CN101565203B - Bismuth sodium titanate nanometer flower and preparation method thereof - Google Patents
Bismuth sodium titanate nanometer flower and preparation method thereof Download PDFInfo
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- CN101565203B CN101565203B CN2008100251095A CN200810025109A CN101565203B CN 101565203 B CN101565203 B CN 101565203B CN 2008100251095 A CN2008100251095 A CN 2008100251095A CN 200810025109 A CN200810025109 A CN 200810025109A CN 101565203 B CN101565203 B CN 101565203B
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Abstract
The invention discloses a bismuth sodium titanate nanometer flower and a preparation method thereof. The nanometer flower comprises crossed vertical nanometer sheets which have the length of 250 nm to350 nm, the height of 50 nm to 150 nm and the thickness of 5 nm to 15 nm and are made of monocrystal perovskite bismuth sodium titanate. The method comprises the following steps: firstly, adding ammo nia to a citric acid aqueous solution with the density of 0.8M to 1.2M and adjusting a pH value to be between 4.5 and 6; adding tetrabutyl titanate and stirring at 50 DEG C to 70 DEG C for longer than5 hours to obtain a clear solution; then, mixing a bismuth nitrate pentahydrate aqueous solution with the clear solution and stirring at 80 DEG C to 100 DEG C for longer than 30 minutes to obtain a m ixed solution; afterwards, adding sodium hydroxide to the mixed solution and continuously stirring for longer than 15 minutes to obtain a synthetic solution; later, keeping the synthetic solution at 80 DEG C to 180 DEG C for 0 to 10 hours and washing to be neutral to obtain a product; and finally, drying the product to obtain the bismuth sodium titanate nanometer flower. The invention can be widely applied to the fields of machinery, electrons, precise control, and the like.
Description
Technical field
The present invention relates to a kind of nanometer flower and preparation method, especially a kind of bismuth sodium titanate nanometer flower and preparation method thereof.
Background technology
Bismuth-sodium titanate is a kind of very important ABO as the unleaded substitute of ferroelectric piezoelectric
3The functional materials of type perovskite structure has a wide range of applications in fields such as machinery, electronics, accurate controls at present.Utilize its dielectric properties, can make ceramic condenser; During as piezoelectric, can be prepared into various transmitters, high-temperature piezoelectric device, PZT (piezoelectric transducer) and drive unit etc.The nanostructure of bismuth-sodium titanate has the extensive concern that big specific surface has caused researcher because of it, people are in order to explore and expand its range of application, some trials and effort have been done, as " Hydrothermal Preparation nanometer Na in " electronic component and material " the 23rd volume o. 11th magazine of publishing in November, 2004
0.5Bi
0.5TiO
3Powder " literary composition once disclosed and a kind ofly prepared nanometer Na with hydrothermal method
0.5Bi
0.5TiO
3The method of powder.It is the bismuth source that this method adopts analytical pure five nitric hydrate bismuths, tetrabutyl titanate is the titanium source, in between the two mol ratio is to add ammoniacal liquor again after 1: 2 ratio is dissolved in it in ethanol, obtain the precursor of bismuth, titanium, afterwards, earlier in the precursor of bismuth, titanium, add sodium hydroxide,, and make product-bismuth-sodium titanate powder again through heating, washing and exsiccant step.But, no matter be product, or the preparation method, all exist weak point, at first, the pattern of product is sphere or cube, rather than nanometer flower structure, particularly the nanometer flower structure of not being made up of nanometer sheet.This sphere or cuboidal nano level bismuth-sodium titanate are because of its lower specific inductivity and higher dielectric loss make its ferroelectric piezoelectric property and traditional Pb-based lanthanumdoped zirconate titanates (PbTiO
3-PbZrO
3, be abbreviated as PZT) and also have a certain distance; Secondly, the preparation method both can not make the bismuth-sodium titanate of the nanometer flower structure of being made up of nanometer sheet, unexposed again concrete manufacture craft parameter, more be to use organism ethanol as solvent, increased the cost of making.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming weak point of the prior art, and a kind of bismuth sodium titanate nanometer flower of the nano flower-like structure of being made up of nanometer sheet is provided.
Another technical problem that the present invention will solve is for providing a kind of preparation method of bismuth sodium titanate nanometer flower.
For solving technical problem of the present invention, the technical scheme that is adopted is: bismuth sodium titanate nanometer flower comprises bismuth-sodium titanate, particularly described bismuth-sodium titanate is spherical flower-shaped, described spherical flower is made up of the nanometer sheet of intersecting on one's feet, the length of described nanometer sheet is 250～350nm, highly is that 50～150nm, thickness are 5～15nm, and it is that monocrystalline perovskite bismuth-sodium titanate by three-legged structure constitutes.
