CN114804228A - Lithium-rich manganese-based positive electrode material precursor and preparation method thereof - Google Patents
Lithium-rich manganese-based positive electrode material precursor and preparation method thereof Download PDFInfo
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Abstract
A precursor of a lithium-rich manganese-based anode material, with the chemical formula of Ni x Co y Mn z (OH) 2 The preparation method comprises the following steps: firstly, preparing Ni, Co, Mn and H 2 O 2 The mixed solution of (1); preparing sodium hydroxide or potassium hydroxide solution as a precipitator; preparing an ammonia water solution as a complexing agent; adding pure water, a precipitator and a complexing agent to prepare a base solution; thirdly, introducing nitrogen or inert gas, and continuously adding the mixed solution, the precipitator and the complexing agent into the kettle for coprecipitation; controlling the solid content in the kettle, and stopping the reaction until the granularity of the material reaches the target; and fourthly, centrifuging, washing and drying the coprecipitation product to obtain a loose and porous lithium-rich manganese-based positive electrode material precursor. Book (I)The invention prepares a layered lithium-rich manganese-based anode material precursor of a loose and porous hydroxide system, and improves the capacity of the anode material corresponding to the precursor.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a lithium-rich manganese-based anode material precursor and a preparation method thereof.
Background
With the rapid development of the new energy automobile industry, people are more urgent for electric automobiles with high endurance capacity, and the development of the energy density of the traditional lithium ion anode material cannot meet the requirement.
Compared with the energy density of the traditional lithium ion anode material, the layered lithium-rich manganese-based anode material has the advantages of high theoretical specific capacity, wide working voltage window, good thermal stability and the like, so that the layered lithium-rich manganese-based anode material is widely researched by people and is expected to become the next-generation lithium ion battery anode material. The layered lithium-rich manganese-based positive electrode material is generally formed by mixing and calcining a layered lithium-rich manganese-based positive electrode material precursor and a lithium source, wherein the layered lithium-rich manganese-based positive electrode material precursor is divided into a carbonate system and a hydroxide system: the layered lithium-rich manganese-based anode material precursor of the carbonate system is relatively loose and porous, is beneficial to the diffusion of lithium in the calcining process, and has higher capacity corresponding to the anode material, but in the process of preparing the layered lithium-rich manganese-based anode material precursor of the carbonate system, partial transition metal ions are lost due to incomplete carbonate precipitation, and the cost is relatively high; in the preparation process of the layered lithium-rich manganese-based cathode material precursor of the hydroxide system, transition metal ions are almost completely precipitated, the cost is low, but the transition metal ions are relatively compact, lithium diffusion is not facilitated, and the capacity of the corresponding cathode material is low.
Therefore, how to prepare a layered lithium-rich manganese-based positive electrode material precursor of a loose and porous hydroxide system to improve the capacity of the corresponding positive electrode material becomes a subject to be studied by the present invention.
Disclosure of Invention
The invention aims to provide a lithium-rich manganese-based positive electrode material precursor and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a kind ofA precursor of the lithium-rich manganese-based anode material with a chemical formula of Ni x Co y Mn z (OH) 2 Wherein x is more than or equal to 0.30 and less than 0.4, y is more than 0 and less than or equal to 0.04, and z is more than 0.6 and less than or equal to 0.7.
The relevant content in the above technical solution is explained as follows:
1. in the scheme, D50 is 10-12 um, the particle size diameter distance is 0.65 < (D90-D10)/D50 < 0.80, and the tap density is 1.15-1.45 g/cm 3 The specific surface area is 60-90 m 2 (iv) g, true density of 3.9-4.1 g/cm 3 。
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a lithium-rich manganese-based positive electrode material precursor comprises the following steps:
step one, preparing Ni, Co, Mn and H 2 O 2 The mixed solution of (1);
preparing a sodium hydroxide or potassium hydroxide solution with the molar concentration of 8-10 mol/L as a precipitator;
preparing an ammonia water solution with the molar concentration of 2-4 mol/L as a complexing agent;
step two, adding pure water, the precipitant and the complexing agent into a closed reaction kettle to prepare a base solution, controlling the pH value of the base solution to be 11-12 by using the precipitant, controlling the ammonia concentration in the base solution to be 0.15-0.45 mol/L by using the complexing agent, and maintaining the temperature to be 60-70 ℃;
step three, keeping the stirring of the reaction kettle open, introducing nitrogen or inert gas, wherein the flow rate is 0.5-0.8 m 3 Step one, continuously adding the mixed solution, the precipitator and the complexing agent in the step one into a reaction kettle at the flow rate of 200-600 mL/min respectively to perform coprecipitation reaction; the pH value is maintained at 11-12 in the reaction process, the reaction temperature is maintained at 60-70 ℃, and the rotating speed of the reaction kettle is 400-600 r/min;
overflowing to the thickener, controlling the solid content in the reaction kettle to be 20-30%, and stopping the reaction until the granularity D50 of the material in the reaction kettle grows to 10-12 um and the granularity diameter distance is 0.65 < (D90-D10)/D50 is less than 0.80;
and step four, centrifuging, washing and drying the coprecipitation product in the step three to obtain a loose and porous lithium-rich manganese-based positive electrode material precursor.
