CN102191571A - Preparation method of coaxial three-layer nano cable NiO@SnO2@TiO2 - Google Patents

Preparation method of coaxial three-layer nano cable NiO@SnO2@TiO2 Download PDF

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CN102191571A
CN102191571A CN2011100579364A CN201110057936A CN102191571A CN 102191571 A CN102191571 A CN 102191571A CN 2011100579364 A CN2011100579364 A CN 2011100579364A CN 201110057936 A CN201110057936 A CN 201110057936A CN 102191571 A CN102191571 A CN 102191571A
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CN102191571B (en
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董相廷
王进贤
宋超
于文生
刘桂霞
徐佳
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Changchun University of Science and Technology
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The invention relates to a preparation method of a coaxial three-layer nano cable NiO@SnO2@TiO2, belonging to the technical field of preparation of nano materials. The method comprises the following three steps: (1) preparation of spinning liquids: adding nickel acetate tetrahydrate and polyvinylpyrrolidone (PVP) into N,N-dimethylformamide (DMF) to form a core layer spinning liquid, adding tin tetrachloride pentahydrate and PVP into DMF to form a middle layer spinning liquid, and adding tetrabutyl titanate, PVP and glacial acetic acid into ethanol to form a shell layer spinning liquid; (2) preparation of [Ni(CH3COO)2+PVP]@[SnCl4+PVP]@[Ti(OC4H9)4+CH3COOH+PVP] precursor composite cable: by using a coaxial electrostatic spinning technology and a coaxial three-layer spinning jet, curing at the room temperature of 22-25 DEG C under the voltage of 18kV, wherein the curing distance is 15cm, and the relative humidity 40-50%; and (3) preparation of coaxial three-layer nano cable NiO@SnO2@TiO2: carrying out heat treatment on the precursor composite cable to obtain the NiO (core layer)@SnO2 (middle layer)@TiO2(shell layer) coaxial three-layer nano cable of which the diameter is 340-434 nm and the length is greater than 300 mu m: heating at a rate of 1 DEG C/min, keeping the temperature of 600 DEG C for 8 hours, cooling at a rate of 1 DEG C/min to 200 DEG C, and naturally cooling to room temperature.

Description

A kind of coaxial three layers of nano-cable NiO@SnO 2@TiO 2The preparation method
Technical field
The present invention relates to the inorganic nano material preparing technical field, relate to a kind of coaxial three layers of nano-cable NiO@SnO specifically 2@TiO 2The preparation method.
Background technology
The preparation of one-dimensional nano structure material and property research are one of forward position focuses of present material science research field.Nano-cable (Nanocables) is because its particular performances, abundant scientific meaning, wide application prospect and the important strategic status of occupying in following nano structure device have caused people's great attention in recent years.The research of coaxial nano cable is started in the mid-90, development later in 2000 is swifter and more violent, and up to the present, people adopt different synthetic methods, different types of material has successfully been prepared hundreds of coaxial nano cable, as: Fe/C, Zn/ZnO, C/C, SiC/C, SiGaN/SiO xN yAnd the Fe-C-BN of three-decker and α-Si 3N 4-Si-SiO 2Deng.In more than ten years in the past, people develop many methods that prepare coaxial nano cable on the basis of original preparation quasi-one-dimensional nanometer material, as: hydro-thermal method, sol-gel process, based on nanometer collimation method, vapor growth method, template 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.
Because titanium dioxide TiO 2Have excellent photocatalysis, high electricity conversion, superpower chemical stability and good performance such as biocompatibility with nickel oxide NiO, thereby obtain extensive use at aspects such as photocatalysis Decomposition organic matter, photocell electrode, pearlescent material, histoorgan, disinfecting, antimicrobials.SnO 2Be a kind of semi-conducting material of extensive use, be used as opacifying agent, catalyst and the sensor material of glaze and enamel.Do not see at present by NiO, SnO 2And TiO 2Make up coaxial three layers of nano-cable NiO@SnO 2@TiO 2Report, @ represents 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 is NiO, the intermediate layer is SnO 2, shell is TiO 2, this nano-cable has special structure, uses widely in the hope of obtaining.
