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Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid

A technology of crystalline lithium iron phosphate and iron hydroxide glue, which is applied in the field of preparation of positive electrode materials for lithium-ion power batteries, can solve problems such as difficult industrialization, large secondary aggregates, and long synthesis cycle, and achieve high specific capacity, Strong specific surface area, high and low temperature effects

Inactive Publication Date: 2011-04-06
杨志宽
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using these raw materials and synthesis methods, the primary particles of lithium iron phosphate materials prepared are relatively large, and the secondary aggregates are relatively large, which is obviously not conducive to material rate discharge, low temperature discharge, etc.
[0005] Invention patent 200710013369.6 discloses a method for preparing homogeneously dispersed lithium iron phosphate nanocrystals by hydrothermal synthesis. The homogeneously dispersed lithium iron phosphate nanocrystals with a particle size of 0.2-0.5 μm are prepared, but the hydrothermal synthesis method used is limited to a small amount For the preparation of powder, if the amount of preparation is to be expanded, it is difficult to design and manufacture large-scale high-temperature and high-pressure reactors, and it is difficult to realize industrialization
[0006] The patent application number is 200810029616.6, which discloses a method for preparing nano-lithium iron phosphate materials by sol-gel method, but requires a large amount of additives and complexing agents, such as polyvinyl alcohol or octadecyltrimethylammonium bromide, lemon Acid, malic acid or tartaric acid, etc., lead to problems such as large drying shrinkage of the precursor, difficulty in industrialization, and long synthesis cycle

Method used

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  • Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid
  • Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid
  • Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid

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Experimental program
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Effect test

Embodiment 1

[0019] 85.61gFeCl 3 ·6H 2 O was dissolved in 93.26 mL of deionized water to form FeCl 3 saturated solution, and dropwise into boiling water to prepare fresh reddish-brown Fe(OH) 3 Colloids are obtained through the verification of Tyndall's phenomenon. Add 32.94gLiH to the above colloid 2 PO 4 At the same time, 19.60 g of starch was added as an organic carbon source, and the mixture was mixed evenly by rapid stirring. Then, the vacuum degree was kept at 0.09 MPa at 50 ° C, and dried for 24 hours to obtain the precursor powder. The precursor was placed in a nitrogen-protected muffle furnace, heated to 500 °C at a rate of 1 °C / min, kept for 24 hours, and then naturally cooled to room temperature. After taking it out, it was ground or pulverized to obtain LiFePO 4 / C powder material.

[0020] The XRD of the product that present embodiment obtains is as figure 2 As shown, it can be seen that a pure-phase olivine-type lithium iron phosphate material was synthesized. The ele...

Embodiment 2

[0023] 85.61gFeCl 3 ·6H 2 O was dissolved in 93.26 mL of deionized water to form FeCl 3 saturated solution, then dropwise into deionized water while adding a small amount of 10% NH 3 ·H 2 O, forming fresh reddish-brown Fe(OH) 3 Colloids are obtained through the verification of Tyndall's phenomenon. Add 12.89gLi to the above colloid 2 CO 3 Solid nanoscale powder and contains 36.43gNH 4 h 2 PO 4 At the same time, 21.40 g of glucose was added as an organic carbon source, stirred rapidly and evenly, and then kept at 100 °C with a vacuum degree of 0.02 MPa, and dried for 5 h to obtain a precursor powder. Put the precursor into a muffle furnace, heat up to 800°C at a rate of 0.5°C / min, keep it warm for 2 hours, and then cool it down to room temperature naturally. After taking it out, it is ground or pulverized to obtain LiFePO 4 / C powder material.

[0024]Test the electrical properties of the above positive electrode materials, the 0.2C discharge specific capacity at 25 ...

Embodiment 3

[0026] 128.03gFe(NO 3 ) 3 9H 2 O was dissolved in 114.31 mL of deionized water to form a saturated solution, and then dropped into deionized water drop by drop while adding a small amount of 10% NH 3 ·H 2 O, forming fresh reddish-brown Fe(OH) 3 Colloids are obtained through the verification of Tyndall's phenomenon. Add a solution containing 7.60g LiOH and 36.55mLH to the above colloid 3 PO 4 (85% w.t.) solution, while adding 19.60 g of starch as an organic carbon source, stirring quickly and uniformly, then keeping the vacuum at 0.08 MPa at 70 ° C, and drying for 15 h to obtain a precursor powder. Put the precursor into a muffle furnace, heat up to 650°C at a rate of 1.5°C / min, keep it warm for 10 hours, and then cool it down to room temperature naturally. After taking it out, it is ground or pulverized to obtain LiFePO 4 / C powder material.

[0027] Test the electrical performance of the above positive electrode material, the 0.2C discharge specific capacity at 25 deg...

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Abstract

The invention relates to a method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid, which comprises the steps of: with Fe(OH)3 colloid as a raw material, adding a lithium source, a phosphorus source and an organic carbon source in the colloid, powerfully and uniformly stirring and drying in vacuum at low temperature to form a uniform nano precursor containing lithium, iron, phosphorus and carbon; and placing in a crucible and raising the temperature to 500-800 DEG C in a muffle furnace protected by inert atmosphere, preserving the temperature for 2-24h, cracking the organic carbon source into carbon under the inert atmosphere, reducing ferric iron into ferrous iron by the carbon to form carbon wrapped lithium iron phosphate, naturally cooling to room temperature, and then grinding or crushing to obtain the nanocrystalline lithium iron phosphate powder. The colloid Fe(OH)3 is used as an iron source, the prepared lithium iron phosphate is of nano level, has excellent electrochemical property and low-temperature discharge property, is simple in process, and is suitable for industrialized production.

Description

Technical field: [0001] The invention relates to a method for preparing nanocrystalline lithium iron phosphate powder by using iron hydroxide colloid, and belongs to a method for preparing positive electrode materials for lithium-ion power batteries. Background technique: [0002] Olivine-type lithium iron phosphate has the advantages of safety, no pollution, wide source of raw materials, and good cycle stability. It is considered to be used in pure electric vehicles, hybrid electric vehicles, electric bicycles, electric tools, energy storage power stations, etc. The best cathode material for power batteries in the field of high power. [0003] However, pure-phase lithium iron phosphate has poor conductivity and low ionic conductivity, so that its capacity decays rapidly during high-current discharge; the diffusion rate of lithium ions has a very direct relationship with temperature, especially at low temperatures (-20°C, -40°C). , the lithium ion diffusion rate is lower, r...

Claims

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Application Information

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IPC IPC(8): H01M4/1397B82Y40/00
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 杨志宽黄文杰都立珍程元胜
Owner 杨志宽
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