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Method for preparing lead zirconate titanate 95/5 porous ceramic from tetra-n-butyl titanate

A technology of tetra-n-butyl titanate and lead zirconate titanate is applied in the field of preparation of porous ceramics, which can solve problems such as poor pore size distribution uniformity and achieve the effect of uniform pore size distribution.

Inactive Publication Date: 2010-09-15
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the disadvantages of the poor uniformity of the pore size distribution of the lead zirconate titanate 95 / 5 porous ceramic prepared by the prior art method, the invention provides a method for preparing the lead zirconate titanate 95 / 5 porous ceramic in tetra-n-butyl titanate, Lead zirconate titanate 95 / 5 powder is prepared by one-step pyrolysis process of Pechini method, and the obtained powder does not add pore-forming agent to burn lead zirconate titanate 95 / 5 porous ceramics, which can make lead zirconate titanate 95 / 5 The pore size of porous ceramics is reduced and evenly distributed

Method used

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  • Method for preparing lead zirconate titanate 95/5 porous ceramic from tetra-n-butyl titanate

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Example 1, in the first step, the molar ratio of ethylene glycol: citric acid: lead nitrate: zirconyl nitrate: tetra-n-butyl titanate is 800: 200: 20: 19: 1, and the tetra-n-butyl titanate Add the ester to a container containing ethylene glycol and stir, add citric acid, and stir at 30°C until completely dissolved;

[0015] In the second step, heat up to 70°C, stir and react for 3 hours, then add lead nitrate, stir and dissolve at 70°C, continue stirring for 3 hours, then add zirconium oxynitrate, stir and dissolve at 70°C, and continue stirring for 4 hours ;

[0016] The third step is to raise the temperature to 150°C and keep it warm for 3 hours to promote the completion of the esterification reaction and obtain a gel;

[0017] The fourth step is to calcinate the obtained gel in a static atmosphere at 500°C for 2 hours to obtain lead zirconate titanate 95 / 5 powder;

[0018] In the fifth step, the obtained lead zirconate titanate 95 / 5 powder is molded by cold isostat...

Embodiment 2

[0020] Example 2, in the first step, the molar ratio of ethylene glycol: citric acid: lead nitrate: zirconyl nitrate: tetra-n-butyl titanate is 800: 200: 20: 19: 1, and the tetra-n-butyl titanate Add the ester to a container containing ethylene glycol and stir, add citric acid, and stir at 35°C until completely dissolved;

[0021] In the second step, heat up to 80°C, stir and react for 2 hours, then add lead nitrate, stir to dissolve at 80°C, continue to stir for 2 hours, then add zirconium oxynitrate, stir to dissolve at 80°C, and continue to stir and react for 3.5 hours ;

[0022] The third step is to raise the temperature to 140°C and keep it warm for 2 hours to promote the completion of the esterification reaction and obtain a gel;

[0023] The fourth step is to calcinate the obtained gel in a static atmosphere at 300°C for 6 hours to obtain lead zirconate titanate 95 / 5 powder;

[0024] In the fifth step, the obtained lead zirconate titanate 95 / 5 powder is molded by cold...

Embodiment 3

[0025] Example 3, in the first step, the molar ratio of ethylene glycol: citric acid: lead nitrate: zirconyl nitrate: tetra-n-butyl titanate is 800: 200: 20: 19: 1, and the tetra-n-butyl titanate Add the ester to a container containing ethylene glycol and stir, add citric acid, and stir at 40°C until completely dissolved;

[0026] In the second step, heat up to 85°C, stir and react for 1.5 hours, then add lead nitrate, stir and dissolve at 85°C, continue stirring for 1.5 hours, then add zirconium oxynitrate, stir and dissolve at 85°C, and continue to stir and react for 3 hours ;

[0027] The third step is to raise the temperature to 135°C and keep it warm for 1.5 hours to promote the completion of the esterification reaction and obtain a gel;

[0028] The fourth step is to calcinate the obtained gel in a static atmosphere at 700°C for 4 hours to obtain lead zirconate titanate 95 / 5 powder;

[0029] In the fifth step, the obtained lead zirconate titanate 95 / 5 powder is molded ...

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Abstract

The invention discloses a method for preparing lead zirconate titanate 95 / 5 porous ceramic from tetra-n-butyl titanate, which is used for solving the technical problem of the poor pore size distribution uniformity of lead zirconate titanate 95 / 5 porous ceramic prepared by the preparation method of a traditional technology. The technical scheme comprises the following steps of: mixing ingredients of glycol, citric acid, lead nitrate, zirconyl nitrate and tetra-n-butyl titanate by the mol ratio of 800:200:20:19:1 to prepare a polyester gel, pyrolyzing the polyester gel to obtain a polymer precursor, preparing the polymer precursor into lead zirconate titanate 95 / 5 powder, and carrying out cold isostatic compaction on the lead zirconate titanate 95 / 5 powder to obtain the lead zirconate titanate 95 / 5 porous ceramic. By using the one-step pyrolysis process of the Pechini method to prepare the lead zirconate titanate 95 / 5 powder and firing the obtained powder into the lead zirconate titanate 95 / 5 porous ceramic without adding a pore forming agent, the lead zirconate titanate 95 / 5 porous ceramic prepared by the method has the advantages of small pore diameter, uniform distribution and small particle diameter of ceramic body, and the density of the ceramic body can be controlled by sintering conditions.

Description

technical field [0001] The invention relates to a method for preparing porous ceramics, in particular to a method for preparing lead zirconate titanate 95 / 5 porous ceramics in tetra-n-butyl titanate. Background technique [0002] Literature "T.Zeng1, X.L.Dong, H.L.He, X.F.Chen, and C.H.Yao, Pressure-induced ferroelectric to antiferroelectric phase transformation in porous PZT95 / 5ceramics, phys.stat.sol.(a)204, No.4(2007)" Disclosed is a preparation method of lead zirconate titanate 95 / 5 porous ceramics. The method uses the addition of a pore-forming agent to sinter to obtain lead zirconate titanate 95 / 5 porous ceramics. The prepared lead zirconate titanate 95 / 5 porous ceramics has Spherical and irregular-shaped pores, this lead zirconate titanate 95 / 5 porous ceramic obtained by adding pore-forming agents and sintering, has a pore size of tens to hundreds of microns, and the pore size distribution is uneven. Contents of the invention [0003] In order to overcome the disad...

Claims

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Application Information

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IPC IPC(8): C04B35/491C04B35/624C04B38/00
Inventor 樊慧庆邱少君
Owner NORTHWESTERN POLYTECHNICAL UNIV
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