CN112210988B - Vanadium dioxide carbon fiber felt composite material and preparation method and application thereof - Google Patents
Vanadium dioxide carbon fiber felt composite material and preparation method and application thereof Download PDFInfo
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- CN112210988B CN112210988B CN202011111037.3A CN202011111037A CN112210988B CN 112210988 B CN112210988 B CN 112210988B CN 202011111037 A CN202011111037 A CN 202011111037A CN 112210988 B CN112210988 B CN 112210988B
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- carbon fiber
- fiber felt
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 60
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- NZVZAJKCDURHBK-UHFFFAOYSA-N [O-2].[O-2].[V+5].[C+4] Chemical compound [O-2].[O-2].[V+5].[C+4] NZVZAJKCDURHBK-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 50
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 41
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 239000003990 capacitor Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007772 electrode material Substances 0.000 abstract description 15
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 7
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910044991 metal oxide Inorganic materials 0.000 description 6
- 150000004706 metal oxides Chemical class 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- WDECIBYCCFPHNR-UHFFFAOYSA-N chrysene Chemical compound C1=CC=CC2=CC=C3C4=CC=CC=C4C=CC3=C21 WDECIBYCCFPHNR-UHFFFAOYSA-N 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/47—Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic System; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/40—Fibres
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention relates to a vanadium dioxide carbon fiber felt composite material and a preparation method and application thereof, belonging to the technical field of electrode materials. The invention provides a preparation method of a vanadium dioxide carbon fiber felt composite material, which comprises the following steps: a. pretreatment of the carbon fiber felt: soaking the carbon fiber felt in acetone, then washing with water, drying, heating at 100-200 ℃ for 3-5 hours, and keeping the treated carbon fiber felt for later use; b. preparing ethylene glycol vanadyl solution: mixing ammonium metavanadate: ethylene glycol is mixed according to the mass ratio of 1: (5-10), and reacting to generate ethylene glycol vanadyl for later use; c. preparing a composite material: b, soaking the carbon fiber felt obtained in the step a into the ethylene glycol vanadyl solution obtained in the step b, taking out the carbon fiber felt, drying, then placing in a tubular furnace, and introducing N 2 And reacting for 2-4 hours at 200-300 ℃ to obtain the catalyst. The preparation method has good popularization and application prospects.
Description
Technical Field
The invention relates to a vanadium dioxide carbon fiber felt composite material and a preparation method and application thereof, belonging to the technical field of electrode materials.
Background
The supercapacitor is an energy storage device with high efficiency, practicality and environmental protection, and has the advantages of high power density, convenient control, high conversion efficiency, wide working temperature range, no pollution and the like. With the improvement of the technical development level and the gradual reduction of the production cost, the super capacitor is more and more applied to the field of energy storage, and the super capacitor can replace a storage battery for storing energy on many occasions in the future. However, the price of the current super capacitor is still expensive, and the application of the super capacitor to large-scale power energy storage is limited. Therefore, further reduction of production cost is an essential step for the development of supercapacitors and the replacement of batteries in the future.
The super capacitor is composed of an electrode material, an electrolyte, a diaphragm, a collector and the like, each part has influence on the super capacitor, and the electrode material plays a decisive role in the performance of the super capacitor. Common electrode materials of the super capacitor include carbon materials, metal oxide materials, conductive polymer materials and composite materials. Among them, carbon materials are widely used as electrode materials for supercapacitors because of their low cost and various existing forms. However, since it stores energy only by using an electric double layer, there is a limitation in performance, and thus electrode development and research of metal oxide materials have been advanced. The metal oxide material is different from a carbon material electrode in an electric double layer capacitor for storing energy, and when the capacitor is charged and discharged, reversible oxidation-reduction reaction occurs at the interface of the metal oxide and a solution, so that higher specific capacity is obtained. Although the metal oxide material electrode has larger specific capacity, the price is expensive, and the development of a super capacitor is not facilitated. Conductive polymers such as polyaniline, polypyrrole and poly (3, 4-vinyl dioxyvinyl chrysene) which are commonly used are also widely used as electrode materials of the super capacitor, and are usually mixed with other electrode materials to prepare the super capacitor, but the price of the super capacitor is very high. The composite material is a composite material for performing a nano-composite technology by using a carbon material as a matrix and a metal oxide as an active substance to improve the charge utilization rate in order to further increase the energy storage of the supercapacitor and enable the supercapacitor to have pseudo-capacitance performance and electric double layer characteristics, and the material is a main direction for developing and researching the electrode material of the supercapacitor in the future.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention aims to provide a preparation method of the vanadium dioxide carbon fiber felt composite material. The invention also aims to provide the vanadium dioxide carbon fiber felt composite material prepared by the preparation method and application of the vanadium dioxide carbon fiber felt composite material in preparing an electrode.
