CN101643358A - Microwave liquid phase compounding process of high-purity barium titanate powder - Google Patents
Microwave liquid phase compounding process of high-purity barium titanate powder Download PDFInfo
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- CN101643358A CN101643358A CN200910017694A CN200910017694A CN101643358A CN 101643358 A CN101643358 A CN 101643358A CN 200910017694 A CN200910017694 A CN 200910017694A CN 200910017694 A CN200910017694 A CN 200910017694A CN 101643358 A CN101643358 A CN 101643358A
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Abstract
The invention relates to a microwave liquid phase compounding process of high-purity barium titanate powder. Main raw materials which are tetraisopropyl titanate or tetrabutyl titanate, barium octahydrate and nitric acid are compounded by microwave auxiliary heating at lower temperature for shorter reaction time to obtain the barium titanate powder in different grain diameter specifications. The process comprises the following concrete steps: (1) hydrolyzing a titanium resource; (2) washing a hydrolyzed product; (3) obtaining the titanium resource; (4) fully dissolving high-purity Ba(OH)2.8H2Oin the pure water in a microwave reaction vessel with a stirring system to obtain barium hydroxide solution; (5) carrying out compounding reaction and obtaining slurry containing barium titanate particles after the reaction; (6) precipitating and washing or filtering the barium titanate slurry obtained in the reaction with high-purity water for many times and then drying to obtain the high-puritycubic phase barium titanate powder. The process has low reaction temperature, short reaction time, controllable particle diameter and high product purity.
Description
Technical field
The present invention relates to a kind of preparing barium titanate powder, the microwave liquid phase that especially relates to a kind of ultra-fine high-purity cubic phase barium titanate powder is synthetic, belongs to electronic ceramics powder body material preparation field.
Technical background
Barium titanate (being called for short BT) is a kind of important base electronic material of electronic ceramics industrial circle, because it has high-k, performances such as good ferroelectric, piezoelectricity, withstand voltage and insulation are widely used in making laminated ceramic capacitor (being called for short MLCC), thermistor, piezoelectric ceramics and photoelectric device etc.Along with electronic devices and components develop towards directions such as " microminiaturization ", " large vol ", high-purity, ultra-fine, the uniform barium carbonate powder material of particle diameter is a key material of realizing this developing direction.
The existing report of the method for microwave-assisted liquid phase synthesis of barium titanate powder.Patent CN 1865154A has reported a kind of method of method for preparing cubic phase babrium titanate using microwave: adopting titanium chloride, bariumchloride is raw material, and sodium hydroxide provides basic reaction conditions, and reaction 20-30min can obtain cubic phase barium titanate.This method can cause the Na+ content in the barium carbonate powder higher owing to used NaOH, and powder washs purification difficult, thereby has a strong impact on the performance of barium carbonate powder.Patent CN 100369862C has reported the method for a kind of microwave hydrothermal synthesis device and synthesizing tetragonal barium titanate thereof.This method temperature of reaction is at least 200 ℃, and needs the microwave reaction kettle of anti-higher malleation.
Summary of the invention
The liquid-phase synthesis process that the purpose of this invention is to provide a kind of high-purity cubic phase barium titanate powder, this method temperature of reaction is low, the reaction times is short, particle diameter is controlled, product purity is high.
Technical scheme of the present invention is:
A kind of microwave liquid-phase synthesis process of high-purity barium titanate powder, main raw material is titanium isopropylate or tetrabutyl titanate, barium hydroxide, nitric acid, utilize microwave-assisted heating, at a lower temperature, by the synthetic barium carbonate powder that obtains the different-grain diameter specification of short reaction times, concrete processing step is as follows:
1) titanium source hydrolysis: the titanium source is titanium isopropylate or tetrabutyl titanate, adds the pure water hydrolysis, follows quick stirring, obtains white or light yellow hydrolysate;
2) hydrolysate washing: the hydrolysate that above-mentioned reaction is obtained washs with pure water, obtains hydrolysate high concentration ground paste or filter cake;
3) titanium source: above-mentioned product slip or filter cake are disperseed with the high purity water reslurry, add nitric acid and carry out the peptization processing, obtain the clear sol system;
4) with high-purity Ba (OH) 28H2O fully dissolving in pure water in the microwave reaction kettle of band stirring system, obtain barium hydroxide solution;
5) building-up reactions: the colloidal sol product that obtains in the step 3) is joined step 4) be equipped with in the microwave reaction kettle of barium hydroxide solution, closed reactor, feed rare gas element or nitrogen, be heated to 70-100 ℃ and begin reaction, can obtain containing the slip of metatitanic acid titanate particle after reaction finishes;
6) above-mentioned reaction is obtained barium titanate slurry with high purity water sedimentation washing or diafiltration several after drying, can obtain high-purity cubic phase barium titanate powder.