As the further improvement of bismuth sodium titanate nanometer flower, described intersection nanometer sheet on one's feet is perpendicular to the centre of sphere of sphere flower; Described nanometer sheet is the curved surface shape.
For solving another technical problem of the present invention, another technical scheme that is adopted is: the preparation method of bismuth sodium titanate nanometer flower comprises hydrothermal method, particularly it is finished according to the following steps: the first step, in being the aqueous citric acid solution of 0.8～1.2M, concentration adds earlier after ammoniacal liquor regulates pH and be 4.5～6.0, again to wherein adding tetrabutyl titanate, and down stir 5h more than in 50～70 ℃ it, obtain settled solution, wherein, the mol ratio between tetrabutyl titanate and citric acid is 1: 2.5～3.5; Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred more than the 30min down in 80～100 ℃, obtain even, transparent, thick mixing solutions, wherein, mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 2.5～3.5, again sodium hydroxide is added in the mixing solutions, and continue to stir more than the 15min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 20～30: 1; The 3rd goes on foot, and earlier resulting solution being placed temperature is 80～180 ℃ of insulation 0～10h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product, afterwards, to the product drying treatment, makes bismuth sodium titanate nanometer flower.
As the preparation method's of bismuth sodium titanate nanometer flower further improvement, described aqueous citric acid solution is for formulated in the water that citric acid is joined temperature 〉=60 ℃; The described five nitric hydrate bismuth aqueous solution are formulated for stirring more than the 15min in the water that five nitric hydrate bismuths is joined temperature 〉=90 ℃; Described washing is water or dehydrated alcohol flushing; The number of times of described flushing is 5～8 times; Described water is deionized water or distilled water; Described drying treatment is to be incubated 4～6h down for 40～60 ℃ in temperature.
Beneficial effect with respect to prior art is, one, use field emission scanning electron microscope, transmission electron microscope and X-ray diffractometer to characterize respectively to the final product that makes, final product is the sphere flower of single discrete distribution as can be known, and this sphere flower is made up of intersection nanometer sheet on one's feet.The length of nanometer sheet is 250～350nm, highly is that 50～150nm, thickness are 5～15nm.This nanometer sheet is that the monocrystalline perovskite bismuth-sodium titanate by three-legged structure constitutes, and it has good monocrystalline; They are two years old, use directric relaxation analyser and ultraviolet-visible spectrometer to detect respectively to bismuth sodium titanate nanometer flower, by the dielectric temperature spectrogram that records and uv-visible absorption spectrum figure as can be known, bismuth sodium titanate nanometer flower has lower dielectric loss and good photocatalytic activity, has opened up bismuth-sodium titanate thus as the application prospect of photocatalyst in environment protection; Its three, preparation technology is simple, easy to operate, starting material are inexpensive and consume fewly, particularly make water as solvent, reduced the cost of preparation widely, make it very easily in suitability for industrialized production.
Further embodiment as beneficial effect, the one, aqueous citric acid solution is preferably and joins in the water of temperature 〉=60 ℃ citric acid formulated, the five nitric hydrate bismuth aqueous solution are preferably five nitric hydrate bismuths are joined and stir more than the 15min formulatedly in the water of temperature 〉=90 ℃, have guaranteed that respectively solute in aqueous citric acid solution, the five nitric hydrate bismuth aqueous solution dissolves fully and fully; The 2nd, the number of times of flushing is preferably 5～8 times during washing, and promptly washing time that can be minimum is extremely neutral with the reaction soln washing.
Description of drawings
Below in conjunction with accompanying drawing optimal way of the present invention is described in further detail.
