CN111206303B - Preparation method of magnesium cobaltate/carbon composite nano fiber with wolf tooth rod structure, fiber prepared by preparation method and electrode - Google Patents
Preparation method of magnesium cobaltate/carbon composite nano fiber with wolf tooth rod structure, fiber prepared by preparation method and electrode Download PDFInfo
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- CN111206303B CN111206303B CN202010113176.3A CN202010113176A CN111206303B CN 111206303 B CN111206303 B CN 111206303B CN 202010113176 A CN202010113176 A CN 202010113176A CN 111206303 B CN111206303 B CN 111206303B
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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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
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of magnesium cobaltate/carbon composite nanofiber with a wolf tooth rod structure. The invention also discloses magnesium cobaltate/carbon composite nano-fiber with a wolfsbane rod structure prepared by the method and an electrode of a capacitor prepared by using the composite nano-fiber. The magnesium cobaltate/carbon composite nanofiber with the wolframic rod structure has excellent electrochemical performance, the electrode is easy to contact with various ions of electrolyte, has high charge and discharge rate, provides good electronic carriers and buffer matrixes for effectively releasing mechanical stress caused by volume change of cobaltate, and solves the problem that expansion and contraction are easy to occur in the charge and discharge process.
Description
Technical Field
The invention relates to the technical field of preparation of composite nanofibers, in particular to a preparation method of magnesium cobaltate/carbon composite nanofibers with a wolf tooth rod structure, and fibers and electrodes prepared by the magnesium cobaltate/carbon composite nanofibers.
Background
The super capacitor, also called electrochemical capacitor, has a power density higher than that of a battery and an energy density of a traditional electrostatic capacitor, and has the characteristics of stable cycle performance, wider working temperature range, energy conservation, safety, environmental friendliness and the like, so that the super capacitor becomes an energy storage device which attracts attention at present, and can be used as a standby or independent power supply to be applied to important fields of communication, electric power and traffic.
Because the expansion and contraction problems are easy to occur in the traditional electrode material charging and discharging processes, the metal oxide material has a stable crystal structure and higher specific capacity and is recently paid extensive attention by people. Currently, the most excellent performance of the metal oxide electrode material is ruthenium oxide, which can have extremely high specific capacitance value and good conductivity, but ruthenium is a noble metal, expensive and toxic, thereby limiting the large-scale application of ruthenium oxide.
Disclosure of Invention
The invention aims at the problems, and researches and designs a preparation method of magnesium cobaltate/carbon composite nano fiber with a wolf tooth rod structure, and the fiber and the electrode prepared by the method. The technical means adopted by the invention are as follows:
a preparation method of magnesium cobaltate/carbon composite nanofibers with a wolf tooth rod structure comprises the steps of preparing precursor fibers by using cobalt salts and magnesium salts as sources of magnesium cobaltate, polyvinylpyrrolidone as a carbon source and graphene quantum dots as a spinning solution conductive additive through an electrostatic spinning technology, and pre-oxidizing and carbonizing the precursor fibers to obtain the magnesium cobaltate/carbon composite nanofibers with the wolf tooth rod structure. The cobalt and magnesium salts may be in particular nitrates or acetates.
Further, the preparation method of the magnesium cobaltate/carbon composite nanofiber with the wolframic rod structure comprises the following steps:
s1, dissolving polyvinylpyrrolidone (PVP) in N, N-Dimethylformamide (DMF) to obtain a PVP solution with the mass fraction of 15-20 wt%;
s2, mixing Mg (Ac)2·4H2O、Co(Ac)2·4H2Mixing O and graphene quantum dots with the PVP solution obtained in the step S1 to obtain a precursor solution, wherein the precursor solution comprises the components of Mg (Ac) in parts by mass2·4H2O：Co(Ac)2·4H2O: graphene quantum dots: PVP: DMF (1.7-1.8): (4.0-4.2): 0.5-0.2): 14.3-18.5): 79.5-75.3);
s3, performing electrostatic spinning by using the precursor solution obtained in the step S2, wherein the spinning voltage is 8-15kV, and the spinning receiving distance is 10-20cm, so as to obtain precursor fibers;
and S4, drying the precursor fiber, and pre-oxidizing and carbonizing the dried precursor fiber to obtain the magnesium cobaltate/carbon composite nanofiber with the wolf tooth rod structure.
