CN115172676A - Electrostatic spinning preparation method of MXene/ferroferric oxide nanofibers - Google Patents

Electrostatic spinning preparation method of MXene/ferroferric oxide nanofibers Download PDF

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CN115172676A
CN115172676A CN202110358772.2A CN202110358772A CN115172676A CN 115172676 A CN115172676 A CN 115172676A CN 202110358772 A CN202110358772 A CN 202110358772A CN 115172676 A CN115172676 A CN 115172676A
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mxene
ferroferric oxide
solution
electrostatic spinning
nano
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罗永松
张德扬
郭音
彭涛
闫海龙
王阳博
柏祖雪
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Xinyang Normal University
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    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • 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

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
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  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Fibers (AREA)

Abstract

The invention discloses MXene (Ti) 3 C 2 ) The method for preparing the ferroferric oxide nano-fiber through electrostatic spinning is characterized in that a single-axis electrostatic spinning technology is applied to the preparation process of the MXene/ferroferric oxide nano-fiber, a few layers of MXene are coated on the ferroferric oxide hollow nanospheres to serve as a main electron transmission path, and then a nitrogen-doped carbon nano-fiber network serves as a second electron transmission path, so that the conductivity of the composite material is greatly improved. The single pieceThe special one-dimensional nano-chain structure composite material not only inherits the high electrochemical activity of ferroferric oxide, but also has excellent electronic conductivity and ionic conductivity, and simultaneously can obtain a novel flexible high-performance lithium storage material. The invention simplifies the production process, improves the material yield, reduces the production cost and meets the actual requirements. The method is simple, and the obtained MXene/ferroferric oxide nano-fiber has uniform size, good dispersion of the ferroferric oxide nano-sphere, high crystallinity, high length-diameter ratio and large specific surface area. The invention also discloses an MXene/ferroferric oxide nanofiber membrane which has a unique nano-chain structure, a cross-linked three-dimensional network structure is formed among the nano-chain fibers, the ion/electron transfer and the electrolyte permeation can be effectively promoted, the diffusion path of electrolyte ions in the material is shortened, the MXene/ferroferric oxide nanofiber membrane has higher specific capacity, excellent rate capability and better circulation stability, and the dynamic performance is greatly improved.

