CN111270348A - SrVO3Nanofiber preparation method and related products - Google Patents
SrVO3Nanofiber preparation method and related products Download PDFInfo
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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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
- D04H1/40—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
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- 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
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The invention provides SrVO3Dissolving a strontium-containing soluble compound and a vanadium-containing soluble compound into a solvent, adding a high-molecular binder, and uniformly stirring to obtain an electrostatic spinning solution; transferring the electrostatic spinning solution to electrostatic spinning equipment for electrostatic spinning to obtain precursor nanofibers; placing the precursor nano-fiber in air for pre-oxidation and calcination to obtain SrO/V2O5The oxide nano-fiber is calcined in a reducing atmosphere to obtain SrVO with a one-dimensional structure3The nano-fiber changes the traditional application structure of the block and the powder.
Description
Technical Field
The invention belongs to a nanofiber technology, and particularly relates to SrVO3Nanofiber preparation method and SrVO prepared by using nanofiber preparation method3Nanofiber and SrVO-containing nanofiber3A nanofiber web of nanofibers.
Background
According to the existing SrVO3Preparation method of nanofiber and SrVO (strontium vanadium oxide) capable of being prepared3Nanofibers are generally three-dimensional blocks, or zero-dimensional powder structures.
On the one hand, SrVO is currently prepared3The process is complicated and expensive, for example, the molecular epitaxial growth method needs to use rare earth metal compounds such as La and the like, which causes expensive production cost and limits SrVO3Is widely applied.
On the other hand, SrVO regarding one-dimensional continuous nanofiber structure3It remains a technical gap. Further, SrVO3Is a well-known material with high conductive perovskite structure, and can be used for manufacturing electrodes. Transparent electrodes are ubiquitous in daily life, but due to the existing preparation process, only three-dimensional or zero-dimensional SrVO can be prepared3Its opacity limits its further application in transparent electrodes.
Disclosure of Invention
In order to solve the above problems, the present invention provides a SrVO3Preparation method of nanofiber, through the method, SrVO with one-dimensional structure can be prepared3Nanofibers, modifiedChanged into SrVO3The application structure of the traditional block and powder, and the method is simple, low-cost and efficient. Further, SrVO of the one-dimensional structure can be utilized3Nanofiber for making SrVO with two-dimensional structure3The nano-fiber net structure ensures SrVO3The conductive material has good light transmittance.
In a first aspect, the invention provides a SrVO3The preparation method of the nanofiber comprises the following steps:
dissolving a strontium-containing soluble compound and a vanadium-containing soluble compound into a solvent, adding a high-molecular binder, and uniformly stirring to obtain an electrostatic spinning solution;
secondly, transferring the electrostatic spinning solution into electrostatic spinning equipment, setting parameters of electrostatic spinning, and collecting precursor nanofibers by using a substrate of the electrostatic spinning equipment;
thirdly, placing the precursor nano-fiber in the air for pre-oxidation and calcination to obtain SrO/V2O5An oxide nanofiber; the obtained SrO/V2O5Transferring the oxide nano-fiber into an atmosphere furnace, and calcining in a reducing atmosphere in the atmosphere furnace to obtain SrVO3And (3) nano fibers.
Wherein, the pre-oxidation calcination process in the air can lead the macromolecular binder to be completely decomposed and obtain SrO/V with higher purity2O5An oxide nanofiber; further, calcination is carried out in a reducing atmosphere in an atmosphere furnace, and SrVO is obtained through a high-temperature oxidation-reduction reaction3And (3) nano fibers.
In a specific embodiment, the mass ratios of the components in the electrostatic spinning solution are respectively as follows: 10-40% of soluble compounds containing strontium and vanadium, 5-30% of high-molecular binder and 40-80% of solvent.
Preferably, the mass ratios of the components in the electrostatic spinning solution are respectively as follows: 20-40% of soluble compounds containing strontium and vanadium, 5-30% of high-molecular binder and 40-80% of solvent.
More preferably, the mass ratios of the components in the electrostatic spinning solution are respectively as follows: 20-40% of soluble compounds containing strontium and vanadium, 10-20% of high-molecular binder and 40-80% of solvent.
In a preferred embodiment, the mass ratios of the components in the electrospinning solution are respectively as follows: 30-40% of soluble compounds containing strontium and vanadium, 10-20% of high-molecular binder and 50-60% of solvent.
