CN111333126A - Nickel cobalt lithium manganate material precursor, preparation method thereof and nickel cobalt lithium manganate positive electrode material - Google Patents

Nickel cobalt lithium manganate material precursor, preparation method thereof and nickel cobalt lithium manganate positive electrode material Download PDF

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CN111333126A
CN111333126A CN202010235056.0A CN202010235056A CN111333126A CN 111333126 A CN111333126 A CN 111333126A CN 202010235056 A CN202010235056 A CN 202010235056A CN 111333126 A CN111333126 A CN 111333126A
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precursor
nickel
cobalt
lithium manganate
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CN111333126B (en
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张娉婷
朱璟
胡志兵
张海艳
刘庭杰
黎力
孙卓
张臻
周春仙
刘玮
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Hunan Changyuan Lico Co Ltd
Jinchi Energy Materials Co Ltd
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Jinchi Energy Materials Co Ltd
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    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract

The invention provides a nickel cobalt lithium manganate material precursor, a preparation method thereof and a positive electrode material prepared from the precursor. The precursor is spherical, primary particles are straight-inserted in a sheet shape, and the section is radial; its chemical formula is NixCoyMnzMt(OH)2+a. The XRD peak intensity ratio of the nickel cobalt lithium manganate material precursor is 1.0 +/-0.1, the median particle size is 9.0-11.0 mu m, and the tap density is 1.9-2.2 g/cm3The specific surface area is 7 to 11m2(ii) in terms of/g. In the preparation process of the precursor, no inert protective gas is introduced in the whole process, and an oxidizing additive is added in the coprecipitation reaction process. The preparation method not onlyThe process flow is simple, the automation degree is high, continuous production can be realized, and the product quality is stable and excellent.

Description

Nickel cobalt lithium manganate material precursor, preparation method thereof and nickel cobalt lithium manganate positive electrode material
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a nickel cobalt lithium manganate material precursor, a preparation method thereof, and a positive electrode material prepared from the precursor.
Background
In the face of increasingly severe energy crisis and environmental problems, the development of new energy will be the key work of the nation and society; the lithium ion battery has the characteristics of high energy density and long cycle life, and becomes a considerable force in the field of new energy. In recent years, the technology of lithium ion batteries has been rapidly advanced, and lithium ion batteries gradually replace other secondary batteries and are widely applied to electric vehicles.
The precursor with excellent performance is the key to prepare the high-energy-density cathode material. At present, the material cost is reduced mainly by increasing the nickel content in the precursor and reducing the cobalt content, the energy density of the battery is improved, and the consumption of other materials of the battery is saved.
The conventional method for preparing the precursor of the nickel cobalt lithium manganate material is a controlled crystal hydroxide coprecipitation method, namely, a mixed metal hydroxide precipitate is obtained by precipitating a mixed metal salt solution and sodium hydroxide under the action of a complexing agent. The anode material sintered by the precursor prepared by the conventional oxidation method has good cycle performance but low capacity, because the particles in the precursor are too loose and the porosity is too high; in addition, the energy density of the material is low due to the overlong diffusion path of lithium ions. Therefore, the research and development of the nickel cobalt lithium manganate material precursor which can give consideration to both the battery capacity and the cycle performance during use have important significance and good market prospect.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a nickel cobalt lithium manganate material precursor for preparing a lithium battery anode material with high capacity and high cycle performance and a preparation method thereof.
The solution of the invention is realized by the following steps:
a precursor of a nickel cobalt lithium manganate material is spherical, primary particles are straight-inserted in a sheet shape, and the section is radial; its chemical formula is NixCoyMnzMt(OH)2+aWherein x + y + z + t is 1, x is more than 0.8 and less than 1.0, y is more than or equal to 0 and less than or equal to 0.2, z is more than or equal to 0 and less than or equal to 0.2, t is more than or equal to 0 and less than or equal to 0.2, and a is more than or equal to 0 and less than or equal to 0.5; the element M is a doping element, and M is any one or more of Al, Zn, Zr, Mg and Ti. The XRD peak intensity ratio of the precursor is 1.0 +/-0.1, the median particle size is 9.0-11.0 mu m, and the tap density is 1.9-2.2 g/cm3The specific surface area is 7 to 11m2/g。
As a general inventive concept, the invention provides a preparation method of the nickel cobalt lithium manganate material precursor, which comprises the following steps:
(1) according to the formula NixCoyMnzMt(OH)2+aIn the medium of Ni, Co, Mn,Preparing a soluble salt solution according to the molar ratio of M, wherein x + y + z + t is 1, x is more than 0.8 and less than 1.0, y is more than or equal to 0 and less than or equal to 0.2, z is more than or equal to 0 and less than or equal to 0.2 (y + z is more than or equal to 0 and less than or equal to 0.2), t is more than or equal to 0 and less than or equal to 0.2, a is more than or equal to 0 and less than or equal to 0.5, the element M is a doping element, and M is any one or more of Al, Zn, Zr, Mg;
(2) adding the soluble salt solution, the complexing agent, the precipitator and the oxidizing additive in the step (1) into a reactor filled with a base solution in a concurrent flow manner, and carrying out continuous coprecipitation reaction at 65-80 ℃ to obtain a coprecipitation product; no inert gas protection is performed in the whole process;
(3) and (3) carrying out solid-liquid separation on the coprecipitation product in the step (2), collecting a solid phase, and carrying out aging, washing, dehydration, drying and screening treatment to obtain the precursor.
