CN103706350B - A kind of In 2o 3/ ZnO heterojunction structure nanotube and preparation method thereof and application - Google Patents
A kind of In 2o 3/ ZnO heterojunction structure nanotube and preparation method thereof and application Download PDFInfo
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Abstract
The present invention relates to a kind of In
2o
3/ ZnO heterojunction structure nanotube and preparation method thereof and application, this nanotube is by In
2o
3nano particle and the distribution of ZnO nano Particle free are formed, ZnO nano particle and In
2o
3the particle diameter of nano particle is respectively 15 ~ 50nm, 10 ~ 15nm; This nanotube internal diameter is 300 ~ 340nm, and external diameter is 360 ~ 400nm, and wall thickness is 15 ~ 30nm.In of the present invention
2o
3/ ZnO heterojunction structure nanotube is hollow tubular structures, than single In
2o
3or ZnO has better photocatalytic activity, under simulated solar irradiation irradiates, in 2 hours, the catalysis degradation modulus of methyl orange reaches 46.6%.This preparation method's step is simple, with low cost, has highlighted the excellent photocatalysis property of heterojunction structure nano material.
Description
Technical field
The present invention relates to the preparation of oxide nano, be specifically related to a kind of In
2o
3/ ZnO heterojunction structure nanotube and preparation method thereof and application, belong to inorganic material chemistry field.
Background technology
Effectively combined by two or more chemical composition and the nano-heterogeneous structure material built, due to the existence of heterogeneous interface, there is multifunctionality, even brand-new functional characteristic, and caused nano material in the application revolution of numerous areas, such as in catalysis, photoelectric device, sensor (see Adv.Mater., 2004,16,1151).At present, people have reported multiple heterojunction structure nano material, such as metal ~ metal heterogeneous structural, metal ~ polymer heterojunction structure, inorganic ~ inorganic semiconductor heterojunction structure, inorganic semiconductor ~ metal heterogeneous structural, inorganic ~ organic semiconductor heterojunction structure and semiconductor ~ carbon nano tube heterojunction structure etc. are (see NanoLetters, 2012,12,2888).For reaching the controlled synthesis of nano-heterogeneous structure material, many preparation methods are suggested and are updated, comprise chemical vapour deposition (CVD), controlled solid phase reaction and solid reaction, electrochemical deposition, template, electrostatic spinning technique etc. (see Chem.Rev., 2012,112,2833).
Electrostatic spinning technique starts from eighties of last century thirties, is one of main method preparing nanofiber.Due to simplicity and the applicability more widely of operating procedure, cause the most attention of people in recent years.The nanofiber prepared due to electrostatic spinning has the character of the aspects such as special electricity, magnetics and optics, in medicine, industry, national defence etc., thus have huge application potential (see Adv.Mater., 2003,5,353).Up to the present, people have successfully synthesized the nanofiber of such as material with carbon element, ceramic material and polymeric material.But existing electrostatic spinning technique often can only obtain solid nanofiber but not nanotube-shaped material (see J.Phys.Chem.C2011,115,362), as CN101905974, CN102251305.
In addition, CN103334179 also reports a kind of method preparing hollow structure indium oxide nanometer fiber, the method adopts polyvinylidene fluoride nanometer fiber to be masterplate, pass through sintering process, obtained hollow structure indium oxide nanometer fiber, the defect of the method is procedure complexity, is not easy to control to the wall thickness etc. of nano tubular structure.
At present, electrostatic spinning technique is adopted directly to prepare In
2o
3/ ZnO heterojunction structure nanotube, has no relevant report.
Summary of the invention
For deficiency of the prior art, the invention provides a kind of In
2o
3/ ZnO heterojunction structure nanotube and preparation method thereof and application.
Technical scheme of the present invention is as follows:
A kind of In
2o
3/ ZnO heterojunction structure nanotube is by In
2o
3nano particle and ZnO nano particle are formed, and the particle diameter of ZnO nano particle is 15 ~ 50nm, In
2o
3the particle diameter of nano particle is 10 ~ 20nm; This nanotube internal diameter is 300 ~ 340nm, and external diameter is 360 ~ 400nm, and wall thickness is 10 ~ 50nm.