The patent No. technical scheme of a relevant electrospinning process (electrospinning) that has been 1975504 U.S. Patent Publication, 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 is mainly used to prepare high polymer nanometer fiber, it is characterized in that making charged Polymer Solution or melt in electrostatic field, to be subjected to the traction of electrostatic force and spray by nozzle, invest the receiving screen on opposite, thereby realization 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 coaxial double-layer 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), @ represents core shell structure, and the material of @ front is a sandwich layer, and the material of @ back is a shell, be sandwich layer @ shell structurre, also be the double-deck construction of cable; Dong Xiangting etc. utilize this technology to prepare TiO 2@SiO 2Sub-micron coaxial cable (chemical journal, 2007,65 (23): 2675-2679), ZnO@SiO 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 this technology prepared PU (Core)/PC (Shell) composite nano fiber (Polymer Composites, 2006,10:381-386).At present, do not see and utilize coaxial electrostatic spinning technology to prepare NiO@SnO 2@TiO 2The relevant report of coaxial three layers of 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 coaxial three layers of spinning head that spinning head is nested together and is formed by three syringe needles that cut flat different-diameters are with four water acetic acid nickel (CH 3COO) 24H 2O, polyvinylpyrrolidone PVP and N, the mixed liquor of dinethylformamide DMF are the sandwich layer spinning solution, with stannic chloride pentahydrate SnCl 45H 2The mixed liquor of O, PVP and DMF is the intermediate layer spinning solution, with PVP, absolute ethyl alcohol CH 3CH 2OH, glacial acetic acid CH 3COOH and butyl titanate Ti (OC 4H 9) 4Mixed liquor be shell layer spinning solution, the viscosity of control spinning solution is most important, under the process conditions of the best, obtains [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable, i.e. sandwich layer @ intermediate layer @ shell structurre composite cable, pass through high-temperature heat treatment again after, obtain coaxial three layers of nano-cable NiO@SnO of novel structure 2@TiO 2
Summary of the invention
The method for preparing coaxial nano cable in background technology has hydro-thermal method, sol-gel process, based on nanometer collimation method, vapor growth method, template etc., what the use coaxial electrostatic spinning technology in the background technology prepared is coaxial double-layer nanometer cables such as inorganic matter inorganic matter, inorganic matter macromolecule and macromolecule high molecular nanometer cable, and the structure of employed raw material, template agent, 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 coaxial three layers of spinning head to prepare coaxial three layers of nano-cable NiO@SnO of novel structure 2@TiO 2, be sandwich layer with NiO, diameter is 60-80nm; The intermediate layer is SnO 2, thickness is 53-76nm; Shell is TiO 2, thickness is 87-101nm, the diameter of coaxial three layers of nano-cable is 340-434nm, cable length＞300 μ m.
