CN109192968B - Composite positive electrode material, preparation method thereof, positive electrode and lithium battery - Google Patents

Composite positive electrode material, preparation method thereof, positive electrode and lithium battery Download PDF

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CN109192968B
CN109192968B CN201811197474.4A CN201811197474A CN109192968B CN 109192968 B CN109192968 B CN 109192968B CN 201811197474 A CN201811197474 A CN 201811197474A CN 109192968 B CN109192968 B CN 109192968B
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positive electrode
ruthenium
composite
aqueous solution
ternary
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CN109192968A (en
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谢迪志
钟毅
王海涛
杨亿华
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Hunan Jinfuli New Energy Co ltd
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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
    • 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
    • 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
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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

Abstract

The invention relates to a composite anode material and a preparation method thereof, the composite anode material comprises a ternary material and ruthenium fluoride coated on the surface of the ternary material, and the molecular formula of the ternary material is as follows: LiNixCoyMn1‑x‑yO2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and the mass content of ruthenium fluoride in the composite anode material is 0.2-0.6%. The composite cathode material has good cycle performance and rate capability. In addition, the application also relates to a positive electrode and a lithium battery.

Description

Composite positive electrode material, preparation method thereof, positive electrode and lithium battery
Technical Field
The invention relates to the technical field of lithium battery materials, in particular to a composite positive electrode material, a preparation method thereof, a positive electrode and a lithium battery.
Background
Lithium ion batteries, as a secondary battery, have been widely used in the current market because of their advantages of no pollution, no memory effect, high energy density, good cycle performance, environmental friendliness, etc. Of all the materials that make up lithium-ion batteries, the positive electrode material is the key component, which directly determines the energy density and cost of the overall battery.
LiCoO is a common cathode material at present2、LiMn2O4、LiNiO2、LiFePO4And the like. Among them, LiCoO2In the charging process, phase change is easy to occur, so that Co loss is caused; LiMn2O4In the circulation process, the octahedral structure is easy to distort, and the capacity attenuation is serious; LiNiO2It is difficult to prepare pure-phase stoichiometric LiNiO2. Ternary material LiNi with laminated structurexCoyMn1-x-yO2(x is more than 0 and less than 1, y is more than 0 and less than 1) can weaken the application disadvantages of the three materials, and simultaneously, the three materials have the advantages because of ternary synergy, thereby having the advantages of three materialsThe characteristics of high specific capacity, stable structure and the like have gradually been widely noticed and regarded by people.
Ternary material LiNixCoyMn1-x-yO2(x is more than 0 and less than 1, and y is more than 0 and less than 1) in practical application, the problems of poor rate capability, unstable cycle performance under high voltage and the like mainly exist. In this regard, the material is generally modified by surface coating and bulk doping. The surface coating is typically a metal oxide, phosphate, organic polymer, and the like, with metal oxides and phosphates being most common. However, the two types of coatings have different weaknesses, and when the metal oxide coating is adopted, the metal oxide coating is attacked by HF generated by decomposition of the electrolyte, and the coating layer of the metal oxide coating becomes unstable along with increase of the cycle number; with phosphate coating, although resistant to HF attack, its low electronic conductivity prevents Li+The rapid migration at the material interface influences the exertion of the rate capability of the material.
Disclosure of Invention
Based on this, there is a need to provide a composite positive electrode material having good cycle performance and rate capability.
A composite positive electrode material comprises a ternary material and ruthenium fluoride coated on the surface of the ternary material, wherein the molecular formula of the ternary material is as follows: LiNixCoyMn1-x-yO2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and the mass content of ruthenium fluoride in the composite anode material is 0.2-0.6%.
The composite anode material has lower Gibbs function of ruthenium fluoride, better chemical stability, can resist the attack of HF in electrolyte, can stably exist in long-time charge-discharge circulation, and the ruthenium fluoride has better electronic conductivity, adopts the ruthenium fluoride to coat the ternary material, and controls the mass content of the ruthenium fluoride in the composite anode material to be within the range of 0.2-0.6 percent, so that the performances of the ruthenium fluoride and the ternary material are fully exerted, the stability of a coating layer can be ensured, the composite anode material has good circulation performance, and Li can ensure that+Fast migration at the material interface, thereby leading the composite anode material to have good performanceRate capability.
