CN112436118A - VO2(B) Carbon cloth self-supporting material and preparation method and application thereof - Google Patents
VO2(B) Carbon cloth self-supporting material and preparation method and application thereof Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
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- 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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to VO2(B) A carbon cloth self-supporting material, a preparation method and an application thereof. VO is directly obtained by a one-time hydrothermal method2(B) Carbon cloth self-supporting material and VO prepared from same2(B) The nano-sheet structure is a nano-sheet structure, the width of the nano-sheet is 100-300nm, the size of the nano-sheet is uniform, and the load on the carbon cloth is very uniform. The preparation method comprises the following steps: firstly, adding vanadium pentoxide and oxalic acid into distilled water, and reacting under the heating condition of a water bath to obtain a blue clear solution; adding 30 percent of H by mass2O2Uniformly stirring the solution; adding anhydrous ethyl acetateAlcohol is evenly stirred; transferring the obtained precursor solution into a reaction kettle, and putting the precursor solution into carbon cloth for hydrothermal reaction; washing the obtained active material with pure water for several times, and then placing the active material in a vacuum drying oven for drying to finally obtain VO2(B) A/carbon cloth self-supporting zinc ion battery anode material. The invention has the characteristics of simple process, mild reaction condition and excellent electrochemical performance of the material.
Description
Technical Field
The invention belongs to the technical field of nano materials and electrochemistry, and particularly relates to a controllable preparation method and application of a B-phase vanadium dioxide/carbon cloth self-supporting material, wherein the material can be used as a positive electrode active material of a zinc ion battery.
Background
With the continuous advance of industrialization, environmental pollution has become a necessary problem to be faced worldwide, and therefore, the development and use of clean green energy without discharging pollutants has become a strategic target of each country. With the improvement of new energy development technology, renewable new energy such as solar energy, wind energy, hydroenergy and the like are becoming important energy industry components. However, due to the unstable characteristic of renewable energy, if the renewable energy is directly incorporated into a power grid, the stable operation of the power grid is greatly influenced, so that the development of a large-scale efficient energy storage system has very important significance for the application of the renewable energy.
The current common lithium ion battery uses organic electrolyte, and the ionic conductivity of the electrolyte is 1-10 mS/cm. The zinc ion battery uses aqueous electrolyte, and the electrolyte has ion conductivity (about 1S/cm) far higher than that of organic electrolyte, so that the rate capability of the material can be greatly improved, and the quick response of a large-scale energy storage device in the power dispatching process is realized. In addition, the zinc ion battery has the advantages of low battery preparation cost, low battery toxicity, stability in aqueous solution, high energy density and power density, and the like, and is widely concerned by researchers.
Due to Zn2+The electrochemical reaction is realized by deintercalation inside the electrode material, and thus researchers believe that there is excellent Li+/Na+The electrode material with electrochemical performance in a layered or tunnel structure can be a potential high-performance zinc ion battery positive electrode material. However, the electrochemical stability window of the water-receiving electrolyte is narrow, and Zn2+Per Zn redox potential ratio Li+high/Li (Zn)2+/Zn：-0.76V vs SHE；Li+[ Li ]: -3.04V vs SHE), etcDue to factors, the number of positive electrode materials that can be used in zinc ion batteries is very limited. VO of B-phase vanadium dioxide through distortion6The octahedron is formed by connecting common angles and common edges and has a typical tunnel structure (the a axis direction is 0.34 nm)2And b-axis direction of 0.82nm2C-axis direction of 0.5nm2) And is beneficial to the rapid de-intercalation of the zinc ion battery. Ding et al investigators prepared VO by a simple hydrothermal method2(B) The discharge capacity of the material under the current density of 0.25A/g can reach 357mA h/g, and the discharge capacity under the current density of 51.2A/g can reach 171mA h/g. Chen et al prepared VO2(B) The nano-rod is used as the anode material of the zinc ion battery, the discharge capacity of the material under the current density of 0.05A/g can reach 325.6mA h/g, and the capacity retention rate after the material is circulated for 5000 times under the current density of 3A/g is 86%. However, Zn2+Has stronger electrostatic action with an interlayer structure in the de-intercalation process, and increases VO2Polarization during the electrochemical process eventually leads to collapse of the host structure. In addition, Zn in the course of electrochemical reaction4SO4(OH)6·0.5H2The O by-product is an electron insulator, and the generation of the by-product lowers the electron conductivity of the active material, deteriorating the electrochemical properties of the electrode material, so that the cycle stability of the material is to be further improved.
