CN102214506B - Method for preparing silicon oxide@zinc silicate@silicon oxide three-layer coaxial nano cable - Google Patents

Method for preparing silicon oxide@zinc silicate@silicon oxide three-layer coaxial nano cable Download PDF

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CN102214506B
CN102214506B CN201110057921A CN201110057921A CN102214506B CN 102214506 B CN102214506 B CN 102214506B CN 201110057921 A CN201110057921 A CN 201110057921A CN 201110057921 A CN201110057921 A CN 201110057921A CN 102214506 B CN102214506 B CN 102214506B
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董相廷
徐淑芝
盖广清
王进贤
浦利
刘桂霞
于淑晶
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Changchun University of Science and Technology
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Abstract

The invention relates to a method for preparing a silicon oxide@zinc silicate@silicon oxide three-layer coaxial nano cable, and belongs to the technical field of nano material preparation. The method comprises the following three steps of: (1) preparing spinning solution, namely adding polyvinylpyrrolidone (PVP) and tetraethoxysilane (TEOS) into a mixed solvent of absolute ethanol and chloroform to form core layer and shell layer spinning solution, and adding PVP and zinc nitrate hexahydrate Zn(NO3)2.6H2O into a mixed solvent of N,N-dimethylformamide and glycerin C3H8O3 to form intermediate layer spinning solution; (2) preparing a [TEOS+PVP]@[Zn(NO3)2+PVP+C3H8O3]@[TEOS+PVP] precursor composite coaxial cable by using a coaxial electrostatic spinning technology and a three-layer coaxial spinneret under the conditions that voltage is 12kV, the curing distance is 15cm, the room temperature is between 15 and 18 DEG C, and relative humidity is 45 to 50 percent; and (3) preparing the SiO2@Zn2SiO4@SiO2 three-layer coaxial nano cable, namely performing heat treatment on the precursor composite coaxial cable, raising the temperature at a rate of 1 DEG C/min, preserving heat at the temperature of 900 DEG C for 8 hours, reducing the temperature to 200 DEG C at a rate of 1 DEG C/min, and naturally cooling to room temperature so as to obtain the SiO2(core layer)@Zn2SiO4(intermediate layer)@SiO2(shell layer) three-layer coaxial nano cable with the diameter of 600 to 700nm and the length of more than 100mu m.