Description

Electrostatic spinning preparation method of MXene/ferroferric oxide nanofibers
Technical Field
The invention relates to the field of transition metal oxide-MXene nano materials, in particular to an electrostatic spinning preparation method of an MXene/ferroferric oxide nano fiber composite material.
Background
Ferroferric oxide has the advantages of large specific capacity, high natural abundance, good environmental protection, difficult combustion, good safety and the like, and is one of the most promising negative electrode materials for replacing graphite anode materials of lithium ion batteries. MXene is a two-dimensional layered transition metal carbide, nitride or carbonitride, and is a two-dimensional material with a graphene-like structure. The laminated MAX material is obtained by etching an intermediate layer (silicon or aluminum) of the laminated MAX material and peeling the laminated MAX material under the action of ultrasound or solvent intercalation. By virtue of their high electrical conductivity and bending stiffness, abundant surface functional groups, and excellent dispersibility in various solvents, have received increasing attention in energy storage and switching applications and have shown competitive performance.
The composite material formed by MXene and the metal oxide coated by the MXene can show a synergistic effect under certain conditions. When the material is applied to an energy storage device, such as a negative electrode material of a lithium ion battery or a sodium ion battery, the MXene/ferroferric oxide nanofiber composite material can utilize the interface effect thereof, and the storage density and the cycling stability of lithium (sodium) ions are increased; and as MXene has higher carrier mobility, the MXene is beneficial to charge migration, and the charge and discharge rate of the battery is increased.
Wang, yesing et al reported that ferroferric oxide nanoparticles were synthesized by a die-hydrothermal method on Journal of Materials Chemistry A6 (2018) 11189-11197, and then dispersed in a multilayer accordion-like MXene aqueous solution for ultrasonic treatment to obtain a composite product of ferroferric oxide and MXene, which is used for the research of lithium ion batteries. In Journal of Materials Chemistry A7 (2019) 269-277, levitt, ariana S. Et al reported that MXene carbon nanofibers were prepared by mixing a small layer of MXene with PAN in a DMF solution to prepare an electrospinning solution and used for the research of supercapacitors. Xu, da et al reported on Chemical Engineering Science 212 (2020) 115342 that a composite product of ferroferric oxide and small-layer MXene was prepared by an electrostatic self-assembly method, and the lithium storage performance of the composite product was studied.
The existing research at present has a plurality of weaknesses in the preparation of the composite product, firstly, the synthesis method is complicated, the yield is low, and the large-scale preparation is not facilitated; on the other hand, the shape of the composite product is not good, the composite product prepared at present is mostly powder, ferroferric oxide of the composite product is easy to agglomerate, MXene lamella is easy to generate and re-stack, so that the surface active sites of the composite product cannot be fully exposed, the material utilization rate is low, the electrochemical energy storage performance and the photocatalytic activity are not improved, and the recycling of the powder catalyst is a difficult problem. Therefore, an MXene composite material with excellent morphology and improved performance is urgently needed by a preparation method which is environment-friendly, low in cost and simple in steps.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the method for preparing the MXene/ferroferric oxide nanofiber composite material by electrostatic spinning, which is economical and effective, has high yield and can be applied in a large scale. The MXene/ferroferric oxide nanofiber prepared by the method has the advantages of controllable shape, good stability, high conductivity and good flexibility.
The technical scheme is as follows: the invention discloses an electrostatic spinning preparation method of an MXene/ferroferric oxide nanofiber composite material, which is characterized by comprising the following steps of: the method comprises the following steps:
s1: 5mL of MXene DMF (N, N-dimethylformamide) solution is subjected to ice bath ultrasound for 1 to 3 hours to obtain the concentration of 40mg mL -1 A stable MXene colloidal solution;
s2: adding 1g of ferroferric oxide hollow nanospheres into the MXene solution in the step S1, and carrying out ice bath ultrasonic treatment for 1 hour;
s3: adding 0.5g of PAN (polyacrylonitrile, molecular weight: 1500000) to the solution in step S2, and continuously stirring for 12 hours to form a viscous black spinning solution;
s4: the electrostatic spinning was carried out by a uniaxial electrostatic spinning device. The electrospinning solution obtained in step S3 was filled into a 5mL plastic syringe equipped with an 18G blunt needle. A positive voltage of 20kv was applied to the tip and the copper collection roller covered with aluminum foil was grounded. The distance between the needle tip and the collector is 15cm, and the injection speed of the solution is controlled to be 1.2mL h -1 The air humidity is less than 30%.
S5: stabilizing the nanofiber membrane obtained in the step S4 in the air for 2 hours at the temperature of 280 ℃ and at the temperature rise rate of 5 ℃ for min -1 。
S6: carbonizing the nanofiber membrane obtained in the step S4 for 3 hours under argon, wherein the carbonization temperature is 800 ℃, and the heating rate is 2 ℃ for min -1 。
Has the beneficial effects that: compared with the prior art, the invention has the following beneficial effects:
1) The preparation method is simple in preparation process and controllable in appearance, and can be used for preparing MXene/ferroferric oxide nanofiber films with uniform appearance, good flexibility and high conductivity in a large scale; the few-layer or single-layer MXene in the prepared nanofiber composite material has the advantages of high loading amount, large specific surface area, good conductivity, self-stacking prevention and the like; the ferroferric oxide hollow nanospheres in the prepared nanofiber composite material have good dispersibility, are tightly coated by the MXene thin layer, and fully utilize the high conductivity of the MXene, the unique three-dimensional structure of the fiber membrane and the high specific surface area.
