CN110718681A - Preparation method of phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material - Google Patents

Preparation method of phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material Download PDF

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CN110718681A
CN110718681A CN201911012534.5A CN201911012534A CN110718681A CN 110718681 A CN110718681 A CN 110718681A CN 201911012534 A CN201911012534 A CN 201911012534A CN 110718681 A CN110718681 A CN 110718681A
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negative electrode
phosphorus
electrode material
preparation
titanium dioxide
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霍京浩
薛雨佳
郭守武
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Shaanxi University of Science and Technology
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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
    • 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
    • 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
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides 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
    • H01M4/36—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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M2004/026—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 a preparation method of a phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material, which comprises the steps of respectively weighing tetra-n-butyl titanate and polyvinylpyrrolidone, dissolving in absolute ethyl alcohol, adding an acetic acid solution, and stirring until the materials are completely dissolved to obtain a mixed solution; weighing disodium hydrogen phosphate, adding into the mixed solution, stirring to dissolve completely to obtain the electrostatic spinningA silk precursor solution; carrying out electrostatic spinning on the electrostatic spinning precursor solution to obtain nano fibers; calcining the nano-fiber in inert atmosphere to obtain P-TiO2the/C nanofiber negative electrode material. The invention prepares P-TiO by electrostatic spinning method2the/C nano fiber has simple preparation process, nontoxic and harmless raw materials, and excellent electrochemical performance, and is a lithium ion battery cathode material with good application prospect.

