CN110835789A - Manganese vanadate hollow tube fiber and preparation method and application thereof - Google Patents

Manganese vanadate hollow tube fiber and preparation method and application thereof Download PDF

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Publication number
CN110835789A
CN110835789A CN201911216177.4A CN201911216177A CN110835789A CN 110835789 A CN110835789 A CN 110835789A CN 201911216177 A CN201911216177 A CN 201911216177A CN 110835789 A CN110835789 A CN 110835789A
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hollow tube
manganese
tube fiber
fiber
vanadate
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原晓艳
王瑞琴
黄文瑞
沙爱明
黄圣琰
郭守武
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • 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
    • 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
    • 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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a manganese vanadate hollow tube fiber and a preparation method and application thereof, manganese acetate and vanadyl acetylacetonate are added into an N, N-dimethylformamide solvent, mixed solution is obtained after stirring and dissolving, then polyvinylpyrrolidone is added into the mixed solution, and electrostatic spinning solution is obtained after stirring at room temperature; preparing the obtained electrostatic spinning solution into one-dimensional nanofibers by adopting electrostatic spinning, and stacking the nanofibers to form a conductive network; calcining the prepared nano-fiber, and naturally cooling to obtain Mn2V2O7Hollow tube fiber. The manganese vanadate hollow tube fiber prepared by the invention has the advantages of complete forming, stable structure, simple preparation method and excellent repeatability, and effectively expands the application field of vanadium nitride.

Description

Manganese vanadate hollow tube fiber and preparation method and application thereof
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to manganese vanadate hollow tube fibers and a preparation method and application thereof.
Background
Vanadium and manganese atoms in the manganese vanadate are of tetrahedral structures, have layered structures, have good optical and electrochemical properties, and have good application prospects in the fields of optical devices, electrochemical sensors and lithium ion batteries. At present, research on manganese vanadate micro-nano structures mainly focuses on synthesizing irregular manganese vanadate micro-nano powder, manganese vanadate nanorods, manganese vanadate nanobelts, manganese vanadate nanosheets and manganese vanadate tubular structures. At present, the research on manganese vanadate nano materials at home and abroad mainly comprises a high-temperature solid phase method, a sol-gel method and a hydrothermal method, the manganese vanadate obtained by the method is a freely dispersed nano structure, and the research shows that various manganese vanadate nano materials show more excellent performance by virtue of special properties such as surface effect, small-size effect and the like and show wider application prospect due to the orientation of the structure of the oriented nano materials, particularly along with the rapid development of nano science and technology, so that the attention of more and more researchers is attracted.
The nanometer effect generated by the special nanometer structure is expected to improve the electrochemical and optical properties of the manganese vanadate. At present for Mn2V2O7The related reports are less, the development of the preparation process is insufficient, and the existing hydrothermal method is adopted to prepare Mn2V2O7The result of the nanorod shows better electrochemical performance. However, for nano materials, the composition, morphology, preparation method and the like of the nano materials are closely related to the performance, and have important significance for the diversification and potential function diversification of the materials, so that the development of manganese vanadate materials with different compositions and morphologies is urgently needed to be broken through in the field of materials.
The invention provides a manganese vanadate hollow tube material with simple synthesis process and excellent performance and a synthesis method thereof, wherein the manganese, vanadium and oxygen are mixed at the molecular level by adopting the electrostatic spinning method, and manganese vanadate (Mn) with different morphologies is prepared by adopting the raw material ratio and process parameters2V2O7) Nano-micro material, andthe application of the manganese vanadate in the lithium battery material is tested, the microstructure and the morphology of the manganese vanadate material are regulated and controlled, and a basis is provided for the application of the manganese vanadate material.
Disclosure of Invention
The invention aims to solve the technical problem of providing the manganese vanadate hollow tube fiber, and the preparation method and the application thereof, aiming at the defects in the prior art, and applying the electrostatic spinning method to the preparation of the manganese vanadate shortens the preparation process and simplifies the preparation flow.
