CN101311377A - Method for preparing barium titanate nanometer powder under room temperature - Google Patents
Method for preparing barium titanate nanometer powder under room temperature Download PDFInfo
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- CN101311377A CN101311377A CNA2008100598842A CN200810059884A CN101311377A CN 101311377 A CN101311377 A CN 101311377A CN A2008100598842 A CNA2008100598842 A CN A2008100598842A CN 200810059884 A CN200810059884 A CN 200810059884A CN 101311377 A CN101311377 A CN 101311377A
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Abstract
The invention discloses a method for preparing a barium titanate nano-powder at room temperature, which comprises the following steps: preparing the oxyhydroxide precipitate of titanium and the deionized aqueous solution of barium acetate as reaction materials, taking ethylene diamine solution or the mixed solution of ethylene diamine and ethanolamine as solvent, adding potassium hydroxide with a suitable viscosity to promote crystallization and obtaining the barium titanate nano-powder with a good dispersion after magnetically stirring for a certain period of time at room temperature. The method has the advantages of exemption from high temperature processing, energy conservation and environment-protection, simple process, easy control, low cost and easy scale production. The prepared product has the advantages of high purity, good dispersion and narrow size distribution which can be adjusted by changing technological parameters. The product has a wide application prospect in the fields of micro-electronic device, EO device, storage material, high dielectric material, gas sensitive material, etc.
Description
Technical field
The present invention relates to a kind of method of preparing barium titanate nanometer powder under room temperature, belong to field of inorganic nonmetallic material.
Background technology
Because the existence of quantum size effect, nano material has the physicochemical property more excellent than block materials, and this also makes the preparation of nano material become the focus of Materials science concern in recent years and research.For pottery, under identical processing condition, if use good dispersity and subglobose nano particle as initial powder, it is finer and close to obtain sintering, and performance is better, the device that homogeneity of product is higher.
Barium titanate is a kind of important electron stupalith, owing to have high-k, low-dielectric loss, pyroelectricity and ferroelectricity, be widely used in making multi-layer ceramic chip electrical condenser (MLCC) and thermistor (PTCR), and on electro-optical device, infrared eye and non-volatility ferroelectric storer, boundless application prospect arranged also.At present, under the megatrend of electronics miniaturization,, just need further to reduce the granularity of barium carbonate powder in order to guarantee the Performance And Reliability of device.For MLCC (multi-layer ceramic chip electrical condenser), in miniaturization, guarantee big capacity and volumetric efficiency especially, just need littler, the more uniform barium carbonate powder of prepared sizes for making device.In addition, granularity is little, the barium carbonate powder of narrow distribution range and good dispersity has good sintering character, just can obtain finer and close stupalith under lower temperature.
The traditional preparation process method of barium carbonate powder is a solid sintering technology, though this method technology is simple, need just can obtain the barium carbonate powder of the good perovskite structure of crystallinity in reaction more than 1200 ℃, and energy consumption is big, and higher to equipment requirements.In addition, the powder purity of solid sintering technology preparation is low, and particle agglomeration is serious, grows up easily, and size is wayward.In order to overcome these shortcomings, some wet chemical methods (comprising sol-gel method, microemulsion method, coprecipitation method (oxalate) method) more and more are used to prepare barium carbonate powder, but these methods also all need the calcination process more than 700 ℃ just can obtain the good barium carbonate powder of crystallinity, although calcining temperature decreases than solid sintering technology, but high-temperature process certainly will cause particulate alligatoring and reunion, is unfavorable for ensuing ceramic post sintering process.Hydrothermal method can be at following preparation crystallinity and the dispersiveness barium carbonate powder preferably all of lower temperature (about 200 ℃), and its particle size range is 0.05～0.4 micron.Yet hydrothermal method is difficult to further reduce particle size again.And the used equipment of hydrothermal method is an airtight autoclave, also has the danger of blast except that the cost height.If can even at room temperature synthesize Barium Titanate nano-powder in lower temperature, will certainly reduce production costs greatly, simplify technology.
