CN108417783B - Niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material and preparation method thereof - Google Patents

Niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material and preparation method thereof Download PDF

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CN108417783B
CN108417783B CN201810014178.XA CN201810014178A CN108417783B CN 108417783 B CN108417783 B CN 108417783B CN 201810014178 A CN201810014178 A CN 201810014178A CN 108417783 B CN108417783 B CN 108417783B
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manganese
niobium
tin oxide
nickel cobalt
mixture
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CN108417783A (en
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许开华
许国干
徐世国
徐中领
张玉军
王星宁
李伟
刘钰
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Greenmei (Hubei) new energy materials Co.,Ltd.
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GEM Wuxi Energy Materials 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
    • H01M4/485—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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • 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
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Abstract

The invention is suitable for the technical field of lithium batteries, and provides a niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material and a preparation method thereof, wherein the method comprises the following steps: s1, weighing tin oxide and oxides of niobium and manganese, mixing and then carrying out low-temperature treatment to obtain a niobium-manganese-tin oxide mixture; s2, weighing a nickel-cobalt-manganese ternary material according to a proportion, and fully and uniformly mixing the nickel-cobalt-manganese ternary material with the niobium-manganese tin oxide mixture to obtain a mixture; and S3, loading the mixture obtained in the step S2 into a sagger, and sintering to obtain the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate positive electrode material. The invention adopts niobium-manganese modified tin oxide to coat the ternary cathode material, can effectively protect the surface structure of the material and reduce Ni2+The generation of the tin oxide can effectively inhibit the escape of lattice oxygen, improve the cycle and rate performance of the material, and simultaneously can effectively reduce the side effect caused by the material defects of the tin oxide, so that the material performance is more excellent.