Researches show that the compounding of carbon-based and other electronic good conductor materials can effectively improve the conductivity of the active substance, and meanwhile, the material has a good electronic channel in the circulating process, so that the polarization of the electrode material in the electrochemical process is reduced, and the rate capability and the circulating stability of the material are improved. Dai et al, prepared RGO/VO2(B) The self-supporting material and the compounding of the graphene not only increase the carrier diffusion coefficient of the material, but also effectively reduce the Zn of the material2+The structural stress generated by the repeated de-intercalation. Therefore, the energy density of the material under the high power density of 7.8kW/kg can reach 65Wh/kg, and the capacity retention rate after 1000 cycles can reach 99%, so that the material shows excellent electrochemical performance. The carbon fiber cloth has wide industrial application, has the advantages of high conductivity, high strength, small density, thin thickness, mature preparation process and the like,carbon fiber cloth and VO2The compound of (A) is expected to effectively improve VO2(B) The electrochemical performance of the material is improved, and the application potential of the material is improved.
Disclosure of Invention
The invention aims to provide a VO (vacuum oxide) system aiming at the prior art2(B) The preparation method has simple process, meets the requirement of green chemistry and is convenient for amplification, and on the basis, VO (vanadium oxide) is prepared2(B) The/carbon cloth self-supporting material also has excellent electrochemical performance.
The technical scheme adopted by the invention for solving the technical problems is as follows: VO (vacuum vapor volume)2(B) A carbon cloth self-supporting material which is VO2(B) Uniformly distributed on carbon cloth, wherein VO2(B) VO of monoclinic system with phase and card number of 01-031-2The standard samples were completely matched with each other,
alpha-gamma-90 deg., beta-106.6 deg., space group C2/m, no hetero-phase peak and good crystallinity, and the VO has good crystallinity2(B) Contains crystal water of formula VO2·0.28H2And O. The introduction of the carbon cloth can provide a good electron transmission channel, and the carbon cloth can be used as a self-supporting carrier of an active material, thereby being beneficial to improving the diffusion rate of carriers and finally improving the electrochemical performance of the material.
According to the scheme, the VO2(B) The nano-sheet has a nano-sheet structure, the width of the nano-sheet is 100-300nm, and the size of the nano-sheet is uniform.
The VO2(B) The preparation method of the carbon cloth self-supporting material comprises the following steps:
1) adding vanadium pentoxide and oxalic acid into distilled water, and reacting under the water bath heating condition to obtain a solution;
2) addition of H2O2Uniformly stirring the solution;
3) adding absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction container, and putting the reaction container into carbon cloth for hydrothermal reaction;
5) cleaning the obtained active material for several times, and then drying in vacuum to finally obtain VO2(B) A carbon cloth self-supporting material.
According to the scheme, the water bath heating temperature in the step 1) is 70-90 ℃.
According to the scheme, the temperature of the hydrothermal reaction in the step 4) is 170-190 ℃, and the time is 80-120 min.
According to the scheme, the vacuum drying temperature in the step 5) is 60-80 ℃.
The VO2(B) The application of the carbon cloth self-supporting material as the positive active material of the zinc ion battery.
In the reaction system, because a large number of oxygen-containing functional groups and surface defects exist on the surface of the carbon cloth, the roughness of the surface of the carbon cloth is increased, and therefore VO2+The carbon cloth is easy to be attached to a carbon cloth substrate to generate a nucleation process. With the increase of the reaction time, ions in the precursor solution continuously diffuse to the nucleation points to further grow the crystal nucleus into a nano-sheet structure. The nano sheet structure realizes in-situ growth on the carbon cloth substrate, so that the nano sheet and the carbon cloth substrate have very strong binding force, thereby reducing agglomeration among the nano sheets, increasing the specific surface area of an electrode material and providing more active sites for electrochemical reaction. Meanwhile, the carbon cloth has the characteristic of high conductivity, and is beneficial to the transmission of electrons, so that the prepared VO2(B) The/carbon cloth self-supporting material can show excellent electrochemical performance.
