CN116168956A - Method for preparing metal oxide electrode material by UV photo-thermal assistance - Google Patents
Method for preparing metal oxide electrode material by UV photo-thermal assistance Download PDFInfo
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- 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
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- H01G11/46—Metal oxides
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a method for preparing a metal oxide electrode material by UV photo-thermal assistance, which comprises the following steps: immersing the foam nickel substrate into dilute hydrochloric acid, performing ultrasonic treatment, and then washing and drying; putting the dried foam nickel substrate into a reaction kettle containing a reaction solution, performing hydrothermal treatment, and drying to obtain a precursor of the CoMnO nano array; and (3) placing the precursor of the CoMnO nano array in the center of a quartz tube, and carrying out photo-thermal treatment under the condition of low flow rate of protective gas to obtain the UV photo-thermal treatment Co/Mn oxide material. The material provided by the invention has the advantages of simple preparation method, no byproduct generation, safe and green operation and short time, and is suitable for large-scale production, and the material can be obtained only by irradiation treatment with UV light under a protective atmosphere. The method can also carry out photo-thermal treatment for a period of time together with a nitrogen source or a sulfur source in a protective atmosphere when the precursor is photo-thermally treated, so that the nitrogen doping or the sulfur doping can be simply and quickly carried out, and the material performance can be further improved.
Description
Technical Field
The invention relates to the technical field of capacitance materials, in particular to a method for preparing a metal oxide electrode material by UV photo-thermal assistance.
Background
At present, many research efforts have demonstrated graphene and RuO 2 、MnO 2 And carbon-based materials such as conductive polymers and pseudocapacitor materials have very excellent capacitance performance as electrode materials of supercapacitors. Since the energy storage of such electrode materials is mainly performed on the surface or near-surface of the active material, there is a limit in improving the energy density. In order to further increase the energy density of the supercapacitor, it is necessary to introduce a battery-type electrode material capable of achieving efficient redox reactions. The faraday redox reaction can go deep into the bulk phase of the material, so battery-type electrode materials can generally provide higher capacities than carbon-based materials and pseudocapacitor materials. Research shows that the hybrid supercapacitor taking the battery material as the positive electrode and the capacitor material as the negative electrode can well balance the power density and the energy density, so the battery type metal oxide electrode material shows great prospect as the supercapacitor electrode.
The metal oxide electrode material has huge potential application in the field of super capacitors due to the ultrahigh theoretical specific capacity. Currently, the transition metal oxide powder material or film material is generally obtained by heat-treating a precursor thereof in a resistance furnace at 300-1000 ℃. Microwave heating and laser heating methods are rarely used for transition metal oxide materials and are too expensive to be applied on a large scale compared to conventional heat treatments.
In recent years, microwave heating and laser heating methods are increasingly applied to synthesis and processing of functional materials with excellent electrochemical energy storage performance, such as graphene, carbon nanotubes, graphene supported catalysts and the like. However, these methods are less useful for transition metal oxide materials and difficult to apply on a large scale.
Therefore, providing a method for preparing an excessive metal oxide electrode material with UV photo-thermal assistance is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the present invention provides a variety of methods for UV photothermal assisted preparation of transition metal oxide electrode materials. The invention uses a high-pressure mercury lamp as a heating light source to heat treat the sample so as to obtain the high-performance electrode material. Compared to expensive laser heating and microwave heating equipment, the equipment required for this method is cheaper and can process samples on a large scale. Because the technology is mainly based on the photo-thermal effect induced by Ultraviolet (UV) light emitted by a high-pressure mercury lamp, compared with the traditional resistance furnace heating treatment, the UV photo-thermal treatment metal oxide material has better electrochemical performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing a metal oxide electrode material by UV photo-thermal assistance, comprising the following steps:
(1) Immersing a foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, respectively washing the foam nickel substrate with water and ethanol, and then placing the foam nickel substrate into a blast drying oven for drying;
(2) Mixing ammonium fluoride, manganese nitrate, urea and cobalt nitrate, dissolving in water to form a reaction solution, putting the dried foam nickel substrate into a reaction kettle containing the reaction solution, performing hydrothermal treatment, and then cleaning and drying the reacted product to obtain a precursor of the CoMnO nano array;
(3) And (3) placing the precursor of the CoMnO nano array in the center of a quartz tube, placing a high-pressure mercury vapor lamp right above the precursor of the CoMnO nano array, carrying out photo-thermal treatment under the condition of protective gas, then preserving heat, and naturally cooling to room temperature to obtain the UV photo-thermal treatment Co/Mn oxide material.