Description

Niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material and preparation method thereof
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material and a preparation method thereof.
Background
The nickel-cobalt-manganese ternary lithium ion battery anode material is widely applied to the industry of new energy batteries due to the high energy density and the relatively low cost. The nickel cobalt lithium manganate (LNCM), especially a high nickel product, has poor structural stability, and is easy to cause the escape of lattice oxygen due to the de-intercalation of Li ions and the change of valence states of Ni, Co and Mn ions in the charging and discharging processes, so that the collapse of the material structure is caused, and the cycle life and the safety of the material are greatly damaged; at the same time, the surface structure is easy to react with the electrolyte, Ni3+Is very easy to be reduced into Ni2+Inert valence state, surface Ni thereof2+Ni content in the whole crystal structure2+Two thirds of the total weight of Li, thereby resulting in Li+、Ni2+Mixed arrangement affects the first effect and the cycle performance of the product.
Disclosure of Invention
In view of the above problems, the invention aims to provide a niobium-manganese modified tin oxide coated lithium nickel cobalt manganese oxide positive electrode material and a preparation method thereof, and aims to solve the technical problem of poor cycle performance of the existing lithium nickel cobalt manganese oxide battery.
The preparation method of the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate positive electrode material comprises the following steps:
s1, weighing tin oxide and oxides of niobium and manganese, mixing and then carrying out low-temperature treatment to obtain a niobium-manganese-tin oxide mixture;
s2, weighing a nickel-cobalt-manganese ternary material according to a proportion, and fully and uniformly mixing the nickel-cobalt-manganese ternary material with the niobium-manganese tin oxide mixture to obtain a mixture;
and S3, loading the mixture obtained in the step S2 into a sagger, and sintering to obtain the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate positive electrode material.
Further, in the tin oxide-niobium-manganese oxide weighed in step S1, the molar ratio Sn of tin, niobium and manganese: nb: mn is 1 (0.1-0.3): (0.2-0.5), the low temperature treatment range is 200 ℃ and 500 ℃. .
Further, in step S2, the nickel-cobalt-manganese ternary material is weighed according to the mass ratio that the niobium-manganese-tin oxide mixture accounts for 0.05-0.4% of the nickel-cobalt-manganese ternary material.
Further, in step S3, the sintering temperature in the sintering process is 600-1000 ℃, and the sintering time is 4-12 h.
On the other hand, the nickel cobalt lithium manganate positive electrode material is prepared by the method, the material matrix is a nickel cobalt manganese ternary material, and the material shell layer is a tin oxide-manganese-niobium composite coating layer.
The invention has the beneficial effects that: according to the invention, the manganese modified tin oxide is adopted to form a tin oxide-manganese-niobium composite coating layer on the surface of the material, so that the surface structure of the material is isolated from direct contact with an electrolyte, and meanwhile, the internal resistance is effectively reduced due to the conductivity of the tin oxide, and the electron residue in the charging and discharging process is reduced; in addition, the tin oxide modified by niobium-manganese enables the volume expansion temperature of the tin oxide to be increased due to the addition of niobium in the charging and discharging process, so that the volume expansion of the material is effectively inhibited and slowed down, and due to the addition of manganese, the structure of the niobium-manganese-tin oxide coating layer is more likely to be better matched with a laminated structure and a matrix, so that oxygen vacancies are reduced, and the generation of oxygen defects is inhibited.
Drawings
FIG. 1 is a graph of the number of charge-discharge cycles versus capacity for test example 1 and comparative example 1 of the present invention;
FIG. 2 is a graph showing the number of charge and discharge cycles of the present invention in test example 2 and comparative example 2 as a function of capacity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to explain the technical means of the present invention, the following description will be given by way of specific examples.
The preparation method of the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material provided by the invention comprises the following steps:
and step S1, weighing the tin oxide and the niobium-manganese oxide, mixing and then carrying out low-temperature treatment to obtain the niobium-manganese-tin oxide mixture.
In the oxides of tin oxide, niobium and manganese weighed in the step, the molar ratio of tin, niobium and manganese is Sn: nb: mn is 1 (0.1-0.3): (0.2-0.5), the low temperature treatment range is 200 ℃ and 500 ℃. The tin oxide is tin oxide or tin dioxide. The oxides of niobium and manganese are the general names of oxides of niobium and manganese in various valence states, and there are many choices, for example, niobium oxide can be niobium monoxide, niobium dioxide, niobium trioxide, niobium pentoxide, etc., and manganese oxide can be manganese monoxide, manganese dioxide, etc.
And S2, weighing the nickel-cobalt-manganese ternary material according to the proportion, and fully and uniformly mixing the nickel-cobalt-manganese ternary material with the niobium-manganese tin oxide mixture to obtain a mixture.
The nickel-cobalt-manganese ternary material is weighed according to the mass ratio that the niobium-manganese-tin oxide mixture accounts for 0.05-0.4% of the nickel-cobalt-manganese ternary material.
And S3, loading the mixture obtained in the step S2 into a sagger, and sintering at the sintering temperature of 600-1000 ℃ for 4-12h to obtain the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material.
The nickel-cobalt-manganese ternary material is coated by adopting niobium-manganese modified tin oxide, the inner layer is the nickel-cobalt-manganese ternary material, and the shell layer is a tin oxide-manganese-niobium composite coating layer. The structural stability of nickel cobalt lithium manganate, particularly high nickel products, is not good enough, and the escape of lattice oxygen is easily caused by the de-intercalation of Li ions and the change of valence states of Ni, Co and Mn ions in the charging and discharging processes, so that the collapse of the material structure is caused, and the cycle life and the safety of the material are greatly damaged; if tin oxide is directly used for coating, the tin oxide has the defects that volume expansion is generated in the charging and discharging process, and in addition, the phase structures of the matrix and the tin oxide are not completely the same, the coating layer falls off from the matrix after a period of circulation, and the coating effect is lost. The tin oxide is modified by niobium-manganese, so that the volume expansion temperature of the tin oxide is increased due to the addition of niobium in the charging and discharging processes, the volume expansion of the material is effectively inhibited and slowed down, and the structure of the niobium-manganese-tin oxide coating layer is more likely to have better matching property with a laminated structure and a matrix due to the addition of manganese, so that oxygen vacancy is reduced, and the generation of oxygen defects is inhibited.
The effect of the material is verified by the following test examples and comparative examples.
Test example 1:
weighing tin dioxide, niobium pentoxide and manganese monoxide, wherein the molar ratio of tin, niobium and manganese is Sn: nb: mn 1: 0.1: 0.2, mixing, performing low-temperature treatment at 200 ℃ to obtain a niobium-manganese-tin oxide mixture, weighing an NCM811 ternary material according to the mass ratio of the niobium-manganese-tin oxide mixture accounting for 0.1%, and fully and uniformly mixing the NCM811 ternary material with the niobium-manganese-tin oxide mixture to obtain a mixture; and (3) loading the mixture into a sagger, sintering at 650 ℃ for 6 hours to obtain the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate positive electrode material.
Test example 2:
weighing tin dioxide, niobium pentoxide and manganese monoxide, wherein the molar ratio of tin, niobium and manganese is Sn: nb: mn 1: 0.3: 0.5, mixing, and then processing at 350 ℃ to obtain a niobium-manganese-tin oxide mixture, weighing an NCM523 ternary material according to the mass ratio of the niobium-manganese-tin oxide mixture accounting for 0.25%, and fully and uniformly mixing the NCM523 ternary material with the niobium-manganese-tin oxide mixture to obtain a mixture; and (3) loading the mixture into a sagger, sintering at 890 ℃ for 7.5 hours to obtain the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material.
Comparative example 1:
weighing stannic oxide, weighing NCM811 ternary material according to the mass ratio of stannic oxide accounting for 0.08% of the ternary material, and fully and uniformly mixing the NCM811 ternary material with stannic oxide to obtain a mixture; and (3) putting the mixture into a sagger, sintering at 650 ℃ for 6 hours to obtain the tin oxide coated lithium nickel cobalt manganese oxide cathode material.
Comparative example 2:
weighing tin dioxide, weighing an NCM523 ternary material according to the mass ratio that tin oxide accounts for 0.14% of the ternary material, and fully and uniformly mixing the NCM523 ternary material with the tin oxide to obtain a mixture; and (3) putting the mixture into a sagger, sintering at 890 ℃ for 7.5 hours to obtain the tin oxide coated lithium nickel cobalt manganese oxide cathode material.
The button cell is assembled by taking the positive electrode materials prepared in the experimental examples 1 and 2 and the comparative examples 1 and 2 as positive electrode active materials and taking a lithium sheet as a negative electrode. The composition of the positive electrode sheet is m (active material): m (acetylene black): and m (PVDF) is 80:12:8, a blue test system is adopted for testing, the charge-discharge voltage is 2.75-4.3V, and the cycle performance is tested in the normal temperature environment. The relationship between the number of charge/discharge cycles and the capacity is shown in fig. 1 and 2.
As can be seen from fig. 1, the capacity of the lithium battery prepared from the positive electrode material coated with tin oxide of comparative example 1 decreases rapidly around 70 cycles, while the capacity of the lithium battery prepared from the positive electrode material coated with NCM811 modified with niobium and manganese tends to decrease steadily after cycling to 100 cycles.
As can be seen from fig. 2, the capacity retention rate of the lithium battery prepared from the positive electrode material coated with tin oxide of comparative example 2 is about 98% at about 80 cycles, and the capacity retention rate of the lithium battery prepared from the positive electrode material coated with tin oxide modified with niobium and manganese is about 95.7% at 100 cycles, while the capacity retention rate of the lithium battery prepared from the positive electrode material coated with NCM523 coated with tin oxide modified with niobium and manganese is about 99.3% at 80 cycles, and the capacity retention rate of the lithium battery prepared from the.
Therefore, compared with the nickel cobalt lithium manganate cathode material coated with common tin oxide, the nickel cobalt lithium manganate cathode material coated with niobium-manganese modified tin oxide has the advantage that the cycle performance of the battery is obviously improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (4)