2) The invention utilizes the electrostatic spinning technology to uniformly lack the MXene-coated ferroferric oxide nanospheres in the one-dimensional nanofibers. The unique design fully utilizes the excellent conductivity of MXene, so that electrons can be quickly and effectively transmitted in the photocatalytic degradation and electrochemical oxidation reduction processes, the charge transmission efficiency can be effectively improved, and the excellent photocatalytic and electrochemical energy storage performances of ferroferric oxide are fully exerted; the porous structure of the three-dimensional fiber network is beneficial to the infiltration and migration of electrolyte ions, and the electrochemical performance of the composite material is further improved. In addition, ferroferric oxide is a low-cost and pollution-free raw material.
3) On one hand, the MXene/ferroferric oxide nanofiber membrane prepared by the method can increase the effective contact area of the active material and the conductive substrate; on the other hand, the constructed three-dimensional network structure can accelerate the transmission rate of electrons and electrolyte ions in the electrode, and finally the purpose of improving the electrochemical performance of the material is achieved. In addition, the synthesized nano material can be directly used as an electrode, so that the complicated process of preparing the electrode by using the traditional powder active material and the addition of an insulating polymer binder are avoided; compared with a powder catalyst, the self-supporting film prepared by the electrostatic spinning method is more convenient to recycle and has good environmental protection advantages in the aspect of photocatalytic application, and the separation and transmission of carriers can be effectively promoted in the photocatalytic process, so that the photocatalytic activity can be effectively improved.
4) The MXene/ferroferric oxide nanofiber membrane prepared by the electrostatic spinning method has the advantages of high conductivity of MXene and high electrochemical activity of ferroferric oxide. In addition, the stability of the composite material is enhanced by the high mechanical strength of MXene, and the volume change in the charge-discharge process is buffered. The ferroferric oxide and MXene are compounded, so that the advantages of the ferroferric oxide and MXene are fully exerted, and a composite material with a multi-stage structure is constructed and can be used as a high-performance photocatalyst material and an ideal electrode material of novel energy sources such as a lithium ion battery, a super capacitor and the like.
Drawings
FIG. 1 is an XRD spectrum of an MXene/ferroferric oxide nanofiber composite material synthesized in example 2 of the invention;
FIG. 2 is an optical photograph of MXene/ferroferric oxide nanofiber composite synthesized in example 2 of the present invention;
FIG. 3 is a scanning electron microscope photomicrograph of an MXene/ferroferric oxide nanofiber composite synthesized in example 2 of the present invention at low magnification;
FIG. 4 is a scanning electron microscope photomicrograph of the MXene/ferroferric oxide nanofiber composite synthesized in example 2 of the present invention at high magnification;
fig. 5 is a transmission electron microscope photograph of the MXene/ferroferric oxide nanofiber composite synthesized in example 2 of the present invention.
Detailed Description
The MXene/ferroferric oxide nanofiber membrane is prepared by an electrostatic spinning method through simple process design. The composite material has the obvious advantages that: MXene not only provides a conductive path, but also stabilizes a material structure, and plays a role in connecting ferroferric oxide nanospheres by penetrating through a bridge, and the special structure of the three-dimensional conductive network also provides a good electron and ion diffusion channel for electrochemical reaction, so that the diffusion distance of ions is shortened, the internal resistance of the active electrode is reduced, and the transfer of electrons, ions and the like between electrolyte and an electrode material is facilitated. By utilizing the electrostatic spinning technology, a three-dimensional conductive network can be constructed, and the agglomeration of ferroferric oxide and the self-stacking effect of MXene are inhibited; the porous structure of the three-dimensional conductive network is also beneficial to the migration of ions in the electrochemical reaction process, and the transfer path from the electrolyte to the active site is shortened. Therefore, the two are effectively compounded, and good synergistic effect can be realized, so that the composite material with high activity is prepared.
The technical solution of the present invention will be further described with reference to the following embodiments and the accompanying drawings.
Example 1:
the embodiment discloses an electrospinning preparation method of an MXene/ferroferric oxide nanofiber composite material, which comprises the following steps:
s1: 5mL of MXene DMF (N, N-dimethylformamide) solution is subjected to ultrasonic treatment for 1 to 3 hours to obtain concentrated solutionDegree of 40mg mL -1 A stable MXene colloidal solution;
s2: adding 0.5g of ferroferric oxide hollow nanospheres into the MXene solution in the step S1 and performing ultrasonic treatment for 1 hour;
s3: 0.5g of PAN (polyacrylonitrile, molecular weight: 1500000) was added to the solution in step S2, and continuously stirred for 12 hours to form a viscous black dope;
s4: and carrying out electrostatic spinning by using a single-shaft electrostatic spinning device. The electrospinning solution obtained in step S3 was loaded into a 5mL plastic syringe equipped with an 18G blunt-ended needle. A positive voltage of 20kv was applied to the tip and the copper collection roller covered with aluminum foil was grounded. The distance between the needle tip and the collector is 15cm, and the injection speed of the solution is controlled to be 1.2mL h -1 And the air humidity is less than 30%.
S5: stabilizing the nanofiber membrane obtained in the step S4 in the air for 2 hours at the temperature of 280 ℃ and at the temperature rise rate of 5 ℃ for min -1 。
S6: carbonizing the nanofiber membrane obtained in the step S4 for 3 hours under argon, wherein the carbonization temperature is 800 ℃, and the heating rate is 2 ℃ for min -1 。
Example 2:
the embodiment discloses an electrospinning preparation method of an MXene/ferroferric oxide nanofiber composite material, which comprises the following steps:
