CN114481188B - Preparation method of surface nitrogen-doped electrode - Google Patents

Preparation method of surface nitrogen-doped electrode Download PDF

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CN114481188B
CN114481188B CN202210114158.6A CN202210114158A CN114481188B CN 114481188 B CN114481188 B CN 114481188B CN 202210114158 A CN202210114158 A CN 202210114158A CN 114481188 B CN114481188 B CN 114481188B
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nickel
foam iron
nitrogen
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CN114481188A (en
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焦世惠
王勃然
庞广生
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Jilin University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
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    • 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, and belongs to the technical field of electrode materials. The preparation method comprises the steps of respectively carrying out ultrasonic cleaning on foam iron and nickel in acetone, absolute ethyl alcohol and deionized water in sequence, and then carrying out drying treatment; and placing the foam iron-nickel after cleaning and drying in a tube furnace, and carrying out 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, the prepared electrode exposes rich active sites, and the electrode has the characteristics of high catalytic activity and high structural stability, and meets the requirements of large-scale industrial production and application.

Description

Preparation method of surface nitrogen-doped electrode
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 and the environmental pollution is increasing, and we have urgent need to develop a sustainable new energy source with abundant reserves and green. Hydrogen energy is regarded as the best alternative to fossil fuels as a highly efficient, pollution-free secondary energy source. The industrialized large-scale and low-cost production of hydrogen is the first link for developing and utilizing hydrogen energy. Among various hydrogen production technologies, high-efficiency water electrolysis hydrogen production has become an important point of research in the current scientific field and also will become a core technology of the future hydrogen production industry.
The electrocatalytic cleavage water consists of two half reactions, hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER). The OER process involves the conversion of multiple electrons, multiple protons, and is therefore quite slow in reaction kinetics. In order to accelerate this complex process, there is an urgent need to develop efficient, stable OER electrocatalysts. It is well known that oxides of iridium and ruthenium have high catalytic activity towards OER, but these noble metal-based catalysts have significant drawbacks in practical applications, including low earth abundance, high cost and poor catalytic stability. Most of the non-noble metal-based catalysts reported in the current literature are in powder form, which makes it necessary to use polymer binders such as Nafion to adhere the catalyst to a conductive substrate and assemble the electrode material, which reduces the contact area between the electrolyte and the catalytically active site, resulting in reduced electrocatalytic activity and stability. In addition, the preparation of most catalysts requires high temperature, high pressure or long time for multi-step process, and even high purity hydrogen is consumed, resulting in a lot of time and energy consumption, so that large-scale application is not economical and practical.
Chinese patent publication No. CN111013635A describes a substrate-supported nitrogen-doped carbon nanotube-surrounding 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 inert atmosphere, and introducing nitrogen-containing organic matters into the roasting furnace in the high-temperature annealing process to carry out high-temperature pyrolysis reaction. According to the technical scheme, the substrate-supported 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 in a high-temperature annealing process of the molybdenum oxide precursor in an inert atmosphere, and carrying out a high-temperature pyrolysis reaction, wherein the nitrogen-containing organic matter is acetonitrile or pyridine, has high toxicity and strict process requirements, and the high-temperature pyrolysis reaction temperature is 650-750 ℃ and the preparation cost is high.
Therefore, based on the development needs of the oxygen evolution reaction such as industrial electrolyzed water and the like on the electrode technology, the preparation method with simple and easy operation and low 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 water electrolysis and the like.
The electrode body is made of foam iron-nickel metal material.
The preparation method comprises the following steps: respectively ultrasonically cleaning foam iron nickel in acetone, absolute ethyl alcohol and deionized water in sequence, and then drying; and (3) carrying out surface nitrogen treatment on the foam iron-nickel after cleaning and drying 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 foam iron-nickel after cleaning and drying in a container, and then placing in a tube furnace; after the protective gas is introduced and the air is exhausted, the temperature is raised to 200-600 ℃ and kept for 1-3 hours; and naturally cooling in a protective gas atmosphere to obtain the surface nitrogen doped electrode.
The ratio of the surface area of the foam iron-nickel material to the dosage of urea is (2-4) cm 2 (0.5-3) g; the preferable dosage ratio is (2-4) cm 2 /0.5g。
The protective gas is nitrogen or hydrogen; the air removal time was 2 hours. The shielding gas is preferably nitrogen.
In the preparation method, the temperature rising speed is preferably 5 ℃ per minute;
the preparation method is preferably to raise the temperature to 200 ℃ and keep for 2 hours.
In the preparation method, 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 has simple process and low cost, and the prepared nitrogen-doped foam iron-nickel electrode material can be used as a self-supporting electrode, and compared with the powdered non-noble metal-based catalyst reported in the current literature, the preparation method does not need to use a binder to adhere the catalyst to a conductive substrate to assemble the electrode material, thereby influencing the catalytic activity and stability. And the self-supporting electrode is used as an OER electrode, so that the rapid desorption of gas can be ensured, and the mass transfer of the reaction is facilitated.