Further, the foam nickel substrate in step (1) has a gauge of 2.5cm by 1cm.
Further, the dilute hydrochloric acid concentration in the step (1) is 0.1mol/l
The ultrasonic power is 180W, and the ultrasonic time is 10min.
The beneficial effect of adopting above-mentioned further scheme lies in: the scheme of the invention can effectively remove the pollutants such as oxides and grease on the surface of the foam nickel, and is beneficial to the formation of the nano array.
Further, in the reaction solution in the step (2), the concentration of ammonium fluoride is 0.1mmol/ml, the concentration of manganese nitrate is 0.067mmol/ml, the concentration of urea is 0.2mmol/ml, and the concentration of cobalt nitrate is 0.067mmol/ml.
Further, the hydrothermal reaction temperature in the step (2) is 120 ℃, and the reaction time is 2-8 hours;
the drying temperature is 60 ℃, and the drying time is 2-5h.
Further, the power of the high-pressure mercury vapor lamp used in the photo-thermal treatment in the step (3) is 2KW.
Further, the photo-thermal treatment method in the step (3) is as follows: and heating the precursor of the CoMnO nano array to 350 ℃ at the speed of 10 ℃/min from room temperature under the irradiation of light, and then preserving the heat for 2-5h.
The beneficial effect of adopting above-mentioned further scheme lies in: according to the scheme, the oxide precursor can be annealed by fully utilizing the ultraviolet photothermal effect, and the obtained electrode material sample has excellent charge storage performance compared with a conventional tubular resistance annealing sample.
Further, in the step (3), the shielding gas is one of argon, nitrogen and helium.
The beneficial effect of adopting above-mentioned further scheme lies in: according to the invention, the protective gas is introduced to avoid the oxidation of foam nickel on the sample substrate.
The invention has the beneficial effects that: the material preparation method is simple, can be obtained by only irradiating with UV light for a period of time under a protective atmosphere, has no byproducts, has the advantages of safe and green operation and short time, and is suitable for large-scale production. The method can also carry out photo-thermal treatment for a period of time together with a nitrogen source or a sulfur source in a protective atmosphere when the precursor is photo-thermally treated, so that the nitrogen doping or the sulfur doping can be simply and quickly carried out, and the material performance can be further improved.
According to the method, the microstructure of the nano sheet and the nano wire is regulated and optimized through the photo-thermal synergistic effect induced by ultraviolet light, so that more effective oxidation-reduction reaction occurs, the adsorption of electrolyte ions is more facilitated, the energy storage capacity is increased, and the method has advantages compared with a tube furnace heat treatment method under the same condition.
Compared with the traditional annealing treatment, the method provided by the invention has the advantages of better performance, simple preparation method, safe and green operation and short time, and is suitable for large-scale production.
Drawings
FIG. 1 is an XRD pattern of a UV photothermal treated Co/Mn oxide nanoarray prepared in example 1 of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of a UV photothermal treated Co/Mn oxide nanoarray prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
EXAMPLE 1UV photothermal treatment of Co/Mn oxide precursor
1) Immersing a 2.5cm multiplied by 1cm foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, washing the foam nickel substrate with water and ethanol respectively, and drying in a blast drying oven;
2) Dissolving 3mmol of ammonium fluoride, 2mmol of manganese nitrate, 6mmol of urea and 2mmol of cobalt nitrate in 30mL of deionized water to prepare a reaction solution, placing a clean foam nickel substrate and the prepared reaction solution into a reaction kettle, adding water to carry out hydrothermal reaction at 120 ℃ for 2 hours, carrying out hydrothermal treatment, and drying the reaction product at 60 ℃ for 2 hours after washing. Obtaining a precursor of the CoMnO nano array;
3) And 2) placing the CoMnO precursor obtained in the step 2) in the center of a quartz tube, placing a high-pressure mercury vapor lamp right above a sample, heating the precursor of the CoMnO nano array to 350 ℃ from room temperature at a speed of 10 ℃/min under the condition of inert gas with low flow rate, preserving heat for 3 hours, and naturally cooling to room temperature to obtain the UV photothermal treatment Co/Mn oxide material.
