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Preparation method of manganese-doped potassium-sodium-niobate-base lead-free piezoelectric film

A potassium-sodium niobate-based, lead-free piezoelectric technology is applied in the field of preparation of manganese-doped potassium-sodium niobate-based lead-free piezoelectric films, which can solve the problems that restrict the practical development of KNN lead-free piezoelectric films and the difficulty in obtaining surface The problems of dense film and easy volatilization of alkali metal elements can achieve the effect of improved compactness, easy control and easy hydrolysis

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

with ABO 3 K type perovskite structure 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 promising lead-free piezoelectric material system to replace PZT piezoelectric ceramic materials. In the process of preparing pure KNN lead-free piezoelectric ceramic film, due to the characteristics of easy volatilization of alkali metal elements in the process of film formation and heat treatment, it is difficult to obtain a thin film with a dense surface, and it is difficult to obtain a saturated hysteresis loop. Practical Development of Lead Piezoelectric Thin Film

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Taking the preparation of 200ml of 0.5mol / 1KNN sol as an example, the required raw materials are 0.38g of manganese acetate, 60g of oxalic acid, 20g of niobium hydroxide, 55g of citric acid, 5.86g of potassium acetate, 10.78g of sodium acetate, 29g of ethylene glycol, PVP4.36g, appropriate amount of deionized water, appropriate amount of ammonia water; the specific operation is as follows:

[0023] 1. Preparation of KNN sol

[0024] 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 1h until the solution becomes clear. Then titrate with excess ammonia water to generate Nb(OH) 5 Precipitate until pH 8-9 stops, age in a water bath at 80°C for 5 hours, wash and filter repeatedly to obtain secondary precipitated Nb(OH) 5 precipitation;

[0025] 2) Dissolve 55g of citric acid in 400ml of magnetically stirred deionized water heated at 80°C, and dissolve the newly...

Embodiment 2

[0032] Taking the preparation of 100ml of 0.5mol / 1KNN sol as an example, the required raw materials are 0.19g of manganese acetate, 30g of oxalic acid, 10g of niobium hydroxide, 27.5g of citric acid, 2.93g of potassium acetate, 5.39g of sodium acetate, and 14.5g of ethylene glycol. g, PVP2.18g, appropriate amount of deionized water, appropriate amount of ammonia water; the specific operation is as follows:

[0033] 1. Preparation of manganese-doped potassium sodium niobate sol

[0034] 1) Dissolve 30g of oxalic acid in 400ml of deionized water heated with magnetic stirring at 80°C, and dissolve 10g of Nb(OH) 5 Soluble in the solution, react for 1h until the solution becomes clear. Then titrate with excess ammonia water to generate Nb(OH)5 Precipitate until pH 8-9 stops, age in a water bath at 80°C for 5 hours, wash and filter repeatedly to obtain secondary precipitated Nb(OH) 5 precipitation;

[0035] 2) Dissolve 27.5g of citric acid in 400ml of deionized water heated with ...

Embodiment 3

[0042] Taking the preparation of 50ml of 0.5mol / 1KNN sol as an example, the required raw materials are 0.095g of manganese acetate, 15g of oxalic acid, 5g of niobium hydroxide, 13.75g of citric acid, 1.465g of potassium acetate, 2.695g of sodium acetate, and 7.25g of ethylene glycol. g, PVP1.09g, appropriate amount of deionized water, appropriate amount of ammonia water; the specific operation is as follows:

[0043] 1. Preparation of KNN sol

[0044] 1) Dissolve 15g of oxalic acid in 400ml of deionized water heated with magnetic stirring at 80°C, and dissolve 5g of Nb(OH) 5 Soluble in the solution, react for 1h until the solution becomes clear. Then titrate with excess ammonia water to generate Nb(OH) 5 Precipitate until pH 8-9 stops, age in a water bath at 80°C for 5 hours, wash and filter repeatedly to obtain secondary precipitated Nb(OH) 5 precipitation;

[0045] 2) Dissolve 13.75g of citric acid in 400ml of deionized water heated with magnetic stirring at 80°C, and di...

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Abstract

The invention discloses a preparation method of a manganese-doped potassium-sodium-niobate-base lead-free piezoelectric film. The invention provides a simple and controllable technique on the basis of a non-alcohol niobium salt sol-gel method. The method comprises the following steps: preparing a stable manganese-doped KNN sol, carrying out spin coating on the KNN sol on a (Pt / TiO2 / Ti / SiO2 / Si) substrate for 30 seconds at the rotation speed of 3200 r / min, drying the wet film at 150 DEG C, and keeping the temperature at 600 DEG C for 10 minutes; repeating the previous step 8 times under the same heat treatment conditions to obtain 8 spin coatings; and carrying out annealing treatment at 700 DEG C for 10 minutes. The final film thickness is 2-4 mu m; and the prepared film has the advantages of favorable compactness and improved drain current property.

Description

technical field [0001] A method for preparing manganese-doped potassium sodium niobate-based lead-free piezoelectric 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 K type perovskite structure 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 promising lead-free piezoelectric material system to replace PZT piezoelectric ceramic materials. In the process of preparing pure KNN lead-free pie...

Claims

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Application Information

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IPC IPC(8): C04B35/495C04B35/622
Inventor 张德庆冯连振杨秀英郑方圆刘纪鹏曹茂盛
Owner QIQIHAR UNIVERSITY
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