Fig. 1 be to the final product that makes use take the photograph after the observation of Sirion 200 type scanning electronic microscope (SEM) the SEM photo, can find out by Fig. 1 a, the output of the final product that makes is big and be evenly distributed, can find out that by Fig. 1 b final product is the flower-like nanostructure that the sheet about high 100nm, about long 300nm is formed;
Fig. 2 is an XRD spectra of using Phlips X ' Pert type X-ray diffraction (XRD) instrument to record to final product shown in Figure 1, can be found out that by this XRD spectra final product is the uhligite bismuth-sodium titanate of three-legged structure;
Fig. 3 be take the photograph after using JEM-2010 type transmission electron microscope (TEM) and JEOL-2010 type high resolution transmission electron microscopy (HRTEM) to observe to final product shown in Figure 1 photo.Can find out that by Fig. 3 a the length of nanometer sheet is about about 300nm, highly is about about 100nm and distributes more even.Can be found out that by Fig. 3 b nanometer sheet is along the growth of [110] and [112] direction, the interior illustration in Fig. 3 b upper right corner is the electron diffraction photo in its constituency, illustrates that the bismuth sodium titanate nanometer sheet has good monocrystalline;
Fig. 4 be to adopt final product that different soaking times makes to use to take the photograph after the observation of Sirion 200 type scanning electronic microscope (SEM) photo, wherein, Fig. 4 a is insulation 0 hour, and Fig. 4 b is insulation 0.5 hour, Fig. 4 c is insulation 1 hour, and Fig. 4 d is insulation 10 hours.Can be found out that by Fig. 4 a～d along with the prolongation in reaction times, variation has taken place the pattern of product, explanation can be controlled the pattern of final product by the adjusting of soaking time, and then controls its relevant rerum natura;
Fig. 5 is the dielectric temperature spectrogram that uses Hioki 3531ZHITESTER type directric relaxation analyser to record under 10KHz, 100KHz and three kinds of frequencies of 1MHz respectively to final product shown in Figure 1, and the warm area scope of selection is room temperature～550 ℃.Can find out that by Fig. 5 a, Fig. 5 b the dielectric loss of bismuth sodium titanate nanometer flower and specific inductivity all reduce gradually along with the rising of frequency, especially dielectric loss can be reduced to very little numerical value under high frequency situations;
Fig. 6 is the UV-Vis spectrogram that obtains after methyl orange solution use CARY-5E type ultraviolet-visible spectrum (UV-Vis) instrument of the bismuth sodium titanate nanometer structure of putting into different-shape is tested.Wherein, Fig. 6 a for to the methyl orange solution that is placed with the final product that makes in the contrast UV-Vis spectrogram under different time under the ultraviolet-visible rayed; Fig. 6 b is for to simple methyl orange solution and the methyl orange solution of putting into the bismuth-sodium titanate of cubic block, sphere and nano flower-like structure respectively, respectively at the contrast UV-Vis spectrogram that the ultraviolet-visible rayed descends and separates, the C among the figure in the ordinate zou
0And C
tConcentration behind difference represent methylidene orange initial concentration of solution and the light application time t; Fig. 6 c absorbs spectrogram for the UV-Vis that the methyl orange solution that is placed with final product shown in Figure 1 is recorded after the decline of ultraviolet-visible rayed is separated; (the α h ν) of Fig. 6 d for Fig. 6 c being carried out obtain after the data processing
2-h ν, the h ν among the figure in ordinate zou and the X-coordinate are that photon energy, α are photoabsorption coefficient.
Embodiment
At first make or buy citric acid, ammoniacal liquor, tetrabutyl titanate, five nitric hydrate bismuths, sodium hydroxide, ethanol, deionized water and distilled water from market with ordinary method.Then,
Embodiment 1
The concrete steps of preparation are: the first step, and in being the aqueous citric acid solution of 0.8M, concentration adds earlier after ammoniacal liquor regulates pH and be 4.5, again to wherein adding tetrabutyl titanate, and it is stirred 9h down in 50 ℃, obtain settled solution; Wherein, aqueous citric acid solution is formulated in 60 ℃ the water for citric acid being joined temperature, and the mol ratio between tetrabutyl titanate and citric acid is 1: 2.5.Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred 40min down in 80 ℃, obtain even, transparent, thick mixing solutions; Wherein, the five nitric hydrate bismuth aqueous solution are that to stir 25min in 90 ℃ the water formulated for five nitric hydrate bismuths being joined temperature, and the mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 3.5.Sodium hydroxide is added in the mixing solutions again, and continue to stir 25min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 20: 1.The 3rd goes on foot, and earlier resulting solution being placed temperature is 80 ℃ of insulation 0h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product; Wherein, washing is that water washes, and water is deionized water, and the number of times of flushing is 5 times.Afterwards, to the product drying treatment, wherein, drying treatment is to be incubated 6h down for 40 ℃ in temperature.Make as or be similar to Fig. 1～3 and Fig. 5 and the bismuth sodium titanate nanometer flower shown in Fig. 4 a.
