CN109860592B - Boron molecule-modified nickel cobalt lithium manganate positive electrode material and preparation method thereof - Google Patents
Boron molecule-modified nickel cobalt lithium manganate positive electrode material and preparation method thereof Download PDFInfo
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- CN109860592B CN109860592B CN201811590817.3A CN201811590817A CN109860592B CN 109860592 B CN109860592 B CN 109860592B CN 201811590817 A CN201811590817 A CN 201811590817A CN 109860592 B CN109860592 B CN 109860592B
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Abstract
The invention discloses a boron molecule-modified nickel cobalt lithium manganate positive electrode material and a preparation method thereof, wherein a 4-vinyl phenylboronic acid layer is linked on the surface of the nickel cobalt lithium manganate positive electrode material in a covalent bond mode, and a boron group-containing molecular layer of a monomolecular layer is formed on the surface of nickel cobalt lithium manganate powder, so that the particle size of the material is not influenced; in addition, the electrochemical cycle performance of the lithium ion battery prepared by applying the nickel cobalt lithium manganate positive electrode material prepared by the invention is obviously improved, and the capacity retention rate and the rate capability are also obviously improved.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a boron molecule-modified nickel cobalt lithium manganate positive electrode material and a preparation method thereof.
Background
With the increasing demand for high-capacity and high-power-density lithium ion batteries, materials with high specific capacity have attracted great interest and have received more and more attention in recent years. In particular, high nickel LiNi with low cost, low toxicity and high reversible capacity1-x-yCoxMnyO2The positive electrode material (NCM) is considered to be the best substitute for lithium cobaltate which is the traditional positive electrode material of the lithium ion battery.
High nickel LiNi1-x-yCoxMnyO2The material originated from LiNiO2Can utilize 80% of reversible deintercalated lithium in a matrix structure, and the capacity of the reversible deintercalation lithium is as high as 220 mAh.g-1Relative to having a density of about 140mAh g-1Of LiCoO (R) in a gas phase2，LiNi1-x-yCoxMnyO2The material has better lithium utilization rate. Substitution of Co and Mn for LiNiO2And part of Ni improves the conductivity and structural stability of the material to a great extent. One of the most attractive high nickel LiNi1-x-yCoxMnyO2The material being LiNi0.8Co0.1Mn0.1O2(NCM) having a specific discharge capacity of 200mAh g at a 0.1C charge-discharge current and a 4.3V cutoff voltage-1。
But the defects of rapid capacity fading, resistance increase during storage and circulation and insufficient thermal stability seriously hinder the commercial application of the material, and Ni with high activity on the surface of the material4+Decomposition of the electrolyte can be accelerated, resulting in consumption of the electrolyte and formation of a thick solid electrolyte film (SEI film). Another problematic problem that hinders the practical application of NCM is: the NCM material is quite sensitive to moisture, which results in the formation of LiOH on the surface of the material, which reacts with CO in the environment2Further reaction to produce insulated LiCO3An insulating layer is created on the surface of the material. Therefore, the surface chemistry of NCM has a decisive influence on the performance of lithium ion battery materials.
Researchers are currently overcoming these key problems through technological innovations, and surface coating is a common method of improving NCM performance and stability. Metal fluorides, phosphates and oxides have been used for NCM surface nanolayer coating studies. It is well known that the coating acts as a physical protective layer to inhibit undesirable side reactions between the material and the electrolyte, which can slow the corrosion of HF in the electrolyte. However, it is difficult to precisely control the thickness and uniformity of the coating layer. By passingCoatings that are processed at high temperatures simply after mixing with the NCM precursor are often non-uniform rough coatings. In addition, Al2O3And ZrO2These electrochemical properties and electrical activity are good and are often used as a defense layer for conventional coating. Although a concentration gradient material can solve this problem, it is inevitable to sacrifice part of the specific capacity.
The recent Atomic Layer Deposition (ALD) technology is introduced into the coating modification of the high-nickel material, a pinhole-free surface coating technology is realized on the positive electrode material, and the thickness of the coating layer can be accurately controlled to be 0.1 nm. However, expensive instruments and cumbersome procedures prevent large-scale implementation of this technique.
Therefore, the controllable coating technology for coating the surface of the high nickel material still needs to be designed and controlled carefully.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a boron molecule modified nickel cobalt lithium manganate positive electrode material and a preparation method thereof, wherein the boron molecule is modified on the surface of the positive electrode material, so that the electrochemical performance of the material is effectively improved.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows: a boron molecule-modified nickel cobalt lithium manganate positive electrode material is specifically a nickel cobalt lithium manganate positive electrode material with a surface modified and coated with 4-vinylphenylboronic acid.