Further, in step S3, the air humidity of the electrospinning is 30% ± 10%; in the step S4, the drying temperature is 80-150 ℃, the drying time is 3-12 hours, the pre-oxidation method is pre-oxidation for 2-4 hours at the temperature of 180-.
Further, in step S1, the mass fraction of the PVP solution is 18%; in step S2, the molar ratio of Mg to Co is 1: 2; in the step S3, the spinning voltage is 10kV, and the spinning acceptance distance is 14 cm; in step S4, the drying temperature is 80 ℃, the drying time is 3 hours, the pre-oxidation method is pre-oxidation for 2 hours at 200 ℃, the temperature of oxygen-free calcination is 700 ℃, and the heat preservation time is 4 hours.
Further, the carbonization method is to perform oxygen-free calcination in an argon atmosphere.
Magnesium cobaltate/carbon composite nano fiber with a wolf tooth rod structure is prepared by the method.
An electrode of a super capacitor comprises magnesium cobaltate/carbon composite nano-fibers with a wolfsbane rod structure, wherein the magnesium cobaltate/carbon composite nano-fibers are prepared by the method.
Compared with the prior art, the magnesium cobaltate/carbon composite nanofiber with the wolframic rod structure has rich pore diameter, larger specific surface area and excellent electrochemical performance, the electrode of the supercapacitor disclosed by the invention is easy to contact with various ions of electrolyte, higher charge and discharge rate can be shown even under high current density, the aggregation effect of magnesium cobaltate nanoparticles in main fibers in charge and discharge cycles is inhibited, a good electronic carrier and a buffering matrix are provided for effectively releasing mechanical stress caused by volume change of cobaltate, and the problems that expansion and contraction are easy to occur in the charge and discharge processes are solved.
Drawings
Fig. 1 is a schematic structural diagram of magnesium cobaltate/carbon composite nanofibers with a mace structure according to an embodiment of the present invention.
FIG. 2 is an XRD pattern of magnesium cobaltate/carbon composite nanofibers prepared at different carbonization temperatures according to the examples of the present invention.
Fig. 3a and 3b are SEM images of magnesium cobaltate/carbon composite nanofibers of mace structure prepared by the example of the present invention.
Fig. 4 is a TEM image of magnesium cobaltate/carbon composite nanofibers with single mace structure prepared by the example of the present invention: FIG. 4a is MgCo produced at 700 deg.C2O4TEM images of nanofibers; FIG. 4b is a Selected Area Electron Diffraction (SAED) diagram; FIGS. 4c and 4i are high resolution transmission electron microscopy (HR-TEM) images; FIGS. 4e-4h, 4k, 4l are elemental plane scans; fig. 4d and 4j are enlarged views of the regions.
FIG. 5 shows the N of magnesium cobaltate/carbon composite nanofibers with wolframic rod structure prepared by the example of the present invention2Adsorption and desorption isotherms.
Fig. 6 is an electrochemical performance curve of magnesium cobaltate/carbon composite nanofiber with a mace structure prepared by the embodiment of the present invention: FIG. 6a is a CV curve at different scan rates; FIG. 6b is a CP curve at different current densities; FIG. 6c is an EIS spectrum; FIG. 6d is a cycle life curve at a current density of 1A/g.
Detailed Description
Accurately weighing 4.170g of polyvinylpyrrolidone (PVP) and dissolving in 20mLN, N-Dimethylformamide (DMF), magnetically stirring for 12h until the polymer is completely dissolved, standing for 12h, preparing a PVP solution with the mass fraction of 18 wt%, then adding 0.05 g of graphene quantum dots, and stirring uniformly. Preparing an electrostatic spinning precursor solution according to a molar ratio of Mg to Co being 1 to 2 (the adding amount of each part of salt is 0.002mol), specifically, nitrate or acetate of magnesium and cobalt can be used, as long as the subsequent reaction requirements can be met, and the embodiment takes acetate as an example for explanation: separately, 0.429g of Mg (Ac)2·4H2O、0.996gCo(Ac)2·4H2Dissolving O in the prepared 18 wt% PVP solution, and magnetically stirring for 12 hr to dissolve completely to obtainTo the precursor solution for spinning. The spinning precursor solution is added into a plastic injector and is connected with a metal electrode connected with the positive pole of a high-voltage power supply, and a receiving device is an aluminum foil and is connected with the negative pole of the high-voltage power supply and is grounded. And (3) controlling the spinning voltage to be 10kV, the spinning receiving distance to be 14cm, keeping the air humidity to be (30% +/-10%), carrying out electrostatic spinning to obtain precursor composite nanofiber, and drying in a vacuum oven at 80 ℃ for 3 h. And carrying out pre-oxidation and carbonization processes on the dried precursor composite nano-fiber to obtain the final cobaltate/carbon composite nano-fiber with the wolframic rod structure. Pre-oxidizing the precursor fiber at 200 ℃ for 2h, placing the pre-oxidized precursor fiber into a quartz tube of a high-temperature tube furnace, introducing Ar gas into the high-temperature tube furnace for 1h to remove air completely, heating the precursor nanofiber sample to 650-750 ℃ at the heating rate of 1-5 ℃/min in the Ar atmosphere, preserving the temperature for 4-8h, preferably heating to 700 ℃ at the heating rate of 2 ℃/min, calcining at 700 ℃ for 4h, and naturally cooling to obtain the magnesium cobaltate/carbon composite nanofiber with the wolf tooth rod structure.
