CN110112398B - LiCuVO4Preparation method of nano-fiber, product and application thereof - Google Patents

LiCuVO4Preparation method of nano-fiber, product and application thereof Download PDF

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CN110112398B
CN110112398B CN201910429913.8A CN201910429913A CN110112398B CN 110112398 B CN110112398 B CN 110112398B CN 201910429913 A CN201910429913 A CN 201910429913A CN 110112398 B CN110112398 B CN 110112398B
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licuvo
nanofiber
nano
organic solvent
fiber
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CN110112398A (en
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潘安强
崔荣
郝鹏飞
林建德
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Central South University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • D—TEXTILES; PAPER
    • 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
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • 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
    • D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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 LiCuVO4The preparation method of the nano fiber, the product and the application thereof comprise the following steps: adding vanadyl acetylacetonate, lithium acetate dihydrate and copper acetate monohydrate into an organic solvent, adding polyacrylonitrile, and heating and stirring until the solution is clear and uniform dark blue to obtain a spinning solution; placing the spinning solution in a container loading device of an electrostatic spinning machine, then setting electrospinning process parameters, and then carrying out electrospinning to obtain precursor nanofibers; drying the precursor nanofiber, and then calcining in air to obtain LiCuVO4And (3) nano fibers. The method adopts a vanadium source, a lithium source and a copper source which can be dissolved in an organic solvent, so that the vanadium source, the lithium source and the copper source can react in the organic solvent, and combines an electrostatic spinning process and a calcination process to prepare the nano-fiber, so that the prepared LiCuVO4The size is small, the structure is uniform, and the volume change is small in the charge-discharge process, so that the electrochemical performance can be effectively improved.

