CN113060777A - Preparation method of high-compaction ternary single crystal material - Google Patents
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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 provides a preparation method of a high-compaction ternary single crystal material, which relates to the field of lithium battery anode materials and comprises the following steps: pre-oxidizing a precursor containing Ni, Co and Mn; uniformly mixing the precursor subjected to the pre-oxidation treatment with a lithium salt; carrying out primary sintering on the mixed materials in an oxygen atmosphere, wherein the temperature difference of the upper layer and the lower layer of a kiln is 0-30 ℃, the lower temperature of the upper layer and the lower layer is 800-950 ℃, the higher temperature of the upper layer and the lower layer is 805-980 ℃, the heating rate is 2-8 ℃/min, and the heat preservation time is 5-30 hours; adding a dopant and uniformly mixing; and (3) carrying out secondary sintering in an oxygen atmosphere, wherein the sintering temperature is as follows: the total sintering time is 10-25 hours at 300-600 ℃. The ternary single crystal material obtained by the preparation method has wider particle size distribution and high compaction density, and the preparation method has universality.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a lithium battery positive electrode material.
Background
Lithium batteries have the advantages of light weight, long life, and high energy density, and have been widely used in people's daily lives. With the continuous progress of materials/process technology, the performance of the lithium battery is continuously improved, and the core material which limits the energy density and the service life of the lithium battery is the anode material at present, so that the development of the anode material with high energy density and long service life is the key point of research and development.
The selection of the anode material of lithium battery is many, such as LiCoO2, LiMn2O4, LiFePO4, and ternary anode material, etc. The ternary cathode material secondary spherical particles are formed by agglomerating primary particles, and the size of the primary particles is generally hundreds of nanometers. And the particles of the single crystal ternary cathode material are all dispersed primary particles, and the particle size is generally below 5 microns. Compared with a secondary ball, the single crystal material has the advantages of good structural stability and high normal-temperature and high-temperature cycle performance.
In order to increase the energy density of lithium batteries, it is important to increase the compaction density as much as possible. However, the surface sphericity of the single crystal material is poor, and the particle size distribution is difficult to adjust, so that the compacted density is low, and finally, the energy density is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a high-compaction ternary single crystal material, and solves the technical problems of poor surface sphericity and difficult adjustment of particle size distribution of the ternary single crystal material.
In order to realize the aim, the invention provides a preparation method of a high-compaction ternary single crystal material, which comprises the following steps:
a. carrying out pre-oxidation treatment on a precursor containing Ni, Co and Mn at the temperature of 200-800 ℃, wherein the total time of the pre-treatment is 8-18 h;
b. uniformly mixing the pre-oxidized precursor with lithium salt, wherein the ratio of the total metal mole number in the precursor to the lithium metal mole number in the lithium salt is as follows: 1: 1.02-1.08;
c. carrying out primary sintering on the mixed materials in an oxygen atmosphere, wherein the temperature difference of the upper layer and the lower layer of a kiln is 0-30 ℃, the lower temperature of the upper layer and the lower layer is 800-950 ℃, the higher temperature of the upper layer and the lower layer is 805-980 ℃, the heating rate is 2-8 ℃/min, and the heat preservation time is 5-30 hours;
d. adding a doping agent into the materials after the first sintering, and uniformly mixing;
e. and (3) after the uniformly mixed materials are subjected to jet milling, carrying out secondary sintering, wherein the sintering temperature is as follows: the total sintering time is 10-25 h at 300-600 ℃.
Preferably, the temperature difference between the upper layer and the lower layer of the kiln is 10-25 ℃.
Further, the temperatures of the upper and lower layers in step c were 870 ℃ and 880 ℃, respectively.
Further, the temperatures of the lower layer and the upper layer in step c were 870 ℃ and 890 ℃, respectively.
Further, the temperatures of the upper and lower layers in step c were 870 ℃ and 895 ℃, respectively.