The magnesium cobaltate/carbon composite nanofiber with the wolframic rod structure, the conductive carbon black and the binder (polytetrafluoroethylene solution and 60 wt% of PTFE) are accurately weighed and placed into a colorimetric tube according to the proportion of 85:10:5, a certain amount of absolute ethyl alcohol is added to be used as a solvent to fully mix the magnesium cobaltate/carbon composite nanofiber with the wolframic rod structure, the mixture is taken out and then poured into a watch glass, the watch glass is dried in a 70 ℃ oven until the solution is viscous, the solution is uniformly coated on a foamed nickel wafer, and the foamed nickel wafer is placed into the oven again to be dried. And (3) pressing the current collector and the nickel strip which take the foamed nickel as the electrode material on a hot press under the pressure of 2MPa to finally obtain the electrode plate. The electrochemical performance test of the electrode adopts a three-electrode working system, the prepared magnesium cobaltate/carbon composite nanofiber is used as a working electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, a platinum wire is used as an auxiliary electrode, and a CHI660B electrochemical workstation (Shanghai Chenghua instruments Co.) is used for carrying out the electrochemical performance test.
As shown in fig. 1, the magnesium cobaltate/carbon composite nanofiber with a mace structure prepared in this embodiment includes a fiber body 1 of a magnesium cobaltate/carbon composite, in the figure, 3 is magnesium cobaltate nanoparticles, 4 is graphene quantum dots, and a plurality of carbon nanotubes/carbon nanowires 2 are embedded on the fiber body 1 to form the magnesium cobaltate/carbon composite nanofiber with the mace structure.
As shown in fig. 2, the characteristic peaks appearing in the XRD pattern at 2 θ ═ 18.96 °, 31.20 °, 36.76 °, 38.46 °, 44.71 °, 55.53 °, 59.22 °, 65.08 ° and 73.94 ° correspond to spinel MgCo2O4(JCPDS card 81-0667) having (111), (220), (311), (222), (400), (422), (511), (440), and (620) crystal planes; the weak peaks at 2 θ of 42.82 ° and 62.16 ° correspond to the (200) and (220) plane diffraction peaks of MgO (JCPDS card 75-0447).
As shown in fig. 3a and 3b, the diameter of the host fiber of the magnesium cobaltate/carbon composite nanofiber with the wolf tooth rod structure is about 500nm, and the diameter of the carbon nanowire/carbon nanotube embedded in the host fiber is about 40 nm.
As shown in FIGS. 4a to 4l, the magnesium cobaltate/carbon composite nanofiber body of the wolfsbane rod structure is composed of MgCo2O4The nano particles and the carbon nano particles are arranged, the SAED pattern of the fiber main body can be seen, and the spinel type MgCo can be seen2O4The grain diffraction pattern is a polycrystalline structure, and the HR-TEM representation of the fiber main body shows that the lattice spacing is 0.164nm, and the grain diffraction pattern is similar to spinel MgCo2O4The (422) interplanar spacings of (A) are consistent; the EDS maping test of the fiber main body shows that C, Mg, Co and O elements are uniformly distributed in the fiber main body; the cilia structure can be clearly observed to be composed of a carbon tube and Co nano-particles accumulated at the tip of the carbon tube, the diameter of the carbon tube is about 28nm, and the particle size of the Co nano-particles is about 38 nm; high resolution TEM and masining tests are carried out on the cilia structure, and further prove that carbon nano tubes/carbon nano wires grow on the outer surface of the fiber main body, and cobalt nano particles with simple substances grow at the tips of the carbon nano tubes/carbon nano wires.
