CN107938027A - A kind of pure tungsten nanofiber, its preparation method and application - Google Patents

A kind of pure tungsten nanofiber, its preparation method and application Download PDF

Info

Publication number
CN107938027A
CN107938027A CN201711370838.XA CN201711370838A CN107938027A CN 107938027 A CN107938027 A CN 107938027A CN 201711370838 A CN201711370838 A CN 201711370838A CN 107938027 A CN107938027 A CN 107938027A
Authority
CN
China
Prior art keywords
nanofiber
electrostatic spinning
pure tungsten
preparation
tungstenic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201711370838.XA
Other languages
Chinese (zh)
Other versions
CN107938027B (en
Inventor
李和平
胡三元
严有为
叶品
杨凌霄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huazhong University of Science and Technology
Original Assignee
Huazhong University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Huazhong University of Science and Technology filed Critical Huazhong University of Science and Technology
Priority to CN201711370838.XA priority Critical patent/CN107938027B/en
Publication of CN107938027A publication Critical patent/CN107938027A/en
Application granted granted Critical
Publication of CN107938027B publication Critical patent/CN107938027B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys

Abstract

The invention belongs to field of nanometer material technology, more particularly, to a kind of pure tungsten nanofiber, its preparation method and application.The present invention prepares pure tungsten nanofiber and comprises the following steps:(1) electrostatic spinning liquid is prepared, and transfer them to and electrostatic spinning is carried out in electrospinning device, tungstenic presoma nanofiber is obtained, and the electrostatic spinning liquid is Tungstenic compound and high polymer binder to be dissolved completely in the mixed liquor of water and organic solvent;(2) the tungstenic presoma nanofiber in step (1) is placed in air furnace and is calcined, obtain WO3Nanofiber;(3) by the WO in step (2)3Nanofiber is transferred in high-temperature atmosphere furnace and calcines, and obtains pure tungsten nanofiber.Pure tungsten nanofiber diameter prepared by the present invention is evenly distributed, continuity is good and has excellent electric conductivity, and can realize the large-scale production and extensive use of pure tungsten nanofiber.

