CN102515177A - Preparation method of stannic oxide/silica composite nano-particle - Google Patents
Preparation method of stannic oxide/silica composite nano-particle Download PDFInfo
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- CN102515177A CN102515177A CN2011104348617A CN201110434861A CN102515177A CN 102515177 A CN102515177 A CN 102515177A CN 2011104348617 A CN2011104348617 A CN 2011104348617A CN 201110434861 A CN201110434861 A CN 201110434861A CN 102515177 A CN102515177 A CN 102515177A
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Abstract
The invention discloses a preparation method of a stannic oxide/silica composite nano-particle. The stannic oxide/silica composite nano-particle has a sea urchin-shaped structure. The preparation method provided by the invention comprises the following steps that one or more silicon sources and one or more tin sources are dissolved into a mixed solvent of water and ethanol so that a precursor solution is obtained; and the precursor solution is fed into a burning reactor by an injection pump and then undergoes a hydrolysis reaction at a reaction temperature of 1500 to 2000 DEG C, wherein spherical silica particles are produced in a fire and then heterogeneous nucleation and oriented growth of stannic oxide on the surfaces of the spherical silica particles are carried out so that the stannic oxide/silica composite nano-particles having sea urchin-shaped structures are obtained finally. The preparation method provided by the invention adopts simple equipment, can be realized easily and is conducive to realization of industrial continuous preparation.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to a kind of preparation method with tindioxide/silicon-dioxide composite nanometer particle of sea urchin shape knot.
Background technology
The conductor oxidate nano material has its unique light, electrical property, and is very extensive in the application in fields such as Laser Devices, nanoelectronics, nanophotonics.In order to obtain particular performances, people become various patterns with the conductor oxidate nano material preparation, like nanotube, nanometer rod, nano wire, nano belt, nanometer ball, nanocubes etc.But these structures and performance are single, also have some defective separately, cause it to limit the application of semiconductor material.Therefore, thereby at present one of focus of research is to emerge new three-dimensional structure with these structures are compound each other, so that better properties is arranged.
Tindioxide is a kind of n type semiconductor oxide material of excellent property, and it has wide band gap (3.62eV), low resistivity (10
-4～10
-6Ω cm) rare high light transmittance and in other semi-conductors, thereby be ideal electrode of solar battery and sensor material.Particularly carried out very deeply to the research in sensor application field, wherein better performances is nanometer rod, nano belt, nano-hollow ball and the composite structure between them.At present, the compound method of the three dimensional composite structure of tindioxide mainly is hydrothermal method, template, growth method etc. layer by layer, and aforesaid method often exists complicated process of preparation, severe reaction conditions, highly energy-consuming, yields poorly and introduce problems such as impurity.
Summary of the invention
The object of the present invention is to provide a kind of apparatus and process simple, easy to operate, be easy to realize that industrial continuous preparation has the preparation method of the tindioxide/silicon dioxide nano composite material of sea urchin shape structure, to overcome the above-mentioned defective of existing in prior technology.
The present invention conceives as follows:
Flame is a kind of quick, pyritous reaction process, and with low cost aspect the preparation nano material, product purity is high.High temperature in the formation of these structures and the flame, the thermodynamic property between reaction process and the different components is relevant fast.
The present invention is exactly a difference of utilizing different presomas speed of reaction and nucleation rate in thermal-flame, the slower SnO of control speed of reaction
2At speed of reaction SiO faster
2Surface heterogeneous nucleation and oriented growth, the Nano composite granules that finally obtains having sea urchin shape structure.
Technical scheme of the present invention is following:
The preparation method of a kind of tindioxide/silicon-dioxide composite nanometer particle with the water-soluble and ethanol mixed solvent of Xi Yuan and silicon source, is mixed with precursor solution; Utilize syringe pump that precursor solution is fed combustion reactor; Reaction is hydrolyzed; Temperature of reaction is 1500～2000 ℃; Flame radicals by which characters are arranged in traditional Chinese dictionaries at said combustion reactor generate silica dioxide granule earlier, go out tindioxide in incorgruous again nucleation of said silica particles and oriented growth then, the final tindioxide/silicon-dioxide composite nanometer particle with sea urchin shape structure that generates;
Water and alcoholic acid volume ratio are 1:5～1:11 in the said mixed solvent, and said Xi Yuan and the silicon source total concn in said mixed solvent is 0.5～1mol/L;
Said Xi Yuan is crystal type tin tetrachloride and/or tin protochloride, and said silicon source is tetraethoxy and/or dichlorodimethylsilane.