According to the present invention, preferably, described In
2o
3the length of/ZnO heterojunction structure nanotube is 500nm ~ 5mm.
According to the present invention, preferably, described In
2o
3/ ZnO heterojunction structure nanotube is by ZnO nano particle and In
2o
3nano particle freely distributes formation; Preferred, In
2o
3the wall thickness of/ZnO heterojunction structure nanotube is 15 ~ 30nm, further preferred 20nm.
According to the present invention, preferably, the mol ratio of described metallic element Zn and In is 1:(0.1 ~ 5.0).
According to the present invention, a kind of In
2o
3the preparation method of/ZnO heterojunction structure nanotube, step is as follows:
(1) zinc acetate and indium nitrate are dissolved in the mixed solvent be made up of deionized water and absolute ethyl alcohol, adding polyvinylpyrrolidone (PVP) is 0.1 ~ 1.0PaS to viscosity, stirs, obtains spinnability colloidal sol;
The mol ratio of described metallic element Zn and In is 1:(0.1 ~ 5.0), in described mixed solvent, the volume ratio of deionized water and absolute ethyl alcohol is 1:(0.2 ~ 8.0); The weight average molecular weight of described polyvinylpyrrolidone is 1,000,000 ~ 2,000,000;
(2) by the spinnability colloidal sol electrostatic spinning that step (1) is obtained, obtained precursor fibre;
The condition of electrostatic spinning: the ejection speed of spinnability colloidal sol is 0.05 ~ 3.0mL/h, and voltage is 10 ~ 28kV, and electrostatic spinning temperature controls at 20 ~ 35 DEG C;
(3) by the precursor fibre that step (2) is obtained, in 60 ~ 80 DEG C of drying 6 ~ 24h, with ramp to 300 ~ 700 DEG C of 0.5 ~ 5 DEG C/min, insulation 60 ~ 120min, obtains ZnO/In
2o
3heterogeneous structural nano pipe.
According to the present invention, preferably, the total amount of the indium nitrate described in step (1) and zinc acetate two kinds of materials and the molal volume of mixed solvent are than being 1:(2 ~ 10) mol/L;
Preferably, the mol ratio of described metallic element Zn and In is 1:(0.2 ~ 1), the In that tube wall is thinner can be prepared
2o
3/ ZnO heterojunction structure nanotube; The mol ratio of Zn and In is greater than or less than 1:(0.1 ~ 5.0) then can not get hollow nanotube, but solid nanofiber, nanobelt or nano-powder;
Preferably, in described mixed solvent, the volume ratio of deionized water and absolute ethyl alcohol is 5:2; Ensure that solute fully dissolves, ensure solvent part volatilization in electrospinning process, complete the solidification of fiber;
Preferably, the weight average molecular weight of described polyvinylpyrrolidone is 1,300,000, can obtain best nano tubular structure; The weight average molecular weight of described polyvinylpyrrolidone is less than 1,000,000, then through finally sintering the nano-powder often obtained, be difficult to obtain regular pattern; The weight average molecular weight of described polyvinylpyrrolidone is greater than 2,000,000, then finally sinter the nanofiber often obtained, but not nano tubular structure.
According to the present invention, preferably, the condition of the middle electrostatic spinning of step (2): the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 20kV, electrostatic spinning temperature controls at 25 ~ 30 DEG C, can obtain the hollow nanotube of uniform diameter, structure the best; When spraying speed and being less than 0.05mL/h, ejection be micron ball, and when ejection speed is greater than 3.0mL/h, obtaining is thicker fiber, the product serious agglomeration obtained after finally sintering.
According to the present invention, electrostatic spinning can carry out with existing equipment.Preferably, by the plastic injector of stainless steel syringe needle, spinnability colloidal sol is sprayed onto electrostatic spinning in dash receiver, the distance between the syringe needle of syringe and dash receiver is 15 ~ 28cm, more preferably 18cm.
