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Preparation method of lithium ferrous silicate composite material

A technology of lithium ferrosilicate and composite materials, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of uneven particle size and complex process of lithium ferrosilicate composite materials, and achieve controllable morphology and cycle. High performance, process improvement effect

Inactive Publication Date: 2015-07-29
XIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of lithium ferrous silicate composite material, which solves the problem that the existing preparation method is complex and the particle size of the prepared lithium ferrous silicate composite material is not uniform

Method used

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  • Preparation method of lithium ferrous silicate composite material
  • Preparation method of lithium ferrous silicate composite material
  • Preparation method of lithium ferrous silicate composite material

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preparation example Construction

[0022] The preparation method of lithium ferrous silicate composite material of the present invention, specifically implement according to the following steps:

[0023] Step 1, sequentially dissolving the lithium source compound, iron source compound, silicon source compound and surfactant in the solvent, the molar ratio of lithium in the lithium source compound, iron in the iron source compound, and silicon in the silicon source compound is 1.95-2.1: 1:1; the mass ratio of surfactant to lithium source compound is 0 to 3:1, the molar ratio of solvent to lithium source compound is 100 to 500:1, and then the pH is adjusted to 2 to 6 with organic acid, and then In the reaction kettle, react in low temperature water at 150-200°C for 1-24 hours, wash with water, filter, and finally obtain the precursor by spray drying;

[0024] In step 2, the precursor obtained in step 1 is mixed with the carbon source compound and then ball milled. The quality of the carbon source compound is 1 to...

Embodiment 1

[0034] Step 1, sequentially dissolve 0.01mol of lithium carbonate, 0.02mol of ferrous sulfate, 0.02mol of tetraethyl orthosilicate and 2g of polyethylene glycol in 60ml of deionized water, then adjust the pH to 4 with citric acid, and then React in low temperature water at 180°C for 12 hours, wash with water, filter, and finally spray dry to obtain the precursor;

[0035]Step 2, mix the precursor obtained in step 1 with 0.48g of glucose, ball mill for 24 hours, then in an inert atmosphere, first keep it at 450°C for 2h, then keep it at a high temperature of 750°C for 10h, and after cooling, you can get lithium ferrous silicate composite Material.

[0036] figure 1 It is the X-ray diffraction pattern of the lithium ferrous silicate composite material prepared in Example 1 of the present invention, from figure 1 As can be seen, figure 1 The main peak is the diffraction peak of the lithium ferrous silicate composite material, indicating that the lithium ferrous silicate compos...

Embodiment 2

[0040] Step 1, sequentially dissolve 0.039 lithium acetate, 0.02mol ferrous sulfate, 0.02mol sodium silicate in a mixture of 30ml ethanol and 40ml acetone, then use ascorbic acid to adjust the pH to 2, and then carry out low temperature in the reaction kettle at 150°C After reacting in water for 24 hours, wash with water, filter, and finally spray dry to obtain the precursor;

[0041] Step 2, mix the precursor obtained in step 1 with 0.0322g of conductive graphite and ball mill for 24 hours, then in an inert atmosphere, first keep it at 300°C for 6h, then keep it at a high temperature of 600°C for 24h, after cooling, you can get lithium ferrous silicate composite material.

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Abstract

The invention relates to a preparation method of a lithium ferrous silicate composite material. The method comprises the following concrete steps of: step 1, sequentially dissolving a lithium source compound, an iron source compound, a silicon source compound and a surface active agent into a solvent, and then adjusting the pH to be 2-6 by organic acid, carrying out low temperature water reaction, washing the product by water, filtering, and carrying out spray drying to obtain precursor; step 2, mixing the obtained precursor and a carbon source compound, and carrying out ball-milling and calcination, and cooling to obtain the lithium ferrous silicate composite material. The preparation method of the lithium ferrous silicate composite material combines a hydrothermal method and spray drying, so that the technology is obviously improved; and the obtained lithium ferrous silicate composite material is controllable in morphology and small and even in particle size, and has better charge-discharge property and cycle performance and higher volume ratio.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a method for preparing a lithium ferrous silicate composite material. Background technique [0002] Since lithium ferrous silicate material has the same lattice stability effect as lithium iron phosphate material, and has a high gram capacity, and the silicon element is non-toxic, abundant and cheap, it has become a new type of lithium-ion battery cathode material. The preparation methods of lithium ferrous silicate cathode composite materials mainly include solid-phase method, sol-gel method and hydrothermal synthesis method. The solid-phase method is characterized by simple process and low cost, but the material prepared by it has uneven particle size, large grains, and is easy to be mixed with impurities. The materials prepared by sol-gel method and hydrothermal synthesis method have smaller particle size and better performance, but the control process in the prepa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/587
CPCY02E60/10
Inventor 任冰许云华王娟强静李雯
Owner XIAN UNIV OF TECH
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