Furthermore, the surface modification coating linking mode is a covalent bond linking mode.
Furthermore, the boron-containing molecules coated by surface modification are monomolecular layers; the thickness of the modified layer is 1-5 nm.
More preferably, the lithium nickel cobalt manganese oxide positive electrode material is a lithium nickel cobalt manganese oxide NCM811 material.
The invention also discloses a preparation method of the boron molecule-modified nickel cobalt lithium manganate positive electrode material, which comprises the following steps: dissolving nickel cobalt lithium manganate positive electrode material and 4-vinyl phenylboronic acid in an acetone solvent according to the mass ratio of 300:1-300:2, uniformly stirring until the materials are completely dissolved, refluxing, filtering out precipitate, andwashing with acetone for 3 times, and drying in a drying oven to obtain 4-vinylphenylboronic acid modified LiNi0.8Co0.1Mn0.1O2And (5) obtaining the boron molecule modified nickel cobalt lithium manganate cathode material.
More preferably, the stirring temperature of the stirring is 55 to 65 ℃.
More preferably, the reflux time is 10-13 h.
More preferably, after the acetone washing, the drying temperature of the oven drying is 75-85 ℃; the drying time is 24-26 h.
The principle of the invention is as follows: the 4-vinylphenylboronic acid layer is linked to the surface of the lithium nickel cobalt manganese oxide positive electrode material in a covalent bond mode, and boron atoms in the boron-based anion receptor have high electrophilicity, electron deficiency and strong electron-withdrawing capability, so that the lithium nickel cobalt manganese oxide Li Ni is changed0.8Co0.1Mn0.1O2Surface properties of the positive electrode material; thereby improving the electrochemical performance.
Has the advantages that: according to the boron molecule-modified nickel cobalt lithium manganate positive electrode material and the preparation method thereof, the 4-vinyl phenylboronic acid layer is connected to the surface of the nickel cobalt lithium manganate positive electrode material in a covalent bond mode, and a boron group-containing molecular layer of a monomolecular layer is formed on the surface of the nickel cobalt lithium manganate powder, so that the particle size of the material is not influenced, the preparation method is convenient to operate and implement, the modification temperature required in the preparation process is low, the time consumption is small, and the preparation method is suitable for industrial production; in addition, the electrochemical cycle performance of the lithium ion battery prepared by applying the nickel cobalt lithium manganate positive electrode material prepared by the invention is obviously improved, and the capacity retention rate and the rate capability are also obviously improved.
Description of the drawings:
FIG. 1 is a schematic chemical structure diagram of a boron molecule modified lithium nickel cobalt manganese oxide positive electrode material prepared in embodiment 1-2 of the present invention;
FIG. 2 is a schematic diagram of electrochemical cycle performance of button cells prepared by respectively using example 1 and comparative example 1 as positive electrode materials;
fig. 3 is a schematic diagram of electrochemical cycling performance of button cells prepared by using example 2 and comparative example 1 as positive electrode materials respectively.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
example 1:
a preparation method of a boron molecule-modified nickel cobalt lithium manganate positive electrode material comprises the following specific steps: dissolving 3g of nickel cobalt lithium manganate NCM811 powder and 10mg of 4-vinylphenylboronic acid in an acetone solvent, uniformly stirring at 60 ℃ until the nickel cobalt lithium manganate NCM is completely dissolved, refluxing for 12h, filtering out a precipitate, washing for 3 times by using acetone, and then drying at 80 ℃ for 24h to obtain 4-vinylphenylboronic acid modified LiNi0.8Co0.1Mn0.1O2 powder, namely the boron molecule modified nickel cobalt lithium manganate positive electrode material can be obtained.
Example 2:
a preparation method of a boron molecule-modified nickel cobalt lithium manganate positive electrode material comprises the following specific steps: 3g of NCM811 powder of nickel cobalt lithium manganate and 20mg of 4-vinylphenylboronic acid were put in an acetone solvent and stirred uniformly at 65 ℃ and refluxed for 10 hours, and after filtering off the precipitate and washing with acetone for 3 times, followed by drying at 85 ℃ for 26 hours, 4-vinylphenylboronic acid-modified LiNi was obtained0.8Co0.1Mn0.1O2And (5) obtaining the boron molecule modified nickel cobalt lithium manganate cathode material.
Comparative example 1:
the nickel cobalt lithium manganate NCM811 powder without surface treatment is used as the positive electrode material.
