Determination method of content of cobalt in lithium battery ternary positive electrode material

A technology of positive electrode material and determination method, which is applied in the field of determination of cobalt content in ternary positive electrode materials of lithium batteries, can solve the problems of cumbersome operation, positive interference in the determination result, easy to generate large errors, etc., to simplify steps and eliminate the need for Manganese reduction operation, the effect of improving accuracy

Inactive Publication Date: 2014-05-07
江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院)
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AI Technical Summary

Problems solved by technology

[0005] For the constant analysis of cobalt, the potentiometric titration method is widely used at present. The determination range of cobalt content is 5% to 25%. When the manganese content in the sample is less than 0.05%, the influence of the manganese content can be ignored. When it is greater than 0.05%, manganese (II) is also titrated while excessive potassium ferricyanide is used to oxidize cobalt. Manganese (II) is a positive interference to the measurement result. Other methods must be used to obtain the total manganese content, and then from the measured The total manganese content in the sample is deducted from the total cobalt content to obtain a single cobalt content. This method is not only cumbersome to operate, but also prone to large errors

Method used

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  • Determination method of content of cobalt in lithium battery ternary positive electrode material
  • Determination method of content of cobalt in lithium battery ternary positive electrode material
  • Determination method of content of cobalt in lithium battery ternary positive electrode material

Examples

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Effect test

Embodiment 1

[0038] The sample to be tested is LiNi 0.5 co 0.3 mn 0.2 o 2 Ternary positive electrode material, the weight content of the main influencing elements manganese is 11.32%, and the weight content of cobalt is 18.23%;

[0039] Take 1g of the sample to be tested in a beaker, add 15mL of hydrochloric acid and 5mL of nitric acid and heat until it is completely dissolved. After cooling, transfer it to a 250mL volumetric flask. Dilute to the mark with distilled water and shake well for testing; use a pipette to take 10mL of the above solution Add 5mL of phosphoric acid and 3mL of perchloric acid into the beaker, heat it on an electric furnace until a large amount of perchloric acid fumes are emitted, take it off for about half a minute, add 10mL of distilled water and 2g of sodium fluoride immediately after a little cooling, cool to room temperature for analysis ; Take a beaker and add 3-5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, add the treated l...

Embodiment 2

[0051] The sample to be tested is LiNi 0.4 co 0.2 mn 0.4 o 2 Ternary cathode material, the weight content of the main influencing elements manganese is 22.84%, and the weight content of cobalt is 12.25%;

[0052] Take 1g of the sample to be tested in a beaker, add 15mL of hydrochloric acid and 5mL of nitric acid and heat until it is completely dissolved. After cooling, transfer it to a 250mL volumetric flask. Dilute to the mark with distilled water and shake well for testing; use a pipette to take 10mL of the above solution Add 5mL of phosphoric acid and 3mL of perchloric acid into the beaker, heat it on an electric furnace until a large amount of perchloric acid fumes are emitted, take it off for about half a minute, add 10mL of distilled water and 2g of sodium fluoride immediately after a little cooling, cool to room temperature for analysis ; Take a beaker and add 3-5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, add the treated liquid to be teste...

Embodiment 3

[0064] The sample to be tested is Li 1.2 Ni 0.16 co 0.08 mn 0.56 o 2 Ternary positive electrode material, the weight content of the main influencing elements manganese is 36.1%, and the weight content of cobalt is 5.53%;

[0065] Take 1g of the sample to be tested in a beaker, add 15mL of hydrochloric acid and 5mL of nitric acid and heat until it is completely dissolved. After cooling, transfer it to a 250mL volumetric flask. Dilute to the mark with distilled water and shake well for testing; use a pipette to take 10mL of the above solution Add 5mL of phosphoric acid and 3mL of perchloric acid into the beaker, heat it on an electric furnace until a large amount of perchloric acid fumes are emitted, take it off for about half a minute, add 10mL of distilled water and 2g of sodium fluoride immediately after a little cooling, cool to room temperature for analysis Take a beaker and add 3~5g ammonium sulfate and 60mL ammonium citrate ammonia mixed solution, add the treated liqu...

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Abstract

The invention provides a determination method of the content of cobalt in a lithium battery ternary positive electrode material, relates to a determination method of the content of cobalt in material with high manganese content, and in particular relates to a determination method of the content of cobalt in the lithium battery ternary positive electrode material. The method comprises the following steps: (1) accurately weighing moderate to-be-determined ternary positive electrode material, adding acid to dissolve and making up to volume; (2) adding perchloric acid-phosphoric acid to a certain amount of dissolved solution, heating till perchloric acid smoke emits, and adding a moderate masking agent to eliminate manganese interference; (3) performing back-titration on a potentiometric titrator by using a cobalt standard solution, drawing a differential curve and obtaining titration end point consumed volume according to a second-order differential method; and (4) computing to obtain the cobalt content in a sample according to a formula. According to the method provided by the invention, the manganese reducing operation is unnecessary, and the determination of the content of the cobalt in the sample containing manganese with the weight percent being not more than 40% cannot be influenced, the accuracy is high, the treatment process is simple and the method is easy to popularize.

Description

technical field [0001] The invention relates to a method for measuring cobalt content in materials with relatively high manganese content, in particular to a method for measuring cobalt content in lithium battery ternary positive electrode materials. Background technique [0002] With the increasing demand for energy saving and environmental protection in recent years, the application of lithium batteries has become more and more extensive. As the core material of lithium battery cathode materials, the development prospect of this industry is very good. At present, nickel-cobalt-manganese ternary cathode materials with layered stacking structure are rapidly being researched and utilized by people because of their high specific capacity, excellent cycle performance, good thermal stability and low price. High-performance lithium-ion battery cathode materials. [0003] In the preparation process of lithium-ion ternary cathode materials, the content ratio of nickel, cobalt and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 姚文俐郑攀
Owner 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院)
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