CN113451558A - Organic-inorganic hybrid material and preparation method and application thereof - Google Patents
Organic-inorganic hybrid material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 11
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229960000583 acetic acid Drugs 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- 239000007772 electrode material Substances 0.000 claims description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 5
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910001413 alkali metal ion Inorganic materials 0.000 claims description 2
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000007774 positive electrode material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000007773 negative electrode material Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052783 alkali metal Inorganic materials 0.000 abstract 1
- 150000001340 alkali metals Chemical class 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000010406 cathode material Substances 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910000314 transition metal oxide Inorganic materials 0.000 description 4
- 229910003206 NH4VO3 Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002127 nanobelt Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- ZMLPZCGHASSGEA-UHFFFAOYSA-M zinc trifluoromethanesulfonate Chemical compound [Zn+2].[O-]S(=O)(=O)C(F)(F)F ZMLPZCGHASSGEA-UHFFFAOYSA-M 0.000 description 1
- CITILBVTAYEWKR-UHFFFAOYSA-L zinc trifluoromethanesulfonate Substances [Zn+2].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F CITILBVTAYEWKR-UHFFFAOYSA-L 0.000 description 1
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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
-
- 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
-
- 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
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive 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
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses an organic-inorganic hybrid material and a preparation method and application thereof. The preparation method comprises the following steps: (1) adding a vanadium source into glacial acetic acid, and stirring to form a uniform suspension solution; (2) carrying out hydrothermal reaction on the suspension solution obtained in the step (1) to obtain an organic-inorganic hybrid material, namely VO (CH)3COO)2. The organic-inorganic hybrid material prepared by the invention has good crystallinity and high purity, can be widely used in the fields of batteries, capacitors, catalysis and the like, has excellent electrochemical performance, and is particularly suitable for producing high-performance alkali metal ionsA battery negative electrode material and a water-based zinc ion battery positive electrode material.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to an organic-inorganic hybrid material and a preparation method and application thereof.
Background
The Transition Metal Oxides (TMOs) as the battery electrode material have high theoretical specific capacity and are a battery electrode material with great development prospect. However, the inherently low conductivity has hindered the use of TMOs. If TMOs structures are coupled to conducting polymer ligands, the kinetics of the electrochemical reaction of the corresponding cell may be promoted.
VO(CH3COO)2Is an organic-inorganic hybrid material, belongs to an orthorhombic system, has a space group Cmc21 and has a one-dimensional chain structure, wherein VO6Octahedron connected by vanadium groups, each pair of adjacent VOs6The octahedron is bridged by two acetate ions. In addition, these one-dimensional chains are well separated. The unique structure makes the material have potential application value. But at present VO (CH) is synthesized3COO)2The method has complex process and low product purity.
Disclosure of Invention
In order to overcome the above disadvantages, the present invention aims to provide an organic-inorganic hybrid material, and a preparation method and an application thereof. The preparation method is simple and controllable, and the VO (CH) synthesized by the method3COO)2Has excellent electrochemical performance.
The purpose of the invention is realized by the following technical scheme.
A method for preparing an organic-inorganic hybrid material, comprising the steps of:
(1) adding a vanadium source into glacial acetic acid, and stirring to form a uniform suspension solution;
(2) carrying out hydrothermal reaction on the suspension solution obtained in the step (1) to obtain an organic-inorganic hybrid material, namely VO (CH)3COO)2。
Preferably, the vanadium source in step (1) is ammonium metavanadate (NH)4VO3) Vanadium pentoxide (V)2O5) And sodium orthovanadate (Na)3VO4) One or more of them.
Preferably, the vanadium source is ammonium metavanadate.
Preferably, the temperature of the hydrothermal reaction in the step (2) is 60-220 ℃.
Preferably, the hydrothermal reaction time in the step (2) is 1-30 hours.
Preferably, the temperature of the hydrothermal reaction is 200-220 ℃ and the time is 12-24 hours.
Preferably, the dosage of vanadium in the vanadium source and glacial acetic acid is 0.1-0.25 mmol/ml.
Preferably, in the step (2), after the hydrothermal reaction of the suspension solution, cooling to room temperature, and then sequentially centrifuging, drying and grinding; the drying temperature is between room temperature and 180 ℃.
An organic-inorganic hybrid material prepared by the above-described preparation method.
The organic-inorganic hybrid material is applied to the negative electrode material of the alkali metal ion battery and the positive electrode material of the water-based zinc ion battery.
Compared with the prior art, the invention has the following advantages:
(1) the invention adopts a hydrothermal method to synthesize pure-phase VO (CH)3COO)2The method has the advantages of simple preparation process, controllable yield, rich raw material sources and suitability for industrial production.
