CN114420895A - Method for preparing ternary positive electrode plate based on 3D printing technology - Google Patents
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for preparing a ternary positive electrode plate based on a 3D printing technology, which comprises the following steps of (1) mixing and grinding a ternary positive electrode material, a conductive agent and an adhesive, then adding a solvent, stirring until the mixture is uniformly mixed, and preparing viscous state slurry; (2) and (2) transferring the viscous state slurry obtained in the step (1) into a three-dimensional forming system, and performing electrode plate printing forming through spray deposition forming to prepare the electrode plate with the 3D structure. According to the method disclosed by the invention, the 3D printing technology is applied to the preparation of the ternary anode electrode plate, the 3D printing technology is adopted, and the structure of the electrode plate is optimized through the optimization of the preparation process of the ternary anode material and the optimization of parameters of a three-dimensional forming system and the like, so that the printing forming of a large-surface-area structure can be realized. Through the design of the electrode plate structure, the mass of the active substance in unit area is increased, and the energy density of the battery is improved under the condition of not losing power density.
Description
Technical Field
The invention relates to the field of preparation of ternary positive electrode plates, in particular to a method for preparing a ternary positive electrode plate based on a 3D printing technology.
Background
The traditional electrode scheme is an electrode coating process, and the coating amount of an electrode plate is difficult to control due to the fact that the viscoelastic properties of lithium ion battery slurry of different batches are different. The coating amount of the electrode plate is one of the most important parameters of the formed battery core, and if the coating amount of the electrode plate is not controlled well in the production process, the qualified rate of the electrode plate is inevitably reduced.
Because the traditional coating process can not ensure that all active materials participate in the charging and discharging process while increasing the thickness of the electrode plate, only the part of the surface contacting with the electrolyte can carry out the lithium ion de-intercalation process, the power density of the lithium ion battery is reduced to a great extent, and the thicker the active material is, the lower the power density is. Therefore, the conventional electrode coating process cannot satisfy the requirements of increasing the energy density without losing the power density at the same time. In addition, in the process of charging and discharging, as the deintercalation of the lithium ion battery progresses, the active material gradually detaches from the current collector, so that the cycle life is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for preparing a ternary positive electrode plate based on a 3D printing technology, which specifically comprises the following steps:
a method for preparing a ternary positive electrode plate based on a 3D printing technology comprises the following steps:
(1) mixing and grinding the ternary positive electrode material, the conductive agent and the adhesive, then adding the solvent, stirring until the mixture is uniformly mixed, and preparing viscous state slurry;
(2) transferring the viscous state slurry obtained by the configuration in the step (1) into a three-dimensional forming system, and setting the parameters of the system as follows: the spraying speed is 0.001-1mm/s, the scanning speed is 2-10mm/s, the layering thickness is 0.1-0.2mm, and the electrode plate is printed and formed through spraying deposition forming to prepare the electrode plate with the 3D structure.
Specifically, the conductive agent in the step (1) is one or more of acetylene black, 350G, carbon fiber, carbon nanotube and Ketjen black.
Specifically, the binder in the step (1) is one or more of polyvinylidene fluoride (PVDF) and sodium carboxymethyl cellulose (CMC).
Specifically, the solvent in the step (1) is one or more of N-methylpyrrolidone (NMP) and 1, 4-dioxane.
Specifically, the mass ratio of the ternary cathode material to the conductive agent to the adhesive in the step (1) is 8:1: 1.
Specifically, the stirring method in the step (1) is as follows: firstly stirring at the speed of 500 plus material 600r/min for 10-20min, then stirring at the speed of 200 plus material 300r/min for 10-20min, finally stirring at the speed of 600 plus material 700r/min for 20-30min, and finally taking out the materials to obtain the uniformly mixed slurry.
Specifically, the inner diameter of the nozzle of the three-dimensional forming system in the step (2) is 0.01 mm.