Description

LiCuVO4Preparation method of nano-fiber, product and application thereof
Technical Field
The invention belongs to the technical field of preparation of electrode materials of lithium ion batteries, and particularly relates to LiCuVO4A preparation method of nano-fiber, a product and application thereof.
Background
The vanadate material as the cathode material of the lithium ion battery has the advantages of multivalence, layered structure, safe working voltage and high capacity, wherein LiCuVO4When four lithium ions are inserted, the theoretical capacity can reach 576mAhg-1The lithium ion battery cathode material is a very potential lithium ion battery cathode material. In the process of charging and discharging, LiCuVO4Will decompose into Li3VO4And irreversible copper nanoparticles are uniformly dispersed therein, thereby improving electronic conductivity. Currently, LiCuVO4The preparation method mainly adopts a solid-phase reaction method, for example, in the document LiCuVO4 negative electrode material synthesis and electrochemical performance research thereof, lithium carbonate, vanadium pentoxide and copper nitrate are adopted as raw materials, and the ball-milling mixing is combined with a high-temperature solid-phase method to synthesize blocky LiCuVO4LiCuVO thus prepared4The first charge specific capacity of the material reaches 425.2mAhg-1The charging specific capacity is still maintained at 370.8 mAhg after 50 times of circulation-1. From the above, LiCuVO prepared by solid phase reaction is known4The electrode material has large and uneven particle size, small specific surface area and uneven structure, which causes serious volume change in the charge and discharge process, thereby causing poor performance.
Disclosure of Invention
The invention aims to provide LiCuVO with simple process, uniform appearance and nano-scale size4A preparation method of nano-fiber, a product and application thereof.
The LiCuVO of the invention4The preparation method of the nanofiber comprises the following steps:
1) adding vanadyl acetylacetonate, lithium acetate dihydrate and copper acetate monohydrate into an organic solvent, adding polyacrylonitrile, and heating and stirring until the solution is clear and uniform dark blue to obtain a spinning solution;
2) placing the spinning solution obtained in the step 1) in a container loading device of an electrostatic spinning machine, then setting electrospinning process parameters, and then carrying out electrospinning to obtain precursor nanofibers;
3) drying the precursor nano-fiber in the step 2), and then carrying out drying in the airCalcining to obtain LiCuVO4And (3) nano fibers.
In the step 1), the molar ratio of vanadyl acetylacetonate, lithium acetate dihydrate and copper acetate monohydrate is 1:1: 1; the molar volume ratio of the copper acetate monohydrate to the organic solvent is 0.5-1.0 mol/L; the organic solvent is one or more of DMF and DMSO; the mass volume ratio of the polyacrylonitrile to the organic solvent is 0.06-0.1 g/mL; the heating and stirring temperature is 40-50 ℃. In the step 2), the electrostatic spinning process parameters are as follows: the voltage is 7-12 kV, and the pushing speed is 0.5-0.7 mm/min.
In the step 3), the drying temperature is 200-300 ℃, the heat preservation time is 30-60 min, and the heating rate is 1-5 ℃/min; the calcination temperature is 430-480 ℃, the heat preservation time is 0.5-1 h, and the heating rate is 1-5 ℃/min.
LiCuVO prepared by the preparation method4And (3) nano fibers.
The LiCuVO4The carbon content of the nano-fiber is 3-5%. The calcination in the air for a short time can synthesize a product with a target valence, and a small amount of carbon can be reserved to improve the electrochemical performance of the target product.
The LiCuVO4The application of the nano-fiber in a lithium ion negative electrode material.
The invention has the beneficial effects that: 1) the method adopts a vanadium source, a lithium source and a copper source which can be dissolved in an organic solvent, so that the vanadium source, the lithium source and the copper source can react in the organic solvent, and combines an electrostatic spinning process and a calcination process to prepare the nano-fiber, so that the prepared LiCuVO4The size is small, the structure is uniform, and the volume change is small in the charge-discharge process, so that the electrochemical performance can be effectively improved. 2) In the process, precursor nano-fiber is firstly prepared, the precursor nano-fiber is a core-shell, a core layer is polyacrylonitrile, and a shell layer is LiCuVO4Thus polyacrylonitrile will be mostly burned off and a small part will be carbonized during the calcination process, thus obtaining LiCuVO4The nano fiber is a hollow nano fiber, has very large specific surface area, and can effectively improve the electrochemical performance. 3) In the calcination process of the present invention, calcination is strictly controlledThe burning process causes most of polyacrylonitrile to be burnt and a small part to be carbonized, so that LiCuVO4The carbon content of the nano-fiber is 3% -5%, so that the structural stability is improved, and the conductivity is further improved. 4) LiCuVO prepared by the invention4The nano-fiber has smaller size and higher specific surface area, can be beneficial to the infiltration of electrolyte and the de-intercalation of lithium ions in the charge-discharge process, and effectively improves LiCuVO4The specific capacity, the multiplying power and the cycling stability of the composite material have good application prospect. 5) LiCuVO prepared by the invention4The nano-fiber contains LiVO3The phase doping can be more beneficial to the transmission and the de-intercalation of lithium ions by increasing the crystal defects of the material, and the electrochemical performance of the material can be improved by the synergistic effect of the two phases.
Drawings
FIG. 1 LiCuVO prepared in example 14XRD pattern of nanofibers;
FIG. 2 LiCuVO prepared in example 14Thermogravimetric plot of nanofibers;
FIG. 3 LiCuVO prepared in example 14SEM image of nanofibers;
FIG. 4 LiCuVO prepared in example 14TEM images of nanofibers;
FIG. 5 LiCuVO prepared in example 14The nano fiber is at 100mAg-1A cyclic capacity map under conditions;
FIG. 6 LiCuVO prepared in comparative example4SEM image of nanofibers;
FIG. 7 LiCuVO prepared in comparative example4The nano fiber is at 100mAg-1A cyclic capacity map under conditions;
FIG. 8 LiCuVO prepared in example 24The nano fiber is 500mAg-1Cycle capacity plot under conditions.
Detailed Description
Example 1
Taking vanadyl acetylacetonate (0.2mol), lithium acetate dihydrate (0.2mol) and copper acetate monohydrate (0.2mol), adding the materials into 5mL of N-N dimethylformamide solution, adding 0.4g of polyacrylonitrile, and stirring the mixture at the temperature of 40 ℃ to obtain a dark blue uniform solution, namely the spinning solution.
And (3) injecting the obtained spinning solution into a 10mL disposable injector, applying 8kV voltage, setting the pushing speed to be 0.5 mm/min, carrying out electrostatic spinning, and obtaining a light blue nanofiber precursor after spinning.
