CN109560283B - Preparation method of nickel-cobalt-aluminum ternary precursor with continuous concentration gradient - Google Patents
Preparation method of nickel-cobalt-aluminum ternary precursor with continuous concentration gradient Download PDFInfo
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Abstract
The invention relates to the field of preparation of lithium ion battery anode materials, in particular to a preparation method of a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient, which is characterized by comprising the following steps: (1) adding a mixed solution of a nickel solution, a cobalt solution, an aluminum solution, a complexing agent and a precipitator into a reaction kettle in a parallel flow manner; (2) in the material adding process, adding deionized water into a nickel solution, adding a high-concentration cobalt solution into the cobalt solution until the concentration of the nickel solution is 0.1M or the concentration of the cobalt solution is 1M, stopping adding the raw materials, continuously stirring in the whole process to ensure the uniformity of the solution, controlling the pH value of a reaction system to be 10.5-12, controlling the temperature to be 55-65 ℃, and continuously aging for 6-24 hours after the feeding is stopped; (3) and after aging, taking out the materials, carrying out solid-liquid separation, washing and drying to obtain the nickel-cobalt-aluminum ternary precursor with continuous concentration gradient.
Description
Technical Field
The invention relates to the field of preparation of lithium ion battery anode materials, in particular to a preparation method of a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient.
Background
Lithium ion batteries have a series of advantages of large energy density, long cycle life and the like, and are widely applied to digital, energy storage and electric automobiles at present. At present, the energy density of the lithium battery is mostly 140wh/kg, and the endurance mileage of the corresponding electric vehicle is about 300 kilometers, which far meets the requirement of people on the long endurance mileage of the vehicle.
In order to develop lithium ion batteries with higher energy density, researchers have focused their major efforts on battery positive electrode materials, since the performance of the positive electrode materials largely determines the performance of the batteries. The nickel-cobalt-aluminum ternary cathode material is considered to be a material with high energy density and has excellent safety. The preparation of the nickel-cobalt-aluminum ternary material also needs to prepare an ideal precursor.
However, preparing the ideal precursors faces a number of challenges. Firstly, the hydroxides of three metal elements of nickel, cobalt and aluminum have great solubility product difference, which causes that the three elements are difficult to be uniformly precipitated. Can be solved to a certain extent by adopting sodium metaaluminate or complexing mode for aluminum. Secondly, due to the high nickel content of the nickel-cobalt-aluminum ternary precursor, nickel and lithium are easy to be mixed and discharged in the sintering process of the material, so that the cycle performance of the material is remarkably reduced. Finally, during the charging and discharging process of the battery, the nickel and the electrolyte generate side reaction, and the cycle performance of the material is also reduced. For this reason, we need to prepare a ternary precursor with gradually decreasing nickel concentration. For example, chinese patent CN103715424B discloses a core-shell structure cathode material and a method for preparing the same, wherein nickel-cobalt two-element is first precipitated, and then a layer of aluminum hydroxide is deposited and coated on the surface of the nickel-cobalt two-element, however, the aluminum layer on the surface does not participate in the electrochemical reaction, and the electronic conductivity and the ion diffusivity of the material are reduced, so that the capacity cannot be effectively exerted, and the energy density of the battery is low. For another example, chinese patent CN106207140A discloses a method for preparing a multiple core-shell structure nickel-cobalt-aluminum composite, which prepares a precursor with high internal nickel content and low external nickel content through multiple coprecipitation reactions, the precursor prepared by the method is composed of several layers of coating layers with different nickel-cobalt concentrations, interfaces exist between the coating layers, and due to different components between the coating layers, different volume changes occur during the charging and discharging processes of the battery, and the cycle performance of the battery becomes poor. In addition, the method has complex process and is not suitable for industrial production.
Disclosure of Invention
In order to solve the problems, the inventor skillfully designs a preparation method of a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient.
In order to realize the technical purpose of the invention, the invention adopts the following technical scheme:
a preparation method of a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient comprises the following steps:
(1) adding a nickel solution, a cobalt solution, an aluminum solution and a mixed solution of a complexing agent and a precipitating agent into a reaction kettle in a parallel flow manner;
(2) in the adding process of the raw materials, deionized water is added into the nickel solution to continuously reduce the concentration of nickel in the nickel solution; adding a high-concentration cobalt solution into the cobalt solution to continuously increase the concentration of cobalt in the cobalt solution, and stopping adding the raw materials into the reaction kettle when the concentration of the nickel solution is 0.1M or the concentration of the cobalt solution is 1M;
(3) and after the reaction is finished, performing solid-liquid separation, washing and drying on the materials to obtain the nickel-cobalt-aluminum ternary precursor with continuous concentration gradient.
