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A method of detecting surface lithium of a ternary cathode material
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A positive electrode material and detection method technology, which is applied in the direction of chemical analysis by titration method, can solve the problems of large detection errors of lithium carbonate and lithium hydroxide, achieve the effects of short detection time, reduce errors, and improve accuracy
Inactive Publication Date: 2017-04-05
DO FLUORIDE NEW ENERGY TECHNOLOGY CO LTD
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[0005] The purpose of the present invention is to provide a method for detecting lithium on the surface of a ternary positive electrode material, thereby solving the problem that the detection error of lithium carbonate and lithium hydroxide is relatively large in existing detection methods
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Embodiment 1
[0028] The detection method of the lithium on the surface of the ternary positive electrode material of the present embodiment is to measure the lithium on the surface of the ternary positive electrode material of 622, comprising the following steps:
[0029] 1) Weigh 30g of sample into a 250ml beaker, add 100mL of deionized water, stir on a magnetic stirrer for 30min, then let it stand for 30min, vacuum filter with a 0.45μm microporous membrane, and the filtrate is the sample to be tested solution;
[0030] 2) Take 20mL of filtrate into a 100mL Erlenmeyer flask, place the Erlenmeyer flask on a magnetic stirrer, add two drops of phenolphthalein indicator first, the solution to be tested turns red, and then titrate with 0.1mol / L standard hydrochloric acid solution to Colorless, record the volume V of standard hydrochloric acid solution consumed 1 (mL), then add 5 drops of methyl red indicator, the system turns yellow, titrate to orange with standard hydrochloric acid solution,...
Embodiment 2
[0042] The detection method of the lithium on the surface of the ternary positive electrode material of the present embodiment is to measure the lithium on the surface of the ternary positive electrode material of 622, comprising the following steps:
[0043] 1) Weigh 30g of sample into a 250ml beaker, add 100mL of deionized water, place it on a magnetic stirrer and stir for 40min, then let it stand for 30min, vacuum filter with a 0.45μm microporous membrane, and the filtrate is the sample to be tested solution;
[0044] Step 2), step 3) are identical with embodiment 1.
Embodiment 3
[0046] The detection method of the lithium on the surface of the ternary positive electrode material of the present embodiment is to measure the lithium on the surface of the ternary positive electrode material of 622, comprising the following steps:
[0047] 1) Weigh 30g of sample into a 250ml beaker, add 100mL of deionized water, stir on a magnetic stirrer for 60min, then let it stand for 30min, vacuum filter with a 0.45μm microporous membrane, and the filtrate is the sample to be tested solution;
[0048] Step 2), step 3) are identical with embodiment 1.
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Abstract
The invention relates to a method of detecting surface lithium of a ternary cathode material. The method includes stirring and mixing a ternary cathode material sample and water, filtering the mixture to obtain filtrate that is a solution to be detected, adding a phenolphthalein indicator into the solution to be detected, titrating the mixture with a standard hydrochloric acid solution until the mixture is colorless, recording the volume V1 of the consumed standard hydrochloric acid solution, then adding a methyl red indicator into the mixture, titrating the system with a standard hydrochloric acid solution until the color is turned from yellow to orange, heating and boiling the system to allow the color to be turned back from the orange to yellow, cooling the system to room temperature, titrating the system with the standard hydrochloric acid solution until the system is reddish that is adopted as a terminal point, recording the volume V2 of the consumed standard hydrochloric acid solution in the whole titrating process, and calculating the surface lithium content of the ternary cathode material according to a formula (1). According to the method, the surface lithium content of the ternary cathode material is detected through selecting the indicators and through an acid-base titration process, influences of an intermediate that is LiHCO3 on titration data are taken into full consideration, the surface lithium content measuring error of the acid-base titration process is reduced and detection accuracy is improved.
Description
technical field [0001] The invention belongs to the detection field of positive electrode materials of lithium ion batteries, and in particular relates to a detection method for lithium on the surface of ternary positive electrode materials. Background technique [0002] The ternary positive electrode material (nickel-cobalt-manganese oxide) is prepared by sintering the precursors of lithium carbonate and nickel-cobalt-manganese oxide. In the actual production process, due to the impurity of lithium carbonate and the low melting point of lithium carbonate itself, resulting in At a lower temperature, part of the lithium carbonate is melted, decomposed and volatilized. Therefore, in the actual production of ingredients, the proportion of Li added will be slightly increased to compensate for the loss of lithium caused during the sintering process, resulting in residues on the surface of the ternary cathode material. A certain amount of lithium salts (mainly in the form of lithi...
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