CN101550015A - Method of preparing perovskite niobate titanate nanometer powders - Google Patents
Method of preparing perovskite niobate titanate nanometer powders Download PDFInfo
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- CN101550015A CN101550015A CNA2009101140111A CN200910114011A CN101550015A CN 101550015 A CN101550015 A CN 101550015A CN A2009101140111 A CNA2009101140111 A CN A2009101140111A CN 200910114011 A CN200910114011 A CN 200910114011A CN 101550015 A CN101550015 A CN 101550015A
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Abstract
The invention discloses a method of preparing perovskite niobate titanate nanometer powders. The niobium pentoxide, sodium carbonate, potassium carbonate, titanium dioxide, bismuth oxide are mixed according to the stoichiometric proportion of (1-x) [(Na [0.5] K [0.5]) NbO[3 ]]-x [(Bi [0.5] Na [0.5]) TiO [3]], wherein 0.00 <x <1.00; after high-energy ball mill mixing, pre-sintering, secondary ball milling and other processes, the sodium potassium-sodium bismuth titanate solid solution nanometer powders with particle-size smaller than 30 nanometer are ultimately prepared. The inventive method can prepare a series of perovskite niobate titanates electronic ceramics nanometer powders, which have small granules, uniform grain fineness distribution, medium cost and can satisfy requirements of different fields; the inventive method is simple, energy-saving, time-saving, and suitable for mass production.
Description
Technical field
The present invention relates to a kind of preparation method of perovskite niobate titanate nanometer powders, belong to the function ceramics field.
Background technology
Document " John G.Fisher, Suk-Joong L.Kang, Microstructural changes in (K
0.5Na
0.5) NbO
3Ceramics sintered in various atmospheres, Journal of theEuropean Ceramic Society, doi:10.1016/j.jeurceramsoc.2009.02.006 " use polypropylene ball milling jar, zirconia ball on planetary ball mill through 24 hours ball millings, obtain median size and be the potassium-sodium niobate powder about 140 nanometers.Adopt at present the ball milling method of polymkeric substance ball milling jar and common light ball (as alumina balls, zirconia ball and agate ball), because the restriction of equipment itself, even the ball milling time infinitely prolongs, also be difficult to prepare size uniformly, the ceramic powder of particle diameter below 50 nanometers.
Summary of the invention
In order to overcome the deficiency that existing powder-making technique is difficult to prepare the following powder of 50 nanometers, the present invention adopts toughness reinforcing tungsten-carbide ball of cobalt and wolfram varbide ball milling jar, oxide compound and carbonate powder and tungsten-carbide ball are inserted in the sealing ball grinder altogether, violent rotation or vibration by ball grinder, make between abrading-ball and abrading-ball and tank skin between powder collided, reach and pulverize even the purpose of synthetic powder.Prepared potassium-sodium niobate, bismuth-sodium titanate, the potassium-sodium niobate-sodium bismuth titanate sosoloid nanometer powder of particle size by this method less than 30 nanometers.
Concrete steps are:
(1), be (1-x) [(Na by stoichiometric ratio with Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide
0.5K
0.5) NbO
3]-x[(Bi
0.5Na
0.5) TiO
3] batching, wherein: 0.00＜x＜1.00;
(2) powder that step (1) is prepared is put into the high-energy ball milling jar, adds tungsten-carbide ball in jar, to add powder quality be 1～15% of tungsten-carbide ball quality; Powder ball milling 1～20 hour in high energy ball mill, rotating speed is 150～550 rev/mins, does not add any ball-milling medium; The pre-burning 1～3 hour under 400～900 ℃ of temperature of the later powder of ball milling; Powder after the taking-up pre-burning is smashed, and high-energy ball milling is after 1～3 hour once more; Cross 120 purpose sieves;
(3) use X-ray diffractometer to detect thing phase, the crystalline structure of step (2) gained powder, calculate grain-size;
(4) use laser particle size analyzer and transmission electron microscope to detect the particle size of step (2) gained powder.