Electrochemical performance test:
the positive electrode materials prepared in examples 1-2 and the nickel cobalt lithium manganate NCM811 powder which is not subjected to surface treatment in comparative example 1 are respectively used as positive electrode materials, and button cells are prepared according to the following methods:
fully mixing the positive electrode material, the conductive agent and the binder according to the mass ratio of 90:10:10, stirring to prepare uniform slurry, uniformly coating the uniform slurry on an aluminum foil, cutting the aluminum foil into positive electrode sheets after drying, and drying the positive electrode sheets in vacuum at 100 ℃ for 24 hours; at 1.0mol/L LiPF6/(EC + DMC + EMC) (EC, DMC, EMC volume ratio 1: 1) as electrolyte, metal lithium as counter electrode, Cellgard-2400 type polypropylene film as diaphragmAnd assembling the button cell in an argon atmosphere glove box.
The test is carried out on a LanHECT2001A type battery test system, the charging and discharging voltage range is 2.8-4.3V (vs. Li +/Li), as shown in figures 2-3, and figure 2 is a schematic diagram of the electrochemical cycle performance of the button cell prepared in example 1 and comparative example 1; fig. 3 is a schematic diagram of the electrochemical cycling performance of the button cells prepared in example 2 and comparative example 1; other test results are shown in table 1:
table 1 button cell performance test comparison of examples 1-2 and comparative example 1
| Test index | Example 1 | Example 2 | Comparative example 1 |
| Discharge capacity (mAh/g) of 0.1C | 200.2 | 200.5 | 199.8 |
| Discharge capacity after 500C cycles (mAh/g) | 169.3 | 171.9 | 150 |
| Capacity retention rate | 84.5％ | 85.7％ | 75.1％ |
As can be seen from table 1, the button cell prepared from the lithium nickel cobalt manganese oxide powder without surface treatment in comparative example 1 has a discharge capacity of 150mAh/g after 500 cycles, and a capacity retention rate of 75.1%; after 500 cycles, the discharge capacity of the button cell prepared from the anode material prepared in the embodiment 1 is 169.3mAh/g, and the capacity retention rate is 84.5%; after 500 cycles, the button cell prepared from the positive electrode material prepared in the example 2 has a discharge capacity of 171.9mAh/g and a capacity retention rate of 85.7%. This is a great improvement over comparative example 1.
According to the boron molecule modified nickel cobalt lithium manganate positive electrode material and the preparation method thereof, the 4-vinyl phenylboronic acid layer is connected to the surface of the nickel cobalt lithium manganate positive electrode material in a covalent bond mode, a boron group-containing molecular layer of a single molecular layer is formed on the surface of nickel cobalt lithium manganate powder, the electrochemical cycle performance of a lithium ion battery prepared by applying the prepared nickel cobalt lithium manganate positive electrode material is obviously improved, and the capacity retention rate and the rate capability are also obviously improved.
Claims (6)
1. The boron molecule-modified nickel cobalt lithium manganate positive electrode material is characterized in that the surface of the nickel cobalt lithium manganate positive electrode material is modified and coated with a nickel cobalt lithium manganate positive electrode material which is linked with 4-vinylphenylboronic acid; the surface modification coating linking mode is a covalent bond linking mode; the surface-modified and coated boron-containing molecules are monomolecular layers; the thickness of the modified layer is 1-5 nm.
2. The boron molecule-modified nickel cobalt lithium manganate positive electrode material of claim 1, wherein: the lithium nickel cobalt manganese oxide positive electrode material is a lithium nickel cobalt manganese oxide NCM811 material.
3. The method for preparing the boron molecule-modified nickel cobalt lithium manganate positive electrode material as defined in claim 1, wherein the nickel cobalt lithium manganate positive electrode material and 4-vinylphenylboronic acid are dissolved in an acetone solvent according to the mass ratio of 300:1-300:2Stirring evenly until the mixture is completely dissolved, filtering out precipitates after refluxing, washing the precipitates for 3 times by acetone, and drying the precipitates in a drying oven to obtain the 4-vinylphenylboronic acid modified LiNi0.8Co0.1Mn0.1O2And (5) obtaining the boron molecule modified nickel cobalt lithium manganate cathode material.
4. The method for preparing the boron molecule-modified nickel cobalt lithium manganate positive electrode material according to claim 3, wherein the method comprises the following steps: the stirring temperature of the stirring is 55-65 ℃.
5. The method for preparing the boron molecule-modified nickel cobalt lithium manganate positive electrode material according to claim 4, wherein the method comprises the following steps: the reflux time is 10-13 h.
6. The method for preparing the boron molecule-modified nickel cobalt lithium manganate positive electrode material according to claim 5, characterized in that: after the acetone is washed, the drying temperature of drying in an oven is 75-85 ℃; the drying time is 24-26 h.
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