CN111244403B - Fluorinated graphene modified niobium pentoxide material and preparation and application thereof - Google Patents

Fluorinated graphene modified niobium pentoxide material and preparation and application thereof Download PDF

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CN111244403B
CN111244403B CN201811441454.7A CN201811441454A CN111244403B CN 111244403 B CN111244403 B CN 111244403B CN 201811441454 A CN201811441454 A CN 201811441454A CN 111244403 B CN111244403 B CN 111244403B
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fluorinated graphene
niobium pentoxide
niobium
liquid
graphene modified
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CN111244403A (en
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曲超
张洪章
李先锋
张华民
刘翠连
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Dalian Institute of Chemical Physics of CAS
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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
    • H01M4/364—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
    • 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
    • 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 provides a fluorinated graphene modified niobium pentoxide material and a preparation method and application thereof. A fluorinated graphene modified niobium pentoxide material is formed by compounding fluorinated graphene and niobium pentoxide; the niobium pentoxide accounts for 55-98% of the whole material by mass, preferably 62-97%, most preferably 70-94%. The material surface contains C-F-Nb bonds and F-Nb bonds, the niobium pentoxide accounts for 55-98% of the mass fraction of the whole material, the carbon element accounts for 1-25% of the mass fraction of the whole material, and the fluorine element accounts for 0.2-20% of the mass fraction of the whole material.

