CN103274455A - Bismuth titanate nano-cuboid and preparation method thereof - Google Patents
Bismuth titanate nano-cuboid and preparation method thereof Download PDFInfo
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- CN103274455A CN103274455A CN2013102208654A CN201310220865A CN103274455A CN 103274455 A CN103274455 A CN 103274455A CN 2013102208654 A CN2013102208654 A CN 2013102208654A CN 201310220865 A CN201310220865 A CN 201310220865A CN 103274455 A CN103274455 A CN 103274455A
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Abstract
The invention discloses a bismuth titanate nano-cuboid and a preparation method thereof. The bismuth titanate nano-cuboid has a regular shape, a smooth surface and square undersurfaces. The side length of the bismuth titanate nano-cuboid is 50-300 nm and the height of the bismuth titanate nano-cuboid is 100-400 nm. The preparation method of the nano-cuboid is as follows. First, sodium dodecyl benzene sulfonate is added into bismuth titanate solution with a concentration of 0.02-0.2 mol/L, and stirred until dissolved. NaOH water solution is then added to obtain precipitates. Then, the precipitates are placed in a sealed reactor with the temperature of 200-230 DEG C, with heat preservation for 16-20 h. The precipitates are then washed until the precipitates are neutral. The precipitates are then dried in a drying oven to obtain bismuth titanate nano-cuboids. The bismuth titanate nano-cuboid can achieve controllable and regular growth through a surfactant. The bismuth titanate nano-cuboid is regular in shape and provides convenience to the nano micro-machining technology or the like. The bismuth titanate nano-cuboid has wide application prospects in modern micro-electronics, micro-electro-mechanical system, information storage, new energy, environmental protection or the like.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, particularly relate to a kind of bismuth titanates nanometer rectangular parallelepiped and preparation method thereof.
Background technology
The performance of functional materials depends on their pattern, size and structure to a great extent, and the functional materials of particular geometric pattern has unique physics and chemical property.Therefore, the variation of the pattern of functional materials and size is very important for the physicochemical property of exploring material.
Bismuth titanates (Bi
4Ti
3O
12BTO) be the material of an eka-bismuth laminated perovskite structure, it has excellent ferroelectric properties and photoelectric properties, at aspects such as modern microelectronics, MEMS (micro electro mechanical system), information storage wide application prospect is arranged, and is that potentialization substitutes one of candidate material of leaded ferroelectric material.And it also has excellent photocatalysis performance, and important potential application is also being arranged aspect novel energy and the environment protection.
Bismuth titanates is by (Bi
2O
2)
2+Layer and (Bi
2Ti
3O
10)
2-Layer is alternately arranged and to be formed, and connecting this two-layer is the most weak Bi-O key of bond energy.In crystal growing process, the fastest direction of growth velocity is the strongest direction of chemical bond.Hence one can see that, and the Growth Habit of bismuth titanates is to be parallel to the aspect growth, generates sheet structure easily.Therefore, the pattern of bismuth titanates crystal is more single, bismuth titanates nanometer rectangular structure does not still have report, the bismuth titanates nanometer structure of preparing the pattern novelty is all having very important significance aspect theoretical fundamental research and the practical application, and rectangular structure can facilitate for nanometer micro-processing technology etc., for the practical application of nano material lays the foundation.
Summary of the invention
The object of the present invention is to provide a kind of bismuth titanates nanometer rectangular parallelepiped and preparation method thereof.
Bismuth titanates nanometer rectangular shape rule of the present invention, smooth surface, the bottom surface is square, the length of side is 40nm～600nm, 45nm～500nm, 50～300nm, preferred 70-250nm, more preferably 90-200nm, high (degree) is 100～400nm, preferably 120-300nm, more preferably 130-250nm, more preferably 150-200nm.
A kind of preparation method of bismuth titanates nanometer rectangular parallelepiped, it comprises following step:
The first step: the ethylene glycol monomethyl ether solution of preparation bismuth titanates;
Second step: tensio-active agent is joined in the solution of the first step, be stirred to dissolving;
The 3rd step: aqueous sodium hydroxide solution is added in the solution in second step, obtain precipitation;
The 4th step: earlier precipitation being placed temperature is that 200～230 ℃ closed reactor is incubated 16～20h, again with its washing to being
Neutrality, drying treatment in loft drier then.
A kind of preparation method of bismuth titanates nanometer rectangular parallelepiped, used solvent is ethylene glycol monomethyl ether in the bismuth titanates solution in the first step, the concentration of this bismuth titanates solution is 0.02～0.2mol/L.
A kind of preparation method of bismuth titanates nanometer rectangular parallelepiped, the tensio-active agent that adds in second step is Sodium dodecylbenzene sulfonate.
