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Fluorescence analysis method for measuring element content of lithium iron phosphate

A technology of lithium iron phosphate and fluorescence analysis, applied in measurement devices, analysis materials, material analysis using wave/particle radiation, etc., to achieve the effects of simple operation, reduced use, environmental pollution and environmental protection

Inactive Publication Date: 2016-08-10
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For now, there is no report on the rapid measurement of iron and phosphorus in lithium iron phosphate cathode materials in the lithium ion battery industry using XRF

Method used

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  • Fluorescence analysis method for measuring element content of lithium iron phosphate

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Embodiment 1

[0038] A fluorescence analysis method for determining the content of phosphorus and iron elements in lithium iron phosphate, comprising the following steps:

[0039] (1) Take the same batch of lithium iron phosphate samples and divide them into three equal parts;

[0040] (2) Add the first lithium iron phosphate sample to hydrochloric acid aqueous solution, heat to boil and keep for 18-25min, then cool to room temperature, and filter out unreacted carbon, and reduce the filtered solution with tin dichloride solution Ferric iron, then add CuSO 4 -Isatin indicator turns the light yellow solution into green, then add TiCl dropwise 3 After the green color of the solution disappears, add half a drop in excess, and the solution turns blue after standing; then add sulfuric acid / phosphoric acid mixed acid and sodium diphenylamine sulfonate indicator to form a solution to be tested; titrate it with potassium dichromate standard solution , when the solution changes from blue to purple...

Embodiment 2

[0046] 1. Potassium dichromate standard solution titration method to determine the content of iron in lithium iron phosphate samples:

[0047] Weigh 1.000g±0.005g (accurate to 0.0001g) lithium iron phosphate (sample 1), a positive electrode material in the lithium-ion battery industry, into a 100mL beaker, add (1+1) hydrochloric acid, and heat and boil on an electric heating furnace for 20 minutes Left and right, turn off the electric heating furnace, cool to room temperature, filter and set the volume to a 100mL volumetric flask for later use. Take 20mL of the above solution, add 30mL of water, 5mL (1+1) hydrochloric acid, put it on an electric heating furnace and heat to a slight boil, add 50g / L tin dichloride solution dropwise while it is hot until light yellow, add two drops of CuSO 4 -Isatin indicator turns green, add 20g / L TiCl dropwise 3 Solution until the green color disappears, half a drop in excess, and the solution turns blue when left to stand. Add 20mL of 15% s...

Embodiment 3-5

[0061] Select any batch of lithium iron phosphate samples, which are the positive electrode material of lithium-ion batteries, as samples 3-5, place them in molds such as aluminum rings with a diameter of 30mm, spread them evenly, press them with a little pressure, and then fill the entire mold with boric acid , after applying 20 tons of pressure on the tablet press for 5 seconds, it was pressed into a sheet, and the fluorescence intensity of iron and phosphorus in the sample to be tested was measured by X-ray fluorescence spectrometry, and the XRF standard curve was drawn using Example 2 and Determination of iron and phosphorus content.

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Abstract

The invention discloses a fluorescence analysis method for measuring element content of lithium iron phosphate. The method comprises the following steps: equally dividing a lithium iron phosphate sample into three parts; processing a first part of the lithium iron phosphate sample by the use of hydrochloric acid, filtering and carrying out standard solution titration with potassium dichromate, and measuring content of iron element; processing the second part of the lithium iron phosphate sample by the use of hydrochloric acid, filtering and measuring content of phosphorus element by an ammonium phosphomolybdate volumetric method; preparing six standard samples with different contents from the third part of the lithium iron phosphate sample; respectively compressing into flaky pieces, and measuring fluorescence intensity of iron and phosphorus elements in each flaky standard sample by X-ray fluorescence spectrometry; drawing an XRF standard curve; compressing the lithium iron phosphate sample to be measured into flaky pieces, and measuring fluorescence intensity; and obtaining iron and phosphorus contents through the XRF standard curve. The method of combining a wet chemistry method and an X-ray fluorescent spectrometry is fast and high-speed, is simple to operate, has little error and long consumption time, and is environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a method for determining the content of iron and phosphorus in lithium iron phosphate, a cathode material of lithium batteries, by using an X-ray fluorescence spectroscopic analysis method. Background technique [0002] Lithium iron phosphate is a phosphate with an olivine structure, and its structure is stable. It is one of the cathode materials commonly used in lithium-ion batteries. At present, industrially synthesized lithium iron phosphate also contains a small amount of impurities. Therefore, as a lithium ion battery cathode material, the content of its main elements iron and phosphorus is the key indicator of its qualification standard. [0003] At present, the method for testing the content of iron and phosphorus in the lithium-ion battery industry mostly adopts "GB / T30835-2014 Carbon-composite Lithium Iron Phosphate Cathode Material for Lithium-ion Batter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
CPCG01N23/223G01N2223/076
Inventor 方婷婷夏劲
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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