The mol ratio in said Xi Yuan and silicon source is 1:1～2:1.
The feeding rate of said precursor solution is 3～4ml/min, and the flow of oxygen is 0.3～0.6m in the said combustion reactor
3/ h, shear pressure are 0.15～0.22MPa.
Silicon-dioxide is that spherical, tindioxide is bar-shaped in said tindioxide/silicon-dioxide composite nanometer particle; With diameter be the said spherical silicon dioxide of 200～400nm be core, said bar-shaped tindioxide on said spherical silicon dioxide surface to outgrowth, the rod length of said bar-shaped tindioxide is that 100～300nm, diameter are 20～30nm.
The present invention compares with conventional art and has the following advantages:
(1) apparatus and process is simple, easy to operate, short output of cycle is high, and large-scale production continuously is easy to industrializing implementation;
(2) long excellent ratio is high on the silica nanosphere, and crystallinity is good;
(3) sea urchin shape controllable structure, through regulating water and alcoholic acid ratio, the mol ratio of silicon and tin in oxygen flow and shear pressure and the presoma can make the nanometer rod of different size and the sea urchin shape structure of centrosphere.
Product of the present invention is the composite structure of nanometer rod and nanometer ball; Nanometer tin dioxide rod links together by means of silica nanosphere; Stability Analysis of Structures has better chemical property than single nanometer tin dioxide rod that disperses, and can be used on fields such as gas sensor, lithium ion battery, catalyzer.
Description of drawings
Fig. 1 is the XRD figure of embodiment 1 products therefrom;
Fig. 2 is the field emission scanning electron microscope photo of embodiment 1 products therefrom;
Fig. 3 is the common transmission electron microscope photo of embodiment 1 products therefrom;
Fig. 4 is the high-resolution-ration transmission electric-lens photo of embodiment 1 products therefrom.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
Water-soluble and ethanol mixed solvent is mixed with precursor solution with crystallization tin tetrachloride/tetraethoxy; Utilize syringe pump that precursor solution is fed combustion reactor, the reaction that is hydrolyzed, temperature of reaction is 1500 ℃.The spherical silicon dioxide particle generates earlier in flame, and tindioxide is at its surperficial heterogeneous nucleation and oriented growth then, and final generation has the nano composite structure of the tindioxide/silicon-dioxide of sea urchin shape structure.
Wherein: water and alcoholic acid volume ratio are 1:5, and Xi Yuan and the silicon source total concn in said mixed solvent is 0.5mol/L, and the mol ratio in said Xi Yuan and silicon source is 1:1.
The feeding rate of precursor solution is 3ml/min, and the flow of oxygen is 0.3m
3/ h, shear pressure are 0.15MPa.
Shown in Fig. 1～4; Tindioxide/silicon-dioxide the composite nanometer particle of preparation has sea urchin shape structure; The silica spheres that with the diameter is 200nm is a core; To outgrowth, said nanometer tin dioxide rod is grown 100～150nm, diameter 20～30nm to nanometer tin dioxide rod on said nano silicon ball surface.
Embodiment 2
Will be for tin protochloride/dichlorodimethylsilane water-soluble and ethanol mixed solvent, be mixed with precursor solution; Utilize syringe pump that precursor solution is fed combustion reactor, the reaction that is hydrolyzed, temperature of reaction is 2000 ℃.The spherical silicon dioxide particle generates earlier in flame, and tindioxide is at its surperficial heterogeneous nucleation and oriented growth then, and final generation has the nano composite structure of the tindioxide/silicon-dioxide of sea urchin shape structure.
