CN114804228B - 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 lithium-rich manganese-based positive electrode material has a chemical formula of Ni x Co y Mn z (OH) 2 The preparation method comprises the following steps: 1. formulation Ni, co, mn, H 2 O 2 Is a mixed solution of (a) and (b); preparing sodium hydroxide or potassium hydroxide solution as a precipitator; preparing ammonia water solution as complexing agent; 2. adding pure water, a precipitator and a complexing agent to prepare a base solution; 3. introducing nitrogen or inert gas, and continuously adding the mixed solution, the precipitant and the complexing agent into a kettle for coprecipitation; controlling the solid content in the kettle, and stopping the reaction when the granularity of the material reaches the target; 4. and centrifuging, washing and drying the coprecipitation product to obtain a loose and porous lithium-rich manganese-based positive electrode material precursor. The invention prepares the layered lithium-rich manganese-based positive electrode material precursor of the loose and porous hydroxide system, and improves the capacity of the corresponding positive electrode material.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a precursor of a lithium-rich manganese-based anode material and a preparation method thereof.
Background
With the rapid development of the new energy automobile industry, people are urgent to electric automobiles with high endurance, and the development of the energy density of the traditional lithium ion positive electrode material cannot meet the requirements.
Compared with the energy density of the traditional lithium ion positive electrode material, the layered lithium-rich manganese-based positive electrode 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 positive electrode material is widely researched by people and is expected to become a next-generation lithium ion battery positive electrode 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 positive electrode material precursor of the carbonate system is relatively loose and porous, is favorable for the diffusion of lithium in the calcination process, and corresponds to higher capacity of the positive electrode material, but in the process of preparing the layered lithium-rich manganese-based positive electrode material precursor of the carbonate system, partial transition metal ions are lost due to incomplete carbonate precipitation, so that the cost is relatively higher; in the preparation process of the layered lithium-rich manganese-based positive electrode material precursor of the hydroxide system, transition metal ions almost completely precipitate, the cost is lower, but the transition metal ions are relatively compact, the diffusion of lithium is not facilitated, and the corresponding positive electrode material has lower capacity.
Therefore, how to prepare a layered lithium-rich manganese-based positive electrode material precursor of a loose and porous hydroxide system to increase the capacity of the corresponding positive electrode material is the subject of the research of the 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 above purpose, the invention adopts the following technical scheme:
a precursor of lithium-rich manganese-based positive electrode material 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 or equal to 0.4, y is more than or equal to 0 and less than or equal to 0.04,0.6, and z is more than or equal to 0.7.
The relevant content explanation in the technical scheme is as follows:
1. in the scheme, D50 is 10-12 um, the granularity diameter distance is 0.65 < (D90-D10)/D50 is less than 0.80, and the tap density is 1.15-1.45 g/cm 3 The specific surface area is 60-90 m 2 Per gram, the true density is 3.9-4.1 g/cm 3 。
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a lithium-rich manganese-based positive electrode material precursor comprises the following steps:
step one, preparing Ni, co, mn, H 2 O 2 Is a mixed solution of (a) and (b);
preparing sodium hydroxide or potassium hydroxide solution with the molar concentration of 8-10 mol/L as a precipitant;
preparing an ammonia water solution with the molar concentration of 2-4 mol/L as a complexing agent;
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 through the precipitant, controlling the ammonia concentration in the base solution to be 0.15-0.45 mol/L through the complexing agent, and maintaining the temperature at 60-70 ℃;
step three, keeping stirring of the reaction kettle open, and introducing nitrogen or inert gas with the flow of 0.5-0.8 m 3 And (h) continuously adding the mixed solution, the precipitant and the complexing agent in the first step into a reaction kettle at a flow rate of 200-600 mL/min for coprecipitation reaction; the pH 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;
the overflow flows to a concentration machine, the solid content in the reaction kettle is controlled to be 20-30%, and the reaction is stopped when the granularity D50 of the materials in the reaction kettle grows to 10-12 um and the granularity diameter distance is 0.65 < (D90-D10)/D50 < 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 explanation in the technical scheme is as follows:
1. in the above scheme, in the first step, 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 the catalyst 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 or equal to 0.4, y is more than or equal to 0 and less than or equal to 0.04,0.6, and z is more 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, so that the Co element can maintain the layered structure of the material, and the ionic conductivity of the material and the cycling stability of the material are improved. In addition, the addition amount of Co element cannot be excessive, and excessive amount leads to decrease in capacity of the material, and excessive amount leads to decrease in cycle performance.
