CN110676455A - Homogenizing process for nickel cobalt lithium manganate positive electrode material - Google Patents
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention discloses a homogenizing process of a nickel cobalt lithium manganate positive electrode material, and belongs to the technical field of lithium ion power batteries for new energy automobiles. A homogenating process of a nickel cobalt lithium manganate positive electrode material comprises the following steps: s1, preparing oily binder colloid; s2, drying the nickel cobalt lithium manganate positive electrode material, the solid additive and the conductive agent; s3, adding colloid, nickel cobalt lithium manganate positive electrode material, solid additive, conductive agent and oily solvent into a tank, and putting into a defoaming machine for mixing treatment to prepare slurry; s4, coating, baking, rolling and cutting the slurry to prepare a positive plate; and S5, assembling the positive plate, the negative plate, the diaphragm and the electrolyte into a battery, and then carrying out electrochemical performance test. The coating and calcining process in the traditional anode material preparation process is reduced by adding the solid additive in the slurry preparation process, the anode material preparation process is simplified, the production and manufacturing cost is reduced, and the prepared battery has good high-temperature performance and excellent cycle performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion power batteries for new energy automobiles, and particularly relates to a homogenizing process of a nickel cobalt lithium manganate positive electrode material.
Background
With the development of new energy automobiles, the power battery in China makes great progress. Wherein, the ternary material nickel cobalt lithium manganate (LiNi)xCoyMn1-x-yO2) The current positive electrode material system is the best choice for power batteries and is also considered as the future development trend.
The high nickel ternary material has a high proportion of nickel element and great advantages in energy density, and the high nickel low cobalt has become a future development trend in order to reduce the cost of the high nickel ternary material. However, with the increasing of the content of nickel, the thermal stability of the material is increasingly poor, so that the high-nickel ternary material has potential safety hazard.
At present, the safety of the high-nickel ternary material is mainly solved step by step through the modes of material modification optimization, surface coating, electrolyte adjustment and the like. For example, the structural stability, thermal stability, cycling stability, etc. of the material are improved by doping or coating with other metal elements (Al, Mg, Ti, Zr). However, it is difficult to achieve both of the cycle stability and the thermal stability by these modification means; meanwhile, the doping and coating process relates to a high-temperature calcination section; even some materials need 2-3 times of coating and calcining procedures, so that the cost is greatly increased, and the batch stability of the materials is poor.
Based on the prominent problems of poor cycle performance and poor thermal stability of the high-nickel ternary material, the invention develops the lithium nickel cobalt manganese oxide positive electrode material homogenizing process, and the problems are solved by adding the solid additive in the homogenizing process.
Disclosure of Invention
Based on the existing problems, the invention provides the homogenizing process of the nickel cobalt lithium manganate positive electrode material, the solid additive is added in the homogenizing process to reduce the operation of the coating and calcining process of the positive electrode material, so that the manufacturing cost of the positive electrode material is reduced, the process has the advantages of simple operation, reduction of the firing period of the positive electrode material and great improvement of the production capacity.
The technical scheme adopted by the invention is as follows:
a homogenating process of a nickel cobalt lithium manganate positive electrode material comprises the following steps:
s1, placing the oily binder in a vacuum drying oven for constant-temperature drying, adding the dried oily binder into an oily solvent, stirring and dissolving in a glue beater, and preparing into colloid with the mass concentration of 2-10%;
s2, respectively placing the nickel cobalt lithium manganate positive electrode material, the solid additive and the conductive agent in a 120 ℃ drying oven for drying treatment for later use;
s3, sequentially adding the colloid, the nickel cobalt lithium manganate positive electrode material, the solid additive, the conductive agent and the oily solvent into a polytetrafluoroethylene tank, and then putting the polytetrafluoroethylene tank into a defoaming machine to mix for 15-25 min to obtain slurry;
s4, respectively carrying out coating, baking, rolling and cutting on the slurry to prepare a positive plate, and placing the positive plate in a glove box for later use;
and S5, assembling the positive plate, the negative plate, the diaphragm and the electrolyte into a battery, and then carrying out electrochemical performance test.
Further, the oily solvent is N-methylpyrrolidone.
Further, the oily binder is at least one of polyvinylidene fluoride, vinylidene fluoride/hexafluoropropylene copolymer, and vinylidene fluoride homopolymer/polyvinylidene fluoride copolymer.