The invention has the beneficial effects that: the invention mainly prepares VO by a simple and easy hydrothermal method2(B) The carbon cloth self-supporting material has the characteristics of high energy density, good rate capability and excellent cycling stability when being used as a zinc ion battery anode material; secondly, the method is simple in process, the target product can be obtained by directly carrying out hydrothermal reaction on the carbon cloth in the precursor solution, and a later heat treatment process is not needed. The method has strong feasibility, is easy to enlarge, accords with the characteristics of green chemistry, and is beneficial to market popularization.
Drawings
FIG. 1 is VO of example 1 of the present invention2(B) XRD pattern of/carbon cloth self-supporting material;
FIG. 2 shows VO of example 1 of the present invention2(B) A TG plot of a/carbon cloth self-supporting material;
FIG. 3 shows VO of example 1 of the present invention2(B) SEM image of/carbon cloth self-supporting material;
FIG. 4 shows VO of example 1 of the present invention2(B) A 0.5A/g cycle performance diagram of the carbon cloth self-supporting material;
FIG. 5 shows VO of example 1 of the present invention2(B) Multiplying power performance diagram of the carbon cloth self-supporting material.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
VO2(B) the preparation method of the carbon cloth self-supporting material comprises the following steps:
1) 0.3638g of vanadium pentoxide (V)2O5) And 0.7564g oxalic acid (C)2H2O4·2H2O) is added into 12mL of distilled water and reacts under the heating condition of water bath at 75 ℃ to obtain blue clear solution;
2) 3mL of 30% by mass H was added2O2Uniformly stirring the solution;
3) adding 65mL of absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction kettle, and putting carbon cloth into the reaction kettle to perform hydrothermal reaction, wherein the hydrothermal temperature is 180 ℃, and the hydrothermal time is 100 min;
5) washing the obtained active material with pure water for several times, and then placing the active material in a vacuum drying oven at 60 ℃ for drying to finally obtain VO2(B) A carbon cloth self-supporting material.
With the product VO of the invention2(B) The/carbon cloth self-supporting material is taken as an example, and the structure of the/carbon cloth self-supporting material is determined by an X-ray diffractometer. VO as shown in FIG. 12(B) VO of monoclinic system with phase and card number of 01-031-2The standard samples completely matched (
α ═ γ ═ 90 °, β ═ 106.6 °), space group C2/m, no hetero-phase peak, and good crystallinity. As shown in FIG. 2, the VO was maintained in a nitrogen atmosphere2(B) The weight loss of the material is 5.8 wt%, which is attributable to the removal of crystal water from the material, so that the material has a specific chemical formula of VO2·0.28H2O。
FIG. 3 is VO2(B) SEM image of/carbon cloth self-supporting material, VO is shown in the figure2(B) The nano-sheet structure is a nano-sheet structure, the width of the nano-sheet is 100-300nm, the size of the nano-sheet is uniform, and the nano-sheet is distributed on the carbon cloth very uniformly. The introduction of the carbon cloth can provide a good electron transmission channel, and the carbon cloth can be used as a self-supporting carrier of an active material, thereby being beneficial to improving the diffusion rate of carriers and finally improving the electrochemical performance of the material.
VO obtained in this example2(B) The application of the carbon cloth self-supporting material as the positive active material of the zinc ion battery is as follows: VO thus prepared2(B) The/carbon cloth self-supporting material is a positive electrode, the zinc sheet is a negative electrode, the 3M zinc trifluoromethanesulfonate aqueous solution is electrolyte, the diaphragm is a glass fiber diaphragm, and the battery shell is a CR2016 type stainless steel button battery shell.
