CN111994967A - Preparation method of titanium-doped high-nickel ternary lithium ion positive electrode material - Google Patents

Preparation method of titanium-doped high-nickel ternary lithium ion positive electrode material Download PDF

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CN111994967A
CN111994967A CN202010871897.0A CN202010871897A CN111994967A CN 111994967 A CN111994967 A CN 111994967A CN 202010871897 A CN202010871897 A CN 202010871897A CN 111994967 A CN111994967 A CN 111994967A
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王刚
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Hainan Shanghe Chaodian New Energy Technology Co ltd
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Abstract

The invention relates to a method for preparing a high-nickel ternary lithium ion battery anode material and modifying titanium element doping. The preparation method comprises the following steps: titrating the metal salt solution A and the precipitator B into the complexing agent C to prepare a ternary precursor; carrying out primary sintering after high-pressure stirring to obtain a high-nickel ternary cathode material; and preparing a titanium source material into sol, adding a high-nickel ternary material for doping, and then performing secondary sintering to obtain the titanium-doped high-nickel ternary material. The preparation method of the titanium-doped high-nickel ternary lithium ion cathode material provided by the invention has the advantages that the lattice stability of the material is improved, the delinquent efficiency and the transmission rate of lithium ions are improved, and the charge transfer and ion transport characteristics of the high-nickel ternary cathode material are improved. Thereby increasing the specific capacity of the material, improving the cycle performance of the material and being beneficial to industrial production.