Description

A kind of pure tungsten nanofiber, its preparation method and application
Technical field
The invention belongs to field of nanometer material technology, more particularly, to a kind of pure tungsten nanofiber, its preparation method and answers With.
Background technology
As the fast development and popularization of intelligent movable equipment, the transparency electrode market demand are growing.For a long time, tin Leading material of the doped indium oxide (ITO) as transparency electrode market.Due to the rare and its expensive price of phosphide element, seriously Limit the extensive use of ito transparent electrode.In recent years, domestic and international researcher is directed to developing novel transparent electrode material Material, such as conducting polymer thin film, carbon nanotubes, graphene and metal nano net, it is intended to substitute traditional ITO materials.
At present, metal nanometer line becomes the research heat of transparent electrode material of new generation because of its high-transmission rate and high conductivity Point.But the unstable chemcial property of these metal nanometer lines, cause its performance larger with the variation of environmental condition, example As silver can be with H a small amount of in air2S or CO2React, copper is oxidized easily in atmosphere etc. can all reduce leading for nano wire Electrically.The characteristics such as tungsten electric conductivity with good stability, excellent, high-melting-point and high rigidity, are used for for a long time Filament, cutting element and optical instrumentation etc..Therefore, will if high conductivity and good stability with reference to tungsten material It is applied to transparent electrode material, not only can guarantee that the high-quality-factor of transparency electrode, but also it can be made to have in harsh environments There is good performance stability.Thus, the development and application of the preparation of tungsten nanofiber and performance study to transparency electrode has Important scientific value and research significance.
The content of the invention
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of pure tungsten nanofiber, its preparation The characteristics of method and application, it fully combines tungsten nanofiber product and demand, preparation side of the specific aim to pure tungsten nanofiber Method is redesigned, and crucial preparation technology parameter is made choice and optimized, and accordingly obtaining a kind of has good lead Electrically, homogeneous diameter and the pure tungsten nanofiber of higher draw ratio, thus solve the technology of preparing of pure tungsten nanofiber Problem.
To achieve the above object, one side according to the invention, there is provided a kind of preparation method of pure tungsten nanofiber, Include the following steps:
(1) electrostatic spinning liquid is prepared, its electrostatic spinning is obtained into tungstenic presoma nanofiber, the electrostatic spinning liquid is Tungstenic compound and high polymer binder are dissolved in water and the mixed liquor formed in organic solvent;
(2) the tungstenic presoma nanofiber obtained in step (1) is subjected to first time calcining, is obtained by pre-oxidation WO3Nanofiber;Wherein, first time calcining heating rate be 1 DEG C/min~20 DEG C/min, calcining heat is 400 DEG C~ 800 DEG C, soaking time 0.5h~6h;
(3) WO that will be obtained in step (2)3Nanofiber carries out second and calcines, and obtains pure tungsten by high temperature reduction and receives Rice fiber, wherein the heating rate of second of calcining is 1 DEG C/min~20 DEG C/min, calcining heat is 400 DEG C~1000 DEG C, soaking time 0.5h~4h.
Preferably, in step (1), the percentage by weight of each component is respectively in the electrostatic spinning liquid:Tungstenic chemical combination Thing 5%~20%, high polymer binder 20%~40%, organic solvent 15%~25%, water 30%~50%.
Preferably, in step (1), the voltage of the electrostatic spinning is 8kV~40kV, electrostatic spinning distance for 10cm~ 30cm, electrostatic spinning flow velocity are 2mL/h~5mL/h.
Preferably, in step (1), the Tungstenic compound is ammonium metatungstate, wolframic acid or one kind or more in isopropanol tungsten Kind.
Preferably, in step (1), the high polymer binder for polyacrylonitrile, polyvinyl alcohol, vinyl acetate resin or One or more in polyvinylpyrrolidone.
Preferably, in step (1), selected organic solvent is isopropanol, ethanol, n,N-Dimethylformamide, chloroform Or the one or more in ether.
Preferably, the atmosphere of second calcining described in step (3) be ammonia, carbon source gas or one kind in hydrogen or It is a variety of.
A kind of other side according to the invention, there is provided the pure tungsten nanofiber production obtained by preparation method Product.
Other side according to the invention, there is provided a kind of application of the pure tungsten nanofiber product, as saturating Prescribed electrode material.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show Beneficial effect:
1st, the soluble Tungstenic compound of present invention selection is as tungsten source, and selects water and organic solvent to dissolve tungsten source, utilizes Electrostatic spinning technique directly prepares tungstenic presoma nanofiber;