FIG. 4 shows VO obtained in this example2(B) A cycle performance diagram of the carbon cloth self-supporting material under the current density of 0.5A/g. As can be seen from the figure, the initial discharge capacity of the material can reach 397mAh/g, and the specific discharge capacity after 500 cycles is kept at 194 mAh/g. FIG. 5 is VO2(B) The rate capability of the/carbon cloth self-supporting material under different current densities can reach 388, 339, 317, 304, 292, 281, 272, 264, 253, 244, 235, 224, 216, 210, 203, 197, 190, 186, 181, 176 and 173mAh/g respectively under the current densities of 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 and 20A/g, and the rate capability is very excellent. While the content of the carbon dioxide is not more than 0.5 to 20A/gAfter the charge and discharge with the same current density, the capacity of the material under the current density of 0.5A/g can be quickly recovered to 345mAh/g, which shows that the structure of the material is maintained under the high current density, and the material shows excellent rate performance and cycling stability, and is a potential zinc ion battery cathode material.
Example 2:
VO2(B) the preparation method of the carbon cloth self-supporting material comprises the following steps:
1) 0.3638g of vanadium pentoxide (V)2O5) And 0.7564g oxalic acid (C)2H2O4·2H2O) is added into 12mL of distilled water and reacts under the water bath heating condition of 70 ℃ to obtain blue clear solution;
2) 3mL of 30% by mass H was added2O2Uniformly stirring the solution;
3) adding 65mL of absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction kettle, and putting carbon cloth into the reaction kettle to perform hydrothermal reaction, wherein the hydrothermal temperature is 170 ℃, and the hydrothermal time is 90 min;
5) washing the obtained active material with pure water for several times, and then placing the active material in a vacuum drying oven at 70 ℃ for drying to finally obtain VO2(B) A carbon cloth self-supporting material.
VO obtained in this example2(B) VO at a current density of 0.5A/g for a carbon cloth self-supporting material2(B) The first discharge specific capacity of the carbon cloth self-supporting material can reach 360mAh/g, and the discharge specific capacity after 500 cycles is 180 mAh/g.
Example 3:
VO2(B) the preparation method of the carbon cloth self-supporting material comprises the following steps:
1) 0.3638g of vanadium pentoxide (V)2O5) And 0.7564g oxalic acid (C)2H2O4·2H2O) is added into 12mL of distilled water and reacts under the heating condition of water bath at the temperature of 80 ℃ to obtain blue clear solution;
2) 3mL of 30% by mass H was added2O2The solution is prepared by mixing a solvent and a solvent,stirring uniformly;
3) adding 65mL of absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction kettle, and putting into carbon cloth for hydrothermal reaction, wherein the hydrothermal temperature is 190 ℃ and the hydrothermal time is 80 min;
5) washing the obtained active material with pure water for several times, and then placing the active material in a vacuum drying oven at 80 ℃ for drying to finally obtain VO2(B) A carbon cloth self-supporting material.
VO obtained in this example2(B) VO at a current density of 0.5A/g for a carbon cloth self-supporting material2(B) The first discharge specific capacity of the/carbon cloth self-supporting material can reach 371mA h/g, and the discharge specific capacity after 500 cycles is 167mA h/g.
Example 4:
VO2(B) the preparation method of the carbon cloth self-supporting material comprises the following steps:
1) 0.3638g of vanadium pentoxide (V)2O5) And 0.7564g oxalic acid (C)2H2O4·2H2O) is added into 12mL of distilled water and reacts under the heating condition of water bath at 90 ℃ to obtain blue clear solution;
2) 3mL of 30% by mass H was added2O2Uniformly stirring the solution;
3) adding 65mL of absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction kettle, and putting into carbon cloth for hydrothermal reaction, wherein the hydrothermal temperature is 190 ℃ and the hydrothermal time is 110 min;
5) washing the obtained active material with pure water for several times, and then placing the active material in a vacuum drying oven at 80 ℃ for drying to finally obtain VO2(B) A carbon cloth self-supporting material.
VO obtained in this example2(B) VO at a current density of 0.5A/g for a carbon cloth self-supporting material2(B) The first discharge specific capacity of the/carbon cloth self-supporting material can reach 382mA h/g, and the discharge specific capacity after 500 cycles is 173mA h/g.
