Preparation method of barium-calcium carbonate and potassium-sodium niobate alternative spin-coating lead-free piezoelectric thick film

A potassium sodium niobate, lead-free piezoelectric technology is applied in the field of chemistry, which can solve the problems that restrict the practical development of KNN lead-free piezoelectric films, it is difficult to obtain a dense surface film, and it is difficult to obtain a saturated hysteresis loop. Achieve the effect of promoting industrial practicality, making up for the porous non-dense, and reducing leakage current.

Inactive Publication Date: 2013-08-28
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the temperature of pure BCT lead-free piezoelectric ceramic film exceeds 120°C, its ferroelectricity disappears, which affects its application in the high-temperature field; During the film and heat treatment process, the alkali metal elements are easy to volatilize, it is difficult to obtain a dense film on the surface, and it is difficult to obtain a saturated hysteresis loop, which also restricts the practical development of KNN lead-free piezoelectric film.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Taking the preparation of 60ml of KNN sol with a concentration of 0.6mol / L and 40ml of BCT sol with a concentration of 1mol / L as an example, the required raw materials are 30g of oxalic acid, 10g of niobium hydroxide, 25g of citric acid, 2.74g of potassium acetate, 3.58g of sodium acetate, 15g of ethylene glycol, 3.68g of PVP, appropriate amount of deionized water, appropriate amount of ammonia water; 10.2g of barium acetate, 9.5g of calcium nitrate tetrahydrate, 30mL of glacial acetic acid, 28ml of ethylene glycol monomethyl ether, 8ml of acetylacetone, tetrabutyl titanate 13.6ml. The specific operation is as follows:

[0031] 1. Preparation of KNN sol:

[0032] 1) Dissolve 30g of oxalic acid in 200ml of deionized water heated with magnetic stirring at 80°C, and dissolve 10g of Nb(OH) 5 Soluble in the solution, react for 0.5h until the solution becomes clear. Then titrate with excess ammonia water to generate Nb(OH) 5 Precipitate until the pH ~ 9 stops, age in a wa...

Embodiment 2

[0044] Taking the preparation of 30ml of 0.6mol / L KNN sol and 40ml of 1mol / L BCT sol as an example, the required raw materials are 15g of oxalic acid, 5g of niobium hydroxide, 12.5g of citric acid, 1.32g of potassium acetate, 1.65g of sodium acetate, Ethylene glycol 7.5g, PVP1.34g, deionized water amount, ammonia water amount; barium acetate 10.5g, glacial acetic acid 29mL, calcium nitrate tetrahydrate 9.3g, ethylene glycol monomethyl ether 28.9ml, acetylacetone 8.2ml, titanic acid Tetrabutyl ester 14ml. The specific operation is as follows:

[0045] 1. Preparation of KNN sol:

[0046] 1) Dissolve 15g of oxalic acid in 100ml of magnetically stirred deionized water heated at 80°C, and dissolve 5g of Nb(OH) 5 Soluble in the solution, react for 0.5h until the solution becomes clear. Then titrate with excess ammonia water to generate Nb(OH) 5 Precipitate until the pH ~ 9 stops, age in a water bath at 80°C for 6 hours, wash and filter repeatedly to obtain the secondary precipit...

Embodiment 3

[0058] Taking the preparation of 120ml of KNN sol with a concentration of 0.6mol / l and 20ml of BCT sol with a concentration of 1mol / l as an example, the required raw materials are 60g of oxalic acid, 20g of niobium hydroxide, 50g of citric acid, 5.81g of potassium acetate, and 9.36g of sodium acetate , ethylene glycol 30g, PVP7.56g, appropriate amount of deionized water, appropriate amount of ammonia water; 5.1 g of barium acetate, 4.7 g of calcium nitrate tetrahydrate, 13 ml of ethylene glycol monomethyl ether, 4 g of acetylacetone, 6.9 g of tetrabutyl titanate, Glacial acetic acid 16ml. The specific operation is as follows:

[0059] 1. Preparation of KNN sol:

[0060] 1) Dissolve 60g of oxalic acid in 400ml of deionized water heated with magnetic stirring at 80°C, and dissolve 20g of Nb(OH) 5 Soluble in the solution, react for 0.5h until the solution becomes clear. Then titrate with excess ammonia water to generate Nb(OH) 5 Precipitate until the pH ~ 9 stops, age in a wa...

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Abstract

The invention discloses a preparation method of a barium-calcium carbonate and potassium-sodium niobate alternative spin-coating lead-free piezoelectric thick film. The preparation method comprises the following steps of: based on a sol-gel process, preparing Bi0.5Ca0.5Ti03(BCT) precursor sol with concentration of 1mol/L by adopting barium acetate (Ba(CH3COO)2), calcium nitrate terahydrate (Ca(NO3)2.4H2O) and tetrabutyl titanate (C16H36O4Ti) as the materials, adopting ethylene glycol monomethyl ether (C3H8O2) and glacial acetic acid (CH3COOH) as solvent, and adopting acetylacetone (C5H8O2) as stabilizing agent; preparing K0.5Na0.5NbO3 (KNN) precursor sol with concentration of 0.6mol/L by adopting ethylene glycol (C2H6O2) as esterifying agent, adopting nitric acid as metal coordination agent and introducing polyvinylpyrrolidone (PVP) as modifying agent; coating the KNN sol on the (Pt/TiO2/Ti/SiO2/Si) substrate, and coating the BCT sol after the thermal treatment; repeating the steps by three times, i.e., carrying out spin-coating for six layers alternatively; and obtaining the KNN-BCT film through annealing treatment. The obtained film is uniform in crystalline grain, compact in arrangement, smooth in surface and free of cracks.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a preparation method of barium calcium titanate and potassium sodium niobate alternately spin-coated lead-free piezoelectric thick film. Background technique [0002] With the miniaturization of electronic components and the development of new electronic components (such as microelectromechanical devices, referred to as MEMS), the research on materials has greatly promoted the transformation from bulk materials to membrane materials. Workers are committed to finding a lead-free ceramic film with superior piezoelectric performance, simple preparation method, and no damage to the environment. with ABO 3 type perovskite structure Ba 0.5 Ca 0.5 TiO 3 (BCT) and K 0.5 Na 0.5 NbO 3 (KNN)-based lead-free piezoelectric ceramic film has the characteristics of high piezoelectric coefficient, small dielectric constant, and high Curie temperature, and is considered to be the most promi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/465C04B35/468C04B35/495C04B35/622
Inventor 张德庆杨秀英郑方圆孟菲冯连振曹茂盛
Owner QIQIHAR UNIVERSITY
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