2nd, fabricated in situ pure tungsten nanofiber is realized by calcining twice, is removed first by being calcined in first time air High polymer binder in fiber obtains WO3Nanofiber, then reduces WO in reducing atmosphere stove3Obtain pure tungsten nanofiber;
3rd, the present invention using macromolecule organic as binding agent, by adjust the mass percent of high polymer binder with The viscosity of accurate control electrostatic spinning liquid, can control fiber diameter, and the successful important step of electrostatic spinning process;
4th, the present invention realizes accurately controlling to nanofiber by adjusting electrospinning parameters, and such as improving spinning voltage can To accelerate electrostatic spinning speed, the diameter of nanofiber can be controlled by adjusting the flow velocity of solution;
5th, offer is prepared in situ for pure tungsten nanofiber using carbon source or hydrogen source gas as reducing gas in the present invention Necessary synthesis atmosphere;
6th, the present invention prepare pure tungsten nanofiber calcining heat it is relatively low, both met the reduction bar of tungsten oxide nanofibers Part, also ensure that the continuity of pure tungsten nanofiber;
7th, the present invention prepares pure tungsten nanofiber using electrostatic spinning technique, and this method is simple and quick, cost-effective, is adapted to Large-scale production.
Brief description of the drawings
Fig. 1 is the pure tungsten nanofiber preparation method flow chart constructed by preferred embodiment according to the invention;
The XRD spectrum that it is pure tungsten nanofiber constructed by preferred embodiment 1 according to the invention that Fig. 2, which is,;
Fig. 3 is the pure tungsten nanofiber SEM photograph constructed by preferred embodiment 1 according to the invention;
Fig. 4 is the test device schematic diagram of the pure tungsten nanofiber constructed by preferred embodiment according to the invention;
Fig. 5 is the I-V curve of the pure tungsten nanofiber constructed by preferred embodiment according to the invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below Not forming conflict each other can be mutually combined.
Fig. 1 is the pure tungsten nanofiber preparation method flow chart constructed by preferred embodiment according to the invention, including with Lower step:
(1) electrostatic spinning liquid is prepared, and transfers them to electrostatic spinning in electrospinning device and obtains tungstenic presoma and receive Rice fiber, the electrostatic spinning liquid is the mixed liquor that Tungstenic compound and high polymer binder are dissolved in water and organic solvent In, it is uniformly mixing to obtain the solution of stable homogeneous;Wherein the percentage by weight of each component is respectively in electrostatic spinning liquid:Tungstenic Compound 5%~20%, high polymer binder 20%~40%, organic solvent 15%~25%, water 30%~50%;Static Spinning The voltage of silk is 8kV~40kV, and electrostatic spinning distance is 10cm~30cm, and electrostatic spinning flow velocity is 2mL/h~5mL/h;Contain Tungsten compound is the one or more in ammonium metatungstate, wolframic acid or isopropanol tungsten;High polymer binder is polyacrylonitrile, polyethylene One or more in alcohol, vinyl acetate resin or polyvinylpyrrolidone;Organic solvent is isopropanol, ethanol, N, N- diformazans One or more in base formamide, chloroform or ether.
(2) the tungstenic presoma nanofiber obtained in step (1) is placed in air furnace and calcined for the first time, pass through pre- oxygen Change obtains WO3Nanofiber.Wherein, air furnace heating rate is 1 DEG C/min~20 DEG C/min, and calcining heat is 400 DEG C~800 DEG C, soaking time 0.5h~4h.
(3) WO that will be obtained in step (2)3Nanofiber, which is placed in high-temperature atmosphere furnace, carries out second of calcining, gas atmosphere It is one or more in ammonia, carbon source gas or hydrogen to enclose, pure tungsten nanofiber is obtained by high temperature reduction, wherein atmosphere furnace Heating rate is 1 DEG C/min~20 DEG C/min, and calcining heat is 400 DEG C~1000 DEG C, soaking time 0.5h~4h.
Calcining pre-oxidation for the first time obtains WO3, can be after cooling by gained WO after nanofiber3Nanofiber shifts Carry out calcining for second in another boiler tube;Can also be by first time calcining and second of calcining in same high-temperature atmosphere furnace Middle progress, for the first time calcining directly switch to carbon containing or hydrogeneous atmosphere after terminating by air atmosphere.
There is good electric conductivity according to the pure tungsten nanofiber product obtained by above-mentioned preparation method, its electrical conductivity is up to 1415S/cm, uniform diameter are distributed between 300-500nm, and the length of fiber reaches hundreds of microns to several millimeters, these Excellent performance causes pure tungsten nanofiber to have potential application value in transparent electrode material application aspect.
It is embodiment below:
Embodiment 1:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 600 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 600 DEG C, and soaking time is set as 4h.