2. In the preparation of the precursor, H with the molar concentration of 0.3-0.6 mol/L is added into the metal liquid of Ni, co and Mn 2 O 2 Realize Co to 2+ 、Mn 2+ The structure is favorable for lithium diffusion in the calcination process and is convenient for forming a stable layered structure, the prepared lithium-rich manganese-based positive electrode material inherits the 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 of a layered lithium-rich manganese-based positive electrode material precursor of a hydroxide system due to internal compaction. In addition, H in the mixed solution 2 O 2 The molar concentration is controlled to be 0.3-0.6 mol/L, H 2 O 2 Too high a molar concentration will result in excessive Co 2+ 、Mn 2+ Oxidation, so that the interior of the precursor product is too loose, the sphericity is poor, and the processability is poor; and H is 2 O 2 Too low a molar concentration results 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 a 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 a lithium-rich manganese-based cathode material prepared in comparative example 3 of the present invention;
FIG. 3 is a cross-sectional view of a precursor of a lithium-rich manganese-based cathode material prepared in comparative example 4 of the present invention;
fig. 4 is a graph of the first charge and discharge of the lithium-rich manganese-based cathode material prepared in the embodiment of the invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples:
the present invention will be described in detail with reference to the drawings, wherein modifications and variations are possible in light of the teachings of the present invention, without departing from the spirit and scope of the present invention, as will be apparent to those of skill in the art upon understanding the embodiments of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the present disclosure. As used herein, the terms "comprising," "including," "having," and the like are intended to be open-ended terms, meaning including, but not limited to.
The term (terms) as used herein generally has the ordinary meaning of each term as used in this field, in this disclosure, and in the special context, unless otherwise noted. Certain terms used to describe the present disclosure are discussed below, or elsewhere in this specification, to provide additional guidance to those skilled in the art in connection with the description herein.
Examples:
a preparation method of a lithium-rich manganese-based positive electrode material precursor comprises the following steps:
step one, preparing Ni, co, mn, H 2 O 2 Wherein the total molar concentration of Ni, co and Mn in the mixed solution is 2.0mol/L, the molar ratio is 35:2:63, H 2 O 2 The molar concentration of (2) is 0.4mol/L;
preparing 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;
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 through the precipitant, controlling the ammonia concentration in the base solution to be 0.25mol/L through the complexing agent, and maintaining the temperature of the base solution at 65 ℃;
step three, keeping stirring of the reaction kettle open, and introducing nitrogen with the flow of 0.7m 3 And (h) continuously adding the mixed solution, the precipitant and the complexing agent in the first step into a reaction kettle at the flow rate of 200-600 mL/min for coprecipitation reaction; in the reaction processThe pH is maintained at 11-12, 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 0.25mol/L;
the overflow flows to a concentration machine, the solid content in the reaction kettle is controlled to be 20-30%, until the granularity D50 of the materials in the reaction kettle grows to 10-12 um, the granularity diameter distance is 0.65 < (D90-D10)/D50 < 0.80, and the reaction is stopped;
step four, the coprecipitation product in the step three is subjected to filter pressing, washing and drying 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 The D50 is 11.125um, the granularity diameter distance is 0.698, and the tap density is 1.21g/cm 3 Specific surface area of 88.6m 2 Per g, true density of 4.02g/cm 3 The relevant data are shown in Table 1.
Comparative example 1:
the difference from the examples is that the molar ratio of Co element in the first step is different, co element is not added in this comparative example 1, and the remainder is the same as the examples. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Comparative example 2:
the difference from the examples is that the molar ratio of Co element in the first step is different, 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 examples. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Comparative example 3:
the difference from the embodiment is that in step one, H 2 O 2 In this comparative example 3, H is present at a molar concentration different from that of the other 2 O 2 The molar concentration of (C) was 0.2mol/L, and the remainder was the same as in example. The obtained precursor was washed and dried, and the relevant data are shown in table 1.