Summary of the invention
The objective of the invention is provides a kind of method of preparing barium titanate nanometer powder under room temperature for overcoming the problem that prior art exists.
The preparation method of Barium Titanate nano-powder of the present invention, employing be direct synthesis technique under the room temperature, concrete steps are as follows:
1) tetrabutyl titanate is dissolved in dehydrated alcohol, the Ti in the regulator solution
4+Ionic concn is 0.1～1.0mol/L;
2) under the whipped state, add the ammonia soln of the mass concentration 30% of 1～3ml in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) barium acetate is dissolved in deionized water, forms the barium acetate aqueous solution, Ba in the regulator solution
2+Ionic concentration is 0.5～5.0mol/L;
4) potassium hydroxide is dissolved in deionized water, configuration concentration is the potassium hydroxide aqueous solution of 10～30mol/L;
5) oxyhydroxide precipitation, the barium acetate aqueous solution and the potassium hydroxide aqueous solution with titanium joins in the organic amine solvent, stirred at least 10 minutes, obtain the precursor slurry, wherein the molecular volume mark of the oxyhydroxide of titanium is 0.1～0.2mol/L, the mol ratio of barium and titanium is 1.0～1.1, the molecular volume mark of potassium hydroxide is 0.5～1.0mol/L, and molecular volume fractional volume radix is the cumulative volume of precursor slurry; .
6) the precursor slurry with preparation at room temperature continues to stir 12～72h, allows the products therefrom natural subsidence then, washes repeatedly with diluted acid and deionized water again, filters, and dries, and obtains Barium Titanate nano-powder.
In the preparation process of the present invention, the organic amine solvent of use is the mixing solutions of quadrol or quadrol and thanomin, and wherein the volume of thanomin is no more than 80% of quadrol and thanomin mixing solutions cumulative volume.
In the preparation process of the present invention, the diluted acid that step 6) is used is the dilute acetic acid of volume fraction little 1%.
In the preparation process of the present invention, the purity of said tetrabutyl titanate, barium acetate, potassium hydroxide, dehydrated alcohol, quadrol and thanomin all is not less than chemical pure.
Beneficial effect of the present invention is:
The present invention is solvent with the organic amine, has directly prepared the Barium Titanate nano-powder of purity height, good crystallinity, good dispersity, narrow particle size distribution under room temperature and air atmosphere, and granularity can be regulated by changing processing parameter.Because reaction medium is an organic solvent, has effectively solved the agglomeration traits of primary particle in the crystal growing process.The direct synthetic method of room temperature of the present invention does not need expensive equipment, does not have high-temperature process, and energy consumption is low, and easy control of process conditions is with low cost, is easy to suitability for industrialized production.The Barium Titanate nano-powder of the present invention's preparation has broad application prospects in fields such as microelectronic device, electro-optical device, storage medium, high dielectric material, gas sensitives.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the Barium Titanate nano-powder for preparing of the present invention;
Fig. 2 is transmission electron microscope (TEM) photo of the Barium Titanate nano-powder for preparing of the present invention.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
1) take by weighing the 1.702g tetrabutyl titanate, be dissolved in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, the mass concentration that adds 1ml in the ethanolic soln of the tetrabutyl titanate that step 1) prepares is 30% ammonia soln, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 1.277g barium acetate, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
4) take by weighing 2.736g potassium hydroxide, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
5) measure 15ml quadrol and 15ml thanomin respectively, add in the Erlenmeyer flask, and step 2) solution of the titanium precipitation of preparation and step 3), step 4) preparation all adds in the above-mentioned Erlenmeyer flask, and the room temperature lower magnetic force stirs 24h;
6) stop to stir, allow the product natural sedimentation, upper solution is outwelled, obtaining white precipitate, is 0.5% dilute acetic acid washing precipitation 3 times with volumetric concentration earlier, uses deionized water wash again 3 times, again product is placed 90 ℃ baking oven to dry 24h, promptly obtain the favorable dispersity Barium Titanate nano-powder.Its X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 1, and transmission electron microscope (TEM) photo is seen Fig. 2.
