CN100345765C - Preparation method of cubic phase barium titanate - Google Patents
Preparation method of cubic phase barium titanate Download PDFInfo
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- CN100345765C CN100345765C CNB2006100125407A CN200610012540A CN100345765C CN 100345765 C CN100345765 C CN 100345765C CN B2006100125407 A CNB2006100125407 A CN B2006100125407A CN 200610012540 A CN200610012540 A CN 200610012540A CN 100345765 C CN100345765 C CN 100345765C
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- barium titanate
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Abstract
The present invention relates to a method for preparing single-phase barium titanate nanometer crystal by the hydrothermal method. The present invention is characterized in that barium hydroxide and tetrabutyl titanate are used as raw materials, mixed liquid of n-butanol and water is used as solvent, hydrothermal reaction is carried out in an alkaline medium, and thus, the suspension of the barium titanate crystal is formed, and the single cubic phase barium titanate nanometer crystal is obtained after filtering, washing and drying. The product produced by the production process of the present invention is in a single crystal form. The present invention has the advantages of mild reaction condition, short production period, cyclic use of waste water in the whole process, and no discharge of industrial production.
Description
Technical field
The present invention relates to the compound of titanium, specifically belonging to a kind of is raw material with hydrated barta and tetrabutyl titanate, in alkaline medium with the method for Hydrothermal Preparation barium titanate nano crystalline substance.
Background technology
Barium titanate has higher dielectric constant, good ferroelectric, piezoelectricity, withstand voltage and insulating property, is the key material of environmental harmony type piezoelectricity ferro pottery in electronic industry, the fine ceramics industry.
Along with the electronic ceramics industrial expansion, the demand of barium titanate will constantly increase, and will be also more and more higher to its specification of quality, and single-phase by preparing, high-purity, superfine powdery material is the main path that improves the electron ceramic material performance.
Usually the method for preparing barium titanate adopts calcination method, oxalate method and sol-gel method more, but prepared barium titanate powder is a mixing crystal formation, and its performance can not show a candle to single-phase barium titanate.
The existing report of hydrothermal method synthesizing submicron barium titanate particles.As CN1126717C is hydrous titanium oxide gel and the Ba (OH) that will melt
28H
2O mixes, and makes barium titanate powder under 200 ℃ temperature of reaction condition.There is defective in this method: (1) prepared product reduces the performance of product for mixing crystal formation; (2) used titanium source is a titanium oxide, needs earlier to obtain through the compound hydrolysis of titanium, thereby makes reaction process complicated, the cycle lengthening.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of cubic phase barium titanate, this method not only can obtain single cubic phase nanocrystalline barium titanate barium, and temperature of reaction is low, and technical process is short.
The preparation method of a kind of cubic phase barium titanate provided by the invention is as the titanium source, with Ba (OH) with tetrabutyl titanate
28H
2O is as the barium source, is solvent with the mixed solution of propyl carbinol and water, makes single cubic phase barium titanate through hydrothermal method.Its concrete grammar comprises the steps:
(1) in molar ratio with Ba (OH)
28H
2O: KOH: Ti (OC
4H
9)
4=0.26: successively add in the solvent by propyl carbinol and water by volume 1: 1～3 formed at 1.00: 0.256, stir after 0.5～1 hour, inject water heating kettle;
(2) with the water heating kettle heat temperature raising, make temperature of reaction reach 150 ℃～200 ℃ after, constant temperature 8～12 hours;
(3), obtain the purpose product with reacting liquid filtering, washing and drying.Filtrate is used repeatedly as this preparation method's solvent.
Propyl carbinol and water volume ratio are preferably 1: 2 in the described step (1).
Temperature of reaction is preferably 150 ℃～180 ℃, constant temperature 8～10 hours in the step (2).
Compare with the prior art hydrothermal method, the preparation method of cubic phase barium titanate of the present invention not only can obtain single cubic phase nanocrystalline barium titanate barium, and temperature of reaction is low, and technical process is short.The propyl carbinol that preparation process produced reuse had repeatedly in addition both met energy-conservation requirement, again compliance with environmental protection requirements.
Description of drawings
Embodiment
With three kinds of materials Ba (OH) in molar ratio
28H
2O: KOH: Ti (OC
4H
9)
4=0.26: (be Ba (OH) at 1.00: 0.256
28H
2O 8.2 grams, KOH 5.6 grams, Ti (OC
4H
9)
48.7ml) add by propyl carbinol and pure water volume ratio successively to be in the solvent of being formed at 1: 2, to stir after 0.5 hour, it is injected water heating kettle; In 180 ℃ of following isothermal reactions 10 hours; Mixed solution is poured out, filtered, wash and drying, obtain the barium titanate nano crystalline substance.