According to the present invention, preferably, step is warming up to 500 ~ 600 DEG C with the heating rate of 2 DEG C/min in (3), insulation 60min.Heat up with 2 DEG C/min, make the slowly volatilization such as the water in precursor fibre, organic matter, filament contraction is even; Heat up too fast, fiber easily shrinks, and obtains reunion powder; Heated up slow, polymer unwinds and inorganic salts decomposition are synchronously carried out, and polymer can not play template action, and what obtain is nanofiber.
Zinc acetate and indium nitrate are dissolved in the mixed solvent be made up of deionized water and absolute ethyl alcohol by the present invention, add polyvinylpyrrolidone and obtain spinnability colloidal sol; By controlling rheological characteristic and the spinning technology parameter of spinnability colloidal sol, preparation precursor fibre, then by precursor fibre high-temperature calcination at different temperatures, Zinc oxide nanoparticle and indium oxide nano particle freely distribute and form nanotube tube wall, obtain In
2o
3/ ZnO heterojunction structure nanotube.
According to the present invention, In
2o
3/ ZnO heterojunction structure nanotube is applied to the photocatalytic oxidation degradation of methyl orange.
Beneficial effect of the present invention:
1, In of the present invention
2o
3/ ZnO heterojunction structure nanotube is hollow tubular structures, has good photocatalytic activity, and under simulated solar irradiation irradiates, photocatalysis methyl orange degradation, after 2 hours, degradation rate is 46.6%, significantly improves than the catalytic performance of one-component catalyst.
2, preparation method's step of the present invention is simple, with low cost, and the pipe thickness of nanotube is easy to control.
3, in preparation method of the present invention, preferably material matching makes nanotube be easy to be formed; Preferably spinning condition makes tube diameters even; Preferably calcination condition avoids the fracture of fiber and the doping of a large amount of particulate material.
4, in preparation method of the present invention, calcining heat low (being no more than 700 DEG C), the calcining of a temperature range can complete, and energy consumption is low.
Accompanying drawing explanation
Fig. 1 is that precursor fibre prepared by the embodiment of the present invention 1 after dry 24 hours, calcines X-ray powder diffraction (XRD) spectrogram of gained sample at different temperatures in 60 DEG C of drying boxes; The temperature that curve a, b, c, d and e are corresponding is 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C and 700 DEG C respectively.
Fig. 2 is In prepared by the embodiment of the present invention 1
2o
3eSEM (SEM) photo of/ZnO heterojunction structure nanotube and transmission electron microscope (TEM) photo.
Fig. 3 is In prepared by the embodiment of the present invention 1
2o
3high resolution TEM (HRTEM) photo of/ZnO heterojunction structure nanotube.
Fig. 4 is In prepared by the embodiment of the present invention 2
2o
3eSEM (SEM) photo of/ZnO heterojunction structure nanofiber.
Fig. 5 is In prepared by the embodiment of the present invention 3
2o
3eSEM (SEM) photo of/ZnO heterojunction structure nanotube.
Fig. 6 is the absorbance curve of photocatalytic oxidation degradation methyl orange under simulated visible light irradiates in application examples of the present invention; a
0, a
1, b
1, b
2, b
3be the initial absorbance curve of methyl orange respectively, do not add the curve of any photochemical catalyst illumination after 2 hours, add the curve of Zinc oxide catalytic illumination after 2 hours, add the curve of indium oxide catalyst illumination after 2 hours, add In
2o
3the curve of/ZnO heterojunction structure nano tube catalyst illumination after 2 hours.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described; but be only enumerate as the example of embodiment of the present invention; any restriction is not formed to the present invention, it will be appreciated by those skilled in the art that the amendment in the scope not departing from essence of the present invention and design all falls into protection scope of the present invention.
The electrostatic spinning apparatus used in embodiment is nonstandard electrostatic spinning machine, existing equipment, and woods millions of people industry control Science & Technology Center of Beijing China is on sale.Raw materials usedly in embodiment be conventional reagent, commercial products, wherein: polyvinylpyrrolidone is PVP K90, weight average molecular weight is 1,300,000.
