CN113451568A - Preparation method of ester organic matter in-situ coated high-nickel cathode material - Google Patents

Preparation method of ester organic matter in-situ coated high-nickel cathode material Download PDF

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CN113451568A
CN113451568A CN202110717223.XA CN202110717223A CN113451568A CN 113451568 A CN113451568 A CN 113451568A CN 202110717223 A CN202110717223 A CN 202110717223A CN 113451568 A CN113451568 A CN 113451568A
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organic matter
ester organic
nickel
preparation
cathode material
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汪达
陶旺
李彩婷
刘熙
张子健
张秉坤
吴枫
刘争
张业龙
陈鹏飞
邓魁荣
邱振平
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Wuyi University
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Wuyi University
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • H01M4/52—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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Electrochemistry (AREA)
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  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a preparation method of an ester organic matter in-situ coated high-nickel anode material, which comprises the following steps: s1), slowly dripping a certain amount of ester organic solution into an ether solvent containing a high nickel layered material to obtain a mixed solution; s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder. According to the invention, the coating layers with different thicknesses can be constructed by using the ester organic matter gel liquid; the ester organic matter used in the invention has strong electron-withdrawing groups, is easy to carry out anionic polymerization reaction under the action of a weaker initiator (OH-), can achieve the coating effect by depending on the characteristic of moisture in-situ polymerization of air, improves the electrochemical performance of the high-nickel anode material, achieves the purposes of stable circulation and reduction of storage cost of the high-nickel anode material, and effectively avoids the influence of moisture in the air.

