泰通新能源有限公司 | Preparation method of battery slurry and battery slurry |
| CN111710868A (en) * | 2020-06-30 | 2020-09-25 | 昆山宝创新能源科技有限公司 | High-alkalinity anode slurry and preparation method and application thereof |
| CN112310370A (en) * | 2020-10-19 | 2021-02-02 | 浙江大学 | Graphene-based metal tin composite material of integrated conductive network and lithium battery cathode |
| CN114914451A (en) * | 2022-07-18 | 2022-08-16 | 江苏集萃分子工程研究院有限公司 | Preparation method of conductive material for lithium battery anode |
| CN115395035A (en) * | 2022-09-05 | 2022-11-25 | 嘉兴中科轻合金技术工程中心 | Water-activated magnesium primary battery and preparation process of positive electrode slurry thereof |
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