CN105887332A - Preparation method of nitrogen-doped flexible TiO2-SiO2 nanofiber membrane with visible light catalytic function - Google Patents

Preparation method of nitrogen-doped flexible TiO2-SiO2 nanofiber membrane with visible light catalytic function Download PDF

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CN105887332A
CN105887332A CN201610395493.2A CN201610395493A CN105887332A CN 105887332 A CN105887332 A CN 105887332A CN 201610395493 A CN201610395493 A CN 201610395493A CN 105887332 A CN105887332 A CN 105887332A
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pvp
ethanol
visible light
doping
sio
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张青红
宁伟伟
陈超
王宏志
侯成义
李耀刚
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Donghua University
National Dong Hwa University
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Donghua University
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282—Addition polymers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00—Heating or cooling textile fabrics
    • D06C7/04—Carbonising or oxidising

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Catalysts (AREA)

Abstract

The invention relates to a preparation method of a nitrogen-doped flexible TiO2-SiO2 nanofiber membrane with a visible light catalytic function. The method comprises the steps that 1, at room temperature, a soluble titanium salt is added into an ethanol-acetylacetone mixed solution of PVP, stirring is conducted, a spinning solution A is obtained, a soluble silicon salt is added into an ethanol-dilute nitric acid mixed solution of PVP, stirring is conducted, and a spinning solution B is obtained; 2, the spinning solution B and the spinning solution A are mixed, the mixed liquid is stirred for 0.5 h to 2 h at room temperature, and a spinning solution C is obtained; 3, electrostatic spinning is conducted on the spinning solution C, and PVP non-woven cloth containing titanium and silicon precursors is obtained; 4, the PVP non-woven cloth is calcined and nitrided, and the nitrogen-doped flexible TiO2-SiO2 nanofiber membrane is obtained. The preparation method is simple, easy to control, low in requirement on equipment and suitable for large-scale production; the prepared nitrogen-doped flexible TiO2-SiO2 nanofiber with the visible light catalytic function is regular in morphology, small in diameter and high in specific surface area.