Description

Preparation method of ester organic matter in-situ coated high-nickel cathode material
Technical Field
The invention relates to the technical field of anode materials, in particular to a preparation method of an ester organic matter in-situ coated high-nickel anode material.
Background
Lithium ion batteries, which are one of the typical new energy sources in the 21 st century, are increasingly receiving market pursuits due to the ever-increasing demands of people on electronic products, hybrid power/pure electric vehicles, and large energy storage devices.
In the current commercial market, the most commonly used material is the olivine-type structure LiFePO 4; spinel-type structure LiMn2O4And high nickel layered structure material Li [ Ni ]xMnyCo1-x-y]O2. The three have respective advantages and disadvantages, but the requirements of high voltage and large capacity of the pure electric vehicle are met. High nickel layered structure material Li [ Ni ]xMnyCo1-x-y]O2Has wide development prospect. The electrode has low cost and low toxicity, can provide high capacity of 200mAh/g in the working voltage range of the electrode of 3V-4.5V, has wide development prospect, and has attracted wide commercial attention at present.
Although the high specific capacity nickel-rich layered structure oxide material has obvious advantages in meeting the requirement of a power battery on high specific power, some unavoidable problems exist at present:
in the synthesis process, low-price nickel can migrate into lithium vacancies to cause lithium-nickel mixed discharge, so that the voltage of the material is reduced, and the capacity is reduced; the electrode material is in long-term contact with the electrolyte in the circulating process, the transition metal element is easy to dissolve, the electrolyte is decomposed on the surface of the electrode to form a thick solid electrolyte intermediate layer, and the attack of acidic substances in the electrolyte causes the rapid increase of the impedance of the battery, so that the capacity of the battery is attenuated in the circulating process; under higher cut-off voltage, because transition metal is easy to be oxidized and reduced, element atoms migrate, oxygen element release causes vacancies, defects are generated along with material strain, irreversible phase change occurs, so that the stability of the material is reduced, partial potential safety hazards exist, and the problems seriously restrict large-scale application. Therefore, the optimization and modification of the high nickel layered oxide are very important, so that the aim of further improving the cycle stability and safety of the high nickel cathode material is fulfilled, and the requirements of the commercial market on high specific capacity, low cost, safety and stability are met.
At present, the electrochemical performance of the high-nickel layered material is modified mainly by the following steps:
1. synthesizing and optimizing;
2. doping ions;
3. surface modification;
the surface modification is an effective measure for improving the interface condition and the cycle performance and stability, and can effectively solve the problems of serious capacity attenuation, low cycle performance and poor environmental stability of the high-nickel material.
In order to overcome the disadvantages of poor cyclicity, low stability, voltage decay and the like of the high nickel layered structure material, researchers utilize an inorganic material as a surface coating for coating modification to improve the electrochemical performance of the material.
Researches find that the electrochemical performance of the electrode material with the high nickel laminated structure is improved to different degrees due to different physicochemical properties of the material coated on the surface after the surface coating treatment.
For the coating used for coating the surface of the positive electrode material, most of the coating is made of an inorganic material, alumina (Al)2O3)[7]Titanium dioxide (TiO)2) And lithium iron phosphate (LiFePO)4) And the like.
Although these surface-modified metal oxides are stable in properties and uniform in distribution of the nanoparticles, there are inevitable drawbacks such as: the conductivity is low, and in the circulation process, the lithium ion diffusion is hindered, and the charge transfer resistance is increased, so that the inorganic material is difficult to meet the actual requirement.
In addition, researchers have also proposed the use of conductive polymer polymers such as: polypyrrole; polyaniline; polythiophene and its derivatives, etc., as a coating layer of the high nickel positive electrode material, but inevitably occurs: the coating process is complex and the cost is high; is difficult to dissolve, has agglomeration phenomenon, is difficult to ensure uniformity and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the ester organic matter in-situ coated high-nickel cathode material, and the material prepared by the invention does not need a dry storage environment and has good external storage adaptability.
The technical scheme of the invention is as follows: a preparation method of an ester organic matter in-situ coated high-nickel cathode material comprises the following steps:
s1), slowly dripping a certain amount of ester organic solution into an ether solvent containing a high nickel layered material to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
Preferably, in step S1), the ester organic compound is: has strong electron-withdrawing group-cyano group, and can easily carry out anionic polymerization reaction under the action of a weaker initiator OH-.
Preferably, in step S1), the high-nickel layered material is LiNixMnyCozO2(Ni>0.6)。
Preferably, in step S1), the ether solvent is DME solvent.
Preferably, in step S1), the dropping rate of the ester organic solution is 5 seconds per drop.
Preferably, in step S2), the magnetic stirring conditions are room temperature 25 deg.C, humidity 70%, 200 r/S.
Preferably, in step S2), the conditions of the rotary heating are: the rotation rate was 200r/s and the heating temperature was 85 ℃.
Preferably, in step S1), the mass ratio of the ester organic substance to the high nickel layered material is: 5: 100 or 1: 20.
the invention has the beneficial effects that:
1. according to the invention, the coating layers with different thicknesses can be constructed by using the ester organic matter gel liquid;
2. the ester organic substance solution is slowly dripped and stirred, so that the polymerization of the ester organic substance is initiated by moisture in the air, and the ester organic substance has strong electron-withdrawing groups and is easy to carry out anionic polymerization reaction under the action of a weaker initiator (OH-);
3. the method removes redundant solvent by rotary evaporation to dryness, and retains the organic matter after polymerization to achieve the purpose of uniform coating;
4. the ester organic matter used in the invention has strong electron-withdrawing groups, is easy to carry out anionic polymerization reaction under the action of a weaker initiator (OH-), can achieve the coating effect by relying on the characteristic of moisture in-situ polymerization of air, has a simple process, exceeds the effect which can be achieved by complicated operation steps in the prior art, further improves the effect of the electrochemical performance of the high-nickel anode material, realizes the purposes of stable circulation and reduction of storage cost of the high-nickel anode material, and effectively avoids the influence of moisture in the air.
Drawings
FIG. 1 is a graph comparing the performance of the material prepared in example 1 of the present invention at 0.1C first cycle and 0.5C second cycle at room temperature; wherein, fig. 1(a) is: initial charge-discharge curves of the primary cell and the PBCA-NCM811/Li cell at 0.1C and 100 th charge-discharge curves of the primary cell and the PBCA-NCM811/Li cell at 0.5C, with a voltage range of 4.3-3V (30. C);
FIG. 1(b) shows: comparing the cycling performance curves of the original battery and the PBCA-NCM811/Li battery in the voltage range of 0.5C and 4.3-3V (30. C);
FIG. 2 is a graph comparing the performance of the material prepared in example 1 of the present invention at high temperature 50 ℃ for the first 0.1C cycle and the 0.5C cycle;
wherein, fig. 2(e) is: initial charge-discharge curves of the primary battery and the PBCA-NCM811/Li battery in the voltage range of 0.1C, 4.3-3V (50. C);
FIG. 2(f) is: cycling performance of the pristine and PBCA-NCM811/Li cells in the voltage range of 0.5C and 4.3-3V (50. C).
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings:
example 1
The embodiment provides a preparation method of an ester organic matter in-situ coated high-nickel cathode material, which comprises the following steps:
s1), 0.1g of LiNi containing high-nickel layered material0.8Co0.1Mn0.1O2Dispersing in 1mLDME solvent, and continuously stirring;
s2), slowly dripping 0.001g of ester organic substance enbuester solution into an ether solvent containing a high nickel layered material at a speed of 1 drop in 5 seconds to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
Example 2
The embodiment provides a preparation method of an ester organic matter in-situ coated high-nickel cathode material, which comprises the following steps:
s1), dispersing 0.1g of the high nickel-containing layered material in 1ml dme solvent, and continuously stirring;
s2), 0.003g of ester organic substance enbuester solution is dripped into the ether solvent containing the high-nickel layered material at the speed of 1 drop in 5 seconds to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
Example 3
The embodiment provides a preparation method of an ester organic matter in-situ coated high-nickel cathode material, which comprises the following steps:
s1), dispersing 0.1g of the high nickel-containing layered material in 1ml dme solvent, and continuously stirring;
s2), slowly dripping 0.005g of ester organic substance enbuester solution into an ether solvent containing a high nickel layered material at a speed of 1 drop in 5 seconds to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
Example 4
The embodiment provides a preparation method of an ester organic matter in-situ coated high-nickel cathode material, which comprises the following steps:
s1), dispersing 0.1g of the high nickel-containing layered material in 1ml dme solvent, and continuously stirring;
s2), slowly dripping 0.007g of ester organic substance enbuester solution into an ether solvent containing a high nickel layered material at a speed of 1 drop in 5 seconds to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
Example 5
The embodiment provides a preparation method of an ester organic matter in-situ coated high-nickel cathode material, which comprises the following steps:
s1), dispersing 0.1g of the high nickel-containing layered material in 1ml dme solvent, and continuously stirring;
s2), slowly dripping 0.010g of ester organic substance enbuester solution into an ether solvent containing a high nickel layered material at a speed of 1 drop in 5 seconds to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
Example 6
Performance test of the cathode Material
At room temperature, the first and second cycle performance are compared and the results are shown in FIGS. 1(a), (b), from which it can be seen that: the retention rate of 5% PBCA-NCM811 at 0.5C for 100 cycles reaches 84.3%, while the retention rate of NCM811 at cycles is only 74.3%, which shows that 5% PBCA has obvious effect on the stability of NCM 811.
And the first loop and cycle performance are compared under a high temperature 50 ℃ incubator, and the comparison result is shown in figures 2(e), (f), and can be seen from the figures: under high temperature, 5% PBCA can effectively avoid the phenomenon of capacity 'diving' of NCM811, and the effect on the high-temperature circulation stability is more obvious.
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.