Technical scheme of the present invention also has:
The mass ratio of titanium source and pure water is for being not less than 1: 5, preferred 1 in the hydrolytic process of step 1): 7-12, and temperature of reaction is no more than 40 ℃, and the pH value is 3-7.
In the peptization treating processes of step 3), hydrolysate (in titanium) is 0.3～0.7 with the nitric acid mol ratio, preferred 0.4～0.6; 50～90 ℃ of peptization temperature, preferred 60～80 ℃; Peptization time is 10min～8h, preferred 0.5～3h; Sol system pH is 0.1-3 (50 ℃), preferred 0.5～1.5 (50 ℃); Follow vigorous stirring in the whole process always.
In the step 4), the barium of high-purity Ba (OH) 28H2O and the mol ratio of titanium elements are (1.3～3.0): 1, preferred (1.5～3.0): 1; Solvent temperature is 60～90 ℃; Final barium hydroxide solution concentration is 0.5～3.3mol/L.
All follow quick stirring in colloidal sol adding and the reaction process in the step 5), microwave reaction kettle power is 0-3.0KW, and volume is 2.5L.
Reaction system adopts the microwave-assisted heating, and reaction conditions is normal pressure, 70～100 ℃, reaction times 0.5～3h, obtains epigranular, good dispersity, barium titanium than the high-purity barium titanate powder adjustable, that carbonate content is lower, and preferable reaction temperature is 80-90 ℃.
Can synthesize obtain specific surface area at 5～60m2/g, primary particle size at 200～20nm, barium titanium mol ratio=1.000 ± 0.002, sphericity cubic phase barium titanate powder preferably.
Compared with prior art, advantage of the present invention is: temperature of reaction is low, and the reaction times is short, and particle diameter is controlled, and the product purity height is simple to operate.
Description of drawings
Fig. 1 is the stereoscan photograph of embodiment 1 gained sample.
Fig. 2 is the XRD figure of embodiment 1 gained sample.
Fig. 3 is the stereoscan photograph of embodiment 2 gained samples.
Fig. 4 is the XRD figure of embodiment 2 gained samples.
Fig. 5 is the stereoscan photograph of embodiment 3 gained samples.
Fig. 6 is the XRD figure of embodiment 3 gained samples.
Embodiment
Embodiment 1
(1) takes by weighing 113.68g analytical pure titanium isopropylate, follow quick stirring, with its hydrolysis in the beaker that fills the 2L pure water, behind the stirring 10min, with the hydrolysate filtering and washing.This hydrolysate is disperseed to be diluted to volume again with pure water in beaker be 600ml, add the analytical pure nitric acid 19g of concentration 65%, and moisturizing is 1L to volume.Follow quick stirring then, above-mentioned slip is heated up,, obtain vitreosol in 65 ℃ of insulation 50min.
(2) be to add the 400ml pure water in the 2.5L microwave reaction kettle at capacity, utilize microwave heating to 85 ℃, (purity＞98wt%) 257g adds in the still, and opens and stir auxiliary hydrated barta dissolving to take by weighing barium hydroxide, and moisturizing is 1L to volume, is mixed with near transparent barium hydroxide solution.
(3) under agitation condition, the vitreosol that (1) is obtained joins rapidly in the barium hydroxide solution in the microwave still, and closed reactor feeds N2, at 85 ℃ of reaction 3h.
