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Method for controlling shape and carbon content of iron phosphate material

A technology of lithium iron phosphate and carbon content, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of discrete chemical performance indicators of materials, deviation of material tap density and specific surface area, and large internal resistance of materials. Achieve the effects of controlling the generation of unqualified materials, reducing equipment investment, and simplifying the production process

Active Publication Date: 2014-05-21
SICHUAN JINWANGTONG ELECTRONICS SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, in the production of lithium iron phosphate materials, the raw materials are generally crushed after pre-calcination. Large, general processing performance, large dispersion of chemical performance indicators of materials
At the same time, the coated carbon source and reduced carbon source used in the production process of lithium iron phosphate materials are mainly organic carbon sources, and the discrete medium used is mainly industrial alcohol, so there are differences in the production process of carbon-coated lithium iron phosphate materials. The carbon content deviation of different batches of materials is relatively large. At present, the deviation of carbon content between different batches of international and domestic lithium iron phosphate materials is ±0.3%. These deviations are mainly caused by the mixing and ball milling in the production process. It is difficult to control the degree of dryness to be completely consistent, and the industrial alcohol used as a dispersion medium contains higher alcohols
The direct consequence of the carbon content deviation of this material is the deviation of the tap density and specific surface area of ​​each batch of materials, that is, the deviation of electrochemical performance and processing performance, which also affects the batches of iron phosphate we produce. The consistency of lithium materials has a greater impact on subsequent battery manufacturing

Method used

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  • Method for controlling shape and carbon content of iron phosphate material
  • Method for controlling shape and carbon content of iron phosphate material
  • Method for controlling shape and carbon content of iron phosphate material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Detect the carbon content of the precursor powder of the lithium iron phosphate material after crushing. The measured value is 3.46%, and the control value is 3.38%-3.50%. The measured value is within the range of the control value. Put this batch of powder into the rolling Ball mill shaping is carried out in the ball mill; during ball mill shaping, the grinding balls and powder are mixed at a mass ratio of 1:1, and the grinding balls are proportioned according to the weight ratio Φ20:Φ15:Φ10:Φ5=3:2:1:3, and the rolling time is for 40 minutes; then detect the particle size of the powder, and discharge when the particle size of the powder reaches D50=6.8μ, D100≤69μ; put this batch of powder in a pusher kiln under a nitrogen atmosphere for secondary sintering to With a push rate of 40 minutes / time, the material is sintered at a constant temperature of 720°C, kept for 14 hours, and then pushed out of the pusher kiln at the same speed to obtain the finished product of lithiu...

Embodiment 2

[0055] Detect the carbon content of the precursor powder of the lithium iron phosphate material after crushing. The measured value is 3.18%, and the control value is 3.38%-3.50%. The measured value is outside the control value range. This batch of 160Kg powder and carbon Content is 3.68% 160Kg powder is mixed, then puts into the ball mill according to the capacity of ball mill and carries out ball mill shaping treatment, the condition during ball mill shaping and the condition during secondary sintering are all the same as in embodiment one, makes ferric phosphate thus Lithium material finished product.

[0056] The finished product of the lithium iron phosphate material obtained in this embodiment is analyzed with an X-ray diffractometer to obtain the following crystal structure: Figure 5 The X-ray diffraction pattern shown. From such as Figure 5 It can be seen from the X-ray diffraction pattern of the finished product of the lithium iron phosphate material obtained accor...

Embodiment 3

[0061] Detect the carbon content of the precursor powder of the lithium iron phosphate material after crushing. The measured value is 3.93%, and the control value is 3.38%-3.50%. Mix this batch of 100Kg powder with 160Kg powder with a carbon content of 2.58%. , and then put it into a ball mill according to the capacity of the ball mill for ball mill shaping treatment. The conditions during ball mill shaping and the conditions during secondary sintering are all the same as those in Example 1, thus obtaining the finished product of lithium iron phosphate material.

[0062] The finished product of the lithium iron phosphate material obtained in this embodiment is analyzed with an X-ray diffractometer to obtain the following crystal structure: Figure 7 The X-ray diffraction pattern shown. From such as Figure 7 It can be seen from the X-ray diffraction pattern of the finished product of the lithium iron phosphate material obtained according to the method for controlling the morp...

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Abstract

The invention discloses a method for controlling the shape and the carbon content of an iron phosphate material. The method comprises the steps of: mixing to prepare a raw material of the iron phosphate material, presintering, and then drying to obtain powder of a precursor of the iron phosphate material; smashing the presintered and dried powder of the precursor of the iron phosphate material; detecting the carbon content of the smashed powder, and placing the powder of the measured batch to a ball mill to be subjected to ball-mill and reshaping treatment when the carbon content of the powder of the measured batch is within a control valve range and balancing and mixing the powder batches with positive deviation and negative deviation calculated according to weight percentage when the carbon content of the powder of the measured batch is beyond the control value range and has deviation, and then placing the mixture into the ball mill to be subjected to ball-mill and reshaping treatment; detecting the grain size of the powder subjected to ball-mill and reshaping treatment, and discharging when the grain size of powder of the measured batch meets the requirement of the control value; and performing secondary sintering to obtain the finished product of the iron phosphate material.

Description

technical field [0001] The invention belongs to the technical field of energy material manufacturing, and in particular relates to a method for controlling the morphology and carbon content of the lithium iron phosphate material during the manufacturing process of the lithium iron phosphate material. Background technique [0002] Lithium-ion batteries have become the main choice of rechargeable power supplies for today's portable products because of their advantages such as large specific energy, high power density, long cycle life, low self-discharge, high performance-price ratio, and less pollution. With the development of lithium-ion batteries, cathode materials have become one of the important bottlenecks restricting the development of lithium-ion batteries. Due to the existence of mixed valence states, transition metals often have relatively ideal electronic conductivity and are not prone to disproportionation reactions. Their oxides have become the first choice for lit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/12Y02E60/10
Inventor 刘海润
Owner SICHUAN JINWANGTONG ELECTRONICS SCI & TECH