As shown in FIG. 1, the XRD pattern of the CoMnO of the present example is shown, and after photo-thermal treatment, the diffraction peak CoMn of the CoMnO 2 O 4 (PDF#77-0471) and mixed valence spinel (Co, mn) 2 O 4 (PDF # 18-0408) was very matched, indicating successful Co/Mn oxide preparation by photothermal treatment.
As shown in fig. 2, which is an SEM image of the Co/Mn oxide nano-array subjected to UV photo-thermal treatment in this example, it can be seen from the image that the Co/Mn oxide nano-array subjected to UV photo-thermal treatment is uniformly distributed on the surface of the nickel foam, and these nanowires show rough edges and develop independently, so as to form a three-dimensional porous structure.
EXAMPLE 2UV photothermal treatment of Co/Mn oxide nanoarrays
1) Immersing a 2.5cm multiplied by 1cm foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, washing the foam nickel substrate with water and ethanol respectively, and drying in a blast drying oven;
2) Dissolving 2mmol of manganese nitrate, 1mmol of cobalt nitrate, 3mmol of ammonium fluoride and 6mmol of urea in 30mL of deionized water to prepare a reaction solution, and transferring the prepared solution into a stainless steel autoclave lined with polytetrafluoroethylene;
3) The clean nickel foam was placed in the mixed solution for 24 hours and then heated at 120 ℃ for 6 hours.
4) Cooling the foam nickel loaded with the MnCo hydroxide precursor to room temperature, repeatedly washing with deionized water, and drying at 60 ℃ for 24 hours;
5) And (3) placing the dried MnCo hydroxide precursor into a quartz tube, performing heat treatment on the quartz tube by utilizing a high-pressure mercury lamp under an argon environment for 2 hours, and cooling to room temperature to obtain the foam nickel-loaded MnCo oxide nano array.
EXAMPLE 3UV photothermal treatment of Ni/Co oxide nanoarrays
1) Immersing a 2.5cm multiplied by 1cm foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, washing the foam nickel substrate with water and ethanol respectively, and drying in a blast drying oven;
2) Dissolving 2mmol of nickel nitrate, 1mmol of cobalt nitrate, 3mmol of ammonium fluoride and 6mmol of urea in 30mL of deionized water to prepare a reaction solution, and transferring the prepared solution into a stainless steel autoclave lined with polytetrafluoroethylene;
3) The clean nickel foam was placed in the mixed solution for 24 hours and then heated at 120 ℃ for 6 hours. And cooling the nickel foam loaded with the NiCo hydroxide precursor to room temperature, repeatedly washing with deionized water, and drying at 60 ℃ for 24 hours.
4) And (3) placing the dried nickel-loaded hydroxide precursor into a quartz tube, performing heat treatment on the quartz tube for 2 hours by utilizing a high-pressure mercury lamp in an argon environment, and cooling to room temperature to obtain the nickel-loaded Ni/Co oxide nano array.
Example 4 photothermal treatment of Nitrogen doped Co/Mn oxide nanoarrays
1) Immersing a 2.5cm multiplied by 1cm foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, washing the foam nickel substrate with water and ethanol respectively, and drying in a blast drying oven;
2) 3mmol of ammonium fluoride, 2mmol of manganese nitrate, 6mmol of urea, 2mmol of cobalt nitrate and 30mL of deionized water are taken to prepare a solution, clean foam nickel and the prepared solution are put into a reaction kettle, and water is added to heat for 2 hours at 120 ℃. After the hydrothermal treatment, the washed sample was dried at 60℃for 2 hours. Obtaining a precursor of the CoMnO nano array;
3) And 2) respectively placing the CoMnO precursor obtained in the step 2) and 2g of ammonium bicarbonate in two transparent crucibles, placing the two crucibles in the center of a quartz tube, placing a high-pressure mercury lamp right above a sample, carrying out photo-thermal treatment under the condition of low flow rate of argon, heating to 350 ℃ at the speed of 10 ℃/min, and preserving heat for 3 hours. And finally, naturally cooling to room temperature, and taking out to obtain the nitrogen-doped Co/Mn oxide nano array.