The invention adopts the following technical scheme:
a preparation method of manganese vanadate hollow tube fiber comprises the following steps:
s1, adding manganese acetate and vanadyl acetylacetonate into an N, N-dimethylformamide solvent, stirring and dissolving to obtain a mixed solution, adding polyvinylpyrrolidone into the mixed solution, and stirring at room temperature to obtain an electrostatic spinning solution;
s2, preparing the electrostatic spinning solution obtained in the step S1 into one-dimensional nanofibers by adopting electrostatic spinning, and stacking the nanofibers to form a conductive network;
s3, calcining the nano-fibers prepared in the step S2, and naturally cooling to obtain Mn2V2O7Hollow tube fiber.
Specifically, in step S1, manganese acetate: vanadyl acetylacetonate: polyvinylpyrrolidone: n, N-dimethylformamide solvent ═ 1 mmol: (0.5-3) mmol: (0.4-3) mmol: 10 mL.
Further, in step S1, the concentration of the polyvinylpyrrolidone in the mixed solution is 0.04-0.3 mol/L.
Specifically, in step S1, the stirring time at room temperature is 6 to 12 hours.
Specifically, in step S2, the electrospinning conditions are: a stainless steel needle head with the specification of 20-23 is adopted, and the distance from the needle head to the collector is 15-25 cm; the electrostatic field voltage is 15-30 kV, and the boosting speed is 0.25-1 mL/h.
Specifically, in step S3, the calcination process parameters are as follows: the temperature is 400-600 ℃, the time is 2-5 h, and the atmosphere is air.
According to another technical scheme, the manganese vanadate hollow tube fiber is prepared according to the method.
According to a third technical scheme, the battery comprises the manganese vanadate hollow tube fiber prepared by the method, and Mn is added2V2O7Hollow tube fibers, acetylene black and polyvinylidene fluoride were blended at 8: 1: 1, taking a metal lithium sheet as a negative electrode and porous polypropylene paper as a diaphragm; ethylene carbonate and dimethyl carbonate of 1mol/L LiPF6 were used as an electrolyte.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the preparation method of the manganese vanadate hollow tube fiber, nontoxic vanadyl acetylacetonate is used as a vanadium source, manganese acetate is used as a manganese source, an electrostatic spinning method which is suitable for mass production and simple in operation is adopted, an excellent electrostatic spinning process is explored, the hollow tube fiber is obtained by combining with post-calcination treatment, and the time of the existing preparation process is shortened.
Furthermore, the diameter of the fiber can be conveniently adjusted by adjusting the technological parameters of electrostatic spinning.
Furthermore, in the process of calcining in the air, the polyvinylpyrrolidone is decomposed and removed, and the obtained hollow tube has a stable structure and uniform tube wall thickness, thereby providing favorable conditions for the application of the hollow tube in the aspects of electrochemistry, optical electrical appliances and the like.
The manganese vanadate hollow tube fiber prepared by the invention is used for assembling a battery, and a constant current charge and discharge performance test is carried out after sealing, the test temperature is 25 ℃, the test range is 0.01-3V, the manganese vanadate hollow tube fiber has good electrochemical performance, and more possibilities are provided for the application of electrochemistry and other aspects.
In conclusion, the manganese vanadate hollow tube fiber prepared by the method is complete in forming, stable in structure, simple in preparation method and excellent in repeatability, and the application field of vanadium nitride is effectively expanded.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD spectrum of a manganese vanadate hollow tube fiber;
FIG. 2 is an SEM photograph of hollow tube fibers of manganese vanadate according to example 1;
FIG. 3 is an SEM photograph of hollow-tube fibers of manganese vanadate according to examples 2 to 5;
fig. 4 is a charge-discharge curve of the cycle period of the manganese vanadate hollow tube fibers 1, 2 and 100 prepared in example 5 of the invention.
Detailed Description
The invention relates to a manganese vanadate hollow tube fiber, a preparation method and application thereof, and provides a manganese vanadate hollow tube material with simple synthesis process and excellent performance and a synthesis method thereof2V2O7) The nanometer micron material is tested for application in lithium battery materials, so that the microstructure and morphology of the manganese vanadate material are regulated and controlled, and a basis is provided for the application of the manganese vanadate material.
