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Preparation method of nano-flaky FePO4.2H2O

A technology of fepo4·2h2o and nano flakes, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problem of inability to control the size and shape of lithium iron phosphate, and the inability to effectively control the size and shape of products , It is not conducive to improving the electrochemical performance of lithium iron phosphate cathode materials, etc., to achieve the effect of improving electrochemical performance, simple synthesis method, and good electrochemical performance

Inactive Publication Date: 2011-04-13
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the size and shape of the product cannot be effectively controlled; the second is that the prepared ferric phosphate precipitates are mostly amorphous (that is, amorphous) products
When the iron phosphate prepared by this method is used to produce the lithium iron phosphate cathode material for lithium ion batteries, the size and shape of the obtained lithium iron phosphate cannot be controlled, which is not conducive to improving the electrochemical performance of the lithium iron phosphate cathode material

Method used

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  • Preparation method of nano-flaky FePO4.2H2O
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  • Preparation method of nano-flaky FePO4.2H2O

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 1.4 g of cetyltrimethylammonium bromide (CTAB) and dissolve it in 20 mL of deionized water to obtain a clear and transparent solution, add 3.0 g of FeCl to the solution 3 ·6H 2 O and stir to dissolve it completely, then add 4mL H 3 PO 4 The solution (85 wt%) was dropped into the above solution and stirred for 1 hour. Afterwards, the transparent solution was heated in a water bath at 90 °C for 24 h. The white precipitate obtained by filtration was washed successively with deionized water and ethanol, and then dried at 100°C for 4 hours. The product obtained by the above synthesis method was characterized by XRD, SEM and TEM, and it was proved that the product was FePO with a monoclinic crystal system and a thickness of 100 nanometers. 4 2H 2 O crystal flakes (the resulting FePO 4 2H 2 The SEM and TEM images of the O crystal flakes are shown in the appendix figure 1 And attached figure 2 ).

Embodiment 2

[0031] Get 1.4 g of cetyltrimethylammonium bromide (CTAB) and dissolve it in 200 mL of deionized water to obtain a clear and transparent solution (the concentration of CTAB is one-tenth of that in Example 1), and add 3.0 g of FeCl to the solution 3 ·6H 2 O and stir to dissolve it completely, then add 4mL H 3 PO 4 The solution (85 wt%) was dropped into the above solution and stirred for 1 h. Afterwards, the transparent solution was heated in a water bath at 90 °C for 24 h. The obtained white precipitate was filtered, washed successively with deionized water and ethanol, and then dried at 100°C for 4 hours. The obtained product was characterized by XRD, which showed that the obtained product was monoclinic FePO 4 2H 2 O crystals. The obtained product was characterized by SEM, which indicated that the obtained product was a flake with a thickness of 30 nm. With the FePO 4 2H 2 O crystal flakes as Fe and P sources supplemented with LiOH·H 2 O is used as the lithium sourc...

Embodiment 3

[0033] Take 1.4 g of cetyltrimethylammonium bromide (CTAB) and dissolve it in 20 mL of deionized water to obtain a clear and transparent solution, add 3.0 g of FeCl to the solution 3 ·6H 2 O and stir to dissolve it completely, then add 1mL H 3 PO 4 solution (85 wt%) was dropped into the above solution (H 3 PO 4The concentration is a quarter of that of Example 1) and stirred for 1 hour. Afterwards, the transparent solution was heated in a water bath at 90 oC for 20 h. The white precipitate obtained by filtration was washed successively with deionized water and ethanol, and then dried at 100°C for 4 hours. The product obtained by the above synthesis method was characterized by XRD and SEM, and it was proved to be FePO with a monoclinic crystal system and a thickness of 50 nanometers. 4 2H 2 O crystal flakes. In this synthetic method, H 3 PO 4 A wide concentration range is possible.

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Abstract

The invention belongs to the field of inorganic materials and provides a preparation method of nano-flaky FePO4.2H2O. The preparation method comprises the following steps: preparing an iron salt solution and phosphoric acid, wherein the dosage molar ratio of the iron salt to the H3PO4 is as follows: Fe:P=1:1-1:5; dissolving the surfactant which is taken as an additive into the iron salt solution or the phosphoric acid, wherein the concentration of the surfactant is not less than 3g / L; dropwise adding the phosphoric acid into the iron salt solution or dropwise adding the iron salt solution into the phosphoric acid, and stirring; then, insulating for 6-24h at 70-90 DEG C; and filtering the obtained precipitates, and then, washing and drying the precipitates. The method provided in the invention can be used for preparing a monoclinic or orthorhombic nano-flaky FePO4.2H2O crystal. The lithium iron phosphate used as a positive material of a lithium ion battery, which is synthesized by using the product as an iron source and a phosphorus source, has very good specific capacity, charge-discharge efficiency, cycle performance and high-magnification performance. The preparation method is simple, and the product appearance can be regulated and controlled easily, thereby being suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of nano-flaky iron phosphate, which belongs to the technical field of inorganic materials. Background technique [0002] In order to meet the huge demand for mobile new energy, the development of secondary batteries with excellent performance, safety, low price, and environmental friendliness has attracted widespread attention. Currently LiFePO 4 and FePO 4 As a positive electrode material for power lithium-ion batteries, it is recognized as the best choice. Studies have shown that as a synthetic LiFePO 4 The main raw material FePO 4 , its structure, morphology and particle size will directly affect the product LiFePO 4 structure and performance. [0003] The production method of iron phosphate mainly includes precipitation method, that is, ferrous iron salt is oxidized to ferric iron with hydrogen peroxide, and then phosphoric acid or phosphate and ferric iron are used to form ferric phosphate precipi...

Claims

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Application Information

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IPC IPC(8): C01B25/37
Inventor 张友祥王梦张克立
Owner WUHAN UNIV
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