In the above preparation method, the oxidizing additive in the step (2) is MnO2Solution, H2O2One or more of, compressed air; wherein, MnO2The solution consisting of solid MnO2The sodium hydrogen phosphate is prepared by dissolving in concentrated alkali, and the concentration is 3-4 mol/L; h2O2The concentration of (A) is 1-2.5 mol/L; the feeding flow rate of the compressed air is 400-450L/h.
The appearance of the primary particles is reflected by the tap density of the product, and can change along with the difference of the pH value of the reaction system. The invention adjusts the pH value of the reaction system and changes the reaction environment by controlling the amount of the oxidizing additive, thereby realizing the purposes of modifying and adjusting the primary particle morphology and the tap density of the precursor product. The introduced oxidizing additive oxidizes bivalent cobalt and manganese metal ions in the system into trivalent cobalt and manganese metal ions, and the solubility product of hydroxide of trivalent cobalt and manganese is smaller than that of hydroxide of bivalent cobalt and manganese. The present invention is distinguished from the conventional reaction environment in which an inert protective gas is used at the initial stage of nucleation.
In the preparation method, preferably, in the step (2), the stirring speed is 450-550 r/min, the pH value is controlled to be 11.0-11.6, the reaction temperature is 65-80 ℃, and the reaction time is 48-168 h.
In the above preparation method, preferably, in the step (2), the base solution is added with tapThe density is 1.9-2.2 g/cm3And (4) seed crystal precursor.
In the above preparation method, preferably, the nickel salt in step (1) is nickel sulfate, nickel chloride and/or nickel nitrate; the cobalt salt is cobalt sulfate, cobalt chloride and/or cobalt nitrate; the manganese salt is manganese sulfate, manganese chloride and/or manganese nitrate; the nickel salt, the cobalt salt and the manganese salt are proportioned according to the molar ratio of nickel, cobalt and manganese elements in the nickel-cobalt lithium manganate; the total concentration of nickel ions, cobalt ions and manganese ions in the soluble salt solution in the step (1) is 60-120 g/L.
In the above preparation method, preferably, the complexing agent in the step (2) is ammonia water, and the ammonia concentration is 0.5-7 mol/L; the precipitator is sodium hydroxide aqueous solution, and the concentration of the precipitator is 1-3 mol/L.
In the preparation method, the base solution in the step (2) is preferably an ammonia-alkali mixed solution, the ammonia ion concentration in the base solution is 20-50g/L, the pH value is 11.0-11.6, and the temperature is 65-80 ℃.
Preferably, in the step (3), the aging treatment is to perform an aging reaction on the coprecipitation product by using 0.1-1.0 mol/L sodium carbonate solution, wherein the aging temperature is controlled to be 40-80 ℃, and the reaction time is 10-30 min; during washing, deionized water is adopted for washing, and the pH value of the washing end point is controlled to be 8.2-10.0; controlling the water content of the material to be below 20% after dehydration; when drying, the drying temperature is 90-135 ℃, and the water content of the dried material is 0.3-1.0%.
As a general technical concept, the invention also provides a nickel cobalt lithium manganate positive electrode material, which is characterized in that the positive electrode material is prepared from the nickel cobalt lithium manganate precursor.
