CN103739002A - Preparation method of one-dimensional nanostructured material - Google Patents
Preparation method of one-dimensional nanostructured material Download PDFInfo
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- CN103739002A CN103739002A CN201310321627.2A CN201310321627A CN103739002A CN 103739002 A CN103739002 A CN 103739002A CN 201310321627 A CN201310321627 A CN 201310321627A CN 103739002 A CN103739002 A CN 103739002A
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Abstract
The invention provides a preparation method of one-dimensional nanostructured material, and the method comprises the following steps: (1) placing a proper amount of raw materials into deionized water for dissolving, adding a transparent solution formed by citric acid and glycol, placing the solution into a baking oven at 80 DEG C for forming a sol, and then polymerizing at 140 DEG C for forming a gel resin; (2) placing the formed polymer resin into a crucible with cover, placing the crucible into a box type electric resistance furnace, heating at 400 DEG C for 1 hour for carbonizing the high-molecular polymer, and forming a metal ion -O-C nanometer composite precursor; (3) carrying out a fine grinding for the nanometer composite precursor, placing into a crucible with cover, placing the crucible into a box type electric resistance furnace at 850-1300 DEG C and other temperatures respectively for two-hour sintering, and cooling to room temperature. The preparation method provided by the invention has the advantages of simple operation, and can be used for preparing one-dimensional nanostructured material with uniform morphology and excellent performance at a large scale.
Description
Technical field
The invention belongs to the preparation of nano structural material.
Technical background
One-dimensional nano structure material refers on two-dimensional direction the novel nano-material take nanoscale, length as macro-scale, generally includes nanotube, nanometer rod, nano wire, nano belt and coaxial nano cable etc.In essence, monodimension nanometer material preparation is exactly the linear growth of studying crystal.In recent years, developed the preparation method of a large amount of monodimension nanometer materials, but the growth mechanism of a lot of methods is all identical.According to the feature of growth mechanism, the preparation of monodimension nanometer material can be divided into vapor phase process, liquid phase method and template three major types.
Main mechanism in vapor phase process has: VLS growth mechanism, vapor-solid process; Liquid phase method mainly contains: molten liquid-liquid phase-solid state growth mechanism, solvent-thermal method.Template mainly comprises: electrochemical deposition method, chemical Vapor deposition process, sol-gel method.
Strategy prepared by monodimension nanometer material is on the basis of profound understanding monodimension nanometer material growth mechanism and surface chemistry thereof, to develop the synthetic thought of new control.Under the auxiliary direction of its thought, people can optionally prepare various types of one dimension function nano materials with specified property.Further verify and explore its control strategy, for the control of monodimension nanometer material, synthesize new opportunities and challenges are provided.
Summary of the invention
The object of the invention is to propose a kind of Via Polymeric Precursor Method and prepare the pure and doped one-dimensional nano-structured materials such as oxide compound, carbide and nitride.
Preparation process of the present invention is as follows:
(1) appropriate raw material is dissolved in to deionized water, add citric acid and ethylene glycol to form clear solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
(2) fluoropolymer resin of formation being put into crucible with cover, put into chamber type electric resistance furnace, is high molecular polymer charings at 400 ℃ of heating 1 h, forms the nano combined presoma of metal ion-O-C.
(3) by fine ground nano combined gained presoma, reinstall crucible with cover, put into chamber type electric resistance furnace sintering 2 h under the differing tempss such as 850 ~ 1300 ℃ respectively, be cooled to room temperature.
The described raw material of step of the present invention (1) is a kind of or two or more in metal-salt, or one or more in silicon ester.
The preferred zinc nitrate hexahydrate of the feed metal salt (Zn (NO that step of the present invention (1) is described
3)
26H
2o), aluminum nitrate (Al (NO
3)
3), lead nitrate (Pb (NO
3)
2), tin tetrachloride (SnCl
4), Indium-111 chloride (InCl
3), butter of antimony (SbCl
3), Trichlorobismuthine (BiCl
3), lithium chloride (LiCl), Dysprosium trioxide (Dy
2o
3), Quilonum Retard (Li
2cO
3).
Preferred tetraethyl silicate (the C of raw silicon acid esters that step of the present invention (1) is described
8h
20o
4si).