Preferably, the salt used for preparing the nickel solution is nickel sulfate; the salt used for preparing the cobalt solution is cobalt sulfate; the salt used for preparing the aluminum solution is sodium metaaluminate.
Preferably, the complexing agent in the step (1) is ammonia water, and the precipitator is sodium hydroxide.
Preferably, the concentration of the nickel solution in the step (1) is 1-2M; the concentration of the cobalt solution is 0.5-1M; the concentration of the aluminum solution is 0.2-0.5M; the concentration of ammonia water is 1-3M; the concentration of the sodium hydroxide is 3-6M.
Preferably, the concentration of the high-concentration cobalt solution in the step (2) is 1-1.5M.
Preferably, the flow rate of deionized water added into the nickel solution in the step (2) is 0.1-1L/h; the flow rate of adding the high-concentration cobalt solution into the cobalt solution is 0.1-1L/h.
Preferably, the molar ratio of nickel, cobalt and aluminum in the system in the step (2) is 0.70-0.90: 0.08-0.20: 0.02-0.06.
Preferably, the temperature in the system in the step (2) is 55-65 ℃; the pH value is 10.5-12; the aging time is 6-24 h.
More specifically, ammonia water is added into the reaction device to control the pH value of the reaction to be 10.5-12.
Preferably, the material in the step (3) is washed by hot alkali solution with the pH of 10.5-12 and deionized water successively.
More preferably, in the step (3), the material is washed twice by using a sodium hydroxide solution with the pH of 10.5-12 and the temperature of 55-65 ℃, then washed twice in deionized water, dried for 24 hours at 120 ℃, and sieved by a 200-mesh sieve to obtain the nickel-cobalt-aluminum ternary precursor with continuous concentration.
The beneficial effects of the method are as follows:
1. the nickel-cobalt-aluminum ternary precursor prepared by the method has a continuous concentration gradient, the nickel concentration is gradually reduced from inside to outside, the cobalt concentration is gradually increased, and no obvious interface layer exists.
2. The method realizes the continuous concentration gradient of the nickel-cobalt-aluminum ternary precursor by gradually changing the concentration of the nickel-cobalt solution, and has the advantages of simple process, good product stability and good cycle performance.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a graph of the cycling performance at 0.1C for coin cells made from the samples of example 1.
Detailed description of the preferred embodiment
The present invention will be further described with reference to the following examples. The described embodiments and their results are only intended to illustrate the invention and should not be taken as limiting the invention described in detail in the claims.
Example 1
Preparing solution
Deionized water is used for preparing a nickel sulfate solution with the concentration of 1.5M, a cobalt sulfate solution with the concentration of 0.5M, a sodium metaaluminate solution with the concentration of 0.2M and a mixed solution of ammonia water and sodium hydroxide, wherein the concentration of the ammonia water is 2M, and the concentration of the sodium hydroxide is 4M.
Reaction of
10L of dilute ammonia solution is added into a 100L reaction kettle, and the solution is respectively added into the reaction kettle in a parallel flow mode. Adjusting the concentration of the nickel solution and the cobalt solution at the beginning of adding the raw materials into the reaction kettle: deionized water was added to the nickel solution at a flow rate of 0.5L/h, and a cobalt solution at a concentration of 1.2M was added to the cobalt solution at a flow rate of 0.5L/h. When the concentration of the nickel solution is 0.1M or the cobalt solution is 1M, stopping adding the raw materials into the reaction kettle, and aging for 10 hours. The pH value of the whole process system is 11, and the reaction temperature is 60 ℃.
Post-treatment
Taking the materials out of the reaction kettle, carrying out solid-liquid separation, washing twice by using a sodium hydroxide solution with the pH value of 11 and the temperature of 60 ℃, and washing twice by using deionized water. Drying the cleaned material at 120 deg.C for 24h, sieving with 200 mesh sieve to obtain nickel cobalt aluminum ternary precursor with continuous concentration gradient, wherein the chemical formula is Ni0.82CO0.12Al0.06(OH)2。
After the button cell prepared by the sample is charged and discharged for 50 times at 0.1 ℃, the capacity is 177.7mAh/g, and the capacity retention rate is 97.3%.
Example 2
Preparing solution
Deionized water is used for preparing a nickel sulfate solution with the concentration of 2M, a cobalt sulfate solution with the concentration of 1M, a sodium metaaluminate solution with the concentration of 0.5M and a mixed solution of ammonia water and sodium hydroxide, wherein the concentration of the ammonia water is 3M, and the concentration of the sodium hydroxide is 6M.