Description

A kind of method for preparing three layers of coaxial nano cable of silica silicic acid zinc silica
Technical field
The present invention relates to the nano material preparation technical field, relate to a kind of method for preparing three layers of coaxial nano cable of silica silicic acid zinc silica specifically.
Background technology
The preparation and the property research of monodimension nanometer materials such as nano wire, nano belt, nanotube and nano-cable are one of forward position focuses of present material science research field.Especially nano-cable because of performances such as its unique electricity, magnetics, mechanics, occupies critical role at aspects such as following nano electron device, electric transmission, luminescent devices, has caused showing great attention to of scientific circles.Coaxial nano cable is the nano material with core shell structure, and sandwich layer is conductor or semi-conductive nano wire, and shell is heterogeneous conductor or insulator shell, and sandwich layer and shell are coaxial.Different according to the nano-cable sandwich layer with the shell material, can be divided into following several types: semiconductor-insulator, semiconductor-semiconductor, insulator-insulator, macromolecule-metal, macromolecule-semiconductor, macromolecule-macromolecule, metal-metal, semiconductor-metal etc.The research of coaxial nano cable is started in the mid-90; Development later in 2000 is swifter and more violent; Up to the present; Many methods that prepare coaxial nano cable on the basis of original preparation quasi-one-dimensional nanometer material, have been developed, like: laser ablation method, hydro thermal method, sol-gel process, based on nanometer collimation method, chemical vapour deposition technique, hot carbon reduction method etc.Adopt different synthetic methods, different types of material has successfully been prepared hundreds of coaxial nano cable, as: Si/SiO 2, SiC/SiO 2, La (OH) 3/ Ni (OH) 2, Ag/SiO 2, Si 3N 4/ SiO 2, Te/PVA, InN/In 2O 3And the Fe/C/BN of three-decker, Si/SiO 2/ C, α-Si 3N 4/ Si/SiO 2, Si/SiO 2/ BN, Ga/Ga 2O 3/ ZnO etc.Continue to explore new synthetic technology, constantly develop and improve the preparation science of coaxial nano cable, obtain high-quality coaxial nano cable, be still the main direction of present coaxial nano cable research.
Zinc silicate Zn 2SiO 4Be a kind of good luminous host material of doping, luminous efficiency is high, aspect luminescent device, is widely used, owing to have good thermal stability, chemical stability and insulating properties, also can be used as anticorrosive paint and dielectric substance and is applied to other industrial circle.Silicon oxide sio 2Be a kind of common resistant to elevated temperatures functional material, be easy to form the construction of cable and obtain paying attention to.Use SiO 2To Zn 2SiO 4Coat and be expected to produce new character and application.Do not see through SiO at present 2And Zn 2SiO 4Make up SiO 2Zn 2SiO 4SiO 2The report of three layers of coaxial nano cable, the expression core shell structure, i.e. the construction of cable, this cable is three layers of construction of cable, sandwich layer intermediate layer shell, sandwich layer are SiO 2, the intermediate layer is Zn 2SiO 4, shell is SiO 2, this nano-cable has particular structural, uses widely in the hope of obtaining.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning); This method is a kind of effective ways that prepare continuous, as to have macro length micro nanometer fiber, is at first proposed in 1934 by Formhals.This method mainly is used for preparing high polymer nanometer fiber; It is characterized in that making charged Polymer Solution or melt in electrostatic field, to receive the traction of electrostatic force and spray by nozzle; Invest the receiving screen on opposite, thereby realize wire drawing, solvent evaporation at normal temperatures then; Perhaps melt is cooled to normal temperature and solidifies, and obtains micro nanometer fiber.Over nearly 10 years, occurred adopting electrospinning process to prepare the technical scheme of inorganic compound such as oxidate nano fiber at the inorfil preparing technical field, described oxide comprises TiO 2, ZrO 2, Y 2O 3, Y 2O 3: RE 3+(RE 3+=Eu 3+, Tb 3+, Er 3+, Yb 3+/ Er 3+), NiO, Co 3O 4, Mn 2O 3, Mn 3O 4, CuO, SiO 2, Al 2O 3, V 2O 5, ZnO, Nb 2O 5, MoO 3, CeO 2, LaMO 3(M=Fe, Cr, Mn, Co, Ni, Al), Y 3Al 5O 12, La 2Zr 2O 7Deng metal oxide and composite oxide of metal.Electrostatic spinning technique is improved; Adopt coaxial spinning head, spinning solution is injected into respectively in interior pipe and the outer tube, when adding High Level DC Voltage; Solution in the inner and outer pipes is pulled out by electric field force simultaneously; Solidify the back and form coaxial nano cable, also promptly obtain the double-layer coaxial nano-cable, this technology promptly is a coaxial electrostatic spinning technology.This technology of usefulness such as Wang Ce has prepared silica polymer co-axial nano fiber (SCI, 2005,26 (5): 985-987); The expression core shell structure, the material of front is a sandwich layer, the material of back is a shell; Be the sandwich layer shell structurre, also be the double-deck construction of cable; Utilizations such as Dong Xiangting should technology prepare TiO 2SiO 2Sub-micron coaxial cable (chemical journal, 2007,65 (23): 2675-2679), ZnOSiO 2Coaxial nano cable (Chinese Journal of Inorganic Chemistry, 2010,26 (1), 29-34) and Al 2O 3/ SiO 2Coaxial ultra micro cable (silicate journal, 2009,37 (10): 1712-1717); Han, et al adopt should technology have prepared PU (Core/PC (Shell) composite nano fiber (and Polymer Composites, 2006,10:381-386).At present, do not see and utilize coaxial electrostatic spinning technology to prepare SiO 2Zn 2SiO 4SiO 2The relevant report of three layers of coaxial nano cable.
