CN114481188A - Preparation method of surface nitrogen-doped electrode - Google Patents
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- CN114481188A CN114481188A CN202210114158.6A CN202210114158A CN114481188A CN 114481188 A CN114481188 A CN 114481188A CN 202210114158 A CN202210114158 A CN 202210114158A CN 114481188 A CN114481188 A CN 114481188A
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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Abstract
The invention relates to a preparation method of a surface nitrogen-doped electrode, belonging to the technical field of electrode materials. The preparation method comprises the steps of sequentially ultrasonically cleaning foamed iron-nickel in acetone, absolute ethyl alcohol and deionized water, and then drying; and placing the cleaned and dried foam iron nickel in a tubular furnace, and performing surface nitrogen treatment in a nitrogen atmosphere to obtain the surface nitrogen-doped electrode. The preparation method is simple, the used raw materials are rich in yield and low in price, and the prepared electrode exposes rich active sites, has the characteristics of high catalytic activity and high structural stability, and meets the requirements of large-scale industrial production and application.
Description
Technical Field
The invention relates to a preparation method of a surface nitrogen-doped electrode, in particular to a preparation method of a surface nitrogen-doped oxygen evolution reaction electrode, and belongs to the technical field of electrode materials.
Background
In recent years, with the progress of human civilization, the consumption of fossil fuels is increasing day by day and the environmental pollution is increasing day by day, and the development of a novel sustainable energy source with abundant reserves and green is urgently needed. Hydrogen energy is considered as an efficient, pollution-free secondary energy source as the best alternative to fossil fuels. The industrial large-scale and cheap hydrogen production is the first link for developing and utilizing hydrogen energy. Among various hydrogen production technologies, the high-efficiency water electrolysis hydrogen production becomes the key point of research in the current scientific field and also becomes the core technology of the hydrogen production industry in the future.
Electrocatalytic cracking water consists of two half-reactions, the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER). Since the OER process involves multi-electron, multi-proton conversion, the reaction kinetics are rather slow. In order to accelerate this complex process, the development of efficient, stable OER electrocatalysts is highly desirable. It is well known that oxides of iridium and ruthenium have high catalytic activity for OER, but these noble metal-based catalysts have significant disadvantages in practical applications, including low earth abundance, high cost, and poor catalytic stability. Most of the non-noble metal-based catalysts reported in the literature at present are in a powder state, so that the catalyst has to be adhered to a conductive substrate by using a polymer binder such as Nafion and the like to assemble an electrode material, and thus the contact area of the electrolyte and a catalytic active site is reduced, and the electrocatalytic activity and stability are reduced. In addition, the preparation of most catalysts requires high temperature, high pressure or long time for multi-step process, and even high purity hydrogen consumption, resulting in large time and energy consumption, and thus large-scale application is not economical and practical.
Chinese patent publication CN111013635A describes a substrate-supported nitrogen-doped carbon nanotube-surrounded molybdenum carbide particle composite material, and a preparation method and application thereof. In the patent publication, nitrogen-doped carbon nanotubes surround molybdenum carbide particles and are coated on the surface of a substrate; the composite material is prepared by uniformly coating a molybdenum oxide precursor on a substrate by adopting a hydrothermal synthesis method, then carrying out high-temperature annealing on the molybdenum oxide precursor in a roasting furnace under an inert atmosphere, and introducing a nitrogenous organic matter into the roasting furnace in the high-temperature annealing process to carry out high-temperature pyrolysis reaction. According to the technical scheme, the substrate-loaded nitrogen-doped carbon nanotube surrounding molybdenum carbide particle composite material is obtained by coating a molybdenum oxide precursor on a substrate, introducing a nitrogen-containing organic matter into the molybdenum oxide precursor in a high-temperature annealing process under an inert atmosphere for high-temperature pyrolysis reaction, the substrate material is complex, the nitrogen-containing organic matter is acetonitrile or pyridine, the toxicity is high, the process requirement is strict, the reaction temperature of high-temperature pyrolysis is 650-750 ℃, and the preparation cost is high.