Embodiment 1
A kind of In
2o
3the preparation method of/ZnO heterojunction structure nanotube, step is as follows:
(1) by 0.12gZn (CH
3cOO)
2.2H
2o (6mmol) and 0.46gIn (NO
3)
3.4.5H
2o (1.2mmol) is dissolved in the mixed solution be made up of 4ml deionized water and 10ml absolute ethyl alcohol, is stirred to and dissolves completely; Add 0.71g polyvinylpyrrolidone (PVP), stir, obtain the spinnability colloidal sol that viscosity is 0.5PaS;
(2) spinnability colloidal sol obtained for step (1) is injected electrostatic spinning apparatus, electrostatic spinning, obtained precursor fibre;
The condition of electrostatic spinning: spinnability colloidal sol is sprayed onto in dash receiver with the plastic injector of band stainless steel syringe needle, distance between the syringe needle of syringe and dash receiver is 18cm, the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 20kV, and electrostatic spinning temperature controls at 25 DEG C;
(3) by precursor fibre dry 24h in 60 DEG C of drying boxes that step (2) is obtained, be then placed in high temperature furnace, rise to 600 DEG C with the heating rate of 2 DEG C/min, insulation 60min, obtains In
2o
3/ ZnO heterojunction structure nanotube, its X-ray powder diffraction spectrogram, as Fig. 1 ~ d;
By precursor fibre dry 24h in 60 DEG C of drying boxes in the present embodiment step (3), be warming up to 300 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, the In obtained
2o
3/ ZnO heterojunction structure X-ray powder diffraction spectrogram, as Fig. 1 ~ a;
By precursor fibre dry 24h in 60 DEG C of drying boxes in the present embodiment step (3), be warming up to 400 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, the In obtained
2o
3/ ZnO heterojunction structure X-ray powder diffraction spectrogram, as Fig. 1 ~ b;
By precursor fibre dry 24h in 60 DEG C of drying boxes in the present embodiment step (3), be warming up to 500 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, the In obtained
2o
3/ ZnO heterojunction structure X-ray powder diffraction spectrogram, as Fig. 1 ~ c;
By precursor fibre dry 24h in 60 DEG C of drying boxes in the present embodiment step (3), be warming up to 700 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, the In obtained
2o
3/ ZnO heterojunction structure X-ray powder diffraction spectrogram, as Fig. 1 ~ e;
As shown in Figure 1, after 600 DEG C of sintering, crystallization preferably six side phase ZnO (JCPDS36-1451) and Emission in Cubic In can just be obtained
2o
3(JCPDSNo.65-1730) heterojunction structure nano material.And precursor fiber dry 24h in 60 DEG C of drying boxes, during 300 DEG C of calcinings, sample is amorphous state, but is also nano tube structure; Along with the rising of sintering temperature, diffraction maximum strengthens, and the degree of crystallinity of sample improves; Obtain the obvious product of crystallization when sintering temperature reaches 500 DEG C, and when sintering temperature reaches 600 DEG C, the product of high crystallization can be obtained, obviously can tell In
2o
3and ZnO.
In prepared by the present embodiment
2o
3/ ZnO heterojunction structure nanotube SEM and transmission electron microscope photo are as shown in Figure 2.As shown in Figure 2, this nanotube internal diameter 300 ~ 340nm, external diameter is 360 ~ 400nm, and wall thickness is 15 ~ 30nm, and tube wall has the bulky grain of zinc oxide to inlay.The lattice fringe of nano particle can be found out by Fig. 3 clearly, according to width of fringe, nano particle is marked.