s1: 5mL of MXene DMF (N, N-dimethylformamide) solution is subjected to ice bath ultrasound for 1 to 3 hours to obtain the concentration of 40mg mL -1 A stable MXene colloidal solution;
s2: adding 0.5g of ferroferric oxide hollow nanospheres into the MXene solution in the step S1, and carrying out ice bath ultrasonic treatment for 1 hour;
s3: 0.5g of PAN (polyacrylonitrile, molecular weight: 1500000) was added to the solution in step S2, and continuously stirred for 12 hours to form a viscous black dope;
s4: and carrying out electrostatic spinning by using a single-shaft electrostatic spinning device. The electrospinning solution obtained in step S3 was filled into a 5mL plastic syringe equipped with an 18G blunt needle. A positive voltage of 20kv was applied to the tip and the copper collection roller covered with aluminum foil was grounded. The distance between the needle tip and the collector is 15cm, controlling the solution injection speed to be 1.2mL h -1 The air humidity is less than 30%.
S5: stabilizing the nanofiber membrane obtained in the step S4 in the air for 2 hours at the temperature of 280 ℃ and at the temperature rise rate of 5 ℃ for min -1 。
S6: carbonizing the nanofiber membrane obtained in the step S4 for 3 hours under argon, wherein the carbonization temperature is 800 ℃, and the heating rate is 2 ℃ for min -1 。
Example 3:
the embodiment discloses an electrospinning preparation method of an MXene/ferroferric oxide nanofiber composite material, which comprises the following steps:
s1: 5mL of MXene DMF (N, N-dimethylformamide) solution is subjected to ice bath ultrasound for 1 to 3 hours to obtain the concentration of 40mg mL -1 A stable MXene colloidal solution;
s2: adding 1g of ferroferric oxide hollow nanospheres into the MXene solution in the step S1, and carrying out ice bath ultrasonic treatment for 1 hour;
s3: adding 0.5g of PAN (polyacrylonitrile, molecular weight: 1500000) to the solution in step S2, and continuously stirring for 12 hours to form a viscous black spinning solution;
s4: the electrostatic spinning was carried out by a uniaxial electrostatic spinning device. The electrospinning solution obtained in step S3 was loaded into a 5mL plastic syringe equipped with an 18G blunt-ended needle. A positive voltage of 20kv was applied to the tip and the copper collection roller covered with aluminum foil was grounded. The distance between the needle tip and the collector is 15cm, and the injection speed of the solution is controlled to be 1.2mL h -1 And the air humidity is less than 30%.
S5: stabilizing the nanofiber membrane obtained in the step S4 in the air for 2 hours at the temperature of 280 ℃ and the heating rate of 5 ℃ for min -1 。
S6: carbonizing the nanofiber membrane obtained in the step S4 for 3 hours under argon, wherein the carbonization temperature is 800 ℃, and the heating rate is 2 ℃ for min -1 。
The XRD spectrum of the MXene/ferroferric oxide nanofiber composite material prepared in the embodiment is shown in figure 1, and it can be seen that the crystallinity of the composite material prepared is very high and no impurity phase exists. The results show that: the MXene/ferroferric oxide nanofiber composite material has a diffraction peak at 2 theta =6.5 degrees, and the diffraction peak corresponds to a (002) crystal face of MXene; in addition, the three strong peaks (2 theta angles of 30.08 degrees, 35.43 degrees and 62.53 degrees) of the spectrum are consistent with the three strong peaks of a standard card (PDF # 75-1372) of ferroferric oxide, and the fact that the ferroferric oxide hollow spheres are successfully coated by MXene lamella is shown.
An optical photo of the MXene/ferroferric oxide nanofiber composite material prepared in this example is shown in fig. 2, and the obtained composite material is a black fiber film, has good flexibility, and can be punched into a self-supporting electrode sheet with a diameter of 15 mm.
As shown in fig. 3, an SEM image of the MXene/ferroferric oxide nanofiber composite material prepared in this embodiment shows that the MXene/ferroferric oxide nanofiber composite material has a rich pore structure and is constructed into a three-dimensional nanochain network structure, hollow chain-shaped ferroferric oxide nanospheres are uniformly distributed in fibers, and the fiber diameter is about 500nm and the particle size is about 200-300 nm. From figure 4, the ferroferric oxide hollow nanospheres can be well coated by MXene sheets to form the composite material. The prepared MXene/ferroferric oxide nanofiber composite material has a unique porous structure, and the ferroferric oxide hollow nanospheres are uniformly dispersed on the fibers and are tightly coated by the MXene. Effectively inhibiting the agglomeration of ferroferric oxide and the self-stacking of MXene.
In a TEM image of the MXene/ferroferric oxide nanofiber composite material prepared in this example, as shown in fig. 5, hollow ferroferric oxide nanospheres are tightly wrapped by MXene sheets and form a necklace-like fiber. The design greatly improves the number of active sites which can be utilized by the material, and enhances the rate capability and stability of the electrode in the charging and discharging process.
Example 4:
the embodiment discloses an electrospinning preparation method of an MXene/ferroferric oxide nanofiber composite material, which comprises the following steps:
s1: 5mL of MXene DMF (N, N-dimethylformamide) solution is subjected to ice bath ultrasound for 1 to 3 hours to obtain the concentration of 40mg mL -1 A stable MXene colloidal solution;
s2: adding 1g of ferroferric oxide hollow nanospheres into the MXene solution in the step S1, and carrying out ice bath ultrasound for 1 hour;
s3: adding 0.6g of PAN (polyacrylonitrile, molecular weight: 1500000) to the solution in step S2, and continuously stirring for 12 hours to form a viscous black spinning solution;
s4: the electrostatic spinning was carried out by a uniaxial electrostatic spinning device. The electrospinning solution obtained in step S3 was filled into a 5mL plastic syringe equipped with an 18G blunt needle. A positive voltage of 18kv was applied to the tip and the copper collection roller covered with aluminum foil was grounded. The distance between the needle tip and the collector is 15cm, and the injection speed of the solution is controlled to be 1.2mL h -1 And the air humidity is less than 30%.
S5: stabilizing the nanofiber membrane obtained in the step S4 in the air for 2 hours at the temperature of 280 ℃ and at the temperature rise rate of 5 ℃ for min -1 。
S6: carbonizing the nanofiber membrane obtained in the step S4 for 3 hours under argon, wherein the carbonization temperature is 800 ℃, and the heating rate is 2 ℃ for min -1 。

