CN111200129B - Preparation method of single crystal type high-nickel ternary cathode material - Google Patents
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Abstract
The invention discloses a preparation method of a single-crystal high-nickel ternary cathode material, which comprises the steps of uniformly mixing a nickel-cobalt-manganese hydroxide precursor or a nickel-cobalt-aluminum hydroxide precursor with two or more than two kinds of molten inorganic salts according to a certain stoichiometric ratio, putting the mixture into a crucible, heating to a certain temperature at a preset heating rate, keeping the temperature for a period of time, and naturally cooling to room temperature; washing the obtained mixture with deionized water for multiple times, drying the mixture for several hours in vacuum at the temperature of 100-120 ℃, then putting the dried mixture into a crucible, heating the mixture to a certain temperature at a preset heating rate, keeping the temperature for a period of time, and naturally cooling the mixture to room temperature to obtain the single-crystal high-nickel ternary cathode material. The method adopts a mode of mixing the molten salt with two or more than two kinds, effectively reduces the melting temperature of the molten salt, enables the single crystal type high nickel ternary cathode material to be formed in the molten salt, simultaneously inhibits the phenomenon of lithium-nickel mixed discharge, and ensures that the nickel content in the prepared single crystal type high nickel ternary cathode material is not less than 80%.
Description
Technical Field
The invention relates to a preparation method of a lithium ion battery anode material, in particular to a preparation method of a single crystal high-nickel ternary anode material.
Background
Lithium ion batteries have been widely used as an important energy storage device in electronic products such as mobile phones and computers. Lithium cobaltate is mainly selected as a positive electrode material in the traditional lithium ion battery, but because the lithium cobaltate is expensive and has low energy density, the positive electrode material with high energy density is urgently needed to be found.
At present, most of the researched cathode materials mainly comprise a ternary cathode material with a layered structure, a lithium-rich manganese-based material, lithium manganate, lithium iron phosphate and the like, wherein the nickel cobalt lithium manganate ternary cathode material is favored by people due to high energy density, and particularly is a high nickel ternary material, but the nickel cobalt lithium manganate cathode material has the problems of poor structural stability, rapid capacity attenuation in a high-voltage circulation process and the like, so that the application of the nickel cobalt lithium manganate cathode material in commerce is limited.
Aiming at the problems faced by the nickel cobalt lithium manganate material, at present, two methods are mainly used for improvement, namely ion doping and surface coating. The ion doping is an effective means to improve the structural stability of the main material, and particularly, under high voltage, a small amount of inert ion doping can achieve the purpose of stabilizing the layered structure of the nickel cobalt lithium manganate material, so that the cycling stability of the nickel cobalt lithium manganate material under high voltage can be improved. The traditional ion doping is usually realized by a sol-gel method or a coprecipitation method, and the two methods are complicated to operate and expensive. The surface coating is realized by a solid phase method, and the method has the characteristics of long reaction time, high energy consumption, easy formation of impure phases, unstable electrochemical performance and the like, and needs to be carried out at high temperature. Compared with a polycrystalline structure, the single crystal is more stable, and the cycle performance and the safety performance are improved, so that the method for preparing the ternary material into the large-particle single crystal is another method for improving the ternary material, and the temperature for preparing the single crystal type nickel cobalt lithium manganate by adopting a precursor method is at least over 900 ℃.
Disclosure of Invention
The invention provides a preparation method of a single-crystal high-nickel ternary cathode material, which is characterized in that after the preparation process of a nickel cobalt manganese (lithium) oxide cathode material is analyzed, the temperature of a reaction system is controlled in a proper range by creatively adopting a mode of mixing two or more than two molten salts and reasonably adjusting the material ratio, so that the melting temperature of the molten salts is effectively reduced, the phenomenon of mixed arrangement of lithium and nickel is inhibited, and the single-crystal high-nickel ternary cathode material with high nickel content is obtained.
