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Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process

A technology of ceramic powder and gel method, which is applied in the field of ceramic materials, can solve problems such as easy hydrolysis, and achieve the effects of energy saving, cost reduction, and high sintering activity

Inactive Publication Date: 2011-11-16
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
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Problems solved by technology

The present invention adopts water-based sol-gel method to prepare Li 4S iO 4 In the method of ceramic powder, choose SiO 2 Airgel is used as a silicon source, which solves the problem that TEOS is easily hydrolyzed in aqueous solution as a silicon source; soluble lithium-containing compounds (such as LiOH, CH 3 COOLi, LiNO 3 etc.) as lithium source; with citric acid (C 6 h 8 o 7 ·H 2 O) as a complexing agent and a regulator of the pH value of the solution; with deionized water as the reaction medium, Li with high sintering activity was prepared. 4 SiO 4 Nanopowder; single-phase Li can be obtained by controlling certain preparation conditions 4 SiO 4 Nano powder

Method used

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  • Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process
  • Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process
  • Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process

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Embodiment 1

[0049] Such as figure 1 Shown: Preparation of Li by water-based sol-gel method 4 SiO 4 Process flow of ceramic powder:

[0050] ① Dissolve LiOH in deionized water, prepare 400 mL of LiOH solution with a molar concentration of 0.4 mol / L, and then add dropwise an aqueous solution of citric acid with a molar concentration of 0.5 mol / L to complex Li + , and use C 6 h 8 o 7 ·H 2 O solution adjusts the pH value of the above solution, PH=6; ② Slowly add SiO dropwise to the solution obtained in step ① according to the molar ratio Li / Si=4 / 1 of Li and Si 2 Airgel and stirred continuously for 0.5h to obtain a slightly milky white colloidal solution; ③evaporate the solvent in the solution obtained in step ② at 70°C until sol-gel transition occurs; ④place the prepared gel at 90°C After aging in an oven for 12 hours, dry at 160°C for 12 hours to obtain a xerogel precursor; ⑤calcin the xerogel precursor at 675°C for 4 hours in an air atmosphere to obtain Li 4 SiO 4 Ceramic powder. ...

Embodiment 2

[0054] Dissolve LiOH in deionized water, prepare 400mL of three LiOH solutions with a molar concentration of 0.4mol / L each, and use C with a concentration of 0.5mol / L 6 h 8 o 7 ·H 2 O regulates the pH value of above-mentioned solution, makes the pH of solution be respectively 5,8.5,10, and other process and process parameter are with embodiment 1.

[0055] After testing, the XRD pattern of the ceramic powder obtained under the conditions of the three pH values ​​is the same as figure 2 It is exactly the same, that is, the powders prepared under the conditions of pH=5, 8.5, and 10 are all single-phase Li 4 SiO 4 Nano powder.

Embodiment 3

[0057] Dissolve LiOH in deionized water, prepare 400 mL of LiOH solution with a molar concentration of 0.4 mol / L, and add C with a concentration of 0.5 mol / L 6 h 8 o 7 ·H 2 O adjusts the pH of the above solution=6; slowly add SiO to the above solution according to the molar ratio Li / Si=3.4 / 1 2 Airgel is stirred continuously, and other process parameters are the same as in Example 1. The xerogel was calcined at 675°C for 4 hours, and the main crystal phase of the obtained ceramic powder was Li 4 SiO 4 , containing only a small amount of Li 2 SiO 3 .

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Abstract

The invention belongs to the field of ceramic materials and relates to a method for preparing lithium orthosilicate ceramic powder by a water-based sol-gel process. In the invention, a soluble lithium compound is used as a lithium source, SiO2 aerogel is used as a silicon source, citric acid is used as a complexing agent and a pH regulator for the solution, deionized water is used as a reaction medium, Li4SiO4 nano powder is synthesized at 550 to 700 DEG C, the pure-phase Li4SiO4 can be obtained by controlling some preparation conditions, the nano powder has high sintering activity, and the linear shrinkage at a temperature between room temperature and 1,000 is 3 times higher than that of Li4SiO4 powder prepared by a solid-phase reaction process. In the method, the raw materials are readily available and cheap, water is used as a reaction medium, and cost is lowered; and the reaction temperature is over 200 DEG C lower than that of the solid-reaction process, and energy is saved. The relative density of ceramic prepared by using Li4SiO4 nano powder is up to 82.9 percent, which is much higher than that of ceramic prepared by the solid-phase reaction process.

Description

technical field [0001] The invention belongs to the field of ceramic materials, and relates to a method for preparing lithium orthosilicate ceramic powder by a water-based sol-gel method. Background technique [0002] Lithium orthosilicate (Li 4 SiO 4 ) Synthesis methods of ceramic powder include: solid phase reaction method, precipitation method, combustion method, sol-gel method, etc. The solid phase reaction method and the precipitation method require high reaction temperature (≥900°C), which easily leads to the volatilization of some components, and it is difficult to control the composition of the final product. In addition, the synthesis of powder at high temperature is not conducive to controlling the shape of the product and uniformity etc. Combustion method hardly obtains single-phase Li in air atmosphere 4 SiO 4 , often with Li 2 CO 3 , Li 2 SiO 3 and other heterogeneous phases are generated. The sol-gel method can not only realize the low-temperature syn...

Claims

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Application Information

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IPC IPC(8): C04B35/624C04B35/16
Inventor 温兆银吴相伟吴梅芬张敬超顾中华
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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