Embodiment 2
1) take by weighing the 0.340g tetrabutyl titanate, be dissolved in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, the mass concentration that adds 1ml in the ethanolic soln of the tetrabutyl titanate that step 1) makes is 30% ammonia soln, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 0.281g barium acetate, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
4) take by weighing 1.368g potassium hydroxide, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
5) measure 15ml quadrol and 15ml thanomin respectively, add in the Erlenmeyer flask, and step 2) solution of the titanium precipitation of preparation and step 3), step 4) preparation all adds in the above-mentioned Erlenmeyer flask, and the room temperature lower magnetic force stirs 72h;
6) stop to stir, allow the product natural sedimentation, upper solution is outwelled, obtaining white precipitate, is 0.5% dilute acetic acid washing precipitation 3 times with volumetric concentration earlier, uses deionized water wash again 3 times, again product is placed 90 ℃ baking oven to dry 24h, promptly obtain the favorable dispersity Barium Titanate nano-powder.
Embodiment 3
1) take by weighing the 3.404g tetrabutyl titanate, be dissolved in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, the mass concentration that adds 1ml in the ethanolic soln of the tetrabutyl titanate that step 1) makes is 30% ammonia soln, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 2.554g barium acetate, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
4) take by weighing 4.104g potassium hydroxide, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
5) measure 15ml quadrol and 15ml thanomin respectively, add in the Erlenmeyer flask, and step 2) solution of the titanium precipitation of preparation and step 3), step 4) preparation all adds in the above-mentioned Erlenmeyer flask, and the room temperature lower magnetic force stirs 12h;
6) stop to stir, allow the product natural sedimentation, upper solution is outwelled, obtaining white precipitate, is 0.5% dilute acetic acid washing precipitation 3 times with volumetric concentration earlier, uses deionized water wash again 3 times, again product is placed 90 ℃ baking oven to dry 24h, promptly obtain the favorable dispersity Barium Titanate nano-powder.
Embodiment 4
1) take by weighing the 1.702g tetrabutyl titanate, be dissolved in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, the mass concentration that adds 1ml in the ethanolic soln of the tetrabutyl titanate that step 1) makes is 30% ammonia soln, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 1.277g barium acetate, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
4) take by weighing 2.736g potassium hydroxide, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
5) measure the 15ml quadrol, add in the Erlenmeyer flask, and step 2) solution of the titanium precipitation of preparation and step 3), step 4) preparation all adds in the above-mentioned Erlenmeyer flask, and the room temperature lower magnetic force stirs 24h;
6) stop to stir, allow the product natural sedimentation, upper solution is outwelled, obtaining white precipitate, is 0.5% dilute acetic acid washing precipitation 3 times with volumetric concentration earlier, uses deionized water wash again 3 times, again product is placed 90 ℃ baking oven to dry 24h, promptly obtain the favorable dispersity Barium Titanate nano-powder.
Embodiment 5
1) take by weighing the 1.702g tetrabutyl titanate, be dissolved in the 10ml dehydrated alcohol, magnetic agitation is to dissolving;
2) under the whipped state, the mass concentration that adds 1ml in the ethanolic soln of the tetrabutyl titanate that step 1) makes is 30% ammonia soln, and precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) take by weighing the 1.277g barium acetate, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
4) take by weighing 2.736g potassium hydroxide, be dissolved in the 2ml deionized water, magnetic agitation is to dissolving;
5) measure 25ml quadrol and 5ml thanomin respectively, add in the Erlenmeyer flask, and step 2) solution of the titanium precipitation of preparation and step 3), step 4) preparation all adds in the above-mentioned Erlenmeyer flask, and the room temperature lower magnetic force stirs 24h;
6) stop to stir, allow the product natural sedimentation, upper solution is outwelled, obtaining white precipitate, is 0.5% dilute acetic acid washing precipitation 3 times with volumetric concentration earlier, uses deionized water wash again 3 times, again product is placed 90 ℃ baking oven to dry 24h, promptly obtain the favorable dispersity Barium Titanate nano-powder.