Compared with the prior art, the invention has the following beneficial effects:
(1) the nickel cobalt lithium manganate material precursor has the advantages that the primary particles are straight-inserted in a sheet shape, the sections of the primary particles are uniform and radial, and the secondary particles are spherical; the precursor has uniform internal particle pores, is not only beneficial to the diffusion of lithium ions and the improvement of the capacity and the cycle performance of the material, but also beneficial to the industrial production of the precursor material, increases the convenience of the production process, obviously improves the processing performance of the product, and the ternary cathode material prepared and produced by using the precursor has the advantages of high capacity and high cycle performance, and also has the advantages of high compaction density, good thermal stability, low self-discharge rate and the like.
(2) The preparation method disclosed by the invention is simple in process flow, high in automation degree, capable of realizing continuous production and stable and excellent in product quality.
Drawings
FIG. 1 shows Ni in example 10.825Co0.115Mn0.06(OH)2Scanning Electron Micrographs (SEM) of the precursor;
FIG. 2 shows Ni in example 10.825Co0.115Mn0.06(OH)2Scanning Electron Micrographs (SEM) of the precursor cross section;
FIG. 3 shows Ni in example 10.825Co0.115Mn0.06(OH)2XRD pattern of the precursor.
Detailed Description
The present invention will now be described in detail with reference to the drawings, which are given by way of illustration and explanation only and should not be construed to limit the scope of the present invention in any way.
Example 1:
a preparation method of a nickel cobalt lithium manganate material precursor comprises the following steps:
(1) preparing a nickel, cobalt and manganese soluble salt solution with the total metal concentration of 2mol/L by adopting nickel sulfate, cobalt sulfate and manganese sulfate, wherein the molar ratio of nickel to cobalt to manganese is 82.5:11.5: 6; preparing 2mol/L sodium hydroxide solution as a precipitator; preparing 1 mol/L ammonia water solution as a complexing agent;
(2) adding pure water into a reaction kettle with the volume of 100L, controlling the temperature to be 70 ℃, adjusting the pH value to 11.0 by using alkali, and adjusting the ammonium ion concentration to 50g/L by using ammonia water;
(3) adding the prepared nickel, cobalt and manganese soluble salt solution, sodium hydroxide solution and ammonia water solution into the reaction kettle in the step (2) in a cocurrent manner for reaction; stirring at a rotating speed of 500r/min, and continuously introducing compressed air into the reaction kettle at a flow rate of 410L/h; in the reaction process, the pH value is controlled to be 11.2, and the reaction temperature is 65-80 ℃; the reaction time was 72 h.
(4) Filtering, aging with 1.0mol/L sodium carbonate, washing and drying the slurry obtained by the reaction to obtain Ni with loose inside and compact outside0.825Co0.115Mn0.06(OH)2And (5) precursor products.
Example 1 preparation of Ni0.825Co0.115Mn0.06(OH)2The electron microscope images and XRD images of the precursor products are shown in figures 1-3. The precursor of the nickel cobalt lithium manganate material is spherical, primary particles are straight-inserted in a sheet shape, and the section is radial; the XRD peak intensity ratio of the precursor is 0.999. In addition, the Ni prepared in example 1 was tested0.825Co0.115Mn0.06(OH)2The median particle size of the precursor product is 9.50 mu m, and the tap density is 2.1g/cm3A specific surface area of 9.3m2/g。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A precursor of a nickel cobalt lithium manganate material is spherical, primary particles are straight-inserted in a sheet shape, and the section is radial; its chemical formula is NixCoyMnzMt(OH)2+aWherein x + y + z + t is 1, x is more than 0.8 and less than 1.0, y is more than or equal to 0 and less than or equal to 0.2, z is more than or equal to 0 and less than or equal to 0.2, t is more than or equal to 0 and less than or equal to 0.2, a is more than or equal to 0 and less than or equal to 0.5, and the element M is a doping element; the XRD peak intensity ratio of the nickel cobalt lithium manganate material precursor is 1.0 +/-0.1, the median particle size is 9.0-11.0 mu m, and the tap density is 1.9-2.2 g/cm3The specific surface area is 7 to 11m2/g。
2. The precursor of a nickel cobalt lithium manganate material of claim 1, wherein the doping element M is any one or more of Al, Zn, Zr, Mg and Ti.