(4) reaction finishes, discharging, and washing, drying can obtain very homogeneous high purity cubic phase barium titanate powder of specific surface area=5.37m2g-1, the about 200nm of particle diameter, Ba/Ti=1.0008, particle diameter.
(1) takes by weighing 284g analytical pure titanium isopropylate, follow quick stirring, with its hydrolysis in the beaker that fills the 5L pure water, behind the stirring 10min, with the hydrolysate filtering and washing.This hydrolysate is disperseed to be diluted to volume again with pure water in beaker be 900ml, add the analytical pure nitric acid 47g of concentration 65%, and moisturizing is 1L to volume.Follow quick stirring then, above-mentioned slip is heated up,, obtain vitreosol in 65 ℃ of insulation 3h.
(2) be to add the 700ml pure water in the 2.5L microwave reaction kettle at capacity, utilize microwave heating to 85 ℃, (purity＞98wt%) 643g adds in the still, and opens and stir auxiliary hydrated barta dissolving to take by weighing barium hydroxide, and moisturizing is 1L to volume, is mixed with near transparent barium hydroxide solution.
(3) under agitation condition, the vitreosol that (1) is obtained joins rapidly in the barium hydroxide solution in the microwave still, and closed reactor feeds N2, at 85 ℃ of reaction 30min.
(4) reaction finishes, discharging, and washing, drying can obtain very homogeneous high purity cubic phase barium titanate powder of specific surface area=30m2g-1, the about 40nm of particle diameter, Ba/Ti=0.9990 particle diameter.
Embodiment 3
(1) takes by weighing 454g analytical pure titanium isopropylate, follow quick stirring, with its hydrolysis in the retort that fills the 10L pure water, behind the stirring 10min, with the hydrolysate filtering and washing.This hydrolysate is disperseed to be diluted to volume again with pure water in beaker be 1L, add the analytical pure nitric acid 76g of concentration 65%, and moisturizing is 1.1L to volume.Follow quick stirring then, above-mentioned slip is heated up,, obtain vitreosol in 65 ℃ of insulation 3h.
(2) be the middle 1L of adding pure water in the 2.5L microwave reaction kettle at capacity, utilize microwave heating to 85 ℃, (purity＞98wt%) 1029g adds in the still to take by weighing barium hydroxide, and open and stir auxiliary hydrated barta dissolving, and moisturizing is 1.1L to volume, is mixed with near transparent barium hydroxide solution.
(3) under agitation condition, the vitreosol that (1) is obtained joins rapidly in the barium hydroxide solution in the microwave still, and closed reactor feeds N2, at 85 ℃ of reaction 30min.
(4) reaction finishes, discharging, and washing, drying can obtain very homogeneous high purity cubic phase barium titanate powder of specific surface area=57m2g-1, the about 20nm of particle diameter, Ba/Ti=0.9984, particle diameter.
Claims (7)
1, a kind of microwave liquid-phase synthesis process of high-purity barium titanate powder, it is characterized in that main raw material is titanium isopropylate or tetrabutyl titanate, barium hydroxide, nitric acid, utilize microwave-assisted heating, at a lower temperature, by the synthetic barium carbonate powder that obtains the different-grain diameter specification of short reaction times, concrete processing step is as follows:
1) titanium source hydrolysis: the titanium source is titanium isopropylate or tetrabutyl titanate, adds the pure water hydrolysis, follows quick stirring, obtains white or light yellow hydrolysate;
2) hydrolysate washing: the hydrolysate that above-mentioned reaction is obtained washs with pure water, obtains hydrolysate high concentration ground paste or filter cake;
3) titanium source: above-mentioned product slip or filter cake are disperseed with the high purity water reslurry, add nitric acid and carry out the peptization processing, obtain the clear sol system;
4) with high-purity Ba (OH) 28H2O fully dissolving in pure water in the microwave reaction kettle of band stirring system, obtain barium hydroxide solution;
5) building-up reactions: the colloidal sol product that obtains in the step 3) is joined step 4) be equipped with in the microwave reaction kettle of barium hydroxide solution, closed reactor, feed rare gas element or nitrogen, be heated to 70-100 ℃ and begin reaction, can obtain containing the slip of metatitanic acid titanate particle after reaction finishes;
6) above-mentioned reaction is obtained barium titanate slurry with high purity water sedimentation washing or diafiltration several after drying, can obtain high-purity cubic phase barium titanate powder.