As shown in FIG. 5, the specific surface area of the magnesium cobaltate/carbon composite nanofiber of the wolfsbane tooth rod structure is 314.027m2The pore diameter distribution of the mesoporous silica gel is concentrated to 5-15nm, the mesoporous silica gel belongs to a mesoporous structure, and the total pore volumes of the mesoporous silica gel are respectively 0.398m3/g。
As shown in fig. 6a to 6d, at current densities of 4.0, 2.0, 1.0, 0.5 and 0.25A/g, the specific capacitance values of the magnesium cobaltate/carbon composite nanofiber electrode material of the mace structure are 50.3, 74.3, 92.8, 102.8 and 115.7F/g; the internal resistance of the electrode is 0.385 omega, and the internal resistance of charge transfer is 0.232 omega; the charge-discharge cycle life test is carried out for 1000 times under the current density of 1.0A/g, and after 300 times of cycles, the specific capacity retention rate is kept stable and is 98.05 percent of the initial value.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (6)
1. A preparation method of magnesium cobaltate/carbon composite nano-fiber with a wolf tooth rod structure is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving polyvinylpyrrolidone in N, N-dimethylformamide to obtain PVP solution with the mass fraction of 15-25 wt%;
s2, mixing Mg (Ac)2•4H2O、Co(Ac)2•4H2Mixing O and graphene quantum dots with the PVP solution obtained in the step S1 to obtain a precursor solution, wherein the precursor solution comprises the components of Mg (Ac) in parts by mass2•4H2O：Co(Ac)2•4H2O: graphene quantum dots: PVP: DMF = (1.7-1.8): 4.0-4.2): 0.5-0.2): 14.3-18.5): 79.5-75.3);
s3, performing electrostatic spinning by using the precursor solution obtained in the step S2, wherein the spinning voltage is 8-15kV, the spinning receiving distance is 10-20cm, and precursor fibers are obtained, and the air humidity of the electrostatic spinning is 30% +/-10%;
s4, drying the precursor fiber, and pre-oxidizing and carbonizing the dried precursor fiber to obtain magnesium cobaltate/carbon composite nanofiber with a wolf tooth rod structure;
the carbonization method comprises the following steps: heating the precursor nanofiber sample to 650-750 ℃ at the heating rate of 1-5 ℃/min in Ar atmosphere, and preserving the heat for 4-8 h;
the pre-oxidation method is pre-oxidation at 180-250 ℃ for 2-4 hours.
2. The method for preparing magnesium cobaltate/carbon composite nano fiber with mace structure according to claim 1, wherein the method comprises the following steps: in step S4, the drying temperature is 80-150 ℃, the drying time is 3-12 hours, the carbonization method is anaerobic calcination, the temperature of the anaerobic calcination is 650-750 ℃, the heat preservation time is 4-8 hours, and natural cooling is carried out to obtain the magnesium cobaltate/carbon composite nanofiber with the wolf tooth rod structure.
3. The method for preparing magnesium cobaltate/carbon composite nano fiber with mace structure according to claim 2, wherein the method comprises the following steps:
in step S1, the mass fraction of the PVP solution is 18%;
in step S2, the molar ratio of Mg to Co is 1: 2;
in the step S3, the spinning voltage is 10kV, and the spinning acceptance distance is 14 cm;
in step S4, the drying temperature is 80 ℃, the drying time is 3 hours, the pre-oxidation method is pre-oxidation for 2 hours at 200 ℃, the temperature of oxygen-free calcination is 700 ℃, and the heat preservation time is 4 hours.
4. The method for preparing magnesium cobaltate/carbon composite nanofiber with a mace structure according to any one of claims 1 to 3, wherein: the carbonization method is to perform oxygen-free calcination in an argon atmosphere.
5. A magnesium cobaltate/carbon composite nanofiber with a wolf tooth rod structure is characterized in that: prepared by the method of any one of claims 1 to 4.
6. An electrode of a supercapacitor, characterized in that: magnesium cobaltate/carbon composite nanofibers comprising the mace structure prepared by the method of any one of claims 1 to 4.
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