CN111293305B - Hexagonal flaky nickel cobalt lithium manganate precursor and preparation method thereof - Google Patents
Hexagonal flaky nickel cobalt lithium manganate precursor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hexagonal flaky nickel cobalt lithium manganate precursor and a preparation method thereof. The hexagonal flaky high-nickel cobalt lithium manganate precursor increases nucleation amount of coprecipitation reaction by adding crystal face growth inducer from microscopic morphology of the material, controls growth speed of crystal grains, and generates uniform and concentrated precipitate particles with uniform particle size distribution, so that the precipitate particles preferentially grow on a certain/certain crystal face to form crystal particles with regular hexagonal flaky structure and are inserted into the precursor, the vertical embedded flaky structure which is a punctiform, needle-shaped or flat flaky structure is avoided, the rapid embedded structure of lithium ions in the sintering process is facilitated, the sintering process can be effectively simplified, the sintering temperature is reduced, and the uniform monocrystalline cathode material is facilitated after sintering.
Description
Technical Field
The invention belongs to the field of lithium ion battery materials, and particularly relates to a hexagonal flaky nickel cobalt lithium manganate precursor and a preparation method thereof.
Background
As the demand of new energy automobile markets is increasing, the demand of domestic lithium ion batteries is also rapidly increasing. The positive electrode material of the lithium ion battery directly affects the comprehensive performance of the lithium ion battery and is considered as the most critical part of the lithium ion battery. At present, most of the anode materials researched by various factories at home and abroad are secondary spherical particles formed by agglomeration of fine grains. Conventional ternary materials are typically formed into secondary spheres of about ten microns in size agglomerated from primary particles in order to increase density. However, when the secondary spherical particles are used for manufacturing battery pole pieces, the secondary spherical particles are easy to break under higher rolling pressure. Moreover, the volumetric expansion and contraction of the electrode material during cycling can also lead to breakage of the material particles. The breaking of the secondary particles can expose the internal active substances, increase side reactions with the electrolyte and exacerbate metal ion dissolution, resulting in reduced electrical performance.
The monocrystal material has excellent mechanical strength and pressure resistance, and is not easy to break during compacting, so that it is not easy to break during electrode rolling and charging and discharging. The single crystal ternary material has become an important development direction of ternary materials because the number of grain boundaries is small, stress concentration points are small, interfaces are stable, the generation and diffusion of microcracks caused by phase change of the positive electrode material in the charging and discharging processes can be reduced, and the contact interface between the active material and the electrolyte is reduced, so that the generation of gas is reduced.
For the synthesis of single crystal ternary materials, the selection of the appropriate precursor is critical. The physical and chemical properties of the precursor, such as crystal structure, microscopic morphology, particle size distribution, and the like determine the comprehensive performance of the later-stage positive electrode material. However, the existing monocrystal ternary precursor has the problems of high crystal nucleus crystallization degree and long grain growth time, and most of the monocrystal ternary precursor needs to be subjected to secondary roasting, so that the processing cost of the material is increased, and the energy consumption is high.
Disclosure of Invention
The invention aims to provide a hexagonal flaky nickel cobalt lithium manganate precursor with low cost and unique microstructure and a preparation method thereof.
The hexagonal flaky nickel cobalt lithium manganate precursor provided by the invention has the advantages that the primary particles are of a hexagonal flaky structure, and the secondary particles are loose particles formed by stacking flaky hexagons in an embedding manner.
The D50 of the nickel cobalt lithium manganate precursor is 3-5 um, and the length of the primary particle sheet is 400-600 nm.
The molecular formula of the nickel cobalt lithium manganate precursor is Ni a Co b Mn c (OH) 2 Wherein a+b+c=1, a is equal to or greater than 0.6, b is equal to or less than 0.2, and c is equal to or less than 0.2.
The preparation method of the hexagonal flaky nickel cobalt lithium manganate precursor comprises the following steps:
(1) Solution preparation: according to formula Ni a Co b Mn c (OH) 2 Preparing a soluble salt solution according to the molar ratio of metal elements Ni, co and Mn, wherein a+b+c=1, a is more than or equal to 0.6, b is less than or equal to 0.2, and c is less than or equal to 0.2; complexing agent is prepared into complexing agent aqueous solution; preparing a precipitant into a precipitant water solution; dispersing a crystal face growth inducer into water to serve as a reaction base solution;
(2) Coprecipitation reaction: placing the reaction base solution into a reaction kettle, starting stirring, then adding the soluble salt solution, the complexing agent solution and the precipitant solution into the reaction kettle in parallel flow under the protection of inert gas and at a set temperature, starting precipitation reaction, and stopping adding the solution in parallel flow after the reaction is finished to obtain a reaction product;
(3) Preparing a precursor: and (3) aging, washing, filtering, drying and sieving the reaction product in the step (2) to obtain a precursor.