A preparation method of a single-crystal high-nickel ternary cathode material comprises the following steps:
selecting a nickel-cobalt-manganese hydroxide precursor or a nickel-cobalt-aluminum hydroxide precursor as a reaction precursor;
selecting more than two molten inorganic salts as mixed molten salt;
uniformly mixing a reaction precursor, lithium salt and mixed molten salt according to a molar ratio of 1.0:1.1: x, putting the mixture into a crucible, heating the mixture to 650-800 ℃ at a heating rate of 2-10 ℃/min, keeping the temperature for 2-30 hours, and naturally cooling the mixture to room temperature, wherein x is more than 0 and less than 6;
and washing the cooled mixture with deionized water for multiple times, drying the mixture for several hours in vacuum at the temperature of 100-120 ℃, then putting the dried mixture into a crucible, heating the mixture to the temperature of 650-800 ℃ at the heating rate of 2-10 ℃/min, keeping the temperature for 2-10 hours, and naturally cooling the mixture to the room temperature to obtain the single-crystal high-nickel ternary cathode material.
In a preferred embodiment, the nickel cobalt manganese hydroxide precursor has the formula NixCoyMnz(OH)2Wherein x is more than or equal to 0.8<1，0<y≤0.1，0<z is less than or equal to 0.1, and x + y + z is 1; the chemical formula of the nickel-cobalt-aluminum hydroxide precursor is NiuCovAlw(OH)2u+2v+3wWherein u is more than or equal to 0.8<1，0<v≤0.1，0<w is less than or equal to 0.1, and u + v + w is 1.
In a preferred embodiment, the inorganic salt is A2SO4AX or BSO4Wherein a ═ Li, Na, K, Rb, Cs; x ═ F, Cl, Br, I, NO3，B＝Mg,Ca,Sr,Ba。
In a preferred embodiment, the melting point of the mixed molten salt is not higher than 800 ℃.
In a preferred embodiment, the lithium salt is a salt containing a Li — O bond and a hydrate thereof.
In a preferred embodiment, the lithium salt is lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate or lithium acetate.
A single crystal type high nickel ternary anode material has a chemical formula of LiaNixCoyMnzO2Or LibNiuCovAlwO2Wherein a is more than or equal to 1.0 and less than or equal to 1.05, and x is more than or equal to 0.8<1，0<y≤0.1，0<z is less than or equal to 0.1, and x + y + z is less than or equal to 0.95 and less than or equal to 1; b is more than or equal to 1.0 and less than or equal to 1.05, and u is more than or equal to 0.8<1，0<v≤0.1，0<w is less than or equal to 0.1, and u + v + w is less than or equal to 0.95 and less than or equal to 1.
In a preferred embodiment, the nickel mole percentage content in the single-crystal high-nickel ternary cathode material is not less than 80%.
Compared with the prior art, the invention has the following advantages: the method adopts a mode of mixing two or more than two molten salts, effectively reduces the melting temperature of the molten salts (the melting point is not higher than 800 ℃), provides a good liquid phase environment for chemical reaction, inhibits the phenomenon of lithium-nickel mixed arrangement while forming the single crystal ternary material in a molten salt system, and obtains the single crystal type high-nickel ternary cathode material with good electrochemical performance, wherein the nickel mole percentage content in the material is not less than 80%.
Drawings
FIG. 1 is a graph obtained in example 1 of the present inventionLiNi0.8Mn0.1Co0.1O2SEM picture of (1);
FIG. 2 is LiNi obtained in example 10.8Mn0.1Co0.1O2XRD pattern of (a);
FIG. 3 is LiNi obtained in example 10.8Mn0.1Co0.1O2The charge-discharge curve chart of (1);
FIG. 4 is LiNi obtained in example 2 of the present invention0.85Co0.10Al0.05O2SEM picture of (1);
FIG. 5 is LiNi obtained in example 2 of the present invention0.85Co0.10Al0.05O2XRD pattern of (a);
FIG. 6 is LiNi obtained in example 2 of the present invention0.85Co0.10Al0.05O2A cycle test data graph of (a);
FIG. 7 shows LiNi obtained in example 3 of the present invention0.9Co0.07Al0.03O2SEM picture of (1);
FIG. 8 is LiNi obtained in example 4 of the present invention0.83Co0.08Mn0.09O2SEM image of (d).
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
A preparation method of a single-crystal high-nickel ternary cathode material comprises the following steps:
selecting a nickel-cobalt-manganese hydroxide precursor or a nickel-cobalt-aluminum hydroxide precursor as a reaction precursor;
the reaction precursor is obtained by market purchase or laboratory preparation.