The present invention is achieved in that and at first prepares the sandwich layer with certain viscosity, intermediate layer and the shell layer spinning solution that is used for coaxial electrostatic spinning technology that the viscosity of control spinning solution is most important.Adopt coaxial three layers of spinning head, application coaxial electrostatic spinning technology to carry out electrostatic spinning, under the process conditions of the best, obtain [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable, promptly @ shell structurre composite cable in sandwich layer @ intermediate layer passes through high-temperature heat treatment, PVP and CH 3Volatilize the Ni (CH in the sandwich layer after the COOH oxidation Decomposition 3COO) 2Oxidation Decomposition generates NiO, constitutes the sandwich layer of the nano-cable that is generated, the SnCl in the intermediate layer 4Decomposing oxidation generates SnO 2, the intermediate layer of the nano-cable that formation is generated, the Ti (OC in the shell 4H 9) 4Oxidation Decomposition has generated TiO 2, having constituted the shell of nano-cable, to prepare the coaxial double-layer nano-cable different with employing coaxial electrostatic spinning technology of report in the past for these, finally obtain coaxial three layers of nano-cable NiO@SnO of novel structure 2@TiO 2The steps include:
(1) preparation spinning solution
High polymer templates adopts polyvinylpyrrolidone PVP in the spinning solution, and molecular weight is 90000, and four water acetic acid nickel (CH are used in the nickel source 3COO) 24H 2O, Xi Yuan uses stannic chloride pentahydrate SnCl 45H 2O, butyl titanate Ti (OC is used in the titanium source 4H 9) 4, solvent adopts absolute ethyl alcohol CH 3CH 2OH and N, dinethylformamide DMF, glacial acetic acid CH 3COOH is an additive.With Ni (CH 3COO) 24H 2O and PVP join among the DMF, and the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms the sandwich layer spinning solution, and the mass percent of each material is in the sandwich layer spinning solution: Ni (CH 3COO) 24H 2O is 7%, and PVP is 11%, and DMF is 82%; With SnCl 45H 2O and PVP join among the DMF, and the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms the intermediate layer spinning solution, and the mass percent of each material is in the spinning solution of intermediate layer: SnCl 45H 2O is 8%, and PVP is 11%, and DMF is 81%; With Ti (OC 4H 9) 4, PVP and CH 3COOH joins CH 3CH 2Among the OH, the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms shell layer spinning solution, and the mass percent of each material is in the shell layer spinning solution: Ti (OC 4H 9) 4Be 20%, PVP is 8%, CH 3COOH is 18%, CH 3CH 2OH is 54%.
(2) preparation [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable
Coaxial three layers of spinning head that spinning head is nested together and is formed by three syringe needles that cut flat different-diameters, the sandwich layer shower nozzle is for cutting the 5# stainless steel syringe needle after putting down, external diameter is 0.5mm, internal diameter is 0.232mm, the intermediate layer shower nozzle is for cutting the 12# stainless steel syringe needle after putting down, external diameter is 1.2mm, internal diameter is 0.790mm, and the shell shower nozzle is for cutting the veterinary syringe syringe needle after putting down, and external diameter is 3.6mm, internal diameter is 2.0mm, the sandwich layer spinning solution for preparing is joined in the interior pipe, and the intermediate layer spinning solution joins in the intervalve, and shell layer spinning solution joins in the outer tube, regulate the sandwich layer shower nozzle, successfully flow out to guarantee each layer spinning solution in the gap of intermediate layer shower nozzle and shell shower nozzle, adopt coaxial electrostatic spinning technology, adopt perpendicular spray mode, shower nozzle is vertical with horizontal plane, applying voltage is 18kV, shower nozzle is 15cm to the curing distance of receiving screen wire netting, 22 ℃～25 ℃ of indoor temperatures, and relative humidity is 40%～50%, along with the volatilization of solvent, on as the wire netting of negative pole, just can collect [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable.
(3) the coaxial three layers of nano-cable NiO@SnO of preparation 2@TiO 2
To [Ni (the CH that is obtained 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable heat-treats, and heating rate is 1 ℃/min, at 600 ℃ of insulation 8h, naturally cools to room temperature after reducing to 200 ℃ with the speed of 1 ℃/min then, so far obtains coaxial three layers of nano-cable NiO@SnO 2@TiO 2
Coaxial three layers of nano-cable NiO@SnO of prepared novel structure in the said process 2@TiO 2, be sandwich layer with NiO, diameter is 60-80nm; The intermediate layer is SnO 2, thickness is 53-76nm; Shell is TiO 2, thickness is 87-101nm, the diameter of coaxial three layers of nano-cable is 340-434nm, cable length＞300 μ m.Realized goal of the invention.
Description of drawings
Fig. 1 is [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the SEM photo of presoma composite cable.
Fig. 2 is coaxial three layers of nano-cable NiO@SnO 2@TiO 2XRD spectra.