Preferably, the molar ratio of Sr to V in the electrostatic spinning solution is 1:1, and SrVO with higher purity can be obtained3Nanofibers to ensure SrVO3High conductivity of the nanofibers.
In some embodiments, the strontium-containing soluble compounds in the electrospinning bath comprise: strontium nitrate, strontium acetate, strontium nitrite, strontium chloride, strontium iodide, strontium bromide, strontium hypochlorite, etc., preferably strontium nitrate.
In some embodiments, the vanadium-containing soluble compound comprises: ammonium metavanadate, vanadyl acetylacetonate, and the like, and ammonium metavanadate is preferred.
In some embodiments, the polymeric binder comprises: polyacrylonitrile, polyvinylpyrrolidone, polycaprolactone, polyethylene glycol, polyvinyl alcohol, polypyrrole, or the like, and polyvinylpyrrolidone is preferable.
In some embodiments, the solvent comprises: deionized water, ethanol, acetic acid, N-dimethylformamide, acetonitrile, chloroform or the like, preferably deionized water.
In a specific embodiment, the parameters of electrospinning include: electrostatic spinning voltage is 7kV-30 kV; the spinning speed is 0.5-5 mL/h; the spinning distance is 10cm-25 cm; the environmental humidity is 30-70%; the ambient temperature is 10-40 ℃.
In a preferred embodiment, the parameters of electrospinning can be set as: the electrostatic spinning voltage is 10-20kV, the spinning speed is 1.5mL/h-4mL/h, the spinning distance is 12cm-14cm, the ambient humidity is 40% -60%, and the ambient temperature is 20-30 ℃.
The spinning distance refers to the distance between the anode and the ground in the electrostatic spinning equipment.
In a specific embodiment, the reducing atmosphere comprises: hydrogen, argon-hydrogen mixture, carbon source gas or ammonia gas, etc.
In the specific embodiment, in the process of pre-oxidation calcination in the air, the heating rate is 1-10 ℃/min, the heat preservation temperature is 400-1000 ℃, and the heat preservation time is 1-4 h; in the calcining process in the reducing atmosphere, the heating rate is 1-10 ℃/min, the heat preservation temperature is 600-1200 ℃, and the heat preservation time is 2-4 h.
In a preferred embodiment, in the process of pre-oxidation calcination in the air, the temperature rise rate is 3 ℃/min to 7 ℃/min, the heat preservation temperature is 500 ℃ to 800 ℃, and the heat preservation time is 1.5h to 2.5 h; in the calcining process in the reducing atmosphere, the heating rate is 3 ℃/min to 7 ℃/min, the heat preservation temperature is 600 ℃ to 1200 ℃, and the heat preservation time is 2h to 3 h.
In a second aspect, the invention provides SrVO prepared by the method provided in the first aspect3And (3) nano fibers.
In a third aspect, the present invention provides a pharmaceutical composition comprising SrVO of the second aspect3A nanofiber web of nanofibers.
In a fourth aspect, the present invention provides the SrVO of the second aspect3Nanofibers or SrVO of the third aspect3Use of a nanoweb in a transparent electrode.
Through the technical scheme, compared with the prior art, the invention can at least obtain the following technical effects:
by combining the electrostatic spinning method with high-temperature oxidation-reduction reaction, SrVO with one-dimensional continuous structure can be synthesized3The nano-fiber breaks the traditional SrVO3The inherent existence form of the zero-dimensional powder and the three-dimensional block. The synthesis process has the advantages of simplicity, low cost, large-scale production and the like.
In addition, the diameter of the precursor nanofiber obtained by electrostatic spinning treatment is about hundreds of nanometers, and the precursor nanofiber has extremely high specific surface area, so that the high-temperature oxidation-reduction reaction is fully carried out.
Further, it can also benefitCollecting parallel SrVO by symmetrical electrode method3Nano-fiber to obtain SrVO with two-dimensional structure3A nanofiber web. As the diameter of the nanofiber is nano-scale and can not be identified by naked eyes, the SrVO with a two-dimensional structure3The nanofiber mesh can ensure good conductivity and has excellent light transmittance, and is expected to replace the traditional indium tin oxide transparent electrode to form a novel transparent electrode.