Therefore, based on the development requirement of oxygen evolution reaction such as industrial electrolyzed water on the electrode technology, the preparation method which is simple and easy to operate and low in cost is developed, and the application potential is huge.
Disclosure of Invention
The invention aims to provide a preparation method of a surface nitrogen-doped electrode.
The invention also aims to provide the application of the surface nitrogen-doped electrode as an oxygen evolution reaction electrode in the aspects of water electrolysis and the like.
The electrode body is made of foam iron-nickel metal material.
The preparation method comprises the following steps: respectively putting foamed iron nickel in acetone, absolute ethyl alcohol and deionized water, sequentially ultrasonically cleaning, and then drying; and carrying out surface nitrogen treatment on the cleaned and dried foam iron nickel in a nitrogen atmosphere to obtain the surface nitrogen-doped electrode.
Specifically, in the preparation method, the surface nitrogen treatment is as follows: placing urea and cleaned and dried foam iron-nickel in a container, and then placing the container in a tubular furnace; after protective gas is introduced to exhaust air, the temperature is raised to 200 and 600 ℃, and the temperature is kept for 1 to 3 hours; and naturally cooling under the atmosphere of protective gas to obtain the surface nitrogen-doped electrode.
The ratio of the surface area of the foam iron-nickel material to the dosage of the urea is (2-4) cm2V (0.5-3) g; the preferable dosage ratio is (2-4) cm2/0.5g。
The protective gas is nitrogen or hydrogen; the air removal time was 2 hours. The protective gas is preferably nitrogen.
In the preparation method, the temperature rise speed is preferably 5 ℃ per minute;
the preparation method preferably raises the temperature to 200 ℃ and maintains the temperature for 2 hours.
In the preparation method, the ultrasonic cleaning time of the foam iron-nickel electrode body in acetone, absolute ethyl alcohol and deionized water is preferably 20-30 min.
The ultrasonic power of the ultrasonic cleaning is preferably 40W.
The drying treatment in the preparation method is preferably vacuum drying.
The preparation method disclosed by the patent has the advantages of simple process and low cost, and the prepared nitrogen-doped foamed iron-nickel electrode material can be used as a self-supporting electrode, and compared with a powdery non-noble metal-based catalyst reported in the current literature, the electrode material is obtained by assembling the catalyst on a conductive substrate without using a binder, so that the catalytic activity and the stability are influenced. And with other self-supporting type electrodes, hydrothermal conditions and complex steps required in synthesis are not required, a precursor is not required, and when the electrode is used as an OER electrode, rapid desorption of gas can be ensured, and mass transfer of reaction is facilitated.
The catalyst nitrogen doping normally carried out in the prior art requires the toxic gas NH3Treating the sample at high temperature for a long time, or requiring NH3Or N2This places high demands on the equipment.
The method can prepare the novel OER catalytic electrode with color rendering property, and overcomes the defects of complicated preparation process, expensive equipment and unsuitability for large-scale application in the existing preparation methods of some non-noble metal-based catalysts such as transition metal nitrides and the like.
The preparation method of the surface nitrogen-doped foam iron-nickel electrode has the advantages of simple preparation process and low cost, and the electrode material prepared by the method has excellent oxygen evolution catalytic performance. Especially, the material has good application prospect in the aspect of high-efficiency electrocatalysis water.
The method utilizes commercial foam iron-nickel as a three-dimensional conductive support body and adopts a low-temperature treatment method to prepare the foam iron-nickel electrode with nitrogen doped on the surface. The electrode prepared by the invention has excellent oxygen evolution catalysis function, and has the characteristics of low price, high efficiency and low cost due to the use of non-noble metal. The preparation method is simple, the used raw materials are rich in yield and low in price, and the prepared electrode exposes rich active sites, has the characteristics of high catalytic activity and high structural stability, and meets the requirements of large-scale industrial production and application.