Description

Fluorinated graphene modified niobium pentoxide material and preparation and application thereof
Technical Field
The invention belongs to the field of lithium ion batteries and lithium ion supercapacitors, and particularly relates to a modified niobium dioxide-free negative electrode and a preparation method thereof.
Background
The transition metal oxide niobium pentoxide has a proper working potential (1-2V), and the unique crystal structure of the niobium pentoxide can provide rich storage sites for lithium ions, and meanwhile, the Nb in an orthorhombic crystal form2O5Because the octahedral gaps can provide special ion channels, the charge and discharge speed of the battery is improved.
However, niobium pentoxide is known to have very poor electron conductivity, and it is often desired to compound a conductive base material with it to improve the electron conductivity of the material. However, as the charge and discharge cycle progresses, the niobium pentoxide and the conductive base material tend to fall off, and the battery performance is degraded.
Disclosure of Invention
The invention provides a fluorinated graphene modified niobium pentoxide material and a preparation method and application thereof. A fluorinated graphene modified niobium pentoxide material is formed by compounding fluorinated graphene and niobium pentoxide; the niobium pentoxide accounts for 55-98% of the whole material by mass, preferably 62-97%, most preferably 70-94%.
The surface of the material contains C-F-Nb bonds and F-Nb bonds, the niobium pentoxide accounts for 55-98% of the mass fraction of the whole material, the carbon element accounts for 1-25% of the mass fraction of the whole material, and the fluorine element accounts for 0.2-20% of the mass fraction of the whole material;
the method is better: the niobium pentoxide accounts for 62 to 97 percent of the mass of the whole material, the carbon element accounts for 2 to 20 percent of the mass of the whole material, and the fluorine element accounts for 0.5 to 18 percent of the mass of the whole material;
optimally: the niobium pentoxide accounts for 70-94% of the mass of the whole material, the carbon element accounts for 5-18% of the mass of the whole material, and the fluorine element accounts for 0.8-15% of the mass of the whole material.
1) Fully dispersing and mixing organic alcohol, fluorinated graphene and ammonia water to form uniform liquid;
2) adding niobium halide with the mass of 1.0-20 times (preferably 2.0-15 times, most preferably 4.0-10 times) of the mass of the liquid into the liquid, stirring for 0.5-10 hours (preferably stirring time is 1-8 hours, most preferably stirring time is 1.5-6 hours), stopping stirring, filtering, centrifuging or evaporating the liquid to obtain a mesophase, calcining the mesophase at 300-;
the above-mentioned homogeneous liquid comprises the following components in parts by mass: 40-90 parts by mass of organic alcohol, 0.1-5 parts by mass of fluorinated graphene and 0.5-10 parts by mass of ammonia water (calculated by 40% of ammonia water in mass fraction).
The organic alcohol comprises one or more than two of methanol, ethanol, propanol, isopropanol and butanol;
the inert atmosphere gas is one or more than two of nitrogen, argon and helium;
the F/C ratio in the fluorinated graphene is 0.1-1.5, preferably 0.3-1.3, and most preferably 0.5-1.2; the number of layers of the fluorinated graphene is 1-15, preferably 1-10, and most preferably 1-5.
The niobium halide is one or more than two of niobium fluoride, niobium chloride, niobium bromide and niobium iodide.
The fluorinated graphene modified niobium pentoxide material is applied to a lithium battery cathode as an electrode active material.
According to the method, a C-F-Nb bond can be formed on the surface of the niobium pentoxide, the niobium pentoxide and graphene atoms are compounded in a scale through the C-F-Nb bond, the electronic conduction resistance is greatly reduced, the rate capability of the niobium pentoxide material is improved, the niobium pentoxide structure after the F atoms are doped in situ is more stable, and the cycle performance is greatly improved.
Detailed Description
Dissolving 9.3g of the prepared modified niobium pentoxide material, 0.3g of polyvinylidene fluoride and 0.4g of conductive agent into 18g N-methyl pyrrolidone, uniformly dispersing, and blade-coating on an aluminum foil with an electrode loading of 2mg/cm2. The prepared electrode is subjected to a flexible package battery test, the working electrode is modified niobium pentoxide, the counter electrode is a lithium plate, and the electrolyte is 1mol/L lithium hexafluorophosphate (the solvent is ethylene carbonate: dimethyl carbonate: diethyl carbonate: 1: 1 (volume ratio)). The charge and discharge multiplying power of the battery is 1C/20C/100C, the charge and discharge cutoff voltage is 1V-2.5V, and the unit gram capacity of the electrode is considered. And when the charge-discharge multiplying power is 1C, the percentage of the capacity after 1000 cycles to the initial capacity is considered, namely the capacity retention rate.
Example 1
After 45g of ethanol, 2g of fluorinated graphene (F/C ratio of 1.1, 5 layers) and 2g of ammonia water are mixed uniformly, 50g of niobium chloride is slowly added, the mixture is stirred for 5 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining for 8 hours at 600 ℃ in the argon atmosphere, and cooling to prepare the powder material.
The material is subjected to element analysis, wherein the mass fraction of carbon elements accounts for 10%, the mass fraction of fluorine elements accounts for 5%, and the balance is niobium pentoxide.