Specifically, when the mass content of ruthenium fluoride in the composite cathode material is less than 0.2%, the coating effect is not ideal; when the mass content of the ruthenium fluoride in the composite cathode material is more than 0.6%, the proportion of non-electrochemical activity is increased, so that the capacity exertion of the ternary material is influenced.
Further, the mass content of ruthenium fluoride in the composite cathode material is 0.4%.
The application also provides a preparation method of the composite anode material, and the specific technical scheme is as follows:
a preparation method of the composite cathode material comprises the following steps:
providing a soluble ruthenium salt aqueous solution, an ammonium fluoride aqueous solution and a ternary material, wherein the molecular formula of the ternary material is as follows: LiNixCoyMn1-x-yO2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and the addition amount of the soluble ruthenium salt aqueous solution, the ammonium fluoride aqueous solution and the ternary material is based on the mass content of ruthenium fluoride in the finally prepared composite anode material being 0.2-0.6%;
and mixing the ternary material and a soluble ruthenium salt aqueous solution, adding the ammonium fluoride aqueous solution, heating and stirring until the water is completely evaporated, drying, sintering and crushing to obtain the composite cathode material.
According to the preparation method of the composite cathode material, the soluble ruthenium salt aqueous solution and the ternary material are mixed, the soluble ruthenium salt is partially hydrolyzed in water to form ruthenium hydroxide, the ruthenium hydroxide is gelled on the surface of the ternary material, the ammonium fluoride aqueous solution is added for reaction, the formed coating layer is more uniform and is more tightly combined with the ternary material, and the advantages of ruthenium fluoride and the ternary material can be fully exerted, so that the prepared composite cathode material has good cycle performance and rate capability.
In one embodiment, the soluble ruthenium salt is selected from at least one of ruthenium chloride, ruthenium nitrate, and ruthenium acetate.
In one embodiment, the concentration of the soluble ruthenium salt aqueous solution is 0.02mol/L to 0.08 mol/L; the concentration of the ammonium fluoride aqueous solution is 0.1 mol/L-0.5 mol/L.
The concentration of the soluble ruthenium salt aqueous solution and the concentration of the ammonium fluoride aqueous solution are controlled, so that the continuity and the distribution uniformity of the coating substance on the surface of the substrate can be ensured.
In one embodiment, the ternary material and the soluble ruthenium salt aqueous solution are mixed at a stirring rate of 500r/min to 600 r/min.
The ternary material and the soluble ruthenium salt water solution are mixed at a stirring speed of 500 r/min-600 r/min, so that the coating is more uniform.
In one embodiment, the heating and stirring speed is 400 r/min-500 r/min; the heating temperature is 50-60 ℃.
The heating and stirring speed is controlled to be 400 r/min-500 r/min, the heating temperature is controlled to be 50-60 ℃, so that the reaction is more complete, and the coating is more uniform.
In one embodiment, the drying temperature is 100-120 ℃, and the drying time is 5-10 hours.
And controlling the drying temperature to be 100-120 ℃ and the drying time to be 5-10 hours, so that the water in the composite anode material is completely removed.
In one embodiment, the sintering temperature is 400-500 ℃, and the sintering time is 4-8 hours.
The application also provides a positive pole, and the specific technical scheme is as follows:
a positive electrode is prepared from the composite positive electrode material or the composite positive electrode material prepared by the preparation method of the composite positive electrode material.
The application also provides a lithium battery, and the specific technical scheme is as follows:
the positive electrode of the lithium battery adopts the positive electrode.
Drawings
Fig. 1 is an SEM image of a composite cathode material prepared in example 1;
FIG. 2 is a comparison of the first charging and discharging curves before and after coating of the ternary material in example 1;
FIG. 3 is a graph comparing the cycle performance before and after cladding of the ternary material of example 1;
FIG. 4 is a graph comparing the performance of the ternary energy material before and after coating in example 1;
fig. 5 is an SEM image of a composite cathode material prepared in example 3;
FIG. 6 is a comparison of the first charging and discharging curves before and after coating with the ternary material in example 3;
FIG. 7 is a graph comparing the cycle performance before and after cladding of the ternary material of example 3;
