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Preparation of lead zirconate titanate nanometer powder

A lead zirconate titanate and nano-powder technology is applied in the field of preparation of lead zirconate titanate nano-powder, can solve the problems of long experimental operation time, complicated sintering process, long dry gel time, etc., and achieves simple sintering process, Reasonable preparation process and short time effect

Inactive Publication Date: 2005-05-11
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, in the invention patent "Preparation Method of Lead Zirconate Titanate Stable Sol" (Application No.: 03131070.2) by Liu Yaxin and others, a stable sol was prepared with zirconium nitrate or zirconyl nitrate as the source of zirconium, but ethylene glycol was used in the preparation Monomethyl ether is a solvent, and the method of adding lead salt and zirconium salt aqueous solution to the titanium salt ethylene glycol monomethyl ether solution added with acetylacetone stabilizer is adopted at the same time, which makes the preparation cost higher, and the experimental operation is more complicated. longer time
Guo Hongxia et al. prepared nano-Pb(Zr 0.52 Ti 0.48 )O 3 "In the article ("Applied Chemistry" December, 2002, the 12th phase of volume 19, page 1166), the sol prepared by the above method is sintered to obtain a nanopowder, but it takes a long time to prepare the xerogel and the sintering process is difficult. complex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] To prepare 14.00 g of lead zirconate titanate Pb(Zr 0.52 Ti 0.48 o 3 ) nano powder as an example, the required raw material is butyl titanate Ti(O-C 4 h 9 ) 4 11.70ml, zirconium nitrate Zr (NO 3 ) 4.5 h 2 O 15.75 g, lead acetate Pb(CH 3 COO) 2.3 h 2 O 32.00 g, ethylene glycol C 2 h 6 o 2 Appropriate amount. The specific operation is as follows:

[0017] 1. At 60°C, dissolve 15.75 grams of zirconium nitrate in 35 ml of ethylene glycol, 11.70 ml of butyl titanate in 140 ml of ethylene glycol, and 32.00 grams of lead acetate in 80 ml of ethylene glycol.

[0018] 2. Mix the ethylene glycol solution of zirconium nitrate and the ethylene glycol solution of butyl titanate, and reflux at 60° C. for 30 minutes. Add ethylene glycol solution of lead acetate dropwise to the system, if white flocs appear, use 65% nitric acid HNO 3 Adjust the pH value to 2, and reflux at 60°C for 3 hours until the mixed solution is transparent to obtain a colorless and stable sol.

...

Embodiment 2

[0022] To prepare 6.65 g of lead zirconate titanate Pb(Zr 0.60 Ti 0.48 o 3 ) nano powder as an example, the required raw material is butyl titanate Ti(O-C 4 h 9 ) 4 4.97ml, zirconium nitrate Zr (NO 3 ) 4.5 h 2 O 9.47 g, lead acetate Pb(CH 3 COO) 2.3 h 2 O 13.93 g, ethylene glycol C 2 h 6 o 2 Appropriate amount. The specific operation is as follows:

[0023] 1. Dissolve 9.47g of zirconium nitrate in 21ml of ethylene glycol, 4.97ml of butyl titanate in 59ml of ethylene glycol, and 13.93g of lead acetate in 34ml of ethylene glycol at 65°C.

[0024] 2. Mix the ethylene glycol solution of zirconium nitrate and the ethylene glycol solution of butyl titanate, and reflux at 65° C. for 30 minutes. Add ethylene glycol solution of lead acetate dropwise to the system, if white flocs appear, use 65% nitric acid HNO 3 Adjust the pH value to 2, and reflux at 65°C for 3 hours until the mixed solution is transparent, and a colorless and stable sol is obtained.

[0025] 3. The...

Embodiment 3

[0028] To prepare 5.43 g of lead zirconate titanate Pb(Zr 0.75 Ti 0.25 o 3 ) nano powder as an example, the required raw material is butyl titanate Ti(O-C 4 h 9 ) 4 2.49ml, zirconium nitrate Zr (NO 3 ) 4.5 h2 O 9.47 g, lead acetate Pb(CH 3 COO) 2.3 h 2 O 11.14 g, ethylene glycol C 2 h 6 o 2 Appropriate amount. The specific operation is as follows:

[0029] 1. Dissolve 9.47g of zirconium nitrate in 21ml of ethylene glycol, 2.49ml of butyl titanate in 30ml of ethylene glycol, and 11.14g of lead acetate in 27ml of ethylene glycol at 70°C.

[0030] 2. Mix the ethylene glycol solution of zirconium nitrate and the ethylene glycol solution of butyl titanate, and reflux at 70°C for 30 minutes. Add ethylene glycol solution of lead acetate dropwise to the system, if white flocs appear, use 65% nitric acid HNO 3 Adjust the pH value to 2, reflux at 70°C for 3 hours until the mixed solution is transparent, and a colorless and stable sol is obtained.

[0031] 3. The obtaine...

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PUM

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Abstract

Production for Pb(ZrxTi(1-x)O3) nanometer powder is disclosed. It is carried out by: taking Ti(O-C4H9)4, Zr(NO3)4íñ5H2O, Pb(CH3COO)2íñ3 H2O as raw material, C2H6O2 as solvent, mixing C2H6O2 solution of Zr(NO3)4íñ5H2O with C2H6O2 solution of Ti(O-C4H9)4, back-flowing at temperature 60-70deg.C for 30mins, dripping C2H6O2 solution of Pb(CH3COO)2.3 H2O into system, back-flowing at 60-70deg.C for 3hrs, thermostatic drying for 10hrs in 100deg.C fan drying case, and dried gel powder sintering at temperature 400deg.C and 600deg.C in crucible to obtain yellow nanometer Pb(ZrxTi(1-x)O3) powder. It costs low and is simple.

Description

technical field [0001] A preparation method of lead zirconate titanate nanopowder. Background technique [0002] Lead zirconate titanate Pb(Zr x Ti (1-x) o 3 ), referred to as PZT material for short, is an ABO with a perovskite phase structure 3 Type piezoelectric ceramic materials, because of their good piezoelectricity, pyroelectricity, dielectricity, photoelectricity, ferroelectricity, easy doping modification, good stability and many other advantages, their application fields are constantly increasing. excavated and developed. In recent years, PZT materials have also attracted the close attention of professionals in China, especially the PZT ceramics composed near the quasi-isomorphic phase boundary point (that is, x=0.52~0.55) are prepared for their high dielectric constant and electromechanical coupling coefficient. By the attention. [0003] There are many preparation methods of PZT materials, the most discussed in China is the sol-gel method (Sol-gel method). ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/491C04B35/624
Inventor 张德庆曹茂盛
Owner HARBIN ENG UNIV
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