CN111162262A - Preparation method of high-rate lithium ion battery positive electrode slurry - Google Patents
Preparation method of high-rate lithium ion battery positive electrode slurry Download PDFInfo
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Abstract
The invention relates to the technical field of graphene, and discloses a preparation method of high-rate lithium ion battery anode slurry, which comprises the following steps: a. dissolving a binder in a solvent NMP, stirring and dispersing by double planets to prepare a viscose solution; b. adding the graphene dispersion liquid into the viscose solution, performing ball milling and mixing by using a planetary ball mill to obtain graphene viscose solution A, and sieving and storing the graphene viscose solution A; c. adding the carbon tube conductive slurry into part of the graphene adhesive liquid A, stirring and mixing by using a high-speed dispersion machine, and homogenizing by using a high-pressure homogenizer to obtain composite slurry B; d. adding the positive active substance into the composite slurry B twice, and stirring and dispersing by double planets to obtain slurry C; e. adding the residual graphene viscose solution A into the slurry C, stirring and dispersing by double planets to obtain a slurry D, adding a solvent NMP to adjust the viscosity, measuring the solid content, and filtering and defoaming in vacuum when the solid content meets the requirement to prepare the high-rate lithium ion battery slurry; the positive electrode slurry disclosed by the invention is uniformly dispersed, has good conductivity and is suitable for high-rate charge and discharge.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a preparation method of high-rate lithium ion battery slurry.
Background
Compared with the traditional energy supply mode based on fossil fuel, the appearance of the lithium battery breaks through the traditional carbon-based energy supply mode, reduces the carbon emission and provides a new path for sustainable development. Since the last 90 s, lithium batteries began to enter the market and became the power choice for electrical appliances and IT terminals. The lithium battery has smaller volume, more stable performance and better cyclicity, so that the lithium battery gradually spreads all aspects of daily life of people, and the lithium battery can help people to make an important step towards the cleaning world.
Nowadays, lithium ion batteries are more widely developed and applied, and face a few challenges, for example, in the actual use process of new lithium battery energy automobiles, there are still problems of low energy density, long charging time, low discharging power, etc., and the technological design of the lithium ion batteries needs to be continuously improved and continuous innovation in the field of new materials is required.
The preparation method of the ternary material lithium ion anode slurry commonly used at present comprises the following steps: mixing and stirring PVDF as a binder and NMP as a solvent to prepare a sticky solution, and then uniformly mixing and stirring nickel cobalt lithium manganate and a conductive agent (such as conductive carbon black, graphite, carbon fiber and the like) to prepare corresponding electrode slurry. The prior art uses wet mixing, and has the advantages that the adhesive solution is completely dissolved, and relatively uniform slurry can be obtained.
However, the conductive agent has different characteristics, conductivity and liquid absorption, has different combination degree with PVDF glue, is not easy to disperse uniformly, and cannot be mixed with the positive electrode material fully by one-time addition. Meanwhile, in order to reduce the resistance, the addition amount of the conductive agent is large, which is not favorable for the stability and uniformity of the positive electrode slurry and influences the gram volume performance.
Disclosure of Invention
The invention aims to provide a preparation method of a high-capacity and high-rate positive electrode conductive slurry of a nickel-cobalt-manganese ternary lithium battery, which solves the problems of uniformity and stability existing in the existing preparation method of a lithium ion positive electrode slurry, and improves the conductivity and the gram capacity.
The technical scheme of the invention is as follows:
a preparation method of high-rate lithium ion battery anode slurry comprises the following steps:
a. dissolving a binder in a solvent NMP, stirring and dispersing by double planets to prepare a viscose solution;
b. adding the graphene dispersion liquid into the viscose solution, performing ball milling and mixing by using an all-dimensional planetary ball mill to obtain graphene viscose solution A, and sieving and storing the graphene viscose solution A;
c. adding the carbon tube conductive slurry into part of the graphene adhesive liquid A, stirring and mixing by using a high-speed dispersion machine, and homogenizing by using a high-pressure homogenizer to obtain composite slurry B;
d. adding the positive active substance into the composite slurry B twice, and stirring and dispersing by double planets to obtain slurry C;
e. adding the residual graphene viscose solution A into the slurry C, stirring and dispersing by double planets to obtain a slurry D, adding a solvent NMP according to the material condition to adjust the viscosity and measure the solid content, and filtering and defoaming in vacuum when the solid content meets the requirement to prepare the high-rate lithium ion battery slurry.
Preferably, in the step a, the binder is polyvinylidene fluoride, and the solvent NMP is N-methylpyrrolidone; and d, taking the nickel cobalt lithium manganate as the positive active material in the step d.