The relevant content in the above technical solution is explained as follows:
1. in the scheme, in the step one, the total molar concentration of Ni, Co and Mn in the mixed solution is 1.8-2.5 mol/L.
2. In the above scheme, in the first step, H in the mixed solution 2 O 2 The molar concentration of (a) is 0.3-0.6 mol/L.
3. In the scheme, in the third step, the ammonia concentration is controlled to be 0.15-0.45 mol/L in the reaction process.
4. In the above scheme, the chemical formula of the precursor is Ni x Co y Mn z (OH) 2 Wherein x is more than or equal to 0.30 and less than 0.4, y is more than 0 and less than or equal to 0.04, and z is more than 0.6 and less than or equal to 0.7.
The working principle and the advantages of the invention are as follows:
1. according to the invention, the Co element is introduced in the process of preparing the precursor, and the Co element can maintain the layered structure of the material, improve the ionic conductivity of the material and improve the cycling stability of the material. In addition, the amount of Co element added cannot be excessive, and excessive addition results in a decrease in the capacity of the material, while too little addition results in a decrease in the cycle performance.
2. In the preparation of the precursor, H with the molar concentration of 0.3-0.6 mol/L is added into metal liquid of Ni, Co and Mn 2 O 2 Realize the aim at Co 2+ 、Mn 2+ The prepared lithium-rich manganese-based anode material inherits the loose porous structure, the structure can increase the contact area with electrolyte, shorten the lithium ion transmission path, improve the lithium ion transmission efficiency, and solve the problem of capacity reduction caused by internal compaction of the layered lithium-rich manganese-based anode material precursor of a hydroxide system. Further, H in the mixed solution 2 O 2 The molar concentration needs to be controlled to be 0.3-0.6 mol/L, H 2 O 2 Too high a molar concentration may result in excessive Co 2+ 、Mn 2+ Oxidation leads the interior of the precursor product to be too loose and the sphericity to be poorThe processability becomes poor; and H 2 O 2 Too low a molar concentration may result in Co 2+ 、Mn 2+ Insufficient oxidation, compact inside of the product and reduced electrochemical performance.
Drawings
FIG. 1 is an electron microscope image of a precursor of the lithium-rich manganese-based positive electrode material prepared by the embodiment of the invention;
FIG. 2 is a cross-sectional view of a precursor of the lithium-rich manganese-based positive electrode material prepared in comparative example 3 of the present invention;
FIG. 3 is a cross-sectional view of a precursor of the lithium-rich manganese-based positive electrode material prepared in comparative example 4 of the present invention;
fig. 4 is a first charge-discharge curve diagram of the lithium-rich manganese-based positive electrode material prepared in the embodiment of the invention.
Detailed Description
The invention is further described with reference to the following figures and examples:
the present disclosure will be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the disclosure may be shown and described, and which, when modified and varied by the techniques taught herein, can be made by those skilled in the art without departing from the spirit and scope of the disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used herein, the terms "comprising," "including," "having," and the like are open-ended terms that mean including, but not limited to.
As used herein, the term (terms), unless otherwise indicated, shall generally have the ordinary meaning as commonly understood by one of ordinary skill in the art, in this application, and in the special art. Certain words used to describe the disclosure are discussed below or elsewhere in this specification to provide additional guidance to those skilled in the art in describing the disclosure.
