CN116314745A - Modified high-nickel ternary positive electrode material, preparation method and application - Google Patents

Modified high-nickel ternary positive electrode material, preparation method and application Download PDF

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CN116314745A
CN116314745A CN202310021526.7A CN202310021526A CN116314745A CN 116314745 A CN116314745 A CN 116314745A CN 202310021526 A CN202310021526 A CN 202310021526A CN 116314745 A CN116314745 A CN 116314745A
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positive electrode
electrode material
nickel ternary
modified high
cathode material
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孔凡军
余洋
张清刚
相江峰
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Far East Battery Jiangsu 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
    • H01M4/48—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
    • 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 discloses a modified high-nickel ternary positive electrode material, a preparation method and application thereof, and belongs to the technical field of positive electrode materials. The preparation method comprises the steps of uniformly mixing a ternary precursor and a lithium source, placing the mixture in a crucible for calcination, and uniformly grinding a product to obtain a positive electrode material; adding the positive electrode material into a solution containing a tellurium source, and performing ultrasonic dispersion to obtain a positive electrode material solution; adding a reducing agent, uniformly stirring, performing hydrothermal reaction, and after the reaction is finished, performing centrifugal filtration, crushing and grinding, drying treatment and calcination on a reaction product to obtain the modified high-nickel ternary anode material. According to the invention, tellurium is coated on the surface of the positive electrode material in the preparation process, so that a disperse phase is formed on the surface of the positive electrode material, the electronic conductivity and the ion diffusion rate can be improved, and the safety of the battery can be improved. Meanwhile, the invention adopts liquid phase telluride and high temperature calcination methods, and has good safety and simple operability.

Description

Modified high-nickel ternary positive electrode material, preparation method and application
Technical Field
The invention relates to the technical field related to cathode materials, in particular to a modified high-nickel ternary cathode material, a preparation method and application thereof.
Background
The high-nickel ternary cathode material is an important choice of the cathode material of the high-energy-density battery due to lower cost and higher theoretical specific capacity. However, as the Ni content increases, the cycle performance and safety of the battery also decrease. Ni (Ni) 2+ /Li + The mixed arrangement can cause the irreversibility of the structure of the high-nickel ternary positive electrode material, and the diffusion difficulty of lithium ions is increased. The surface of the high-nickel ternary positive electrode material is easy to be combined with H 2 O reacts to produce LiOH, which reacts with LiPF 6 The reaction produces HF, resulting in dissolution of the transition metal ions. Meanwhile, the high-nickel ternary anode material also has lattice oxygen evolution defect, so that the safety of the battery is reduced. To solve these problems, researchers often use cladding and doping methods to improve the high nickel ternary LiNi 1-x-y Co x Mn y O 2 (1-x-y is more than or equal to 0.6) the cycling stability and safety of the positive electrode material.
The surface coating can effectively improve the electronic and ionic conductivity of the anode material, quicken charge transfer, reduce phase change stress, prevent electrolyte corrosion and reduce the dissolution of transition metal ions. The doping strategy can improve the electron conductivity and ion diffusion coefficient of the electrode material, inhibit the precipitation of lattice oxygen under high voltage and enhance the stability of the structure. The anion coating or doping can achieve improved performance without decreasing the capacity of the active material. Tellurium has better metallic properties than sulfur and selenium, and can improve the electrochemical properties of the electrode material by coating or doping, but solid phase mixing can result in a portion of the particles not being uniformly coated or doped. It is a difficulty how to achieve uniform cladding or doping of Te elements. Therefore, it is necessary to develop a technique that is relatively safe and easy, and that can achieve both surface cladding and bulk doping.
Disclosure of Invention
In order to solve the existing technical problems. The invention provides a modified high-nickel ternary anode material, a preparation method and application thereof, wherein the preparation method comprises the following steps:
a. uniformly mixing the ternary precursor and a lithium source, placing the mixture in a crucible for calcination, and uniformly grinding the product to obtain a positive electrode material;
b. adding the positive electrode material into a solution containing a tellurium source, and performing ultrasonic dispersion to obtain a positive electrode material solution;
c. adding a reducing agent into the positive electrode material solution under stirring, uniformly stirring, performing hydrothermal reaction on the positive electrode material solution added with the reducing agent, and performing centrifugal filtration, crushing and grinding and drying treatment on a reaction product after the reaction is finished to obtain solid powder.
d. And calcining the solid powder to obtain the modified high-nickel ternary anode material.
Preferably or alternatively, the ternary precursor has the chemical formula Ni 1-x-y Co x Mn y CO 3 The lithium source is LiOH.H 2 O; the molar ratio of the ternary precursor to the lithium source is 0.9-1.1; the chemical formula of the positive electrode material is LiNi 1-x- y Co x Mn y O 2 。
Preferably or alternatively, in the step a, the calcining process is specifically: heating to 400-500 ℃ at the speed of 3-7 ℃/min, preserving heat for 3-12 h, heating to 700-800 ℃ at the speed of 3-7 ℃/min, and preserving heat for 5-25 h.
Preferably or alternatively, in the step b, the tellurium source is one or more of tellurium dioxide, telluric acid, tellurite or tellurite.
Preferably or alternatively, the molar amount of the tellurium source is 0.05 to 0.2mmol.
Preferably or alternatively, in the step c, the reducing agent is one or more of hydrazine hydrate, ascorbic acid and sodium borohydride.
Preferably or alternatively, in the step c, the hydrothermal reaction temperature is 140-200 ℃ and the reaction time is 6-18 h.
Preferably or alternatively, in the step d, the calcination temperature is 300-500 ℃ and the heat preservation time is 2-6 h.
The chemical formula of the modified high-nickel ternary positive electrode material prepared based on the preparation method of the modified high-nickel ternary positive electrode material is as follows: liNi 1-x-y Co x Mn y O 2 Wherein 0 is<x<0.4，0<y<0.4,1-x-y is more than or equal to 0.6, and the modified high-nickel ternary positive electrode material is applied as an electrode of a lithium ion battery.
The beneficial effects are that: the invention provides a modified high-nickel ternary cathode material, a preparation method and application thereof, wherein tellurium is coated on the surface of the cathode material in the preparation process, a disperse phase is formed on the surface of the cathode material, a stable physical-chemical interface is constructed, the dissolution of transition metal ions is reduced, the internal stress and volume change of a structure are relieved, and the cycle performance of an electrode is improved. And the doped tellurium can form Te-metal bond with transition metal ions, thereby effectively inhibiting the precipitation of lattice oxygen and the formation of microcracks in particles, improving the electronic conductivity and the diffusion rate of ions and improving the safety of the battery. Meanwhile, the invention adopts liquid phase telluride and high temperature calcination methods, can realize uniform coating and doping of particles, has simple process and good safety and simple operability.
Drawings
Fig. 1 is an SEM image of the high nickel ternary cathode material prepared in example 1.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the invention may be practiced without one or more of these details. In other instances, well-known features have not been described in detail in order to avoid obscuring the invention.
The invention is further illustrated below in conjunction with examples, examples of which are intended to illustrate the invention and are not to be construed as limiting the invention. The specific techniques and reaction conditions not specified in the examples may be carried out according to the techniques or conditions described in the literature in this field or the product specifications. Reagents, instruments or equipment not specifically mentioned in the manufacturer are commercially available.
Example 1
0.1mmol tellurium dioxide was dissolved in 70ml deionized water, then added1g high nickel ternary LiNi 1-x-y Co x Mn y O 2 And (5) carrying out ultrasonic dispersion on the positive electrode material for 30min. 10ml of hydrazine hydrate (concentration: 50%) was added to the solution under continuous magnetic stirring, stirred for 30min, transferred to a 100ml reaction vessel, subjected to hydrothermal reaction in a forced air drying oven, and incubated at 180℃for 12h. After the reaction is finished, the solid-liquid mixture is centrifugally filtered, dried for 24 hours at 80 ℃ in vacuum, and calcined for 4 hours in a 400 ℃ nitrogen atmosphere tube furnace, so that the tellurium-coated and doped high-nickel ternary positive electrode material is obtained, and the morphology of the tellurium-coated and doped high-nickel ternary positive electrode material is shown in figure 1.
Example 2
Weigh 5mmol Ni 1-x-y Co x Mn y CO 3 Mixing and grinding the ternary precursor (1-x-y is more than or equal to 0.6) and 5.25mmol of lithium hydroxide monohydrate uniformly, heating to 450 ℃ at the speed of 5 ℃/min in an oxygen atmosphere tube furnace, preserving heat for 7h, and heating to 750 ℃ at the speed of 5 ℃/min again, and preserving heat for 15h. After the calcination is finished, the product is uniformly ground to obtain the high-nickel ternary LiNi 1-x- y Co x Mn y O 2 (1-x-y is more than or equal to 0.6).
Example 3
0.05mmol tellurium dioxide was dissolved in 70ml deionized water, followed by 1g high nickel ternary LiNi 1-x-y Co x Mn y O 2 And (5) carrying out ultrasonic dispersion on the positive electrode material for 30min. 10ml of hydrazine hydrate (concentration: 50%) was added to the solution under continuous magnetic stirring, stirred for 30min, transferred to a 100ml reaction vessel, subjected to hydrothermal reaction in a forced air drying oven, and incubated at 180℃for 12h. And after the reaction is finished, carrying out centrifugal filtration and vacuum drying at 80 ℃ for 24 hours on the solid-liquid mixture, and calcining for 4 hours in a 400 ℃ nitrogen atmosphere tube furnace to obtain the tellurium-coated and doped high-nickel ternary cathode material.
Example 4
0.2mmol tellurium dioxide was dissolved in 70ml deionized water, then 1g high nickel ternary LiNi was added 1-x-y Co x Mn y O 2 And (5) carrying out ultrasonic dispersion on the positive electrode material for 30min. 10ml of hydrazine hydrate (concentration 50%) is added into the solution under continuous magnetic stirring, the solution is transferred into a 100ml reaction kettle after stirring for 30min, and the hydrothermal reaction is carried out in a blast drying boxPreserving heat for 12h at 180 ℃. And after the reaction is finished, carrying out centrifugal filtration and vacuum drying at 80 ℃ for 24 hours on the solid-liquid mixture, and calcining for 4 hours in a 400 ℃ nitrogen atmosphere tube furnace to obtain the tellurium-coated and doped high-nickel ternary cathode material.
Example 5
0.1mmol tellurium dioxide was dissolved in 70ml deionized water, followed by 1g high nickel ternary LiNi 1-x-y Co x Mn y O 2 And (5) carrying out ultrasonic dispersion on the positive electrode material for 30min. 10ml of hydrazine hydrate (concentration: 50%) was added to the solution under continuous magnetic stirring, stirred for 30min, transferred to a 100ml reaction vessel, subjected to hydrothermal reaction in a forced air drying oven, and incubated at 180℃for 12h. And after the reaction is finished, carrying out centrifugal filtration and vacuum drying at 80 ℃ for 24 hours on the solid-liquid mixture, and calcining for 4 hours in a 300 ℃ nitrogen atmosphere tube furnace to obtain the tellurium-coated and doped high-nickel ternary cathode material.
Example 6
0.1mmol tellurium dioxide was dissolved in 70ml deionized water, followed by 1g high nickel ternary LiNi 1-x-y Co x Mn y O 2 And (5) carrying out ultrasonic dispersion on the positive electrode material for 30min. 10ml of hydrazine hydrate (concentration: 50%) was added to the solution under continuous magnetic stirring, stirred for 30min, transferred to a 100ml reaction vessel, subjected to hydrothermal reaction in a forced air drying oven, and incubated at 180℃for 12h. And after the reaction is finished, carrying out centrifugal filtration and vacuum drying at 80 ℃ for 24 hours on the solid-liquid mixture, and calcining for 4 hours in a 500 ℃ nitrogen atmosphere tube furnace to obtain the tellurium-coated and doped high-nickel ternary cathode material.
Comparative example 1
0.1mmol tellurium dioxide was dissolved in 70ml deionized water, followed by 1g high nickel ternary LiNi 1-x-y Co x Mn y O 2 And (5) carrying out ultrasonic dispersion on the positive electrode material for 30min. 10ml of hydrazine hydrate (concentration: 50%) was added to the solution under continuous magnetic stirring, stirred for 30min, transferred to a 100ml reaction vessel, subjected to hydrothermal reaction in a forced air drying oven, and incubated at 180℃for 12h. And after the reaction is finished, centrifugally filtering the solid-liquid mixture, and vacuum drying at 80 ℃ for 24 hours to obtain the tellurium-coated high-nickel ternary anode material.
Performance testing
The active substances prepared in each example and comparative example, polyvinylidene fluoride and acetylene black are mixed according to the mass ratio of 8:1:1, N-methyl-2-pyrrolidone solution is added, the mixture is coated on aluminum foil after electric stirring, the mixture is dried for 12 hours in a vacuum oven at 90 ℃, and a round electrode plate with the diameter of 11mm is punched. The metal lithium sheet is used as a counter electrode, celgard2500 is used as a diaphragm, and the electrolyte is 1mol/LiPF 6 EC (ethylene carbonate)/DMC (dimethyl carbonate)/EMC (methyl ethyl carbonate) (EC to DMC to EMC volume ratio 1:1:1), nickel foam was used as a filler and CR2016 coin cell was assembled in an argon filled glove box. After the battery is kept stand for 12 hours, the circulation performance test is carried out with the current density of 50mA/g and the cut-off voltage of 2.7-4.3V. The test results are shown in the following table.
Figure BDA0004042517050000041
As can be seen from the above table in combination with FIG. 1, with pure high nickel ternary LiNi 1-x-y Co x Mn y O 2 Compared with the positive electrode material (example 2), the particle surface of the positive electrode material of example 1 is smoother, and the tellurium cladding doping shows the best cycle stability and the highest cycle capacity, so that the tellurium cladding and the doping can effectively improve the lithium storage capacity of the high-nickel ternary positive electrode material. Comparative examples 3 and 4 show that the tellurium coating and doping amounts have a suitable ratio, too little or too much to achieve the optimal modification effect. Comparative examples 5 and 6 show that the calcination temperature also has a certain effect on the cycle performance of the high nickel ternary cathode material. Too low a temperature, tellurium cannot effectively replace the oxygen sites, while too high a temperature results in a decrease in the surface-coated tellurium due to dissolution (the melting point of tellurium is 452 ℃). Comparing example 1, example 2 and comparative example 1, it is demonstrated that tellurium cladding and tellurium doping both play an important role in improving the cycle performance of the high nickel ternary cathode material.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.

