Process for preparing stable lead zirconate-titanate sol

A lead zirconate titanate, stable technology, applied in the field of preparation of lead zirconate titanate stable sol, can solve the problems of high cost of zirconium alkoxide, complicated experimental operation, etc., and achieve the effect of simple equipment, convenient experimental operation and less time consumption

Inactive Publication Date: 2003-10-29
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1985, K.D.Budd et al. used zirconium propoxide as the starting material to prepare PZT stable sol in Br.Ceram.Proc, volume 36, page 107. Due to the high cost of zirconium alkoxide, domestic scholars tried to use zirconium inorganic Salt was introduced into zirconium. In 1999, Wang Xicheng et al. used zirconium oxynitrate as the starting material to introduce zirconium into a stable sol of PZT on page 16 of the second phase of Material Engineering in 1999. However, in the preparation process, sufficient distillation at 124°C was required to obtain clear Transparent PZT sol, the experimental operation is more complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] The raw material is Pb(Ac) 2 ·3H 2 O(A.R), ZrO(NO 3 ) 2 2H 2 O(A.R), Ti(OC 4 h 9 ) 4 (C.P). Weigh 0.005molPb(Ac) 2 ·3H 2 O and 0.0026molZrO(NO 3 ) 2 2H 2 O, mix two solid reagents and dissolve in a small amount of H 2 In O, let it stand in a sealed state for 3.36h, so that it can be completely dissolved to form a supersaturated solution. Measure 0.0024mol of Ti(OC 4 h 9 ) 4 Soluble in ethylene glycol monomethyl ether (CH 3 OCH 2 CH 2 OH) solvent, wherein the solvent H 2 O:CH 3 OCH 2 CH 2 OH=1:11, after complete dissolution, 0.40ml of acetylacetone was added dropwise to the solution as a stabilizer. Add the above-mentioned Pb and Zr aqueous solutions dropwise to the Ti organic solution under stirring, stop stirring after the dropwise addition, filter, seal and let stand. A beam of white light passing through the obtained liquid can produce obvious Tyndall phenomenon, which proves that Pb(Zr 0.52 Ti 0.48 )O 3 stable sol.

Embodiment 2

[0011] The raw material is Pb(Ac) 2 ·3H 2 O(A.R), ZrO(NO 3 ) 2 2H 2 O(A.R), Ti(OC 4 h 9 ) 4 (C.P). Weigh 0.005molPb(Ac) 2 ·3H 2 O and 0.0025molZrO(NO 3 ) 2 2H 2 O, mix two solid reagents and dissolve in a small amount of H 2 In O, let it stand in a sealed state for 3.15h, so that it can be completely dissolved to form a supersaturated solution. Measure 0.0025mol of Ti(OC 4 h 9 ) 4 Soluble in isopropanol (CH 3 CHOHCH 3 ) solvent, wherein the solvent H 2 O:CH 3 CHOHCH 3 =1:12.5, after the solution is completely dissolved, 0.50ml of acetylacetone is added dropwise to the solution as a stabilizer. Add the above-mentioned Pb and Zr aqueous solutions dropwise to the Ti organic solution under stirring, stop stirring after the dropwise addition, filter, seal and let stand. A beam of white light passing through the obtained liquid can produce obvious Tyndall phenomenon, which proves that Pb(Zr 0.50 Ti 0.50 )O 3 stable sol.

Embodiment 3

[0013] The raw material is Pb(Ac) 2 ·3H 2 O(A.R), ZrO(NO 3 ) 2 2H 2 O(A.R), Ti(OC 4 h 9 ) 4 (C.P). Weigh 0.005molPb(Ac) 2 ·3H 2 O and 0.00265molZrO(NO 3 ) 2 2H 2 O, mix two solid reagents and dissolve in a small amount of H 2 In O, let it stand in a sealed state for 3.38h to make it dissolve completely to form a supersaturated solution. Measure 0.00235mol of Ti(OC 4 h 9 ) 4 Soluble in ethanol (CH 3 CH 2 OH) solvent, wherein the solvent H 2 O:CH 3 CH 2 OH=1:15.9, after complete dissolution, 0.55ml of acetylacetone was added dropwise to the solution as a stabilizer. Add the above-mentioned Pb and Zr aqueous solutions dropwise to the Ti organic solution under stirring, stop stirring after the dropwise addition, filter, seal and let stand. A beam of white light passing through the obtained liquid can produce obvious Tyndall phenomenon, which proves that Pb(Zr 0.53 Ti 0.47 )O 3 stable sol.

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PUM

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Abstract

A process for preparing the stable sol of lead zirconate titanate from Ti(OC4H9)4 or Ti(OCH(CH3)2)4, Zr(NO3)4 or ZrO(NO3)2.2H2O and Pb(Ac)2.3H3O or Pb(NO3)2 through dissolving the inorganic salts of Pb and Zr in distilled water to obtain over-saturated solution, stirring while adding dropwise it to the organic solution of titanium alkoxide to which acetylacetone as stabilizer has been added, and stopping stirring. Its advantages are simple equipment and high stability and quality.

Description

technical field [0001] The invention belongs to a preparation method of lead zirconate titanate stable sol. Background technique [0002] The rapid development of the electronics industry has made large-scale planar integration technology increasingly demanding compatibility. Ferroelectric thin films, especially lead zirconate titanate Pb(Zr) with high dielectric properties, piezoelectricity and excellent ferroelectricity x Ti 1-x )O 3 (PZT) solid solution system has attracted people's attention. Among the commonly used preparation methods of PZT ferroelectric thin films, the sol-gel method has the characteristics of good uniformity, easy control of stoichiometric ratio, low heat treatment process, large film forming area, and simple equipment. , are widely used in the preparation process of ferroelectric thin films. [0003] The quality of the sol directly affects the film-forming performance, so how to obtain the sol suitable for the coating needs is the primary proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00C04B35/49C04B35/491C04B35/624
Inventor 刘雅信郭宏霞郝先李莹
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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