Claims (4)
1. the method for a preparing barium titanate nanometer powder under room temperature is characterized in that may further comprise the steps:
1) tetrabutyl titanate is dissolved in dehydrated alcohol, the Ti in the regulator solution
4+Ionic concn is 0.1～1.0mol/L;
2) under the whipped state, add the ammonia soln of the mass concentration 30% of 1～3ml in the ethanolic soln of the tetrabutyl titanate that step 1) prepares, precipitation is filtered, washing, and the oxyhydroxide that obtains titanium precipitates;
3) barium acetate is dissolved in deionized water, forms the barium acetate aqueous solution, Ba in the regulator solution
2+Ionic concentration is 0.5～5.0mol/L;
4) potassium hydroxide is dissolved in deionized water, configuration concentration is the potassium hydroxide aqueous solution of 10～30mol/L;
5) oxyhydroxide precipitation, the barium acetate aqueous solution and the potassium hydroxide aqueous solution with titanium joins in the organic amine solvent, stirred at least 10 minutes, obtain the precursor slurry, wherein the molecular volume mark of the oxyhydroxide of titanium is 0.1～0.2mol/L, the mol ratio of barium and titanium is 1.0～1.1, the molecular volume mark of potassium hydroxide is 0.5～1.0mol/L, and molecular volume fractional volume radix is the cumulative volume of precursor slurry;
6) the precursor slurry with preparation at room temperature continues to stir 12～72h, allows the products therefrom natural subsidence then, washes repeatedly with diluted acid and deionized water again, filters, and dries, and obtains Barium Titanate nano-powder.
2. the method for preparing barium titanate nanometer powder under room temperature according to claim 1, it is characterized in that said organic amine solvent is the mixing solutions of quadrol or quadrol and thanomin, wherein the volume of thanomin is no more than 80% of quadrol and thanomin mixing solutions cumulative volume.
3. the method for preparing barium titanate nanometer powder under room temperature according to claim 1 is characterized in that said diluted acid is a volume fraction less than 1% dilute acetic acid.
4. the method for preparing barium titanate nanometer powder under room temperature according to claim 1 is characterized in that the purity of said tetrabutyl titanate, barium acetate, potassium hydroxide, dehydrated alcohol, quadrol and thanomin all is not less than chemical pure.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095919A (en) * | 2018-08-01 | 2018-12-28 | 浙江大学 | A kind of barium titanate/cobaltosic oxide complex phase millimeter wave wave-absorbing powder and preparation method with multistage microstructural distribution |
| WO2022027786A1 (en) * | 2020-08-05 | 2022-02-10 | 深圳市华星光电半导体显示技术有限公司 | Method for preparing optical film, and optical film |
| CN114315349A (en) * | 2021-12-17 | 2022-04-12 | 西安理工大学 | Method for preparing mesoporous barium zirconate titanate ceramic nanoparticles |
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2008
- 2008-02-26 CN CNA2008100598842A patent/CN101311377A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095919A (en) * | 2018-08-01 | 2018-12-28 | 浙江大学 | A kind of barium titanate/cobaltosic oxide complex phase millimeter wave wave-absorbing powder and preparation method with multistage microstructural distribution |
| WO2022027786A1 (en) * | 2020-08-05 | 2022-02-10 | 深圳市华星光电半导体显示技术有限公司 | Method for preparing optical film, and optical film |
| CN114315349A (en) * | 2021-12-17 | 2022-04-12 | 西安理工大学 | Method for preparing mesoporous barium zirconate titanate ceramic nanoparticles |
| CN114315349B (en) * | 2021-12-17 | 2023-01-24 | 西安理工大学 | Method for preparing mesoporous barium zirconate titanate ceramic nanoparticles |
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