Description

Preparation method of titanium-doped high-nickel ternary lithium ion positive electrode material
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a high-nickel ternary battery anode material and a Ti-doped coating preparation method.
Background
At present, lithium iron phosphate, lithium cobaltate, lithium manganate and ternary nickel cobalt manganese materials are the most commonly used lithium ion battery anode materials in the industry at present. With the development of portable electronic products and electric vehicles, higher requirements are put on the high-energy-density battery cathode material. The nickel-rich ternary material has higher energy density and lower raw material cost, and is considered to be an ideal anode material of the lithium ion battery suitable for industrialization at present.
Nickel-cobalt-manganese ternary positive electrode material LiNixCoyMn1-x-yO2The battery product with different characteristics can be obtained by adjusting the proportion of the three metal elements. The inherent defects and electrochemical performance decay mechanism of the nickel-rich cathode material per se reduce the stability of the material with the increase of Ni element, and the structural defects and unstable interface chemical characteristics deteriorate the electrochemical properties, thermodynamic stability and safety performance of the material, so that the cycle performance of the material is reduced, and the capacity decay is accelerated. The above material defects restrict the industrialization process. Therefore, the existing technology for preparing the high-nickel ternary material and coating improvement thereof needs to be further improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-nickel ternary lithium ion battery anode material and a doping modification preparation method thereof aiming at the technical defects of the material performance. The high-nickel ternary material with higher specific capacity and rate capability and the doped coating material with improved cycle characteristics are prepared by the following preparation method.
Weighing a certain amount of nickel acetate, cobalt acetate and manganese acetate according to the molar ratio x: y: z, dissolving in deionized water to prepare a metal salt solution A, and uniformly stirring for later use. Wherein x is more than or equal to 0.85 and less than or equal to 0.77, y is more than or equal to 0.07 and less than or equal to 0.12, and z is more than or equal to 0.07 and less than or equal to 0.12.
Dissolving lithium hydroxide in deionized water according to the proportion of M (Li) to M (Ni, Co, Mn) = a:1 to prepare a precipitator B. Wherein a is more than or equal to 5.5 and less than or equal to 6.5.
Preparing an ammonia water solution with the mass fraction of b% as a complexing agent C, placing the complexing agent C in a three-neck flask, uniformly stirring, placing the three-neck flask in a constant-temperature water bath kettle, keeping the temperature at 55 ℃, and continuously stirring at the speed of C revolutions per minute. Wherein b is more than or equal to 1 and less than or equal to 3, and c is more than or equal to 300 and less than or equal to 500.
And (3) titrating the metal salt solution A and the precipitator B into the complexing agent C simultaneously by using two burettes, and uniformly mixing, wherein the titration speeds are d ml/min respectively. Wherein d is more than or equal to 20 and less than or equal to 30. The pH of the solution was maintained at about 11 during the dropping.
After the titration is finished, the pH value of the solution is adjusted to be about 11, the opening of the three-neck flask is sealed, the solution is continuously stirred for e hours, the stirring speed is increased to f revolutions per minute, and then the solution is kept standing for 5 hours. Wherein e is more than or equal to 8 and less than or equal to 12, and f is more than or equal to 500 and less than or equal to 800.
The solution after standing was placed in an autoclave and kept at gMPa and h ℃ for 48 hours. Wherein g is more than or equal to 2 and less than or equal to 5, and h is more than or equal to 130 and less than or equal to 200.
And (3) carrying out suction filtration on the reaction liquid, drying for 12h, then sintering, carrying out heat preservation at i ℃ for 5h in a slow oxygen flow atmosphere, then heating to j ℃, carrying out heat preservation for 5h, and naturally cooling to room temperature, wherein the heating rate in the process is 5 ℃/min, so as to obtain the high-nickel ternary material sample. Wherein i is more than or equal to 450 and less than or equal to 570, and j is more than or equal to 730 and less than or equal to 900.
Weighing tetrabutyl titanate in a proportion of corresponding to the molar ratio k% of the high-nickel ternary material, slowly dissolving the tetrabutyl titanate in a certain amount of absolute ethyl alcohol at the dissolving temperature of m ℃, stirring at the stirring speed of 400 r/min, stirring for 2h, and then carrying out ultrasonic treatment for 20min to prepare titanic acid and titanium dioxide sol. Wherein k is more than or equal to 1 and less than or equal to 3, and m is more than or equal to 45 and less than or equal to 55.
Adding the high-nickel ternary material with a preset molar ratio into the sol, and finally forming the gel, wherein the stirring condition is n ℃, and the stirring speed is 700 revolutions per minute. Wherein n is more than or equal to 55 and less than or equal to 65.
And transferring the gel into an air atmosphere high-temperature furnace, preserving heat for o hours at 550 ℃, and then preserving heat for p hours at 850 ℃ to finally prepare the titanium dioxide coated high-nickel ternary material. Wherein o is more than or equal to 3 and less than or equal to 5, and p is more than or equal to 3 and less than or equal to 5.
The gain effect of the invention is as follows:
the invention synthesizes the high nickel ternary anode material LiNi by using a coprecipitation methodxCoyMnzO2(x is more than or equal to 0.85 and less than or equal to 0.77). And the titanium doping method is used for carrying out lattice modification on the high-nickel ternary positive electrode material, so that the lithium-nickel mixed-discharging degree is reduced, the lattice stability is improved, the lithium ion default efficiency and the transmission rate are improved, and the lithium ion default rate and the transmission rate are improvedCharge transfer and ion transport properties of high nickel ternary positive electrode materials.