A kind of preparation method of bismuth titanates nanometer rectangular parallelepiped, the surfactant concentrations that adds in second step is 0.08～0.12mol/L.
A kind of preparation method of bismuth titanates nanometer rectangular parallelepiped, the concentration sodium hydroxide that adds in the 3rd step is 4～6mol/L.
A kind of preparation method of bismuth titanates nanometer rectangular parallelepiped, the volume ratio of second step with the 3rd step solution is 5:3～7:1.
Bismuth titanates nanometer rectangular shape rule, smooth surface that the present invention makes.
The present invention has realized the controlled growth regularity of bismuth titanates nanometer rectangular parallelepiped by the control of tensio-active agent, and technological process is simple, and cost is low, is easy to accomplish scale production.The bismuth titanates nanometer rectangular shape rule that the present invention is prepared, for nanometer micro-processing technology etc. facilitates, this product has wide application prospect at aspects such as modern microelectronics, MEMS (micro electro mechanical system), information storage, novel energy and environment protection.
Description of drawings
The stereoscan photograph of the bismuth titanates nanometer rectangular parallelepiped that Fig. 1 obtains for the invention process case 1.
The X-ray diffractogram of the bismuth titanates nanometer rectangular parallelepiped that Fig. 2 obtains for the invention process case 2.
Embodiment
Below in conjunction with concrete embodiment technical scheme of the present invention is described further.
Case study on implementation 1
The first step: 0.08mol/L five water Bismuth trinitrates and 0.06mol/L butyl (tetra) titanate are dissolved in the ethylene glycol monomethyl ether;
Second step: the 0.08mol/L Sodium dodecylbenzene sulfonate is dissolved in the solution of the first step, adds ethylene glycol monomethyl ether to 25ml;
The 3rd step: 4mol/L sodium hydroxide is dissolved in the deionized water preparation 15ml aqueous sodium hydroxide solution;
The 4th step: the aqueous sodium hydroxide solution of the 3rd step preparation is joined in the solution in second step, obtain white precipitate, continue to stir 5h, transfer in the polytetrafluoroethyllining lining, in the stainless steel cauldron of then this liner being packed into, be heated to 230 ℃ of reaction 16h, after naturally cooling to room temperature after reaction is finished, outwell the upper strata stillness of night, with the precipitation distilled water of bottom, ethanol repeatedly cleans, and puts into 80 ℃ of dry 12h of vacuum drying oven.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 2
The first step: 0.4mol/L five water Bismuth trinitrates and 0.3mol/L butyl (tetra) titanate are dissolved in the ethylene glycol monomethyl ether;
Second step: the 0.1mol/L Sodium dodecylbenzene sulfonate is dissolved in the solution of the first step, adds ethylene glycol monomethyl ether to 30ml;
The 3rd step: 5mol/L sodium hydroxide is dissolved in the deionized water preparation 10ml aqueous sodium hydroxide solution;
The 4th step: the solution in the 3rd step is joined in the solution in second step, obtain white precipitate, continue to stir 5h, transfer in the polytetrafluoroethyllining lining, in the stainless steel cauldron of then this liner being packed into, be heated to 210 ℃ of reaction 18h, after naturally cooling to room temperature after reaction is finished, outwell the upper strata stillness of night, with the precipitation distilled water of bottom, ethanol repeatedly cleans, and puts into 80 ℃ of dry 12h of vacuum drying oven.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 3
The first step: 0.8mol/L five water Bismuth trinitrates and 0.6mol/L butyl (tetra) titanate are dissolved in the ethylene glycol monomethyl ether;
Second step: the 0.12mol/L Sodium dodecylbenzene sulfonate is dissolved in the solution of the first step, adds ethylene glycol monomethyl ether to 35ml;
The 3rd step: 6mol/L sodium hydroxide is dissolved in the deionized water preparation 5ml aqueous sodium hydroxide solution;
The 4th step: the solution in the 3rd step is joined in the solution in second step, obtain white precipitate, continue to stir 5h, transfer in the polytetrafluoroethyllining lining, in the stainless steel cauldron of then this liner being packed into, be heated to 200 ℃ of reaction 20h, after naturally cooling to room temperature after reaction is finished, outwell the upper strata stillness of night, with the precipitation distilled water of bottom, ethanol repeatedly cleans, and puts into 80 ℃ of dry 12h of vacuum drying oven.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 4
The 0.1mol/L Sodium dodecylbenzene sulfonate is dissolved in the bismuth titanates solution, and all the other are with case study on implementation 1.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 5
The 0.12mol/L Sodium dodecylbenzene sulfonate is dissolved in the bismuth titanates solution, and all the other are with case study on implementation 1.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 6
The 0.08mol/L Sodium dodecylbenzene sulfonate is dissolved in the bismuth titanates solution, and all the other are with case study on implementation 2.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 7
The 0.12mol/L Sodium dodecylbenzene sulfonate is dissolved in the bismuth titanates solution, and all the other are with case study on implementation 2.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 8
The 0.08mol/L Sodium dodecylbenzene sulfonate is dissolved in the bismuth titanates solution, and all the other are with case study on implementation 3.Obtain bismuth titanates nanometer rectangular parallelepiped.