Example 5:
VO2(B) the preparation method of the carbon cloth self-supporting material comprises the following steps:
1) 0.3638g of vanadium pentoxide (V)2O5) And 0.7564g oxalic acid (C)2H2O4·2H2O) is added into 12mL of distilled water and reacts under the heating condition of water bath at 75 ℃ to obtain blue clear solution;
2) 3mL of 30% by mass H was added2O2Uniformly stirring the solution;
3) adding 65mL of absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction kettle, and putting into carbon cloth for hydrothermal reaction, wherein the hydrothermal temperature is 190 ℃ and the hydrothermal time is 120 min;
5) washing the obtained active material with pure water for several times, and then placing the active material in a vacuum drying oven at 70 ℃ for drying to finally obtain VO2(B) A carbon cloth self-supporting material.
VO obtained in this example2(B) VO at a current density of 0.5A/g for a carbon cloth self-supporting material2(B) The first discharge specific capacity of the/carbon cloth self-supporting material can reach 386mA h/g, and the discharge specific capacity after 500 cycles is 187mA h/g.
Claims (7)
1.VO2(B) A carbon cloth self-supporting material which is VO2(B) Uniformly distributed on carbon cloth, wherein VO2(B) VO of monoclinic system with phase and card number of 01-031-2The standard samples were completely matched with each other,
alpha-gamma-90 deg., beta-106.6 deg., space group C2/m, no hetero-phase peak and good crystallinity, and the VO has good crystallinity2(B) Contains crystal water of formula VO2·0.28H2O。
2. VO according to claim 12(B) The/carbon cloth self-supporting material is characterized in that the VO is2(B) The nano-sheet has a nano-sheet structure, the width of the nano-sheet is 100-300nm, and the size of the nano-sheet is uniform.
3. VO according to claim 12(B) The preparation method of the carbon cloth self-supporting material comprises the following steps:
1) adding vanadium pentoxide and oxalic acid into distilled water, and reacting under the water bath heating condition to obtain a solution;
2) addition of H2O2Uniformly stirring the solution;
3) adding absolute ethyl alcohol, and uniformly stirring to obtain a precursor solution;
4) transferring the precursor solution obtained in the step 3) into a reaction container, and putting the reaction container into carbon cloth for hydrothermal reaction;
5) cleaning the obtained active material for several times, and then drying in vacuum to finally obtain VO2(B) A carbon cloth self-supporting material.
4. VO according to claim 32(B) The preparation method of the carbon cloth self-supporting material is characterized in that the water bath heating temperature in the step 1) is 70-90 ℃.
5. VO according to claim 32(B) The preparation method of the carbon cloth self-supporting material is characterized in that the temperature of the hydrothermal reaction in the step 4) is 170-190 ℃, and the time is 80-120 min.
6. VO according to claim 32(B) The preparation method of the carbon cloth self-supporting material is characterized in that the vacuum drying temperature in the step 5) is 60-80 ℃.
7. VO according to claim 12(B) The application of the carbon cloth self-supporting material as the positive active material of the zinc ion battery.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113506873A (en) * | 2021-06-29 | 2021-10-15 | 常熟理工学院 | MXene composite modified VO2Zinc ion battery anode material and preparation method thereof |
| CN113511679A (en) * | 2021-06-30 | 2021-10-19 | 南京邮电大学 | Method for preparing carbon-coated vanadium dioxide positive electrode material |
| CN114335427A (en) * | 2021-11-18 | 2022-04-12 | 南京航空航天大学 | Three-dimensional V2O3@ carbon nanofiber composite flexible electrode and preparation method and application thereof |
| CN114335427B (en) * | 2021-11-18 | 2023-06-06 | 南京航空航天大学 | Three-dimensional V 2 O 3 Carbon nanofiber composite flexible electrode and preparation method and application thereof |
| CN114142107A (en) * | 2021-11-30 | 2022-03-04 | 江苏警官学院 | Aqueous lithium ion battery based on monoclinic-phase vanadium dioxide cathode |
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| CN114188542A (en) * | 2021-12-09 | 2022-03-15 | 中南大学 | Zinc-based MOF-loaded vanadium dioxide nano material and preparation and application thereof |
| CN114188542B (en) * | 2021-12-09 | 2024-01-26 | 中南大学 | Zinc-based MOF-loaded vanadium dioxide nano material and preparation and application thereof |
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