Example (b):
a preparation method of a lithium-rich manganese-based positive electrode material precursor comprises the following steps:
step one, preparing Ni, Co, Mn and H 2 O 2 Wherein the total molar concentration of Ni, Co and Mn in the mixed solution is 2.0mol/L, and the molar ratio is 35:2:63，H 2 O 2 The molar concentration of (A) is 0.4 mol/L;
preparing a sodium hydroxide or potassium hydroxide solution with the molar concentration of 10mol/L as a precipitator;
preparing an ammonia water solution with the molar concentration of 2.5mol/L as a complexing agent;
step two, adding pure water, the precipitant and the complexing agent into a closed reaction kettle to prepare a base solution, controlling the pH value of the base solution to be 11-12 by using the precipitant, controlling the ammonia concentration in the base solution to be 0.25mol/L by using the complexing agent, and maintaining the temperature of the base solution at 65 ℃;
step three, keeping the stirring of the reaction kettle open, introducing nitrogen with the flow of 0.7m 3 Continuously adding the mixed solution, the precipitator and the complexing agent in the step one into a reaction kettle at the flow rate of 200-600 mL/min respectively for coprecipitation reaction; the pH value is maintained at 11-12 in the reaction process, the reaction temperature is maintained at 65 ℃, the rotating speed of the reaction kettle is 550r/min, and the ammonia concentration in the process is controlled at 0.25 mol/L;
overflowing to the thickener, controlling the solid content in the reaction kettle to be 20-30%, until the granularity D50 of the material in the reaction kettle grows to 10-12 um, the granularity diameter distance is 0.65 < (D90-D10)/D50 is less than 0.80, and stopping the reaction;
step four, carrying out filter pressing, washing and drying on the coprecipitation product in the step three to obtain a loose and porous lithium-rich manganese-based positive electrode material precursor, wherein the chemical formula of the product is Ni 0.35 Co 0.2 Mn 0.63 (OH) 2 D50 is 11.125um, the particle size diameter distance is 0.698, and the tap density is 1.21g/cm 3 The specific surface area is 88.6m 2 G, true density of 4.02g/cm 3 The relevant data are shown in table 1.
Comparative example 1:
the difference from the example is that the molar ratio of Co element is different in the first step, and Co element is not added in the comparative example 1, and the rest is exactly the same as the example. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Comparative example 2:
the difference from the example is that the molar ratio of Co element in the first step is different, and the molar ratio of Ni, Co and Mn in the comparative example 2 is 35:6:59, and the rest is the same as the example. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Comparative example 3:
the difference from the example is that in step one, H 2 O 2 In the molar concentration of (1), in this comparative example 3H 2 O 2 The molar concentration of (b) is 0.2mol/L, and the rest is the same as in the examples. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Comparative example 4:
the difference from the example is that in step one, H 2 O 2 Difference in molar concentration of (1), comparative example 4H 2 O 2 The molar concentration of (B) was 0.8mol/L, and the rest was the same as in the examples. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Table 1 shows the comparison of the final product data between the examples and the products obtained in the comparative examples.
From the data in table 1, it can be seen that: doping amount of Co element and H 2 O 2 The molar concentration of the Co element has no obvious influence on the granularity D50 and the granularity radial distance of the precursor, and proper amount of the Co element can stabilize the structure of the anode material, improve the capacity retention rate and improve the cycle performance. With H 2 O 2 The molar concentration of the precursor is improved, the tap density of the obtained precursor is reduced, the specific surface area is increased, the interior of the precursor is too loose, the mechanical property is reduced, and the electrical property is further deteriorated.
Fig. 1, fig. 2 and fig. 3 are electron microscope images of the lithium-rich manganese-based positive electrode material precursors prepared in the examples, the comparative examples 3 and the comparative examples 4, respectively, and it can be seen from fig. 1 that the lithium-rich manganese-based positive electrode material precursors have a loose and porous structure, and the pores are relatively uniform. In comparative example 3 (FIG. 2), due to H 2 O 2 The molar concentration of the precursor is low, so that the oxidation is insufficient, and the precursor is relatively compact; while comparative example 4 (FIG. 3) is due to H 2 O 2 Is prepared from (A) and (B)Too high a molar concentration leads to peroxidation, too loose precursor and poor processability.