(2) VO (CH) synthesized by the invention3COO)2The material has not been applied to the battery field at present, and the material is used as a battery electrode material for the first time as an attempt application.
(3) VO (CH) synthesized by the invention3COO)2The material has wide application, not only can be used as an electrode material in the field of energy storage, but also can be used in the fields of catalysis and the like.
Drawings
FIG. 1 shows VO (CH) in example 1 of the present invention3COO)2X-ray diffraction patterns of (a);
FIG. 2 shows VO (CH) in example 1 of the present invention3COO)2Scanning electron microscope pictures;
FIG. 3 shows VO (CH) in example 1 of the present invention3COO)2Transmission electron microscope pictures;
FIG. 4 shows VO (CH) in example 1 of the present invention3COO)2As a cycle performance curve diagram of the lithium ion battery cathode;
FIG. 5 shows VO (CH) in example 2 of the present invention3COO)2As a cycle performance curve diagram of the positive electrode of the zinc ion battery;
FIG. 6 shows an embodiment of the present inventionVO (CH) in 33COO)2X-ray diffraction patterns of (a);
FIG. 7 shows VO (CH) in example 4 of the present invention3COO)2X-ray diffraction pattern of (a).
Detailed Description
The practice of the present invention will be further illustrated, but is not limited, by the following examples and the accompanying drawings.
Example 1
Adding 10mmol NH4VO3Adding 40ml of glacial acetic acid, and uniformly stirring on a magnetic stirrer to form a uniform suspension solution; transferring the obtained suspension solution to a high-pressure reaction kettle for hydrothermal reaction at 200 ℃ for 24 hours, cooling to room temperature, centrifuging, drying, and grinding to obtain VO (CH)3COO)2。
The X-ray diffraction pattern of the product obtained in this example is shown in FIG. 1, and it can be seen from FIG. 1 that VO (CH) in a pure phase orthorhombic crystal form is synthesized by the method3COO)2A material. And an impurity peak does not exist in a spectrogram, so that the product purity is high. The scanning electron micrograph of the product is shown in FIG. 2, and it can be seen that VO (CH)3COO)2The nano-belt structure is presented, the length is several micrometers to dozens of micrometers, and the width is about 300-1000 nm. The transmission electron microscope picture of the product is shown in fig. 3, and the surface of a single nanobelt is very smooth and the width of the nanobelt is about 300 nm.
Manufacturing an electrode plate: VO (CH) prepared in this example3COO)2Fully mixing and grinding a conductive agent Super P and a binder PVDF in NMP (1-methyl-2 pyrrolidone) according to the proportion of 70:15:15 to obtain uniform slurry, coating the slurry on a current collector copper foil, then copying for 30 minutes under an infrared lamp to bake a surface solvent, and finally completely drying in a vacuum oven at 90 ℃ for one night to obtain the electrode plate;
assembling the battery: VO (CH) obtained above3COO)2The pole piece is a working electrode, the lithium piece is a counter electrode, and 1M LiPF6EC (EC) of (C) DEC (EMC) (1:1:1 vol.%) is electrolyte, Celgard2320 is diaphragm, and the diaphragm is assembled into a CR2032 type button cell in a high-purity argon glove box.
And (3) testing the battery: the button cell prepared above was tested in the wuhan blue-electricity system with a room temperature constant at 25 ℃.
VO (CH) of this example3COO)2When the lithium ion battery cathode material is used in a voltage range of 0.01-3V and the current density is 200mA/g, the cycle performance is shown in figure 4. VO (CH) is shown in FIG. 43COO)2As the activation behavior of the lithium ion battery cathode material, the initial charging specific capacity is about 613mAh/g, and after 100 cycles of activation, the specific capacity of the battery reaches 1065 mAh/g. Illustrates VO (CH) prepared in this example3COO)2The lithium ion battery cathode material has high specific capacity and excellent cycling stability, and is a very potential lithium ion battery cathode material.