In the step (1), the total concentration of metal ions in the soluble salt solution is 0.5-5 mol, the soluble nickel salt is one of nickel sulfate, nickel nitrate, nickel acetate and nickel chloride, the soluble cobalt salt is one of cobalt sulfate, cobalt nitrate, cobalt acetate and cobalt chloride, and the soluble manganese salt is one of manganese sulfate, manganese nitrate, manganese acetate and manganese chloride; the complexing agent is one of ammonia water, ammonium bicarbonate and ammonium carbonate, and the concentration of the complexing agent aqueous solution is 2-14 mol/L; the precipitant is one of sodium hydroxide, potassium hydroxide and lithium hydroxide, and the concentration of the aqueous solution of the precipitant is 1-10 mol/L; the crystal face growth inducer is one or more of polyacrylamide, polyvinyl alcohol, polyethylene oxide, sodium polyacrylate, sodium alginate and polyvinylpyrrolidone, and the mass ratio of the crystal face growth inducer to the aqueous solution is (0.01-0.1)%: 1.
In the step (2), the temperature is set to be 40-80 ℃ and the stirring speed is 200-1200 r/min; when the three solutions are added in parallel, the pH value of the reaction system needs to be controlled to be 11.0-12.5, the increase of the pH value is favorable for leading the nucleation speed of crystal grains to be larger than the growth speed at the initial stage of the reaction, so that a precursor with uniform and concentrated particle size distribution is obtained, and the increase of ammonia water is favorable for changing the shape and the size of primary particles. The solid content in the reaction system is controlled to be 50-220 g/L, and the residence time of the materials in the reactor is controlled to be 5-50 h.
Preferably, the stirring speed is 300-900 r/min; when the stirring rotation speed is controlled to be 300-900 r/min, particles with too low stirring speed cannot obtain sufficient friction, collision and shearing, so that the tap density of the particles can be reduced, and when the stirring speed is too high, the reaction time can be prolonged, and the cost is increased.
Preferably, the complexing agent is ammonia water, and in the coprecipitation reaction, the concentration of the ammonia water of the reaction system is controlled to be 10-28 g/L;
in the step 3), during aging, the stirring speed is reduced to 100-500 r/min, and the aging time is controlled to be 4-48 h; during washing, sodium hydroxide solution is adopted for washing; when drying, the drying temperature is 60-150 ℃ until the material is light black or dark brown.
The principle of the invention is as follows: the crystal face growth inducer is added into the precursor in the synthesis process, and the effect of the crystal face growth inducer is as follows: (1) the method is favorable for reducing the supersaturation degree of the system in the initial stage of the reaction, forming a large number of crystal nuclei and controlling the growth speed of crystal grains, thereby generating particles with uniform and concentrated particle size distribution. (2) The precipitated particles preferentially grow on a certain crystal face or certain crystal faces to form crystal particles with regular hexagonal flaky structures, so that the crystal particles are prevented from forming a punctiform, needle-shaped or tiled flaky structure. This structure is advantageous for forming a uniform single crystal positive electrode material after sintering. However, the mass of the crystal face growth inducer is not more than 0.1% of the mass of the base solution, excessive organic matters can influence a precipitation system after entering precipitation, and the higher the oil content of the feed liquid is, the lower the tap density is, so that particles cannot grow, and the particle size distribution is widened.
The invention has the beneficial effects that: 1) The primary particles of the precursor are hexagonal flaky, and the primary flaky particles are stacked to form secondary particles with a loose structure, so that the structure is favorable for forming a single crystal positive-stage material with stable, superior and uniform performance after sintering. 2) The hexagonal flaky high-nickel cobalt lithium manganate precursor increases nucleation amount of coprecipitation reaction by adding crystal face growth inducer from microscopic morphology of the material, controls growth speed of crystal grains, and generates uniform and concentrated precipitate particles with uniform particle size distribution, so that the precipitate particles preferentially grow on a certain/certain crystal face to form crystal particles with regular hexagonal flaky structure and are inserted into the precursor, the vertical embedded flaky structure which is a punctiform, needle-shaped or flat flaky structure is avoided, the rapid embedded structure of lithium ions in the sintering process is facilitated, the sintering process can be effectively simplified, the sintering temperature is reduced, and the uniform monocrystalline cathode material is facilitated after sintering. 3) The production method of the hexagonal flaky high-nickel cobalt lithium manganate precursor is simple and feasible, can effectively save cost and is easy to realize industrialization. 4) The hexagonal flaky nickel cobalt lithium manganate precursor provided by the invention is high in specific capacity and good in cycle performance.