Further, the solid additive is one or more of nanoscale solid matters or organic easily-soluble solid matters, preferably Al2O3、Al(PO3)3Or (NH)4)3PO4。
In particular, the solid additive may also be B2O3、ZrO、MgO、V2O5、SiO2、Y2O3、La(PO3)3、TiO2、Y(PO3)3、(NH4)3AlF6At least one of; the dosage of the solid additive is 0.02-2% of the mass of the nickel cobalt lithium manganate positive electrode material, preferably 0.02-0.12%.
Further, the conductive agent is at least one of SUPER-P, Ketjen black, acetylene black and Ks-6.
Further, the mass ratio of the nickel cobalt lithium manganate positive electrode material to the colloid to the conductive agent is as follows: 9-9.6: 0.2-0.5: 0.2 to 0.5.
Further, the solid content of the slurry is 45-65%.
Further, the general formula of the nickel cobalt lithium manganate positive electrode material is LiNixCoyMnzO2And x + y + z is 1.
Specifically, x is more than or equal to 0.5 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.2, and z is more than or equal to 0 and less than or equal to 0.2; preferably 0.8. ltoreq. x.ltoreq.1, 0. ltoreq. y.ltoreq.0.15, 0. ltoreq. z.ltoreq.0.15.
Further, the average particle size of the nickel cobalt lithium manganate positive electrode material is D50:4~12μm;DmaxLess than 35 μm; the specific surface area is 0.20-0.70 m2(ii)/g; free lithium is less than or equal to 1800 ppm; the pH value is 11.60-12.00.
Further, the baking temperature is 80-100 ℃, and the baking time is 12-36 hours; the rolling pressure is 4-10 MPa.
Specifically, the electrochemical performance test conditions are that the charge-discharge system of the button cell is as follows: 3.0-4.3V, and circulating for 0.5C/1.0C; the charging and discharging system of the full battery is as follows: 3.0-4.2V, 1.0C/1.0C in circulation, and the type of the full-cell is a 3Ah small-sized soft package cell.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: according to the invention, the solid additive is added in the homogenizing process of the battery anode material to reduce the operation times of the traditional coating and calcining process of the anode material, so that the cycle performance and the thermal stability of the anode material are improved, and the method is adapted to the existing battery homogenizing process and is simple and easy to operate; and the manufacturing cost and the sintering period of the anode material are further reduced, and the production capacity is greatly improved.
Drawings
FIG. 1 is a high-power scanning electron microscope image of a positive plate in example 2 (after modification);
FIG. 2 is a high-power scanning electron microscope image of the positive plate in example 3 (after modification);
FIG. 3 is a 45 ℃ high temperature cycle comparison graph of the positive electrode sheets (positive electrode materials) obtained in example 2 (after modification) and comparative example 2 (before modification);
fig. 4 is a 45 ℃ high temperature cycle comparison graph of the positive electrode sheet (positive electrode material) full cell (3Ah pouch cell) obtained in example 2 (after modification) and comparative example 2 (before modification).
Detailed Description
The embodiments of the present invention can be obtained by different substitutions in specific ranges based on the above technical solutions, and therefore, the following embodiments are only preferred embodiments of the embodiments, and any technical substitutions made by the above technical solutions are within the protection scope of the present invention.
Example 1
A homogenating process of a nickel cobalt lithium manganate positive electrode material comprises the following steps:
s1, placing the vinylidene fluoride/hexafluoropropylene copolymer in a vacuum drying oven for drying at a constant temperature of 110 ℃, adding the dried vinylidene fluoride/hexafluoropropylene copolymer into N-methyl pyrrolidone, stirring and dissolving in a glue beater, and preparing into colloid with the mass concentration of 2%;
s2, preparing LiNi of nickel cobalt lithium manganate anode material0.80Co0.10Mn0.10O2、Al2O3Respectively drying the nanoparticles and the Ks-6 in a 120 ℃ oven for later use;
s3, mixing the colloid with LiNi-Co-Mn acid lithium positive electrode material0.80Co0.10Mn0.10O2、Al2O3Sequentially adding the nano particles, Ks-6 and N-methylpyrrolidone into a polytetrafluoroethylene tank, putting the polytetrafluoroethylene tank into a defoaming machine, mixing at 800rpm for 15min to obtain slurry, and controlling the solid content of the slurry to be 55%; the Al is2O3The addition amount of the nano particles is LiNi which is a positive electrode material of nickel cobalt lithium manganate0.80Co0.10Mn0.10O20.02% of the mass; the nickel cobalt lithium manganate cathode material LiNi0.80Co0.10Mn0.10O2The adding mass ratio of the colloid to the Ks-6 is 9.5: 0.25: 0.25;
s4, uniformly coating the slurry on an aluminum foil, wherein the scale of a scraper is 20 microns, then placing the aluminum foil into a vacuum drying oven at 80 ℃ for baking for 36 hours, cutting the aluminum foil into a positive plate with the diameter of 14mm through tabletting, rolling at 4MPa and punching after drying, and placing the positive plate into a glove box for later use;
and S5, according to the negative electrode shell and the lithium sheet, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and celgard 2500 diaphragm are dripped into the needle cylinder, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and the positive electrode sheet are dripped into the needle cylinder, the button cell is assembled in a glove box filled with argon, and the assembled button cell is subjected to cycle performance test under the conditions of 3.0-4.3V, 0.5C/1.0C charging system and the ambient temperature of 45 ℃.