Description

Preparation method of phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of a phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material.
Background
The diversification of electronic products and the continuous development of electric automobiles promote research on lithium ion batteries by researchers, and meanwhile, the conversion and storage of renewable energy sources with high benefit, low cost and environmental friendliness become research hotspots. Lithium ion batteries are becoming increasingly indispensable as the core of energy conversion and storage technologies, and are widely used in the fields of mobile phones, notebook computers, hybrid vehicles, and the like.
The transition metal oxide has excellent specific capacity, cycle life and rate capability when being used as an electrode material, so that the transition metal oxide has attracted wide attention in the field of lithium ion batteries. Titanium dioxide (TiO) as a transition metal oxide lithium storage material2) Has attracted extensive attention because of its advantages of abundant reserves, high safety, low cost, environmental protection, etc. However, TiO2As a semiconductor material, it has poor conductivity and a small diffusion coefficient of lithium ions, thereby limiting its application in lithium ion batteries.
Disclosure of Invention
The invention aims to provide a preparation method of a phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material, and aims to solve the problem of TiO2The invention has the defects of poor conductivity, small lithium ion diffusion coefficient and the like when being used as a negative electrode material, and prepares phosphorus-doped titanium dioxide/carbon (P-TiO) by an electrostatic spinning method2the/C) nano fiber has simple preparation process, nontoxic and harmless raw materials, and excellent electrochemical performance, and is a lithium ion battery cathode material with good application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material comprises the following steps:
1) respectively weighing tetra-n-butyl titanate and polyvinylpyrrolidone, dissolving in absolute ethyl alcohol, adding acetic acid solution, and stirring to completely dissolve to obtain a mixed solution;
2) weighing disodium hydrogen phosphate, adding the disodium hydrogen phosphate into the mixed solution in the step 1), and stirring until the disodium hydrogen phosphate is completely dissolved to obtain electrostatic spinning precursor solution;
3) performing electrostatic spinning on the electrostatic spinning precursor solution obtained in the step 2) to obtain nano fibers;
4) calcining the nano-fiber obtained in the step 3) in an inert atmosphere to obtain P-TiO2the/C nanofiber negative electrode material.
Further, the mass ratio of tetra-n-butyl titanate to polyvinylpyrrolidone in step 1) is 5: 1.
Further, 5g of tetra-n-butyl titanate and 1g of polyvinylpyrrolidone were added per 10mL of anhydrous ethanol in step 1).
Further, the volume ratio of the absolute ethyl alcohol to the acetic acid solution in the step 1) is 10: 1.
Further, in the step 2), the mass of the disodium hydrogen phosphate is 1% -7% of that of the tetrabutyl titanate.
Further, the electrostatic spinning process in the step 3) specifically comprises the following steps: adding the electrostatic spinning precursor solution obtained in the step 2) into a needle tube, and carrying out electrostatic spinning at a voltage of 15kV, a distance between a needle head and a receiving shaft of 20cm and a pushing speed of 1 mL/h.
Further, the inert atmosphere in the step 4) is Ar atmosphere.
Further, the calcination temperature in the step 4) is 500 ℃ and the calcination time is 2 h.
Compared with the prior art, the invention has the following beneficial technical effects:
the preparation method of the invention is to take DHP as a phosphorus source and add TiO2In the electrostatic spinning precursor solution, P-TiO is obtained by electrostatic spinning and calcination in inert atmosphere2a/C nanofiber. The nanofiber has large specific surface area, excellent conductivity and abundant active sites, shows excellent electrochemical performance when being used as a negative electrode material of a lithium ion battery, and is doped with 5 percent of phosphorus at 0.1A g-1The specific capacity under the current density reaches 340mAh g-1After the multiplying power performance test, 50 cycles (0.1A g) are tested-1) The specific capacity is still 340mAh g-1。
Drawings
FIG. 1 is the P-TiO prepared in example 22SEM image of/C nanofibers.
FIG. 2 is a diagram showing the preparation of P-TiO according to examples 1, 2 and 32And the/C nanofiber is used as a rate performance graph of the lithium ion battery cathode material.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation method of a phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material comprises the following steps:
1) respectively weighing tetra-n-butyl titanate (C)16H36O4Ti, TBOT)5.0g and polyvinylpyrrolidone (PVP)1.0g are dissolved in 10mL of absolute ethanol, then 1mL of acetic acid solution is added, and the mixture is stirred for 12 hours until the PVP is completely dissolved, so that a light yellow mixed solution is obtained.
2) Disodium hydrogen phosphate (Na) containing crystal water was weighed2HPO4·12H2O, DHP) is added into the solution obtained in the step 1), wherein the mass of the DHP accounts for 1% -7% of that of the TBOT, and the solution is stirred for 24h until the DHP is completely dissolved, so that the electrostatic spinning precursor solution is obtained.
3) Adding the electrostatic spinning precursor solution obtained in the step 2) into a needle tube, and carrying out electrostatic spinning at a voltage of 15kV, a distance between a needle head and a receiving shaft of 20cm and a pushing speed of 1 mL/h.
4) Calcining the nano-fiber obtained in the step 3) for 2 hours at 500 ℃ in Ar atmosphere to obtain P-TiO2a/C nanofiber.
5) The prepared P-TiO2Mixing the/C nano-fiber with a binder and conductive carbon black to prepare slurry, coating the slurry to be used as a negative electrode material, and assembling the battery in a glove box.
6) The assembled cell was subjected to electrochemical performance testing.
The present invention is described in further detail below with reference to examples:
example 1
1) Respectively weighing tetra-n-butyl titanate (C)16H36O4Ti, TBOT)5.0g, polyvinylpyrrolidone (PVP: (VIP:)PVP)1.0g is dissolved in 10mL of absolute ethyl alcohol, then 1mL of acetic acid solution is added, and stirring is carried out for 12 hours until PVP is completely dissolved, so as to obtain a light yellow mixed solution.
2) Disodium hydrogen phosphate (Na) containing crystal water was weighed2HPO4·12H2O, DHP) is added into the solution obtained in the step 1), wherein the mass of the DHP accounts for 1% of that of the TBOT, and the solution is stirred for 24 hours until the DHP is completely dissolved, so that the electrostatic spinning precursor solution is obtained.
3) Adding the electrostatic spinning precursor solution obtained in the step 2) into a needle tube, and carrying out electrostatic spinning at a voltage of 15kV, a distance between a needle head and a receiving shaft of 20cm and a pushing speed of 1 mL/h.
4) Calcining the nano-fiber obtained in the step 3) for 2 hours at 500 ℃ in Ar atmosphere to obtain P-TiO2a/C nanofiber.
5) The prepared P-TiO2Mixing the/C nano-fiber with a binder and conductive carbon black to prepare slurry, coating the slurry to be used as a negative electrode material, and assembling the battery in a glove box.
6) The assembled cell was tested for electrochemical performance at 0.1Ag-1The specific capacity under the current density reaches 279mAhg-1。
Example 2
1) Respectively weighing tetra-n-butyl titanate (C)16H36O4Ti, TBOT)5.0g and polyvinylpyrrolidone (PVP)1.0g are dissolved in 10mL of absolute ethanol, then 1mL of acetic acid solution is added, and the mixture is stirred for 12 hours until the PVP is completely dissolved, so that a light yellow mixed solution is obtained.
2) Disodium hydrogen phosphate (Na) containing crystal water was weighed2HPO4·12H2O, DHP) is added into the solution obtained in the step 1), wherein the mass of the DHP accounts for 5% of that of the TBOT, and the solution is stirred for 24h until the DHP is completely dissolved, so that the electrostatic spinning precursor solution is obtained.
3) Adding the electrostatic spinning precursor solution obtained in the step 2) into a needle tube, and carrying out electrostatic spinning at a voltage of 15kV, a distance between a needle head and a receiving shaft of 20cm and a pushing speed of 1 mL/h.
4) Calcining the nano-fiber obtained in the step 3) for 2 hours at 500 ℃ in Ar atmosphere to obtain P-TiO2a/C nanofiber.
5) The prepared P-TiO2the/C nano-fiber, the binder and the conductorAnd mixing the electric carbon black to prepare slurry, coating the slurry to be used as a negative electrode material, and assembling the battery in a glove box.
6) The assembled cell was tested for electrochemical performance at 0.1Ag-1The specific capacity under the current density reaches 340mAhg-1。
Example 3
1) Respectively weighing tetra-n-butyl titanate (C)16H36O4Ti, TBOT)5.0g and polyvinylpyrrolidone (PVP)1.0g are dissolved in 10mL of absolute ethanol, then 1mL of acetic acid solution is added, and the mixture is stirred for 12 hours until the PVP is completely dissolved, so that a light yellow mixed solution is obtained.
2) Disodium hydrogen phosphate (Na) containing crystal water was weighed2HPO4·12H2O, DHP) is added into the solution obtained in the step 1), wherein the mass of the DHP accounts for 7% of the mass of the TBOT, and the solution is stirred for 24h until the DHP is completely dissolved, so that the electrostatic spinning precursor solution is obtained.
3) Adding the electrostatic spinning precursor solution obtained in the step 2) into a needle tube, and carrying out electrostatic spinning at a voltage of 15kV, a distance between a needle head and a receiving shaft of 20cm and a pushing speed of 1 mL/h.
4) Calcining the nano-fiber obtained in the step 3) for 2 hours at 500 ℃ in Ar atmosphere to obtain P-TiO2a/C nanofiber.
5) The prepared P-TiO2Mixing the/C nano-fiber with a binder and conductive carbon black to prepare slurry, coating the slurry to be used as a negative electrode material, and assembling the battery in a glove box.
6) The assembled cells were tested for electrochemical performance at 0.1A g-1The specific capacity under the current density reaches 281mAhg-1。
As can be seen from FIG. 1, when the P-doping content is 5%, a fiber having a smooth surface can be prepared, and in addition, P-TiO2Some nanopores also appear on the surface of the/C nanofiber, and are the result of decomposition of DHP in the carbonization process; as can be seen from FIG. 2, P-TiO2the/C (5%) nano fiber shows better electrochemical performance and is 0.1A g-1The specific capacity under the current density reaches 340mAh g-1And tested for 50 cycles after rate capability testing (0.1A g)-1) The specific capacity can still be kept at 340mAh g-1。