Claims (2)

1. The invention discloses a preparation method of an MXene/ferroferric oxide nanofiber composite material, which is characterized by comprising the following steps of: the method comprises the following steps:
s1: 5mL of DMF (N, N-dimethylformamide) solution of 5mL of Xene is subjected to ice bath ultrasound for 1 to 3 hours to obtain the solution with the concentration of 40mg mL -1 A stable MXene colloidal solution;
s2: adding 1g of ferroferric oxide hollow nanospheres into the MXene solution in the step S1, and carrying out ice bath ultrasonic treatment for 1 hour;
s3: 0.5g of PAN (polyacrylonitrile, molecular weight: 1500000) was added to the solution in step S2, and continuously stirred for 12 hours to form a viscous black dope;
s4: the electrostatic spinning was carried out by a uniaxial electrostatic spinning device. The electrospinning solution obtained in step S3 was loaded into a 5mL plastic syringe equipped with an 18G blunt-ended needle. A positive voltage of 20kv was applied to the tip and the copper collection roller covered with aluminum foil was grounded. The distance between the needle tip and the collector is 15cm, and the solution injection speed is controlled to be 1.2mLh -1 And the air humidity is less than 30%.
S5: stabilizing the nanofiber membrane obtained in the step S4 in the air for 2 hours at the temperature of 280 ℃ and at the temperature rise rate of 5 ℃ for min -1 。
S6: carbonizing the nanofiber membrane obtained in the step S4 for 3 hours under argon, wherein the carbonization temperature is 800 ℃, and the heating rate is 2 ℃ for min -1 。
2. An MXene/ferroferric oxide nanofiber is characterized in that: the MXene/ferroferric oxide nano-fiber electrostatic spinning preparation method according to claim 1.
CN202110358772.2A 2021-04-02 2021-04-02 Electrostatic spinning preparation method of MXene/ferroferric oxide nanofibers Pending CN115172676A (en)

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