Reaction of
15L of dilute ammonia solution was added to a 100L reactor, and the above solutions were each added to the reactor cocurrently. Adjusting the concentration of the nickel solution and the cobalt solution at the beginning of adding the raw materials into the reaction kettle: deionized water was added to the nickel solution at a flow rate of 1L/h, and a cobalt solution at a concentration of 1M was added to the cobalt solution at a flow rate of 1L/h. When the concentration of the nickel solution is 0.1M or the cobalt solution is 1M, stopping adding the raw materials into the reaction kettle, and aging for 12 hours. The pH of the whole process system is 11.5, and the reaction temperature is 65 ℃.
Post-treatment
Taking the materials out of the reaction kettle, carrying out solid-liquid separation, washing twice by using a sodium hydroxide solution with the pH value of 11.5 and the temperature of 65 ℃, and then washing twice by using deionized water. Drying the cleaned material at 120 ℃ for 24h, sieving with a 200-mesh sieve to obtain a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient,having a chemical formula of Ni0.80CO0.15Al0.05(OH)2。
After the button cell prepared by the sample is charged and discharged for 50 times at 0.1 ℃, the capacity is 175.6mAh/g, and the capacity retention rate is 97.5%.
Example 3
Preparing solution
Deionized water is used for preparing a nickel sulfate solution with the concentration of 1M, a cobalt sulfate solution with the concentration of 0.3M, a sodium metaaluminate solution with the concentration of 0.3M and a mixed solution of ammonia water and sodium hydroxide, wherein the concentration of the ammonia water is 1M, and the concentration of the sodium hydroxide is 3M.
Reaction of
A100L reaction vessel was charged with 20L of a dilute aqueous ammonia solution, and the solutions were each fed into the reaction vessel in parallel. Adjusting the concentration of the nickel solution and the cobalt solution at the beginning of adding the raw materials into the reaction kettle: deionized water was added to the nickel solution at a flow rate of 0.1L/h, and a cobalt solution at a concentration of 1.5M was added to the cobalt solution at a flow rate of 0.5L/h. When the concentration of the nickel solution is 0.1M or the cobalt solution is 1M, stopping adding the raw materials into the reaction kettle, and aging for 24 hours. The pH of the whole process system is 12, and the reaction temperature is 55 ℃.
Post-treatment
Taking the materials out of the reaction kettle, carrying out solid-liquid separation, washing twice by using a sodium hydroxide solution with the pH value of 12 and the temperature of 55 ℃, and washing twice by using deionized water. Drying the cleaned material at 120 deg.C for 24h, sieving with 200 mesh sieve to obtain nickel cobalt aluminum ternary precursor with continuous concentration gradient, wherein the chemical formula is Ni0.72CO0.18Al0.10(OH)2。
After the button cell prepared by the sample is charged and discharged for 50 times at 0.1 ℃, the capacity is 169.8mAh/g, and the capacity retention rate is 98.1%.
Example 4
Preparing solution
Deionized water is used for preparing a nickel sulfate solution with the concentration of 1.6M, a cobalt sulfate solution with the concentration of 0.8M, a sodium metaaluminate solution with the concentration of 0.4M and a mixed solution of ammonia water and sodium hydroxide, wherein the concentration of the ammonia water is 1M, and the concentration of the sodium hydroxide is 4M.
Reaction of
10L of dilute ammonia solution is added into a 100L reaction kettle, and the solution is respectively added into the reaction kettle in a parallel flow mode. Adjusting the concentration of the nickel solution and the cobalt solution at the beginning of adding the raw materials into the reaction kettle: deionized water was added to the nickel solution at a flow rate of 0.5L/h, and a cobalt solution at a concentration of 1M was added to the cobalt solution at a flow rate of 0.5L/h. When the concentration of the nickel solution is 0.1M or the cobalt solution is 1M, stopping adding the raw materials into the reaction kettle, and aging for 16 hh. The pH of the whole process system is 12, and the reaction temperature is 62 ℃.
Post-treatment
Taking the materials out of the reaction kettle, carrying out solid-liquid separation, washing twice by using a sodium hydroxide solution with the pH value of 12 and the temperature of 62 ℃, and washing twice by using deionized water. Drying the cleaned material at 120 deg.C for 24h, sieving with 200 mesh sieve to obtain nickel cobalt aluminum ternary precursor with continuous concentration gradient, wherein the chemical formula is Ni0.90CO0.08Al0.02(OH)2。
After the button cell prepared by the sample is charged and discharged for 50 times at 0.1 ℃, the capacity is 180.8mAh/g, and the capacity retention rate is 96.5%.