Preferably, the graphene dispersion liquid in the step b comprises 3 parts of graphene and 97 parts of N-methyl pyrrolidone, the solid content of the graphene dispersion liquid is 1% -5%, the sheet diameter of graphene contained in the graphene dispersion liquid is 10-40um, and the thickness of graphene is 3-10 nm.
Preferably, the carbon tube conductive slurry in the step c comprises 3% -5% of a conductive agent, 1% -2% of a binder and 93% -96% of a solvent NMP, and the prepared carbon tube conductive slurry has a solid content of 4% -6%.
Preferably, the conductive agent comprises carbon nanotubes and graphene, wherein the content of the carbon nanotubes is 40-80%, and the content of the graphene is 20-60%; the diameter of the carbon nano tube is 5-20nm, and the length of the carbon tube is 5-20 um.
Preferably, the mass fraction of the positive electrode active material in the step d is 96-98%.
Preferably, the mass ratio of the viscose solution to the graphene dispersion liquid in the step b is 1.0:0.6-1.0, a planetary ball mill is used for mixing treatment, the forward rotation speed is 200-500rpm, and the time is 30 min; after pausing for 5min, reversing the operation speed to be 100-500rpm for 30min, and repeating the forward and reverse rotation operation for 3 times; during the operation, the vertical direction 360 is always keptoTipping bucket type turning at 5-10rpm, and ball milling medium is zirconia beads.
Preferably, the mass ratio of the graphene viscose liquid to the carbon tube conductive slurry in the step c is 1.0:0.8-1.2, a high-pressure homogenizer is used for dispersion treatment, the homogenization pressure is 1000-2000bar, and the circulation treatment is performed for 3-5 times.
Preferably, when the solvent is used for adjusting the viscosity in the step e, the stirring revolution speed is 10-20rpm, the rotation speed is 1000-1500rpm, the stirring time is 0.5h after each solvent addition, and then the solid content is measured until the solid content of the slurry reaches a set value of 62%, so that the high-rate lithium ion battery anode slurry is prepared.
Compared with the prior art, the invention has the beneficial effects that:
⑴ the conductive agent used in the application is carbon nano tube and graphene, the carbon nano tube has good electronic conductivity, the fibrous structure can form a continuous conductive network in the electrode active material, the graphene is conductive through point-surface contact, the liquid absorption capability is relatively weak and easy to disperse, the graphene and the carbon nano tube are compounded and matched to form a complete three-dimensional conductive network structure, compared with the traditional conductive agent such as conductive carbon black and the like, the conductive agent has higher electronic conductivity, the required dosage is relatively low, and the addition of the conductive agent is only 0.5-2%.
⑵ the application proposes that the graphene dispersion liquid and the viscose liquid are mixed by using an all-directional ball mill, the ball milling tank not only has revolution motion in the horizontal direction, but also has tipping bucket type turnover in the vertical direction, so that the materials are mixed more fully, and in addition, the ball milling mixing can process the materials with higher viscosity.
⑶ the application proposes that the carbon tube conductive slurry and the graphene dispersion liquid are homogenized, on one hand, the interlayer stripping of graphene can be more thorough, and the PVDF glue fully coats the graphene, on the other hand, the carbon tube and the graphene are mutually permeated and mixed in a high-pressure homogeneous state, so that a compact and uniform three-dimensional conductive network can be formed, after the composite slurry is mixed with the anode active material, the carbon nanotube can completely cover the anode active material due to the high surface area and the super-large length-diameter ratio of the carbon nanotube, so that a short-distance conductive network is realized, and the specific surface area of the anode material is improved, so that the anode material can absorb the electrolyte.
⑷ the graphene viscose is used for adjusting the viscosity of the anode slurry, the large-area coverage and flexibility of graphene build a long-range conductive network, the internal resistance of the anode piece is greatly reduced, and the high-magnification charge and discharge performance is facilitated.
⑸ this application uses graphite alkene and PVDF to glue and mixes, makes a graphite alkene adhesive, is favorable to the bonding of mass flow body and anodal thick liquids, guarantees simultaneously that graphite alkene network is connected with the mass flow body, improves anodal electron conductivity.
Drawings
FIG. 1 is a scanning electron microscope image of a high-magnification lithium ion battery anode slurry coated on an aluminum foil.
Detailed Description
The following describes the embodiment of the present invention in detail with reference to fig. 1.