In the above synthesis method, the precursor is preferably nixcoymnz (oh)2 or NixCoyMnzCO3, x, y, and z are the number of moles of Ni, Co, and Mn, respectively, and x + y + z is 1.
In the synthesis method, the molar ratio of nickel, cobalt and manganese in the precursor is preferably 1: 1: 1 or 5-5.5: 1.5-2: 3 or 6 to 7.5: 0.5-2: 0.5 to 3.5. The molar ratio of Ni, Co and Mn is more preferably 6.3:0.8: 2.9.
In the above synthesis method, the lithium salt is preferably lithium carbonate or lithium hydroxide monohydrate.
Preferably, the dopant is one or multiple combinations of Zr, Al, Ti, Mg, Sr and the like.
According to the technical scheme, the precursor is subjected to preoxidation heat treatment, and the precursor can be subjected to dehydration, impurity removal and preoxidation so as to improve BET of the material and oxidize nickel into a high valence state, so that the material is easier to sinter. Under the same precursor, by adjusting the temperature difference of the temperatures of the upper layer and the lower layer of the kiln in the step c, the ternary single crystal material with different particle size distribution and high compaction density can be obtained.
Has the advantages that:
(1) the ternary single crystal material prepared by the method has wider particle size distribution.
(2) The ternary single crystal material prepared by the method has high compaction density which can reach 3.5-3.7 g/cc.
(3) The preparation method of the ternary single crystal material has universality and is suitable for preparation of ternary single crystal materials consisting of different nickel, cobalt and manganese.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer and more fully describe the technical solutions in the embodiments of the present invention, it is obvious that the described embodiments are a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and similar words are intended to mean that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
Aiming at the problems in the prior art, the embodiment of the invention provides a preparation method of a high-compaction ternary single crystal material.
Example 1:
the first step is as follows: ni precursor at 200 deg.c and in oxygen atmosphere0.63Co0.08Mn0.29(OH)2And carrying out pre-oxidation treatment for 18 hours.
The second step is that: and (3) mixing the pre-oxidized precursor with lithium carbonate according to the ratio of the metal mole number to the lithium metal mole number of 1: 1.05 mix well.
The third step: first sintering
Experimental groups: sintering the mixture for the first time in an oxygen atmosphere, wherein the upper layer temperature of a kiln is 870 ℃, and the lower layer temperature is: at 880 ℃, the heating speed is 2-8 ℃/min; preserving the heat for 20 hours;
reference group: sintering the mixture for the first time in an oxygen atmosphere, wherein the temperatures of the upper layer and the lower layer of the kiln are 875 ℃, and the heating rate is 2-8 ℃/min; and keeping the temperature for 20 hours.
The fourth step: adding aluminum hydroxide as a dopant in an amount of 0.2% (mass fraction) into the experimental group and the reference group after the first sintering, and mixing uniformly.
The fifth step: and (3) respectively carrying out secondary sintering on the mixture of the experimental group and the reference group after the doping agent is added in an oxygen atmosphere, wherein the secondary sintering temperature is 300 ℃, and the total sintering time is 25 hours.
The performance of the experimental group and the reference group after the five-step treatment is detected,
and (3) performance detection results:
the particle size distributions of the materials tested in the experimental and reference groups of this example are shown in table 1;
table 1:
| categories | D10 | D50 | D90 | D99 |
| Reference group | 1.63μm | 3.32μm | 6.42μm | 10.39μm |
| Experimental group | 1.10μm | 3.48μm | 7.56μm | 11.10μm |
The tap densities and capacities of the experimental group and the reference group of the present example were determined to be shown in table 2;
table 2:
testing the compaction density of the pole piece: the same areal density pole pieces (400g/m2) were prepared by mixing the reference and experimental materials with the binder (PVDF5130) and the conductive agent (Super P) respectively in the same proportions (main material: binder: conductive agent: 96.5: 1.5: 2), and the compaction densities were measured as in table 3:
table 3:
| categories | Compacted density g/cc |
| Reference group | 3.25 |
| Experimental group | 3.37 |
Example 2:
the first step is as follows: ni precursor at 600 deg.c and oxygen atmosphere0.33Co0.33Mn0.33CO3Carrying out pre-oxidation heat treatment for 15 hours,
the second step is that: and (3) mixing the precursor subjected to preoxidation treatment with lithium hydroxide monohydrate according to the ratio of the metal mole number to the lithium metal mole number of 1: 1.02; and (4) fully mixing.