Wherein, the lithium nickel cobalt manganese oxide positive electrode material LiNi0.80Co0.10Mn0.10O2Average particle diameter of D50:10.5μm;DmaxLess than 35 μm; the specific surface area is 0.2m2(ii)/g; free lithium is 1350 ppm; the pH was 11.60.
Example 2
A homogenating process of a nickel cobalt lithium manganate positive electrode material comprises the following steps:
s1, placing polyvinylidene fluoride into a vacuum drying oven for drying at a constant temperature of 110 ℃, adding the dried polyvinylidene fluoride into N-methyl pyrrolidone, stirring and dissolving in a glue-making machine, and preparing into colloid with a mass concentration of 5%;
s2, preparing LiNi of nickel cobalt lithium manganate anode material0.83Co0.12Mn0.05O2、Al(PO3)3Respectively drying the nano particles and the acetylene black in a 120 ℃ oven for later use;
s3, mixing the colloid with LiNi-Co-Mn acid lithium positive electrode material0.83Co0.12Mn0.05O2、Al(PO3)3Sequentially adding the nano particles, acetylene black and N-methyl pyrrolidone into a polytetrafluoroethylene tank, putting the polytetrafluoroethylene tank into a defoaming machine, mixing at 800rpm for 25min to obtain slurry, and controlling the solid content of the slurry to be 45%; the Al (PO)3)3The addition amount of the nano particles is LiNi which is a positive electrode material of nickel cobalt lithium manganate0.83Co0.12Mn0.05O20.06% of the mass; the nickel cobalt lithium manganate cathode material LiNi0.83Co0.12Mn0.05O2The mass ratio of the colloid to the acetylene black is 9.0: 0.5: 0.5;
s4, uniformly coating the slurry on an aluminum foil, wherein the scale of a scraper is 20 microns, then putting the aluminum foil into a vacuum drying oven at 100 ℃ for baking for 12 hours, cutting the aluminum foil into a positive plate with the diameter of 14mm through tabletting, 7MPa rolling and punching after drying, and putting the positive plate into a glove box for later use;
and S5, according to the negative electrode shell and the lithium sheet, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and celgard 2500 diaphragm are dripped into the needle cylinder, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and the positive electrode sheet are dripped into the needle cylinder, the button cell is assembled in a glove box filled with argon, and the assembled button cell is subjected to cycle performance test under the conditions of 3.0-4.3V, 0.5C/1.0C charging system and the ambient temperature of 45 ℃.
Wherein, the lithium nickel cobalt manganese oxide positive electrode material LiNi0.83Co0.12Mn0.05O2Average particle diameter of D50:12.0μm;DmaxLess than 35 μm; the specific surface area is 0.51m2(ii)/g; 1460ppm free lithium; the pH was 11.70.