When utilizing electrostatic spinning technique to prepare nano material, the structure of the composition of the kind of raw material, the molecular weight of high polymer templates, spinning solution, spinning process parameter, Technology for Heating Processing and spinning head all has material impact to the pattern and the size of final products.The present invention adopts coaxial electrostatic spinning technology, and three layers of coaxial spinning head that spinning head adopts the stainless steel tubule of three different sizes to be nested together and to form are with tetraethoxysilane TEOS, polyvinylpyrrolidone PVP, absolute ethyl alcohol CH 3CH 2OH and chloroform CHCl 3Mixed liquor be sandwich layer and shell layer spinning solution, with zinc nitrate hexahydrate Zn (NO 3) 26H 2O, N, dinethylformamide DMF and glycerine C 3H 8O 3Mixed liquor be the intermediate layer spinning solution, the viscosity and the non-intersolubility between each layer spinning solution of control sandwich layer, intermediate layer and shell layer spinning solution are most important, under the process conditions of the best, obtain [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma, i.e. sandwich layer intermediate layer shell structurre composite cable, pass through high-temperature heat treatment again after, obtain the SiO of novel structure 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable.
Summary of the invention
Preparation Fe/C/BN in background technology, Si/SiO 2/ C, α-Si 3N 4/ Si/SiO 2, Si/SiO 2/ BN, Ga/Ga 2O 3Three layers of coaxial nano cable of/ZnO, employing be carbon thermal reduction and gas-solid growth method, laser ablation method and thermal evaporation etc.What the use coaxial electrostatic spinning technology in the background technology prepared is double-layer coaxial nano-cables such as inorganic matter inorganic matter, inorganic matter macromolecule and macromolecule high molecular nanometer cable, and the structure of employed raw material, template, solvent, spinning head is different with method of the present invention with the final objective product.The present invention uses coaxial electrostatic spinning technology, adopts three layers of coaxial spinning head to prepare the SiO of novel structure 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable are with amorphous state SiO 2Be sandwich layer and shell, crystalline state Zn 2SiO 4Be the intermediate layer, sandwich layer SiO 2Diameter is 340nm-400nm, intermediate layer Zn 2SiO 4Thickness is 65nm-75nm, shell SiO 2Thickness is 65nm-75nm, and cable size is 600nm-700nm, cable length＞100 μ m.
The present invention realizes like this; At first prepare the sandwich layer with certain viscosity, intermediate layer and the shell layer spinning solution that are used for coaxial electrostatic spinning technology, the viscosity and the non-intersolubility between each layer spinning solution of control sandwich layer, intermediate layer and shell layer spinning solution are most important.Adopt three layers of coaxial spinning head, application coaxial electrostatic spinning technology to carry out electrostatic spinning, under the process conditions of the best, obtain [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma, promptly shell structurre compound coaxial cable in sandwich layer intermediate layer passes through high-temperature heat treatment, PVP and C 3H 8O 3Volatilize after the oxidation Decomposition, the TEOS decomposing oxidation in the sandwich layer generates SiO 2, constituted the sandwich layer of the nano-cable that is generated, the Zn (NO in the intermediate layer 3) 2With with the approaching part TEOS in intermediate layer oxidation reaction to take place at high temperature in the shell generated Zn 2SiO 4, having constituted the intermediate layer of the nano-cable that is generated, remaining TEOS decomposing oxidation has generated SiO in the shell 2, having constituted the shell of nano-cable, to prepare the double-layer coaxial nano-cable different with employing coaxial electrostatic spinning technology of report in the past for these, finally obtain the SiO of novel structure 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable.The steps include:
(1) preparing spinning solution
High polymer templates adopts polyvinylpyrrolidone PVP in the spinning solution, and molecular weight is 1300000, and tetraethoxysilane TEOS is used in the silicon source, and zinc nitrate hexahydrate Zn (NO is used in the zinc source 3) 26H 2O, solvent adopts absolute ethyl alcohol CH 3CH 2OH, N, dinethylformamide DMF, chloroform CHCl 3With glycerine C 3H 8O 3It is 7: 1 CH that TEOS and PVP are joined volume ratio 3CH 2OH and CHCl 3Mixed solvent in, the room temperature lower magnetic force stirs 4h, and leaves standstill 2h, promptly forms sandwich layer and shell layer spinning solution, the mass percent of each material is in sandwich layer and the shell layer spinning solution: TEOS is 19%, PVP is 15%, solvent is 66%.With Zn (NO 3) 26H 2It is 6: 1 DMF and C that O and PVP join volume ratio 3H 8O 3Mixed solvent in, the room temperature lower magnetic force stirs 4h, and leaves standstill 2h, promptly forms the intermediate layer spinning solution, the mass percent of each material is in the spinning solution of intermediate layer: Zn (NO 3) 26H 2O is 10%, and PVP is 17%, and solvent is 73%.
(2) preparation [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma
Three layers of coaxial spinning head that spinning head adopts the stainless steel tubule of three different sizes to be nested together and to form; Three stainless steel tubule internal diameters are respectively 0.9mm, 1.6mm and 2.0mm; Three good backs of tubule cover are fixing, and the sandwich layer nozzle, joins the sandwich layer spinning solution for preparing in the interior pipe than the short about 0.5mm of shell nozzle than intermediate layer nozzle, intermediate layer nozzle; The intermediate layer spinning solution joins in the intervalve; Shell layer spinning solution joins in the outer tube, and adjusting sandwich layer, intermediate layer and shell nozzle are in coaxial, and the gap is enough to guarantee that intermediate layer spinning solution and shell layer spinning solution can flow out smoothly.Adopt coaxial electrostatic spinning technology, use perpendicular spray mode, shower nozzle is vertical with horizontal plane; Applying voltage is 12kV; Shower nozzle is 15cm to the curing distance of receiving screen wire netting, 15 ℃-18 ℃ of indoor temperatures, and relative humidity is 45%-50%; Along with the volatilization of solvent, on as the wire netting of negative pole, just can collect [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma.