The invention has the beneficial effects as follows: adopted the tungsten-carbide ball of extreme hardness and wolfram varbide ball milling jar to come oxide compound and carbonate raw material are carried out ball milling, improved the pulverizing dynamics and the grinding efficiency of raw material greatly.Make that raw material just can mix in the very short time, grain refine even directly synthetic required product.For sintering temperature and the preparation nano ceramics that reduces pottery provides strong assurance.Effective simplification of the present invention niobate-titanate nano-powder preparation technology and shortened preparation time, successful preparation potassium-sodium niobate, bismuth-sodium titanate and the potassium-sodium niobate-sodium bismuth titanate sosoloid nano-powder of particle size below 30 nanometers.
Description of drawings
Fig. 1 is the grain-size of the potassium-sodium niobate powder of different ball milling times.
Fig. 2 is the X ray collection of illustrative plates and the size-grade distribution of potassium-sodium niobate-sodium bismuth titanate solid solution powder.
Fig. 3 is the bismuth-sodium titanate powder X ray collection of illustrative plates of different ball milling times.
Embodiment
Embodiment 1:
With analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood powder is raw material, and 120 ℃ of oven dry are after 24 hours, according to chemical formula Na
0.5K
0.5NbO
3Proportioning, the various raw material powders of weighing.Raw material directly carries out the mechanical alloying ball milling without any special processing, does not add any ball-milling medium, and powder quality accounts for 3% of tungsten-carbide ball quality, and the ball milling time is 2 hours, and rotating speed is 450 rev/mins; Powder after having ground was calcined 2.5 hours down at 850 ℃, made each raw material powder fully react; Resulting powder is put into ball grinder once more, and secondary ball milling 2 hours takes out powder and crosses 120 purpose sieves.Use X-ray diffraction to differentiate the thing phase of powder, crystalline structure and calculating grain-size; Use transmission electron microscope and laser particle size analyzer to measure the particle size of powder.Fig. 1 has provided the average grain size of 2 hours potassium-sodium niobate powder of ball milling first, about 23.5 nanometers (calculating) by the X ray collection of illustrative plates, and provided the average grain size of the potassium-sodium niobate powder of other ball milling times.
Embodiment 2:
With analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide powder is raw material, and 120 ℃ of oven dry are after 24 hours, according to chemical formula 0.80Na
0.5K
0.5NbO
3-0.20Bi
0.5Na
0.5TiO
3Proportioning, the various raw material powders of weighing.Raw material directly carries out the mechanical alloying ball milling without any special processing, does not add any ball-milling medium, and powder quality accounts for 5% of tungsten-carbide ball quality, and the ball milling time is 8 hours, and rotating speed is 400 rev/mins; Powder after having ground was calcined 2 hours down at 850 ℃, made each raw material powder fully react; Resulting powder is put into ball grinder once more, and secondary ball milling 1 hour takes out powder and crosses 120 purpose sieves.Use X-ray diffraction to differentiate the thing phase of powder, crystalline structure and calculating grain-size; Use transmission electron microscope and laser particle size analyzer to measure the particle size of powder.Fig. 2 has provided its X ray diffracting spectrum, shows it is pure uhligite cube phase; Give their size-grade distribution simultaneously among the figure of Cha Ruing, its size-grade distribution is approximately 27 nanometers in a narrow scope as seen from the figure, shows the epigranular of powder.
Embodiment 3:
With analytical pure grade titanium dioxide, bismuthous oxide bismuth trioxide powder is raw material, and 120 ℃ of oven dry are after 24 hours, according to chemical formula Bi
0.5Na
0.5TiO
3Proportioning, the various raw material powders of weighing.Raw material directly carries out the mechanical alloying ball milling without any special processing, does not add any ball-milling medium, and powder quality accounts for 8% of tungsten-carbide ball quality, and the ball milling time is respectively 2,4, and 6,8 hours, rotating speed was 450 rev/mins; Powder after all have ground was calcined 2 hours down at 400 ℃, made each raw material powder fully react; Resulting powder is put into ball grinder once more, and secondary ball milling 1 hour takes out powder and crosses 120 purpose sieves.Take out powder after ball milling is intact and cross 120 purpose sieves.Use X-ray diffraction to differentiate the thing phase of powder, crystalline structure and calculating grain-size; Use transmission electron microscope and laser particle size analyzer to measure the particle size of powder.Fig. 3 has provided the different ball milling times does not have incinerating bismuth-sodium titanate X ray diffracting spectrum, there is collection of illustrative plates as can be known, along with the increase of ball milling time, bismuth-sodium titanate content increases gradually in the powder, is comprising in the powder that crystalline bismuth-sodium titanate crystalline phase is mutually unformed with the part bismuth-sodium titanate.In order to obtain the bismuth sodium titanate nanometer powder of complete crystallization, the powder that ball milling is crossed is through low temperature calcination, and the average grain size that utilizes the X ray collection of illustrative plates to calculate 8 hours bismuth-sodium titanate powder gained of ball milling is 12 nanometers.
