CN112467101A - Ternary lithium ion storage battery positive electrode material and preparation method thereof - Google Patents
Ternary lithium ion storage battery positive electrode material and preparation method thereof Download PDFInfo
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- CN112467101A CN112467101A CN202011214714.4A CN202011214714A CN112467101A CN 112467101 A CN112467101 A CN 112467101A CN 202011214714 A CN202011214714 A CN 202011214714A CN 112467101 A CN112467101 A CN 112467101A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- 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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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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 relates to the field of ternary lithium ion storage batteries, in particular to a ternary lithium ion storage battery anode material and a preparation method thereof. The preparation method of the specific anode material comprises the following steps: 1) with M (Ac) 4H2O(M＝Ni、Mn、Co)、LiAc·H2Mixing the raw materials O according to a certain ratio, adding absolute ethyl alcohol, and fully dissolving; 2) igniting alcohol in a wide place or a high-temperature box after the solution is fully dissolved, and fully burning to obtain a purple precursor; 3) grinding and sieving the precursor obtained in the step 2; 4) sieving to obtain powder, placing into a tube furnace, introducing air, and heating at room temperature at 1 deg.C/minHeating to 550 ℃, keeping the temperature for 5h, continuously heating to 800 ℃ at the speed of 2 ℃/min respectively, sintering, and keeping the temperature for 9 h; 5) naturally cooling to 60 deg.C, taking out, grinding, and sieving. In the invention, the anode material is prepared by an alcohol combustion method, so that the ternary material structure is improved, and the cycle life of the battery is prolonged; the calcining temperature requirement is reduced.
Description
Technical Field
The invention relates to the field of ternary lithium ion storage batteries, in particular to a ternary lithium ion storage battery anode material and a preparation method thereof.
Background
Co, Ni and Mn all belong to the 4 th period transition metal element, and the ionic radius, the extra-nuclear electron arrangement, the crystal structure and the physical and chemical properties are very close, so that the alpha-NaFeO 4 layered solid solution can be formed according to any proportion; the lithium-rich layered oxide anode material has the advantages of high specific capacity, low price, environmental friendliness, no pollution and the like, and when the charging voltage range of the material is 2-4.6V or 2-4.8V, the material has higher specific discharge capacity which can exceed 200mAhg-1However, this material has the disadvantages of large irreversible capacity loss for the first time, unstable cycle, and the like. The cycle service life of the ternary lithium ion storage battery can be prolonged by improving the preparation method at present.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a ternary lithium ion storage battery positive electrode material and a preparation method thereof.
The technical scheme for realizing the purpose of the invention is as follows:
the positive electrode material of ternary lithium ion accumulator is lithium-rich layered oxide with chemical formula of LixNiyMnzCowO2(ii) a Wherein x: 1.10-1.30, y: 0.45-0.63, z: 0.08 to 1.18, w: 0.08 to 1.18, wherein x + y + z + w is 2.
A preparation method of a ternary lithium ion storage battery anode material comprises the following specific steps:
s1, using M (Ac) 4H2O(M＝Ni、Mn、Co)、LiAc·H2Mixing the raw materials O according to a certain ratio, adding absolute ethyl alcohol, and fully dissolving;
s2, igniting alcohol in a wide place or a high-temperature box after the solution is fully dissolved, and fully burning to obtain a purple precursor;
s3, grinding and sieving the precursor obtained in the step S2;
s4, sieving to obtain powder, putting the powder into a tubular furnace, introducing air, heating to 550-800 ℃, sintering, and keeping the temperature for 9-15 hours;
s5, naturally cooling to 60 ℃, taking out, grinding and sieving.
After the technical scheme is adopted, the invention has the following positive effects:
(1) the invention is prepared by an alcohol combustion method, improves the ternary material structure and prolongs the cycle life of the battery.
(2) The invention adopts the alcohol combustion method for preparation, reduces the requirement on the calcination temperature, and is suitable for industrial production.
(3) The invention shortens the preparation time and improves the efficiency.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is Li1.2Mn0.54Ni0.13Co0.13O2XRD pattern of the material;
FIG. 2 is Li1.2Mn0.54Ni0.13Co0.13O2SEM image of material.
Detailed Description
(example 1)
In this embodiment, the positive electrode material of the ternary lithium ion battery is a lithium-rich layered oxide with a chemical formula of Li1.2Mn0.54Ni0.13Co0.13O2。
(1) With M (Ac) 4H2O(M＝Ni、Mn、Co)、LiAc·H2O is the raw material according to the ratio of the measured weight, whereinLi: mn: co: ni ═ 1.20: 0.54: 0.13: 0.13. adding absolute ethyl alcohol, and fully dissolving.