Drawings
FIG. 1 is a graph showing the relationship between the amount of urea used and the performance of an electrode.
FIG. 2 is a graph of process temperature versus electrode performance.
Fig. 3 is a graph showing the relationship between the protective gas and the performance of the electrode.
FIG. 4 is a photograph of a glass instrument used in the experiment.
Fig. 5 is an SEM image of the surface of the electrode prepared in example 1.
FIG. 6 is an EDS map of the iron element on the surface of the electrode prepared in example 1.
FIG. 7 is an EDS map of nitrogen element on the surface of the electrode prepared in example 1.
FIG. 8 is an EDS diagram of nickel elements on the surface of the electrode prepared in example 1.
Fig. 9 is an XRD pattern of the electrode prepared in example 1.
Detailed Description
Example 1
Cleaning of the substrate:
sequentially ultrasonically cleaning a foamed iron-nickel metal sheet in acetone, absolute ethyl alcohol and deionized water for 30min with ultrasonic power of 40W, ultrasonically treating to remove impurities on the surface of the foamed iron-nickel, and then drying the cleaned foamed iron-nickel in vacuum for subsequent use;
surface nitrogen doping treatment:
0.5g of urea was added to the lower end of the glass apparatus, a clean piece of foam iron nickel metal (1cm x 2cm) was placed in the crucible, on top of the glass apparatus (see fig. 4), and the whole glass apparatus was placed in a tube furnace. Nitrogen was first introduced to remove air for 2 hours. Thereafter, the tube furnace was heated to 200 ℃ under a nitrogen atmosphere at a heating rate of 5 ℃ per minute and held for 2 hours. And naturally cooling the tubular furnace to room temperature in a nitrogen atmosphere to obtain the foamed iron-nickel electrode subjected to surface nitrogen doping treatment.
The prepared electrode is subjected to test characterization of scanning electron microscope SEM, energy spectrum EDS and XRD, and the result is shown in the figure:
FIG. 5 is an SEM image of the electrode surface. It can be seen from the SEM images that the material still maintains a smooth surface characteristic after the nitrogen doping treatment.
FIG. 6 is EDS diagram of iron element on the surface of electrode.
FIG. 7 is an EDS diagram of nitrogen on the surface of an electrode.
FIG. 8 is EDS diagram of nickel element on the surface of electrode.
It can be seen from FIGS. 6-8 that the nitrogen element is uniformly distributed in the sample.
Figure 9 is an electrode XRD pattern. As can be seen from fig. 9, after the nitrogen doping treatment, all diffraction peaks still corresponded to the standard cards of the foam iron-nickel substrate, and no new diffraction peaks appeared, indicating that no new products appeared, and the surface doping was achieved by this treatment.
Example 2
In the embodiment, variable regulation is performed by the addition amount of urea, the time length and the temperature for surface nitrogen doping treatment, and the optimal experimental conditions are selected according to the final performance of the obtained foam iron-nickel electrode.
Referring to the preparation process of example 1, the foam iron nickel is treated by 0.5g, 1g and 3g of urea respectively, and under the condition that other conditions are not changed, the foam iron nickel electrode plate with nitrogen doped on the surface is prepared, and the relation between the electrode plate and the urea amount is researched. Since the amount of ammonia gas generated during the preparation process is proportional to the amount of urea, a suitable amount of urea can be selected, as can be seen in fig. 1, the sample treated with 0.5g of urea has a catalytic activity similar to that of the sample treated with 3g of urea, thus determining that an amount of 0.5g of urea is most suitable. The amount of ammonia gas generated by decomposition is in direct proportion to the amount of urea, and under the condition that other conditions are kept unchanged (the flow rate of protective gas is 50sccm, the air exhaust time is 1 hour, the temperature rise speed is 5 ℃/min, the treatment temperature is 200 ℃, the treatment time is 2 hours, and the size of a foam iron-nickel metal sheet is 1cm x 2cm), the foam iron-nickel is treated by 0.5-3g of urea respectively. As can be seen in FIG. 1, the samples treated with 0.5g of urea had catalytic activity similar to that of the 3g urea-treated samples, so we determined that the amount of 0.5g of urea was the most suitable to meet the nitrogen-doped nitrogen source provision while avoiding excessive nitrogen spill.