Embodiment 2
With three kinds of materials Ba (OH) in molar ratio
28H
2O: KOH: Ti (OC
4H
9)
4=0.26: (be Ba (OH) at 1.00: 0.256
28H
2O 8.3 grams, KOH 5.7 grams, Ti (OC
4H
9)
48.8ml) add by propyl carbinol and pure water volume ratio successively to be in the solvent of being formed at 1: 2, to stir after 1 hour, it is injected water heating kettle; In 150 ℃ of following isothermal reactions 8 hours; Mixed solution is poured out, filtered, wash and drying, obtain the barium titanate nano crystalline substance.
The barium titanate sample that is used for X-ray diffraction (XRD) analysis makes by dry, grinding.Phase purity XRD analysis adopts Japanese D/Max-IIIBX x ray diffractometer x of science to carry out under 20～50 degree, 2 θ.
The crystal spectrogram of above-mentioned two embodiment products is identical.As shown in Figure 1, product cubic phase barium titanate crystalline X-ray diffracting spectrum figure of the present invention.(110), (111), (200) peak substantially all are unimodal as we can see from the figure, and do not have impurity peaks basically.
Claims (3)
1, a kind of preparation method of cubic phase barium titanate is characterized in that comprising the steps:
(1) in molar ratio with Ba (OH)
28H
2O: KOH: Ti (OC
4H
9)
4=0.26: successively add in the solvent by propyl carbinol and water by volume 1: 1～3 formed at 1.00: 0.256, stir after 0.5～1 hour, inject water heating kettle;
(2) with water heating kettle heating, make temperature of reaction reach 150 ℃～200 ℃ after, constant temperature 8～12 hours;
(3), obtain the purpose product with reacting liquid filtering, washing and drying.
According to the preparation method of the described a kind of cubic phase barium titanate of claim 1, it is characterized in that 2, propyl carbinol and water volume ratio are 1: 2 in the described step (1).
According to the preparation method of the described a kind of cubic phase barium titanate of claim 1, it is characterized in that 3, temperature of reaction is 150 ℃～180 ℃ in the described step (2), constant temperature 8～10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100125407A CN100345765C (en) | 2006-03-29 | 2006-03-29 | Preparation method of cubic phase barium titanate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100125407A CN100345765C (en) | 2006-03-29 | 2006-03-29 | Preparation method of cubic phase barium titanate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1830806A CN1830806A (en) | 2006-09-13 |
| CN100345765C true CN100345765C (en) | 2007-10-31 |
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|---|---|---|---|
| CNB2006100125407A Expired - Fee Related CN100345765C (en) | 2006-03-29 | 2006-03-29 | Preparation method of cubic phase barium titanate |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449512B (en) * | 2013-08-29 | 2015-02-25 | 陕西师范大学 | Method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of microwave hydrothermal method |
| CN109225193B (en) * | 2018-09-21 | 2021-03-30 | 陕西师范大学 | Semiconductor photocatalytic material Na0.23TiO2Preparation method of (1) |
| CN113499765B (en) * | 2021-07-05 | 2024-02-06 | 南方科技大学 | Composite piezoelectric photocatalyst capable of being coated on surface of magnetic micro-robot and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6129903A (en) * | 1998-07-01 | 2000-10-10 | Cabot Corportion | Hydrothermal process for making barium titanate powders |
| JP2002060219A (en) * | 2000-08-11 | 2002-02-26 | Murata Mfg Co Ltd | Barium titanate fine powder, calcium-modified barium titanate fine powder and its manufacturing method |
| CN1418819A (en) * | 2002-12-23 | 2003-05-21 | 童忠良 | Tech for prepn. of nano barium titanate powder |
| CN1715243A (en) * | 2004-06-30 | 2006-01-04 | 北京化工大学 | Process for preparing tetra phase barium titanate powder |
-
2006
- 2006-03-29 CN CNB2006100125407A patent/CN100345765C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6129903A (en) * | 1998-07-01 | 2000-10-10 | Cabot Corportion | Hydrothermal process for making barium titanate powders |
| JP2002060219A (en) * | 2000-08-11 | 2002-02-26 | Murata Mfg Co Ltd | Barium titanate fine powder, calcium-modified barium titanate fine powder and its manufacturing method |
| CN1418819A (en) * | 2002-12-23 | 2003-05-21 | 童忠良 | Tech for prepn. of nano barium titanate powder |
| CN1715243A (en) * | 2004-06-30 | 2006-01-04 | 北京化工大学 | Process for preparing tetra phase barium titanate powder |
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| CN1830806A (en) | 2006-09-13 |
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Granted publication date: 20071031 Termination date: 20100329 |