Example 2
Adding 10mmol NH4VO3Adding 40ml of glacial acetic acid, and uniformly stirring on a magnetic stirrer to form a uniform suspension solution; transferring the obtained suspension solution to a high-pressure reaction kettle for hydrothermal reaction at 200 ℃ for 24 hours, cooling to room temperature, centrifuging, drying, and grinding to obtain VO (CH)3COO)2。
Manufacturing an electrode plate: VO (CH) prepared in this example3COO)2Fully mixing and grinding a conductive agent Super P and a binder PVDF in NMP (1-methyl-2 pyrrolidone) according to the proportion of 70:15:15 to obtain uniform slurry, coating the slurry on a current collector titanium foil, then copying for 30 minutes under an infrared lamp to bake a surface solvent, and finally completely drying in a vacuum oven at 90 ℃ for one night to obtain an electrode plate;
assembling the battery: VO (CH) obtained above3COO)2The CR2032 type button cell is assembled in the air by taking the pole piece as a working electrode, the zinc piece as a counter electrode, 3M zinc trifluoromethanesulfonate as electrolyte and glass fiber as a diaphragm.
And (3) testing the battery: the button cell prepared above was tested in the wuhan blue-electricity system with a room temperature constant at 25 ℃.
VO (CH) prepared in this example3COO)2The cycle performance of the zinc electrode material in the voltage range of 0.2-1.6V is shown in figure 5. VO (CH) is shown in FIG. 53COO)2As an activation behavior of the positive electrode material of the zinc ion battery, the initial charging specific capacity is about 100mAh/g, and after 8 cycles of activation, the specific capacity of the battery is up to 222 mAh/g. Illustrates VO (CH) prepared in this example3COO)2The zinc ion battery cathode material has excellent electrochemical performance and is a very potential zinc ion battery cathode material.
Example 3
Adding 3mmol NH4VO3Adding the mixture into 30ml of glacial acetic acid, and uniformly stirring the mixture on a magnetic stirrer to form a uniform suspension solution; transferring the obtained suspension solution to a high-pressure reaction kettle for hydrothermal reaction at 220 ℃ for 12 hours, cooling to room temperature, centrifuging, drying, and grinding to obtain VO (CH)3COO)2。
The X-ray diffraction pattern of the product obtained in this example is shown in FIG. 6, and it can be seen from FIG. 6 that VO (CH) in orthorhombic form was synthesized by this method3COO)2A material.
Example 4
Mixing 5mmol V2O5Adding 40ml of glacial acetic acid, and uniformly stirring on a magnetic stirrer to form a uniform suspension solution; transferring the obtained suspension solution to a high-pressure reaction kettle for hydrothermal reaction at 200 ℃ for 24 hours, cooling to room temperature, centrifuging, drying, and grinding to obtain VO (CH)3COO)2。
The X-ray diffraction pattern of the product obtained in this example is shown in FIG. 7, and it can be seen from FIG. 7 that VO (CH) in orthorhombic form was synthesized by this method3COO)2A material.
As can be seen from the above examples, the organic-inorganic hybrid material VO (CH) prepared by the present invention3COO)2The zinc-ion battery anode and the zinc-ion battery cathode both have excellent electrochemical performance, and the preparation method is simple and easy to implement, low in cost and suitable for industrial production. Due to the fact thatVO (CH) prepared by hydrothermal method3COO)2Is expected to become a next-generation novel battery electrode material.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (10)
1. A method for preparing an organic-inorganic hybrid material, comprising the steps of:
(1) adding a vanadium source into glacial acetic acid, and stirring to form a uniform suspension solution;
(2) carrying out hydrothermal reaction on the suspension solution obtained in the step (1) to obtain an organic-inorganic hybrid material, namely VO (CH)3COO)2。
2. The preparation method according to claim 1, wherein the vanadium source in step (1) is one or more of ammonium metavanadate, vanadium pentoxide and sodium orthovanadate.
3. The method according to claim 2, wherein the vanadium source is ammonium metavanadate.
4. The method according to any one of claims 1 to 3, wherein the hydrothermal reaction in step (2) is carried out at a temperature of 60 to 220 ℃ for 1 to 30 hours.
5. The method according to claim 4, wherein the hydrothermal reaction is carried out at a temperature of 200 to 220 ℃ for 12 to 24 hours.
6. The method according to claim 4, wherein the vanadium source has a vanadium/glacial acetic acid ratio of 0.1-0.25 mmol/ml.
7. The preparation method according to claim 4, wherein in the step (2), the suspension solution is cooled to room temperature after hydrothermal reaction, and then is subjected to centrifugation, drying and grinding in sequence; the drying temperature is between room temperature and 180 ℃.
8. An organic-inorganic hybrid material produced by the production method according to any one of claims 1 to 7.
9. Use of the organic-inorganic hybrid material according to claim 8 as a battery electrode material, catalyst.
10. Use according to claim 9, wherein the battery is an alkali metal ion battery or an aqueous zinc ion battery.
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-
2021
- 2021-06-28 CN CN202110716359.9A patent/CN113451558A/en active Pending
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