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Preparation method of Ba0.9Ca0.1Ti0.9Zr0.1O3 nano lead-free piezoelectric ceramic

A lead-free piezoelectric and nanotechnology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of uneven grain size, low powder purity, abnormal grain growth, etc. , to achieve uniform distribution of components, lower reaction temperature, and small grain size.

Active Publication Date: 2014-03-19
江苏向宽设计有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In view of the low purity of the powder prepared by this method and the uneven grain size, and the ceramics prepared by the traditional solid-state method are prone to abnormal grain growth in the microwave sintering environment.

Method used

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  • Preparation method of Ba0.9Ca0.1Ti0.9Zr0.1O3 nano lead-free piezoelectric ceramic
  • Preparation method of Ba0.9Ca0.1Ti0.9Zr0.1O3 nano lead-free piezoelectric ceramic
  • Preparation method of Ba0.9Ca0.1Ti0.9Zr0.1O3 nano lead-free piezoelectric ceramic

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) According to the molar ratio of Ba:Ca=9:1, BaCl 2 2H 2 O and CaCl 2 Add it into water to form a mixed solution, stir the mixed solution, and let it stand;

[0025] 2) According to the molar ratio of Ti:Zr:[OH-]=9:1:36, ZrOCl 2 ·8H 2 O solution and TiCl 4 Add it into the KOH solution and keep it warm for 4 hours in a water bath at 60°C to obtain Ti(OH) x and Zr(OH) y mixed gel;

[0026] 3) According to the molar ratio of Ba:Ti=1:1, add the mixed solution prepared in step 1) to Ti(OH) x and Zr(OH) y In the mixed gel, stir to obtain the precursor solution of hydrothermal reaction;

[0027] 4) Move the precursor solution into the inner lining of the hydrothermal kettle, then put the inner lining into the hydrothermal kettle, set the reaction temperature to 60°C, and the reaction time to 20h, wherein, the amount of the precursor solution in the hydrothermal kettle lining is The filling ratio is 70%;

[0028] 5) After the reaction is finished, after the temperat...

Embodiment 2

[0031] 1) According to the molar ratio of Ba:Ca=9:1, BaCl 2 2H 2 O and CaCl 2 Add it into water to form a mixed solution, stir the mixed solution, and let it stand;

[0032] 2) According to the molar ratio of Ti:Zr:[OH-]=9:1:64, ZrOCl 2 ·8H 2 O solution and TiCl 4 Add it into the KOH solution and keep it warm for 3 hours in a water bath at 80°C to obtain Ti(OH) x and Zr(OH) y mixed gel;

[0033] 3) According to the molar ratio of Ba:Ti=1:1, add the mixed solution prepared in step 1) to Ti(OH) x and Zr(OH) y In the mixed gel, stir to obtain the precursor solution of hydrothermal reaction;

[0034] 4) Move the precursor solution into the inner lining of the hydrothermal kettle, then put the inner lining into the hydrothermal kettle, set the reaction temperature to 80°C, and the reaction time to 15h, wherein, the amount of the precursor solution in the hydrothermal kettle lining is The filling ratio is 75%;

[0035] 5) After the reaction is finished, after the temperat...

Embodiment 3

[0038] 1) According to the molar ratio of Ba:Ca=9:1, BaCl 2 2H 2 O and CaCl 2 Add it into water to form a mixed solution, stir the mixed solution, and let it stand;

[0039] 2) According to the molar ratio of Ti:Zr:[OH-]=9:1:90, ZrOCl 2 ·8H 2 O solution and TiCl 4 Add it into the KOH solution, and keep it in a water bath at 100°C for 2 hours to obtain Ti(OH) x and Zr(OH) y mixed gel;

[0040] 3) According to the molar ratio of Ba:Ti=1:1, add the mixed solution prepared in step 1) to Ti(OH) x and Zr(OH) y In the mixed gel, stir to obtain the precursor solution of hydrothermal reaction;

[0041] 4) Move the precursor solution into the inner lining of the hydrothermal kettle, then put the inner lining into the hydrothermal kettle, set the reaction temperature to 100°C, and the reaction time to 10h, wherein, the amount of the precursor solution in the hydrothermal kettle lining is The filling ratio is 80%;

[0042] 5) After the reaction is finished, after the temperatur...

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Abstract

The invention provides a preparation method of Ba0.9Ca0.1Ti0.9Zr0.1O3 nano lead-free piezoelectric ceramic, and the preparation method includes the following steps: adding BaCl2.2H2O and CaCl2 into water to mix into a mixed liquid, stirring the mixed liquid and standing; adding a ZrOCl2[.]8H2O solution and TiCl4 into a KOH solution to obtain Ti (OH) x and Zr (OH) y mixed gel; adding the mixed liquid prepared in the step 1) into the Ti (OH) x and Zr (OH) y mixed gel, and stirring to obtain a hydrothermal reaction precursor solution; transferring the precursor liquid into a hydrothermal kettle for reaction; after the reaction is finished, cooling the hydrothermal kettle to room temperature, taking the hydrothermal kettle out, washing a product in the hydrothermal kettle, and drying to obtain lead-free piezoelectric ceramic powder; and performing microwave sintering on a formed body to obtain the nano lead-free piezoelectric ceramic. According to the preparation method, the sol-gel modification hydrothermal method is used for preparation of the ceramic powder, at the same time a microwave sintering technology is used for sintering to obtain the nano lead-free piezoelectric ceramic with the grain size below 100nm, and the nano lead-free piezoelectric ceramic contains no lead and avoids the harm of lead poisoning on human body and environment.

Description

【Technical field】 [0001] The invention belongs to the field of functional materials, in particular to a Ba 0.9 Ca 0.1 Ti 0.9 Zr 0.1 o 3 A preparation method of nano lead-free piezoelectric ceramics. 【Background technique】 [0002] BaTiO 3 It is the earliest discovered perovskite piezoelectric material, which has been widely used in various electronic material components. However, with the continuous advancement of technology, BaTiO 3 Lower piezoelectric coefficient (d 33 <100) can no longer meet people's growing demand for piezoelectric properties of piezoelectric materials. PZT (PbZrTiO 3 ) has gradually replaced the traditional BaTiO due to its better piezoelectric properties (d33>500) 3 As an emerging piezoelectric material, it is used in the field of electronic materials. In recent years, with the increasing awareness of environmental protection and the harm of lead poisoning to the environment and human health, piezoelectric materials based on PZT have ...

Claims

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Application Information

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IPC IPC(8): C04B35/468C04B35/626C04B35/64B82Y30/00
Inventor 蒲永平孙梓雄
Owner 江苏向宽设计有限公司
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