The XPS test and peak separation are carried out on the material, wherein 670.5e V belongs to a Nb-F bond 686.6e V belongs to a C-F bond, and 675.3e V belongs to a C-F-Nb bond, so that the fluorinated graphene modified niobium pentoxide material is proved to contain the C-F-Nb bond, the Nb-F bond and the C-F bond, and the bonds are beneficial to greatly reducing the electronic conduction resistance by compounding niobium pentoxide and fluorinated graphene on an atomic scale.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Comparative examples 1,
After 45g of ethanol and 2g of ammonia water are mixed uniformly, 50g of niobium chloride is slowly added, the mixture is stirred for 5 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining for 8 hours at 600 ℃ in the argon atmosphere, and cooling to prepare the powder material.
The above material was subjected to elemental analysis to obtain niobium pentoxide.
The above materials were XPS tested and peak fractionated with no 670.5e V, 686.6e V, 675.3e V present.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Comparative example 2
After mixing 45g of ethanol, 2g of graphene (5 layers) and 2g of ammonia water uniformly, slowly adding 50g of niobium chloride, stirring for 5 hours, and evaporating the liquid to dryness to obtain an intermediate phase. Then calcining for 8 hours at 600 ℃ in the argon atmosphere, and cooling to prepare the powder material.
And performing element analysis on the material, wherein the mass fraction of carbon elements accounts for 10.5%, and the balance is niobium pentoxide.
The above materials were XPS tested and peak fractionated with no 670.5e V, 686.6e V, 675.3e V present.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 2
After 45g of methanol, 3g of fluorinated graphene (with an F/C ratio of 1.2 and 4 layers) and 2g of ammonia water are mixed uniformly, 50g of niobium fluoride is slowly added, the mixture is stirred for 4.5 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining the mixture for 6 hours at 800 ℃ in the nitrogen atmosphere, and cooling the mixture to prepare the powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 3
After 80g of isopropanol, 2.7g of ammonia water and 3g of fluorinated graphene (F/C ratio is 1.1, 5 layers) are mixed uniformly, 100g of niobium bromide is slowly added, the mixture is stirred for 3 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining the mixture for 10 hours at 500 ℃ in an argon atmosphere, and cooling the mixture to prepare a powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 4
After 50g of ethanol, 2g of fluorinated graphene (F/C ratio of 1.1, 5 layers) and 4g of ammonia water are mixed uniformly, 60g of niobium chloride is slowly added, the mixture is stirred for 7 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining for 8 hours at 700 ℃ in the argon atmosphere, and cooling to prepare the powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 5
After 50g of butanol, 1.6g of fluorinated graphene (with an F/C ratio of 1.2 and 3 layers) and 6g of ammonia water are uniformly mixed, 70g of niobium chloride is slowly added, the mixture is stirred for 5 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining for 8 hours at 600 ℃ in the argon atmosphere, and cooling to prepare the powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 6
Mixing 50g of ethanol, 2g of fluorinated graphene (with an F/C ratio of 0.28 and 12 layers) and 7g of ammonia uniformly, slowly adding 60g of niobium chloride, stirring for 5 hours, and evaporating the liquid to dryness to obtain an intermediate phase. Then calcining the mixture for 8 hours at 550 ℃ in an argon atmosphere, and cooling the mixture to prepare a powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 7
After 50g of methanol, 3g of fluorinated graphene (with an F/C ratio of 1.4 and 12 layers) and 5g of ammonia water are uniformly mixed, 80g of niobium iodide is slowly added, the mixture is stirred for 6 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining for 7.5 hours at 700 ℃ in the argon atmosphere, and cooling to prepare a powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 8
40g of propanol, 2g of fluorinated graphene (F/C ratio of 1.1, 5 layers) and 6g of ammonia water are mixed uniformly, 60g of niobium chloride is slowly added, the mixture is stirred for 5 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining for 8 hours at 600 ℃ in the argon atmosphere, and cooling to prepare the powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 9
Mixing 37g of ethanol, 2g of fluorinated graphene (F/C ratio of 1.1, 5 layers) and 5g of ammonia water uniformly, slowly adding 50g of niobium chloride, stirring for 5 hours, and evaporating the liquid to obtain an intermediate phase. Then calcining for 8 hours at 600 ℃ in the argon atmosphere, and cooling to prepare the powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Example 10
After 50g of ethanol, 2g of fluorinated graphene (F/C ratio of 1.1, 5 layers) and 8g of ammonia water are mixed uniformly, 65g of niobium chloride is slowly added, the mixture is stirred for 7 hours, and then the liquid is evaporated to dryness to obtain an intermediate phase. Then calcining the mixture for 12 hours at 800 ℃ in an argon atmosphere, and cooling the mixture to prepare a powder material.
The materials are subjected to electrode preparation and battery test, and the conditions of the electrode preparation and the battery test are shown in a table.
Figure GDA0002981917160000041
Figure GDA0002981917160000051
The data in the table show that when the electrode material is applied to a lithium ion battery as a negative electrode, the discharge capacity of the battery is obviously increased under a high-rate condition, the battery structure is more stable, and the capacity retention rate is improved by nearly one time.