And carrying out heat treatment on the obtained precursor in air at 250 ℃ for 40min, wherein the temperature rise speed is 3 ℃/min. Then, the solidified material is continuously calcined in the air at 450 ℃ for 0.5h at the heating rate of 5 ℃/min to obtain the carbon-containing LiCuVO4The nanofiber had a carbon content of 4.07%.
The obtained carbon-containing LiCuVO4XRD analysis of the nanofibers showed that: the prepared material can be matched with LiCuVO4And LiVO3The PDF cards of (a) match well with a slight carbon bulge visible around 24 degrees. To further determine the carbon content in the LiCuVO produced4The presence and amount of carbon in the nanofibers was subjected to thermogravimetric testing as shown in FIG. 2 to yield LiCuVO prepared in example 14The carbon content of the nano-fiber is 4.07%.
The obtained carbon-containing LiCuVO4SEM and TEM microscopic morphology analysis of the nano-fiber is carried out, and the result is shown in figures 3 and 4: carbon-containing LiCuVO in FIG. 34The average size of the nanofibers is 300nm, and it can also be roughly seen that the fibers are hollow; in FIG. 4, it is evident that LiCuVO containing carbon4The internal structure of the nanofiber is a porous hollow structure.
And (3) performance testing: carbon-containing LiCuVO4The nanofiber is uniformly mixed with 80 wt.% of active material, 10 superp10wt and 10 wt.% of CMC to prepare slurry, the slurry is uniformly coated on copper foil, and the copper foil is vacuum-dried at 100 ℃ for 8 hours to assemble a button cell for electrochemical performance test. The ring test voltage range is 0.01-3V, and the current density is 100mA g-1The cycle performance results are shown in fig. 5: the first discharge specific capacity is 810.6mAh g-1The specific discharge capacity of the 2 nd circle is 828.3mA h g-1After 50 cycles, 576.1mAhg can still be maintained-1The capacity retention ratio was 84.7% with respect to the second turn. LiCuVO prepared by solid-phase synthesis method in background technology4The carbon-containing LiCuVO prepared by the invention4The nanofiber has more excellent electrochemical cycle performance.
Comparative example
Taking vanadyl acetylacetonate (0.2mol), lithium acetate dihydrate (0.2mol) and copper acetate monohydrate (0.2mol), adding the materials into 5mL of N-N dimethylformamide solution, adding 0.4g of polyacrylonitrile, and stirring the mixture at the temperature of 40 ℃ to obtain a dark blue uniform solution, namely the spinning solution.
And (3) injecting the obtained spinning solution into a 10mL disposable injector, applying 8kV voltage, setting the pushing speed to be 0.5 mm/min, carrying out electrostatic spinning, and obtaining a light blue nanofiber precursor after spinning.
And carrying out heat treatment on the obtained precursor in air at 250 ℃ for 40min, wherein the temperature rise speed is 3 ℃/min. Then, the solidified material is continuously calcined in the oxygen atmosphere at 550 ℃ for 0.5h with the heating rate of 5 ℃/min to obtain LiCuVO4The nanofiber had a carbon content of 0% as measured.
LiCuVO prepared in comparative example 14The microstructure of the nanofiber is shown in FIG. 6, and LiCuVO can be seen from FIG. 64The nano-fiber is changed into a coral-shaped network shape and does not have a hollow structure, which is mainly caused by collapse of a fiber structure due to complete calcination of carbon, so that LiCuVO is obtained4The nanofibers no longer have a hollow structure.
The carbon-containing LiCuVO prepared in this example was tested according to the Performance test method in example 14The nanofibers were tested and the results are shown in fig. 7: the voltage range of the cycle performance test is 0.01-3V, and the current density is 0.1A g-1After circulating for 50 circles, the specific discharge capacity is 482mAh g-1The capacity retention ratio with respect to the second turn was 70.8%. Both the specific capacity and the cycle life performance are significantly reduced compared to example 1.
Example 2
Adding vanadyl acetylacetonate (0.2mol), lithium acetate dihydrate (0.2mol) and copper acetate monohydrate (0.2mol) into 5mL of N-N dimethylformamide solution, adding 0.3g of polyacrylonitrile, and stirring at 40 ℃ to obtain a dark blue uniform solution, namely the spinning solution.
And (3) injecting the spinning solution into a 10mL disposable injector, applying 8kV voltage, setting the pushing speed to be 0.5 mm/min, carrying out electrostatic spinning, and obtaining a light blue nanofiber precursor after spinning.
And carrying out heat treatment on the obtained precursor in air at 250 ℃ for 40min, wherein the temperature rise speed is 3 ℃/min. Then, the solidified material is continuously calcined in the air at 450 ℃ for 0.5h with the heating rate of 5 ℃/min to obtain the carbon-containing LiCuVO4The nanofiber had a carbon content of 3.83% as measured.
The carbon-containing LiCuVO prepared in this example was tested according to the Performance test method in example 14The nanofiber was tested and the results are shown in fig. 8: the voltage range of the cycle performance test is 0.01-3V, and the current density is 0.5A g-1Initial discharge specific capacity 822mAh g-1After 200 cycles, the specific discharge capacity is 415.1mAh g-1The capacity retention ratio with respect to the second turn was 72.1%.
Example 3
Taking vanadyl acetylacetonate (0.2mol), lithium acetate dihydrate (0.2mol) and copper acetate monohydrate (0.2mol), adding the materials into 5mL of N-N dimethylformamide solution, adding 0.5g of polyacrylonitrile, and stirring the mixture at the temperature of 45 ℃ to obtain a dark blue uniform solution, namely the spinning solution.
And (3) injecting the obtained spinning solution into a 10mL disposable injector, applying a voltage of 10kV, setting a pushing speed of 0.7mm/min, carrying out electrostatic spinning, and obtaining a light blue nanofiber precursor after spinning.
The obtained precursor is subjected to heat treatment in air at 300 ℃ for 30min, and the temperature rise speed is 5 ℃/min. Then, the solidified material is continuously calcined in the air at 480 ℃ for 0.5h at the heating rate of 3 ℃/min to obtain the carbon-containing LiCuVO4The nanofiber had a carbon content of 4.58% as measured.
Example 4
Taking vanadyl acetylacetonate (0.2mol), lithium acetate dihydrate (0.2mol) and copper acetate monohydrate (0.2mol), adding the materials into 5mL of N-N dimethylformamide solution, adding 0.3g of polyacrylonitrile, and stirring the mixture at the temperature of 50 ℃ to obtain a dark blue uniform solution, namely the spinning solution.
And (3) injecting the obtained spinning solution into a 10mL disposable injector, applying 12kV voltage, setting the pushing speed to be 0.6mm/min, carrying out electrostatic spinning, and obtaining a light blue nanofiber precursor after spinning.
The obtained precursor is subjected to heat treatment in air at 200 ℃ for 60min, and the temperature rise speed is 1 ℃/min. Then, the solidified material is continuously calcined in the air at 430 ℃ for 1h at the heating rate of 1 ℃/min to obtain the carbon-containing LiCuVO4The nanofiber had a carbon content of 4.11% as measured.

