CN107742711B - Preparation method of diboron trioxide coated ternary cathode material - Google Patents
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- CN107742711B CN107742711B CN201710978003.6A CN201710978003A CN107742711B CN 107742711 B CN107742711 B CN 107742711B CN 201710978003 A CN201710978003 A CN 201710978003A CN 107742711 B CN107742711 B CN 107742711B
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- 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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Abstract
The invention discloses a preparation method of a boron trioxide coated ternary cathode material, which comprises the following steps: (1) dissolving hydroxypropyl guar gum in water under a stirring state, stopping stirring, and standing to obtain a hydroxypropyl guar gum solution; (2) adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1) under the stirring condition, then continuously stirring for 20-30min, then adding borax, wherein the mass of the borax is 0.1% -1% of that of the hydroxypropyl guar gum solution, and further continuously stirring for 3-5min to obtain a cross-linked hydroxypropyl guar gum solution; (3) drying the cross-linked hydroxypropyl guar gum solution, and calcining at 400-600 ℃ for 5-15 h. The method provided by the invention can be used for coating the layer B2O3The uniform coating is on the surface of the ternary cathode material, so that the corrosion of the electrolyte to the material can be effectively reduced, and the circulation stability of the electrode material is improved.
Description
Technical Field
The invention belongs to the technical field of new energy materials, and particularly relates to a preparation method of a boron trioxide coated ternary cathode material.
Background
The lithium battery has excellent performances of high working voltage, high specific energy, good safety and the like, and is widely applied as a power source of electronic products. The electrode material is used as one of the core components of the battery and plays a key role in the comprehensive performance of the battery. However, the ternary electrode material still has a certain problem, and the electrolyte has a certain corrosion effect on the electrode material, so that the capacity of the material is attenuated, and the cycling stability of the electrode material is influenced. Therefore, modifying the electrode material is an important means for improving the material performance, and a commonly used modification method is surface coating.
At present, the surface coating substance for the ternary lithium ion battery anode material comprises boron trioxide B2O3、Al2O3、AlPO4、AlF3、LiAlO2、TiO2、ZrO2Carbon, graphene, V2O5、Y2O3Etc. bag usedThe coating method is often a precipitation method and a ball milling method. The so-called precipitation method, in which metal ions are deposited on the surface of a material by a precipitation reaction, is prone to cause unevenness in the thickness of a coating layer. The ball milling method is that the coated object and the coated object are mixed according to a certain proportion and ball milled to ensure that the coated object is distributed on the surface of the material, and the method easily causes the uneven distribution of the coating layer, and the uneven distribution of the coating layer can influence the performance of the material. Currently coated B2O3Ball milling is generally used.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the diboron trioxide-coated ternary cathode material, which can ensure that the thickness of a coating layer on the surface of the ternary cathode material is uniform, and improve the cycle stability of the electrode material.
A preparation method of a boron trioxide coated ternary cathode material comprises the following steps:
(1) according to the mass ratio of hydroxypropyl guanidine gum to water of 1: (50-100), weighing hydroxypropyl guar gum, dissolving in water under a stirring state, stopping stirring after 2-6min, and standing for 2-4h to obtain a hydroxypropyl guar gum solution;
(2) under the stirring condition, according to the mass ratio of the hydroxypropyl guar gum to the ternary cathode material of 1: (0.01-1.5), adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1), continuing to stir for 20-30min, then adding borax, wherein the mass of the borax is 0.1% -1% of that of the hydroxypropyl guar gum solution, and continuing to stir for 3-5min to obtain a cross-linked hydroxypropyl guar gum solution;
(3) drying the cross-linked hydroxypropyl guar gum solution, and calcining at 400-600 ℃ for 5-15 h.
Preferably, the ternary cathode material in step (2) is a ternary cathode material in the prior art.
Preferably, the ternary cathode material in the step (2) is L iNi1/3Co1/3Mn1/3O2、LiNi1/2Co1/6Mn1/3O2、LiNi0.5Co0.2Mn0.3O2、LiNi0.4Co0.2Mn0.4O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.8Co0.1Mn0.1O2、Li(Ni0.42Mn0.42Co0.16)O2Or a doped ternary positive electrode material.
Preferably, the stirring speed in step (2) is 500-2000 r/min.
Preferably, the drying conditions in step (3) are as follows: the temperature is 100 ℃ and 150 ℃, and the time is 4-6 h.