Embodiment 2:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 700 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 600 DEG C, and soaking time is set as 4h.
Embodiment 3:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 800 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 600 DEG C, and soaking time is set as 4h.
Embodiment 4:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, solution that is homogeneous, stablizing is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred to spinning equipment Middle carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, Spinning flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 900 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 600 DEG C, and soaking time is set as 4h.
Embodiment 5:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 600 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 700 DEG C, and soaking time is set as 4h.
Embodiment 6:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 600 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 800 DEG C, and soaking time is set as 4h.
Embodiment 7:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 600 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 900 DEG C, and soaking time is set as 4h.
Embodiment 8:
As shown in Figure 1, first, electrostatic spinning liquid is prepared, 10g ammonium metatungstates and 30g PVP are dissolved in 20g water and 40g In the mixed solution of ethanol, the solution of stable homogeneous is uniformly mixing to obtain;Then, electrostatic spinning liquid is transferred in spinning equipment Carry out electrostatic spinning, you can obtain tungstenic presoma nanofiber.Wherein, spinning voltage 18kV, spinning distance is 15cm, is spun Silk flow velocity is 4mL/h.Secondly, above-mentioned tungstenic presoma nanofiber is placed in progress pre-oxidation treatment in resistance furnace to obtain WO3Nanofiber.Wherein, the heating rate of resistance furnace is set as 8 DEG C/min, and holding temperature is 600 DEG C, soaking time 4h. Finally, by WO3Nanofiber is transferred to progress reduction treatment in tube furnace and obtains pure tungsten nanofiber.Wherein heating rate is 10 DEG C/min, holding temperature is 1000 DEG C, and soaking time is set as 4h.
Fig. 2 is the XRD spectrum for the pure tungsten nanofiber being prepared according to technology in embodiment 1.By mutually being marked with pure tungsten Quasi- XRD diffraction card contrast is it can be found that all diffraction maximums both correspond to pure tungsten phase in embodiment 1.Thus illustrate, utilize the system Preparation Method, can realize the preparation of pure tungsten nanofiber in as low as 600 DEG C of reduction temperature.
Fig. 3 is the SEM figures for the pure tungsten nanofiber being prepared according to technology in embodiment 1.It can be seen from the figure that system Standby pure tungsten nanofiber diameter is uniformly distributed between 300-500nm.Nanofiber still keeps good after calcining Continuity, single fiber length, which can reach, some tens of pm or even arrives several millimeters.In addition, the Nanowire after calcining Dimension table face is smooth, and crystal grain is tiny and fine and close.This fine and close and continuous fibre structure ensure that the good electricity of pure tungsten nanofiber Learn performance.
Fig. 4 is the electrical performance testing device schematic diagram of one-dimensional pure tungsten nanofiber in the present invention.First, bipolar electrode is utilized Method collects pure tungsten nanofiber arranged in parallel, and nanofiber arranged in parallel is transferred on quartz plate;Then, will be above-mentioned Quartz plate, which is sequentially placed into resistance furnace and tube furnace, to be pre-oxidized and high temperature reduction, you can obtains parallel on quartz plate surface The pure tungsten nanofiber of row;Finally, gold electrode is sputtered at fiber both ends, leaves 500 μm of conducting channel, thus obtain pure tungsten and receive The electrical performance testing device of rice fiber.
Fig. 5 is the I-V curve figure that one-dimensional pure tungsten nanofiber tests device in embodiment 1.As shown in the figure, in test device Electrode both ends apply test voltage, and test the electric current by device channel.Wherein, voltage range arrives 1V, test voltage for -1V Step pitch is 0.02V, and test number of fiber is 10.Find by test, closed by the electric current for testing device with voltage linear System, illustrates that gold electrode maintains good Ohmic contact with pure tungsten nanofiber.According to Ohm's law, pure tungsten nanometer is calculated The electrical conductivity of fiber is 1415S/cm, has exceeded the electric property of most of Electrospun nano-fibers.Since tungsten has in itself Preferable heat endurance and corrosion resistance, with reference to itself excellent electric property so that tungsten nanofiber is in transparency electrode etc. The preparation field of micro photo electric device is with a wide range of applications.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., should all include Within protection scope of the present invention.