The first embodiment is as follows:
a preparation method of high-rate lithium ion battery anode slurry comprises the following steps:
1. the preparation method comprises the following steps of (1) taking a multi-wall carbon nano tube as a conductive agent, polyvinylidene fluoride as a binder and N-methyl pyrrolidone as a solvent, wherein the three components are as follows: polyvinylidene fluoride: conductive agent = 94: 1: 5, preparing carbon tube conductive slurry; and preparing graphene dispersion liquid by taking 3 parts of graphene and 97 parts of N-methyl pyrrolidone.
2. Dissolving polyvinylidene fluoride in N-methyl pyrrolidone 13 times of the weight of polyvinylidene fluoride, dispersing at high speed for 4h under vacuum condition, stirring and revolving at 18rpm and dispersing at 1200rpm to obtain viscose liquid.
3. Adding the weighed graphene dispersion liquid and the viscose liquid with the same mass into a ball milling tank, putting 1.0mm of zirconia beads into the ball milling tank, and rotating forward at the speed of 300rpm for 30 min; after pausing for 5min, the operation speed is reversed again to 300rpm for 30min, and the forward and reverse rotation operations are repeated for 3 times. During the operation, the vertical direction 360 is always keptoTipping bucket type turnover, and the rotating speed is 5 rpm. And sieving for later use to obtain the graphene adhesive liquid A.
4. And weighing half of the graphene adhesive A, adding the carbon nano tube conductive slurry into the graphene adhesive A, and stirring the mixture for 30min under a vacuum condition at the stirring speed of 1500 rpm. And then using a high-pressure homogenizer for processing, wherein the homogenizing pressure is 1200bar, and circularly processing for 5 times to obtain the slurry B.
5. Adding an active substance of nickel cobalt lithium manganate into the slurry B twice, wherein the adding amount of the active substance of nickel cobalt lithium manganate is 50% of the total adding amount of the nickel cobalt lithium manganate for the first time, the revolution speed is 20rpm, and the stirring time is 0.5 h; and adding the rest of the nickel cobalt lithium manganate for the second time, wherein the revolution speed is 20rpm, the dispersion speed is 1300rpm, the stirring time is 3 hours, and the slurry C is prepared after the stirring is finished.
6. And adding the residual graphene adhesive A into the slurry C, stirring and dispersing for 3 hours in vacuum, wherein the stirring revolution speed is 25rpm, the dispersion speed is 1200rpm, and stirring is finished to obtain slurry D.
7. After stirring is finished, when the temperature of the slurry D is cooled to 25 ℃, the viscosity of the slurry is tested, N-methyl pyrrolidone is added according to a test result to adjust the viscosity, the solid content is measured, the stirring revolution speed is 10rpm after the addition, the dispersion speed is 1000rpm, the stirring time is 30min, the viscosity condition and the solid content of the adjusted slurry are required to be measured every time the viscosity is adjusted, and the high-rate lithium ion battery anode slurry is prepared until the solid content of the prepared slurry is 62%.
The slurry was applied to an aluminum foil and subjected to scanning electron microscopy, the scan being shown in FIG. 1.
Example two:
a preparation method of high-rate lithium ion battery anode slurry comprises the following steps:
1. the preparation method comprises the following steps of (1) taking a multi-wall carbon nano tube as a conductive agent, polyvinylidene fluoride as a binder and N-methyl pyrrolidone as a solvent, wherein the three components are as follows: polyvinylidene fluoride: conductive agent = 94: 1: 5, preparing carbon tube conductive slurry; and preparing graphene dispersion liquid by taking 3 parts of graphene and 97 parts of N-methyl pyrrolidone.
2. Dissolving polyvinylidene fluoride in N-methyl pyrrolidone 13 times of the weight of polyvinylidene fluoride, dispersing at high speed for 4h under vacuum condition, stirring and revolving at 18rpm and dispersing at 1200rpm to obtain viscose liquid.
3. Adding the weighed graphene dispersion liquid and the viscose liquid with the same mass into a ball milling tank, putting 1.0mm of zirconia beads into the ball milling tank, and rotating forward at the speed of 200rpm for 30 min; after pausing for 5min, the operation speed is reversed again to 100rpm for 30min, and the forward and reverse rotation operations are repeated for 3 times. During the operation, the vertical direction 360 is always keptoTipping bucket type turnover, and the rotating speed is 8 rpm. And sieving for later use to obtain the graphene adhesive liquid A.
4. And weighing half of the graphene adhesive A, adding the carbon nano tube conductive slurry into the graphene adhesive A, and stirring the mixture for 30min under a vacuum condition at the stirring speed of 1500 rpm. And then using a high-pressure homogenizer for processing, wherein the homogenizing pressure is 1000bar, and circularly processing for 5 times to obtain the slurry B.