The invention provides a composite electrode material especially suitable for a super capacitor, which is prepared by the following method: the method comprises the steps of taking ammonium metavanadate as a raw material, converting the ammonium metavanadate into ethylene glycol vanadyl, attaching the ethylene glycol vanadyl to a carbon fiber felt, and decomposing the ethylene glycol vanadyl into vanadium dioxide through calcination to obtain the vanadium dioxide carbon fiber felt composite material.
Specifically, the preparation method of the vanadium dioxide carbon fiber felt composite material comprises the following steps:
a. pretreatment of the carbon fiber felt: soaking the carbon fiber felt in acetone, then washing with water, drying, heating at 100-200 ℃ for 3-5 hours, and keeping the treated carbon fiber felt for later use;
b. preparing ethylene glycol vanadyl solution: mixing ammonium metavanadate: ethylene glycol is mixed according to the mass ratio of 1: (5-10), and reacting to generate ethylene glycol vanadyl for later use;
c. Preparing a composite material: b, soaking the carbon fiber felt obtained in the step a into the ethylene glycol vanadyl solution obtained in the step b, taking out the carbon fiber felt, drying, then placing in a tubular furnace, and introducing N 2 And reacting for 2-4 hours at 200-300 ℃ to obtain the catalyst.
Wherein, the step a and the step b can be carried out simultaneously or sequentially without specific operation sequence requirements.
Through the pretreatment step of the carbon fiber felt, impurities on the carbon fiber felt can be removed, active groups on the carbon fiber felt are increased, and the surface roughness of the carbon fiber felt is increased. After pretreatment, the ethylene glycol vanadyl can be effectively attached to the carbon fiber felt, the specific surface area of the composite material can be increased, and the performance of the electrode can be improved.
Further, in the step a, the carbon fiber felt is placed into acetone to be soaked for 24-48 hours.
Further, the drying in the step a is carried out in an oven at 60-80 ℃.
Further, the reaction temperature in the step b is 50-90 ℃.
Further, the reaction time in the step b is 3-6 hours.
Further, stirring at a speed of 400-600 r/min in the reaction process of the step b.
Further, the drying in the step c is carried out in an oven at 60-80 ℃.
And c, soaking to completely immerse the carbon fiber felt.
The invention provides a vanadium dioxide carbon fiber felt composite material prepared by the preparation method.
The invention provides application of the vanadium dioxide carbon fiber felt composite material in preparing an electrode.
Furthermore, the electrode is used for a super capacitor.
Compared with the prior art, the vanadium dioxide carbon fiber felt composite material and the preparation method thereof provided by the invention have the following advantages:
1. the production cost is low. The invention takes the carbon fiber felt and the ammonium metavanadate as raw materials to prepare the electrode material, and has lower production cost compared with the prior preparation method or other types of metal material electrodes.
2. The electrode material has good performance. The carbon fiber felt used in the invention has an activating effect through a special pretreatment process, and the electrode performance is effectively improved. On the other hand, the ammonium metavanadate is used as a raw material, is converted into ethylene glycol vanadyl oxide and then is attached to the carbon fiber felt, and then the ethylene glycol vanadyl oxide is decomposed into vanadium dioxide through calcination, so that the nano-scale vanadium dioxide can be introduced, and the performance of the electrode is better improved.
3. The production process is simple. The preparation method provided by the invention is simple to operate, short in flow, and suitable for industrial production, especially the content and the particle size of the introduced nano vanadium dioxide can be effectively controlled by adjusting the content of the ethylene glycol vanadyl oxide, so that convenient control can be realized, and other complicated operations are avoided.
4. Is environment-friendly. The invention has no generation and residue of toxic and harmful substances in the whole preparation process, and is beneficial to sustainable production.
Detailed Description
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The carbon fiber mats used below were pretreated as follows: and (2) soaking the carbon fiber felt in acetone for 24-48 hours, repeatedly washing with deionized water for 3-6 times, drying in an oven at 60-80 ℃, and heating to 100-200 ℃ for 3-5 hours.
Example 1 vanadium dioxide carbon fiber felt composite material prepared by the method of the present invention
Mixing ammonium metavanadate: mixing ethylene glycol according to the mass ratio of 1:6, reacting at 50 ℃ for 6 hours, stirring at the speed of 600r/min during the reaction, cooling to room temperature, filtering (the purpose of filtering is to remove part of incompletely reacted ammonium metavanadate), and standing the filtrate. Directly immersing the carbon fiber felt obtained through the pretreatment into the filtrate, taking out the carbon fiber felt, and putting the carbon fiber felt into an oven to dry at 60 ℃. And (3) putting the dried carbon fiber felt into a tubular furnace, and reacting for 3 hours at 300 ℃. The prepared composite material is used as an electrode material, and the specific capacitance of the electrode is 0.198F-cm -2 At a current density of 10 mA/cm -2 Then, the specific capacitance was 91.05% of the initial value after 2000 cycles of charge and discharge. Through detection, the particle size of the vanadium dioxide in the composite material is 70-90 nm.