FIG. 8 is a graph comparing the performance of the ternary energy material of example 3 before and after coating.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The following are specific examples.
Example 1
1.41g of ruthenium acetate (0.005mol) and 0.51g of ammonium fluoride drug (0.014mol) were weighed out and placed in different beakers, and 150mL and 50mL of pure water were added thereto, and stirred uniformly to prepare an aqueous ruthenium acetate solution and an aqueous ammonium fluoride solution. 200g of LiNi0.5Co0.2Mn0.3The mixture was added to an aqueous ruthenium acetate solution and stirred at a rate of 600 r/min. After about 20min, the stirring speed is reduced to 500r/min, ammonium fluoride aqueous solution is slowly dripped, the mixture is heated in water bath at 55 ℃ until the water is completely evaporated, and the mixture is dried for 6 hours at 110 ℃, thenThen sintering for 6 hours at 450 ℃, crushing, and sieving with a 325-mesh sieve to obtain the composite anode material.
Through detection, the mass content of the ruthenium fluoride in the composite cathode material is 0.4%.
SEM images after coating, comparison of first charge and discharge curves before and after coating, and comparison of cycle performance, and the comparison of multiplying power performance are respectively shown in figures 1-4.
As can be seen from the figures 1 to 4, the microscopic morphology of the material is not affected after the ruthenium fluoride is coated, the first charging voltage can be reduced, and the cycle performance and the rate performance under high rate of the material are greatly improved.
Example 2
0.71g of ruthenium acetate (0.0025mol) and 0.26g of ammonium fluoride drug (0.007mol) are weighed and respectively placed in different beakers, 150mL of pure water and 50mL of pure water are respectively added, and the mixture is uniformly stirred to prepare ruthenium acetate aqueous solution and ammonium fluoride aqueous solution. 200g of LiNi0.8Co0.1Mn0.1The mixture was put into an aqueous ruthenium acetate solution and stirred at a rate of 500 r/min. After about 20min, the stirring speed is reduced to 400r/min, ammonium fluoride aqueous solution is slowly dropped and heated in a water bath at the temperature of 60 ℃ until the water is completely evaporated. Drying at 100 ℃ for 10 hours, then sintering at 500 ℃ for 4 hours, crushing, and sieving with a 325-mesh sieve to obtain the composite cathode material.
Through detection, the mass content of the ruthenium fluoride in the composite cathode material is 0.2%.
Example 3
1.41g of ruthenium acetate (0.005mol) and 0.51g of ammonium fluoride drug (0.014mol) were weighed out and placed in different beakers, and 150mL and 50mL of pure water were added thereto, and stirred uniformly to prepare an aqueous ruthenium acetate solution and an aqueous ammonium fluoride solution. 200g of LiNi0.8Co0.1Mn0.1The mixture was added to an aqueous ruthenium acetate solution and stirred at a rate of 600 r/min. After about 20min, the stirring speed is reduced to 500r/min, ammonium fluoride aqueous solution is slowly dropped, and the mixture is heated in a water bath at the temperature of 50 ℃ until the water is completely evaporated. Drying at 120 ℃ for 5 hours, then sintering at 400 ℃ for 8 hours, crushing, and sieving with a 325-mesh sieve to obtain the composite cathode material.
Through detection, the mass content of the ruthenium fluoride in the composite cathode material is 0.4%.
SEM images after coating, comparison of first charge and discharge curves before and after coating, and comparison of cycle performance, and the comparison of rate performance are respectively shown in FIGS. 5 to 8.
As can be seen from the graphs of 5-8, the microscopic morphology of the material is not affected after the ruthenium fluoride is coated, the first charging voltage can be reduced, and the cycle performance and the rate performance under high rate of the material are greatly improved.
Comparative example 1
Comparative example 1 is substantially the same as example 3 except that in comparative example 1, 5.6g (0.02mol) of ruthenium acetate and 2.22g (0.06mol) of ammonium fluoride drug were added.
The detection shows that the mass content of the ruthenium fluoride in the composite anode material is 1.6%, the first charging specific capacity of the material is only 160.8mAh/g when the material is charged and discharged at 2.75-4.2V, 0.2C and 25 ℃, and is about 10mAh/g lower than that of a matrix material, so that the material capacity is greatly reduced.
Comparative example 2
Comparative example 2 is substantially the same as example 3 except that in comparative example 2, 0.28g (0.001mol) of ruthenium acetate and 0.111g (0.003mol) of ammonium fluoride drug were added.
The detection shows that the mass content of the ruthenium fluoride in the composite anode material is 0.07%, the cycle performance and the rate performance of the material are both close to those of a base material, and the coating effect is not obvious.
Example 4