Specifically, the preparation method of the ternary cathode material comprises the following steps:
(a) preparing soluble nickel salt, cobalt salt and manganese salt into ternary liquid according to the molar ratio of nickel, cobalt and manganese being (5-8) to (1-2) to (1-3);
(b) preparing an ammonia water solution with the mass fraction of 1% -5%, and adding the ammonia water solution into a reaction kettle to serve as a reaction bottom solution;
(c) adding the ternary liquid into a reaction kettle, adding a hydroxide solution as a precipitator, keeping the temperature of a reaction system at 40-60 ℃, the pH at 10-12, stirring the reaction kettle at a stirring speed of 200-400r/min, stopping stirring after reacting for a period of time, standing and aging for a period of time, then carrying out solid-liquid separation, and drying the obtained precursor;
(d) crushing and grinding the dried precursor, mixing the lithium salt and the precursor powder according to a certain proportion, and grinding for 4-6 h;
(e) putting the ground powder into a heating furnace, heating the heating furnace to 500-550 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 4-6 h; then heating to 800-; and cooling to room temperature after heat preservation is finished to obtain the ternary cathode material.
Specifically, the hydroxide in the step (c) is sodium hydroxide; the drying treatment method comprises the following steps: and putting the obtained precursor into an oven for drying.
Specifically, the molar ratio of the lithium salt in the step (d) to the metal element in the precursor powder is Li (Ni + Co + Mn): 1-1.1): 1.
The invention has the beneficial effects that: according to the method disclosed by the invention, the 3D printing technology is applied to the preparation of the ternary anode electrode plate, the 3D printing technology is adopted, and the structure of the electrode plate is optimized through the optimization of the preparation process of the ternary anode material and the optimization of parameters of a three-dimensional forming system and the like, so that the printing forming of a large-surface-area structure can be realized. Through the design of the electrode plate structure, the mass of the active substance in unit area is increased, and the energy density of the battery is improved under the condition of not losing power density.
Detailed Description
The present invention will be described in detail with reference to the following embodiments. The embodiments shown below do not limit the inventive content described in the claims. The entire contents of the configurations shown in the following embodiments are not limited to those required as solutions of the inventions described in the claims.
A method for preparing a ternary positive electrode plate based on a 3D printing technology comprises the following steps:
(1) mixing and grinding the ternary positive electrode material, the conductive agent and the adhesive, then adding the solvent, stirring until the mixture is uniformly mixed, and preparing viscous state slurry;
(2) transferring the viscous state slurry obtained by the configuration in the step (1) into a three-dimensional forming system, and setting the parameters of the system as follows: the spraying speed is 0.001-1mm/s, the scanning speed is 2-10mm/s, the layering thickness is 0.1-0.2mm, and the electrode plate is printed and formed through spraying deposition forming to prepare the electrode plate with the 3D structure.
The conductive agent in the step (1) can be one or more of acetylene black, 350G, carbon fiber, carbon nano tube and Ketjen black; the adhesive can be one or more of polyvinylidene fluoride (PVDF) and sodium carboxymethyl cellulose (CMC); the solvent can be one or more of N-methyl pyrrolidone (NMP) and 1, 4-dioxane; the mass ratio of the ternary positive electrode material to the conductive agent to the adhesive is 8:1: 1; the stirring method comprises the following steps: firstly stirring at the speed of 500r/min, or 520r/min, or 550r/min, or 580r/min, or 600r/min for 10min, or 12min, or 16min, or 20min, then stirring at the speed of 200r/min, or 230r/min, or 250r/min, or 300r/min for 10min, or 12min, or 16min, or 20min, finally stirring at the speed of 600r/min, or 650r/min, or 700r/min for 20min, or 25min, or 28min, or 30min, and finally taking out the materials to obtain uniform slurry.
The inner diameter of the nozzle of the three-dimensional forming system in the step (2) is 0.01mm, the spraying speed can be 0.001mm/s, 0.01mm/s, 0.1mm/s, 0.5mm/s, 1mm/s and the like, the scanning speed can be 2mm/s, 5mm/s, 8mm/s, 10mm/s and the like, and the layered thickness can be 0.1mm, 0.15mm, 0.18mm, 0.2mm and the like.
The invention discloses a preparation method of a ternary cathode material used in a method for preparing a ternary cathode electrode plate based on a 3D printing technology, which comprises the following steps:
(a) preparing soluble nickel salt, cobalt salt and manganese salt into ternary liquid according to the molar ratio of nickel, cobalt and manganese being (5-8) to (1-2) to (1-3);
(b) preparing an ammonia water solution with the mass fraction of 1% -5%, and adding the ammonia water solution into a reaction kettle to serve as a reaction bottom solution;
(c) adding the ternary solution into a reaction kettle, adding a hydroxide solution as a precipitator, keeping the temperature of a reaction system at 40-60 ℃, the pH at 10-12, the stirring speed of the reaction kettle at 400r/min, maintaining the pH value of the solution at about 11, stopping stirring after reacting for a period of time, standing and aging for a period of time, then carrying out solid-liquid separation, and drying the obtained precursor;
(d) crushing and grinding the dried precursor, mixing the lithium salt and the precursor powder according to a certain proportion, and grinding for 4-6 h;
(e) putting the ground powder into a heating furnace, heating the heating furnace to 500-550 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 4-6 h; then heating to 800-; and cooling to room temperature after heat preservation is finished to obtain the ternary cathode material.