Description

A kind of flexible TiO of the N doping with visible light catalytic2/SiO2The preparation method of nano-fiber film
Technical field
The invention belongs to nanofiber field, particularly to the flexible TiO of a kind of N doping with visible light catalytic2/SiO2Nanometer The preparation method of fiber membrane.
Background technology
In recent years, the semi-conducting material with photocatalytic activity has wide application due to it in the field such as photocatalysis, opto-electronic conversion Prospect and become the focus of research.Wherein titanium dioxide has photocatalytic activity height, stable chemical nature, nontoxic and valency because of it The advantages such as lattice are cheap, and make it all have a wide range of applications in sewage disposal, air cleaning, automatically cleaning field etc..But due to two Titanium oxide powder easy in inactivation, easily reunion, difficult recovery, and substance system can be caused secondary pollution, it is impossible to weight under blood circulation The fatal defects such as multiple utilization, seriously limit the titanic oxide material application development in every field.At present, research worker uses Different methods is prepared for titanium deoxid film, such as sol-gal process, chemical vapour deposition technique, hydro-thermal method, method of electrostatic spinning Deng.Wherein, electrostatic spinning technique can prepare the titanium deoxid film of the 1-dimention nano fibre structure with large specific surface area, And obtain the favor of more researcher.
Single titanium deoxid film often limits its application in practice because of its mechanical strength difference.In order to improve its mechanics Intensity, researcher adds backing material in titanium dioxide.Such as Chen et al. is at Journal of the American Ceramic Society, 2014,97 (6): 1944-1951 report with SiO2As TiO2Backing material and the shelly nanometer that synthesizes Fiber, thin film has preferable flexibility.Wu et al., at Applied Surface Science, synthesizes in 2014,319:136-142 Flexible TiO with ultrafine carbon fiber as backing material2Thin film.Relative to using ultrafine carbon fiber as backing material, with silicon dioxide Resistance to elevated temperatures as the titanium deoxid film of backing material gained is more excellent.
There are two subject matters in titanium dioxide in the research and application of reality: first, being easily combined of photo-generate electron-hole pair And the inactivation caused, cause photocatalysis quantum efficiency low；Secondly as anatase TiO2Energy gap is 3.2eV, can only absorb The wavelength ultraviolet light (only accounting for 3%～the 5% of solar spectrum) less than 387.5nm, causes solar energy utilization ratio extremely low.
For solving above-mentioned two problems, it is proposed that schemes such as noble metal loading, ion doping, semiconductors coupling, load and sensitizations. Wu et al., at .Journal of the American Ceramic Society, has synthesized N doping on 2014,97 (6): 1944-1951 Titanium dioxide/carbon fiber felt, adds titanium dioxide absorption in visible-range, also reduces the recombination rate in electronics and hole, Make it have preferably absorption at visible ray and ultraviolet region, thus have preferable photocatalysis effect.Can be seen that；Nitrogen element is mixed Live together reason TiO2The N-TiO obtained2TiO can be widened2Photoresponse scope, make initial absorption wavelength produce red shift, it is achieved right Effective utilization of visible ray, improves TiO2Photocatalytic activity in visible region.
Summary of the invention
The technical problem to be solved is to provide the flexible TiO of a kind of N doping with visible light catalytic2/SiO2Nanometer The preparation method of fiber membrane, the method is simple, is easily controlled, the highest to equipment requirements, is suitable for large-scale production；It is prepared into To have visible light catalytic N doping flexible TiO2/SiO2Nanofiber regular appearance, diameter is little, and specific surface area is high.
A kind of flexible TiO of the N doping with visible light catalytic of the present invention2/SiO2The preparation method of nano-fiber film, bag Include:
(1) at room temperature, solubility titanium salt is joined in the ethanol/acetylacetone,2,4-pentanedione mixed solution of PVP, stirring, obtain spinning liquid A； Soluble silicon salt is joined in the ethanol/dust technology mixed solution of PVP, stirring, obtain spinning liquid B；
(2) by spinning liquid A in 50～70 DEG C of heated and stirred, then spinning liquid B is encased in syringe, spinning liquid B is noted in 1～2h Enter in spinning liquid A, after injection, 0.5～2h will be stirred under mixing liquid room temperature, and obtain spinning liquid C；Wherein, spinning liquid In C, solubility titanium salt is 1:5～3:1 with the mol ratio of soluble silicon salt；
(3) spinning liquid C is carried out electrostatic spinning, obtain the PVP non-woven fabrics of titaniferous and silicon precursor；
(4) PVP non-woven fabrics step (3) obtained is calcined, nitridation, obtains the flexible TiO of N doping2/SiO2Nanofiber is thin Film.
Solubility titanium salt in described step (1) is butyl titanate, iso-butyl titanate or titanium tetrachloride, solubility titanium salt with The mass volume ratio of the ethanol of PVP/acetylacetone,2,4-pentanedione mixed solution is 1:2～1:8g/mL.
Soluble silicon salt in described step (1) is tetraethyl orthosilicate or KH-560；The ethanol of soluble silicon salt and PVP/ The mass volume ratio of dust technology mixed solution is 1:2～1:5g/mL.
The compound method of the ethanol of the PVP in described step (1)/acetylacetone,2,4-pentanedione mixed solution is: be dissolved in ethanol by PVP To the ethanol solution of PVP, add acetylacetone,2,4-pentanedione, to obtain final product；Wherein, the ethanol solution mass concentration of PVP is 4%～16%, Acetylacetone,2,4-pentanedione is 1:1～1:5 with the mol ratio of solubility titanium salt.
The compound method of the ethanol of the PVP in described step (1)/dust technology mixed solution is: is dissolved in ethanol by PVP and obtaining The ethanol solution of PVP, adds dilute nitric acid solution, to obtain final product；Wherein, the ethanol solution mass concentration of PVP is 4%～16%, Dilute nitric acid solution is 1:5～1:10 with the volume ratio of the ethanol solution of PVP.
The weight average molecular weight of the PVP in described step (1) is 1,300,000.
Electrostatic spinning process parameter in described step (3) is: voltage is 1.2～20,000 volts, and the flow velocity of micro-injection pump is 0.5～2mL/h, spinning head is 10～20cm from the distance of reception device, and reception device is aluminium foil.
Calcining heat in described step (4) is 500～700 DEG C, and calcination time is 1～3h.
Nitridation in described step (4) is particularly as follows: NH30.5～2h is nitrogenized at 500～700 DEG C, NH under atmosphere3Flow velocity is 200～300mL/min.
The mixed method used in the present invention serves vital effect in course of reaction, makes the TiO of synthesis2/SiO2Nanometer Fiber membrane has preferable flexibility, and fiber morphology is regular, and specific surface area is high, absorbs and be remarkably reinforced in visible-range.
The nanofiber regular appearance of gained of the present invention, uniformly, diameter is between 150～300nm, with the tune of preparation technology parameter Whole and change, and its absorption in visible region is remarkably reinforced.
Beneficial effect
(1) preparation method of the present invention is simple, is easily controlled, with low cost, the highest to equipment requirements, is suitable for large-scale production；
(2) the flexible TiO of the N doping with visible light catalytic prepared by the present invention2/SiO2Nanofiber regular appearance is uniform, compares table Area is high, has preferably absorption in visible region, has a wide range of applications in photocatalysis field, can be used for air cleaning, dirty Water harnessing and hydrogen manufacturing etc..
Accompanying drawing explanation
Fig. 1 is the mol ratio of titanium and silicon flexible TiO of N doping when being 1:12/SiO2The digital photograph of nano-fiber film；
Fig. 2 is the mol ratio of titanium and silicon flexible TiO of N doping when being 1:12/SiO2Scanning electron microscope (SEM) figure of nanofiber；
Fig. 3 is the mol ratio of titanium and silicon flexible TiO of N doping when being 2:12/SiO2X-ray diffraction (XRD) figure of nanofiber, figure Middle diffraction maximum is anatase phase titanium dioxide；In figure, abscissa is the 2 θ angles of diffraction, and unit is degree；Vertical coordinate is relative intensity；
Fig. 4 is the mol ratio of titanium and silicon flexible TiO of N doping when being 2:12/SiO2The UV-vis DRS spectrum of nano-fiber film.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
(1) configuration of spinning liquid
Take 0.6g PVP and put into beaker, and be added thereto to dehydrated alcohol 14mL, magnetic agitation 1h；Take 0.5g acetylacetone,2,4-pentanedione solution Join in beaker；The ethanol solution that 3.40ml butyl titanate under agitation joins above-mentioned PVP is molten with the mixing of acetylacetone,2,4-pentanedione In liquid, magnetic agitation 1h, obtain the spinning liquid A of titanium dioxide.