5. Adding an active substance of nickel cobalt lithium manganate into the slurry B twice, wherein the adding amount of the active substance of nickel cobalt lithium manganate is 50% of the total adding amount of the nickel cobalt lithium manganate for the first time, the revolution speed is 20rpm, and the stirring time is 0.5 h; and adding the rest of the nickel cobalt lithium manganate for the second time, wherein the revolution speed is 20rpm, the dispersion speed is 1300rpm, the stirring time is 3 hours, and the slurry C is prepared after the stirring is finished.
6. And adding the residual graphene adhesive A into the slurry C, stirring and dispersing for 3 hours in vacuum, wherein the stirring revolution speed is 25rpm, the dispersion speed is 1000rpm, and stirring is finished to obtain slurry D.
7. After stirring is finished, when the temperature of the slurry D is cooled to 25 ℃, the viscosity of the slurry is tested, N-methyl pyrrolidone is added according to a test result to adjust the viscosity, the solid content is measured, the stirring revolution speed is 10rpm after the addition, the dispersion speed is 1200rpm, the stirring time is 30min, the viscosity condition and the solid content of the adjusted slurry are required to be measured every time the viscosity is adjusted, and the high-rate lithium ion battery anode slurry is prepared until the solid content of the prepared slurry is 62%.
Example three:
a preparation method of high-rate lithium ion battery anode slurry comprises the following steps:
1. the preparation method comprises the following steps of (1) taking a multi-wall carbon nano tube as a conductive agent, polyvinylidene fluoride as a binder and N-methyl pyrrolidone as a solvent, wherein the three components are as follows: polyvinylidene fluoride: conductive agent = 94: 1: 5, preparing carbon tube conductive slurry; and preparing graphene dispersion liquid by taking 3 parts of graphene and 97 parts of N-methyl pyrrolidone.
2. Dissolving polyvinylidene fluoride in N-methyl pyrrolidone 13 times of the weight of polyvinylidene fluoride, dispersing at high speed for 4h under vacuum condition, stirring and revolving at 18rpm and dispersing at 1200rpm to obtain viscose liquid.
3. Adding the weighed graphene dispersion liquid and the viscose liquid with the same mass into a ball milling tank, putting 1.0mm of zirconia beads into the ball milling tank, and rotating forward at the speed of 500rpm for 30 min; after pausing for 5min, the operation speed is reversed again to 500rpm for 30min, and the forward and reverse rotation operations are repeated for 3 times. During the operation, the vertical direction 360 is always keptoTipping bucket type turnover, and the rotating speed is 10 rpm. And sieving for later use to obtain the graphene adhesive liquid A.
4. And weighing half of the graphene adhesive A, adding the carbon nano tube conductive slurry into the graphene adhesive A, and stirring the mixture for 30min under a vacuum condition at the stirring speed of 1500 rpm. And then using a high-pressure homogenizer for processing, wherein the homogenizing pressure is 2000bar, and circularly processing for 5 times to obtain the slurry B.
5. Adding an active substance of nickel cobalt lithium manganate into the slurry B twice, wherein the adding amount of the active substance of nickel cobalt lithium manganate is 50% of the total adding amount of the nickel cobalt lithium manganate for the first time, the revolution speed is 10rpm, and the stirring time is 0.5 h; and adding the rest of nickel cobalt lithium manganate for the second time, wherein the revolution speed is 10rpm, the dispersion speed is 1500rpm, the stirring time is 3 hours, and the slurry C is prepared after the stirring is finished.
6. And adding the residual graphene adhesive A into the slurry C, stirring and dispersing for 3 hours in vacuum, wherein the stirring revolution speed is 25rpm, the dispersion speed is 1200rpm, and stirring is finished to obtain slurry D.
7. After stirring is finished, when the temperature of the slurry D is cooled to 25 ℃, the viscosity of the slurry is tested, N-methyl pyrrolidone is added according to a test result to adjust the viscosity, the solid content is measured, the stirring revolution speed is 10rpm after the addition, the dispersion speed is 2000rpm, the stirring time is 30min, the viscosity condition and the solid content of the adjusted slurry are required to be measured every time the viscosity is adjusted, and the high-rate lithium ion battery anode slurry is prepared until the solid content of the prepared slurry is 62%.
The foregoing is merely a preferred embodiment of the invention and all such equivalent alterations and permutations and derivations thereof are intended to be included within the scope of the invention.