The invention relates to a manganese vanadate hollow tube fiber and a preparation method thereof, comprising the following steps:
s1, adding 0.9g of manganese acetate and 0.9-3 g of vanadyl acetylacetonate into 10mL of N, N-dimethylformamide solvent, stirring and dissolving, adding 0.36-3 g of polyvinylpyrrolidone into the mixed solution, placing the mixture at room temperature (25 ℃) and stirring for 6-12 hours to obtain electrostatic spinning solution with certain viscosity, wherein the mass ratio of vanadyl acetylacetonate: polyvinylpyrrolidone: n, N-dimethylformamide solvent ═ 1 mmol: (0.5-3) mmol: (0.4-3) mmol: 10 mL;
s2, selecting a stainless steel needle with the specification of No. 20-23, setting the distance from the needle to the collector to be 15-25 cm, setting the electrostatic field voltage to be 15-30 kV, and setting the boosting speed to be 0.25-1 mL/h to obtain one-dimensional nanofibers in directional arrangement;
s3, calcining the nanofiber obtained in the second step at 400-600 ℃ for 2-5 h at a heating rate of 1-6 ℃/min in the following atmosphere:air to finally obtain Mn2V2O7Hollow tube fibers;
s4 testing electrochemical performance of the assembled battery by adding Mn2V2O7Hollow tube fibers, acetylene black and polyvinylidene fluoride (PVDF) were blended at 8: 1: 1, preparing a working electrode by fully mixing, taking a metal lithium sheet as a negative electrode, and taking porous polypropylene paper as a diaphragm; ethylene Carbonate (EC) and dimethyl carbonate (DMC) of 1mol/L LiPF6 are used as electrolyte.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 0.9g of manganese acetate and 0.9g of vanadyl acetylacetonate into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 0.9g of polyvinylpyrrolidone into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 7 hours to obtain uniformly dispersed electrostatic spinning solution with certain viscosity;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 20 stainless steel needle head, injecting at a speed of 0.5mL/h, a distance between a spinning nozzle and a collector of 19cm, a spinning voltage of 30kV, an indoor temperature of 24 ℃, a relative humidity of 25-30%, and obtaining PVP/C on the collector along with volatilization of the solvent15H21O6V/C4H14MnO8Compounding nano fiber;
mixing the PVP/C15H21O6V/C4H14MnO8Putting the composite nano-fiber into a box-type furnace, heating to 400 ℃ at the speed of 2 ℃/min for 2h, preserving the heat for 2h, and naturally cooling to room temperature to obtain Mn2V2O7Hollow tube fibers;
Mn2V2O7the hollow tube fiber has good crystallinity, characteristic peak position and relative strength and Mn2V2O7The PDF standard card (73-1806) is basically consistent, and the product is monoclinic Mn2V2O7The product has strong characteristic peak intensity and sharp peak shape, which indicates that the crystallinity of the product is high, and other hetero-phase peaks are not observed in the figure, which indicates that the purity of the product is high, and is shown in figure 1; PVP/C15H21O6V/C4H14MnO8The composite nanofiber has a complete fiber structure and uniform diameter distribution, and forms good directional arrangement, as shown in fig. 2 (a); mn2V2O7The diameter distribution of the hollow tube fibers was uniform at 500 nm, exhibiting the characteristics of a complete hollow tube, as shown in fig. 2 (b).
