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Method for preparing gradient niobium-tungsten-tantalum-doped cobaltosic oxide

A technology of cobalt tetroxide and niobium tungsten is applied in the field of lithium ion batteries, which can solve the problems of uneven distribution of doping elements, uneven precipitation, and easy hydrolysis.

Inactive Publication Date: 2018-11-13
LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when this method is used to prepare lithium doped with high-valence and large atomic weight elements niobium, tungsten, and tantalum cobaltate, there is a problem that niobium, tungsten, and tantalum chlorides are easily hydrolyzed as wet dopants, resulting in the formation of niobium, tungsten, and tantalum elements. Inhomogeneous precipitation with cobalt, resulting in uneven distribution of doping elements in cobalt tetroxide

Method used

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  • Method for preparing gradient niobium-tungsten-tantalum-doped cobaltosic oxide

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Experimental program
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Effect test

Embodiment 1

[0026] Prepare a cobalt chloride solution with a concentration of 1mol / L as solution A, and accurately measure 4500L for use; prepare a sodium hydroxide solution with a concentration of 2mol / L, add 0.05 times the volume of ammonia solution with a concentration of 180g / L as solution B ; The hydrogen peroxide solution with a concentration of 5mol / L is prepared as the C solution; the niobium pentachloride absolute ethanol solution with a concentration of 4g / L is prepared as the D solution, according to the formula: D solution volume = (xx × A solution concentration × preparation product requirements niobium doping amount) / (concentration of D solution × percentage of cobalt in cobalt tetroxide), the calculated volume of required D solution is 450L, and accurately measure 450L of absolute ethanol for use;

[0027] When the synthesis reaction starts, determine that the synthesis time is 15 hours, add the D solution to the spare absolute ethanol at a flow rate of 30L / h to be the E sol...

Embodiment 2

[0030] Prepare a cobalt sulfate solution with a concentration of 1.5 mol / L as solution A, and accurately measure 5400 L for use; prepare a sodium hydroxide solution with a concentration of 4 mol / L, add 0.08 times the volume of ammonia solution with a concentration of 180 g / L as solution B ; Prepare a hydrogen peroxide solution with a concentration of 8mol / L as the C solution; prepare a tungsten hexachloride absolute ethanol solution with a concentration of 6g / L as the D solution, according to the formula: D solution volume = (xx × A solution concentration × preparation product requirements Doped tungsten amount) / (concentration of D solution × percentage of cobalt in cobalt tetroxide), the calculated volume of required D solution is 540L, and accurately measure 540L of absolute ethanol for use;

[0031] When the synthesis reaction starts, determine that the synthesis time is 18 hours, add the D solution to the spare absolute ethanol at a flow rate of 30L / h to form the E solution...

Embodiment 3

[0034] Prepare a cobalt nitrate solution with a concentration of 2mol / L as the A solution, and accurately measure 6000L for subsequent use; prepare a sodium hydroxide solution with a concentration of 6mol / L, add 0.1 times the volume and a concentration of 180g / L ammonia solution to be the B solution; Prepare hydrogen peroxide solution with a concentration of 10mol / L as solution C; prepare tantalum pentachloride absolute ethanol solution with a concentration of 8g / L as solution D. Quantity of tantalum) / (concentration of D solution × percentage of cobalt in cobalt tetroxide), the calculated volume of required D solution is 600L, and accurately measure 600L of absolute ethanol for use;

[0035] When the synthesis reaction starts, determine that the synthesis time is 20h, add the D solution to the spare absolute ethanol at a flow rate of 30L / h to form the E solution, and simultaneously add the A solution at a flow rate of 300L / h, the B solution and the C solution In the reaction k...

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Abstract

The invention discloses a method for preparing gradient niobium-tungsten-tantalum-doped cobaltosic oxide and belongs to the technical field of lithium ion batteries. The method comprises the followingstep: by taking a cobalt solution of a certain solution as a cobalt source, a sodium hydroxide solution as a precipitant, an ammonia water solution as a complexing agent, a hydrogen peroxide solutionas an oxidant, and a niobium-tungsten-tantalum chloride absolute ethyl alcohol solution as a doping solution, putting the doping solution into a reaction kettle to be subjected to reactions in a dispersion liquid addition mode in a reaction process, thereby obtaining a gradient niobium-tungsten-tantalum-doped cobaltosic oxide product. By adopting the method that the niobium-tungsten-tantalum chloride is dissolved into absolute ethyl alcohol to be used as the doping agent solution, the problems that the niobium-tungsten-tantalum chloride is liable to hydrolyze can be well solved, and uniform gradient distribution of niobium-tungsten-tantalum elements in a prepared product can be ensured. The doped cobaltosic oxide product prepared by using the method disclosed by the invention has a dopingamount of 0.5-1.0%, has doping elements in uniform gradient distribution, has laser granularity of 5-8mu m, a tap density greater than or equal to 2.5g / cm<3>, a specific surface area of 1.0-3.0m<2> / g, and has a blocky or sphere-like morphology.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a preparation method for gradiently doped niobium tungsten tantalum tricobalt tetroxide used for preparing lithium cobalt oxide, a cathode material of lithium ion batteries. Background technique [0002] Lithium cobalt oxide is currently the main cathode material in commercial lithium-ion batteries. However, the actual specific capacity of lithium cobalt oxide is only about 140mAh / g, which is only about 50% of its theoretical capacity (274mAh / g); and the anti-overcharge performance of lithium cobalt oxide is poor, and the specific capacity decreases rapidly at a higher charging voltage . Studies have proved that doping is one of the most effective methods to improve the performance of lithium-ion battery cathode materials, especially the cycle performance. It can not only improve the stability of the ion lattice, but also greatly improve the cycle performance of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/525H01M10/0525
CPCH01M4/362H01M4/525H01M10/0525Y02E60/10
Inventor 曹笃盟陈晓闯王红忠刘世红吴来红赵宗明李俊杰杜江赵亮何艳
Owner LANZHOU JINCHUAN NEW MATERIAL SCI & TECH
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