Example 2 vanadium dioxide carbon fiber felt composite material prepared by the method of the invention
Mixing ammonium metavanadate: mixing ethylene glycol according to the mass ratio of 1:8, reacting at 60 ℃ for 5 hours, stirring at the speed of 500r/min during the reaction, cooling to room temperature, filtering (the purpose of filtering is to remove part of incompletely reacted ammonium metavanadate), and standing the filtrate. Directly immersing the carbon fiber felt obtained through pretreatment into the filtrate, taking out the carbon fiber felt, and putting the carbon fiber felt into an oven to be dried at 70 ℃. And (3) putting the dried carbon fiber felt into a tubular furnace, and reacting for 3 hours at 250 ℃. To prepare to obtainThe composite material of (2) as an electrode material, the specific capacitance of the electrode being 0.211F-cm -2 At a current density of 15mA cm -2 Then, the specific capacitance was 90.02% of the initial value after 2000 cycles of charge and discharge. Through detection, the particle size of the vanadium dioxide in the composite material is 55-90 nm.
Example 3 vanadium dioxide carbon fiber felt composite material prepared by the method of the invention
Mixing ammonium metavanadate: mixing ethylene glycol according to the mass ratio of 1:10, reacting at 80 ℃ for 4 hours, stirring at the speed of 400r/min during the reaction, cooling to room temperature, filtering (the purpose of filtering is to remove part of incompletely reacted ammonium metavanadate), and standing the filtrate. Directly immersing the carbon fiber felt obtained through pretreatment into the filtrate, taking out the carbon fiber felt, and putting the carbon fiber felt into an oven to be dried at 80 ℃. And (3) putting the dried carbon fiber felt into a tube furnace, and reacting for 3 hours at 200 ℃. The prepared composite material is used as an electrode material, and the specific capacitance of the electrode is 0.241F-cm -2 At a current density of 15mA · cm -2 Then, the specific capacitance after 2000 cycles was 92.11% of the initial value. Through detection, the particle size of the vanadium dioxide in the composite material is 40-90 nm.
It should be appreciated that the particular features, structures, materials, or characteristics described in this specification may be combined in any suitable manner in any one or more embodiments. Furthermore, the various embodiments and features of the various embodiments described in this specification can be combined and combined by one skilled in the art without contradiction.
Claims (9)
1. The preparation method of the vanadium dioxide carbon fiber felt composite material is characterized by comprising the following steps: the method comprises the following steps:
a. pretreatment of the carbon fiber felt: soaking the carbon fiber felt in acetone, then washing with water, drying, heating at 100-200 ℃ for 3-5 hours, and keeping the treated carbon fiber felt for later use;
b. preparing ethylene glycol vanadyl solution: mixing ammonium metavanadate: ethylene glycol is mixed according to the mass ratio of 1: (5-10), and reacting to generate ethylene glycol vanadyl for later use;
c. preparing a composite material: b, soaking the carbon fiber felt obtained in the step a into the ethylene glycol vanadyl solution obtained in the step b, taking out the carbon fiber felt, drying, then placing in a tubular furnace, and introducing N 2 And reacting for 2-4 hours at 200-300 ℃ to obtain the catalyst.
2. The method of claim 1, wherein: step a, soaking the carbon fiber felt in acetone for 24-48 hours.
3. The method of claim 1, wherein: and a step a, drying in an oven at 60-80 ℃.
4. The method of claim 1, wherein: the reaction temperature in the step b is 50-90 ℃.
5. The method of claim 1, wherein: the reaction time in the step b is 3-6 hours.
6. The method of claim 1, wherein: and c, drying in an oven at 60-80 ℃.
7. The vanadium dioxide carbon fiber felt composite material prepared by the preparation method of any one of claims 1 to 6.
8. Use of the vanadium dioxide carbon fiber mat composite material according to claim 7 for the production of electrodes.
9. Use according to claim 8, characterized in that: the electrode is used for a super capacitor.
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| WO2017049466A1 (en) * | 2015-09-22 | 2017-03-30 | 许昌学院 | Composite electrode material, manufacturing method thereof, and use thereof in vanadium flow battery |
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| CN102795968A (en) * | 2012-09-12 | 2012-11-28 | 西南大学 | Preparation method of vanadyl ethylene glycol and method for preparing M-phase vanadium dioxide powder from vanadyl ethylene glycol |
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