Drawings
FIG. 1 is a one-dimensional continuous SrVO3A flow chart for preparing the nano-fiber;
FIG. 2 is a one-dimensional continuous SrVO constructed in accordance with example 13An X-ray diffraction analysis pattern of the nanofibers;
FIG. 3 is a one-dimensional continuous SrVO constructed in accordance with example 13A high-resolution image of a field emission transmission electron microscope of the nanofiber;
FIG. 4 is a one-dimensional continuous SrVO constructed in accordance with example 13A field emission scanning electron microscopy image of the nanofibers;
FIG. 5 is a one-dimensional continuous SrVO3A schematic diagram of a testing device for electrical property characterization of nanofibers;
FIG. 6 shows different one-dimensional continuous SrVO constructed according to examples 1-43Voltammetric profiles of nanofibers.
Detailed Description
The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The principles of the present invention are described below in conjunction with specific embodiments. It should be noted that the particular embodiments described herein are provided for the purpose of illustrating and explaining the principles of the invention and should not be taken in any way as limiting the scope of the invention which is defined in particular by the claims and not by any particular feature described herein.
FIG. 1 is a one-dimensional continuous SrVO3Production flow of nanofibersThe preparation process is mainly divided into the following three steps:
(a) preparing electrostatic spinning solution
Specifically, according to the stoichiometric ratio of Sr to V being 1:1, a strontium-containing soluble compound and a vanadium-containing soluble compound are dissolved in a proper solvent, a certain high molecular binder is added, and uniform and stable electrostatic spinning solution is obtained by uniformly stirring. Wherein the electrostatic spinning solution comprises the following components in percentage by mass: 20-40% of soluble compounds containing strontium and vanadium, 5-30% of high-molecular binder and 40-80% of solvent.
(b) Electrostatic spinning
Specifically, the electrospinning solution is transferred to electrospinning equipment, appropriate electrospinning voltage, distance, spinning speed and other electrospinning parameters are set, and the precursor nanofibers are collected by using a substrate of the electrospinning equipment. Wherein, the parameters of electrostatic spinning can be as follows: electrostatic spinning voltage is 7kV-30 kV; the spinning speed is 0.5-5 mL/h; the spinning distance is 10cm-25 cm; the environmental humidity is 30-70%; the ambient temperature is 10-40 ℃.
(c) High temperature calcination synthesis
Specifically, the precursor nanofiber is put in air for pre-oxidation and calcination to obtain SrO/V2O5An oxide nanofiber; then, the obtained SrO/V2O5Transferring the oxide nano-fiber into an atmosphere furnace, and calcining at a certain temperature in a reducing atmosphere in the atmosphere furnace to obtain SrVO3And (3) nano fibers.
Wherein, in the process of pre-oxidation in the air, the heating rate is 1 ℃/min-10 ℃/min, the heat preservation temperature is 400 ℃ to 1000 ℃, and the heat preservation time is 1h-4 h.
In the high-temperature reduction process, namely the calcining process in the reducing atmosphere, the heating rate is 1-10 ℃/min; the heat preservation temperature is 600-1200 ℃, and the heat preservation time is 2-4 h.
The technical solution of the present invention will be further described with reference to specific examples.
Example 1
According to the flow chart shown in FIG. 1, firstWeighing 2.11g of strontium nitrate and 1.17g of ammonium metavanadate, dissolving the strontium nitrate and the ammonium metavanadate in 5.22g of heated deionized water, stirring the mixture until the strontium nitrate and the ammonium metavanadate are fully dissolved, adding 1.5g of polyvinylpyrrolidone into the mixture after the mixture is fully dissolved, and fully stirring the mixture until the solution is clarified to obtain the electrostatic spinning solution. Then, the above electrospinning solution was transferred to an electrospinning device. Further, the parameters of electrostatic spinning are set as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the ambient humidity is 50%, the ambient temperature is 25 ℃, and a receiving device, such as a substrate of electrostatic spinning equipment, is utilized to receive the precursor nanofiber. Finally, placing the collected precursor nano-fibers in air at 500 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then the SrO/V is obtained after pre-oxidation and calcination in the air2O5Transferring the oxide nano-fiber into a hydrogen pipe type furnace, setting the heating rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 600 ℃, and obtaining the one-dimensional continuous SrVO after annealing at the furnace temperature3And (3) nano fibers.