Claims (9)

1. a kind of preparation method of pure tungsten nanofiber, it is characterised in that include the following steps:
(1) electrostatic spinning liquid is prepared, its electrostatic spinning is obtained into tungstenic presoma nanofiber, the electrostatic spinning liquid is tungstenic Compound and high polymer binder are dissolved in water and the mixed liquor formed in organic solvent;
(2) the tungstenic presoma nanofiber obtained in step (1) is subjected to first time calcining, WO is obtained by pre-oxidation3Nanometer Fiber;Wherein, the first time calcining heating rate is 1 DEG C/min~20 DEG C/min, and calcining heat is 400 DEG C~800 DEG C, is protected Warm time 0.5h~6h;
(3) WO that will be obtained in step (2)3Nanofiber carries out second and calcines, and pure tungsten Nanowire is obtained by high temperature reduction Dimension, wherein the heating rate of second of calcining is 1 DEG C/min~20 DEG C/min, calcining heat is 400 DEG C~1000 DEG C, is protected Warm time 0.5h~4h.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), each component in the electrostatic spinning liquid Percentage by weight be respectively:Tungstenic compound 5%~20%, high polymer binder 20%~40%, organic solvent 15%~ 25%, water 30%~50%.
3. preparation method as claimed in claim 1 or 2, it is characterised in that in step (1), the voltage of the electrostatic spinning is 8kV~40kV, electrostatic spinning distance is 10cm~30cm, and electrostatic spinning flow velocity is 2mL/h~5mL/h.
4. preparation method as claimed in claim 1, it is characterised in that in step (1), the Tungstenic compound is metatungstic acid One or more in ammonium, wolframic acid or isopropanol tungsten.
5. preparation method as claimed in claim 1, it is characterised in that in step (1), the high polymer binder is poly- third One or more in alkene nitrile, polyvinyl alcohol, vinyl acetate resin or polyvinylpyrrolidone.
6. preparation method as claimed in claim 1, it is characterised in that in step (1), selected organic solvent is isopropyl One or more in alcohol, ethanol, n,N-Dimethylformamide, chloroform or ether.
7. preparation method as claimed in claim 1, it is characterised in that the atmosphere of second of calcining described in step (3) It is the one or more in ammonia, carbon source gas or hydrogen.
A kind of 8. pure tungsten nanofiber product as obtained by claim 1-7 any one of them preparation methods.
9. a kind of application of pure tungsten nanofiber product as claimed in claim 8, it is characterised in that as transparency electrode material Material.
CN201711370838.XA 2017-12-19 2017-12-19 A kind of pure tungsten nanofiber, preparation method and application Active CN107938027B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711370838.XA CN107938027B (en) 2017-12-19 2017-12-19 A kind of pure tungsten nanofiber, preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711370838.XA CN107938027B (en) 2017-12-19 2017-12-19 A kind of pure tungsten nanofiber, preparation method and application

Publications (2)

Publication Number Publication Date
CN107938027A true CN107938027A (en) 2018-04-20
CN107938027B CN107938027B (en) 2019-09-13

Family

ID=61940764

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711370838.XA Active CN107938027B (en) 2017-12-19 2017-12-19 A kind of pure tungsten nanofiber, preparation method and application

Country Status (1)

Country Link
CN (1) CN107938027B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109898367A (en) * 2019-01-31 2019-06-18 华中科技大学 It is a kind of it is inkless can erasable nanofiber paper repeatedly preparation method and products thereof
CN109926063A (en) * 2019-04-04 2019-06-25 台州学院 A kind of preparation method of copper tungstate nanofiber photocatalyst
CN111270348A (en) * 2020-03-19 2020-06-12 东莞东阳光科研发有限公司 SrVO3Nanofiber preparation method and related products
CN112481740A (en) * 2020-10-15 2021-03-12 南昌航空大学 Brush-shaped WO3Preparation method and application of/C nanowire
CN113791124A (en) * 2021-05-20 2021-12-14 中国石油大学(华东) NO driven by wind power friction nano generator2Gas monitoring system and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101869842A (en) * 2010-06-11 2010-10-27 哈尔滨工业大学深圳研究生院 Tungsten carbide nano fiber oxygen reducing catalyst, preparation method and application thereof
CN102505185A (en) * 2011-09-29 2012-06-20 东北师范大学 Method for preparing polyoxometallate composite mesoporous material by electrostatic spinning
CN105040161A (en) * 2015-07-22 2015-11-11 宁波工程学院 Preparation method of high purity WO<3> mesoporous nano-belt

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101869842A (en) * 2010-06-11 2010-10-27 哈尔滨工业大学深圳研究生院 Tungsten carbide nano fiber oxygen reducing catalyst, preparation method and application thereof
CN102505185A (en) * 2011-09-29 2012-06-20 东北师范大学 Method for preparing polyoxometallate composite mesoporous material by electrostatic spinning
CN105040161A (en) * 2015-07-22 2015-11-11 宁波工程学院 Preparation method of high purity WO<3> mesoporous nano-belt

