Method for producing carbon coated nano stage lithium iron phosphate by precipitation

A lithium iron phosphate, carbon coating technology, applied in electrode manufacturing, electrical components, battery electrodes and other directions, can solve the problem of uneven mixing, and achieve the effects of simple process, low consumption of lithium source and low cost

Inactive Publication Date: 2010-08-25
南京海泰纳米材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] In view of the shortcomings of the above method, the present invention provides a method for preparing carbon-coated nano-scale lithium iron phosphate by precipitation method, directly using ferrous salt, phosphorus-containing compound and lithium salt as raw materials, and using liquid phase synthesis The process directly synthesizes lithium iron phosphate materials with excellent electrochemical properties, avoiding the shortcomings of uneven mixing in other synthesis methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: LiFePO 4 / C synthesis

[0035] After stirring and mixing 27.8 grams (0.1 moles) of ferrous sulfate and 300 grams of deionized water, add 11.50 grams (0.1 moles) of ammonium dihydrogen phosphate, stir again, add 6 grams of citric acid, and add ammonia water to control pH 5.5, at 30 The reaction was stirred in a vessel at °C for 5 hours, and after standing for 15 hours, the precipitate was filtered and washed.

[0036] 200 grams of deionized water, 5 grams of glucose and 4.2 grams (0.1 mol) of lithium hydroxide were added to the precipitate to mix well, and the reaction was stirred again in a 30°C container for 4 hours, and then dried at 100°C. After the product was pulverized, the temperature was heated at a heating rate of 10 °C / min under nitrogen protection, and the temperature was maintained at 725 °C for 600 min, and then cooled to room temperature with the furnace. After pulverization, a lithium iron phosphate nanoscale product was obtained.

[0037] Ma...

Embodiment 2

[0039] Example 2: LiFePO doped with metal element Mg 4 / C synthesis

[0040] Stir and mix 27.8 g (0.1 mol) of ferrous sulfate and 400 g of deionized water, add 11.50 g (0.1 mol) of ammonium dihydrogen phosphate, and stir again and add 0.246 g (0.001 mol) of MgSO 4 .7H 2 O, continue to stir and add 4 grams of citric acid, and add ammonia water to control pH 7.2, stir and react in a container at 50 ° C for 2 hours, and after standing for 5 hours, filter and wash the precipitate.

[0041] 600 grams of deionized water, 5 grams of glucose and 4.16 grams (0.099 moles) of lithium hydroxide were respectively added to the precipitate to mix uniformly. After stirring and reacting again in a container of 50°C for 4 hours, the water was dried at 90°C. After the product is pulverized, the temperature is heated at a heating rate of 10°C / min under nitrogen protection, and is incubated at a constant temperature of 650°C for 600 minutes, and then cooled to room temperature with the furnace. ...

Embodiment 3

[0042] Example 3: LiFePO doped with metal elements Mn and W 4 / C synthesis

[0043] 0.246 g (0.001 mol) MgSO in Example 2 4 .7H 2 O was replaced by 0.0017 g (0.00001 mol) MnSO 4 .H 2 O and 0.13 g (0.00099 mol) ammonium tungstate, and other preparation ratios and operation steps are the same as those in Example 2, to obtain a lithium iron phosphate nanoscale product doped with metal elements Mn and W.

[0044] The button battery was prepared according to the method of Example 1, and its battery cycle performance was tested. The average particle size of the product is 70nm, and the tap density can reach 1.5g / cm 3 , the first discharge specific capacity at room temperature can reach 150mAh / g.

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Abstract

The invention discloses a precipitation method for preparing nanometer level iron phosphate lithium coated with carbon. The method comprises the following steps: firstly, weighing iron salt, deionized water and a compound of metallic elements; after the stirring and the mixing are performed, adding a phosphorous compound and citric acid diluted with water to the mixture; after the stirring is performed again, adding a precipitation agent to the mixture and controlling to the neutrality; stirring to react in a container, and after the static placement, respectively adding the deionized water, a carbon source and lithium salt to mix uniformly after the precipitate is filtered and washed; stirring again to react, and drying the water at 30 to 160 DEG C and warming up at the heating rate under the protection of non-oxidized gas after a product is crashed; baking at a constant temperature of 450 to 850 DEG C, cooling down to a room temperature at a cooling rate or with a stove, and finallyobtaining the nanometer level ferric phosphate lithium coated with the carbon after crashing is performed. The precipitation method has the advantage that the raw material cost and the processing cost are low because bivalent iron is taken as the raw material. The iron phosphate lithium prepared by using the process has the characteristics of good physical processing performance and good electrochemistry performance, and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to a method for preparing battery materials, more particularly to a method for preparing liquid-phase precipitation of carbon-coated metal element-doped nano-scale lithium iron phosphate. Background technique [0002] LiFePO was first reported since 1997 4 Since it has the function of de-intercalating lithium, the olivine-type phosphate-based lithium-intercalating material LiMPO has 4 (M: Mn, Fe, Co, Ni) has attracted much attention as a potential cathode material for lithium-ion batteries. Among them, LiFePO with a theoretical capacity of 170mAh / g 4 , with its rich iron resources, low price, excellent thermal stability and environmental friendliness, is considered to be the most promising cathode material for lithium-ion batteries. [0003] At present, the methods for synthesizing lithium iron phosphate include high-temperature solid-phase reaction method, liquid-phase co-deposition method, sol-gel method, hydrothermal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/04H01M4/1397
CPCY02E60/10
Inventor 周海燕姜华张玉梅杜彩侠张翠芬资利云
Owner 南京海泰纳米材料有限公司
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