Wet chemical prepn process of leadless functional barium titanate ceramic film

A lead-free barium zirconate titanate and functional ceramic technology, applied in liquid chemical plating, piezoelectric/electrostrictive device manufacturing/assembly, coating, etc., can solve the problem of long preparation time, cumbersome process and high preparation cost problem, to achieve the effect of long storage period, good stability and good dielectric

Inactive Publication Date: 2002-05-22
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to prepare a high-quality precursor solution, high-purity starting materials are necessary, so before preparing the precursor solution, the raw materials must first be rectified several times to remove impurities and moisture, and then add appropriate Water controls the speed and degree of hydrolysis, so the whole process is cumbersome and takes a long time to prepare
Moreover, the preparation cost is relatively high, and it is not suitable for large-scale preparation of lead-free barium zirconate titanate

Method used

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  • Wet chemical prepn process of leadless functional barium titanate ceramic film
  • Wet chemical prepn process of leadless functional barium titanate ceramic film
  • Wet chemical prepn process of leadless functional barium titanate ceramic film

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Embodiment 1

[0011] Concentration is 0.3 mol / liter metal ion mol concentration ratio in precursor solution is Ba: Zr: Ti=1: 0.05: 0.95 (abbreviated as BZT5), its preparation method is to dissolve barium acetate in glacial acetic acid, control heating to 70 ℃, Stir for 30 minutes to obtain a clear barium acetate solution; add zirconium propoxide and butyl titanate to ethylene glycol methyl ether respectively, add 10% acetylacetone to stabilize the solution, and stir for 10 minutes. Heat to 70°C according to the above ratio, stir for 30 minutes, and filter out impurities with rapid qualitative filter paper to prepare a precursor solution. Choose Pt / Ti / SiO 2 / Si is the substrate, the glue-spinning speed is 3600 rpm, the time is 30 seconds, the pretreatment temperature is 450° C., the time is 10 minutes, and repeated six times. After annealing at 720°C for 10 minutes in an oxygen atmosphere with a heating rate of 100°C / s, a film with a thickness of 490nm was obtained, with perfect crystalliza...

Embodiment 2

[0013] The concentration of the precursor solution is 0.3 mol / liter, the molar concentration ratio of metal ions is Ba:Zr:Ti=1:0.5:0.5 (abbreviated as BZT50 / 50), the speed of plastic rejection is 3800 rpm, and the time is 30 seconds. 420°C, time 10 minutes, repeated six times, and 730°C, rapid annealing treatment under oxygen atmosphere for 10 minutes to obtain a film with a thickness of 300nm, and a BZT50 / 50 film with perfect crystallization and random orientation. All the other are with embodiment 1.

Embodiment 3

[0015] The concentration of the precursor solution is 0.3 mol / liter, the molar concentration ratio of metal ions is Ba:Zr:Ti=1:1:0 (abbreviated as BZ), the glue-spinning speed is 3000 rpm, the time is 30 seconds, and the pretreatment temperature is 420°C each time , time 10 minutes, repeated six times, after rapid annealing at 730°C for 10 minutes under an oxygen atmosphere, a film with a thickness of 600nm was obtained, and a BZ film with perfect crystallization and random orientation was obtained. All the other are with embodiment 1.

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Abstract

The method for preparing barium zirconate titanate (BZT) film belongs to the field of functional ceramic film. Its precursor liquor for preparing BZT is made up by using barium acetate, zirconium propylate and butyl titanate as raw material, using glycol methyl ether as solvent and using acetylacetone and glacial acetic acid as stabilizing agent according to the gran molecular concentration mixing ratio of Ba:Zr:Ti=I:X:1-X (X is greater than or equal to O and is less than or equal to 1), and its concentration is 0.2-0.3M. The above-mentioned precursor is undergone the process of filting, film-forming, whirl coating (its speed is 3000-4000 rpm and time is 30 sec.), pretreating, multiple film-forming, pretreating and film-forming to reach to required thickness, and annealing at 650-750 deg.c so as to obtain the invented product. The lead-free BZT functional film prepared by said ivnention possesses good dielectric feeraelectric and piezoelectric properties.

Description

technical field [0001] The invention relates to a preparation technology of a lead-free barium zirconate titanate (BZT) functional ceramic thin film, more precisely relates to the preparation of a BZT functional ceramic thin film by a wet chemical method, and belongs to the field of functional ceramic thin films. Background technique [0002] Barium zirconate titanate (BZT) functional ceramics have good dielectric, piezoelectric, ferroelectric, pyroelectric and other effects, and have great application prospects in the field of microelectronics, and are ideal for microelectromechanical systems (MEMS). One of the materials, it can be used to make large-capacity capacitors, non-volatile ferroelectric memories, piezoelectric drivers, infrared detectors, etc. It is lead-free material, suitable for environmental protection requirements. With the miniaturization and integration of devices, it is necessary to prepare BZT into functional thin films. There is no patent report on th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/468C23C18/12H01L41/39
Inventor 唐新桂丁爱丽叶扬李国荣殷庆瑞
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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