Example 5
Preparing solution
Deionized water is used for preparing a nickel sulfate solution with the concentration of 1.4M, a cobalt sulfate solution with the concentration of 0.6M, a sodium metaaluminate solution with the concentration of 0.2M and a mixed solution of ammonia water and sodium hydroxide, wherein the concentration of the ammonia water is 2M, and the concentration of the sodium hydroxide is 4M.
Reaction of
15L of dilute ammonia solution was added to a 100L reactor, and the above solutions were each added to the reactor cocurrently. Adjusting the concentration of the nickel solution and the cobalt solution at the beginning of adding the raw materials into the reaction kettle: deionized water was added to the nickel solution at a flow rate of 0.8L/h, and a cobalt solution at a concentration of 1.5M was added to the cobalt solution at a flow rate of 0.3L/h. Stopping adding the raw materials into the reaction kettle when the concentration of the nickel solution is 0.1M or the cobalt solution is 1M, and aging for 20 hours. The pH of the whole process system is 10.5, and the reaction temperature is 60 ℃.
Post-treatment
Taking the materials out of the reaction kettle, carrying out solid-liquid separation, and then using the pH value of 10.5 and the temperatureWashed twice with 60 ℃ sodium hydroxide solution and twice with deionized water. Drying the cleaned material at 120 deg.C for 24h, sieving with 200 mesh sieve to obtain nickel cobalt aluminum ternary precursor with continuous concentration gradient, wherein the chemical formula is Ni0.86CO0.12Al0.04(OH)2。
After the button cell prepared by the sample is charged and discharged for 50 times at 0.1 ℃, the capacity is 178.3mAh/g, and the capacity retention rate is 96.8%.
Claims (2)
1. A preparation method of a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient is characterized by comprising the following steps:
(1) adding a nickel solution into the reaction kettle in a parallel flow manner; a cobalt solution; an aluminum solution; a mixed solution of a complexing agent and a precipitating agent;
(2) in the adding process of the raw materials, deionized water is continuously added into the nickel solution, so that the concentration of nickel in the nickel solution is continuously reduced; continuously adding a high-concentration cobalt solution into the cobalt solution to continuously increase the concentration of cobalt in the cobalt solution; stopping adding the raw materials into the reaction kettle when the concentration of the nickel solution is 0.1M or the concentration of the cobalt solution is 1M;
(3) after the reaction is finished, carrying out solid-liquid separation, washing and drying on the materials to obtain a nickel-cobalt-aluminum ternary precursor with continuous concentration gradient;
the salt used for preparing the nickel solution in the step (1) is nickel sulfate; the salt used for preparing the cobalt solution is cobalt sulfate; the salt used for preparing the aluminum solution is sodium metaaluminate;
the complexing agent in the step (1) is ammonia water, and the precipitator is sodium hydroxide;
the concentration of the nickel solution in the step (1) is 1-2M; the concentration of the cobalt solution is 0.5-1M; the concentration of the aluminum solution is 0.2-0.5M; the concentration of ammonia water is 1-3M; the concentration of sodium hydroxide is 3-6M;
the concentration of the high-concentration cobalt solution in the step (2) is 1-1.5M;
in the step (2), the flow rate of adding deionized water into the nickel solution is 0.1-1L/h, and the flow rate of adding the high-concentration cobalt solution into the cobalt solution is 0.1-1L/h;
the molar ratio of nickel, cobalt and aluminum in the system in the step (2) is 0.70-0.90: 0.08-0.20: 0.02-0.06;
in the step (2), the temperature in the system is 55-65 ℃, the pH value is 10.5-12, and the aging time is 6-24 h.
2. The method of claim 1, wherein: and (4) washing the materials in the step (3) by using a hot alkali solution with the pH of 10.5-12 and deionized water successively.
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| CN112537801A (en) * | 2019-09-20 | 2021-03-23 | 格林美股份有限公司 | Continuous concentration gradient aluminum-titanium doped cobaltosic oxide and preparation method and application thereof |
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| CN114249354B (en) * | 2021-12-09 | 2023-07-14 | 格林美（江苏）钴业股份有限公司 | Preparation method of continuously concentration gradient doped cobaltosic oxide |
| CN115180657A (en) * | 2022-06-30 | 2022-10-14 | 金川集团股份有限公司 | Preparation method of aluminum-doped nickel-doped gradient cobalt carbonate material |
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