Claims (9)
1. A preparation method of high-rate lithium ion battery anode slurry is characterized by comprising the following steps:
a. dissolving a binder in a solvent NMP, stirring and dispersing by double planets to prepare a viscose solution;
b. adding the graphene dispersion liquid into the viscose solution, performing ball milling and mixing by using an all-dimensional planetary ball mill to obtain graphene viscose solution A, and sieving and storing the graphene viscose solution A;
c. adding the carbon tube conductive slurry into part of the graphene adhesive liquid A, stirring and mixing by using a high-speed dispersion machine, and homogenizing by using a high-pressure homogenizer to obtain composite slurry B;
d. adding the positive active substance into the composite slurry B twice, and stirring and dispersing by double planets to obtain slurry C;
e. adding the residual graphene viscose solution A into the slurry C, stirring and dispersing by double planets to obtain a slurry D, adding a solvent NMP according to the material condition to adjust the viscosity and measure the solid content, and filtering and defoaming in vacuum when the solid content meets the requirement to obtain the high-rate lithium ion battery anode slurry.
2. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 1, characterized by comprising the following steps: in the step a, the binder is polyvinylidene fluoride, and the solvent NMP is N-methyl pyrrolidone; and d, taking the nickel cobalt lithium manganate as the positive active material in the step d.
3. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 1, characterized by comprising the following steps: the graphene dispersion liquid in the step b comprises 3 parts of graphene and 97 parts of N-methyl pyrrolidone, the solid content of the graphene dispersion liquid is 1% -5%, the sheet diameter of graphene contained in the graphene dispersion liquid is 10-40um, and the thickness of the graphene is 3-10 nm.
4. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 1, characterized by comprising the following steps: the carbon tube conductive slurry in the step c comprises 3-5% of conductive agent, 1-2% of binder and 93-96% of solvent NMP, and the prepared carbon tube conductive slurry contains 4-6% of solid.
5. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 4, characterized by comprising the following steps: the conductive agent comprises carbon nano tubes and graphene, wherein the content of the carbon nano tubes is 40-80%, and the content of the graphene is 20-60%; the diameter of the carbon nano tube is 5-20nm, and the length of the carbon tube is 5-20 um.
6. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 1, characterized by comprising the following steps: and d, the mass fraction of the positive active substance in the step d is 96-98%.
7. The high-rate lithium ion battery positive electrode slurry of claim 1The preparation method of the material is characterized by comprising the following steps: the mass ratio of the viscose solution to the graphene dispersion liquid in the step b is 1.0:0.6-1.0, a planetary ball mill is used for mixing treatment, the forward rotation speed is 200-500rpm, and the time is 30 min; after pausing for 5min, reversing the operation speed to be 100-500rpm for 30min, and repeating the forward and reverse rotation operation for 3 times; during the operation, the vertical direction 360 is always keptoTipping bucket type turning at 5-10rpm, and ball milling medium is zirconia beads.
8. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 1, characterized by comprising the following steps: and c, performing dispersion treatment by using a high-pressure homogenizer at the homogenizing pressure of 1000-2000bar, and performing circulation treatment for 3-5 times, wherein the mass ratio of the graphene viscose liquid to the carbon tube conductive slurry in the step c is 1.0: 0.8-1.2.
9. The preparation method of the high-rate lithium ion battery positive electrode slurry according to claim 1, characterized by comprising the following steps: and e, when the solvent is used for adjusting the viscosity in the step e, the stirring revolution speed is 10-20rpm, the rotation speed is 1000-1500rpm, the stirring time is 0.5h after the solvent is added each time, and then the solid content is measured until the solid content of the slurry reaches a set value of 62%, so that the high-rate lithium ion battery anode slurry is prepared.
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| CN112121660A (en) * | 2020-08-26 | 2020-12-25 | 风帆有限责任公司 | Method for preparing anode slurry of lithium ion battery |
| CN112234199A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery positive electrode plate |
| CN112271285A (en) * | 2020-11-02 | 2021-01-26 | 江西安驰新能源科技有限公司 | Preparation process of lithium ion battery anode slurry |
| CN112786828A (en) * | 2021-02-22 | 2021-05-11 | 宁波容百新能源科技股份有限公司 | Prussian positive plate with high compaction density and high rate performance, preparation method of prussian positive plate and sodium ion battery |
| CN114242992A (en) * | 2021-12-21 | 2022-03-25 | 深圳市和盈新能电子有限公司 | Preparation method of carbon-silicon negative electrode slurry, carbon-silicon negative electrode slurry and lithium ion battery |
| CN117039125A (en) * | 2023-08-10 | 2023-11-10 | 广东钠壹新能源科技有限公司 | Sodium ion battery, sodium ion battery anode slurry and preparation method thereof |
| WO2024179160A1 (en) * | 2023-02-27 | 2024-09-06 | 天能电池集团股份有限公司 | Preparation method for positive electrode slurry of solid-state battery, and positive electrode sheet and battery |
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