Example 2
Adding 1.4g of manganese acetate and 1g of vanadyl acetylacetonate into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 0.5g of polyvinylpyrrolidone into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 6 hours to obtain uniformly dispersed electrostatic spinning solution with certain viscosity;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 23 stainless steel needle, injecting at 0.25mL/h, at a spinning nozzle-collector spacing of 25cm, at a spinning voltage of 25kV, at an indoor temperature of 24 ℃, at a relative humidity of 25% -30%, and allowing the solvent to volatilize to obtain PVP/C on the collector15H21O6V/C4H14MnO8Compounding nano fiber;
mixing the PVP/C15H21O6V/C4H14MnO8Putting the composite nano-fiber into a box-type furnace, heating to 500 ℃ at the speed of 1 ℃/min for 3h, preserving the heat for 1h, and naturally cooling to room temperature to obtain Mn2V2O7Hollow tube fibers;
SEM test of the obtained sample shows that the prepared Mn is obtained2V2O7The diameter of the hollow tube fiber was still 500 nm, and as a result of comparison with example 1, the aspect ratio was decreased and the length of the fiber was decreased because the morphology of the sample was affected by changing the process parameters, as shown in fig. 3 (a).
Example 3
Adding 2g of manganese acetate and 1g of vanadyl acetylacetonate into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 2g of polyvinylpyrrolidone into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 12 hours to obtain uniformly dispersed electrostatic spinning solution with certain viscosity;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 21 stainless steel needle, injecting at 0.5mL/h, at a spinning nozzle-collector spacing of 15cm, a spinning voltage of 15kV, an indoor temperature of 24 ℃, a relative humidity of 25-30%, and allowing the solvent to volatilize to obtain PVP/C on the collector15H21O6V/C4H14MnO8Compounding nano fiber;
mixing the PVP/C15H21O6V/C4H14MnO8Putting the composite nano-fiber into a box-type furnace, heating to 500 ℃ at a speed of 3 ℃/min for 4h, preserving heat for 3h, and naturally cooling to room temperature to obtain Mn2V2O7Hollow tube fibers;
SEM test of the obtained sample shows that the prepared Mn is obtained2V2O7The diameter of the hollow tube fiber was still 500 nm, and as a result of comparison with example 2, the thickness of the tube wall was reduced and the length of the fiber was comparable because the morphology of the sample was affected by changing the process parameters, as shown in fig. 3 (b).
Example 4
Adding 1g of manganese acetate and 1.5g of vanadyl acetylacetonate into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 1.8g of polyvinylpyrrolidone into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 8 hours to obtain uniformly dispersed electrostatic spinning solution with certain viscosity;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 22 stainless steel needle head, injecting at a speed of 1mL/h, a distance between a spinning nozzle and a collector of 20cm, a spinning voltage of 20kV, an indoor temperature of 24 ℃, a relative humidity of 25-30%, and obtaining PVP/C on the collector along with volatilization of the solvent15H21O6V/C4H14MnO8Compounding nano fiber;
mixing the PVP/C15H21O6V/C4H14MnO8Placing the composite nano-fiber into a box-type furnace, heating to 600 ℃ at a speed of 5 ℃/min for 5h, preserving heat for 2h, and naturally cooling to room temperature to obtain Mn2V2O7Hollow tube fibers;
SEM test of the obtained sample shows that the prepared Mn is obtained2V2O7The diameter of the hollow tube fiber was still 500 nm, and the thickness of the tube wall was increased as compared with the result of example 3, but the hollow tube molding was still maintained intact, and the length of the fiber was comparable, because the morphology of the sample was affected by changing the process parameters, as shown in fig. 3 (c).
Example 5
Adding 1.5g of manganese acetate and 3g of vanadyl acetylacetonate into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 2g of polyvinylpyrrolidone into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 9 hours to obtain uniformly dispersed electrostatic spinning solution with certain viscosity;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 22 stainless steel needle with the injection speed of 0.8mL/h, the distance between a spinning nozzle and a collector of 17cm, the spinning voltage of 16kV, the indoor temperature of 24 ℃, and the relative humidity of 25% > -E30 percent, PVP/C can be obtained on a collector along with the volatilization of the solvent15H21O6V/C4H14MnO8Compounding nano fiber;
mixing the PVP/C15H21O6V/C4H14MnO8Putting the composite nano-fiber into a box-type furnace, heating to 600 ℃ at a speed of 4 ℃/min for 4h, preserving the heat for 2h, and naturally cooling to room temperature to obtain Mn2V2O7Hollow tube fibers;
SEM test of the obtained sample shows that the prepared Mn is obtained2V2O7The diameter of the hollow tube fiber is still about 500 nm, and compared with the result of example 4, the length of the fiber is greatly reduced, and the smoothness of the surface is greatly different from that of other examples, because the morphology of the sample is influenced after the process parameters are changed, as shown in fig. 3 (d).