3. A method of preparing a precursor of a nickel cobalt lithium manganate material according to claim 1 or 2, comprising the steps of:
(1) according to the formula NixCoyMnzMt(OH)2+aPreparing a soluble salt solution according to the molar ratio of Ni, Co, Mn and M, wherein x + y + z + t is 1, x is more than 0.8 and less than 1.0, y is more than or equal to 0 and less than or equal to 0.2, z is more than or equal to 0 and less than or equal to 0.2, t is more than or equal to 0 and less than or equal to 0.2, and a is more than or equal to 0 and less than or equal to 0.5; the element M is a doping element and is any one or more of Al, Zn, Zr, Mg and Ti;
(2) adding the soluble salt solution, the complexing agent, the precipitator and the oxidizing additive in the step (1) into a reactor filled with a base solution in a concurrent flow manner, and carrying out continuous coprecipitation reaction at 65-80 ℃ to obtain a coprecipitation product; no inert gas is introduced in the whole process;
(3) and (3) carrying out solid-liquid separation on the coprecipitation product in the step (2), collecting a solid phase, and carrying out aging, washing, dehydration, drying and screening treatment to obtain the precursor.
4. The method of claim 3, wherein the oxidizing additive in step (2) is MnO2Solution, H2O2One or more of, compressed air; wherein, MnO2The solution consisting of solid MnO2The sodium hydrogen phosphate is prepared by dissolving in concentrated alkali, and the concentration is 3-4 mol/L; h2O2The concentration of (A) is 1-2.5 mol/L; the feeding flow rate of the compressed air is 400-450L/h.
5. The preparation method of claim 3, wherein in the step (2), the stirring speed is 450-550 r/min, the pH value is controlled to be 11.0-11.6, the reaction temperature is 65-80 ℃, and the reaction time is 48-168 h.
6. The method according to claim 3, wherein the base solution in the step (2) is an ammonia-alkali mixed solution, the ammonia ion concentration in the base solution is 20-50g/L, and the pH value is set to be the same as that of the base solution11.0-11.6 ℃, the temperature is 65-80 ℃, and the tap density of the added base solution is 1.9-2.2 g/cm3The seed crystal precursor of (1).
7. The method according to claim 3, wherein the nickel salt in the step (1) is nickel sulfate, nickel chloride and/or nickel nitrate; the cobalt salt is cobalt sulfate, cobalt chloride and/or cobalt nitrate; the manganese salt is manganese sulfate, manganese chloride and/or manganese nitrate; the nickel salt, the cobalt salt and the manganese salt are proportioned according to the molar ratio of nickel, cobalt and manganese elements in the nickel-cobalt lithium manganate; the total concentration of nickel ions, cobalt ions and manganese ions in the soluble salt solution in the step (1) is 60-120 g/L.
8. The preparation method according to claim 3, wherein the complexing agent in the step (2) is ammonia water with a concentration of 0.5 to 7 mol/L; the precipitator is sodium hydroxide aqueous solution, and the concentration of the precipitator is 1-3 mol/L.
9. The method according to claim 3, wherein in the step (3), the aging is performed by aging the coprecipitate product with 0.1 to 1.0mol/L sodium carbonate solution.
10. A lithium nickel cobalt manganese oxide positive electrode material, which is characterized in that the positive electrode material is prepared from the lithium nickel cobalt manganese oxide precursor of claim 1 or 2.
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CN111732132A (en) * 2020-07-06 2020-10-02 金驰能源材料有限公司 Nickel-cobalt-manganese core-shell structure precursor, preparation method thereof and positive electrode material
CN112047399A (en) * 2020-09-07 2020-12-08 厦门厦钨新能源材料股份有限公司 Precursor with reticular structure, composite oxide powder, preparation method and application thereof
CN112226820A (en) * 2020-12-14 2021-01-15 河南科隆新能源股份有限公司 Single-crystal lithium nickel cobalt manganese oxide precursor, preparation method thereof and single-crystal lithium nickel cobalt manganese oxide
CN113258062A (en) * 2021-07-05 2021-08-13 中南大学 Ternary precursor with radial spherical-roof cone structure, positive electrode material and preparation method
CN113582246A (en) * 2021-06-30 2021-11-02 南通金通储能动力新材料有限公司 Preparation method of high-nickel polycrystalline quaternary precursor
CN113697867A (en) * 2021-06-30 2021-11-26 南通金通储能动力新材料有限公司 Preparation method of power type high-nickel ternary precursor
CN113735190A (en) * 2021-08-24 2021-12-03 南通金通储能动力新材料有限公司 Small-particle ternary precursor and preparation method thereof
CN115064691A (en) * 2022-06-22 2022-09-16 重庆长安新能源汽车科技有限公司 Electrode material, preparation method, lithium ion battery and application thereof
CN117083247A (en) * 2023-06-27 2023-11-17 广东邦普循环科技有限公司 Ternary material precursor and ternary material prepared from ternary material precursor

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