(3) preparation SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable
To [TEOS+PVP] [Zn (NO that is obtained 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma heat-treats, heating rate is 1 ℃/min, at 900 ℃ of insulation 8h, naturally cools to room temperature after reducing to 200 ℃ with the speed of 1 ℃/min then, so far obtains SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable.
The SiO of prepared novel structure in the said process 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable are with amorphous state SiO 2Be sandwich layer and shell, crystalline state Zn 2SiO 4Be the intermediate layer, sandwich layer SiO 2Diameter is 340nm-400nm, intermediate layer Zn 2SiO 4Thickness is 65nm-75nm, shell SiO 2Thickness is 65nm-75nm, and cable size is 600nm-700nm, cable length＞100 μ m.Realized goal of the invention.
Description of drawings
Fig. 1 is SiO 2Zn 2SiO 4SiO 2The XRD spectra of three layers of coaxial nano cable.
Fig. 2 is SiO 2Zn 2SiO 4SiO 2The SEM photo of three layers of coaxial nano cable.
Fig. 3 is SiO 2Zn 2SiO 4SiO 2The EDS spectrogram of three layers of coaxial nano cable.
Fig. 4 is SiO 2Zn 2SiO 4SiO 2The TEM photo of three layers of coaxial nano cable, the double accompanying drawing that makes an abstract of this figure.
Embodiment
Embodiment: it is 7: 1 absolute ethyl alcohol CH that tetraethoxysilane TEOS and polyvinylpyrrolidone PVP (molecular weight is 1300000) are joined volume ratio 3CH 2OH and chloroform CHCl 3Mixed solvent in, the room temperature lower magnetic force stirs 4h, and leaves standstill 2h, promptly forms sandwich layer and shell layer spinning solution, the mass percent of each material is in sandwich layer and the shell layer spinning solution: TEOS is 19%, PVP is 15%, solvent is 66%.With zinc nitrate hexahydrate Zn (NO 3) 26H 2It is 6: 1 N, dinethylformamide DMF and glycerine C that O and PVP join volume ratio 3H 8O 3Mixed solvent in, the room temperature lower magnetic force stirs 4h, and leaves standstill 2h, promptly forms the intermediate layer spinning solution, the mass percent of each material is in the spinning solution of intermediate layer: Zn (NO 3) 26H 2O is 10%, and PVP is 17%, and solvent is 73%.Adopt coaxial electrostatic spinning technology to spray silk.Three layers of coaxial spinning head that spinning head adopts the stainless steel tubule of three different sizes to be nested together and to form; Three stainless steel tubule internal diameters are respectively 0.9mm, 1.6mm and 2.0mm; Three good backs of tubule cover are fixing, and the sandwich layer nozzle, joins the sandwich layer spinning solution for preparing in the interior pipe than the short about 0.5mm of shell nozzle than intermediate layer nozzle, intermediate layer nozzle; The intermediate layer spinning solution joins in the intervalve; Shell layer spinning solution joins in the outer tube, and adjusting sandwich layer, intermediate layer and shell nozzle are in coaxial, and the gap is enough to guarantee that intermediate layer spinning solution and shell layer spinning solution can flow out smoothly.Adopt coaxial electrostatic spinning technology, use perpendicular spray mode, shower nozzle is vertical with horizontal plane; Applying voltage is 12kV; Shower nozzle is 15cm to the curing distance of receiving screen wire netting, 15 ℃-18 ℃ of indoor temperatures, and relative humidity is 45%-50%; Along with the volatilization of solvent, on as the wire netting of negative pole, just can collect [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma.With spun [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma heat-treats, heating rate is 1 ℃/min, at 900 ℃ of insulation 8h, naturally cools to room temperature after reducing to 200 ℃ with the speed of 1 ℃/min then, obtains SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable.Prepared SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable have good crystal formation, with amorphous state SiO 2Be sandwich layer and shell, crystalline state Zn 2SiO 4Be the intermediate layer, the d value of its diffraction maximum and relative intensity and Zn 2SiO 4The listed d value of JCPDS standard card (14-0653) consistent with relative intensity, belong to the Zn of iris type 2SiO 4, see shown in Figure 1.Prepared SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable diameter are 600nm-700nm, and cable length＞100 μ m is seen shown in Figure 2.Prepared SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable are formed (the Au conductive layer of surface plating when Au comes from the SEM sample preparation) by Si, Zn and three kinds of elements of O, see shown in Figure 3.Prepared SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable, sandwich layer SiO 2Diameter is 340nm-400nm, intermediate layer Zn 2SiO 4Thickness is 65nm-75nm, shell SiO 2Thickness is 65nm-75nm, sees shown in Figure 4.
The polyvinylpyrrolidone that the present invention selected for use, absolute ethyl alcohol, N, dinethylformamide, glycerine, chloroform, tetraethoxysilane and zinc nitrate hexahydrate are commercially available analysis net product.Used glass apparatus and equipment are commonly used in the laboratory.
Certainly; The present invention also can have other various embodiments; Under the situation that does not deviate from spirit of the present invention and essence thereof; Those of ordinary skill in the art work as can make various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection range of the appended claim of the present invention.