Claims (6)

1. LiCuVO4The preparation method of the nanofiber comprises the following steps:
1) adding vanadyl acetylacetonate, lithium acetate dihydrate and copper acetate monohydrate into an organic solvent according to a set proportion, adding polyacrylonitrile, and heating and stirring until the solution is clear and uniform dark blue to obtain a spinning solution;
2) placing the spinning solution obtained in the step 1) in a container loading device of an electrostatic spinning machine, then setting electrospinning process parameters, and then carrying out electrospinning to obtain precursor nanofibers;
3) drying the precursor nanofiber obtained in the step 2), and then calcining in air to obtain LiCuVO4A nanofiber;
in the step 2), the electrospinning process parameters are as follows: the voltage is 7-12 kV, and the pushing speed is 0.5-0.7 mm/min;
in the step 3), the drying temperature is 200-300 ℃, the drying time is 30-60 min, and the heating rate is 1-5 ℃/min; the calcination temperature is 430-480 ℃, the calcination time is 0.5-1 h, and the heating rate is 1-5 ℃/min;
the LiCuVO4The nanofiber is of a porous hollow structure, the carbon content of the nanofiber is 3% -5%, and the nanofiber comprises LiVO3The phase doping can increase the crystal defects of the material.
2. LiCuVO according to claim 14A method for preparing nano-fiber is characterized in that,in the step 1), the molar ratio of vanadyl acetylacetonate, lithium acetate dihydrate and copper acetate monohydrate is 1:1: 1; the molar volume ratio of the copper acetate monohydrate to the organic solvent is 0.5-1.0 mol/L.
3. LiCuVO according to claim 1 or 24The preparation method of the nanofiber is characterized in that in the step 1), the organic solvent is one or more of DMF and DMSO; the mass volume ratio of the polyacrylonitrile to the organic solvent is 0.06-0.1 g/mL.
4. LiCuVO according to claim 14The preparation method of the nanofiber is characterized in that in the step 1), the heating and stirring temperature is 40-50 ℃.
5. LiCuVO prepared by the preparation method of claim 14And (3) nano fibers.
6. LiCuVO according to claim 54The application of the nano-fiber in a lithium ion negative electrode material.
CN201910429913.8A 2019-05-22 2019-05-22 LiCuVO4Preparation method of nano-fiber, product and application thereof Active CN110112398B (en)

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WO2011068389A2 (en) * 2009-12-04 2011-06-09 주식회사 아모그린텍 Multicomponent nano composite oxide powder and a preparation method therefor, a fabrication method of an electrode using the same, a thin film battery having the electrode and a fabrication method for the battery
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