The third step: first sintering
Experimental groups: sintering the mixture for the first time in an oxygen atmosphere, wherein the upper layer temperature of a kiln is as follows: 890 ℃, lower layer temperature: 870 ℃, and the heating rate is 2-8 ℃/min; preserving the heat for 20 hours;
reference group: sintering the mixture for the first time in an oxygen atmosphere, wherein the temperatures of the upper layer and the lower layer of the kiln are 875 ℃, and the heating rate is 2-8 ℃/min; preserving the heat for 20 hours;
the fourth step: adding aluminum hydroxide as a dopant in an amount of 0.2% (mass fraction) into the experimental group and the reference group after the first sintering, and mixing uniformly.
The fifth step: and (3) respectively sintering the mixture of the experimental group and the reference group after the doping agent is added in an oxygen atmosphere for the second time, wherein the sintering temperature is as follows: sintering was carried out at 500 ℃ for a total time of 15 hours.
Performing performance detection on the experimental group and the reference group after the treatment of the fifth step,
and (3) performance detection results:
the particle size distributions of the materials tested in the experimental and reference groups of this example are shown in table 4;
table 4:
| categories | D10 | D50 | D90 | D99 |
| Reference group | 1.63μm | 3.32μm | 6.42μm | 10.39μm |
| Experimental group | 1.25μm | 3.62μm | 8.13μm | 11.92μm |
The tap densities and capacities of the experimental group and the reference group of this example were determined to be shown in table 5;
table 5:
testing the compaction density of the pole piece: the materials of the reference group and the experimental group are respectively mixed with an adhesive (PVDF5130) and a conductive agent (Super P) according to the same proportion (main material: adhesive: conductive agent: 96.5: 1.5: 2) to prepare an identical surface density pole piece (400g/m2), and the actual compaction densities are shown in the table 6;
table 6:
| categories | Compacted density g/cc |
| Reference group | 3.25 |
| Experimental group | 3.45 |
Example 3:
the first step is as follows: ni precursor at 800 deg.c in oxygen atmosphere0.55Co0.15Mn0.3(OH)2And carrying out pre-oxidation treatment for 8 hours.
The second step is that: and (3) mixing the precursor subjected to preoxidation treatment with lithium salt according to the ratio of the metal mole number to the lithium salt mole number of 1: 1.08 mixing well.
The third step: first sintering
Experimental groups: sintering the mixture for the first time in an oxygen atmosphere, wherein the upper layer temperature of a kiln is 870 ℃, and the lower layer temperature is: 895 ℃, and the heating rate is 2-8 ℃/min; preserving the heat for 20 hours;
reference group: sintering the mixture for the first time in an oxygen atmosphere, wherein the temperatures of the upper layer and the lower layer of the kiln are 875 ℃, and the heating rate is 2-8 ℃/min; and keeping the temperature for 20 hours.
The fourth step: adding aluminum hydroxide as a dopant in an amount of 0.2% (mass fraction) into the experimental group and the reference group after the first sintering, and mixing uniformly.
The fifth step: and (3) respectively carrying out secondary sintering on the mixture of the experimental group and the reference group after the doping agent is added in an oxygen atmosphere, wherein the secondary sintering temperature is 600 ℃, and the total sintering time is 10 hours.