The invention uses hydroxypropyl guar gum and borax to react to generate a gel system with three-dimensional net effect, the borax is used as a cross-linking agent, the main component of hydroxypropyl guar gum powder is galactomannan, the molecules of the galactomannan contain a large amount of cis-ortho hydroxyl, when a boron cross-linking agent is cross-linked with the guar gum, multi-stage ionization is firstly generated to generate borate ions B (OH)4 -And then forms a stable hydrogen bond with cis-ortho hydroxyl in the guanidine gum molecule, and generates the viscoelastic jelly glue through intermolecular crosslinking reaction. Therefore, the ternary cathode material is uniformly distributed in the hydroxypropyl guar gum solution under the stirring condition, a gel system with uniform distribution can be formed after cross-linking by the cross-linking agent, water is removed by heating and then high-temperature oxidation is carried out, finally, the hydroxypropyl guar gum is oxidized into gas, and boron (B) in borax is oxidized into B2O3The ternary cathode material is deposited on the surface of the ternary cathode material, the thickness of a coating layer can be controlled by controlling the addition of the cross-linking agent, and the ternary cathode material can be uniformly distributed by stirring, so that the uniformly coated ternary cathode material is obtained.
The invention has the advantages that:
the method provided by the invention can be used for coating the layer B2O3The ternary cathode material is uniformly coated on the surface of the ternary cathode material, the thickness of the coating layer can be controlled by controlling the addition of the cross-linking agent, and finally, the coated ternary cathode material can effectively reduce the corrosion of electrolyte to the material and improve the circulation stability of the electrode material.
Detailed Description
Example 1
A preparation method of a boron trioxide coated ternary cathode material comprises the following steps:
(1) weighing hydroxypropyl guar gum according to the mass ratio of the hydroxypropyl guar gum to water of 1:50, dissolving the hydroxypropyl guar gum in water under the stirring state of 1000r/min, stopping stirring for 2min, and standing for 4h to obtain a hydroxypropyl guar gum solution;
(2) selecting the ternary cathode material as L iNi1/3Co1/3Mn1/3O2Adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1) according to the mass ratio of hydroxypropyl guar gum to the ternary positive electrode material of 1:0.01 under the stirring condition of 500r/min, then continuously stirring for 20min, then adding borax, wherein the mass of borax is 0.1% of the mass of the hydroxypropyl guar gum solution, and then continuously stirring for 5min to obtain a cross-linked hydroxypropyl guar gum solution;
(3) the cross-linked hydroxypropyl guar gum solution was dried at 100 ℃ for 6h and then calcined at 400 ℃ for 15 h.
Example 2
A preparation method of a boron trioxide coated ternary cathode material comprises the following steps:
(1) weighing hydroxypropyl guar gum according to the mass ratio of the hydroxypropyl guar gum to water of 1:100, dissolving the hydroxypropyl guar gum in water under the stirring state of 1000r/min, stopping stirring for 6min, and standing for 4h to obtain a hydroxypropyl guar gum solution;
(2) selecting the ternary cathode material as L iNi1/2Co1/6Mn1/3O2Adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1) according to the mass ratio of hydroxypropyl guar gum to the ternary positive electrode material of 1:1.5 under the stirring condition of 2000r/min, then continuing to stir for 30min, then adding borax, wherein the mass of borax is 1% of the mass of the hydroxypropyl guar gum solution, and continuing to stir for 3min to obtain a cross-linked hydroxypropyl guar gum solution;
(3) the cross-linked hydroxypropyl guar gum solution was dried at 150 ℃ for 4h and then calcined at 600 ℃ for 5 h.
Example 3
A preparation method of a boron trioxide coated ternary cathode material comprises the following steps:
(1) weighing hydroxypropyl guar gum according to the mass ratio of the hydroxypropyl guar gum to water of 1:70, dissolving the hydroxypropyl guar gum in water under the stirring state of 1000r/min, stopping stirring for 4min, and standing for 3h to obtain a hydroxypropyl guar gum solution;
(2) selecting the ternary cathode material as L iNi0.5Co0.2Mn0.3O2Adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1) according to the mass ratio of hydroxypropyl guar gum to the ternary positive electrode material of 1:1.0 under the stirring condition of 1000r/min, then continuously stirring for 25min, then adding borax, wherein the mass of borax is 0.5% of the mass of the hydroxypropyl guar gum solution, and then continuously stirring for 4min to obtain a cross-linked hydroxypropyl guar gum solution;
(3) the cross-linked hydroxypropyl guar gum solution was dried at 120 ℃ for 5h and then calcined at 500 ℃ for 8 h.
Example 4
A preparation method of a boron trioxide coated ternary cathode material comprises the following steps:
(1) weighing hydroxypropyl guar gum according to the mass ratio of the hydroxypropyl guar gum to water of 1:80, dissolving the hydroxypropyl guar gum in water under the stirring state of 1000r/min, stopping stirring for 5min, and standing for 3h to obtain a hydroxypropyl guar gum solution;
(2) selecting the ternary cathode material as L iNi0.6Co0.2Mn0.2O2Adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1) according to the mass ratio of hydroxypropyl guar gum to the ternary positive electrode material of 1:0.07 under the stirring condition of 1500r/min, then continuously stirring for 25min, then adding borax, wherein the mass of borax is 0.8% of the mass of the hydroxypropyl guar gum solution, and then continuously stirring for 4min to obtain a cross-linked hydroxypropyl guar gum solution;
(3) the cross-linked hydroxypropyl guar gum solution was dried at 120 ℃ for 5h and then calcined at 500 ℃ for 15 h.
COMPARATIVE EXAMPLE 1 (ball milling method)
Weighing L iNi1/3Co1/3Mn1/3O25.0g，0.05gB2O3Mechanically mixing, grinding for 2h by using absolute ethyl alcohol as a grinding medium, and then calcining for 15h at 500 ℃ to prepare the ternary material with the surface coated with the boron oxide.
The ternary cathode material in the prior art can realize the functions that the finally coated ternary cathode material can effectively reduce the corrosion of electrolyte to the material and improve the cycle stability of the electrode material by adopting the method provided by the invention.
The modified ternary cathode materials obtained in the examples and the comparative examples are subjected to performance detection, and the results are shown in table 1.
Table 1 results of performance test of the ternary cathode material coated and modified in each of examples and comparative examples
As can be seen from table 1, the ternary cathode material modified by the method provided by the present invention can maintain the original first discharge specific capacity, and after 300 cycles, the capacity retention rate can reach more than 94%, while after 300 cycles, the capacity retention rate of the ternary cathode material without any substance is only about 80%. Compared with the uncoated material, the initial specific discharge capacity of the ternary cathode material is reduced to some extent after the modification by the ball milling method under the condition that the original cathode material is not changed, and after 300 cycles, the capacity retention rate is about 85 percent and is far lower than that of the modified ternary cathode material.
Claims (4)
1. A preparation method of a boron trioxide coated ternary cathode material is characterized by comprising the following steps: the method comprises the following steps:
(1) according to the mass ratio of hydroxypropyl guanidine gum to water of 1: (50-100), weighing hydroxypropyl guar gum, dissolving in water under a stirring state, stopping stirring after 2-6min, and standing for 2-4h to obtain a hydroxypropyl guar gum solution;
(2) under the stirring condition, according to the mass ratio of the hydroxypropyl guar gum to the ternary cathode material of 1: (0.01-1.5), adding a ternary positive electrode material into the hydroxypropyl guar gum solution obtained in the step (1), continuing to stir for 20-30min, then adding borax, wherein the mass of the borax is 0.1% -1% of that of the hydroxypropyl guar gum solution, and continuing to stir for 3-5min to obtain a cross-linked hydroxypropyl guar gum solution;
(3) drying the cross-linked hydroxypropyl guar gum solution, and calcining at 400-600 ℃ for 5-15 h.
2. The method for preparing the diboron trioxide-coated ternary cathode material according to claim 1, wherein the ternary cathode material obtained in the step (2) is L iNi1/3Co1/3Mn1/3O2、LiNi1/2Co1/6Mn1/3O2、LiNi0.5Co0.2Mn0.3O2、LiNi0.4Co0.2Mn0.4O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.8Co0.1Mn0.1O2、Li(Ni0.42Mn0.42Co0.16)O2Or a doped ternary positive electrode material.
3. The method for preparing the diboron trioxide-coated ternary cathode material according to claim 1, wherein the method comprises the following steps: the stirring speed in the step (2) is 500-2000 r/min.
4. The method for preparing the diboron trioxide-coated ternary cathode material according to claim 1, wherein the method comprises the following steps: the drying conditions in the step (3) are as follows: the temperature is 100 ℃ and 150 ℃, and the time is 4-6 h.
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