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Method for preparing lithium phosphate crystal used as material of lithium battery

A lithium phosphate and crystal technology, applied in the field of optoelectronic materials, can solve the problems of unreported bulk lithium phosphate crystals, and achieve the effects of avoiding internal wrapping and defects, complete crystal form, and high crystal quality

Active Publication Date: 2014-07-02
SHANDONG UNIV
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology allows for better control over the properties of Lithium Phosphates during their production compared to previous methods that resulted in poorly formed or imperfect products. By controllably growing them at specific temperatures, they have improved performance characteristics such as higher capacity, longer lifetimes, less volatility than existing solutions, etc., resulting in more efficient use of resources within various industries like medicine, science exploration, defense, space development, and others.

Problems solved by technology

This patents describes different methods for producing lithiated metal oxides such as LixMnOz(LMNO) and LaFePO4. These techniques involve mixing certain compounds together during heat treatment, allowing them to be formed into desired shapes through solid state chemistry processes like sintering. However, these existing methods result in impurities from other sources including oxygen introduced during the process due to their poor control over temperature and humid conditions when compared to traditional methods.

Method used

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  • Method for preparing lithium phosphate crystal used as material of lithium battery
  • Method for preparing lithium phosphate crystal used as material of lithium battery
  • Method for preparing lithium phosphate crystal used as material of lithium battery

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Use a combination of LiCl-NaF molar ratio of 1:2 as a flux, raw material lithium carbonate: ammonium dihydrogen phosphate = 3:2 molar ratio and mix evenly into a platinum crucible, control the concentration of solute (ammonium dihydrogen phosphate + lithium carbonate) to 20wt%, heating up to 700°C.

[0032] The chemical reaction equation is: 3Li 2 CO 3 +2NH 4 h 2 PO 4 =2Li 3 PO 4 +2NH 3 ↑+3H 2 O↑+3CO 2 ↑

[0033] Raise the temperature to 800°C and keep the temperature constant for 24 hours to ensure that the material is fully melted and then stirred to make the melt fully mixed and even. Use the seed crystal test method to measure the solution saturation point temperature, select the lithium phosphate seed crystal obtained by spontaneous nucleation without defects, and when the temperature is 4°C higher than the solution saturation point temperature, introduce the seed crystal into the growth furnace, and place it in an appropriate position above the liquid surf...

Embodiment 2

[0035] use MoO 3 -KH 2 PO 4 The molar ratio of 1:3 is used as a flux, the raw material lithium carbonate: ammonium dihydrogen phosphate=3:2 molar ratio is mixed evenly and put into a platinum crucible, and the concentration of the solute (ammonium dihydrogen phosphate + lithium carbonate) is controlled to 20 w t%, heating up to 900°C.

[0036] The chemical reaction equation is: 3Li 2 CO 3 +2NH 4 h 2 PO 4 =2Li 3 PO 4 +2NH 3 ↑+3H 2 O↑+3CO 2 ↑

[0037] Raise the temperature to 900°C and keep the temperature constant for 24 hours to ensure that the material is fully melted and then stirred to make the melt fully mixed and even. Use the seed crystal test method to measure the solution saturation point temperature, select the lithium phosphate seed crystal obtained by spontaneous nucleation without defects, and when the temperature is 4°C higher than the solution saturation point temperature, introduce the seed crystal into the growth furnace, and place it in an appropr...

Embodiment 3

[0039] Use the combination of LiCl-NaF molar ratio 1:1.5 as the flux, the raw material lithium carbonate: ammonium dihydrogen phosphate = 3:2 molar ratio, mix evenly and put it into the platinum crucible, control the concentration of solute (ammonium dihydrogen phosphate + lithium carbonate) to 25wt%, heating up to 750°C.

[0040] The chemical reaction equation is: 3Li 2 CO 3 +2NH 4 h 2 PO 4 =2Li 3 PO 4 +2NH 3 ↑+3H 2 O↑+3CO 2 ↑

[0041] Keep the temperature at 750°C for 26 hours, and stir evenly after the material is fully melted. Seed according to the method of Example 1, then lower the temperature to 1°C above the saturation point, rotate at a rotation rate of 35 revolutions per minute, rotate in a forward-stop-reverse cycle, and start cooling after 4.5 hours. The cooling rate is 0.2-0.6°C / day for the first 16 days in the early growth period, 0.5-1.5°C / day for the second 16 days in the mid-growth period, and 1-2°C / day for the third 16 days in the later stage. The ...

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Abstract

The invention relates to a method for preparing lithium phosphate crystal used as a material of a lithium battery. According to the method, lithium phosphate and ammonium dihydrogen phosphate are used as raw materials, LiCl-NaF or MoO3-KH2PO4 is used as the fluxing agent, the concentration of solute is controlled at 20-50 wt%, and Li3PO4 bulk crystal with complete crystal form is prepared by using a flux growth method. The lithium phosphate crystal prepared according to the method can be used as the material of batteries for electric apparatuses such as medical treatment, scientific research and military.

Description

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Claims

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Application Information

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Owner SHANDONG UNIV
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