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109898367A (en) * 2019-01-31 2019-06-18 华中科技大学 It is a kind of it is inkless can erasable nanofiber paper repeatedly preparation method and products thereof
CN109898367B (en) * 2019-01-31 2020-06-05 华中科技大学 Preparation method of inkless repeatedly erasable nanofiber paper and product thereof
CN109926063A (en) * 2019-04-04 2019-06-25 台州学院 A kind of preparation method of copper tungstate nanofiber photocatalyst
CN109926063B (en) * 2019-04-04 2021-11-30 台州学院 Preparation method of copper tungstate nanofiber photocatalyst
CN111270348A (en) * 2020-03-19 2020-06-12 东莞东阳光科研发有限公司 SrVO3Nanofiber preparation method and related products
CN112481740A (en) * 2020-10-15 2021-03-12 南昌航空大学 Brush-shaped WO3Preparation method and application of/C nanowire
CN112481740B (en) * 2020-10-15 2023-02-21 南昌航空大学 Brush-shaped WO 3 Preparation method and application of/C nanowire
CN113791124A (en) * 2021-05-20 2021-12-14 中国石油大学(华东) NO driven by wind power friction nano generator2Gas monitoring system and preparation method and application thereof

Also Published As

Publication number Publication date
CN107938027B (en) 2019-09-13

Similar Documents

Publication Publication Date Title
CN107938027B (en) A kind of pure tungsten nanofiber, preparation method and application
Du et al. Formaldehyde gas sensor based on SnO2/In2O3 hetero-nanofibers by a modified double jets electrospinning process
CN104099687B (en) A kind of graphene fiber and preparation method thereof
Cao et al. Controllable synthesis and HCHO-sensing properties of In2O3 micro/nanotubes with different diameters
Kundu et al. Binder-free electrodes consisting of porous NiO nanofibers directly electrospun on nickel foam for high-rate supercapacitors
Chen et al. Design of Novel Wearable, Stretchable, and Waterproof Cable‐Type Supercapacitors Based on High‐Performance Nickel Cobalt Sulfide‐Coated Etching‐Annealed Yarn Electrodes
CN107103966B (en) A kind of silver nanowires based on electrospinning/Kynoar composite Nano cable
CN107587208B (en) Preparation method and product of tungsten nitride nanofiber
CN106001583B (en) A kind of preparation method of nano-silver thread
CN104649260A (en) Preparation method of graphene nano fibers or nanotubes
CN108597894B (en) preparation method of boron-doped porous carbon material
Huang et al. Durable washable wearable antibacterial thermoplastic polyurethane/carbon nanotube@ silver nanoparticles electrospun membrane strain sensors by multi-conductive network
CN108048955B (en) Preparation method of strontium iron molybdenum based double perovskite type metal oxide nano fiber
Li et al. Mechanical design of brush coating technology for the alignment of one-dimension nanomaterials
Li et al. Fabrication and piezoelectric-pyroelectric properties of electrospun PVDF/ZnO composite fibers
Yin et al. The application of highly flexible ZrO 2/C nanofiber films to flexible dye-sensitized solar cells
CN109369185A (en) A kind of preparation method of nitrogen-doped graphene complex carbon material
CN108922686A (en) A kind of transparent high conductivity flexible wearable electrode and its preparation method and application
Moniz et al. Electrospray Deposition of PEDOT: PSS on Carbon Yarn Electrodes for Solid-State Flexible Supercapacitors
CN106637679A (en) Micro-nano fiber arrays and preparation method and device thereof
Shen et al. Comparative investigation of three types of ethanol sensor based on NiO-SnO 2 composite nanofibers
Chen et al. Colloidal oxide nanoparticle inks for micrometer-resolution additive manufacturing of three-dimensional gas sensors
Bai et al. Room-temperature processing of silver submicron fiber mesh for flexible electronics
Mohamadbeigi et al. Improving the multi-step fabrication approach of copper nanofiber networks based transparent electrode for achieving superb conductivity and transparency
CN111270348B (en) SrVO 3 Nanofiber preparation method and related products

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant