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A kind of sol-hydrothermal preparation process of tetragonal barium titanate powder

A phase barium titanate and preparation process technology, applied in titanate, chemical instruments and methods, alkaline earth metal titanate and other directions, can solve the problem of high synthesis temperature, achieve low synthesis temperature, high sintering activity and simple operation. Effect

Active Publication Date: 2019-01-15
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method also has a gel process, and the synthesized barium titanate is also a cubic phase and the synthesis temperature is relatively high (200°C).

Method used

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  • A kind of sol-hydrothermal preparation process of tetragonal barium titanate powder
  • A kind of sol-hydrothermal preparation process of tetragonal barium titanate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] According to the molar ratio of titanium source and barium source as 1:1, weigh 11.0005 g of tetrabutyl titanate, add glacial acetic acid and absolute ethanol, and control the volume ratio of tetrabutyl titanate, glacial acetic acid and absolute ethanol to 1 :2:3, magnetically stirred to obtain a tetrabutyl titanate solution; then weighed 7.8971g of barium chloride, added 40mL of distilled water and heated and stirred to completely dissolve to obtain a barium acetate solution; the barium chloride solution was added dropwise to titanate In the tetrabutyl ester solution, heat at 50°C and magnetically stir to obtain a uniform light yellow transparent sol; then, add a mineralizer 4mol / L NaOH solution to the above sol, adjust the pH value to ≥ 13, and continue to stir to obtain a white Barium titanate precursor suspension; add the obtained precursor suspension into a hydrothermal reaction kettle, conduct a hydrothermal reaction at 120°C for 24 hours, and cool the reaction ket...

Embodiment 2

[0037]According to the molar ratio of titanium source and barium source as 1:1, weigh 9.9990 g of tetrabutyl titanate, add glacial acetic acid and absolute ethanol, and control the volume ratio of tetrabutyl titanate, glacial acetic acid and absolute ethanol to 1 :2:3, magnetically stirred to obtain a tetrabutyl titanate solution; then weighed 7.5061g of barium acetate, added 40mL of distilled water and heated and stirred to completely dissolve to obtain a barium acetate solution; the barium acetate solution was added dropwise to tetrabutyl titanate In the ester solution, heat at 50°C and magnetically stir to obtain a uniform light yellow transparent sol; then, add a mineralizer 4mol / L NaOH solution to the above sol, adjust the pH value to ≥ 13, and continue stirring to obtain white titanic acid Barium precursor suspension: Add the obtained precursor suspension into a hydrothermal reaction kettle, conduct a hydrothermal reaction at 120°C for 12 hours, and cool the reaction kett...

Embodiment 3

[0039] According to the molar ratio of titanium source and barium source as 1:1, weigh 10.9004 g of tetrabutyl titanate, add glacial acetic acid and methanol, and control the volume ratio of tetrabutyl titanate, glacial acetic acid and absolute ethanol to 1:2 : 3, magnetically stirred to obtain tetrabutyl titanate solution; then weighed 7.8252g barium chloride, added 40mL distilled water and heated and stirred to completely dissolve to obtain barium chloride solution; barium chloride solution was added dropwise to tetrabutyl titanate In the butyl ester solution, heat at 50°C and magnetically stir to obtain a uniform light yellow transparent sol; then, add a mineralizer 4mol / L NaOH solution to the above sol, adjust the pH value to ≥ 13, and continue to stir to obtain white titanium Barium acid precursor suspension; add the obtained precursor suspension into a hydrothermal reaction kettle, conduct a hydrothermal reaction at 100°C for 48 hours, and cool the reaction kettle to room...

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Abstract

The invention relates to a sol-hydrothermal process preparation technique of a tetragonal barium titanate powder body, which includes steps of mixing tetrabutyl titanate, glacial acetic acid and short-chain alcohol to prepare tetrabutyl titanate solution; slowly adding barium salt in the tetrabutyl titanate solution, and magnetically stirring to form uniform sol; then adjusting pH value of the solution to be not less than 13 by mineralizer, and acquiring hydrothermal process precursor; transferring the precursor to a hydrothermal reaction kettle; and then putting the reaction kettle in a drying tank to perform hydrothermal process; after cooling, washing and drying the powder body, and acquiring the barium titanate powder body. The technique method is simple in operation, controllable in powder particle dimension, high in purity, good in dispersing property, and low in reaction temperature; the powder is a tetragonal structure and free from impure phase. The powder body can be used as a base material of MLCC (multiplayer ceramic chip capacitor) for a super capacitor.

Description

technical field [0001] The invention relates to a tetragonal phase barium titanate nanopowder and a preparation method thereof, in particular to a process for preparing tetragonal phase barium titanate powder by a sol-hydrothermal method, and belongs to the field of preparation of inorganic non-metallic materials. Background technique [0002] Barium titanate has high dielectric constant, low dielectric loss, excellent ferroelectric and piezoelectric properties, and is environmentally friendly. It is widely used as the dielectric of thermistors, ferroelectric components and multilayer ceramic capacitors (MLCC) Materials, known as the pillar of the electronic ceramics industry. In particular, high-purity tetragonal barium titanate powder is the key matrix material for ceramic supercapacitors. Therefore, the preparation method of high-purity tetragonal barium titanate powder has become a research hotspot. [0003] The powder prepared by the traditional solid-state method is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00B82Y40/00H01C7/00H01G4/30H01G4/12
CPCB82Y40/00C01G23/006C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2004/64C01P2006/80H01C7/008H01G4/12H01G4/30Y02E60/13
Inventor 俞鹏飞李辉陈永仁张倩朱非晏朱毅宋婕
Owner CHANGAN UNIV
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