Fig. 3 is coaxial three layers of nano-cable NiO@SnO 2@TiO 2The SEM photo.
Fig. 4 is coaxial three layers of nano-cable NiO@SnO 2@TiO 2The EDS spectrogram.
Fig. 5 is coaxial three layers of nano-cable NiO@SnO 2@TiO 2The TEM photo, the double accompanying drawing that makes an abstract of this figure.
The specific embodiment
Embodiment: with four water acetic acid nickel (CH 3COO) 24H 2O and polyvinylpyrrolidone PVP (molecular weight is 90000) join N, and among the dinethylformamide DMF, the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms the sandwich layer spinning solution, and the mass percent of each material is in the sandwich layer spinning solution: Ni (CH 3COO) 24H 2O is 7%, and PVP is 11%, and DMF is 82%; With SnCl 45H 2O and PVP join among the DMF, and the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms the intermediate layer spinning solution, and the mass percent of each material is in the spinning solution of intermediate layer: SnCl 45H 2O is 8%, and PVP is 11%, and DMF is 81%; With butyl titanate Ti (OC 4H 9) 4, PVP and glacial acetic acid CH 3COOH joins absolute ethyl alcohol CH 3CH 2Among the OH, the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms shell layer spinning solution, and the mass percent of each material is in the shell layer spinning solution: Ti (OC 4H 9) 4Be 20%, PVP is 8%, CH 3COOH is 18%, CH 3CH 2OH is 54%.Adopt coaxial electrostatic spinning technology to spray silk.Coaxial three layers of spinning head that spinning head is nested together and is formed by three syringe needles that cut flat different-diameters, the sandwich layer shower nozzle is for cutting the 5# stainless steel syringe needle after putting down, external diameter is 0.5mm, internal diameter is 0.232mm, the intermediate layer shower nozzle is for cutting the 12# stainless steel syringe needle after putting down, external diameter is 1.2mm, internal diameter is 0.790mm, the shell shower nozzle is for cutting the veterinary syringe syringe needle after putting down, and external diameter is 3.6mm, and internal diameter is 2.0mm, the sandwich layer spinning solution for preparing is joined in the interior pipe, the intermediate layer spinning solution joins in the intervalve, and shell layer spinning solution joins in the outer tube, regulates the sandwich layer shower nozzle, successfully flow out to guarantee each layer spinning solution in the gap of intermediate layer shower nozzle and shell shower nozzle, adopt perpendicular spray mode, shower nozzle is vertical with horizontal plane, and applying voltage is 18kV, and shower nozzle is 15cm to the curing distance of receiving screen wire netting, 22 ℃～25 ℃ of indoor temperatures, relative humidity is 40%～50%, along with the volatilization of solvent, just can collect [Ni (CH on as the wire netting of negative pole 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable.With spun [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable puts into the temperature programmed control stove and heat-treats, and heating rate is 1 ℃/min, at 600 ℃ of insulation 8h, naturally cools to room temperature after reducing to 200 ℃ with the speed of 1 ℃/min then, obtains coaxial three layers of nano-cable NiO@SnO 2@TiO 2Prepared [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable, see shown in Figure 1.Prepared coaxial three layers of nano-cable NiO@SnO 2@TiO 2Having good crystal formation, is sandwich layer with NiO, and the intermediate layer is SnO 2, the d value of its diffraction maximum and relative intensity and SnO 2The listed d value of JCPDS standard card (41-1445) consistent with relative intensity, belong to tetragonal crystal system, space group is P4 2/ mnm, rutile TiO 2Be shell, the d value of its diffraction maximum and relative intensity and TiO 2The listed d value of JCPDS standard card (21-1276) consistent with relative intensity, belong to tetragonal crystal system, space group is P4 2/ mnm sees shown in Figure 2.Prepared coaxial three layers of nano-cable NiO@SnO 2@TiO 2Diameter be 340-434nm, cable length＞300 μ m is seen shown in Figure 3.Coaxial three layers of nano-cable NiO@SnO 2@TiO 2Form (the Au conductive layer of surface plating when Au comes from the SEM sample preparation) by Ni, Sn, Ti and O element, see shown in Figure 4.Prepared coaxial three layers of nano-cable NiO@SnO 2@TiO 2The diameter of sandwich layer NiO be 60-80nm, intermediate layer SnO 2Thickness be 53-76nm; Shell TiO 2Thickness be 87-101nm, see shown in Figure 5.