Example 3
A homogenating process of a nickel cobalt lithium manganate positive electrode material comprises the following steps:
s1, placing polyvinylidene fluoride into a vacuum drying oven for drying at a constant temperature of 110 ℃, adding the dried polyvinylidene fluoride into N-methyl pyrrolidone, stirring and dissolving in a glue-making machine, and preparing into colloid with a mass concentration of 10%;
s2, preparing LiNi-Co lithium manganate (single crystal) anode material0.83Co0.12Mn0.05O2、(NH4)3PO4Respectively placing SUPER-P in an oven at 120 ℃ for drying for later use;
s3, mixing the colloid with LiNi-Co-Mn acid lithium (monocrystal) anode material LiNi0.83Co0.12Mn0.05O2、(NH4)3PO4Sequentially adding SUPER-P, N-methyl pyrrolidone into a polytetrafluoroethylene tank, putting the polytetrafluoroethylene tank into a defoaming machine, mixing at 800rpm for 20min to obtain slurry, and controlling the solid content of the slurry to be 65%; said (NH)4)3PO4The additive amount of the lithium nickel cobalt manganese oxide (single crystal) anode material LiNi0.83Co0.12Mn0.05O20.12% of the mass; the nickel cobalt lithium manganate (single crystal) cathode material LiNi0.83Co0.12Mn0.05O2The adding mass ratio of the colloid to the SUPER-P is 9.2: 0.4: 0.4;
s4, uniformly coating the slurry on an aluminum foil, wherein the scale of a scraper is 20 microns, then putting the aluminum foil into a vacuum drying oven at 90 ℃ for baking for 24 hours, cutting the aluminum foil into a positive plate with the diameter of 14mm through tabletting, rolling at 10MPa and punching after drying, and putting the positive plate into a glove box for later use;
and S5, according to the negative electrode shell and the lithium sheet, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and celgard 2500 diaphragm are dripped into the needle cylinder, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and the positive electrode sheet are dripped into the needle cylinder, the button cell is assembled in a glove box filled with argon, and the assembled button cell is subjected to cycle performance test under the conditions of 3.0-4.3V, 0.5C/1.0C charging system and the ambient temperature of 45 ℃.
Wherein the single crystal lithium nickel cobalt manganese oxide (single crystal) cathode material LiNi0.83Co0.12Mn0.05O2Average particle diameter of D50:4.6μm;DmaxLess than 15 μm; the specific surface area is 0.47m2(ii)/g; 1260ppm of free lithium; the pH was 11.65.
Example 4
A homogenating process of a nickel cobalt lithium manganate positive electrode material comprises the following steps:
s1, placing the vinylidene fluoride homopolymer/polyvinylidene fluoride copolymer in a vacuum drying oven for drying at a constant temperature of 110 ℃, adding the dried vinylidene fluoride homopolymer/polyvinylidene fluoride copolymer into N-methyl pyrrolidone, stirring and dissolving in a glue-making machine, and preparing into colloid with the mass concentration of 8%;
s2, preparing LiNi of nickel cobalt lithium manganate anode material0.90Co0.06Mn0.04O2、Al2O3Respectively drying the nano particles and the Keqin black in a 120 ℃ oven for later use;
s3, mixing the colloid with LiNi-Co-Mn acid lithium positive electrode material0.90Co0.06Mn0.04O2、Al2O3Sequentially adding the nano particles, the Ketjen black and the N-methyl pyrrolidone into a polytetrafluoroethylene tank, putting the polytetrafluoroethylene tank into a defoaming machine, mixing at 800rpm for 20min to obtain slurry, and controlling the solid content of the slurry to be 50%; the Al is2O3The addition amount of the nano particles is LiNi which is a positive electrode material of nickel cobalt lithium manganate0.90Co0.06Mn0.04O22% of the mass; the nickel cobalt lithium manganate cathode material LiNi0.90Co0.06Mn0.04O2The mass ratio of the colloid to the ketjen black is 9.6: 0.2: 0.2;
s4, uniformly coating the slurry on an aluminum foil, wherein the scale of a scraper is 20 microns, then putting the aluminum foil into a vacuum drying oven at 90 ℃ for baking for 24 hours, cutting the aluminum foil into a positive plate with the diameter of 14mm through tabletting, rolling at 8MPa and punching after drying, and putting the positive plate into a glove box for later use;
and S5, according to the negative electrode shell and the lithium sheet, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and celgard 2500 diaphragm are dripped into the needle cylinder, 3 drops of DEC/EC (volume ratio of 1:1) electrolyte and the positive electrode sheet are dripped into the needle cylinder, the button cell is assembled in a glove box filled with argon, and the assembled button cell is subjected to cycle performance test under the conditions of 3.0-4.3V, 0.5C/1.0C charging system and the ambient temperature of 45 ℃.
