CN110911670A - Doping modification method of lithium nickel manganese oxide positive electrode material - Google Patents
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Abstract
The invention discloses a doping modification method of a lithium nickel manganese oxide positive electrode material. The method comprises the following steps: (1) dissolving manganese sulfate in a mixed solution of deionized water and ethanol, and uniformly stirring to obtain a product A; (2) dissolving ammonium bicarbonate in deionized water, and stirring to obtain product B; (3) pouring the product B into the product A, stirring for reaction, standing, performing suction filtration, washing, drying and sintering to obtain black solid of manganese dioxide, namely a product C; (4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into an ethanol solution, performing ultrasonic dispersion, and drying to obtain product D; (5) grinding the product D, adding into a magnetic boat, sintering at high temperature, and cooling to obtain product E; (6) grinding the product E to obtain a finished product. The doping method of the lithium nickel manganese oxide positive electrode material has the beneficial effects of low energy consumption and regular appearance.
Description
Technical Field
The invention relates to a doping modification method, in particular to a doping modification method of a lithium nickel manganese oxide positive electrode material.
Background
Since the industrial revolution has occurred, the human society has rapidly developed and fossil energy has been increasingly consumed. The fossil energy used at present mainly comprises coal, petroleum, natural gas and the like, and the reserves on the earth are limited and cannot be regenerated. The use of fossil energy also creates serious environmental problems such as greenhouse effect, atmospheric pollution, etc. For the sustainable development of human society, the development of clean, pollution-free and recyclable energy is urgent. The novel energy sources such as solar energy, wind energy, tidal energy, nuclear energy and the like are generated at the same time. But cannot be used in large quantities due to the influence of factors such as regions, environment, safety and the like. Because the earth crust contains a large amount of lithium, the use and development of lithium ion batteries are not blocked. In recent years, new energy automobiles are rapidly developed, and lithium ion batteries have wide application prospects in power batteries. The development of high-performance lithium ion power batteries has become one of the hot spots of research.
With the progress of science and technology and the rapid increase and diversification of market demands, the lithium ion battery with high development quantity density, long cycle life, low cost and environmental friendliness is a research hotspot in the field of batteries at present. Spinel-type LiNi0.5Mn1.5O4The high-rate performance, high working voltage and other superior performances of the lithium ion battery are considered to be one of the most influential and attractive positive electrode materials in the development of the lithium ion battery in the future. The development of the spinel type lithium nickel manganese oxide cathode material has important social significance and economic value. It becomes a research hotspot to modify the performance of the material. The main modification methods at present mainly include coating and doping. The conventional doping methods include a solid phase method and a sol-gel method, and have the defects that particles cannot keep a regular shape and energy loss is large. In conclusion, the traditional doping method has the defects of disordered appearance and high energy consumption.
Disclosure of Invention
The invention aims to provide a doping modification method of a lithium nickel manganese oxide positive electrode material. The doping method of the lithium nickel manganese oxide positive electrode material has the characteristics of low energy consumption and regular appearance.
The technical scheme of the invention is as follows: a doping modification method of a lithium nickel manganese oxide positive electrode material comprises the following steps:
(1) dissolving manganese sulfate in a mixed solution of deionized water and ethanol, and uniformly stirring to obtain a product A;
(2) dissolving ammonium bicarbonate in deionized water, and stirring to obtain product B;
(3) pouring the product B into the product A, stirring for reaction, standing, performing suction filtration, washing, drying and sintering to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into an ethanol solution, performing ultrasonic dispersion, and drying to obtain product D;
(5) grinding the product D, adding into a magnetic boat, sintering at high temperature, and cooling to obtain product E;
(6) grinding the product E to obtain a finished product.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (1), 0.01 to 0.05mol of manganese sulfate is dissolved in a mixed solution of 1000ml of deionized water and 200ml of ethanol.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (2), 0.2 to 0.5mol of ammonium bicarbonate is dissolved in 1000ml of deionized water.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (3), the product B is poured into the product A, the mixture is stirred and reacted for 30-50min at the temperature of 20-50 ℃ and the stirring speed of 400r/min, the mixture is kept stand for 3-5h, filtered, washed, dried for 2-5h at the temperature of 50-70 ℃, and then the dried mixture is placed into a box-type muffle furnace and sintered for 8h at the temperature of 450-.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (4), the product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate are added into 20-30ml of ethanol solution; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (4), ultrasonic dispersion is carried out for 10-20min, and drying is carried out at 90-100 ℃ for 1-2 h.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (5), the product D is ground to 0.001-0.005mm, then the ground product D is added into a magnetic boat, the temperature is raised from room temperature to 700-900 ℃ at a rate of 4-6 ℃/min, the high-temperature sintering is carried out at the temperature of 700-900 ℃ for 10-17 hours, and then the product E is obtained after cooling.
In the doping modification method of the lithium nickel manganese oxide positive electrode material, in the step (6), the product E is ground to 0.001-0.005mm, so as to obtain a finished product.
Compared with the prior art, the invention has the following beneficial effects:
1. dissolving manganese sulfate in a mixed solution of deionized water and ethanol in the step (1), and uniformly stirring to obtain a product A; (2) dissolving ammonium bicarbonate in deionized water, and stirring to obtain product B; (3) pouring the product B into the product A, stirring for reaction, standing, performing suction filtration, washing, and drying to obtain manganese carbonate, and sintering the manganese carbonate to obtain black solid of manganese dioxide, namely product C; (4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into the ethanol solution, performing ultrasonic dispersion, and drying to remove the ethanol solution to obtain product D; (5) grinding the product D, adding into a magnetic boat, sintering at high temperature, and cooling to obtain product E; (6) grinding the E product to obtain a finished product, namely the finished product is Al-processed3+Doped material LiNi0.5Mn1.45Al0.05O4。
2. The black solid (product C) of the manganese dioxide prepared in the step (3) of the invention is manganese dioxide with regular spherical morphology, and can be used as a template for the subsequent battery anode material synthesis, so that the synthesized battery material also has regular spherical morphology, and the performance of the battery material is obviously improved.
3. The traditional doping method is mainly a sol-gel method, and has the advantages of simple operation, stable element proportion, obvious defects, difficult control of morphology, disordered morphology of prepared materials, long synthesis period, expensive partial raw materials, even harm to the environment and low operability of the preparation process. According to the microsphere template method, the prepared microsphere manganese dioxide is used as a synthesis template, so that a lithium source, a nickel source and an aluminum source which are added subsequently can be fully fused with the template, the advantage of controllable morphology of a coprecipitation method is inherited, and the stability of element proportion is ensured.
4. In the step (4), the manganese dioxide, the lithium acetate, the nickel acetate and the aluminum chloride are fully and uniformly mixed by using an ethanol impregnation method, and the lithium acetate, the nickel acetate and the aluminum chloride are dissolved in ethanol and then invaded into spherical manganese dioxide particles, so that the spherical manganese dioxide template can be retained in the subsequent high-temperature sintering process, and the Al-treated manganese dioxide template prepared in the step (5) is obtained3+Doped LiNi0.5Mn1.45Al0.05O4The material has a more regular morphology.
In conclusion, the doping method of the lithium nickel manganese oxide positive electrode material has the beneficial effects of low energy consumption and regular appearance.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1. A doping modification method of a lithium nickel manganese oxide positive electrode material comprises the following steps:
(1) dissolving 0.01mol of manganese sulfate in a mixed solution of 1000ml of deionized water and 200ml of ethanol, and uniformly stirring to obtain a product A;
(2) dissolving 0.2mol ammonium bicarbonate in 1000ml deionized water, and stirring uniformly to obtain product B;
(3) pouring the product B into the product A, stirring and reacting for 30min at 20 ℃ and the stirring speed of 300r/min, standing for 3h, filtering, washing, drying for 2h at 50 ℃, putting into a box-type muffle furnace, and sintering for 8h at 450 ℃ to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into 20ml ethanol solution, ultrasonically dispersing for 10min, and drying at 90 deg.C for 1h to obtain product D; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05;
(5) adding the product D into a magnetic boat after the diameter of the product D is 0.001mm, heating the product D to 700 ℃ from room temperature at a speed of 4 ℃/min, sintering the product D at the temperature of 700 ℃ for 10 hours, and cooling the product D to obtain a product E;
(6) grinding the product E to 0.001mm to obtain a finished product.
Example 2. A doping modification method of a lithium nickel manganese oxide positive electrode material comprises the following steps:
(1) dissolving 0.02mol of manganese sulfate in a mixed solution of 1000ml of deionized water and 200ml of ethanol, and uniformly stirring to obtain a product A;
(2) dissolving 0.3mol of ammonium bicarbonate in 1000ml of deionized water, and uniformly stirring to obtain a product B;
(3) pouring the product B into the product A, stirring and reacting for 40min at 30 ℃ and the stirring speed of 350r/min, standing for 4h, performing suction filtration, washing, drying for 3h at 60 ℃, putting into a box-type muffle furnace, and sintering for 8h at 470 ℃ to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into 25ml ethanol solution, ultrasonically dispersing for 13min, and drying at 95 deg.C for 1.5h to obtain product D; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05;
(5) adding the product D into a magnetic boat after the diameter of the product D is 0.002mm, heating the product D to 750 ℃ from room temperature at the speed of 5 ℃/min, sintering the product D at the temperature of 750 ℃ for 12 hours, and cooling the product D to obtain a product E;
(6) grinding the product E to 0.002mm to obtain the finished product.
Example 3. A doping modification method of a lithium nickel manganese oxide positive electrode material comprises the following steps:
(1) dissolving 0.03mol of manganese sulfate in a mixed solution of 1000ml of deionized water and 200ml of ethanol, and uniformly stirring to obtain a product A;
(2) dissolving 0.4mol ammonium bicarbonate in 1000ml deionized water, and stirring uniformly to obtain product B;
(3) pouring the product B into the product A, stirring and reacting for 50min at 40 ℃ and the stirring speed of 400r/min, standing for 5h, performing suction filtration, washing, drying for 4h at 70 ℃, putting into a box-type muffle furnace, and sintering for 8h at 490 ℃ to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into 30ml ethanol solution, ultrasonically dispersing for 15min, and drying at 100 deg.C for 1h to obtain product D; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05;
(5) adding the product D into a magnetic boat after the diameter of the product D is 0.003mm, heating the product D to 800 ℃ from room temperature at the speed of 6 ℃/min, sintering the product D at the temperature of 800 ℃ for 14 hours, and cooling the product D to obtain a product E;
(6) grinding the product E to 0.003mm to obtain a finished product.
Example 4. A doping modification method of a lithium nickel manganese oxide positive electrode material comprises the following steps:
(1) dissolving 0.04mol of manganese sulfate in a mixed solution of 1000ml of deionized water and 200ml of ethanol, and uniformly stirring to obtain a product A;
(2) dissolving 0.5mol ammonium bicarbonate in 1000ml deionized water, and stirring to obtain product B;
(3) pouring the product B into the product A, stirring and reacting for 50min at 30 ℃ and the stirring speed of 300r/min, standing for 4h, performing suction filtration, washing, drying for 4h at 60 ℃, putting into a box-type muffle furnace, and sintering for 8h at 500 ℃ to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into 25ml ethanol solution, ultrasonically dispersing for 18min, and drying at 95 deg.C for 1.5h to obtain product D; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05;
(5) adding the product D into a magnetic boat after the product D is 0.004mm, heating the product D to 850 ℃ from room temperature at a speed of 4 ℃/min, sintering the product D at 850 ℃ for 15 hours, and cooling the product D to obtain a product E;
(6) grinding the product E to 0.004mm to obtain a finished product.
Example 5. A doping modification method of a lithium nickel manganese oxide positive electrode material comprises the following steps:
(1) dissolving 0.05mol of manganese sulfate in a mixed solution of 1000ml of deionized water and 200ml of ethanol, and uniformly stirring to obtain a product A;
(2) dissolving 0.5mol ammonium bicarbonate in 1000ml deionized water, and stirring to obtain product B;
(3) pouring the product B into the product A, stirring and reacting for 50min at 50 ℃ and the stirring speed of 400r/min, standing for 5h, filtering, washing, drying for 5h at 70 ℃, putting into a box-type muffle furnace, and sintering for 8h at 520 ℃ to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into 30ml ethanol solution, ultrasonically dispersing for 20min, and drying at 100 deg.C for 2h to obtain product D; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05;
(5) adding the product D into a magnetic boat after the diameter of the product D is 0.005mm, heating the product D to 900 ℃ from room temperature at the speed of 6 ℃/min, sintering the product D at the temperature of 900 ℃ for 17 hours, and cooling the product D to obtain a product E;
(6) grinding the product E to 0.005mm to obtain the finished product.
Claims (8)
1. A doping modification method of a lithium nickel manganese oxide positive electrode material is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving manganese sulfate in a mixed solution of deionized water and ethanol, and uniformly stirring to obtain a product A;
(2) dissolving ammonium bicarbonate in deionized water, and stirring to obtain product B;
(3) pouring the product B into the product A, stirring for reaction, standing, performing suction filtration, washing, drying and sintering to obtain black solid of manganese dioxide, namely a product C;
(4) adding product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into an ethanol solution, performing ultrasonic dispersion, and drying to obtain product D;
(5) grinding the product D, adding into a magnetic boat, sintering at high temperature, and cooling to obtain product E;
(6) grinding the product E to obtain a finished product.
2. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (1), 0.01-0.05mol of manganese sulfate is dissolved in a mixed solution of 1000ml of deionized water and 200ml of ethanol.
3. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (2), 0.2-0.5mol of ammonium bicarbonate is dissolved in 1000ml of deionized water.
4. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (3), the product B is poured into the product A, stirred and reacted for 30-50min at the temperature of 20-50 ℃ and the stirring speed of 300-400r/min, kept stand for 3-5h, filtered, washed, dried for 2-5h at the temperature of 50-70 ℃, put into a box-type muffle furnace, and sintered for 8h at the temperature of 450-520 ℃ to obtain black solid of manganese dioxide, namely a product C.
5. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (4), adding the product C, nickel acetate tetrahydrate, lithium acetate and aluminum nitrate into 20-30ml of ethanol solution; wherein the molar ratio of the product C, the nickel acetate tetrahydrate, the lithium acetate and the aluminum nitrate is 1.45:0.5:1: 0.05.
6. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (4), ultrasonic dispersion is carried out for 10-20min, and drying is carried out for 1-2h at the temperature of 90-100 ℃.
7. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (5), the product D is ground to 0.001-0.005mm, then is added into a magnetic boat, is heated to 700-900 ℃ from room temperature at 4-6 ℃/min, is sintered at the temperature of 700-900 ℃ for 10-17 hours, and is cooled to obtain the product E.
8. The doping modification method of the lithium nickel manganese oxide positive electrode material according to claim 1, characterized by comprising the following steps: in the step (6), grinding the product E to 0.001-0.005mm to obtain a finished product.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898799A (en) * | 2010-07-28 | 2010-12-01 | 复旦大学 | Method for preparing lithium manganate hollow ball material |
| CN109643787A (en) * | 2016-06-24 | 2019-04-16 | 宝马股份公司 | The purposes of electrode material, electrode material for the electrochemical cell based on lithium ion, the electrochemical cell based on lithium ion |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898799A (en) * | 2010-07-28 | 2010-12-01 | 复旦大学 | Method for preparing lithium manganate hollow ball material |
| CN109643787A (en) * | 2016-06-24 | 2019-04-16 | 宝马股份公司 | The purposes of electrode material, electrode material for the electrochemical cell based on lithium ion, the electrochemical cell based on lithium ion |
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