Embodiment 2
A kind of In
2o
3the preparation method of/ZnO heterojunction structure nanotube, step is as follows:
(1) by 0.12gZn (CH
3cOO)
2.2H
2o (6mmol) and 0.46gIn (NO
3)
3.4.5H
2o (1.2mmol) is dissolved in the mixed solution be made up of 4ml deionized water and 11ml absolute ethyl alcohol, is stirred to and dissolves completely; Add 0.71g polyvinylpyrrolidone (PVP), stir, obtain the spinnability colloidal sol that viscosity is 0.4PaS;
(2) spinnability colloidal sol obtained for step (1) is injected electrostatic spinning apparatus, electrostatic spinning, obtained precursor fibre;
The condition of electrostatic spinning: spinnability colloidal sol is sprayed onto in dash receiver with the plastic injector of band stainless steel syringe needle, distance between the syringe needle of syringe and dash receiver is 20cm, the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 20kV, and electrostatic spinning temperature controls at 25 DEG C;
(3) by precursor fibre dry 24h in 60 DEG C of drying boxes that step (2) is obtained, be then placed in high temperature furnace and calcine; Be warming up to 600 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, obtain In
2o
3/ ZnO heterojunction structure nanotube.
Gained In
2o
3the SEM photo of/ZnO heterojunction structure nanotube is distinguished as shown in Figure 4, as shown in Figure 4, and In
2o
3the external diameter of/ZnO heterojunction structure nanotube is 360 ~ 400nm, and this nanotube is by In
2o
3nano particle and ZnO nano particle are formed, ZnO nano particle and In
2o
3the particle diameter of nano particle is respectively 15 ~ 50nm, 10 ~ 15nm.
Embodiment 3
A kind of In
2o
3the preparation method of/ZnO heterojunction structure nanotube, step is as follows:
(1) by 0.12gZn (CH
3cOO)
2.2H
2o (2.5mmol) and 0.56gIn (NO
3)
3.4.5H
2o (2.5mmol) is dissolved in the mixed solution be made up of 10ml deionized water and 4ml absolute ethyl alcohol, is stirred to and dissolves completely; Add 0.71g PVP, stir, obtain the spinnability colloidal sol that viscosity is 0.5PaS;
(2) spinnability colloidal sol obtained for step (1) is injected electrostatic spinning apparatus, electrostatic spinning, obtained precursor fibre;
The condition of electrostatic spinning: spinnability colloidal sol is sprayed onto in dash receiver with the plastic injector of band stainless steel syringe needle, distance between the syringe needle of syringe and dash receiver is 20cm, the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 20kV, and electrostatic spinning temperature controls at 25 DEG C;
(3) by precursor fibre dry 24h in 60 DEG C of drying boxes that step (2) is obtained, be then placed in high temperature furnace and calcine, be warming up to 600 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, obtain In
2o
3/ ZnO heterojunction structure nanotube.
Gained In
2o
3the SEM photo of/ZnO heterojunction structure nanotube as shown in Figure 5, as shown in Figure 5, the present embodiment gained In
2o
3the about 400nm of external diameter of/ZnO heterojunction structure nanotube, wall thickness is about 30nm, the program nanotube, internal diameter is narrower, and tube wall is thicker.
Comparative example 1
A kind of In
2o
3the preparation method of nanotube, step is as follows:
(1) by 0.46gIn (NO
3)
3.4.5H
2o (1.2mmol) is dissolved in the mixed solution be made up of 4ml deionized water and 10ml absolute ethyl alcohol, is stirred to and dissolves completely; Add 7.1g PVP, stir, obtain the spinnability colloidal sol that viscosity is 0.5PaS;
(2) spinnability colloidal sol obtained for step (1) is injected electrostatic spinning apparatus, electrostatic spinning, obtained precursor fibre;
The condition of electrostatic spinning: spinnability colloidal sol is sprayed onto in dash receiver with the plastic injector of band stainless steel syringe needle, distance between the syringe needle of syringe and dash receiver is 20cm, the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 20kV, and electrostatic spinning temperature controls at 25 DEG C;
(3) by precursor fibre dry 24h in 60 DEG C of drying boxes that step (2) is obtained, be then placed in high temperature furnace and calcine, be warming up to 600 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, obtain In
2o
3nanotube.
Comparative example 2
A preparation method for ZnO nanotube/, step is as follows:
(1) by Zn (CH
3cOO)
2.2H
2o (0.6mmol) is dissolved in the mixed solution be made up of 3ml deionized water and 10ml absolute ethyl alcohol, is stirred to and dissolves completely; Add 0.70g PVP, stir, obtain the spinnability colloidal sol that viscosity is 0.5PaS;
(2) spinnability colloidal sol obtained for step (1) is injected electrostatic spinning apparatus, electrostatic spinning, obtained precursor fibre;
The condition of electrostatic spinning: spinnability colloidal sol is sprayed onto in dash receiver with the plastic injector of band stainless steel syringe needle, distance between the syringe needle of syringe and dash receiver is 20cm, the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 20kV, and electrostatic spinning temperature controls at 25 DEG C;
(3) by precursor fibre dry 24h in 60 DEG C of drying boxes that step (2) is obtained, be then placed in high temperature furnace and calcine, be warming up to 600 DEG C with the heating rate of 2 DEG C/min, and at this temperature 60min, obtain ZnO nanotube/.
Application examples
By In prepared by embodiment 1
2o
3/ ZnO heterojunction structure nanotube, the one-component indium oxide nanotube of comparative example 1,2 preparation, zinc oxide nano mitron are applied to the photocatalytic oxidation degradation of methyl orange, analog light source used is the xenon lamp of 500W, and the concentration of methyl orange solution is 20mg/L, and step is as follows:
Indium oxide nanotube, zinc oxide nano mitron prepared by 0.04g comparative example 1,2, In prepared by 0.04g embodiment 1
2o
3/ ZnO heterojunction structure nanotube joins in the methyl orange solution of 20ml respectively, logical cooling water, open analog light source, illumination closes light source in 2 hours, get 4ml solution, supernatant liquor is got in centrifugation, tests its absorbance at top place (464nm), and calculate photocatalytic oxidation degradation efficiency by formula (I) with UV-2550 spectrophotometer.
Formula (I): η=[(A
0-A
t)/A
0] × 100%,
In formula (I), A
0for the absorbance that solution records first, A
tbe the absorbance that records of time after two hours, test result as shown in Figure 6: wherein, the initial absorbance curve of methyl orange is a
0; When not having photochemical catalyst, absorbance curve is a
1, η=1.3%; When photochemical catalyst is ZnO nanotube/, absorbance curve is b
1, η=5.1%; Photochemical catalyst is In
2o
3during nanotube, absorbance curve is b
2, η=13.9%; Photochemical catalyst is In
2o
3during/ZnO heterojunction structure nanotube, absorbance curve is b
3, η=46.6%.
As shown in Figure 6, In
2o
3/ ZnO heterojunction structure nanotube significantly improves than the photocatalysis performance of one-component catalyst.
Claims (11)
1. an In
2o
3/ ZnO heterojunction structure nanotube, is characterized in that this nanotube is by ZnO nano particle and In
2o
3nano particle is formed, ZnO nano particle and In
2o
3the particle diameter of nano particle is respectively 15 ~ 50nm and 10 ~ 15nm; This nanotube internal diameter is 300 ~ 340nm, and external diameter is 360 ~ 400nm, and wall thickness is 10 ~ 50nm; Described In
2o
3/ ZnO heterojunction structure nanotube is by ZnO nano particle and In
2o
3nano particle freely distributes formation, and the mol ratio of described metallic element Zn and In is 1:(0.1 ~ 5.0).
2. according to claim 1
2o
3/ ZnO heterojunction structure nanotube, is characterized in that described In
2o
3the length of/ZnO heterojunction structure nanotube is 500nm ~ 5mm.
3. according to claim 1
2o
3/ ZnO heterojunction structure nanotube, is characterized in that described In
2o
3the wall thickness of/ZnO heterojunction structure nanotube is 15 ~ 30nm.
4. according to claim 3
2o
3/ ZnO heterojunction structure nanotube, is characterized in that described In
2o
3the wall thickness of/ZnO heterojunction structure nanotube is 20nm.
5. the In described in an any one of claim 1 ~ 4
2o
3the preparation method of/ZnO heterojunction structure nanotube, step is as follows:
(1) zinc acetate and indium nitrate are dissolved in the mixed solvent be made up of deionized water and absolute ethyl alcohol, adding polyvinylpyrrolidone (PVP) to viscosity is 0.1 ~ 1.0Pa
.s, stirs, and obtains spinnability colloidal sol;
The mol ratio of described metallic element Zn and In is 1:(0.1 ~ 5.0), in described mixed solvent, the volume ratio of deionized water and absolute ethyl alcohol is 1:(0.2 ~ 8.0); The weight average molecular weight of described polyvinylpyrrolidone is 1,000,000 ~ 2,000,000;
(2) by the spinnability colloidal sol electrostatic spinning that step (1) is obtained, obtained precursor fibre;
The condition of electrostatic spinning: the ejection speed of spinnability colloidal sol is 0.05 ~ 3.0mL/h, and voltage is 10 ~ 28kV, and electrostatic spinning temperature controls at 20 ~ 35 DEG C;
(3) by the precursor fibre that step (2) is obtained, in 60 ~ 80 DEG C of drying 6 ~ 24h, with ramp to 300 ~ 700 DEG C of 0.5 ~ 5 DEG C/min, insulation 60 ~ 120min, obtains ZnO/In
2o
3heterogeneous structural nano pipe.
6. according to claim 5
2o
3the preparation method of/ZnO heterojunction structure nanotube, is characterized in that the total amount of the zinc acetate described in step (1) and indium nitrate two kinds of materials is 1:(2 ~ 10 with the molal volume ratio of mixed solvent) mol/L; The mol ratio of described metallic element Zn and In is 1:(0.2 ~ 1).
7. according to claim 5
2o
3the preparation method of/ZnO heterojunction structure nanotube, is characterized in that the volume ratio of the deionized water described in step (1) and ethanol is 5:2.
8. according to claim 5
2o
3the preparation method of/ZnO heterojunction structure nanotube, is characterized in that the weight average molecular weight of the polyvinylpyrrolidone described in step (1) is 1,300,000.
9. according to claim 5
2o
3the preparation method of/ZnO heterojunction structure nanotube, is characterized in that the condition of electrostatic spinning in step (2): the ejection speed of spinnability colloidal sol is 0.08mL/h, and voltage is 18kV, and electrostatic spinning temperature controls at 20 ~ 25 DEG C.
10. according to claim 5
2o
3the preparation method of/ZnO heterojunction structure nanotube, is characterized in that being warming up to 500 ~ 600 DEG C with the heating rate of 2 DEG C/min in step (3), insulation 60min.
In described in 11. any one of claim 1 ~ 3
2o
3the application of/ZnO heterojunction structure nanotube in the photocatalytic oxidation degradation of methyl orange.
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| CN114695685A (en) * | 2020-12-28 | 2022-07-01 | Tcl科技集团股份有限公司 | Nano material, light-emitting diode device and preparation method thereof |
| CN113231055B (en) * | 2021-04-09 | 2022-08-19 | 厦门大学 | Composite catalyst, method for degrading high molecular organic compound by synergistic electron beam irradiation of composite catalyst and application of composite catalyst in sewage treatment |
| CN113552184B (en) * | 2021-07-29 | 2024-01-09 | 陕西师范大学 | In (In) 2 O 3 (ZnO) 19 Base composite nanotube material, preparation method thereof and gas-sensitive detection of NO 2 Application in (a) |
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| Preparation and characterization of In2O3/ZnO heterostructured microbelts by sol–gel combined with electrospinning method;Fei Zhao et al.;《J Sol-Gel Sci Technol》;20131203;第69卷;第357-363页 * |
| 静电纺丝法制备一维氧化物纳米材料及其传感和发光性质的研究;徐琳;《中国博士学位论文全文数据库工程科技I辑》;20111015(第10期);第63页，第96-104页 * |
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