Wherein, the lithium nickel cobalt manganese oxide positive electrode material LiNi0.90Co0.06Mn0.04O2Average particle diameter of D50:10.7μm;DmaxLess than 35 μm; the specific surface area is 0.7m2(ii)/g; free lithium is 1800 ppm; the pH was 12.00.
Comparative example 1
Cells were prepared by homogenization in the same time period according to the procedure of example 1, except that the solid additive Al was not added2O3And (3) nanoparticles.
Comparative example 2
Cells were prepared by homogenization in the same time period according to the procedure of example 2, except that the solid additive Al (PO) was not added3)3And (3) nanoparticles.
Comparative example 3
Cells were prepared by homogenization in the same time period according to the procedure of example 3, except that no solid additive (NH) was added4)3PO4。
Comparative example 4
Cells were prepared by homogenization in the same time period according to the procedure of example 4, except that the solid additive Al was not added2O3And (3) nanoparticles.
The results of the relevant electrochemical performance tests on the batteries and positive electrode sheets (positive electrode materials) obtained in examples and comparative examples are shown in table 1 and fig. 1 to 4.
TABLE 1 test results of electrochemical Properties of each cell
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (10)
1. A homogenating process of a nickel cobalt lithium manganate positive electrode material is characterized by comprising the following steps:
s1, placing the oily binder in a vacuum drying oven for constant-temperature drying, adding the dried oily binder into an oily solvent, stirring and dissolving in a glue beater, and preparing into colloid with the mass concentration of 2-10%;
s2, respectively placing the nickel cobalt lithium manganate positive electrode material, the solid additive and the conductive agent in a 120 ℃ drying oven for drying treatment for later use;
s3, sequentially adding the colloid, the nickel cobalt lithium manganate positive electrode material, the solid additive, the conductive agent and the oily solvent into a polytetrafluoroethylene tank, and then putting the polytetrafluoroethylene tank into a defoaming machine to mix for 15-25 min to obtain slurry;
s4, respectively carrying out coating, baking, rolling and cutting on the slurry to prepare a positive plate, and placing the positive plate in a glove box for later use;
and S5, assembling the positive plate, the negative plate, the diaphragm and the electrolyte into a battery, and then carrying out electrochemical performance test.
2. The process for homogenizing a lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein the oily solvent is N-methylpyrrolidone.
3. The homogenizing process of the nickel cobalt lithium manganate positive electrode material as claimed in claim 1, wherein said oily binder is at least one of polyvinylidene fluoride, vinylidene fluoride/hexafluoropropylene copolymer, vinylidene fluoride homopolymer/polyvinylidene fluoride copolymer.
4. The homogenizing process of the nickel cobalt lithium manganate positive electrode material as claimed in claim 1, wherein the solid additive is one or more of nano-scale solid substance or organic easily-soluble solid substance, preferably Al2O3、Al(PO3)3Or (NH)4)3PO4。
5. The process for homogenizing a lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein the conductive agent is at least one of SUPER-P, Ketjen black, acetylene black and Ks-6.
6. The homogenating process of the lithium nickel cobalt manganese oxide positive electrode material of claim 1, wherein the mass ratio of the lithium nickel cobalt manganese oxide positive electrode material, the colloid and the conductive agent is as follows: 9-9.6: 0.2-0.5: 0.2 to 0.5.
7. The process for homogenizing a lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein the solid content of the slurry is 45-65%.
8. The homogenizing process of the lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein the general formula of the lithium nickel cobalt manganese oxide positive electrode material is LiNixCoyMnzO2And x + y + z is 1.
9. The homogenizing process of the nickel cobalt lithium manganate positive electrode material as set forth in claim 1, wherein the average particle diameter of the nickel cobalt lithium manganate positive electrode material is D50:4~12μm;DmaxLess than 35 μm; the specific surface area is 0.20-0.70 m2(ii)/g; free lithium is less than or equal to 1800 ppm; the pH value is 11.60-12.00.
10. The homogenating process of the nickel cobalt lithium manganate positive electrode material as set forth in claim 1, wherein the baking temperature is 80-100 ℃, and the baking time is 12-36 h; the rolling pressure is 4-10 MPa.
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CN112234188A (en) * | 2020-10-15 | 2021-01-15 | 四川虹微技术有限公司 | Preparation method of medium-high nickel ternary cathode material slurry |
CN114361378A (en) * | 2021-12-14 | 2022-04-15 | 宁德厦钨新能源材料有限公司 | Electrochemical performance detection method of ternary material |
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