Selecting two or more than two molten inorganic salts as mixed molten salt;
the molar ratio between two or more than two mixed molten salts is any ratio as long as the melting point of the mixed molten salt is not higher than 800 ℃.
The heating temperature is not lower than the melting point of the mixed molten salt, and the preferable heating temperature range of the application is 650-800 ℃.
Uniformly mixing a reaction precursor, lithium salt and mixed molten salt according to a molar ratio of 1.0:1.1: x, putting the mixture into a crucible, heating the mixture to 650-800 ℃ at a heating rate of 2-10 ℃/min, keeping the temperature for 2-30 hours, and naturally cooling the mixture to room temperature, wherein x is more than 0 and less than 6; the hardening of reaction products is easily caused by too high proportion of mixed molten salt, which is not beneficial to the subsequent treatment and utilization.
The lithium salt is any salt containing a Li-O bond and hydrates thereof.
And washing the cooled mixture with deionized water for multiple times, drying the mixture for several hours in vacuum at the temperature of 100-120 ℃, then putting the dried mixture into a crucible, heating the mixture to the temperature of 650-800 ℃ at the heating rate of 2-10 ℃/min, keeping the temperature for 2-10 hours, and naturally cooling the mixture to the room temperature to obtain the single-crystal high-nickel ternary cathode material.
The retention time is too short, the reaction is not completed, and the energy waste is easily caused by too long time.
Too high a heating temperature easily causes the occurrence of lithium-nickel mixed-row to affect the crystal form and the performance of the reaction product. The proportion of a reaction precursor, lithium salt and mixed molten salt and the reaction temperature influence the crystal form and the electrochemical performance of the finally formed ternary cathode material, and the single-crystal high-nickel ternary cathode material needs to be prepared, so that the single-crystal high-nickel ternary cathode material can be generated only by specially limiting the parameters such as the proportion, the reaction temperature and the like.
Example 1
0.1mol of precursor Ni0.8Co0.1Mn0.1(OH)2，0.11mol LiOH，0.05mol Li2SO4-Cs2SO4Mixing molten salt (molar ratio 1:1, melting point about 740 deg.C), placing into crucible, heating to 780 deg.C at heating rate of 10 deg.C/min, maintaining for 15 hr, naturally cooling to room temperature, washing the mixture with deionized water for 3 times, vacuum drying at 120 deg.C for 3 hr, placing into crucible, heating to 750 deg.C at heating rate of 10 deg.C/min, maintaining for 6 hr, naturally cooling to room temperature to obtain single crystal 811(LiNi type)0.8Mn0.1Co0.1O2) A ternary material.
The ternary material formed is a single crystal polyhedron morphology as can be seen in fig. 1. From the XRD data of FIG. 2, it can be seen that the crystallinity is very good and the structure is highly ordered.
Electrochemical testing: mixing the active material, conductive carbon and PVDF binder in NMP according to the ratio of 90:5:5, coating the mixture on an aluminum foil, drying the aluminum foil in a blowing oven at 80 ℃, and drying the aluminum foil in a vacuum oven at 120 ℃ overnight. The dried pole piece is used as the battery anode, the lithium metal is used as the battery cathode, the single-layer polyethylene film is used as the diaphragm, and 1M LiPF6EC-EMC (3:7) is electrolyte, and the 2032 battery is assembled to carry out electrochemical test. The test method was first 1 cycle at 0.1C current (1C ═ 170mA/g) and then a 0.2C-0.2C charge-discharge cycle was performed. The test voltage range is 4.3-2.8V. From the charge-discharge curve shown in FIG. 3, it can be seen that LiNi0.8Mn0.1Co0.1O2The first discharge capacity of the single crystal ternary material is 182mAh/g (0.1C current), and the first coulombic efficiency is 87%. The performance is excellent under the condition of 0.2C, and the discharge capacity exceeds 170 mAh/g.