Take 0.3g PVP and put into beaker, and be added thereto to dehydrated alcohol 7mL, magnetic agitation 1h；By positive for 2.10mL silicic acid tetrem Ester joins in the ethanol solution of PVP, is added thereto to the dilute nitric acid solution of 0.6mL pH=2.5 under stirring, magnetic agitation 2h, Obtain the spinning liquid B of silicon dioxide.
Spinning liquid A puts into heated and stirred in 60 DEG C of oil bath pans, then is encased in syringe by spinning liquid B, uses syringe pump by spinning Liquid B is slowly injected in spinning liquid A in 1h, after injection, will mix liquid magnetic agitation 1h under normal temperature condition, and obtain Spinning liquid C.
(2) electrostatic spinning
The precursor spinning liquid C of above-mentioned preparation is carried out spinning on device for spinning, voltage 1.5 ten thousand volts, micro-injection pump are set Flow velocity be 1.5mL/h, spinning head from receive device distance be 18cm, reception device is aluminium foil, thus obtains crisscross PVP/Ti (OBu)4/ TEOS superfine composite nanofiber, diameter is about between 150～300nm.
(3) subsequent heat treatment
By above-mentioned prepared PVP/Ti (OBu)4/ TEOS composite nano fiber puts into Muffle furnace calcining, and heating rate is 3 DEG C/min. When temperature rises to 600 DEG C, constant temperature 2h, obtain flexible TiO2/SiO2Nano-fiber film；Again thin film is put in tube furnace, gas Atmosphere is NH3, heating rate is 3 DEG C/min, NH3Flow velocity is 200mL/min, when temperature rises to 600 DEG C, and constant temperature 1h, i.e. obtain N doping flexibility TiO2/SiO2Nano-fiber film.
Fig. 1 is the flexible TiO of N doping prepared by the present embodiment2/SiO2The digital photograph of nano-fiber film；Fig. 2 is the present embodiment The flexible TiO of the N doping of preparation2/SiO2The scanning electron microscope diagram of nanofiber, it can be seen that the regular appearance of nanofiber, Between a diameter of 150～300nm.
Embodiment 2
(1) configuration of spinning liquid
Taking 2.5g PVP and put into beaker, and be added thereto to dehydrated alcohol 35mL, magnetic agitation solution is homogeneous transparent state；Measure 0.5g acetylacetone,2,4-pentanedione solution joins in beaker；6.80ml butyl titanate is under agitation joined the ethanol solution of above-mentioned PVP with In the mixed solution of acetylacetone,2,4-pentanedione, stir 2h, obtain the spinning liquid A of titanium dioxide；
Take 0.45g PVP and put into beaker, and be added thereto to dehydrated alcohol 6mL, magnetic agitation 1h；By positive for 2.10mL silicic acid tetrem Ester joins in the ethanol solution of PVP, is added thereto to the dilute nitric acid solution of 0.6mL pH=2.5 under stirring, magnetic agitation 1h, Obtain the spinning liquid B of silicon dioxide；
Spinning liquid A is put into heated and stirred in 60 DEG C of oil bath pans, then spinning liquid B is encased in syringe, use syringe pump to spin Silk liquid B is slowly injected in spinning liquid A in 1h, after injection, will mix liquid magnetic agitation 1h under normal temperature condition, To spinning liquid C.
(2) electrostatic spinning
The precursor spinning liquid C of above-mentioned preparation is carried out spinning on device for spinning, voltage 1.8 ten thousand volts, micro-injection pump are set Flow velocity be 1.2mL/h, spinning head from receive device distance be 15cm, reception device is aluminium foil, thus obtains crisscross PVP/Ti (OBu)4/ TEOS superfine composite nanofiber, diameter is about between 150～300nm.
(3) subsequent heat treatment
By above-mentioned prepared PVP/Ti (OBu)4/ TEOS composite nano fiber puts into Muffle furnace calcining, and heating rate is 3 DEG C/min. When temperature rises to 700 DEG C, constant temperature 1.5h, obtain flexible TiO2/SiO2Nano-fiber film；Again thin film is put in tube furnace, Atmosphere is NH3, heating rate is 3 DEG C/min, NH3Flow velocity is 300mL/min, when temperature rises to 700 DEG C, and constant temperature 1.5h, i.e. Obtain the flexible TiO of N doping2/SiO2Nano-fiber film.
Fig. 3 is the flexible TiO of N doping prepared by the present embodiment2/SiO2The X-ray diffractogram of nano-fiber film, reference standard XRD figure stave is bright: the TiO in this nanofiber2For Anatase structure；
Fig. 4 is the flexible TiO of N doping prepared by the present embodiment2/SiO2The UV-vis DRS spectrum of nano-fiber film, After can be seen that nitrogen-doping, the absorption spectrum of nano-fiber film there occurs red shift, and the absorption intensity in visible-range It is remarkably reinforced.