In order to investigate the influence of the hollow tube structure on the performance of the lithium ion battery, the battery was sealed and then subjected to a constant current charge-discharge performance test at a test temperature of 25 ℃, and Mn is shown in FIG. 42V2O7The hollow tube fiber circulates the charge-discharge curves of the 1 st, 2 nd and 100 th circles under the conditions that the current density is 0.1mA/g and the voltage range is 0.01-3V; it can be seen that: mn2V2O7The first charge and discharge capacity of the hollow tube fiber electrode is 347mAh/g and 758mAh/g respectively: after the circulation once, the charge and discharge capacities are respectively 258mAh/g and 360 mAh/g; mn with increasing number of charge and discharge2V2O7The charge and discharge performance of the hollow tube fiber electrode is gradually stabilized, the discharge capacity after 100 times of circulation is 269mAh/g respectively, and the performance is good.
In conclusion, the electrostatic spinning preparation process combined with different calcination processes in the later stage provided by the invention enables a polymer to form a good hollow tube structure in the cracking process, and the electrochemical performance of the polymer is preliminarily tested, and the result shows good electrochemical performance, which shows that the hollow tube structure provides more possibility for the application of electrochemistry and other aspects in the future.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (8)

1. A preparation method of manganese vanadate hollow tube fiber is characterized by comprising the following steps:
s1, adding manganese acetate and vanadyl acetylacetonate into an N, N-dimethylformamide solvent, stirring and dissolving to obtain a mixed solution, adding polyvinylpyrrolidone into the mixed solution, and stirring at room temperature to obtain an electrostatic spinning solution;
s2, preparing the electrostatic spinning solution obtained in the step S1 into one-dimensional nanofibers by adopting electrostatic spinning, and stacking the nanofibers to form a conductive network;
s3, calcining the nano-fibers prepared in the step S2, and naturally cooling to obtain Mn2V2O7Hollow tube fiber.
2. The method as claimed in claim 1, wherein in step S1, the ratio of manganese acetate: vanadyl acetylacetonate: polyvinylpyrrolidone: n, N-dimethylformamide solvent ═ 1 mmol: (0.5-3) mmol: (0.4-3) mmol: 10 mL.
3. The method according to claim 1 or 2, wherein in step S1, the concentration of polyvinylpyrrolidone in the mixed solution is 0.04-0.3 mol/L.
4. The method according to claim 1, wherein in step S1, the stirring time at room temperature is 6-12 h.
5. The method of claim 1, wherein in step S2, the electrospinning conditions are: a stainless steel needle head with the specification of 20-23 is adopted, and the distance from the needle head to the collector is 15-25 cm; the electrostatic field voltage is 15-30 kV, and the boosting speed is 0.25-1 mL/h.
6. The method of claim 1, wherein in step S3, the calcination process has the following process parameters: the temperature is 400-600 ℃, the time is 2-5 h, and the atmosphere is air.
7. A manganese vanadate hollow tube fiber prepared by the method of claim 1.
8. A battery comprising a manganese vanadate hollow tube fiber prepared by the method of claim 1, wherein Mn is added to the manganese vanadate hollow tube fiber2V2O7Hollow tube fibers, acetylene black and polyvinylidene fluoride were blended at 8: 1: 1, taking a metal lithium sheet as a negative electrode and porous polypropylene paper as a diaphragm; ethylene carbonate and dimethyl carbonate of 1mol/L LiPF6 were used as an electrolyte.
CN201911216177.4A 2019-12-02 2019-12-02 Manganese vanadate hollow tube fiber and preparation method and application thereof Pending CN110835789A (en)

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CN113764661A (en) * 2020-06-01 2021-12-07 南京航空航天大学 Transition metal vanadate zinc ion battery positive electrode material and preparation method thereof
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Application publication date: 20200225