Example 2
0.1mol of precursor Ni0.85Co0.1Al0.05(OH)2.05，0.11mol LiOH，0.05mol Li2SO4-K2SO4Mixing molten salt (the molar ratio is 8:2, the melting point is about 530 ℃) uniformly, putting the mixture into a crucible, heating the mixture to 750 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 15 hours, naturally cooling the mixture to the room temperature, washing the mixture for 3 times by deionized water, drying the mixture in vacuum at 120 ℃ for 3 hours, putting the mixture into the crucible, heating the mixture to 750 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 6 hours, and naturally cooling the mixture to the room temperature to obtain LiNi0.85Co0.10Al0.05O2。
It can be seen from fig. 4 that the ternary material is in the shape of a single-crystal polyhedron. From the XRD data of FIG. 5, it can be seen that the crystallinity is good and the structure is highly ordered.
Electrochemical testing: mixing an active material, conductive carbon and PVDF binder in a ratio of 90:5:5 in NMP, coating the mixture on an aluminum foil, drying the aluminum foil in a 80-DEG air-blast oven, and putting the aluminum foil into the air-blast ovenDried overnight in a 120 degree vacuum oven. The dried pole piece is used as a battery anode, lithium metal is used as a battery cathode, the single-layer polyethylene film is used as a diaphragm, 1M LiPF6 EC-EMC (3:7) is used as electrolyte, and the 2032 battery is assembled for electrochemical test. The test method was first to cycle 3 cycles at 0.1C current (1C 190mA/g) and then to perform 1C-1C charge-discharge cycles. The test voltage range is 4.3-2.8V. From the charge-discharge curve shown in FIG. 6, it can be seen that LiNi0.85Co0.10Al0.05O2The first discharge capacity of the single crystal ternary material is 212.7mAh/g (0.1C current), and the first coulombic efficiency is 89.7%. The performance is excellent under the condition of 1C, the discharge capacity exceeds 186mAh/g, and the capacity of 154mAh/g is still maintained after 300 cycles.
Example 3
0.1mol of precursor Ni0.9Co0.07Al0.03(OH)2.03，0.11mol LiNO30.2mol CsBr-LiBr mixed molten salt (the mol ratio is 1:1, the melting point is about 311 ℃) is uniformly mixed, the mixture is put into a crucible, the mixture is heated to 660 ℃ at the heating rate of 3 ℃/min and is kept for 5 hours, the mixture is naturally cooled to the room temperature, the mixture is washed 3 times by deionized water, the mixture is dried in vacuum at 100 ℃ for 3 hours, then the mixture is put into the crucible, the mixture is heated to 650 ℃ at the heating rate of 3 ℃/min and is kept for 3 hours, and the mixture is naturally cooled to the room temperature, so that the single crystal Li Ni is obtained0.9Co0.07Al0.03O2A ternary material. It can be seen from fig. 7 that the formed ternary material has a single crystal polyhedral morphology.
Example 4
0.1mol of precursor Ni0.83Co0.08Mn0.09(OH)2，0.11mol LiCH3COO and 0.3mol LiI-KI mixed molten salt (the molar ratio is 0.634:0.366, the melting point is about 286 ℃) are uniformly mixed, the mixture is put into a crucible, heated to 740 ℃ at the heating rate of 7 ℃/min and kept for 25 hours, naturally cooled to room temperature, the mixture is washed for 3 times by deionized water, dried for 4 hours in vacuum at 110 ℃, then put into the crucible, heated to 710 ℃ at the heating rate of 7 ℃/min and kept for 10 hours, and naturally cooled to room temperature to obtain the single crystal Li Ni0.83Co0.08Mn0.09O2A ternary material. From FIG. 8The formed ternary material is in the shape of a monocrystal polyhedron.
The above-mentioned embodiments only express one or several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications are possible without departing from the inventive concept, and such equivalent variations are also within the scope of the invention as defined in the appended claims.
Claims (8)
1. A preparation method of a single-crystal high-nickel ternary cathode material is characterized by comprising the following steps:
selecting a nickel-cobalt-manganese hydroxide precursor or a nickel-cobalt-aluminum hydroxide precursor as a reaction precursor;
selecting more than two molten inorganic salts as mixed molten salt;
uniformly mixing a reaction precursor, lithium salt and mixed molten salt according to a molar ratio of 1.0:1.1: x, putting the mixture into a crucible, heating the mixture to 650-800 ℃ at a heating rate of 2-10 ℃/min, keeping the temperature for 2-30 hours, and naturally cooling the mixture to room temperature, wherein x is more than 0 and less than 6;
and washing the cooled mixture with deionized water for multiple times, drying the mixture for several hours in vacuum at the temperature of 100-120 ℃, then putting the dried mixture into a crucible, heating the mixture to the temperature of 650-800 ℃ at the heating rate of 2-10 ℃/min, keeping the temperature for 2-10 hours, and naturally cooling the mixture to the room temperature to obtain the single-crystal high-nickel ternary cathode material.