Claims (8)

1. the flexible TiO of a N doping with visible light catalytic2/SiO2The preparation method of nano-fiber film, including:
(1) at room temperature, solubility titanium salt is joined in the ethanol/acetylacetone,2,4-pentanedione mixed solution of PVP, stirring, obtain spinning liquid A； Soluble silicon salt is joined in the ethanol/dust technology mixed solution of PVP, stirring, obtain spinning liquid B；
(2) by spinning liquid A in 50～70 DEG C of heated and stirred, then spinning liquid B is encased in syringe, spinning liquid B is noted in 1～2h Enter in spinning liquid A, after injection, 0.5～2h will be stirred under mixing liquid room temperature, and obtain spinning liquid C；Wherein, spinning liquid In C, solubility titanium salt is 1:5～3:1 with the mol ratio of soluble silicon salt；
(3) spinning liquid C is carried out electrostatic spinning, obtain the PVP non-woven fabrics of titaniferous and silicon precursor；
(4) PVP non-woven fabrics step (3) obtained is calcined, nitridation, obtains the flexible TiO of N doping2/SiO2Nanofiber is thin Film.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: the solubility titanium salt in described step (1) is butyl titanate, iso-butyl titanate or titanium tetrachloride, Solubility titanium salt is 1:2～1:8g/mL with the mass volume ratio of the ethanol/acetylacetone,2,4-pentanedione mixed solution of PVP.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: the soluble silicon salt in described step (1) is tetraethyl orthosilicate or KH-560；Soluble silicon Salt is 1:2～1:5g/mL with the mass volume ratio of the ethanol/dust technology mixed solution of PVP.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: the compound method of the ethanol of the PVP in described step (1)/acetylacetone,2,4-pentanedione mixed solution is: will PVP is dissolved in ethanol the ethanol solution obtaining PVP, adds acetylacetone,2,4-pentanedione, to obtain final product；Wherein, the ethanol solution quality of PVP Concentration is 4%～16%, and acetylacetone,2,4-pentanedione is 1:1～1:5 with the mol ratio of solubility titanium salt.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: the compound method of the ethanol of the PVP in described step (1)/dust technology mixed solution is: by PVP It is dissolved in ethanol the ethanol solution obtaining PVP, adds dilute nitric acid solution, to obtain final product；Wherein, the ethanol solution quality of PVP is dense Degree is 4%～16%, and dilute nitric acid solution is 1:5～1:10 with the volume ratio of the ethanol solution of PVP.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: the electrostatic spinning process parameter in described step (3) is: voltage is 1.2～20,000 volts, trace The flow velocity of syringe pump is 0.5～2mL/h, and spinning head is 10～20cm from the distance of reception device, and reception device is aluminium foil.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: the calcining heat in described step (4) is 500～700 DEG C, and calcination time is 1～3h.
The flexible TiO of a kind of N doping with visible light catalytic the most according to claim 12/SiO2The system of nano-fiber film Preparation Method, it is characterised in that: nitridation in described step (4) is particularly as follows: NH30.5～2h is nitrogenized at 500～700 DEG C under atmosphere, NH3Flow velocity is 200～300mL/min.
CN201610395493.2A 2016-06-06 2016-06-06 Preparation method of nitrogen-doped flexible TiO2-SiO2 nanofiber membrane with visible light catalytic function Pending CN105887332A (en)

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CN106835502A (en) * 2017-01-19 2017-06-13 湖南天健泰荣科技有限公司 A kind of nanofiber mats and preparation method thereof
CN108325564A (en) * 2018-04-03 2018-07-27 青岛大学 Has the flexible TiO of visible light catalytic performance2/PVDF@MoS2Composite nano fiber and preparation method thereof
CN109023727A (en) * 2018-08-30 2018-12-18 华南理工大学 A kind of preparation method for the micro/nano fibrous membrane material that can actively capture PM2.5
CN110143827A (en) * 2019-06-28 2019-08-20 东北大学 A kind of ultra-light elastic inorganic oxide fibres aeroge and preparation method thereof
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CN113737395A (en) * 2021-08-06 2021-12-03 华南理工大学 Flexible titanium dioxide nanofiber membrane and preparation method and application thereof
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CN115418730A (en) * 2022-09-29 2022-12-02 中国人民解放军海军工程大学 Preparation method of silicon dioxide/titanium dioxide infrared heat insulation composite fiber
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