The molar ratio of the nickel, the cobalt and the manganese in the step (a) can be 8:1:1, or 5:2:3, or 6:2:2, or 7:1:2, and the like;
the mass concentration of the ammonia water solution in the step (b) can be 1%, 2%, 3%, 4%, 5% and the like;
the hydroxide in step (c) is sodium hydroxide; the temperature of the reaction system can be 40 ℃, or 50 ℃, or 55 ℃, or 60 ℃ and the like; the pH is about 10, 11 or 12; the stirring speed of the reaction kettle can be 200r/min, 300r/min, 350r/min, 400r/min and the like; the drying method comprises the following steps: putting the obtained precursor into an oven for drying;
in the step (d), the molar ratio of the lithium salt to the metal element in the precursor powder is Li (Ni + Co + Mn) 1:1, or 1.05:1, or 1.1:1, etc.; the grinding mode is ball milling, and the ball milling time can be 4h, or 5h, or 5.5h, or 6h and the like;
the heating rate in the step (e) can be 5 ℃/min, or 7 ℃/min, or 9 ℃/min, or 10 ℃/min, and the like; the temperature of the first heat preservation can be 500 ℃, or 520 ℃, or 535 ℃, or 550 ℃ and the like, and the time of the first heat preservation can be 4h, or 5h, or 5.5h, or 6h and the like; the temperature of the second heat preservation can be 800 ℃, 820 ℃, 835 ℃, 850 ℃ and the like, and the time of the second heat preservation can be 15h, 16h, 17h, 18h and the like.
Example 1:
step 1, preparing a nickel sulfate solution, a cobalt sulfate solution and a manganese sulfate solution according to the molar ratio of Ni to Co to Mn of 8 to 1 to prepare a ternary solution.
And 2, preparing an ammonia water solution with the mass fraction of 1% as a base solution. And (3) putting sodium hydroxide as a precipitator and the ternary solution into a reaction kettle, using nitrogen as protective gas, setting a mold temperature machine to be 55 ℃ for heat preservation, and setting the rotating speed of a stirring device of the reaction kettle to be 300 r/min. The pH of the solution was maintained at about 11. Standing and aging after the reaction is finished, carrying out solid-liquid separation by a centrifugal machine, and transferring the obtained precursor into a titanium oven for drying.
And 3, crushing and grinding the dried precursor, weighing a certain amount of lithium carbonate as a lithium source according to the molar ratio Li (Ni Co Mn) of 1.1:1, mixing the lithium carbonate with the precursor, then ball-milling and mixing the lithium carbonate and the precursor for 6 hours by using a ball mill to obtain uniformly mixed powder, and transferring the powder into a resistance heating tube furnace to carry out secondary temperature rise and solid phase formation. Firstly, heating to 500 ℃ at a heating rate of 10 ℃/min and preserving heat for 6 hours; then, the temperature was raised to 850 ℃ at the same temperature raising rate for 18 hours, followed by natural cooling to room temperature to prepare a desired sample.
Step 4, synthesizing the nickel cobalt lithium manganate (LiNiMnCoO)2) Mixing and grinding the active substance, conductive agent Keqin black and adhesive PVDF uniformly, then dripping a certain amount of NMP to prepare viscous state slurry, and adjusting the solid-to-liquid ratio to: sample, conductive agent and binder 8:1:1 to obtain slurry with certain viscosity, and stirring for 20min to obtain uniform slurry.
And 5, transferring the prepared slurry into a three-dimensional forming system, setting parameters of the system as a spraying speed (0.001mm/s), a scanning speed (2mm/s) and a layering thickness (0.1mm), setting the inner diameter of a nozzle to be 0.01mm, and carrying out electrode plate printing and forming through spraying deposition forming.
Example 2
Step 1, preparing a nickel sulfate solution, a cobalt sulfate solution and a manganese sulfate solution according to the molar ratio of Ni to Co to Mn of 5 to 2 to 3 to prepare a ternary solution.