2. The method for preparing a single-crystal high-nickel ternary cathode material according to claim 1, wherein the chemical formula of the nickel-cobalt-manganese hydroxide precursor is NixCoyMnz(OH)2Wherein x is more than or equal to 0.8<1，0<y≤0.1，0<z is less than or equal to 0.1, and x + y + z is 1; the chemical formula of the nickel-cobalt-aluminum hydroxide precursor is NiuCovAlw(OH)2u+2v+3wWherein u is more than or equal to 0.8<1，0<v≤0.1，0<w is less than or equal to 0.1, and u + v + w is 1.
3. The method for preparing a single-crystal high-nickel ternary positive electrode material as claimed in claim 1, wherein the inorganic salt is A2SO4AX or BSO4Wherein a ═ Li, Na, K, Rb, Cs; x ═ F, Cl, Br, I, NO3；B＝Mg,Ca,Sr,Ba。
4. The method for preparing the single-crystal high-nickel ternary cathode material according to claim 1 or 3, wherein the melting point of the mixed molten salt is not higher than 800 ℃.
5. The method for preparing a single-crystal high-nickel ternary positive electrode material according to claim 1, wherein the lithium salt is a salt having a Li-O bond and a hydrate thereof.
6. The method for preparing a single-crystal high-nickel ternary positive electrode material according to claim 1 or 5, wherein the lithium salt is lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate or lithium acetate.
7. The single-crystal high-nickel ternary cathode material obtained by the preparation method according to any one of claims 1 to 6, wherein the chemical formula of the single-crystal high-nickel ternary cathode material is LiaNixCoyMnzO2Or LibNiuCovAlwO2Wherein a is more than or equal to 1.0 and less than or equal to 1.05, and x is more than or equal to 0.8<1，0<y≤0.1，0<z is less than or equal to 0.1, and x + y + z is less than or equal to 0.95 and less than or equal to 1; b is more than or equal to 1.0 and less than or equal to 1.05, and u is more than or equal to 0.8<1，0<v≤0.1，0<w is less than or equal to 0.1, and u + v + w is less than or equal to 0.95 and less than or equal to 1.
8. The single crystal type high nickel ternary cathode material as claimed in claim 7, wherein the nickel mole percentage content in the single crystal type high nickel ternary cathode material is not less than 80%.
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| CN113381005B (en) * | 2021-05-27 | 2022-10-11 | 厦门大学 | Single-crystal ternary cathode material, continuous preparation method and device and application |
| CN113707873A (en) * | 2021-06-08 | 2021-11-26 | 宁夏汉尧石墨烯储能材料科技有限公司 | Lithium ion battery positive electrode material using eutectic lithium salt and preparation method thereof |
| CN113764658B (en) * | 2021-08-31 | 2024-04-16 | 中南大学 | Anion-cation co-doped high-nickel monocrystal ternary cathode material, and preparation method and application thereof |
| CN114000195B (en) * | 2021-11-01 | 2023-09-08 | 佛山科学技术学院 | Preparation method of monodisperse high-nickel ternary monocrystal positive electrode material |
| CN114156448B (en) * | 2021-11-26 | 2023-08-22 | 格林美（无锡）能源材料有限公司 | Layered high-nickel NCA single-crystal ternary positive electrode material and preparation method thereof |
| CN114678525B (en) * | 2022-04-12 | 2023-08-18 | 浙江极氪智能科技有限公司 | Ternary positive electrode material, preparation method thereof and lithium ion battery |
| CN116750810A (en) * | 2023-07-11 | 2023-09-15 | 广东省科学院资源利用与稀土开发研究所 | Single-crystal type high-nickel ternary positive electrode material for high-voltage lithium ion battery and preparation method thereof |
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