Embodiment 2
The concrete steps of preparation are: the first step, and in being the aqueous citric acid solution of 0.9M, concentration adds earlier after ammoniacal liquor regulates pH and be 5, again to wherein adding tetrabutyl titanate, and it is stirred 8h down in 55 ℃, obtain settled solution; Wherein, aqueous citric acid solution is formulated in 63 ℃ the water for citric acid being joined temperature, and the mol ratio between tetrabutyl titanate and citric acid is 1: 2.8.Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred 38min down in 85 ℃, obtain even, transparent, thick mixing solutions; Wherein, the five nitric hydrate bismuth aqueous solution are that to stir 23min in 93 ℃ the water formulated for five nitric hydrate bismuths being joined temperature, and the mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 3.3.Sodium hydroxide is added in the mixing solutions again, and continue to stir 23min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 23: 1.The 3rd goes on foot, and earlier resulting solution being placed temperature is 110 ℃ of insulation 1h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product; Wherein, washing is that water washes, and water is distilled water, and the number of times of flushing is 6 times.Afterwards, to the product drying treatment, wherein, drying treatment is to be incubated 5.5h down for 45 ℃ in temperature.Make as or be similar to Fig. 1～3 and Fig. 5 and the bismuth sodium titanate nanometer flower shown in Fig. 4 c.
Embodiment 3
The concrete steps of preparation are: the first step, and in being the aqueous citric acid solution of 1M, concentration adds earlier after ammoniacal liquor regulates pH and be 5.3, again to wherein adding tetrabutyl titanate, and it is stirred 7h down in 60 ℃, obtain settled solution; Wherein, aqueous citric acid solution is formulated in 65 ℃ the water for citric acid being joined temperature, and the mol ratio between tetrabutyl titanate and citric acid is 1: 3.Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred 35min down in 90 ℃, obtain even, transparent, thick mixing solutions; Wherein, the five nitric hydrate bismuth aqueous solution are that to stir 20min in 95 ℃ the water formulated for five nitric hydrate bismuths being joined temperature, and the mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 3.Sodium hydroxide is added in the mixing solutions again, and continue to stir 20min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 25: 1.The 3rd goes on foot, and earlier resulting solution being placed temperature is 130 ℃ of insulation 5h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product; Wherein, washing is that water washes, and water is deionized water, and the number of times of flushing is 7 times.Afterwards, to the product drying treatment, wherein, drying treatment is to be incubated 5h down for 50 ℃ in temperature.Make as or be similar to Fig. 1～3 and Fig. 5, and be similar to the bismuth sodium titanate nanometer flower shown in Fig. 4 c.
Embodiment 4
The concrete steps of preparation are: the first step, and in being the aqueous citric acid solution of 1.1M, concentration adds earlier after ammoniacal liquor regulates pH and be 5.7, again to wherein adding tetrabutyl titanate, and it is stirred 6h down in 65 ℃, obtain settled solution; Wherein, aqueous citric acid solution is formulated in 68 ℃ the water for citric acid being joined temperature, and the mol ratio between tetrabutyl titanate and citric acid is 1: 3.3.Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred 33min down in 95 ℃, obtain even, transparent, thick mixing solutions; Wherein, the five nitric hydrate bismuth aqueous solution are that to stir 18min in 98 ℃ the water formulated for five nitric hydrate bismuths being joined temperature, and the mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 2.8.Sodium hydroxide is added in the mixing solutions again, and continue to stir 18min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 28: 1.The 3rd goes on foot, and earlier resulting solution being placed temperature is 150 ℃ of insulation 8h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product; Wherein, washing is that water washes, and water is distilled water, and the number of times of flushing is 8 times.Afterwards, to the product drying treatment, wherein, drying treatment is to be incubated 4.5h down for 55 ℃ in temperature.Make as or be similar to Fig. 1～3 and Fig. 5, and be similar to the bismuth sodium titanate nanometer flower shown in Fig. 4 d.
Embodiment 5
The concrete steps of preparation are: the first step, and in being the aqueous citric acid solution of 1.2M, concentration adds earlier after ammoniacal liquor regulates pH and be 6.0, again to wherein adding tetrabutyl titanate, and it is stirred 5h down in 70 ℃, obtain settled solution; Wherein, aqueous citric acid solution is formulated in 70 ℃ the water for citric acid being joined temperature, and the mol ratio between tetrabutyl titanate and citric acid is 1: 3.5.Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred 30min down in 100 ℃, obtain even, transparent, thick mixing solutions; Wherein, the five nitric hydrate bismuth aqueous solution are that to stir 15min in 100 ℃ the water formulated for five nitric hydrate bismuths being joined temperature, and the mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 2.5.Sodium hydroxide is added in the mixing solutions again, and continue to stir 15min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 30: 1.The 3rd goes on foot, and earlier resulting solution being placed temperature is 180 ℃ of insulation 10h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product; Wherein, wash to washing with dehydrated alcohol, the number of times of flushing is 8 times.Afterwards, to the product drying treatment, wherein, drying treatment is to be incubated 4h down for 60 ℃ in temperature.Make as or be similar to Fig. 1～3 and Fig. 5 and the bismuth sodium titanate nanometer flower shown in Fig. 4 d.