The electrochemical performance of the nickel-rich ternary material is improved by a doping modification method, particularly in the aspects of cycle characteristics and capacity attenuation. For example, the specific capacity at 0.2C multiplying power is 198mAh/g, the charge-discharge capacity retention rate of 100 circles is 89%, and excellent cycle stability is shown.
The modified material obtained by modifying the high-nickel ternary cathode material by the titanium element doping method has better specific capacity and cycling stability, and the practical value of the ternary material is improved.
The method for preparing the modified titanium-coated high-nickel ternary cathode material has the advantages of simple process, low raw material price, low equipment requirement, easy process control and stable output, and can be beneficial to realizing large-scale mass production.
Drawings
FIG. 1 is a flow chart of a preparation process;
FIG. 2 is an XRD (X-ray diffraction) spectrum of a high-nickel ternary lithium ion battery anode material;
FIG. 3 is a diagram of the result of a cyclic charge-discharge test of a titanium-doped high-nickel ternary lithium ion battery positive electrode material at 0.2C.
Detailed Description
Example 1
Weighing a certain amount of nickel acetate, cobalt acetate and manganese acetate according to the molar ratio of 8.2:0.9:0.9, dissolving in deionized water to prepare a metal salt solution A, and uniformly stirring for later use.
Dissolving lithium hydroxide in deionized water according to the proportion of M (Li) to M (Ni, Co, Mn) =6:1 to prepare a precipitator B.
Preparing an ammonia water solution with the mass fraction of 3% as a complexing agent C, placing the complexing agent C into a three-neck flask, uniformly stirring, placing the three-neck flask into a constant-temperature water bath kettle, keeping the temperature at 55 ℃, and continuously stirring at the speed of 400 revolutions per minute.
And (3) titrating the metal salt solution A and the precipitator B into the complexing agent C simultaneously by using two burettes, and uniformly mixing at the titration speeds of 25 ml/min respectively. The pH of the solution was maintained at about 11 during the dropping.
After the titration is finished, the pH value of the solution is adjusted to be about 11, the opening of the three-neck flask is sealed, the solution is continuously stirred for 10 hours, the stirring speed is increased to 800 r/min, and then the solution is kept standing for 5 hours.
The solution after standing was placed in an autoclave and kept at 2MPa and 180 ℃ for 48 hours.
And (3) carrying out suction filtration on the reaction liquid, drying for 12h, then sintering, carrying out heat preservation for 5h at 500 ℃ in a slow oxygen flow atmosphere, then heating to 800 ℃, carrying out heat preservation for 5h, and naturally cooling to room temperature, wherein the heating rate in the process is 5 ℃/min, so as to obtain the high-nickel ternary material sample.
Weighing tetrabutyl titanate with a proportion of 3 percent of the molar ratio corresponding to the high-nickel ternary material, slowly dissolving the tetrabutyl titanate in a certain amount of absolute ethyl alcohol at the dissolving temperature of 50 ℃ and the stirring speed of 400 r/min, stirring for 2h, and then carrying out ultrasonic treatment for 20min to prepare titanic acid and titanium dioxide sol.
Adding the high-nickel ternary material with a preset molar ratio into the sol, and stirring at the temperature of 58 ℃ and the stirring speed of 700 revolutions per minute to finally form the gel.
And transferring the gel into an air atmosphere high-temperature furnace, preserving heat for 5 hours at 550 ℃, and then preserving heat for 5 hours at 850 ℃ to finally prepare the titanium dioxide coated high-nickel ternary material.
Example 2
Weighing a certain amount of nickel acetate, cobalt acetate and manganese acetate according to the molar ratio of 8.4:0.8:0.8, dissolving in deionized water to prepare a metal salt solution A, and uniformly stirring for later use.
Dissolving lithium hydroxide in deionized water according to the proportion of M (Li) to M (Ni, Co, Mn) =6.5:1 to prepare a precipitator B.
Preparing an ammonia water solution with the mass fraction of 2% as a complexing agent C, placing the complexing agent C into a three-neck flask, uniformly stirring, placing the three-neck flask into a constant-temperature water bath kettle, keeping the temperature at 55 ℃, and continuously stirring at the speed of 300 revolutions per minute.
And (3) titrating the metal salt solution A and the precipitator B into the complexing agent C simultaneously by using two burettes, and uniformly mixing at the titration speeds of 30 ml/min respectively. The pH of the solution was maintained at about 11 during the dropping.
After the titration is finished, the pH value of the solution is adjusted to be about 11, the opening of the three-neck flask is sealed, the solution is continuously stirred for 12 hours, the stirring speed is increased to 600 revolutions per minute, and then the solution is kept standing for 5 hours.
The solution after standing was placed in an autoclave and kept at 2.8MPa and 175 ℃ for 48 hours.
And (3) carrying out suction filtration on the reaction liquid, drying for 12h, then sintering, carrying out heat preservation for 5h at 580 ℃ in a slow oxygen flow atmosphere, then heating to 880 ℃, carrying out heat preservation for 5h, and naturally cooling to room temperature, wherein the heating rate in the process is 5 ℃/min, so as to obtain the high-nickel ternary material sample.
Weighing tetrabutyl titanate with a d proportion of 2.8 percent of the molar ratio of the high-nickel ternary material, slowly dissolving the tetrabutyl titanate in a certain amount of absolute ethyl alcohol at the dissolving temperature of 55 ℃ and the stirring speed of 400 r/min, stirring for 2h, and then carrying out ultrasonic treatment for 20min to prepare titanic acid and titanium dioxide sol.
Adding the high-nickel ternary material with a preset molar ratio into the sol, and stirring at 65 ℃ and 700 rpm to finally form the gel.
And transferring the gel into an air atmosphere high-temperature furnace, preserving heat for 4 hours at 550 ℃, and then preserving heat for 4 hours at 850 ℃ to finally prepare the titanium dioxide coated high-nickel ternary material.
The above description is only an example of the invention, which is easy to operate, and is not intended to limit the invention in any way. Any modification, change or equivalent changes made to the above embodiments according to the technical method of the present invention belong to the protection scope of the technical solution of the present invention.