Case study on implementation 9
The 0.1mol/L Sodium dodecylbenzene sulfonate is dissolved in the bismuth titanates solution, and all the other are with case study on implementation 3.Obtain bismuth titanates nanometer rectangular parallelepiped.
Claims (7)
1. bismuth titanates nanometer rectangular parallelepiped is characterized in that: described bismuth titanates nanometer rectangular shape rule, smooth surface, bottom surface are square, and the length of side is 50～300nm, and height is 100～400nm.
2. the preparation method of the described bismuth titanates nanometer of claim 1 rectangular parallelepiped is characterized in that, it comprises following step:
The first step: the ethylene glycol monomethyl ether solution of preparation bismuth titanates;
Second step: tensio-active agent is joined in the solution of the first step, be stirred to dissolving;
The 3rd step: aqueous sodium hydroxide solution is added in the solution in second step, obtain precipitation;
The 4th step: earlier precipitation being placed temperature is that 200～230 ℃ closed reactor is incubated 16～20h, again with its washing to being neutral, drying treatment in loft drier then.
3. the preparation method of bismuth titanates nanometer rectangular parallelepiped according to claim 2 is characterized in that: the tensio-active agent that adds in second step is Sodium dodecylbenzene sulfonate.
4. the preparation method of bismuth titanates nanometer rectangular parallelepiped according to claim 2 is characterized in that: the surface that adds in second step
The concentration of promoting agent is 0.08～0.12mol/L.
5. the preparation method of bismuth titanates nanometer rectangular parallelepiped according to claim 2, it is characterized in that: the concentration of bismuth titanates solution is 0.02～0.2mol/L in the first step.
6. the preparation method of bismuth titanates nanometer rectangular parallelepiped according to claim 2 is characterized in that: the concentration sodium hydroxide that adds in the 3rd step is 4～6mol/L.
7. the preparation method of bismuth titanates nanometer rectangular parallelepiped according to claim 2 is characterized in that: the volume ratio of solution is 5:3～7:1 in second step and the 3rd step.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104211120A (en) * | 2014-08-26 | 2014-12-17 | 浙江大学 | Micron-scale Bi4Ti3O12 cuboid and preparation method thereof |
Citations (4)
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| CN102093049A (en) * | 2010-12-22 | 2011-06-15 | 南京工业大学 | Bismuth lanthanum titanate nano-particles with quasi-cubic morphology and preparation method thereof |
| US20110155971A1 (en) * | 2009-12-14 | 2011-06-30 | Board of Regents of the Nevada System of Higher Education, | Hydrothermal synthesis of nanocubes of sillenite type compounds for photovoltaic applications and solar energy conversion of carbon dioxide to fuels |
| US20110281111A1 (en) * | 2010-05-11 | 2011-11-17 | Board Of Regents Of The Nevada System Of Higher Education, On Behalf Of The University Of Nevada, | Synthesis of pyrochlore nanostructures and uses thereof |
| CN102963929A (en) * | 2012-11-16 | 2013-03-13 | 华南理工大学 | Method for preparing lanthanum-doped bismuth titanate nano powder by sol-gel hydrothermal method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110155971A1 (en) * | 2009-12-14 | 2011-06-30 | Board of Regents of the Nevada System of Higher Education, | Hydrothermal synthesis of nanocubes of sillenite type compounds for photovoltaic applications and solar energy conversion of carbon dioxide to fuels |
| US20110281111A1 (en) * | 2010-05-11 | 2011-11-17 | Board Of Regents Of The Nevada System Of Higher Education, On Behalf Of The University Of Nevada, | Synthesis of pyrochlore nanostructures and uses thereof |
| CN102093049A (en) * | 2010-12-22 | 2011-06-15 | 南京工业大学 | Bismuth lanthanum titanate nano-particles with quasi-cubic morphology and preparation method thereof |
| CN102963929A (en) * | 2012-11-16 | 2013-03-13 | 华南理工大学 | Method for preparing lanthanum-doped bismuth titanate nano powder by sol-gel hydrothermal method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211120A (en) * | 2014-08-26 | 2014-12-17 | 浙江大学 | Micron-scale Bi4Ti3O12 cuboid and preparation method thereof |
| 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 |
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