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Method for preparation of lithium tantalate nano-powder by hydrothermal process

A nano-powder, lithium tantalate preparation technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of difficulty in synthesizing nanoparticles, requiring high temperature, and long reaction time, etc. Achieve the effect of small, complete and uniform grains, low reaction temperature and short reaction time

Inactive Publication Date: 2014-06-04
SHANGHAI MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of LiTaO3 usually has methods such as molten salt method, co-precipitation method, sol-gel method and deionized hydrothermal method. However, there are three main problems in the preparation and synthesis technology: (1 ) The current synthesis technology is difficult to synthesize nanoparticles with uniform size and fine grain; (2) Due to the high cost, most nano powder synthesis technologies cannot be industrialized; (3) The self-agglomeration of nano powder cannot be effectively solved solve
The above problems largely limit the wide application of LiTaO3
[0003] Through literature search of the prior art, it is found that the Chinese patent whose publication number is CN103011839A discloses a deionized hydrothermal method to prepare a mixture of cubes and pellets structure of LiTaO3 lead-free piezoelectric ceramic powder, the disadvantage of this method is that the reaction time is long, and high-purity LiTaO3 nanopowder cannot be obtained
After literature search, it was also found that Li Lihong and others published "Synthesis of LiTaO3 powder by molten salt method" in "Journal of Inorganic Chemistry" (August 2006, No. 8, pp. 1491-1494), The specific method is: using LiCl, Li2CO3, Ta2O5 as raw materials, Weigh the raw materials, then grind them with an agate mortar, and then add ethanol without deionized water to wet mix, so that the powder is fully mixed, dried, and reacted in the air at 650-900 °C for 3 h, cooled with the furnace, and used The hot deionized water was washed several times until no Cl― was detected in the filtrate with silver nitrate reagent, and LiTaO3 was obtained by drying at 120°C. Requires high temperature, not suitable for mass production

Method used

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  • Method for preparation of lithium tantalate nano-powder by hydrothermal process

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Experimental program
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Effect test

Embodiment 1

[0023] Add 150mL of reaction solvent deionized water into the autoclave with magnetic rotation stirring, then add 1g Li 2 CO 3 and 3.59g Ta(OH) 5 , to ensure that the molar ratio of tantalum ions to lithium ions is 1:2, react for 12 hours, and the reaction temperature is 240 ° C. After the reaction is completed, wash twice with deionized water, and then wash twice with ethanol to obtain lithium tantalate nanoparticles. Powder. The scanning electron microscope picture of lithium tantalate nanopowder is attached figure 1 , the grain size is 100-150nm, the powder has no impurities, the crystallinity is good and there is no impurity phase, the crystal is square columnar, and there is no agglomeration phenomenon.

Embodiment 2

[0025] Add 180mL of reaction solvent deionized water into the autoclave with magnetic rotation stirring, then add 1g Li 2 CO 3 and 2.983g Ta 2 o 5 , to ensure that the molar ratio of tantalum ions to lithium ions is 1:2, react for 12 hours, and the reaction temperature is 240 ° C. After the reaction is completed, wash twice with deionized water, and then wash twice with ethanol to obtain lithium tantalate nanoparticles. Powder. Lithium tantalate nano-powder has a grain size of 200-250nm, and the powder has no impurities, good crystallinity, no impurity phase, and regular shape.

Embodiment 3

[0027] Add 200mL of reaction solvent deionized water into the autoclave with magnetic rotation stirring, then add 1g LiOH and 2.63g Ta 2 o 5 , to ensure that the molar ratio of tantalum ions to lithium ions is 1:3.5, react for 12 hours, and the reaction temperature is 240 ° C. After the reaction, wash twice with deionized water, and then wash twice with ethanol to obtain lithium tantalate nanoparticles Powder. Lithium tantalate nano-powder has a grain size of 250-300nm, and the powder has no impurities, good crystallinity, no impurity phase, and regular shape.

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Abstract

The invention discloses a method for preparation of lithium tantalate nano-powder by a hydrothermal process. The method includes: using deionized water as a reaction solvent, adding a lithium source and a tantalum source, ensuring the mole ratio of tantalum ions to lithium ions at 1:(1-8), carrying out reaction for 8-24h in an autoclave, keeping the reaction temperature at 200-260DEG C, and at the end of the reaction, firstly conducting washing by deionized water, and then performing washing by an alcohol solvent, thus obtaining the lithium tantalate nano-powder. The lithium source is LiOH or Li2CO3, and the tantalum source is Ta(OH)5 or Ta2O5. The method provided by the invention adopts different lithium sources and different tantalum sources as the raw materials, and takes deionized water as a reaction solvent to synthesize the LiTaO3 nano-powder. The prepared LiTaO3 powder has a regular shape, fine, complete and uniform grains, high purity, no aggregation or less agglomeration, and has no need for high-temperature calcination treatment. The method provided by the invention has the advantages of fewer steps, simple preparation, short reaction time, low reaction temperature, and is suitable for mass production.

Description

technical field [0001] The invention relates to the field of preparation of lithium tantalate nano powders, in particular to the preparation of lithium tantalate nano powders by a hydrothermal method. Background technique [0002] Lithium tantalate (LiTaO 3 ) is an important ferroelectric piezoelectric material. In recent years, the research and development competition of lead-free piezoelectric ceramics has become increasingly fierce. LiTaO 3 The excellent properties of ceramics have attracted extensive attention from scholars. Preparation of LiTaO 3 Usually there are methods such as molten salt method, co-precipitation method, sol-gel method and deionized hydrothermal method, but there are three main problems in the preparation and synthesis technology: (1) the current synthesis technology is difficult to synthesize crystals with uniform size (2) Due to the high cost, most nanopowder synthesis technologies cannot be industrialized; (3) The self-agglomeration problem of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G35/00B82Y30/00
Inventor 高林强陈海邹鑫
Owner SHANGHAI MARITIME UNIVERSITY
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