Claims (8)

1. A preparation method of a phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material is characterized by comprising the following steps:
1) respectively weighing tetra-n-butyl titanate and polyvinylpyrrolidone, dissolving in absolute ethyl alcohol, adding acetic acid solution, and stirring to completely dissolve to obtain a mixed solution;
2) weighing disodium hydrogen phosphate, adding the disodium hydrogen phosphate into the mixed solution in the step 1), and stirring until the disodium hydrogen phosphate is completely dissolved to obtain electrostatic spinning precursor solution;
3) performing electrostatic spinning on the electrostatic spinning precursor solution obtained in the step 2) to obtain nano fibers;
4) calcining the nano-fiber obtained in the step 3) in an inert atmosphere to obtain P-TiO2the/C nanofiber negative electrode material.
2. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material as claimed in claim 1, wherein the mass ratio of tetra-n-butyl titanate to polyvinylpyrrolidone in step 1) is 5: 1.
3. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material as claimed in claim 1, wherein 5g of tetra-n-butyl titanate and 1g of polyvinylpyrrolidone are added to 10mL of absolute ethanol in step 1).
4. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material as claimed in claim 1, wherein the volume ratio of the absolute ethanol to the acetic acid solution in the step 1) is 10: 1.
5. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material as claimed in claim 1, wherein the mass of disodium hydrogen phosphate in the step 2) is 1% -7% of that of tetra-n-butyl titanate.
6. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material as claimed in claim 1, wherein the electrostatic spinning process in the step 3) is specifically as follows: adding the electrostatic spinning precursor solution obtained in the step 2) into a needle tube, and carrying out electrostatic spinning at a voltage of 15kV, a distance between a needle head and a receiving shaft of 20cm and a pushing speed of 1 mL/h.
7. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber anode material as claimed in claim 1, wherein the inert atmosphere in the step 4) is Ar atmosphere.
8. The preparation method of the phosphorus-doped titanium dioxide/carbon nanofiber anode material as claimed in claim 1, wherein the calcination temperature in the step 4) is 500 ℃ and the calcination time is 2 hours.
CN201911012534.5A 2019-10-23 2019-10-23 Preparation method of phosphorus-doped titanium dioxide/carbon nanofiber negative electrode material Pending CN110718681A (en)

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Application publication date: 20200121