CN103274455B - Bismuth titanate nano-cuboid and preparation method thereof - Google Patents
Bismuth titanate nano-cuboid and preparation method thereof Download PDFInfo
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- CN103274455B CN103274455B CN201310220865.4A CN201310220865A CN103274455B CN 103274455 B CN103274455 B CN 103274455B CN 201310220865 A CN201310220865 A CN 201310220865A CN 103274455 B CN103274455 B CN 103274455B
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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 chemistry performance.Therefore, the pattern of functional materials and the variation of size are 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 storages, all has broad application prospects, and is to have potentiality most to substitute one of candidate material of leaded ferroelectric material.And it also has excellent photocatalysis performance, aspect novel energy and environment protection, also there iing important potential application.
Bismuth titanates is by (Bi
2o
2)
2+layer and (Bi
2ti
3o
10)
2-layer alternative arrangement forms, 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 direction that chemical bond is the strongest.Hence one can see that, and the Growth Habit of bismuth titanates is to be parallel to aspect growth, easily generates sheet structure.Therefore, the pattern of bismuth titanates crystal is more single, bismuth titanates nanometer rectangular structure there is no report, the bismuth titanates nanometer structure of preparing pattern novelty is all having very important significance aspect theoretical basis research and 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, bottom surface is square, the length of side is 40nm～600nm, 45nm～500nm, 50～300nm, preferably 70-250nm, more preferably 90-200nm, high (degree) is 100～400nm, preferred 120-300nm, more preferably 130-250nm, more preferably 150-200nm.
A preparation method for 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 of second step, obtain precipitation;
The 4th step: the closed reactor that first precipitation is placed in to temperature and is 200～230 ℃ is incubated 16～20h, then is washed to being
Neutrality, then drying treatment in loft drier.
A preparation method for bismuth titanates nanometer rectangular parallelepiped, in the bismuth titanates solution in the first step, solvent used is ethylene glycol monomethyl ether, the concentration of this bismuth titanates solution is 0.02～0.2mol/L.
A preparation method for bismuth titanates nanometer rectangular parallelepiped, the tensio-active agent adding in second step is Sodium dodecylbenzene sulfonate.
A preparation method for bismuth titanates nanometer rectangular parallelepiped, the concentration of the tensio-active agent adding in second step is 0.08～0.12mol/L.
A preparation method for bismuth titanates nanometer rectangular parallelepiped, the concentration of the sodium hydroxide adding in the 3rd step is 4～6mol/L.
A preparation method for bismuth titanates nanometer rectangular parallelepiped, the volume ratio of second step and the 3rd step solution is 5:3～7:1.
Bismuth titanates nanometer rectangular shape rule, smooth surface that the present invention makes.
The control of the present invention by tensio-active agent has realized the controllable rules of bismuth titanates nanometer rectangular parallelepiped and has grown, and technological process is simple, and cost is low, is easy to accomplish scale production.The prepared bismuth titanates nanometer rectangular shape of the present invention rule, for nanometer micro-processing technology etc. facilitates, this product has broad application prospects at aspects such as modern microelectronics, MEMS (micro electro mechanical system), information storage, novel energy and environment protection.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the bismuth titanates nanometer rectangular parallelepiped that obtains of the invention process case 1.
Fig. 2 is the X-ray diffractogram of the bismuth titanates nanometer rectangular parallelepiped that obtains of 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 ethylene glycol monomethyl ether;
Second step: 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 deionized water to preparation 15ml aqueous sodium hydroxide solution;
The 4th step: the aqueous sodium hydroxide solution of the 3rd step preparation is joined in the solution of second step, obtain white precipitate, continue to stir 5h, transfer in polytetrafluoroethyllining lining, then this liner is packed in stainless steel cauldron, be heated to 230 ℃ of reaction 16h, after having reacted, naturally cool to after room temperature, outwell the upper strata stillness of night, by 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 ethylene glycol monomethyl ether;
Second step: 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 deionized water to preparation 10ml aqueous sodium hydroxide solution;
The 4th step: the solution in the 3rd step is joined in the solution of second step, obtain white precipitate, continue to stir 5h, transfer in polytetrafluoroethyllining lining, then this liner is packed in stainless steel cauldron, be heated to 210 ℃ of reaction 18h, after having reacted, naturally cool to after room temperature, outwell the upper strata stillness of night, by 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 ethylene glycol monomethyl ether;
Second step: 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 deionized water to preparation 5ml aqueous sodium hydroxide solution;
The 4th step: the solution in the 3rd step is joined in the solution of second step, obtain white precipitate, continue to stir 5h, transfer in polytetrafluoroethyllining lining, then this liner is packed in stainless steel cauldron, be heated to 200 ℃ of reaction 20h, after having reacted, naturally cool to after room temperature, outwell the upper strata stillness of night, by 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
0.1mol/L Sodium dodecylbenzene sulfonate is dissolved in 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
0.12mol/L Sodium dodecylbenzene sulfonate is dissolved in 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
0.08mol/L Sodium dodecylbenzene sulfonate is dissolved in 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
0.12mol/L Sodium dodecylbenzene sulfonate is dissolved in 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
0.08mol/L Sodium dodecylbenzene sulfonate is dissolved in 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
0.1mol/L Sodium dodecylbenzene sulfonate is dissolved in bismuth titanates solution, and all the other are with case study on implementation 3.Obtain bismuth titanates nanometer rectangular parallelepiped.
Claims (3)
1. a preparation method for bismuth titanates nanometer rectangular parallelepiped, is characterized in that, it comprises following step:
The first step: five water Bismuth trinitrates and butyl (tetra) titanate are dissolved in ethylene glycol monomethyl ether;
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 of second step, obtain precipitation;
The 4th step: the closed reactor that first precipitation is placed in to temperature and is 200 ~ 230 ℃ is incubated 16 ~ 20 h, then washed to being neutral, then drying treatment in loft drier;
The tensio-active agent adding in second step is Sodium dodecylbenzene sulfonate;
The concentration of the tensio-active agent adding in second step is 0.08～0.12mol/L,
Described bismuth titanates nanometer rectangular shape rule, smooth surface, bottom surface is square, and the length of side is 50～300nm, and height is 100～400nm.
2. according to the preparation method of the bismuth titanates nanometer rectangular parallelepiped described in claim 1, it is characterized in that: the concentration of the sodium hydroxide adding in the 3rd step is 4～6mol/L.
3. the preparation method of bismuth titanates nanometer rectangular parallelepiped according to claim 1, is characterized in that: the solution of second step and the volume ratio of aqueous sodium hydroxide solution are 5:3～7:1.
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| RU2802703C1 (en) * | 2022-12-06 | 2023-08-31 | Федеральное государственное бюджетное учреждение науки Физико-технический институт им. А.Ф. Иоффе Российской академии наук | Method for producing powder of composite bismuth, iron and tungsten oxide with pyrochlore phase structure using microreactor with intensively swirling flows |
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| 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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| 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 |
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| US8900537B2 (en) * | 2010-05-11 | 2014-12-02 | Board Of Regents Of The Nevada System Of Higher Education, On Behalf Of The University Of Nevada, Reno | Synthesis of pyrochlore nanostructures and uses thereof |
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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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2802703C1 (en) * | 2022-12-06 | 2023-08-31 | Федеральное государственное бюджетное учреждение науки Физико-технический институт им. А.Ф. Иоффе Российской академии наук | Method for producing powder of composite bismuth, iron and tungsten oxide with pyrochlore phase structure using microreactor with intensively swirling flows |
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