FIG. 2 shows a one-dimensional continuous SrVO constructed according to example 13X-ray diffraction analysis spectrum of the nano-fiber, all diffraction peaks are similar to SrVO3The standard card is relatively intact, and thus, it was preliminarily confirmed that the one-dimensional continuous nanofiber constructed according to example 1 had SrVO as a main component3。
To further confirm SrVO3Microstructure and texture composition of nanofiber, one-dimensional continuous SrVO constructed as shown in fig. 3 according to example 13High-power resolution image of field emission projection electron microscope of nanofiber. From the analysis in FIG. 3, SrVO3The nano-fiber has clear lattice stripes, which shows that the material has good crystallinity after high-temperature calcination treatment. Interplanar spacing of
And SrVO3(200) The crystal faces are perfectly fit. From this, it was confirmed that the one-dimensional continuous nanofiber prepared in example 1 was SrVO having good crystallinity3And (3) nano fibers.
FIG. 4 shows a one-dimensional interconnect constructed in accordance with example 1Continuous SrVO3Field emission scanning electron microscopy of nanofibers. It can be found that after the two-step calcination, the nanofiber still has a complete morphology, and the nanofiber remains continuous without significant breakage. SrVO3The diameter of the nano fiber is about hundreds of nanometers, and the nano fiber has extremely high length-diameter ratio and specific surface area. The structure has important significance for fully carrying out high-temperature oxidation-reduction reaction and improving the electrical property of the nano fiber.
The above results show that the one-dimensional SrVO constructed according to example 13The nanofiber has a continuous structure and is perfect in crystallinity.
Example 2
According to the flow chart shown in fig. 1, firstly, 2.11g of strontium nitrate and 1.17g of ammonium metavanadate are weighed and dissolved in 5.22g of heated deionized water, 1.5g of polyvinylpyrrolidone is added after stirring until the strontium nitrate and the ammonium metavanadate are fully dissolved, and the electrostatic spinning solution is obtained after fully stirring until the solution is clarified. Then, transferring the electrostatic spinning solution into electrostatic spinning equipment, and setting electrostatic spinning parameters as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the ambient humidity is 50%, the ambient temperature is 25 ℃, and a receiving device, such as a substrate of electrostatic spinning equipment, is utilized to receive the precursor nanofiber. Finally, placing the collected precursor nano-fibers in air at 500 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then transferring the fibers subjected to preoxidation calcination in the air into a hydrogen pipe type furnace, setting the temperature rise rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 800 ℃, and carrying out furnace temperature annealing to obtain the one-dimensional continuous SrVO3And (3) nano fibers.
Example 3
According to the flow chart shown in fig. 1, firstly, 2.11g of strontium nitrate and 1.17g of ammonium metavanadate are weighed and dissolved in 5.22g of heated deionized water, 1.5g of polyvinylpyrrolidone is added after stirring until the strontium nitrate and the ammonium metavanadate are fully dissolved, and the electrostatic spinning solution is obtained after fully stirring until the solution is clarified. Then, transferring the electrostatic spinning solution into electrostatic spinning equipment, and setting electrostatic spinning parameters as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the environmental humidity is 50 percent, and the environmental temperature is 25 DEG CAnd receiving the precursor nanofibers using a receiving device, such as a substrate of an electrospinning apparatus. Finally, placing the collected precursor nano-fibers in air at 500 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then transferring the fibers subjected to preoxidation calcination in the air into a hydrogen pipe type furnace, setting the temperature rise rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 1000 ℃, and annealing the furnace temperature to obtain the one-dimensional continuous SrVO3And (3) nano fibers.
Example 4
According to the flow chart shown in fig. 1, firstly, 2.11g of strontium nitrate and 1.17g of ammonium metavanadate are weighed and dissolved in 5.22g of heated deionized water, 1.5g of polyvinylpyrrolidone is added after stirring until the strontium nitrate and the ammonium metavanadate are fully dissolved, and the electrostatic spinning solution is obtained after fully stirring until the solution is clarified. Then, transferring the electrostatic spinning solution into electrostatic spinning equipment, and setting electrostatic spinning parameters as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the ambient humidity is 50%, the ambient temperature is 25 ℃, and a receiving device, such as a substrate of electrostatic spinning equipment, is utilized to receive the precursor nanofiber. Finally, placing the collected precursor nano-fibers in air at 500 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then transferring the fibers subjected to preoxidation calcination in the air into a hydrogen pipe type furnace, setting the temperature rise rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 1200 ℃, and annealing in the furnace to obtain the one-dimensional continuous SrVO3And (3) nano fibers.