The citric acid that step of the present invention (1) is described and the ratio of ethylene glycol are 1:4, and the ratio of citric acid and metal ion is 3:1.
The described crucible of step of the present invention (2) is crucible with cover.Carbonization temperature is 400 ℃, and the time is 1 h.
The described sintering temperature of step of the present invention (3) is 900-1300 ℃, and the time is 2 h.
It is simple that polymer precursor of the present invention is prepared the method for one dimension Nano structure, can prepare on a large scale pattern homogeneous, the one-dimensional nano structure material of excellent property, can for present stage one-dimensional nano structure material preparation method reliable reference and using value are provided.
Accompanying drawing explanation
Fig. 1 is the SnO preparing under embodiment 2 conditions
2the stereoscan photograph of one dimension Nano structure.
Fig. 2 is the In preparing under embodiment 3 conditions
2o
3the stereoscan photograph of one dimension Nano structure.
Fig. 3 is the Si preparing under embodiment 7 conditions
3n
4the stereoscan photograph of one dimension Nano structure.
Fig. 4 is the stereoscan photograph of the ZnO:Sb one dimension Nano structure prepared under embodiment 9 conditions.
Fig. 5 is the ZnO:Dy preparing under embodiment 10 conditions, the stereoscan photograph of Li one dimension Nano structure.
Embodiment
Below by embodiment, the Via Polymeric Precursor Method that further describes the present invention's proposition is prepared one-dimensional nano structure material.
Embodiment 1.
Adopt Zn (NO
3)
26H
2o is as starting material.By Zn (NO
3)
26H
2o dissolves in deionized water, then adds citric acid and ethylene glycol, forms transparent solution, puts into baking oven and first at 80 ℃, forms colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Zn-O-C.
Finally, by fine ground this nano combined presoma, pack in crucible with cover, put into chamber type electric resistance furnace sintering 2 hours at 1000 ℃ respectively, under cool to room temperature.
Embodiment 2.
Adopt SnCl
4as starting material.By SnCl
4dissolve in deionized water, then add citric acid and ethylene glycol, form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Sn-O-C.
Finally, by fine ground this nano combined presoma, pack in crucible with cover, put into chamber type electric resistance furnace, sintering 2 hours at 1000 ℃, under cool to room temperature.
Embodiment 3.
Adopt InCl
3as starting material.By InCl
3dissolve in deionized water, then add citric acid and ethylene glycol, form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of In-O-C.
Finally, by fine ground this nano combined presoma, pack in crucible with cover, put into chamber type electric resistance furnace, sintering 2 hours at 900 ℃, under cool to room temperature.
Embodiment 4.
Adopt Zn (NO
3)
26H
2o and SnCl
4as starting material, Zn:Sn=2%(mol ratio).By Zn (NO
3)
26H
2o and SnCl
4dissolve in deionized water, then add citric acid and ethylene glycol, form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Zn-Sn-O-C.
Finally, by fine ground this nano combined presoma, pack in crucible with cover, put into chamber type electric resistance furnace sintering 2 hours at 950 ℃, under cool to room temperature, obtain Zn
2snO
4one dimension Nano structure.
Embodiment 5.
Adopt InCl
3as starting material.By InCl
3dissolve in deionized water, then add citric acid and ethylene glycol, form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of In-O-C.
Finally, by fine ground this nano combined presoma, put into tube furnace middle part, pass into 95%N
2+ 5%NH
3in gas mixture crucible with cover, sintering 2 hours at 1200 ℃, under cool to room temperature, obtains InN one dimension Nano structure.
Embodiment 6.
Adopt Al (NO
3)
3as starting material.By Al (NO
3)
3dissolve in deionized water, then add citric acid and ethylene glycol, form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Al-O-C.
Finally, by fine ground this nano combined presoma, put into tube furnace middle part, pass into 95%N
2+ 5%NH
3in gas mixture crucible with cover, sintering 2 hours at 1250 ℃, under cool to room temperature, obtains AlN one dimension Nano structure.
Embodiment 7.
Adopt tetraethyl silicate as starting material.Tetraethyl silicate is added in deionized water, and add a small amount of acetic acid, stir and allow it be hydrolyzed, form transparent colloidal sol, then add citric acid and ethylene glycol, put into baking oven and first at 80 ℃, form colloidal sols, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Si-O-C.
