Preparation method of submicron-level relaxor ferroelectric

A ferroelectric, sub-micron technology, applied in the field of preparation of sub-micron relaxor ferroelectrics, can solve the problems of weakening the electrical properties of ceramics, poor frequency stability, poor temperature stability, etc., and achieve excellent relaxor ferroelectric behavior , high density, fine and uniform grain size

Active Publication Date: 2014-10-22
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional electronic ceramic materials often have defects such as poor temperature stability or poor frequency stability, and relaxor ferroelectrics just make up for this loophole
[0004] The traditional PMN-PT system relaxor ferroelectric has limited its application fields due to lead poisoning to the human body and the environment, while the frequency dispersion range of the new BaSrTiO3 system relaxor ferroelectric is around -50°C, and it cannot obtain good vibration at room temperature. application
Since the BCTZ system is a well-known lead-free piezoelectric system, its grain size is often very large, reaching several microns or even more than ten microns. Such a large grain size weakens the electrical properties of ceramics.

Method used

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  • Preparation method of submicron-level relaxor ferroelectric
  • Preparation method of submicron-level relaxor ferroelectric
  • Preparation method of submicron-level relaxor ferroelectric

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1) First weigh BaCl according to the molar ratio of 0.9:0.1:0.03 2 2H 2 O, CaCl 2 and Bi(NO 3 ) 3 and respectively configured into solutions, mixed and left to stand to obtain a mixed solution A;

[0039] 2) Press Ca 2+ with Ti 4+ The molar ratio is 0.1:1, the TiCl 4 Add dropwise to mixed solution A and stir to make mixed solution B. At the same time, adjust the pH value of mixed solution B to be greater than 14 by NaOH, and stir until mixed solution B becomes white and viscous to obtain Ba 0.9 Ca 0.1 TiO 3 -0.03Bi powder precursor;

[0040] 3) the prepared Ba 0.9 Ca 0.1 TiO 3 Pour the -0.03Bi powder precursor into a hydrothermal kettle with a filling ratio of 70%, and keep it in a hydrothermal environment at 240°C for 12h to obtain Ba 0.9 Ca 0.1 TiO 3 -0.03Bi powder, the powder is washed and precipitated, and finally the green body is formed;

[0041] 4) Microwave sintering the formed green body, the sintering temperature is 1200°C, the holding time is ...

Embodiment 2

[0043] 1) First weigh BaCl according to the molar ratio of 0.9:0.1:0.03:0.03 2 2H 2 O, CaCl 2 ZrOCl 2 ·8H 2 O and Bi(NO 3 ) 3 and respectively configured into solutions, mixed and left to stand to obtain a mixed solution A;

[0044] 2) Press Ca 2+ with Ti 4+ The molar ratio is 0.1:0.97, the TiCl 4 Add dropwise to mixed solution A and stir to make mixed solution B. At the same time, adjust the pH value of mixed solution B to be greater than 14 by NaOH, and stir until mixed solution B becomes white and viscous to obtain Ba 0.9 Ca 0.1 Ti 0.97 Zr 0.03 o 3 -0.03Bi powder precursor;

[0045] 3) the prepared Ba 0.9 Ca 0.1 Ti 0.97 Zr 0.03 o 3 Pour the -0.03Bi powder precursor into a hydrothermal kettle with a filling ratio of 70%, and keep it in a hydrothermal environment at 180°C for 12h to obtain Ba 0.9 Ca 0.1 Ti 0.97 Zr 0.03 o 3 -0.03Bi powder, the powder is washed and precipitated, and finally the green body is formed;

[0046] 4) Microwave sintering the fo...

Embodiment 3

[0048] 1) First weigh BaCl according to the molar ratio of 0.9:0.1:0.06:0.03 2 2H 2 O, CaCl 2 ZrOCl 2 ·8H 2 O and Bi(NO 3 ) 3 and respectively configured into solutions, mixed and left to stand to obtain a mixed solution A;

[0049] 2) Press Ca 2+ with Ti 4+ The molar ratio is 0.1:0.94, the TiCl 4 Add dropwise to mixed solution A and stir to make mixed solution B. At the same time, adjust the pH value of mixed solution B to be greater than 14 by NaOH, and stir until mixed solution B becomes white and viscous to obtain Ba 0.9 Ca 0.1 Ti 0.94 Zr 0.06 o 3 -0.03Bi powder precursor;

[0050] 3) the prepared Ba 0.9 Ca 0.1 Ti 0.94 Zr 0.06 o3 Pour the -0.03Bi powder precursor into a hydrothermal kettle with a filling ratio of 80%, and keep it in a hydrothermal environment at 150°C for 15h to obtain Ba 0.9 Ca 0.1 Ti 0.94 Zr 0.06 o 3 -0.03Bi powder, the powder is washed and precipitated, and finally the green body is formed;

[0051] 4) Microwave sintering the form...

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Abstract

The invention relates to a preparation method of a submicron-level relaxor ferroelectric. The preparation method comprises the following steps of: firstly preparing water-soluble barium source, calcium source, zirconium source, bismuth source and titanium source into a mixed solution according to the stoichiometric ratio of the relaxor ferroelectric to be prepared; regulating the mixed solution to alkality to prepare a powdery precursor of the relaxor ferroelectric; then carrying out hydrothermal reaction on the powdery precursor to prepare powder of the relaxor ferroelectric; and carrying out blank forming and sintering to the powder to obtain the submicron-level relaxor ferroelectric. According to the preparation method, the submicron-level relaxor ferroelectric which is high in purity, high in compactness and small and uniform in grain size can be obtained within a short time through the combination of a hydrothermal method and a microwave sintering technology; the electric property and microstructure of ceramic are changed within a wide range by changing the quantity of doped elements, and the behavior of the relaxor ferroelectric of the ceramic is optimized, and therefore the submicron-level relaxor ferroelectric can be widely applied to the field of electronic ceramics.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a method for preparing a submicron-level relaxor ferroelectric. Background technique [0002] BaTiO 3 It is the earliest discovered perovskite dielectric material, which exhibits good ferroelectric behavior at room temperature. It was once known as the pillar of the electronic ceramic industry and is widely used in various electronic material components. Relaxor ferroelectrics have been valued by more and more material researchers due to their superior characteristics over traditional ferroelectrics (such as wide Curie temperature region and high temperature hysteresis loop, etc.), among which BaTiO 3 The relaxation ferroelectric based on the base is one of the biggest research hotspots. It is well known that Ba 1-x Ca x Ti 1-x Zr y o 3 The ceramic system is a good lead-free piezoelectric material, but it also has the properties of a relaxor ferroelectric in addition to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/49C04B35/622
Inventor 蒲永平孙梓雄
Owner SHAANXI UNIV OF SCI & TECH
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