Further, the one-dimensional SrVO constructed in examples 1 to 4 was tested using an apparatus as shown in FIG. 53The voltammetric cycling profile of the nanofibers is shown in FIG. 6. The nano-fibers obtained by calcining at different temperatures show different conductive performances. SrVO obtained by high-temperature reduction at 1200 ℃ under the same bias voltage3The nano-fiber has the best conductive performance. The conductivities of the nanofibers constructed in examples 1-4 were calculated to be 175.1S/cm, 204.2S/cm, 1495.2S/cm and 1897S/cm, respectively. One-dimensional SrVO constructed as in example 43The electrical property of the nano-fiber exceeds that of most one-dimensional nano-fibers, even the electrical property of the nano-fiber is higher than that of the nano-fiberThe electrical property of the ITO is beyond that of the current commercial transparent electrode material, and the ITO is hopeful to be replaced by a novel transparent electrode material in the future.
Example 5
According to the flow chart shown in fig. 1, firstly, 2.11g of strontium nitrate and 1.17g of ammonium metavanadate are weighed and dissolved in 5.22g of heated deionized water, 1.5g of polyvinylpyrrolidone is added after stirring until the strontium nitrate and the ammonium metavanadate are fully dissolved, and the electrostatic spinning solution is obtained after fully stirring until the solution is clarified. Then, transferring the electrostatic spinning solution into electrostatic spinning equipment, and setting electrostatic spinning parameters as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the ambient humidity is 50%, the ambient temperature is 25 ℃, and a receiving device, such as a substrate of electrostatic spinning equipment, is utilized to receive the precursor nanofiber. Finally, placing the collected precursor nano-fibers in air at 600 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then transferring the fibers subjected to preoxidation calcination in the air into a hydrogen pipe type furnace, setting the temperature rise rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 1200 ℃, and annealing in the furnace to obtain the one-dimensional continuous SrVO3And (3) nano fibers.
Example 6
According to the flow chart shown in fig. 1, firstly, 2.11g of strontium nitrate and 1.17g of ammonium metavanadate are weighed and dissolved in 5.22g of heated deionized water, 1.5g of polyvinylpyrrolidone is added after stirring until the strontium nitrate and the ammonium metavanadate are fully dissolved, and the electrostatic spinning solution is obtained after fully stirring until the solution is clarified. Then, transferring the electrostatic spinning solution into electrostatic spinning equipment, and setting electrostatic spinning parameters as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the ambient humidity is 50%, the ambient temperature is 25 ℃, and a receiving device, such as a substrate of electrostatic spinning equipment, is utilized to receive the precursor nanofiber. Finally, placing the collected precursor nano-fibers in air at 700 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then transferring the fibers subjected to preoxidation calcination in the air into a hydrogen pipe type furnace, setting the temperature rise rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 1200 ℃, and annealing in the furnace to obtain the one-dimensional continuous SrVO3And (3) nano fibers.
Example 7
According to the flow chart shown in fig. 1, firstly, 2.11g of strontium nitrate and 1.17g of ammonium metavanadate are weighed and dissolved in 5.22g of heated deionized water, 1.5g of polyvinylpyrrolidone is added after stirring until the strontium nitrate and the ammonium metavanadate are fully dissolved, and the electrostatic spinning solution is obtained after fully stirring until the solution is clarified. Then, transferring the electrostatic spinning solution into electrostatic spinning equipment, and setting electrostatic spinning parameters as follows: the electrostatic spinning voltage is 12kV, the spinning speed is 2mL/h, the spinning distance is 15cm, the ambient humidity is 50%, the ambient temperature is 25 ℃, and a receiving device, such as a substrate of electrostatic spinning equipment, is utilized to receive the precursor nanofiber. Finally, placing the collected precursor nano-fibers in air at 800 ℃ for pre-oxidation calcination, setting the heating rate to be 5 ℃/min and the heat preservation time to be 2 h; then transferring the fibers subjected to preoxidation calcination in the air into a hydrogen pipe type furnace, setting the temperature rise rate to be 5 ℃/min, the heat preservation time to be 2h, the heat preservation temperature to be 1200 ℃, and annealing in the furnace to obtain the one-dimensional continuous SrVO3And (3) nano fibers.