Claims (8)

1. A method for preparing a high-nickel ternary lithium ion battery anode material and doping and modifying a titanium element comprises the following steps: weighing a certain amount of nickel acetate, cobalt acetate and manganese acetate according to the molar ratio x, y and z, dissolving the weighed nickel acetate, cobalt acetate and manganese acetate in deionized water to prepare a metal salt solution A, and simultaneously dissolving lithium hydroxide in deionized water according to the ratio of M (Li) to M (Ni, Co and Mn) = a:1 to prepare a precipitator B; step two, preparing an ammonia water solution with the mass fraction of b% as a complexing agent C, placing the complexing agent C into a three-neck flask, uniformly stirring, placing the three-neck flask into a constant-temperature water bath kettle, keeping the temperature at 55 ℃, and continuously stirring at the speed of C revolutions per minute; step three, titrating the metal salt solution A and the precipitant B into the complexing agent C by using two burettes simultaneously, mixing uniformly, wherein the titration speeds are d ml/min respectively, the PH value of the solution is maintained at about 11 during titration, after the titration is finished, the PH value of the solution is adjusted to about 11, sealing the opening of the three-neck flask, continuously stirring the solution for e hours, increasing the stirring speed to f revolutions per minute, and then standing for 5 hours; step four, placing the solution after standing in a high-pressure kettle, and keeping for 48 hours under the conditions of gMpa and h ℃; carrying out suction filtration on the reaction liquid, drying for 12h, then sintering, carrying out heat preservation at i ℃ for 5h in a slow oxygen flow atmosphere, then heating to j ℃, carrying out heat preservation for 5h, and naturally cooling to room temperature, wherein the heating rate in the process is 5 ℃/min, so as to obtain a high-nickel ternary material sample; step five, measuring tetrabutyl titanate with a proportion corresponding to the molar ratio k% of the high-nickel ternary material, slowly dissolving the tetrabutyl titanate in a certain amount of absolute ethyl alcohol at the dissolving temperature of m ℃, stirring at the stirring speed of 400 r/min, stirring for 2h, and then carrying out ultrasonic treatment for 20min to prepare titanic acid and titanium dioxide sol; step six, adding the high-nickel ternary material with a preset molar ratio into the sol, and finally forming gel, wherein the stirring condition is n ℃, and the stirring speed is 700 revolutions per minute; and seventhly, transferring the gel into an air atmosphere high-temperature furnace, preserving heat for o hours at 550 ℃, and then preserving heat for p hours at 850 ℃ to finally prepare the titanium dioxide coated high-nickel ternary material.
2. The method for preparing the high-nickel ternary lithium ion battery positive electrode material and doping and modifying the titanium element according to claim 1, wherein x is more than or equal to 0.85 and less than or equal to 0.77, y is more than or equal to 0.07 and less than or equal to 0.12, z is more than or equal to 0.07 and less than or equal to 0.12, and a is more than or equal to 5.5 and less than or equal to 6.5 in the first step.
3. The method for preparing the high-nickel ternary lithium ion battery anode material and doping and modifying the titanium element according to claim 1 is characterized in that in the second step, b is more than or equal to 1 and less than or equal to 3, and c is more than or equal to 300 and less than or equal to 500.
4. The method for preparing the high-nickel ternary lithium ion battery anode material and doping and modifying the titanium element according to claim 1 is characterized in that d is more than or equal to 20 and less than or equal to 30, e is more than or equal to 8 and less than or equal to 12, and f is more than or equal to 500 and less than or equal to 800 in the third step.
5. The method for preparing the high-nickel ternary lithium ion battery cathode material and doping and modifying the titanium element according to claim 1 is characterized in that in the fourth step, g is more than or equal to 2 and less than or equal to 5, h is more than or equal to 130 and less than or equal to 200, i is more than or equal to 450 and less than or equal to 570, and j is more than or equal to 730 and less than or equal to 900.
6. The method for preparing the high-nickel ternary lithium ion battery anode material and doping and modifying the titanium element according to claim 1 is characterized in that in the fifth step, k is more than or equal to 1 and less than or equal to 3, and m is more than or equal to 45 and less than or equal to 55.
7. The method for preparing the high-nickel ternary lithium ion battery positive electrode material and doping and modifying the titanium element according to claim 1 is characterized in that n is more than or equal to 55 and less than or equal to 65 in the sixth step.
8. The method for preparing the high-nickel ternary lithium ion battery cathode material and doping and modifying the titanium element according to claim 1 is characterized in that in the seventh step, o is more than or equal to 3 and less than or equal to 5, and p is more than or equal to 3 and less than or equal to 5.
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Cited By (1)

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CN113130901A (en) * 2021-03-05 2021-07-16 广东省科学院稀有金属研究所 Titanium-doped high-nickel ternary lithium ion battery positive electrode material and preparation method thereof

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CN111477867A (en) * 2020-05-21 2020-07-31 苏州大学 Modification method of high-nickel ternary cathode material of lithium ion battery

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CN113130901A (en) * 2021-03-05 2021-07-16 广东省科学院稀有金属研究所 Titanium-doped high-nickel ternary lithium ion battery positive electrode material and preparation method thereof

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