Polyvinylpyrrolidone, absolute ethyl alcohol, N that the present invention is selected, dinethylformamide, butyl titanate, four water acetic acid nickel, stannic chloride pentahydrate and glacial acetic acid 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 domain of the appended claim of the present invention.

Claims (2)

1. coaxial three layers of nano-cable NiO@SnO 2@TiO 2The preparation method, it is characterized in that, use coaxial electrostatic spinning technology, coaxial three layers of spinning head that spinning head is nested together and is formed by three syringe needles that cut flat different-diameters, preparing product is coaxial three layers of nano-cable NiO@SnO 2@TiO 2, i.e. sandwich layer @ intermediate layer @ shell structurre, sandwich layer is NiO, the intermediate layer is SnO 2, shell is TiO 2, the steps include:
1) preparation spinning solution
High polymer templates adopts polyvinylpyrrolidone PVP, and four water acetic acid nickel (CH are used in the nickel source 3COO) 24H 2O, Xi Yuan uses stannic chloride pentahydrate SnCl 45H 2O, butyl titanate Ti (OC is used in the titanium source 4H 9) 4, solvent adopts absolute ethyl alcohol CH 3CH 2OH and N, dinethylformamide DMF, glacial acetic acid CH 3COOH is an additive, with Ni (CH 3COO) 24H 2O and PVP join among the DMF, and the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms the sandwich layer spinning solution, and the mass percent of each material is in the sandwich layer spinning solution: Ni (CH 3COO) 24H 2O is 7%, and PVP is 11%, and DMF is 82%, with SnCl 45H 2O and PVP join among the DMF, and the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms the intermediate layer spinning solution, and the mass percent of each material is in the spinning solution of intermediate layer: SnCl 45H 2O is 8%, and PVP is 11%, and DMF is 81%, with Ti (OC 4H 9) 4, PVP and CH 3COOH joins CH 3CH 2Among the OH, the room temperature lower magnetic force stirs 6h, and leaves standstill 3h, promptly forms shell layer spinning solution, and the mass percent of each material is in the shell layer spinning solution: Ti (OC 4H 9) 4Be 20%, PVP is 8%, CH 3COOH is 18%, CH 3CH 2OH is 54%;
(2) preparation [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable
Coaxial three layers of spinning head that spinning head is nested together and is formed by three syringe needles that cut flat different-diameters, the sandwich layer shower nozzle is for cutting the 5# stainless steel syringe needle after putting down, external diameter is 0.5mm, internal diameter is 0.232mm, the intermediate layer shower nozzle is for cutting the 12# stainless steel syringe needle after putting down, external diameter is 1.2mm, internal diameter is 0.790mm, and the shell shower nozzle is for cutting the veterinary syringe syringe needle after putting down, and external diameter is 3.6mm, internal diameter is 2.0mm, the sandwich layer spinning solution for preparing is joined in the interior pipe, and the intermediate layer spinning solution joins in the intervalve, and shell layer spinning solution joins in the outer tube, regulate the sandwich layer shower nozzle, successfully flow out to guarantee each layer spinning solution in the gap of intermediate layer shower nozzle and shell shower nozzle, adopt coaxial electrostatic spinning technology, adopt perpendicular spray mode, shower nozzle is vertical with horizontal plane, applying voltage is 18kV, shower nozzle is 15cm to the curing distance of receiving screen wire netting, 22 ℃～25 ℃ of indoor temperatures, and relative humidity is 40%～50%, along with the volatilization of solvent, on as the wire netting of negative pole, just can collect [Ni (CH 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable;
(3) the coaxial three layers of nano-cable NiO@SnO of preparation 2@TiO 2
To [Ni (the CH that is obtained 3COO) 2+ PVP] @[SnCl 4+ PVP] @[Ti (OC 4H 9) 4+ CH 3COOH+PVP] the presoma composite cable heat-treats, and heating rate is 1 ℃/min, at 600 ℃ of insulation 8h, naturally cools to room temperature after reducing to 200 ℃ with the speed of 1 ℃/min then, so far obtains NiO@SnO 2@TiO 2Coaxial three layers of nano-cable.
2. a kind of coaxial three layers of nano-cable NiO@SnO according to claim 1 2@TiO 2The preparation method, it is characterized in that high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=90000.
CN 201110057936 2011-03-11 2011-03-11 Preparation method of coaxial three-layer nano cable NiO@SnO2@TiO2 Expired - Fee Related CN102191571B (en)

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CN102586945A (en) * 2012-02-21 2012-07-18 长春理工大学 Method for preparing SiO2/SnO2/TiO2 three-component parallel nanofiber bundle
CN102618967A (en) * 2012-04-17 2012-08-01 东华大学 Preparation method of heterojunction nanofiber containing TiO2/SnO2
CN107321358A (en) * 2017-07-12 2017-11-07 三峡大学 A kind of sea cucumber shape SnO2/ NiO composite nano-tube materials and preparation method and application
CN107785565A (en) * 2017-10-31 2018-03-09 湘潭大学 A kind of Sn TiO2The electrostatic spinning preparation method of C nano fiber
CN108987736A (en) * 2018-09-21 2018-12-11 合肥国轩高科动力能源有限公司 A kind of preparation method of coaxial carbon/LiFePO4/graphene nano fiber positive electrode
CN113406155A (en) * 2021-06-23 2021-09-17 长春理工大学 Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof
CN114426302A (en) * 2022-01-10 2022-05-03 东南大学 SnO with hollow structure2Preparation of NiO nanotube and application of NiO nanotube in super capacitor

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Publication number Priority date Publication date Assignee Title
CN102515744A (en) * 2011-12-12 2012-06-27 苏州大学 CaCu3Ti4O12 micro nano sized fiber and its preparation method
CN102515744B (en) * 2011-12-12 2013-07-24 苏州大学 CaCu3Ti4O12 micro nano sized fiber and its preparation method
CN102586945A (en) * 2012-02-21 2012-07-18 长春理工大学 Method for preparing SiO2/SnO2/TiO2 three-component parallel nanofiber bundle
CN102586945B (en) * 2012-02-21 2014-06-11 长春理工大学 Method for preparing SiO2/SnO2/TiO2 three-component parallel nanofiber bundle
CN102618967A (en) * 2012-04-17 2012-08-01 东华大学 Preparation method of heterojunction nanofiber containing TiO2/SnO2
CN107321358A (en) * 2017-07-12 2017-11-07 三峡大学 A kind of sea cucumber shape SnO2/ NiO composite nano-tube materials and preparation method and application
CN107785565A (en) * 2017-10-31 2018-03-09 湘潭大学 A kind of Sn TiO2The electrostatic spinning preparation method of C nano fiber
CN107785565B (en) * 2017-10-31 2021-01-22 湘潭大学 Sn-TiO2Electrostatic spinning preparation method of-C nanofibers
CN108987736A (en) * 2018-09-21 2018-12-11 合肥国轩高科动力能源有限公司 A kind of preparation method of coaxial carbon/LiFePO4/graphene nano fiber positive electrode
CN113406155A (en) * 2021-06-23 2021-09-17 长春理工大学 Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof
CN114426302A (en) * 2022-01-10 2022-05-03 东南大学 SnO with hollow structure2Preparation of NiO nanotube and application of NiO nanotube in super capacitor

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