(2) And igniting alcohol in the solution after the solution is fully dissolved in a wide place or a high-temperature box, and fully combusting to obtain the purple precursor.
(3) Grinding and sieving the precursor obtained in the step (2).
(4) Sieving to obtain powder, placing into a tube furnace, introducing air, heating to 550 deg.C at 1 deg.C/min from room temperature, holding the temperature for 5 hr, heating to 800 deg.C at 2 deg.C/min respectively, sintering, and holding the temperature for 9 hr.
(5) Naturally cooling to 60 deg.C, taking out, grinding, and sieving.
(example 2)
This example is substantially the same as example 1, and is distinguished by: the anode material of the ternary lithium ion storage battery is a lithium-rich layered oxide with the chemical formula of Li1.15Mn0.55Ni0.15Co0.15O2。
Li：Mn：Co：Ni＝1.15：0.55：0.15：0.15。
FIG. 1 shows Li prepared1.2Mn0.54Ni0.13Co0.13O2XRD patterns of the materials, from which it can be seen that both materials are alpha-NaFeO4The structure, 006/012 and 018/110 peaks have obvious splitting, which is a typical characteristic of a laminated structure, and the result shows that the cathode material obtained by the method maintains the typical laminated structure, has complete material structure and has good crystal form.
FIG. 2 shows Li prepared1.2Mn0.54Ni0.13Co0.13O2SEM images of the materials, it can be seen that these three materials are also composed of lumps and irregular agglomerates of small particles.
Compared with the anode material of the ternary lithium ion storage battery, the ternary lithium ion storage battery prepared by the preparation method of the anode material effectively improves the structure of the anode material, reduces the calcination temperature requirement, and prolongs the 100% DOD cycle life, wherein the number of times of the battery prepared in the embodiment 1 is 1040, the number of times of the battery prepared in the embodiment 2 is 1000, and the cycle life of the battery is improved by about 25% when the conventional common battery is only 800.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A ternary lithium ion battery positive electrode material is characterized in that: the positive electrode material is a lithium-rich layered oxide with a chemical formula of LixNiyMnzCowO2(ii) a Wherein x: 1.10-1.30, y: 0.45-0.63, z: 0.08 to 1.18, w: 0.08 to 1.18, wherein x + y + z + w is 2.
2. The preparation method of the ternary lithium ion battery positive electrode material of claim 1, which is characterized by comprising the following specific steps:
s1, using M (Ac) 4H2O(M＝Ni、Mn、Co)、LiAc·H2Mixing the raw materials O according to a certain ratio, adding absolute ethyl alcohol, and fully dissolving;
s2, igniting alcohol in a wide place or a high-temperature box after the solution is fully dissolved, and fully burning to obtain a purple precursor;
s3, grinding and sieving the precursor obtained in the step S2;
s4, sieving to obtain powder, putting the powder into a tube furnace, introducing air, heating to 550 ℃ from room temperature at a speed of 1 ℃/min, keeping the temperature for 5 hours, continuously heating to 800 ℃ at a speed of 2 ℃/min respectively, sintering, and keeping the temperature for 9 hours;
s5, naturally cooling to 60 ℃, taking out, grinding and sieving.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102779992A (en) * | 2012-07-31 | 2012-11-14 | 浙江大学 | Lithium ion battery positive electrode material in layer structure and preparation method thereof |
| CN102800870A (en) * | 2012-08-29 | 2012-11-28 | 浙江谷神能源科技股份有限公司 | Cylindrical power lithium-ion battery and preparation method |
| CN104009221A (en) * | 2014-06-06 | 2014-08-27 | 山东海特电子新材料有限公司 | Method for preparing positive electrode material rich in lithium via sol-gel self-propagating combustion method |
| CN106784797A (en) * | 2017-01-20 | 2017-05-31 | 中国科学院青海盐湖研究所 | The preparation method of tertiary cathode material |
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2020
- 2020-11-04 CN CN202011214714.4A patent/CN112467101A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102779992A (en) * | 2012-07-31 | 2012-11-14 | 浙江大学 | Lithium ion battery positive electrode material in layer structure and preparation method thereof |
| CN102800870A (en) * | 2012-08-29 | 2012-11-28 | 浙江谷神能源科技股份有限公司 | Cylindrical power lithium-ion battery and preparation method |
| CN104009221A (en) * | 2014-06-06 | 2014-08-27 | 山东海特电子新材料有限公司 | Method for preparing positive electrode material rich in lithium via sol-gel self-propagating combustion method |
| CN106784797A (en) * | 2017-01-20 | 2017-05-31 | 中国科学院青海盐湖研究所 | The preparation method of tertiary cathode material |
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Application publication date: 20210309 |