Wherein: water and alcoholic acid volume ratio are 1:11, and Xi Yuan and the silicon source total concn in said mixed solvent is 1mol/L, and the mol ratio in said Xi Yuan and silicon source is 2:1.
The feeding rate of precursor solution is 4ml/min, and the flow of oxygen is 0.6m
3/ h, shear pressure are 0.22MPa.
Tindioxide/silicon-dioxide the composite nanometer particle of preparation has sea urchin shape structure; The silica spheres that with the diameter is 400nm is a core; To outgrowth, said nanometer tin dioxide rod is grown 200～300nm, diameter 20～30nm to nanometer tin dioxide rod on said nano silicon ball surface.
Claims (4)
1. the preparation method of tindioxide/silicon-dioxide composite nanometer particle is characterized in that, with the water-soluble and ethanol mixed solvent of Xi Yuan and silicon source, is mixed with precursor solution; Utilize syringe pump that precursor solution is fed combustion reactor; Reaction is hydrolyzed; Temperature of reaction is 1500～2000 ℃; Flame radicals by which characters are arranged in traditional Chinese dictionaries at said combustion reactor generate silica dioxide granule earlier, go out tindioxide in incorgruous again nucleation of said silica particles and oriented growth then, the final tindioxide/silicon-dioxide composite nanometer particle with sea urchin shape structure that generates;
Water and alcoholic acid volume ratio are 1:5～1:11 in the said mixed solvent, and said Xi Yuan and the silicon source total concn in said mixed solvent is 0.5～1mol/L;
Said Xi Yuan is crystal type tin tetrachloride and/or tin protochloride, and said silicon source is tetraethoxy and/or dichlorodimethylsilane.
2. preparation method according to claim 1 is characterized in that, the mol ratio in said Xi Yuan and silicon source is 1:1～2:1.
3. preparation method according to claim 1 is characterized in that, the feeding rate of said precursor solution is 3～4ml/min, and the flow of oxygen is 0.3～0.6m in the said combustion reactor
3/ h, shear pressure are 0.15～0.22MPa.
4. preparation method according to claim 1; It is characterized in that; Silicon-dioxide is that spherical, tindioxide is bar-shaped in said tindioxide/silicon-dioxide composite nanometer particle; With diameter be the said spherical silicon dioxide of 200～400nm be core, said bar-shaped tindioxide on said spherical silicon dioxide surface to outgrowth, the rod length of said bar-shaped tindioxide is that 100～300nm, diameter are 20～30nm.
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Cited By (3)
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|---|---|---|---|---|
| CN103146396A (en) * | 2013-02-26 | 2013-06-12 | 中南林业科技大学 | Preparation method for tin-doped mesoporous silica smoke suppressant |
| CN108493421A (en) * | 2018-04-08 | 2018-09-04 | 深圳新恒业电池科技有限公司 | A kind of preparation method of lithium ion battery tin-silicon substrate graphene ball negative material |
| CN109081369A (en) * | 2018-07-16 | 2018-12-25 | 杭州电子科技大学 | It is a kind of to prepare SnO using colloidal sol steam fog auto-combustion method2The method of the nano combined bead of amorphous carbon |
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| CN101659440A (en) * | 2009-09-25 | 2010-03-03 | 上海大学 | Preparation method of tin dioxide nano wire |
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| CN103146396A (en) * | 2013-02-26 | 2013-06-12 | 中南林业科技大学 | Preparation method for tin-doped mesoporous silica smoke suppressant |
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| CN108493421A (en) * | 2018-04-08 | 2018-09-04 | 深圳新恒业电池科技有限公司 | A kind of preparation method of lithium ion battery tin-silicon substrate graphene ball negative material |
| CN109081369A (en) * | 2018-07-16 | 2018-12-25 | 杭州电子科技大学 | It is a kind of to prepare SnO using colloidal sol steam fog auto-combustion method2The method of the nano combined bead of amorphous carbon |
| CN109081369B (en) * | 2018-07-16 | 2020-11-17 | 杭州电子科技大学 | SnO prepared by sol-vapor self-combustion method2Method for producing amorphous carbon nanocomposite pellets |
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