Example 3
The urea is decomposed to generate ammonia gas when being heated to 160 ℃, and under the condition that other conditions are kept unchanged (the protective gas is nitrogen, the nitrogen flow rate is 50sccm, the air exhaust time is 1 hour, the temperature rise speed is 5 ℃/min, the temperature is kept for 2 hours after the target temperature is reached, the urea dosage is 0.5g, and the size of a foam iron nickel metal sheet is 1cm × 2cm), the foam iron nickel is respectively treated at the temperature of 200 plus materials and 600 ℃, and the result is shown in figure 2. It can be seen that the sample obtained after treatment at 200 ℃ has the best OER catalytic activity, which can reach 100mA/cm at a low overpotential of 280mV2The current density of (1). Therefore, 200 ℃ is considered as the optimum temperature condition.
Example 4
Inert gas nitrogen and reducing gas hydrogen are respectively used as protective gases, the dosage of urea is 0.5g, and the size of the foam iron-nickel metal sheet is 1cm x 2 cm. A gas flow rate of 50sccm was maintained throughout the process. After the vent body exhausts air for one hour, the temperature is raised at the temperature rise speed of 5 ℃/min, and after the temperature is raised to 200 ℃, the temperature is kept for two hours, and the H can be obtained by naturally cooling2Nickel iron foam and N2-foam iron nickel. Through the catalytic activity test, see fig. 3, it can be determined that the introduction of nitrogen, which is an inert gas, is preferable to the introduction of hydrogen, which is a reducing gas.
Claims (10)
1. A preparation method of a surface nitrogen-doped electrode is characterized in that an electrode body is foamed iron nickel, and the method comprises the following steps: respectively putting foamed iron nickel in acetone, absolute ethyl alcohol and deionized water, sequentially carrying out ultrasonic cleaning, and then carrying out drying treatment; and carrying out surface nitrogen treatment on the cleaned and dried foam iron nickel in a nitrogen atmosphere to obtain the surface nitrogen-doped electrode.
2. The method of claim 1, wherein the surface nitrogen treatment is: placing urea and cleaned and dried foam iron-nickel in a container, and then placing the container in a tubular furnace; after protective gas is introduced to exhaust air, the temperature is raised to 200 and 600 ℃, and the temperature is kept for 1 to 3 hours; and naturally cooling under the atmosphere of protective gas to obtain the surface nitrogen-doped electrode.
3. The method of claim 2, wherein the ratio of the surface area of the foam iron-nickel material to the amount of urea is (2-4) cm2/(0.5-3)g。
4. The method according to claim 3, wherein the ratio of the surface area of the foamed iron-nickel material to the amount of urea is (2-4) cm2/0.5g。
5. The production method according to claim 2, wherein the protective gas is nitrogen or hydrogen; the air removal time was 2 hours.
6. The method according to claim 2, wherein the temperature is raised at a rate of 5 ℃ per minute to 200 ℃ for 2 hours.
7. The preparation method of claim 1, wherein the foamed iron-nickel electrode body is ultrasonically cleaned in acetone, absolute ethyl alcohol and deionized water for 20-30 min.
8. The method for preparing a ceramic material according to claim 7, wherein the ultrasonic power of the ultrasonic cleaning is 40W.
9. The method according to claim 1, wherein the drying treatment is vacuum drying.
10. Use of the surface nitrogen-doped electrode prepared by the method of claims 1-9 as an oxygen evolution reaction electrode in water electrolysis and the like.
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CN115196681A (en) * | 2022-08-15 | 2022-10-18 | 南京理工大学 | N-doped molybdenum trioxide and preparation method thereof |
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