2, the microwave liquid-phase synthesis process of a kind of high-purity barium titanate powder according to claim 1 is characterized in that: all follow quick stirring in colloidal sol adding and the reaction process in the step 5), microwave reaction kettle power is 0-3.0KW, and volume is 2.5L.
3, the microwave liquid-phase synthesis process of a kind of high-purity barium titanate powder according to claim 1, it is characterized in that: the mass ratio of titanium source and pure water is for being not less than 1: 5 in the hydrolytic process of step 1), preferred 1: 7-12, temperature of reaction is no more than 40 ℃, and the pH value is 3-7.
4, the microwave liquid-phase synthesis process of a kind of high-purity barium titanate powder according to claim 1 is characterized in that: in the peptization treating processes of step 3), hydrolysate (in titanium) is 0.3～0.7 with the nitric acid mol ratio, preferred 0.4～0.6; 50～90 ℃ of peptization temperature, preferred 60～80 ℃; Peptization time is 10min～8h, preferred 0.5～3h; Sol system pH is 0.1-3 (50 ℃), preferred 0.5～1.5 (50 ℃); Follow vigorous stirring in the whole process always.
5, the microwave liquid-phase synthesis process of a kind of high-purity barium titanate powder according to claim 1 is characterized in that: in the step 4), the barium of high-purity Ba (OH) 28H2O and the mol ratio of titanium elements are (1.3～3.0): 1, preferred (1.5～3.0): 1; Solvent temperature is 60～90 ℃; Final barium hydroxide solution concentration is 0.5～3.3mol/L.
6, the microwave liquid-phase synthesis process of a kind of high-purity barium titanate powder according to claim 1, it is characterized in that: reaction system adopts the microwave-assisted heating, reaction conditions is normal pressure, 70～100 ℃, reaction times 0.5～3h, obtain epigranular, good dispersity, barium titanium than the high-purity barium titanate powder adjustable, that carbonate content is lower, preferable reaction temperature is 80-90 ℃.
7, the microwave liquid-phase synthesis process of a kind of high-purity barium titanate powder according to claim 1, it is characterized in that synthesizing obtain specific surface area at 5～60m2/g, primary particle size at 200～20nm, barium titanium mol ratio=1.000 ± 0.002, sphericity cubic phase barium titanate powder preferably.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584219A (en) * | 2012-02-22 | 2012-07-18 | 上海大学 | Method for quickly compounding barium titanate nano-powder |
| CN103449512A (en) * | 2013-08-29 | 2013-12-18 | 陕西师范大学 | Method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of microwave hydrothermal method |
| CN106115775A (en) * | 2016-06-29 | 2016-11-16 | 攀枝花学院 | Adulterate the preparation method of positive metatitanic acid |
| CN107601554A (en) * | 2017-09-26 | 2018-01-19 | 上海大学 | The method of microwave assisted aqueous extraction hot preparation nanometer tetragonal-phase barium titanate powder |
-
2009
- 2009-08-24 CN CN200910017694A patent/CN101643358A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584219A (en) * | 2012-02-22 | 2012-07-18 | 上海大学 | Method for quickly compounding barium titanate nano-powder |
| CN103449512A (en) * | 2013-08-29 | 2013-12-18 | 陕西师范大学 | Method for preparing monodisperse and cuboid nano-barium titanate powder by virtue of microwave hydrothermal method |
| CN106115775A (en) * | 2016-06-29 | 2016-11-16 | 攀枝花学院 | Adulterate the preparation method of positive metatitanic acid |
| CN107601554A (en) * | 2017-09-26 | 2018-01-19 | 上海大学 | The method of microwave assisted aqueous extraction hot preparation nanometer tetragonal-phase barium titanate powder |
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