Method of preparing Bi3TiNbO9 micro-nano piezoelectricity ferro-electricity powder

A micro-nano, piezoelectric technology

Inactive Publication Date: 2008-01-09
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention prepares Bi for existing high-temperature solid phase method 3 TiNbO 9 Problems existing in the powder, provide a low-temperature preparation of Bi 3 TiNbO 9 The method of micronano piezoelectric ferroelectric powder, the Bi prepared by this method 3 TiNbO 9 The powder particle size distribution is uniform, the purity is high, and the components are mixed at the molecular level. After the thermal annealing process, the controllable growth of the particle size in the nanometer to micrometer range can be realized.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Nb 2 o 5 Dissolve in 40% HF at 80-90°C, then drop NH into it 3 ·H 2 O solution to pH 8.5-9.5, forming white Nb(OH) 5 Precipitate, aging at room temperature for 10 hours, the precipitate was filtered, washed and dissolved in citric acid aqueous solution, citric acid and Nb 2 o 5 The molar ratio of is 8: 1, forms transparent Nb-citric acid solution;

[0014] (2) According to the molar ratio Nb 5+ : Ti 4+ : Bi 3+ :EDTA=1:1:3:3.3 and NH 4 NO 3 : The ratio of citric acid=6:1 will Ti(C 4 h 9 O) 4 , Bi(NO 3 ) 3 ·5H 2 O, EDTA and NH 4 NO 3 Sequentially added to the Nb-citric acid solution prepared in step (1) to form a transparent solution, heated and stirred at 95-105°C to obtain a light yellow precursor gel;

[0015] (3) Sinter the precursor gel at 480°C for 50 minutes to obtain Bi 3 TiNbO 9 Nano powder material.

[0016] (4) will get Bi 3 TiNbO 9 Nanoparticles were annealed at 550°C for 6 hours to obtain Bi 3 TiNbO 9 Powder.

Embodiment 2

[0018] (1) Nb 2 o 5 Dissolve in 40% HF at 80-90°C, then drop NH into it 3 ·H 2 O solution to pH 8.5-9.5, forming white Nb(OH) 5 Precipitate, aging at room temperature for 10 hours, the precipitate was filtered, washed and dissolved in citric acid aqueous solution, citric acid and Nb 2 o 5 The molar ratio of is 12: 1, forms transparent Nb-citric acid solution;

[0019] (2) According to the molar ratio Nb 5+ : Ti 4+ : Bi 3+ :EDTA=1:1:3:3.3 and NH 4 NO 3 : The ratio of citric acid=5:1 will Ti(C 4 h 9 O) 4 , Bi(NO 3 ) 3 ·5H 2 O, EDTA and NH 4 NO 3 Sequentially added to the Nb-citric acid solution prepared in step (1) to form a transparent solution, heated and stirred at 95-105°C to obtain a light yellow precursor gel;

[0020] (3) Sinter the precursor gel at 600°C for 15 minutes to obtain Bi 3 TiNbO 9 Nano powder material.

[0021] (4) will get Bi 3 TiNbO 9 Nanoparticles were annealed at 650°C for 30 hours to obtain Bi with a particle size distribution of 12...

Embodiment 3

[0023] (1) Nb 2 o 5 Dissolve in 40% HF at 80-90°C, then drop NH into it 3 ·H 2 O solution to pH 8.5-9.5, forming white Nb(OH) 5 Precipitate, aging at room temperature for 12 hours, the precipitate was filtered, washed and dissolved in citric acid aqueous solution, citric acid and Nb 2 o 5 The molar ratio of is 16: 1, forms transparent Nb-citric acid solution;

[0024] (2) According to the molar ratio Nb 5+ : Ti 4+ : Bi 3+ :EDTA=1:1:3:3.6 and NH 4NO 3 : The ratio of citric acid=5:1 will Ti(C 4 h 9 O) 4 , Bi(NO 3 ) 3 ·5H 2 O, EDTA and NH 4 NO 3 Sequentially added to the Nb-citric acid solution prepared in step (1) to form a transparent solution, heated and stirred at 95-105°C to obtain a light yellow precursor gel;

[0025] (3) Sinter the precursor gel at 700°C for 10 minutes to obtain Bi 3 TiNbO 9 Nano powder material.

[0026] (4) will get Bi 3 TiNbO 9 Nanoparticles were annealed at 700°C for 40 hours to obtain Bi with a particle size distribution of 200...

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Abstract

This invention relates to a method for low temperature preparation of Bi3TiNb09 nanometer power. The preparation procedures are: (1) niobium pentoxide is dissolved in hydrofluoric acid under 80-90deg.C, then ammonia water is dropped into the solution, regulating the pH value to 8.5-9.5, to obtain precipitate of niobium hydroxide, which, after filtration and washing, is then dissolved in citric acid solution to produce Nb-citric acid solution; (2), tetrabutyl titanate, pentahydrate bismuth nitrate, EDTA and ammonium nitrate are added successively into aboved-mentioned solution, together with heating and agitation to obtain pre-product-gelatin; (3), said gelatin is then sintered to obtain this inventive product. This invention utilizes oxidation-reduction method having advantages of simple process, low reaction temperature, short reaction time, small particle size and even distribution and high-pureness.

Description

technical field [0001] The invention relates to a low-temperature preparation of Bi 3 TiNbO 9 The invention discloses a method for micronano piezoelectric ferroelectric powder, which belongs to the technical field of inorganic material preparation. Background technique [0002] In order to protect the ecological environment and promote the sustainable development of human society, the development and application of lead-free piezoelectric ferroelectric materials has become a hot spot in the field of piezoelectric ferroelectric materials. Among them, bismuth layered structure materials have excellent properties such as high Curie temperature Tc, low dielectric constant, low aging rate, high resistivity, high dielectric breakdown strength and obvious anisotropy of electromechanical coupling coefficient. It is playing an increasingly important role in many high-tech fields such as laser and biology, and has become the most promising lead-free material to replace traditional l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/495
Inventor 吕孟凯马谦周媛媛邱子凤张爱玉
Owner SHANDONG UNIV
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