And 2, preparing an ammonia water solution with the mass fraction of 5% as a base solution. And (3) putting sodium hydroxide as a precipitator and the ternary solution into a reaction kettle, using nitrogen as protective gas, setting a mold temperature machine to keep the temperature at 40 ℃, and setting the rotating speed of a stirring device of the reaction kettle at 200 r/min. The pH of the solution was maintained at about 10.5. Standing and aging after the reaction is finished, carrying out solid-liquid separation by a centrifugal machine, and transferring the obtained precursor into a titanium oven for drying.
And 3, crushing and grinding the dried precursor, weighing a certain amount of lithium carbonate as a lithium source according to the molar ratio Li (Ni Co Mn) of 1:1, mixing the lithium carbonate with the precursor, then carrying out ball milling and mixing for 4 hours by using a ball mill to obtain uniformly mixed powder, and transferring the powder into a resistance heating tube furnace to carry out secondary temperature rise and solid phase. Firstly, heating to 550 ℃ at the heating rate of 5 ℃/min and preserving heat for 4 hours; then, the temperature was raised to 800 ℃ at the same temperature raising rate for 15 hours, followed by natural cooling to room temperature to obtain the desired sample.
Step 4, synthesizing the nickel cobalt lithium manganate (LiNiMnCoO)2) Mixing and grinding the active substance, the conductive agent carbon nano tube and the binding agent CMC uniformly, then dripping a certain amount of 1, 4-dioxane to prepare viscous state slurry, and adjusting the solid-liquid ratio to be: the sample is conductive agent and adhesive agent is 8:1:1, mixed slurry is obtained, the mixed slurry is firstly stirred for 10-20min at the speed of 600r/min 500-.
And 5, transferring the prepared slurry into a three-dimensional forming system, setting parameters of the system as a spraying speed (1mm/s), a scanning speed (2mm/s) and a layering thickness (0.2mm), setting the inner diameter of a nozzle as 0.01mm, and carrying out electrode plate printing and forming through spraying deposition forming.
Example 3
Step 1, preparing a nickel sulfate solution, a cobalt sulfate solution and a manganese sulfate solution according to the molar ratio of Ni to Co to Mn of 6 to 2 to prepare a ternary solution.
And 2, preparing an ammonia water solution with the mass fraction of 2.5% as a base solution. And (3) putting sodium hydroxide as a precipitator and the ternary solution into a reaction kettle, using nitrogen as protective gas, setting a mold temperature machine to be 60 ℃ for heat preservation, and setting the rotating speed of a stirring device of the reaction kettle to be 400 r/min. The pH of the solution was maintained at about 11.5. Standing and aging after the reaction is finished, carrying out solid-liquid separation by a centrifugal machine, and transferring the obtained precursor into a titanium oven for drying.
And 3, crushing and grinding the dried precursor, weighing a certain amount of lithium carbonate as a lithium source according to the molar ratio Li (Ni Co Mn) of 1:1, mixing the lithium carbonate with the precursor, then carrying out ball milling and mixing for 4 hours by using a ball mill to obtain uniformly mixed powder, and transferring the powder into a resistance heating tube furnace to carry out secondary temperature rise and solid phase. Firstly, heating to 5250 ℃ at a heating rate of 8 ℃/min and preserving heat for 5 hours; the sample was then warmed up to 825 ℃ at the same rate for 17 hours, and then allowed to cool to room temperature to obtain the desired sample.
Step 4, synthesizing the nickel cobalt lithium manganate (LiNiMnCoO)2) Mixing and grinding the active substance, the conductive agent 350G and the binding agent CMC uniformly, then dripping a certain amount of NMP to prepare viscous state slurry, and adjusting the solid-to-liquid ratio to be: and (3) mixing a sample, namely a conductive agent and a binder, at a ratio of 8:1:1 to obtain mixed slurry, stirring at a speed of 600r/min for 15min, then stirring at a speed of 300r/min for 20min, and finally stirring at a speed of 700r/min for 30min to obtain uniform viscous-state slurry.
And 5, transferring the prepared slurry into a three-dimensional forming system, setting parameters of the system as a spraying speed (0.05mm/s), a scanning speed (5mm/s) and a layering thickness (0.15mm), setting the inner diameter of a nozzle to be 0.01mm, and carrying out electrode plate printing and forming through spraying deposition forming.