Claims (10)

1. The application of the fluorinated graphene modified niobium pentoxide material as an electrode active material in a lithium battery cathode is characterized in that the fluorinated graphene modified niobium pentoxide material is formed by compounding fluorinated graphene and niobium pentoxide, and the surface of the material contains C-F-Nb bonds and F-Nb bonds; the niobium pentoxide accounts for 55-98% of the mass fraction of the fluorinated graphene modified niobium pentoxide material;
the preparation method of the fluorinated graphene modified niobium pentoxide material comprises the following specific steps:
1) fully dispersing and mixing organic alcohol, fluorinated graphene and ammonia water to form uniform liquid;
2) adding niobium halide with the mass of 1.0-20 times of that of the liquid into the liquid, stirring for 0.5-10 hours, stopping stirring, filtering, centrifuging or evaporating the liquid to obtain an intermediate phase, calcining the intermediate phase at the high temperature of 1000 ℃ under the inert atmosphere for 1-24 hours, and cooling to prepare a powder material;
the homogeneous liquid comprises the following components in parts by mass: 40-90 parts of organic alcohol, 0.1-5 parts of fluorinated graphene and 0.5-10 parts of ammonia water by mass percent, wherein the mass percent of the ammonia water is 40%.
2. Use according to claim 1, characterized in that:
the niobium pentoxide accounts for 55-98% of the mass fraction of the fluorinated graphene modified niobium pentoxide material, the carbon element accounts for 1-25% of the mass fraction of the fluorinated graphene modified niobium pentoxide material, and the fluorine element accounts for 0.2-20% of the mass fraction of the fluorinated graphene modified niobium pentoxide material.
3. Use according to claim 1, characterized in that: the mass fraction of niobium pentoxide in the fluorinated graphene modified niobium pentoxide material is 62-97%, the mass fraction of carbon in the fluorinated graphene modified niobium pentoxide material is 2-20%, and the mass fraction of fluorine in the fluorinated graphene modified niobium pentoxide material is 0.5-18%.
4. Use according to claim 1, characterized in that: the mass fraction of niobium pentoxide in the fluorinated graphene modified niobium pentoxide material is 70-94%, the mass fraction of carbon in the fluorinated graphene modified niobium pentoxide material is 5-18%, and the mass fraction of fluorine in the fluorinated graphene modified niobium pentoxide material is 0.8-15%.
5. Use according to claim 1, characterized in that:
and 2) adding niobium halide with the mass being 2.0-15 times of that of the liquid into the liquid, stirring for 1-8 hours, stopping stirring, filtering, centrifuging or evaporating the liquid to obtain an intermediate phase, calcining the intermediate phase at the temperature of 900 ℃ under an inert atmosphere for 2-20 hours at the temperature of 350-.
6. Use according to claim 1, characterized in that:
and 2) adding niobium halide with the mass being 4.0-10 times of that of the liquid into the liquid, stirring for 1.5-6 hours, stopping stirring, filtering, centrifuging or evaporating the liquid to obtain an intermediate phase, calcining the intermediate phase at the high temperature of 850 ℃ under an inert atmosphere, calcining for 3-12 hours, and cooling to prepare the powder material.
7. Use according to claim 1, characterized in that: the organic alcohol comprises one or more than two of methanol, ethanol, propanol, isopropanol and butanol;
the inert atmosphere is one or more than two of nitrogen, argon and helium;
the F/C ratio in the fluorinated graphene is 0.1-1.5; the number of layers of the fluorinated graphene is 1-15.
8. Use according to claim 1, characterized in that: the F/C ratio in the fluorinated graphene is 0.3-1.3; the number of layers of the fluorinated graphene is 1-10.
9. Use according to claim 1, characterized in that: the F/C ratio in the fluorinated graphene is 0.5-1.2; the number of layers of the fluorinated graphene is 1-5.
10. Use according to claim 1, characterized in that: the niobium halide is one or more than two of niobium fluoride, niobium chloride, niobium bromide and niobium iodide.
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Citations (2)

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CN108448104A (en) * 2018-05-10 2018-08-24 中南大学 A kind of niobium pentaoxide/carbon double quantum point nanocomposite and its preparation method and application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107413355A (en) * 2017-06-13 2017-12-01 中国矿业大学 A kind of Nb3O7The preparation method of F nano-arrays/graphene heterojunction composite
CN108448104A (en) * 2018-05-10 2018-08-24 中南大学 A kind of niobium pentaoxide/carbon double quantum point nanocomposite and its preparation method and application

Non-Patent Citations (2)

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Title
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Liaona She，et al..（"Nb2O5 Nanoparticles Anchored on an N-Doped Graphene Hybrid Anode for a Sodium-Ion Capacitor with High Energy Density".《ACS Omega》.2018,第3卷(第11期),第15943-15951页. *

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