Constant pressure hydro-thermal preparation method for barium zirconate titanate powder

A barium zirconate titanate and atmospheric pressure hydrothermal technology is applied in the field of preparation of barium zirconate titanate powder, which can solve the problems of high performance requirements of reaction equipment, high energy consumption in the reaction process, uneven particle size distribution, etc., and achieves low cost , reaction conditions in real time, easy to adjust and control effects

Active Publication Date: 2008-01-16
仙桃市中星电子材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention mainly solves the technical problems existing in the production method of barium zirconate titanate powder in the prior art, such as complex process, high requirements on the performance of reaction equipment, high energy consumption, long time and high cost of the reaction process.
[0005] At the same time, the invention also solves the technical problems of low powder purity, large particles and uneven particle size distribution existing in the existing production technology of barium zirconate titanate powder.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: prepare BaTi 0.8 Zr 0.2 o 3 . Use a measuring cylinder to measure 0.2 liters of 4.0mol / L titanium tetrachloride solution, 0.2 liters of 1.0mol / L zirconium oxychloride solution and 1 liter of 1.2 mol / L barium chloride solution in the container, and add 0.6 liters of deionized water to stir to mix evenly; then pour the above mixed solution into the normal pressure reactor, start stirring, and add 312g of sodium hydroxide solid to it, heat up to 80°C with an electric heating mantle and keep the temperature for 6 hours, cool to room temperature, and then use Rinse with deionized water; the above washing process is carried out in a fully enclosed state. After washing until the conductivity is less than 50us / cm, it is qualified when the element ratio of Ba / (Ti+Zr) is between 0.995-1.005 through XRF detection. , dried and pulverized after passing the test to obtain barium zirconate titanate powder.

Embodiment 2

[0023] Embodiment 2: prepare BaTi 0.82 Zr 0.18 o 3 Use a graduated cylinder to measure 0.328 liters of 2.5mol / L titanium tetrachloride solution, 0.06 liters of 3.0mol / L zirconium oxychloride and 1.5 liters of 0.8mol / L barium chloride solution in the container, and add 3.11 liters of deionized water to stir until the mixture is uniform; then pour the above mixed solution into the normal pressure reaction kettle, start stirring, and add 460g of sodium hydroxide solid to it, heat up to 100°C with an electric heating mantle and keep the temperature for 2 hours, cool to room temperature, and then use Rinse with deionized water. The above washing process is carried out in a fully enclosed state. After washing until the conductivity is less than 50us / cm, send it to XRF for inspection. When the Ba / (Ti+Zr) element ratio is between 0.995-1.005, it is qualified , dried and pulverized after passing the test to obtain barium zirconate titanate powder.

Embodiment 3

[0024] Embodiment 3: prepare BaTi 0.82 Zr 0.18 o 3 ; Measure 0.16 liters of 5.0mol / L titanium tetrachloride solution, 0.1 liters of 2.0mol / L zirconium oxychloride and 1 liter of 1.1mol / L barium chloride solution in a container, and add 0.41 liters of deionized water Stir until evenly mixed; then pour the above mixed solution into a normal-pressure reactor, start stirring, and add 325g of sodium hydroxide solid to it, heat up to 90°C with an electric heating mantle and keep the temperature for 4 hours, then cool to room temperature, and then Rinse with deionized water. The above washing process is carried out in a fully enclosed state. After washing until the conductivity is less than 50us / cm, send it to XRF for inspection. When the element ratio of Ba / (Ti+Zr) is between 0.995-1.005, the If it is qualified, it is dried and pulverized to obtain barium zirconate titanate powder.

[0025] Analysis of the barium zirconate titanate dry powders in the above-mentioned examples 1 an...

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Abstract

Disclosed is a normal-pressure hydrothermal preparation method for barium zirconate titanate powder. Pure titanium tetrachloride is used as the source of titanium; zirconia oxygen dichlorohydrate is used as the source for zirconium; barium chloride is used as the barium source; sodium hydroxide is taken as the reaction agent; in conjunction with technology, the reaction conditions are timely and strictly controlled, thus the reaction speed is greatly accelerated and the sodium chloride and other remnants left after the reaction are easy to be washed to cause less pollution on environment. The reaction of the invention is carried through in normal-pressure and low-temperature environment, thus the various parameters in the reaction process can be easily adjusted and controlled. The barium zirconate titanate powder prepared through the invention has the advantages of integral grains, even granularity distribution, non-reunion, high activity and low cost, which can fully meet the requirements on the high-performance of barium zirconate titanate in the electronic industry.

Description

technical field [0001] The invention relates to a preparation method of barium zirconate titanate powder, in particular to a normal-pressure hydrothermal preparation method of barium zirconate titanate powder. Background technique [0002] Electronic ceramics made of barium zirconate titanate powder have good dielectric, piezoelectric, ferroelectric, and pyroelectric effects, and can be used to make large-capacity capacitors, non-volatile ferroelectric memories, piezoelectric drivers, etc., so in The field of microelectronics has great application prospects. The existing methods for preparing barium zirconate titanate powder mainly include solid-phase method and sol-gel method. The solid phase method uses BaCO 3 、TiO 2 , ZrO 2 Mixed in proportion and calcined at high temperature (1280°C-1300°C), this method requires high synthesis equipment, and it is difficult to control the uniformity of raw materials during production; and the prepared powder has low purity, large par...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/622C04B35/468C04B35/49
Inventor 赵中友黄敏杨锋林贡王敏
Owner 仙桃市中星电子材料有限公司
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