Example 5 photothermal treatment of Sulfur doped Co/Mn oxide nanoarrays
1) Immersing a 2.5cm multiplied by 1cm foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, washing the foam nickel substrate with water and ethanol respectively, and drying in a blast drying oven;
2) 3mmol of ammonium fluoride, 2mmol of manganese nitrate, 6mmol of urea and 2mmol of cobalt nitrate are dissolved in 30mL of deionized water to prepare a reaction solution, clean foam nickel and the prepared solution are put into a reaction kettle, and water is added for hydrothermal reaction for 2 hours at 120 ℃. After the hydrothermal treatment, drying the cleaned sample for 2 hours at 60 ℃ to obtain a precursor of the CoMnO nano array;
3) And 2) respectively placing the CoMnO precursor obtained in the step 2) and 600mg of sublimed sulfur in two transparent crucibles, placing the two crucibles in the center of a quartz tube, placing a high-pressure mercury lamp right above a sample, performing photo-thermal treatment under the condition of low flow rate of argon, heating to 350 ℃ at the speed of 10 ℃/min, preserving heat for 3 hours, naturally cooling to room temperature, and taking out to obtain the sulfur-doped Co/Mn oxide nano array.
Comparative example 1 comparison of tube furnace annealing and photothermal treatment: XPS spectrum analysis, performance comparison
The annealing scheme of the tube furnace is as follows:
1) Immersing a 2.5cm multiplied by 1cm foam nickel substrate into dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, washing the foam nickel substrate with water and ethanol respectively, and drying in a blast drying oven;
2) 3mmol of ammonium fluoride, 2mmol of manganese nitrate, 6mmol of urea, 2mmol of cobalt nitrate and 30mL of deionized water are taken to prepare a solution, clean foam nickel and the prepared solution are put into a reaction kettle, and water is added to heat for 2 hours at 120 ℃. After the hydrothermal treatment, the washed sample was dried at 60℃for 2 hours. Obtaining a precursor of the CoMnO nano array;
3) And (3) putting the obtained CoMnO precursor into the middle of a quartz tube of a tube furnace, annealing in an argon atmosphere, heating to 350 ℃ at a speed of 5 ℃/min, preserving heat for 120min, and cooling to room temperature to obtain the foam nickel-loaded CoMnO nano array.
Compared with example 1, the two main peaks of Co2p of tubular furnace annealed CoMnO and UV photo-heat treated CoMnO were 796.93eV,780.83eV and 7, respectively96.4eV,780.52eV, and the transfer of the Co2p binding energy of the CoMnO to the lower binding energy by UV photo-thermal treatment indicate that the barrier for extracting electrons from Co ions is small, and the effective oxidation-reduction reaction of Co species occurs. Fitting of the spectra showed Co 2+ And Co 3+ Co-existence and by fitting Co 2+ And Co 3+ XPS peak area of (C) to obtain Co in photothermal treatment CoMnO 2+ With Co 3+ The ratio is 1.86, which is far smaller than that of tube furnace annealing treatment (Co 2+ /Co 3+ ＝2.28)，Co 3+ The increase in (2) facilitates hydroxide adsorption, thereby increasing energy storage capacity.
Compared with example 1, the UV photo-thermal treatment of CoMnO was carried out at 1mA/cm 2 The mass specific capacitance of 1940F/g is far greater than 1376F/g of the tube furnace annealing treatment, which shows that the UV light treatment successfully prepares the high-performance CoMnO electrode material.
Comparative example 2 comparison of pure light with light nitrogen doping: XPS spectrum analysis, performance comparison
Comparing example 1 (pure light) with example 5 (light nitrogen doping), example 5 shows less pronounced characteristic peaks of nitrogen in the full spectrum after photo-thermal nitrogen doping compared to example 1. The N1s profile consisted of two characteristic peaks of pyridine nitrogen (398.5 eV) and pyrrole nitrogen (399.8 eV). Wherein, the pyridine nitrogen accounts for 42 percent and the pyrrole nitrogen accounts for 58 percent. The binding energy of Co2p after nitrogen doping was transferred to lower binding energy of 796.3eV (Co 2p 1/2 ) And 780.27eV (Co 2 p) 3/2 ) This is due to the charge transfer effect caused by the adsorption of foreign nitrogen atoms in the gap. At the same time by fitting Co 2+ And Co 3+ XPS peak area of (C) is obtained after photo-thermal nitrogen doping 2+ With Co 3+ The ratio was 1.41, and the far smaller Yu Chunguang irradiation treatment (Co 2+ /Co 3+ =1.86). It was demonstrated that nitrogen adsorption was successfully completed on the CoMnO nanowire array after photo-thermal treatment.