Claims (10)

1. The preparation method of the modified high-nickel ternary cathode material is characterized by comprising the following steps of:
a. uniformly mixing the ternary precursor and a lithium source, placing the mixture in a crucible for calcination, and uniformly grinding the product to obtain a positive electrode material;
b. adding the positive electrode material into a solution containing a tellurium source, and performing ultrasonic dispersion to obtain a positive electrode material solution;
c. adding a reducing agent into the positive electrode material solution under stirring, uniformly stirring, performing hydrothermal reaction on the positive electrode material solution added with the reducing agent, and performing centrifugal filtration, crushing and grinding and drying treatment on a reaction product after the reaction is finished to obtain solid powder.
d. And calcining the solid powder to obtain the modified high-nickel ternary anode material.
2. The method for preparing a modified high-nickel ternary positive electrode material according to claim 1, wherein the ternary precursor has a chemical formula of Ni 1-x-y Co x Mn y CO 3 The lithium source is LiOH.H 2 O; the molar ratio of the ternary precursor to the lithium source is 0.9-1.1; the chemical formula of the positive electrode material is LiNi 1-x-y Co x Mn y O 2 。
3. The method for preparing a modified high-nickel ternary cathode material according to claim 1, wherein in the step a, the calcining process specifically comprises: heating to 400-500 ℃ at the speed of 3-7 ℃/min, preserving heat for 3-12 h, heating to 700-800 ℃ at the speed of 3-7 ℃/min, and preserving heat for 5-25 h.
4. The method for preparing a modified high nickel ternary cathode material according to claim 1, wherein in the step b, the tellurium source is one or more of tellurium dioxide, telluric acid, tellurite, hydrogen tellurite or hydrogen tellurite.
5. The method for producing a modified high-nickel ternary cathode material according to claim 4, wherein the molar amount of the tellurium source is 0.05 to 0.2mmol.
6. The method for preparing the modified high-nickel ternary cathode material according to claim 1, wherein in the step c, the reducing agent is one or more of hydrazine hydrate, ascorbic acid and sodium borohydride.
7. The method for preparing the modified high-nickel ternary cathode material according to claim 1, wherein in the step c, the hydrothermal reaction temperature is 140-200 ℃ and the reaction time is 6-18 h.
8. The method for preparing a modified high-nickel ternary cathode material according to claim 1, wherein in the step d, the calcining temperature is 300-500 ℃ and the heat preservation time is 2-6 h.
9. A modified high-nickel ternary cathode material prepared based on the preparation method of the modified high-nickel ternary cathode material according to any one of claims 1 to 8, wherein the modified high-nickel ternary cathode material has a chemical formula: liNi 1-x- y Co x Mn y O 2 Wherein 0 is<x<0.4，0<y<0.4，1-x-y≥0.6。
10. The use of the high nickel ternary cathode material according to claim 9 as an electrode for a lithium ion battery.
CN202310021526.7A 2023-01-07 2023-01-07 Modified high-nickel ternary positive electrode material, preparation method and application Pending CN116314745A (en)

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