It should be noted that, based on examples 5-7, it can be determined that, for the same precursor nanofiber, the fibers obtained after pre-oxidation calcination at different temperatures have no significant difference in the components and electrical properties after further reduction with hydrogen at the same temperature.
The invention combines the electrostatic spinning method with the high-temperature oxidation-reduction reaction to synthesize SrVO with a one-dimensional continuous structure3The nano-fiber breaks the traditional SrVO3The inherent existence form of the zero-dimensional powder and the three-dimensional block. The synthesis process has the advantages of simplicity, low cost, large-scale production and the like.
In addition, the diameter of the precursor nanofiber obtained by electrostatic spinning treatment is about hundreds of nanometers, and the precursor nanofiber has extremely high specific surface area, so that the high-temperature oxidation-reduction reaction is fully carried out.
Example 8
The invention can also collect SrVO arranged in parallel by using a symmetrical electrode method3Nano-fiber to obtain SrVO with two-dimensional structure3A nanofiber web. Because the diameter of the nano fiber is nanoGrade, unidentifiable by naked eyes, and SrVO with two-dimensional structure3A nanofiber web.
Further, SrVO with one-dimensional structure3Nanofibers or SrVO3The nanofiber can be applied to transparent electrodes, can ensure good conductivity and has excellent light transmittance, and is expected to replace the traditional indium tin oxide transparent electrode to form a novel transparent electrode.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (11)
1. SrVO3The preparation method of the nanofiber is characterized by comprising the following steps:
dissolving a strontium-containing soluble compound and a vanadium-containing soluble compound into a solvent, adding a high-molecular binder, and uniformly stirring to obtain an electrostatic spinning solution;
secondly, transferring the electrostatic spinning solution to electrostatic spinning equipment for electrostatic spinning to obtain precursor nano-fibers;
thirdly, placing the precursor nano-fiber in the air for pre-oxidation and calcination to obtain SrO/V2O5The oxide nano-fiber is calcined in a reducing atmosphere to obtain SrVO3And (3) nano fibers.
2. SrVO of claim 13The preparation method of the nano-fiber is characterized in that the electrostatic spinning solution comprises the following components in parts by mass: 10-40% of soluble compounds containing strontium and vanadium, 5-30% of high-molecular binder and 40-80% of solvent.
3. SrVO of claim 13The preparation method of the nanofiber is characterized in that Sr to V in electrostatic spinning solution is 1 to 1 molar ratio.
4. SrVO of claim 33A method of making nanofibers, wherein said soluble strontium containing compound in said electrospun fiber is selected from the group consisting of: strontium nitrate, strontium acetate, strontium nitrite, strontium chloride, strontium iodide, strontium bromide or strontium hypochlorite;
the vanadium-containing soluble compound is selected from: ammonium metavanadate or vanadyl acetylacetonate.
5. SrVO of claim 13The preparation method of the nanofiber is characterized in that the macromolecular binder is selected from the following groups: polyacrylonitrile, polyvinylpyrrolidone, polycaprolactone, polyethylene glycol, polyvinyl alcohol or polypyrrole.
6. SrVO of claim 13A method for preparing nanofibers, characterized in that the solvent is selected from the group consisting of: deionized water, ethanol, acetic acid, N-dimethylformamide, acetonitrile or chloroform.
7. SrVO according to any one of claims 1-63The preparation method of the nanofiber is characterized in that the electrostatic spinning parameters comprise: electrostatic spinning voltage is 7kV-30 kV; the spinning speed is 0.5-5 mL/h; the spinning distance is 10cm-25 cm; the environmental humidity is 30-70%; the ambient temperature is 10-40 ℃.
8. SrVO of claim 13The preparation method of the nanofiber is characterized in that in the process of pre-oxidation calcination in the air, the heating rate is 1-10 ℃/min, the heat preservation temperature is 400-1000 ℃, and the heat preservation time is 1-4 h;
in the calcining process in the reducing atmosphere, the heating rate is 1-10 ℃/min, the heat preservation temperature is 600-1200 ℃, and the heat preservation time is 2-4 h.
9. SrVO prepared by the method of any one of claims 1 to 83And (3) nano fibers.
10. Containing SrVO according to claim 93SrVO of nanofiber3A nanofiber web.
11. SrVO of claim 93Nanofiber or SrVO according to claim 103Use of a nanoweb in a transparent electrode.
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