Drawings
FIG. 1 is a scanning electron microscope image of a hexagonal flaky lithium nickel cobalt manganese oxide precursor prepared in example 1
Fig. 2 is an electron microscope scanning photograph of the lithium nickel cobalt manganese oxide single crystal positive electrode material prepared in example 1.
FIG. 3 is a scanning electron microscope image of a hexagonal plate-shaped lithium nickel cobalt manganese oxide precursor prepared in example 2
Fig. 4 is a scanning electron microscope image of the nickel cobalt lithium manganate single crystal positive electrode material prepared in example 2.
FIG. 5 is a scanning electron microscope image of a hexagonal plate-shaped lithium nickel cobalt manganese oxide precursor prepared in example 3
Fig. 6 is a scanning electron microscope image of a hexagonal plate-shaped lithium nickel cobalt manganese oxide precursor prepared in comparative example 1.
FIG. 7 is a scanning electron microscope image of the nickel cobalt lithium manganate single crystal positive electrode material prepared in comparative example 1.
Detailed Description
Example 1
The molecular formula of the hexagonal flaky nickel cobalt lithium manganate precursor in the embodiment is Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 。
The preparation method comprises the following steps:
(1) Preparing nickel sulfate, cobalt sulfate and manganese sulfate into nickel cobalt manganese salt solution with total metal ion concentration of 2mol/L (wherein the nickel ion concentration is 1.6mol/L, the cobalt particle concentration is 0.2mol/L and the manganese ion concentration is 0.2 mol/L) according to the molar ratio of nickel, cobalt and manganese in the molecular formula; the sodium hydroxide solution is prepared into a precipitator solution with the concentration of 4mol/L, and the ammonia water is prepared into a complexing agent solution with the concentration of 6 mol/L.
(2) Adding 5L of deionized water and 5g of polyacrylamide into a reaction kettle, starting stirring, controlling the rotating speed at 600r/min, heating to 60 ℃, and continuously introducing nitrogen.
(3) And (3) adding the metal salt solution, the precipitant solution and the complexing agent solution in the step (1) into a reaction kettle in parallel flow for coprecipitation reaction, keeping the pH value stable at 12.0 during the reaction, controlling the solid matter content in the reaction system to be 80g/L, controlling the concentration of ammonia water in the reaction system to be 28g/L, and continuously reacting for 37 hours to finish the reaction.
(4) Stopping feeding after the reaction is finished, aging for 8 hours at the rotating speed of 300r/min, washing, filtering and drying for 12 hours at the temperature of 100 ℃ after the aging is finished, thus obtaining the hexagonal flaky high-nickel cobalt lithium manganate precursor.
The precursor prepared in this example was subjected to SEM test, and its microscopic morphology is shown in fig. 1, and as can be seen from fig. 1, the primary particles of the precursor are hexagonal flakes, and the hexagonal flakes are stacked to form secondary particles having a loose structure. The precursor was tested to have a median particle size of 3.0 μm and a length of the complete primary particles (platelet hexagons) of 500 to 600nm.
After the precursor of this example was sintered at high temperature with lithium, a nickel cobalt lithium manganate single crystal positive electrode material was obtained, SEM analysis was performed on the positive electrode material, the result is shown in fig. 2, and the nickel cobalt lithium manganate positive electrode material was fabricated into a battery, and the electrochemical performance data is shown in table 1.
Example 2
The molecular formula of the hexagonal flaky nickel cobalt lithium manganate precursor in the embodiment is Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 。
The preparation method comprises the following steps:
(1) Preparing nickel sulfate, cobalt sulfate and manganese sulfate into nickel cobalt manganese salt solution with total metal ion concentration of 1.5mol/L (wherein nickel ion concentration is 1.2mol/L, cobalt particle concentration is 0.15mol/L and manganese ion concentration is 0.15 mol/L) according to the molar ratio of nickel, cobalt and manganese in the molecular formula; the sodium hydroxide solution is prepared into a precipitator solution with the concentration of 5mol/L, and the ammonia water is prepared into a complexing agent solution with the concentration of 8 mol/L.
(2) Adding 5L of deionized water and 5g of polyacrylamide into a reaction kettle, starting stirring, controlling the rotating speed at 800r/min, heating to 55 ℃, and continuously introducing nitrogen.
(3) And (3) adding the metal salt solution, the precipitant solution and the complexing agent solution in the step (1) into a reaction kettle in parallel flow for coprecipitation reaction, keeping the pH value stable at 11.6 during the reaction, controlling the solid matter content in the reaction system to be 100g/L, controlling the concentration of ammonia water in the reaction system to be 28g/L, and continuously reacting for 21h.
(4) Stopping feeding after the reaction is finished, aging for 12 hours at the rotating speed of 400r/min, washing, filtering and drying for 12 hours at 120 ℃ after the aging is finished, thus obtaining the hexagonal flaky high-nickel cobalt lithium manganate precursor.
The precursor prepared in this example was subjected to SEM test, and its microscopic morphology is shown in fig. 3, and as can be seen from fig. 1, the primary particles of the precursor are hexagonal flakes, and the hexagonal flakes are stacked to form secondary particles having a loose structure. The precursor was tested to have a median particle size of 5.5 μm and a length of the complete primary particles (platelet hexagons) of 400 to 500nm.
After the precursor of this example was sintered at high temperature with lithium, a nickel cobalt lithium manganate single crystal positive electrode material was obtained, SEM analysis was performed on the positive electrode material, the result is shown in fig. 4, and the nickel cobalt lithium manganate positive electrode material was fabricated into a battery, and the electrochemical performance data is shown in table 1.
Example 3
The molecular formula of the hexagonal flaky nickel cobalt lithium manganate precursor in the embodiment is Ni 0.6 Co 0.2 Mn 0.2 (OH) 2 。
The preparation method comprises the following steps:
(1) Preparing nickel sulfate, cobalt sulfate and manganese sulfate into nickel cobalt manganese salt solution with the total concentration of metal ions of 2.5mol/L according to the molar ratio of nickel, cobalt and manganese in the molecular formula (wherein the concentration of nickel ions is 1.5mol/L, the concentration of cobalt particles is 0.5mol/L and the concentration of manganese ions is 0.5 mol/L); the sodium hydroxide solution is prepared into a precipitator solution with the concentration of 9mol/L, and the ammonia water is prepared into a complexing agent solution with the concentration of 11 mol/L.
(2) Adding 5L of deionized water and 0.5g of polyacrylamide into a reaction kettle, starting stirring, controlling the rotating speed at 900r/min, heating to 50 ℃, and continuously introducing nitrogen.
(3) And (3) adding the metal salt solution, the precipitant solution and the complexing agent solution in the step (1) into a reaction kettle in parallel flow for coprecipitation reaction, keeping the pH value stable at 12.0 during the reaction, controlling the solid matter content in the reaction system to be 110g/L, controlling the concentration of ammonia water in the reaction system to be 18g/L, and continuously reacting for 28h to finish the reaction.
(4) Stopping feeding after the reaction is finished, aging for 12 hours at the rotating speed of 400r/min, washing, filtering and drying for 12 hours at 120 ℃ after the aging is finished, thus obtaining the hexagonal flaky high-nickel cobalt lithium manganate precursor.
The precursor prepared in this example was subjected to SEM test, and its microscopic morphology is shown in fig. 5, and as can be seen from fig. 5, the primary particles of the precursor are hexagonal flakes, and the surface structure of the secondary particles is loose. The precursor was tested to have a median particle size of 3.5 μm and a length of the complete primary particles (platelet hexagons) of 500 to 600nm.
Comparative example 1
In this comparative example, the molecular formula of the precursor is Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 ，
The preparation method comprises the following steps:
(1) Preparing nickel sulfate, cobalt sulfate and manganese sulfate into nickel cobalt manganese salt solution with total metal ion concentration of 2mol/L (wherein the nickel ion concentration is 1.6mol/L, the cobalt particle concentration is 0.2mol/L and the manganese ion concentration is 0.2 mol/L) according to the molar ratio of nickel, cobalt and manganese in the molecular formula; the sodium hydroxide solution is prepared into a precipitator solution with the concentration of 4mol/L, and the ammonia water is prepared into a complexing agent solution with the concentration of 6 mol/L.
(2) Adding 5L of deionized water into a reaction kettle, adding ammonia water and sodium hydroxide to enable the pH to be 12.1, taking the mixture as a reaction base solution, starting stirring, controlling the rotating speed to be 600r/min, heating to 60 ℃, and continuously introducing nitrogen.
(3) And (3) adding the metal salt solution, the precipitator solution and the complexing agent ammonia solution in the step (1) into a reaction kettle in parallel flow for coprecipitation reaction, keeping the pH value stable at 12.1 during the reaction, controlling the solid matter content in the reaction system to be 80g/L, controlling the concentration of ammonia water in the reaction system to be 28g/L, continuously reacting for 37 hours, and stopping feeding.
(4) Stopping feeding after the reaction is finished, aging for 8 hours at the rotating speed of 300r/min, washing, filtering and drying for 12 hours at the temperature of 100 ℃ after the aging is finished, thus obtaining the nickel cobalt lithium manganate monocrystal precursor.
The precursor prepared in this comparative example was subjected to SEM characterization, and the results are shown in FIG. 6, precursor Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 The primary particles are grain-shaped, the secondary particles are spheroid with good dispersibility, uniform particles and compact interior, the particle size in the precursor is about 5.0 mu m, and the length of the primary particles is 200-300 nm.
The precursor of the comparative example is matched with lithium to be sintered at high temperature to obtain a nickel cobalt lithium manganate monocrystal positive electrode material, the result of SEM analysis of the positive electrode material is shown in figure 7, the nickel cobalt lithium manganate positive electrode material is prepared into a battery, the electrochemical performance data of the battery are shown in table 1,
table 1 electrochemical properties of the batteries in examples 1-2 and comparative example
Example 4
The molecular formula of the hexagonal flaky nickel cobalt lithium manganate precursor in the embodiment is Ni 0.7 Co 0.15 Mn 0.15 (OH) 2 。
The preparation method comprises the following steps:
(1) Preparing nickel sulfate, cobalt sulfate and manganese sulfate into nickel cobalt manganese salt solution with total metal ion concentration of 5mol/L (wherein the nickel ion concentration is 3.5mol/L, the cobalt particle concentration is 0.75mol/L and the manganese ion concentration is 0.75 mol/L) according to the molar ratio of nickel, cobalt and manganese in the molecular formula; the sodium hydroxide solution is prepared into a precipitator solution with the concentration of 6mol/L, and the ammonia water is prepared into a complexing agent solution with the concentration of 6 mol/L.
(2) Adding 5L of deionized water and 0.5g of polyacrylamide into a reaction kettle, starting stirring, controlling the rotating speed at 900r/min, heating to 80 ℃, and continuously introducing nitrogen.
(3) And (3) adding the metal salt solution, the precipitant solution and the complexing agent solution in the step (1) into a reaction kettle in parallel flow for coprecipitation reaction, keeping the pH value stable at 12.0 during the reaction, controlling the solid matter content in the reaction system to be 200g/L, controlling the concentration of ammonia water in the reaction system to be 28g/L, and continuously reacting for 50h, thus finishing the reaction.
(4) Stopping feeding after the reaction is finished, aging for 12 hours at the rotating speed of 400r/min, washing, filtering and drying for 12 hours at 120 ℃ after the aging is finished, thus obtaining the hexagonal flaky high-nickel cobalt lithium manganate precursor.
Example 5
The molecular formula of the hexagonal flaky nickel cobalt lithium manganate precursor in the embodiment is Ni 0.8 Co 0.2 Mn 0.2 (OH) 2 。
The preparation method comprises the following steps:
(1) Preparing nickel sulfate, cobalt sulfate and manganese sulfate into nickel cobalt manganese salt solution with total metal ion concentration of 1.0mol/L (wherein nickel ion concentration is 0.8mol/L, cobalt particle concentration is 0.2mol/L and manganese ion concentration is 0.2 mol/L) according to the molar ratio of nickel, cobalt and manganese in the molecular formula; the sodium hydroxide solution is prepared into a precipitant solution with the concentration of 2mol/L, and the ammonia water is prepared into a complexing agent solution with the concentration of 1 mol/L.
(2) Adding 5L of deionized water and 3g of polyacrylamide into a reaction kettle, starting stirring, controlling the rotating speed at 400r/min, heating to 40 ℃, and continuously introducing nitrogen.
(3) And (3) adding the metal salt solution, the precipitant solution and the complexing agent solution in the step (1) into a reaction kettle in parallel flow for coprecipitation reaction, keeping the pH value stable at 11.4 during the reaction, controlling the solid matter content in the reaction system to be 50g/L, controlling the concentration of ammonia water in the reaction system to be 10g/L, and continuously reacting for 50h, thus finishing the reaction.
(4) Stopping feeding after the reaction is finished, aging for 10 hours at the rotating speed of 300r/min, washing, filtering and drying for 12 hours at the temperature of 100 ℃ after the aging is finished, thus obtaining the hexagonal flaky high-nickel cobalt lithium manganate precursor.
Claims (4)
1. The hexagonal flaky lithium nickel cobalt manganese oxide precursor is characterized in that primary particles are of a hexagonal flaky structure, and secondary particles are loose particles formed by stacking flaky hexagons in an embedding manner;
the molecular formula of the nickel cobalt lithium manganate precursor is Ni a Co b Mn c (OH) 2 Wherein a+b+c=1, a is not less than 0.6, b is not less than 0.2, and c is not more than 0.2; the D50 of the nickel cobalt lithium manganate precursor is 3-6 um, and the length of the primary particle sheet is 400-600 nm;
the preparation method of the hexagonal flaky nickel cobalt lithium manganate precursor comprises the following steps:
(1) Solution preparation: according to formula Ni a Co b Mn c (OH) 2 Preparing a soluble salt solution by the molar ratio of metal elements Ni, co and Mn; complexing agent is prepared into complexing agent aqueous solution; preparing a precipitant into a precipitant water solution; dispersing a crystal face growth inducer into water to serve as a reaction base solution;
(2) Coprecipitation reaction: placing the reaction base solution into a reaction kettle, starting stirring, then adding the soluble salt solution, the complexing agent aqueous solution and the precipitant aqueous solution into the reaction kettle in parallel flow under the protection of inert gas and at a set temperature, starting precipitation reaction, and stopping adding the solution in parallel flow after the reaction is finished to obtain a reaction product;
(3) Preparing a precursor: aging, washing, filtering, drying and sieving the reaction product in the step (2) to obtain a precursor;
in the step (1), the total concentration of metal ions in the soluble salt solution is 0.5-5 mol/L, the soluble nickel salt is one of nickel sulfate, nickel nitrate, nickel acetate and nickel chloride, the soluble cobalt salt is one of cobalt sulfate, cobalt nitrate, cobalt acetate and cobalt chloride, and the soluble manganese salt is one of manganese sulfate, manganese nitrate, manganese acetate and manganese chloride; the complexing agent is one of ammonia water, ammonium bicarbonate and ammonium carbonate, and the concentration of the complexing agent aqueous solution is 2-14 mol/L; the precipitant is one of sodium hydroxide, potassium hydroxide and lithium hydroxide, and the concentration of the aqueous solution of the precipitant is 1-10 mol/L; the crystal face growth inducer is polyacrylamide, and the ratio of the mass of the inducer to the mass of water in the reaction base solution is (0.01-0.1)%;
in the step (2), the temperature is set to be 40-80 ℃, and the stirring speed is 200-1200 r/min; when the three solutions are added in parallel, the pH value of the reaction system is controlled to be 11.0-12.5, the solid content in the reaction system is controlled to be 5-220 g/L, and the residence time of the materials in the reactor is controlled to be 5-50 h.
2. The hexagonal flake lithium nickel cobalt manganese oxide precursor according to claim 1, wherein in the step (2), the stirring speed is 300-900 r/min.
3. The hexagonal flaky lithium nickel cobalt manganese oxide precursor according to claim 1, wherein the concentration of the complexing agent ammonia water in the coprecipitation reaction is controlled to be 10-35 g/L.
4. The hexagonal flaky lithium nickel cobalt manganese oxide precursor according to claim 1, wherein in the step (3), the stirring speed is reduced to 100-500 r/min during aging, and the aging time is controlled to be 4-48 h; during washing, sodium hydroxide solution is adopted for washing; and (3) in the drying process, the drying temperature is 60-150 ℃ until the material is light black or dark brown.
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| CN112768682B (en) * | 2020-09-25 | 2022-06-17 | 深圳石墨烯创新中心有限公司 | Preparation method of plate-shaped high-nickel single crystal ternary material |
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