Obviously, those skilled in the art can carry out various changes and modification to bismuth sodium titanate nanometer flower of the present invention and preparation method thereof and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (9)
1. bismuth sodium titanate nanometer flower, comprise bismuth-sodium titanate, it is characterized in that described bismuth-sodium titanate is for spherical flower-shaped, described spherical flower is made up of the nanometer sheet of intersecting on one's feet, the length of described nanometer sheet is 250～350nm, highly is that 50～150nm, thickness are 5～15nm, and it is that monocrystalline perovskite bismuth-sodium titanate by three-legged structure constitutes.
2. bismuth sodium titanate nanometer flower according to claim 1 is characterized in that nanometer sheet is the curved surface shape.
3. the preparation method of the described bismuth sodium titanate nanometer flower of claim 1 comprises hydrothermal method, it is characterized in that finishing according to the following steps:
The first step, in being the aqueous citric acid solution of 0.8～1.2M, concentration adds earlier after ammoniacal liquor regulates pH and be 4.5～6.0, again to wherein adding tetrabutyl titanate, and down stir 5h more than in 50～70 ℃ it, obtain settled solution, wherein, the mol ratio between tetrabutyl titanate and citric acid is 1: 2.5～3.5;
Second step, earlier the five nitric hydrate bismuth aqueous solution are mixed mutually with settled solution, and it is stirred more than the 30min down in 80～100 ℃, obtain even, transparent, thick mixing solutions, wherein, mol ratio between the citric acid in five nitric hydrate bismuths and the settled solution is 1: 2.5～3.5, again sodium hydroxide is added in the mixing solutions, and continue to stir more than the 15min, obtain resulting solution, wherein, the mol ratio between the citric acid in sodium hydroxide and the mixing solutions is 20～30: 1;
The 3rd goes on foot, and earlier resulting solution being placed temperature is 80～180 ℃ of insulation 0～10h down, obtains to have sedimentary reaction soln, reaction soln is washed to being neutral again, obtains product, afterwards, to the product drying treatment, makes bismuth sodium titanate nanometer flower.
4. the preparation method of bismuth sodium titanate nanometer flower according to claim 3 is characterized in that aqueous citric acid solution is to join in the water of temperature 〉=60 ℃ citric acid formulated.
5. the preparation method of bismuth sodium titanate nanometer flower according to claim 3 is characterized in that the five nitric hydrate bismuth aqueous solution are formulated for stirring more than the 15min in the water that five nitric hydrate bismuths is joined temperature 〉=90 ℃.
6. the preparation method of bismuth sodium titanate nanometer flower according to claim 3 is characterized in that washing is water or dehydrated alcohol flushing.
7. the preparation method of bismuth sodium titanate nanometer flower according to claim 6 is characterized in that the number of times that washes is 5～8 times.
8. according to the preparation method of claim 4,5 or 6 described bismuth sodium titanate nanometer flowers, it is characterized in that water is deionized water or distilled water.
9. the preparation method of bismuth sodium titanate nanometer flower according to claim 3 is characterized in that drying treatment is to be incubated 4～6h down for 40～60 ℃ in temperature.
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| CN102603292B (en) * | 2012-03-20 | 2014-11-05 | 广西新未来信息产业股份有限公司 | Composite oxide used for sintering microwave dielectric ceramics at low temperature |
| CN103265075B (en) * | 2013-06-05 | 2014-08-06 | 湘潭大学 | Preparation method of bismuth titanate microsphere with multilevel structure |
| CN104211116B (en) * | 2014-08-26 | 2016-01-20 | 浙江大学 | A kind of Bi 4ti 3o 12the preparation method of monocrystal nano rod and product |
| CN104211120B (en) * | 2014-08-26 | 2016-04-13 | 浙江大学 | A kind of micron order Bi 4ti 3o 12the preparation method of rectangular parallelepiped and product |
| CN106179311A (en) * | 2014-11-20 | 2016-12-07 | 熊菊莲 | A kind of photocatalyst of Graphene bismuth titanates composite |
| CN107089680B (en) * | 2017-05-15 | 2019-01-15 | 上海理工大学 | A kind of bismuth-sodium titanate raw powder's production technology |
| CN107055610B (en) * | 2017-05-31 | 2018-06-26 | 济南大学 | It is a kind of to prepare even microballoon Na0.5Bi0.5TiO3The method of crystal |
| CN109160540A (en) * | 2018-08-14 | 2019-01-08 | 沈阳工业大学 | A kind of method that two one-step hydrothermals prepares bismuth-sodium titanate spherical powder |
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