Performing performance detection on the experimental group and the reference group after the treatment of the fifth step,
and (3) performance detection results:
the particle size distributions of the materials tested in the experimental and reference groups of this example are shown in table 7;
table 7:
the tap densities and capacities of the experimental and reference groups of this example were determined to be shown in table 8;
table 8:
testing the compaction density of the pole piece: the materials of the reference group and the experimental group are respectively mixed with an adhesive (PVDF5130) and a conductive agent (Super P) according to the same proportion (main material: adhesive: conductive agent: 96.5: 1.5: 2) to prepare an identical surface density pole piece (400g/m2), and the actual compaction densities are shown in the table 9;
table 9:
| categories | Compacted density g/cc |
| Reference group | 3.25 |
| Experimental group | 3.52 |
Although the embodiments of the present invention have been described in detail hereinabove, it is apparent to those skilled in the art that various modifications and variations can be made to these embodiments. However, it is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention as described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (10)
1. The preparation method of the high-compaction ternary single crystal material is characterized by comprising the following steps of:
a. carrying out pre-oxidation treatment on a precursor containing Ni, Co and Mn in an oxygen atmosphere at the temperature of 200-800 ℃, wherein the total pretreatment time is 8-18 hours;
b. uniformly mixing the pre-oxidized precursor with lithium salt, wherein the ratio of the total metal mole number in the precursor to the lithium metal mole number in the lithium salt is as follows: 1: 1.02-1.08;
c. carrying out primary sintering on the mixed materials in an oxygen atmosphere, wherein the temperature difference of the upper layer and the lower layer of a kiln is 0-30 ℃, the lower temperature of the upper layer and the lower layer is 800-950 ℃, the higher temperature of the upper layer and the lower layer is 805-980 ℃, the heating rate is 2-8 ℃/min, and the heat preservation time is 5-30 hours;
d. adding a doping agent into the materials after the first sintering, and uniformly mixing;
e. and (3) after the materials which are uniformly mixed are subjected to jet milling, carrying out secondary sintering, wherein the sintering temperature is as follows: the total sintering time is 10-25 hours at 300-600 ℃.
2. The method for preparing the high-compaction ternary single crystal material according to claim 1, wherein the temperature difference between the upper layer and the lower layer of the kiln is 10-25 ℃.
3. The method for preparing a highly compacted ternary single crystal material according to claim 2, wherein the temperatures of the upper and lower layers in step c are 870 ℃ and 880 ℃, respectively.
4. The method for preparing a highly compacted ternary single crystal material according to claim 2, wherein the temperatures of the lower layer and the upper layer in step c are 870 ℃ and 890 ℃, respectively.
5. The method as claimed in claim 2, wherein the temperatures of the upper and lower layers in the step c are 870 ℃ and 895 ℃ respectively.
6.The method for preparing a high-compaction ternary single crystal material according to any one of claims 1 to 5, wherein the precursor is NixCoyMnz(OH)2Or NixCoyMnzCO3X, y and z are the mole numbers of Ni, Co and Mn respectively, and x + y + z is 1.
7. The method according to claim 6, wherein the molar ratio of Ni, Co and Mn in the precursor is 1: 1: 1 or 5-5.5: 1.5-2: 3 or 6 to 7.5: 0.5-2: 0.5 to 3.5.
8. The method of claim 7, wherein the molar ratio of Ni, Co, Mn is 6.3:0.8: 2.9.
9. The method of claim 8, wherein the lithium salt is lithium carbonate or lithium hydroxide monohydrate.
10. The method of claim 9, wherein the dopant is one or more of Zr, Al, Ti, Mg, Sr.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114251941A (en) * | 2021-11-30 | 2022-03-29 | 广东邦普循环科技有限公司 | Lithium battery positive electrode material and production process thereof |
| CN114251941B (en) * | 2021-11-30 | 2024-01-05 | 广东邦普循环科技有限公司 | Lithium battery anode material and production process thereof |
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