Claims (1)
1. the preparation method of a perovskite niobate titanate nanometer powders is characterized in that concrete steps are:
(1), be (1-x) [(Na by stoichiometric ratio with Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide
0.5K
0.5) NbO
3]-x[(Bi
0.5Na
0.5) TiO
3] batching, wherein: 0.00＜x＜1.00;
(2) powder that step (1) is prepared is put into the high-energy ball milling jar, adds tungsten-carbide ball in jar, to add powder quality be 1～15% of tungsten-carbide ball quality; Powder ball milling 1～20 hour in high energy ball mill, rotating speed is 150～550 rev/mins, does not add any ball-milling medium;
(3) with the pre-burning 1～3 hour under 400～900 ℃ of temperature of step (2) gained powder; Powder after the taking-up pre-burning is smashed, and high-energy ball milling is after 1～3 hour once more; Cross 120 purpose sieves;
(4) use X-ray diffractometer to detect thing phase, the crystalline structure of step (3) gained powder, calculate grain-size;
(5) use laser particle size analyzer and transmission electron microscope to detect the particle size of step (3) gained powder.
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|---|---|---|---|
| CNA2009101140111A CN101550015A (en) | 2009-04-23 | 2009-04-23 | Method of preparing perovskite niobate titanate nanometer powders |
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|---|---|---|---|
| CNA2009101140111A CN101550015A (en) | 2009-04-23 | 2009-04-23 | Method of preparing perovskite niobate titanate nanometer powders |
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| CN101550015A true CN101550015A (en) | 2009-10-07 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798227A (en) * | 2010-03-24 | 2010-08-11 | 桂林理工大学 | Solid phase synthetic method of niobate-titanate nano-powder |
| CN101891475A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Preparation method of potassium-sodium niobate-potassium-bismuth titanate nano ceramics |
| CN102603299A (en) * | 2012-03-22 | 2012-07-25 | 中北大学 | High conductivity nanometer complex phase perovskite type proton conductor |
| CN101775289B (en) * | 2009-12-25 | 2012-12-19 | 上海师范大学 | Method for synthesizing bismuth-doped calcium niobate nano luminous material |
| CN105732025A (en) * | 2016-01-20 | 2016-07-06 | 武汉理工大学 | Preparation method of sodium-bismuth-titanate-base X9R multilayer ceramic capacitor material and device thereof |
| CN112871002A (en) * | 2021-01-12 | 2021-06-01 | 长飞光纤光缆股份有限公司 | Uniform mixing method of multi-component powder raw materials |
-
2009
- 2009-04-23 CN CNA2009101140111A patent/CN101550015A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775289B (en) * | 2009-12-25 | 2012-12-19 | 上海师范大学 | Method for synthesizing bismuth-doped calcium niobate nano luminous material |
| CN101798227A (en) * | 2010-03-24 | 2010-08-11 | 桂林理工大学 | Solid phase synthetic method of niobate-titanate nano-powder |
| CN101891475A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Preparation method of potassium-sodium niobate-potassium-bismuth titanate nano ceramics |
| CN102603299A (en) * | 2012-03-22 | 2012-07-25 | 中北大学 | High conductivity nanometer complex phase perovskite type proton conductor |
| CN105732025A (en) * | 2016-01-20 | 2016-07-06 | 武汉理工大学 | Preparation method of sodium-bismuth-titanate-base X9R multilayer ceramic capacitor material and device thereof |
| CN105732025B (en) * | 2016-01-20 | 2019-03-08 | 武汉理工大学 | A kind of bismuth-sodium titanate base X9R type multi-layer ceramic capacitor material and its device preparation method |
| CN112871002A (en) * | 2021-01-12 | 2021-06-01 | 长飞光纤光缆股份有限公司 | Uniform mixing method of multi-component powder raw materials |
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