Finally, by fine ground this nano combined presoma, put into tube furnace middle part, pass into 95%N
2+ 5%NH
3in gas mixture crucible with cover, sintering 2 hours at 1250 ℃, under cool to room temperature, obtains Si
3n
4one dimension Nano structure.
Embodiment 8.
Adopt tetraethyl silicate as starting material.Tetraethyl silicate is added in deionized water, and add a small amount of acetic acid, stir and allow it be hydrolyzed, form transparent colloidal sol, then add citric acid and ethylene glycol, put into baking oven and first at 80 ℃, form colloidal sols, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1h, make high molecular polymer charing, form the nano combined presoma of Si-O-C.
Finally, by fine ground this nano combined presoma, put into tube furnace middle part, pass in the crucible of Ar band of gas lid, sintering 2 hours at 1300 ℃, under cool to room temperature, obtains SiC one dimension Nano structure.
Embodiment 9.
Adopt Zn (NO
3)
26H
2o and SbCl
3as starting material, Sb:Zn=5%(mol ratio).By Zn (NO
3)
26H
2o and SbCl
3dissolve in deionized water, then add citric acid and ethylene glycol, form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Zn-Sb-O-C.
Finally, by fine ground this nano combined presoma, pack in crucible with cover, put into chamber type electric resistance furnace, sintering 2 hours at 1050 ℃, under cool to room temperature, obtains the ZnO one dimension Nano structure of Sb doping.
Embodiment 10.
Adopt Zn (NO
3)
26H
2o, Dy
2o
3and Li
2cO
3as starting material (Dy:Li:Zn=2:2:100, in mol), first Dy
2o
3dissolve in HNO
3form Dy (NO
3) solution.Then appropriate citric acid is dissolved in to nitric acid, then Li
2cO
3with volume required Dy (NO
3) solution adds formation clear solution, then Zn (NO
3)
26H
2o and ethylene glycol add, and form transparent solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃.
The fluoropolymer resin of formation is placed in crucible with cover, puts into chamber type electric resistance furnace, first at 400 ℃ of heating 1 h, make high molecular polymer charing, form the nano combined presoma of Zn-Dy-Li-O-C.
Finally, by fine ground nano combined presoma, pack in crucible with cover, put into chamber type electric resistance furnace sintering 2 hours at 950 ℃, under cool to room temperature, obtain Dy, the ZnO one dimension Nano structure of Li doping.
Claims (3)
1. the preparation method of one-dimensional nano structure material, is characterized in that step is as follows:
(1) appropriate raw material is dissolved in to deionized water, add citric acid and ethylene glycol to form clear solution, put into baking oven and first at 80 ℃, form colloidal sol, then aggregate into gel resin at 140 ℃;
(2) fluoropolymer resin of formation being put into crucible with cover, put into chamber type electric resistance furnace, is high molecular polymer charings at 400 ℃ of heating 1 h, forms the nano combined presoma of metal ion-O-C;
(3) by fine ground nano combined gained presoma, reinstall crucible with cover, put into chamber type electric resistance furnace sintering 2 h under the differing tempss such as 850 ~ 1300 ℃ respectively, be cooled to room temperature;
The described raw material of step (1) is a kind of or two or more in metal-salt, or one or more in silicon ester;
The citric acid that step (1) is described and the ratio of ethylene glycol are 1:4, and the ratio of citric acid and metal ion is 3:1;
The described crucible of step (2) is crucible with cover, and carbonization temperature is 400 ℃, and the time is 1 h;
The described sintering temperature of step (3) is 900-1300 ℃, and the time is 2 h.
2. preparation method according to claim 1, is characterized in that the described feed metal salt of step (1) is zinc nitrate hexahydrate, aluminum nitrate, lead nitrate, tin tetrachloride, Indium-111 chloride, butter of antimony, Trichlorobismuthine, lithium chloride, Dysprosium trioxide, Quilonum Retard.
3. preparation method according to claim 1, is characterized in that the described raw silicon acid esters of step (1) is tetraethyl silicate.
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2013
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Application publication date: 20140423 |