Example 5 compared to example 1, the light and heat nitrogen doping was followed by a time of 1mA/cm 2 The mass specific capacitance of 2534F/g is far greater than 1940F/g of pure light treatment, which shows that the method successfully carries out nitrogen doping when the precursor is subjected to photo-thermal treatment, and the electrochemical performance of the mixed metal oxide material is improved.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (8)
1. A method for preparing a metal oxide electrode material by using UV photo-thermal assistance, which is characterized by comprising the following steps:
(1) Immersing the foam nickel substrate into 0.1M dilute hydrochloric acid, ultrasonically removing impurities and oxide layers on the surface, then washing the foam nickel substrate with water and ethanol respectively, and then drying in a blast drying oven at 60 ℃;
(2) Mixing ammonium fluoride, manganese nitrate, urea and cobalt nitrate, dissolving in water to form a reaction solution, putting the dried foam nickel substrate into a reaction kettle containing the reaction solution, performing hydrothermal treatment, and then cleaning and drying the reacted product to obtain a precursor of the CoMnO nano array;
(3) And (3) placing the precursor of the CoMnO nano array in the center of a quartz tube, placing a high-pressure mercury vapor lamp right above the precursor of the CoMnO nano array, carrying out photo-thermal treatment under the condition of protective gas, then preserving heat, and naturally cooling to room temperature to obtain the UV photo-thermal treatment Co/Mn oxide material.
2. The method for preparing a metal oxide electrode material with the aid of UV light and heat according to claim 1, wherein the specification of the foam nickel substrate in the step (1) is 2.5cm×1cm.
3. The method for preparing a metal oxide electrode material with the aid of UV light and heat according to claim 1, wherein the concentration of the dilute hydrochloric acid in the step (1) is 0.1M
The ultrasonic power is 180W, and the ultrasonic time is 10min.
4. The method for preparing a metal oxide electrode material with the aid of UV light and heat according to claim 1, wherein in the step (2), the concentration of ammonium fluoride in the reaction solution is 0.1mmol/ml, the concentration of manganese nitrate is 0.067mmol/ml, the concentration of urea is 0.2mmol/ml, and the concentration of cobalt nitrate is 0.067mmol/ml.
5. The method for preparing a metal oxide electrode material by using UV photo-thermal assistance according to claim 1, wherein the hydrothermal reaction temperature in the step (2) is 120 ℃ and the reaction time is 2-8h;
the drying temperature is 60 ℃, and the drying time is 2-5h.
6. A method for the photo-thermal assisted production of metal oxide electrode materials according to claim 1, characterized in that the high-pressure mercury vapor lamp power used in the photo-thermal treatment in step (3) is 2KW.
7. The method for preparing a metal oxide electrode material with the aid of UV light and heat according to claim 6, wherein the photo-thermal treatment method in the step (3) is as follows: the precursor of the CoMnO nano array is heated to 350 ℃ from room temperature at the speed of 10 ℃/min under the irradiation of light, and then the temperature is kept for 2-5h.
8. The method for preparing a metal oxide electrode material with the aid of UV light and heat according to claim 1, wherein the shielding gas in the step (3) is one of argon, nitrogen and helium.
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| CN116651402A (en) * | 2023-07-07 | 2023-08-29 | 中国矿业大学 | Integral CO 2 Adsorbent and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116651402A (en) * | 2023-07-07 | 2023-08-29 | 中国矿业大学 | Integral CO 2 Adsorbent and preparation method and application thereof |
| CN116651402B (en) * | 2023-07-07 | 2024-04-05 | 中国矿业大学 | Integral CO 2 Adsorbent and preparation method and application thereof |
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