Fig. 4 shows a first charge-discharge curve diagram of the lithium-rich manganese-based positive electrode material prepared in the example, and it can be known from the graph that the first charge capacity of the lithium-rich manganese-based positive electrode material can reach 312mAh/g, and the discharge capacity can reach 260 mAh/g.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A lithium-rich manganese-based positive electrode material precursor is characterized in that: has a chemical formula of Ni x Co y Mn z (OH) 2 Wherein x is more than or equal to 0.30 and less than 0.4, y is more than 0 and less than or equal to 0.04, and z is more than 0.6 and less than or equal to 0.7.
2. A precursor according to claim 1, wherein: d50 is 10-12 um, the particle size diameter distance is 0.65 < (D90-D10)/D50 < 0.80, and the tap density is 1.15-1.45 g/cm 3 The specific surface area is 60-90 m 2 (iv) g, true density of 3.9-4.1 g/cm 3 。
3. A preparation method of a precursor of a lithium-rich manganese-based positive electrode material is characterized by comprising the following steps: the method comprises the following steps:
step one, preparing Ni, Co, Mn and H 2 O 2 The mixed solution of (1);
preparing a sodium hydroxide or potassium hydroxide solution with the molar concentration of 8-10 mol/L as a precipitator;
preparing an ammonia water solution with the molar concentration of 2-4 mol/L as a complexing agent;
step two, adding pure water, the precipitant and the complexing agent into a closed reaction kettle to prepare a base solution, controlling the pH value of the base solution to be 11-12 by using the precipitant, controlling the ammonia concentration in the base solution to be 0.15-0.45 mol/L by using the complexing agent, and maintaining the temperature to be 60-70 ℃;
step three, keeping the stirring of the reaction kettle open, introducing nitrogen or inert gas, wherein the flow is 0.5-0.8 m 3 Step one, continuously adding the mixed solution, the precipitator and the complexing agent in the step one into a reaction kettle at the flow rate of 200-600 mL/min respectively to perform coprecipitation reaction; the pH value is maintained at 11-12 in the reaction process, the reaction temperature is maintained at 60-70 ℃, and the rotating speed of the reaction kettle is 400-600 r/min;
overflowing to the thickener, controlling the solid content in the reaction kettle to be 20-30%, and stopping the reaction until the granularity D50 of the material in the reaction kettle grows to 10-12 um and the granularity diameter distance is 0.65 < (D90-D10)/D50 is less than 0.80;
and step four, centrifuging, washing and drying the coprecipitation product in the step three to obtain a loose and porous lithium-rich manganese-based positive electrode material precursor.
4. The production method according to claim 3, characterized in that: in the first step, the total molar concentration of Ni, Co and Mn in the mixed solution is 1.8-2.5 mol/L.
5. The production method according to claim 3, characterized in that: in step one, H in the mixed solution 2 O 2 The molar concentration of (a) is 0.3-0.6 mol/L.
6. The production method according to claim 3, characterized in that: in the third step, the ammonia concentration is controlled to be 0.15-0.45 mol/L in the reaction process.
7. The method of claim 7, wherein: the chemical formula of the precursor is Ni x Co y Mn z (OH) 2 Wherein x is more than or equal to 0.30 and less than 0.4, y is more than 0 and less than or equal to 0.04, and z is more than 0.6 and less than or equal to 0.7.
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| WO2022027981A1 (en) * | 2020-08-04 | 2022-02-10 | 厦门厦钨新能源材料股份有限公司 | Environment-friendly precursor and preparation method therefor, and composite oxide powder and preparation method therefor, and application |
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| CN107221656A (en) * | 2017-06-07 | 2017-09-29 | 北京当升材料科技股份有限公司 | A kind of lithium ion battery rich lithium manganese base solid solution positive electrode and preparation method thereof |
| CN107265520A (en) * | 2017-07-19 | 2017-10-20 | 金驰能源材料有限公司 | The preparation method and product of a kind of spherical nickel cobalt manganese persursor material |
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| WO2022027981A1 (en) * | 2020-08-04 | 2022-02-10 | 厦门厦钨新能源材料股份有限公司 | Environment-friendly precursor and preparation method therefor, and composite oxide powder and preparation method therefor, and application |
| CN113716627A (en) * | 2021-09-28 | 2021-11-30 | 南通金通储能动力新材料有限公司 | High-performance ternary precursor and preparation method thereof |
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