2.13g of ruthenium acetate (0.0076mol) and 0.78g of ammonium fluoride (0.021mol) are weighed and placed in different beakers, 150mL of pure water and 50mL of pure water are respectively added, and the mixture is uniformly stirred to prepare ruthenium acetate aqueous solution and ammonium fluoride aqueous solution. 200g of LiNi0.8Co0.1Mn0.1The solution was added to ruthenium acetate and stirred at 600 r/min. After about 20min, the stirring rate was reduced to 500r/min, and an aqueous ammonium fluoride solution was slowly dropped and heated in a water bath at 55 ℃ until the water evaporation was completed. Drying at 120 ℃ for 6 hours, then sintering at 450 ℃ for 6 hours, crushing, and sieving with a 325-mesh sieve to obtain the composite cathode material.
Through detection, the mass content of the ruthenium fluoride in the composite cathode material is 0.6%.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The composite cathode material is characterized by comprising a ternary material and ruthenium fluoride coated on the surface of the ternary material, wherein the molecular formula of the ternary material is as follows: LiNixCoyMn1-x-yO2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and the mass content of ruthenium fluoride in the composite anode material is 0.2-0.6%.
2. The preparation method of the composite cathode material is characterized by comprising the following steps of:
providing a soluble ruthenium salt aqueous solution, an ammonium fluoride aqueous solution and a ternary material, wherein the molecular formula of the ternary material is as follows: LiNixCoyMn1-x-yO2Wherein x is more than 0 and less than 1, y is more than 0 and less than 1, and the addition amount of the soluble ruthenium salt aqueous solution, the ammonium fluoride aqueous solution and the ternary material is based on the mass content of ruthenium fluoride in the finally prepared composite anode material being 0.2-0.6%;
and mixing the ternary material and a soluble ruthenium salt aqueous solution, adding the ammonium fluoride aqueous solution, heating and stirring until the water is completely evaporated, drying, sintering and crushing to obtain the composite anode material, wherein the composite anode material comprises the ternary material and ruthenium fluoride coated on the surface of the ternary material.
3. The method for preparing a composite positive electrode material according to claim 2, wherein the soluble ruthenium salt is at least one selected from the group consisting of ruthenium chloride, ruthenium nitrate and ruthenium acetate.
4. The method for preparing the composite positive electrode material according to claim 2, wherein the concentration of the soluble ruthenium salt aqueous solution is 0.02 to 0.08 mol/L; the concentration of the ammonium fluoride aqueous solution is 0.1 mol/L-0.5 mol/L.
5. The method for preparing the composite positive electrode material according to claim 2, wherein the ternary material is mixed with the aqueous solution of the soluble ruthenium salt at a stirring rate of 500 to 600 r/min.
6. The method for preparing the composite positive electrode material according to claim 2, wherein the heating and stirring rate is 400 to 500 r/min; the heating temperature is 50-60 ℃.
7. The preparation method of the composite cathode material according to claim 2, wherein the drying temperature is 100 ℃ to 120 ℃, and the drying time is 5 to 10 hours.
8. The method for producing a composite positive electrode material according to any one of claims 2 to 7, wherein the sintering temperature is 400 ℃ to 500 ℃ and the sintering time is 4 to 8 hours.
9. A positive electrode, characterized in that a raw material for producing the positive electrode comprises the composite positive electrode material according to claim 1 or the composite positive electrode material produced by the method for producing the composite positive electrode material according to any one of claims 2 to 8.
10. A lithium battery characterized in that the positive electrode of claim 9 is used as the positive electrode.
CN201811197474.4A 2018-10-15 2018-10-15 Composite positive electrode material, preparation method thereof, positive electrode and lithium battery Active CN109192968B (en)

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Citations (2)

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CN101156260A (en) * 2005-04-15 2008-04-02 能原材公司 Cathode active material coated with fluorine compound for lithium secondary batteries and method for preparing the same
CN102738458A (en) * 2012-06-13 2012-10-17 北京有色金属研究总院 Surface modification method of lithium-rich cathode material

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CN102496722A (en) * 2011-12-22 2012-06-13 南开大学 Layered lithium-rich anode material clad by metal fluoride, and preparation method thereof
KR101561608B1 (en) * 2014-10-14 2015-10-20 한국화학연구원 The method for preparation of positive active material for lithium air battery and the positive active material thereby
KR20170073217A (en) * 2015-12-18 2017-06-28 삼성전자주식회사 Composite positive active material, preparing method thereof, positive electrode including the same, and lithium battery including the positive electrode
CN106654209B (en) * 2016-12-22 2019-01-29 华中科技大学 A kind of lithium ion battery composite cathode material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101156260A (en) * 2005-04-15 2008-04-02 能原材公司 Cathode active material coated with fluorine compound for lithium secondary batteries and method for preparing the same
CN102738458A (en) * 2012-06-13 2012-10-17 北京有色金属研究总院 Surface modification method of lithium-rich cathode material

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