According to the method disclosed by the invention, the 3D printing technology is applied to the preparation of the ternary anode electrode plate, the 3D printing technology is adopted, and the structure of the electrode plate is optimized through the optimization of the preparation process of the ternary anode material and the optimization of parameters of a three-dimensional forming system and the like, so that the printing forming of a large-surface-area structure can be realized. Through the design of the electrode plate structure, the mass of the active substance in unit area is increased, and the energy density of the battery is improved under the condition of not losing power density.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for preparing a ternary positive electrode plate based on a 3D printing technology is characterized by comprising the following steps:
(1) mixing and grinding the ternary positive electrode material, the conductive agent and the adhesive, then adding the solvent, stirring until the mixture is uniformly mixed, and preparing viscous state slurry;
(2) transferring the viscous state slurry obtained by the configuration in the step (1) into a three-dimensional forming system, and setting the parameters of the system as follows: the spraying speed is 0.001-1mm/s, the scanning speed is 2-10mm/s, the layering thickness is 0.1-0.2mm, and the electrode plate is printed and formed through spraying deposition forming to prepare the electrode plate with the 3D structure.
2. The method for preparing the ternary positive electrode sheet based on the 3D printing technology according to claim 1, wherein the conductive agent in the step (1) is one or more of acetylene black, 350G, carbon fiber, carbon nanotube and Ketjen black.
3. The method for preparing the ternary positive electrode sheet based on the 3D printing technology is characterized in that the binder in the step (1) is one or more of polyvinylidene fluoride (PVDF) and sodium carboxymethylcellulose (CMC).
4. The method for preparing the ternary positive electrode sheet based on the 3D printing technology according to claim 1, wherein the solvent in the step (1) is one or more of N-methylpyrrolidone (NMP) and 1, 4-dioxane.
5. The method for preparing the ternary positive electrode plate based on the 3D printing technology as claimed in claim 1, wherein the mass ratio of the ternary positive electrode material to the conductive agent to the adhesive in step (1) is 8:1: 1.
6. The method for preparing the ternary positive electrode sheet based on the 3D printing technology according to claim 1, wherein the stirring method in the step (1) is as follows: firstly stirring at the speed of 500 plus material 600r/min for 10-20min, then stirring at the speed of 200 plus material 300r/min for 10-20min, finally stirring at the speed of 600 plus material 700r/min for 20-30min, and finally taking out the materials to obtain the uniformly mixed slurry.
7. The method for preparing the ternary positive electrode sheet based on the 3D printing technology as claimed in claim 1, wherein the inner diameter of the nozzle of the three-dimensional forming system in the step (2) is 0.01 mm.
8. The method for preparing the ternary positive electrode slice based on the 3D printing technology according to claim 1, wherein the preparation method of the ternary positive electrode material comprises the following steps:
(a) preparing soluble nickel salt, cobalt salt and manganese salt into ternary liquid according to the molar ratio of nickel, cobalt and manganese being (5-8) to (1-2) to (1-3);
(b) preparing an ammonia water solution with the mass fraction of 1% -5%, and adding the ammonia water solution into a reaction kettle to serve as a reaction bottom solution;
(c) adding the ternary liquid into a reaction kettle, adding a hydroxide solution as a precipitator, keeping the temperature of a reaction system at 40-60 ℃, the pH at 10-12, stirring the reaction kettle at a stirring speed of 200-400r/min, stopping stirring after reacting for a period of time, standing and aging for a period of time, then carrying out solid-liquid separation, and drying the obtained precursor;
(d) crushing and grinding the dried precursor, mixing the lithium salt and the precursor powder according to a certain proportion, and grinding for 4-6 h;
(e) putting the ground powder into a heating furnace, heating the heating furnace to 500-550 ℃ at the heating rate of 5-10 ℃/min, and preserving heat for 4-6 h; then heating to 800-; and cooling to room temperature after heat preservation is finished to obtain the ternary cathode material.
9. The method for preparing the ternary positive electrode sheet based on the 3D printing technology according to claim 8, wherein the hydroxide in the step (c) is sodium hydroxide; the drying treatment method comprises the following steps: and putting the obtained precursor into an oven for drying.
10. The method for preparing the ternary positive electrode sheet based on the 3D printing technology is characterized in that the molar ratio of the lithium salt in the step (D) to the metal elements in the precursor powder is Li (Ni + Co + Mn): 1-1.1: 1.
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