1. The preparation method of the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate cathode material is characterized by comprising the following steps of:
s1, weighing tin oxide and oxides of niobium and manganese, mixing and then carrying out low-temperature treatment to obtain a niobium-manganese-tin oxide mixture;
s2, weighing a nickel-cobalt-manganese ternary material according to a proportion, and fully and uniformly mixing the nickel-cobalt-manganese ternary material with the niobium-manganese tin oxide mixture to obtain a mixture;
step S3, loading the mixture obtained in the step S2 into a sagger, and sintering to obtain the niobium-manganese modified tin oxide coated nickel cobalt lithium manganate positive electrode material;
in the oxide of tin oxide and niobium manganese weighed in step S1, the molar ratio Sn of tin, niobium and manganese is: nb: mn =1 (0.1-0.3): (0.2-0.5), the low temperature treatment range is 200 ℃ and 500 ℃.
2. The method for preparing the lithium nickel cobalt manganese oxide coated positive electrode material of claim 1, wherein in step S2, the ternary nickel cobalt manganese material is weighed so that the mass ratio of the mixture of niobium manganese tin oxide to nickel cobalt manganese material is 0.05-0.4%.
3. The method for preparing the lithium nickel cobalt manganese oxide coated positive electrode material of claim 1, wherein in step S3, the sintering temperature in the sintering process is 600-1000 ℃, and the sintering time is 4-12 h.
4. The nickel cobalt lithium manganate positive electrode material coated with niobium manganese modified tin oxide is characterized by being prepared by the method of any one of claims 1 to 3, wherein a material matrix is a nickel cobalt manganese ternary material, and a material shell layer is a tin oxide-manganese-niobium composite coating layer.
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CN104810512A (en) * 2015-05-06 2015-07-29 中信国安盟固利电源技术有限公司 Coated and modified anode material and preparation method thereof
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CN106684325A (en) * 2017-01-10 2017-05-17 郑州大学 Niobium-doped tin dioxide thin film lithium ion battery negative pole plate, preparation method thereof and lithium ion battery

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CN102332585A (en) * 2011-10-20 2012-01-25 中国科学院过程工程研究所 Lithium nickel cobalt manganese oxygen/stannic oxide composite anode material doped with metal elements and method for preparing lithium nickel cobalt manganese oxygen/stannic oxide composite anode material
CN105449196A (en) * 2014-08-28 2016-03-30 宁德时代新能源科技股份有限公司 composite positive electrode active material and lithium ion secondary battery
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