Claims (2)

1. a method for preparing three layers of coaxial nano cable of silica silicic acid zinc silica is characterized in that, uses coaxial electrostatic spinning technology, three layers of coaxial spinning head that spinning head adopts the stainless steel tubule of three different sizes to be nested together and to form, and the preparation product is SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable, i.e. sandwich layer intermediate layer shell structurre, sandwich layer is SiO 2, the intermediate layer is Zn 2SiO 4, shell is SiO 2, the steps include:
(1) preparing spinning solution
High polymer templates adopts polyvinylpyrrolidone PVP in the spinning solution, and tetraethoxysilane TEOS is used in the silicon source, and zinc nitrate hexahydrate Zn (NO is used in the zinc source 3) 26H 2O, solvent adopts absolute ethyl alcohol CH 3CH 2OH, N, dinethylformamide DMF, chloroform CHCl 3With glycerine C 3H 8O 3, it is 7: 1 CH that TEOS and PVP are joined volume ratio 3CH 2OH and CHCl 3Mixed solvent in, the room temperature lower magnetic force stirs 4h, and leaves standstill 2h, promptly forms sandwich layer and shell layer spinning solution, the mass percent of each material is in sandwich layer and the shell layer spinning solution: TEOS is 19%, PVP is 15%, solvent is 66%, with Zn (NO 3) 26H 2It is 6: 1 DMF and C that O and PVP join volume ratio 3H 8O 3Mixed solvent in, the room temperature lower magnetic force stirs 4h, and leaves standstill 2h, promptly forms the intermediate layer spinning solution, the mass percent of each material is in the spinning solution of intermediate layer: Zn (NO 3) 26H 2O is 10%, and PVP is 17%, and solvent is 73%;
(2) preparation [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma
Three layers of coaxial spinning head that spinning head adopts the stainless steel tubule of three different sizes to be nested together and to form; Three stainless steel tubule internal diameters are respectively 0.9mm, 1.6mm and 2.0mm; Three good backs of tubule cover are fixing, and the sandwich layer nozzle, joins the sandwich layer spinning solution for preparing in the interior pipe than the short 0.5mm of shell nozzle than intermediate layer nozzle, intermediate layer nozzle; The intermediate layer spinning solution joins in the intervalve; Shell layer spinning solution joins in the outer tube, and adjusting sandwich layer, intermediate layer and shell nozzle are in coaxial, and the gap is enough to guarantee that intermediate layer spinning solution and shell layer spinning solution can flow out smoothly.Adopt coaxial electrostatic spinning technology, use perpendicular spray mode, shower nozzle is vertical with horizontal plane; Applying voltage is 12kV; Shower nozzle is 15cm to the curing distance of receiving screen wire netting, 15 ℃-18 ℃ of indoor temperatures, and relative humidity is 45%-50%; Along with the volatilization of solvent, on as the wire netting of negative pole, just can collect [TEOS+PVP] [Zn (NO 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma;
(3) preparation SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable
To [TEOS+PVP] [Zn (NO that is obtained 3) 2+ PVP+C 3H 8O 3] the compound coaxial cable of [TEOS+PVP] presoma heat-treats, heating rate is 1 ℃/min, at 900 ℃ of insulation 8h, naturally cools to room temperature after reducing to 200 ℃ with the speed of 1 ℃/min then, so far obtains SiO 2Zn 2SiO 4SiO 2Three layers of coaxial nano cable.
2. a kind of method for preparing three layers of coaxial nano cable of silica silicic acid zinc silica according to claim 1 is characterized in that high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=1300000.
CN201110057921A 2011-03-11 2011-03-11 Method for preparing silicon oxide@zinc silicate@silicon oxide three-layer coaxial nano cable Expired - Fee Related CN102214506B (en)