Claims (8)

1. The preparation method of the ester organic matter in-situ coated high-nickel cathode material is characterized by comprising the following steps of:
s1), slowly dripping a certain amount of ester organic solution into an ether solvent containing a high nickel layered material to obtain a mixed solution;
s2), stirring the mixed solution in air by magnetic stirring to make the water in the air initiate the polymerization of the organic matter, then rotary heating to evaporate the solvent to dryness, and collecting the powder.
2. The preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in step S1), the ester organic compound is: has strong electron-withdrawing group-cyano group, and can easily carry out anionic polymerization reaction under the action of a weaker initiator OH-.
3. The preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in step S1), the high-nickel layered material is LiNixMnyCozO2(Ni>0.6)。
4. The preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in the step S1), the ether solvent is DME solvent.
5. The preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in the step S1), the dropping speed of the ester organic solution is 5 seconds per drop.
6. The preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in step S1), the mass ratio of the ester organic substance to the high nickel layered material is: 5: 100 or 1: 20.
7. the preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in the step S2), the magnetic stirring conditions are that the room temperature is 25 ℃, the humidity is 70 percent and the stirring speed is 200 r/S.
8. The preparation method of the ester organic matter in-situ coated high-nickel cathode material according to claim 1, characterized by comprising the following steps: in step S2), the conditions of the rotary heating are: the rotation rate was 200r/s and the heating temperature was 80 ℃.
CN202110717223.XA 2021-06-28 2021-06-28 Preparation method of ester organic matter in-situ coated high-nickel cathode material Pending CN113451568A (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
US20170338490A1 (en) * 2016-05-20 2017-11-23 GM Global Technology Operations LLC Polymerization process for forming polymeric ultrathin conformal coatings on electrode materials
CN111211299A (en) * 2020-01-07 2020-05-29 中南大学 Modified lithium ion battery positive electrode material coated with strong electronegative organic matter layer and preparation method thereof
CN111916693A (en) * 2020-06-28 2020-11-10 南昌大学 Method for preparing organic matter coated high-nickel cathode material

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US20170338490A1 (en) * 2016-05-20 2017-11-23 GM Global Technology Operations LLC Polymerization process for forming polymeric ultrathin conformal coatings on electrode materials
CN111211299A (en) * 2020-01-07 2020-05-29 中南大学 Modified lithium ion battery positive electrode material coated with strong electronegative organic matter layer and preparation method thereof
CN111916693A (en) * 2020-06-28 2020-11-10 南昌大学 Method for preparing organic matter coated high-nickel cathode material

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Application publication date: 20210928