Comparative example 4:
the difference from the embodiment is that in step one, H 2 O 2 In this comparative example 4, H was present at a different molar concentration 2 O 2 The molar concentration of (C) was 0.8mol/L, and the remainder was the same as in example. Washing and drying the obtained precursor, and the related data are shown inTable 1.
Table 1 shows the data of the products obtained in the examples and 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 cobalt element has no obvious influence on the granularity D50 and granularity diameter distance of the precursor, and the proper amount of the cobalt element can stabilize the structure of the positive electrode material, improve the capacity retention rate and improve the cycle performance. With H 2 O 2 The tap density of the obtained precursor is reduced, the specific surface area is increased, and the precursor is too loose, resulting in a decrease in mechanical properties and thus in a deterioration of electrical properties.
Fig. 1, 2 and 3 are electron microscope diagrams of lithium-rich manganese-based positive electrode material precursors prepared in examples, comparative example 3 and comparative example 4, respectively, and it can be seen from fig. 1 that the lithium-rich manganese-based positive electrode material precursors have a loose porous structure and pores are relatively uniform, respectively. In comparative example 3 (FIG. 2), due to H 2 O 2 The molar concentration of (2) is low, resulting in insufficient oxidation and relatively dense precursor; whereas in comparative example 4 (FIG. 3) because of H 2 O 2 Too high a molar concentration leads to peroxidation, too loose precursors and poor processability.
Fig. 4 shows a first charge-discharge graph of the lithium-manganese-rich cathode material prepared in the embodiment, and it can be seen from the graph that the first charge capacity of the lithium-manganese-rich cathode material can reach 312mAh/g and the discharge capacity can reach 260mAh/g.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (5)
1. A preparation method of a lithium-rich manganese-based positive electrode material precursor is characterized by comprising the following steps of: comprising the following steps:
step one, preparing Ni, co, mn, H 2 O 2 Is a mixed solution of (a) and (b);
preparing sodium hydroxide or potassium hydroxide solution with the molar concentration of 8-10 mol/L as a precipitant;
preparing an ammonia water solution with the molar concentration of 2-4 mol/L as a complexing agent;
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 through the precipitant, controlling the ammonia concentration in the base solution to be 0.15-0.45 mol/L through the complexing agent, and maintaining the temperature at 60-70 ℃;
step three, keeping stirring of the reaction kettle open, and introducing nitrogen or inert gas with the flow of 0.5-0.8 m 3 And (h) continuously adding the mixed solution, the precipitant and the complexing agent in the first step into a reaction kettle at a flow rate of 200-600 mL/min for coprecipitation reaction; the pH 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;
the overflow flows to a concentration machine, the solid content in the reaction kettle is controlled to be 20-30%, and the reaction is stopped when the granularity D50 of the materials in the reaction kettle grows to 10-12 um and the granularity diameter distance is 0.65 < (D90-D10)/D50 < 0.80;
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 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 or equal to 0.4, y is more than or equal to 0 and less than or equal to 0.04,0.6, and z is more than or equal to 0.7.
2. The method of manufacturing according to claim 1, 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.
3. The method of manufacturing according to claim 1, characterized in that: in step one, the mixed solutionH in liquid 2 O 2 The molar concentration of the catalyst is 0.3-0.6 mol/L.
4. The method of manufacturing according to claim 1, characterized in that: in the third step, the ammonia concentration is controlled to be 0.15-0.45 mol/L in the reaction process.
5. The method of manufacturing according to claim 1, characterized in that: the D50 of the precursor is 10-12 um, the granularity diameter distance is 0.65 < (D90-D10)/D50 is less than 0.80, and the tap density is 1.15-1.45 g/cm 3 The specific surface area is 60-90 m 2 Per gram, the true density is 3.9-4.1 g/cm 3 。
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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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| CN111498908A (en) * | 2020-04-27 | 2020-08-07 | 中信大锰矿业有限责任公司 | Preparation method of quasi-spherical manganese-rich ternary precursor |
| 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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