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CN1858308A (en) * 2006-04-21 2006-11-08 东南大学 Preparing low density porous tin dioxide nano fiber laser target material by electro-static spinning method
CN101694018A (en) * 2009-10-14 2010-04-14 长春理工大学 Process for preparing uropium-doped yttrium oxide @ silicon dioxide bean-shaped nano-cables
CN101763917A (en) * 2010-03-04 2010-06-30 长春理工大学 Method for preparing tin dioxide and titanium dioxide nano cable
CN101786600A (en) * 2010-03-04 2010-07-28 长春理工大学 SnO2/ZnO composite polycrystal nanobelt preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1975504A (en) * 1929-12-07 1934-10-02 Richard Schreiber Gastell Process and apparatus for preparing artificial threads
CN1858308A (en) * 2006-04-21 2006-11-08 东南大学 Preparing low density porous tin dioxide nano fiber laser target material by electro-static spinning method
CN101694018A (en) * 2009-10-14 2010-04-14 长春理工大学 Process for preparing uropium-doped yttrium oxide @ silicon dioxide bean-shaped nano-cables
CN101763917A (en) * 2010-03-04 2010-06-30 长春理工大学 Method for preparing tin dioxide and titanium dioxide nano cable
CN101786600A (en) * 2010-03-04 2010-07-28 长春理工大学 SnO2/ZnO composite polycrystal nanobelt preparation method

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Inventor after: Dong Xiangting

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Inventor after: Wang Jinxian

Inventor after: Pu Li

Inventor after: Liu Guixia

Inventor after: Yu Shujing

Inventor before: Dong Xiangting

Inventor before: Xu Shuzhi

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Inventor before: Wang Jinxian

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