The prior art generally requires toxic gas NH for catalyst nitrogen doping 3 Treating the sample at elevated temperature for prolonged periods of time, or requiring NH 3 Or N 2 This places high demands on the equipment.
The method can prepare the novel OER catalytic electrode with excellent performance, and overcomes the defects that the preparation process is complicated, the use equipment is expensive and the method is not suitable for large-scale application in the existing preparation methods of non-noble metal-based catalysts such as transition metal nitrides.
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 electrocatalytic water.
The patent uses commercial foam iron-nickel as a three-dimensional conductive support body, adopts a low-temperature treatment method, and prepares the foam iron-nickel electrode doped with surface nitrogen. The electrode prepared by the invention has excellent oxygen evolution catalysis function, and has the characteristics of low cost, high efficiency, and low cost due to the use of non-noble metals. The preparation method is simple, the used raw materials are rich in yield and low in price, the prepared electrode exposes rich active sites, and the electrode 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 urea amount and electrode performance.
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 electrode performance.
FIG. 4 is a photograph of a glassware 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 diagram of the iron element on the surface of the electrode prepared in example 1.
Fig. 7 is an EDS diagram of nitrogen element on the surface of the electrode prepared in example 1.
Fig. 8 is an EDS diagram of the nickel element 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 a substrate:
respectively ultrasonically cleaning foam iron-nickel metal sheets in acetone, absolute ethyl alcohol and deionized water for 30min in sequence, ultrasonically treating and washing out impurities on the surface of the foam iron-nickel, and then vacuum drying the cleaned foam iron-nickel for subsequent use;
surface nitrogen doping treatment:
0.5g of urea was added to the lower end of the glass apparatus, a clean foam iron nickel metal sheet (1 cm x 2 cm) was placed in a crucible, placed on the upper end of the glass apparatus (see fig. 4), and the entire glass apparatus was placed in a tube furnace. Nitrogen is firstly introduced to remove air for 2 hours. Thereafter, the tube furnace was warmed to 200℃under a nitrogen atmosphere at a warming rate of 5℃per minute and maintained for 2 hours. And naturally cooling the tube furnace to room temperature in a nitrogen atmosphere to obtain the foam iron-nickel electrode with the surface subjected to nitrogen doping treatment.
And carrying out test characterization of Scanning Electron Microscope (SEM), energy spectrum EDS and XRD on the prepared electrode, wherein the result is shown in the figure:
fig. 5 is an SEM image of the electrode surface. From the SEM image it can be seen that the material still maintains a flat and smooth surface profile after the nitrogen doping treatment.
Fig. 6 is an EDS diagram of the elemental iron on the surface of the electrode.
Fig. 7 is an EDS diagram of the nitrogen element at the electrode surface.
Fig. 8 is an EDS diagram of the nickel element on the electrode surface.
From fig. 6-8 it can be seen that the nitrogen element is uniformly distributed in the sample.
Fig. 9 is an electrode XRD pattern. As can be seen from fig. 9, after the nitrogen doping treatment, all diffraction peaks still correspond to standard cards of the foam iron-nickel substrate, no new diffraction peaks appear, indicating no new products appear, and the treatment process achieves surface doping.
Example 2
According to the embodiment, variable regulation and control are carried out on the addition amount of urea, the duration and the temperature of 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, 0.5g, 1g and 3g of urea are respectively used for treating foam iron and nickel, under the condition that other conditions are kept unchanged, foam iron and nickel electrode plates doped with surface nitrogen are prepared, and the relation between the electrode plates and urea amount is studied. Since the amount of ammonia produced during the preparation is proportional to the amount of urea, the amount of urea used may be selected to be suitable, 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 the amount of urea of 0.5g is most suitable. The amount of ammonia gas generated by decomposition is proportional to the amount of urea, and under the condition that other conditions are kept unchanged (the protective gas is nitrogen, the flow rate of the nitrogen is 50sccm, the evacuation time is 1 hour, the heating rate is 5 ℃/min, the treatment temperature is 200 ℃, the treatment time is 2 hours, and the size of the foam iron-nickel metal sheet is 1cm x 2 cm), 0.5-3g of urea is used for treating the foam iron-nickel respectively. As can be seen in fig. 1, the samples treated with 0.5g urea had similar catalytic activity to the samples treated with 3g urea, so we determined that the 0.5g urea was most suitable, both to meet the nitrogen source supply of nitrogen doping and to avoid excessive nitrogen overflow.
Example 3
Urea is decomposed to generate ammonia gas when heated to 160 ℃, under the condition that other conditions are kept unchanged (the flow rate of the protective gas is nitrogen, the flow rate of the nitrogen is 50sccm, the evacuation time is 1 hour, the heating rate is 5 ℃/min, the urea is kept for 2 hours after reaching the target temperature, the urea dosage is 0.5g, and the size of a foam iron nickel metal sheet is 1cm x 2 cm), and the foam iron nickel is treated at 200-600 ℃ respectively, and the result is shown in figure 2. It can be seen that the samples obtained after 200℃treatment have an optimal OER catalytic activity, which can reach 100mA/cm at a low overpotential of 280mV 2 Is used for the current density of the battery.200℃is therefore considered to be the optimal 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 sizes of foam iron nickel metal sheets are 1cm x 2cm. The gas flow rate of 50sccm was maintained throughout the treatment. After the ventilation body discharges air for one hour, the temperature is raised at a speed of 5 ℃/min, and after the temperature reaches 200 ℃, the ventilation body is kept for two hours and naturally cooled, so that H can be obtained 2 Foam iron nickel and N 2 -foamed iron nickel. By catalytic activity testing, see fig. 3, it was determined that the introduction of inert gas nitrogen was better than the introduction of reducing gas hydrogen.

Claims (10)

1. The preparation method of the surface nitrogen doped electrode is characterized in that the electrode body is foam iron nickel, and the method comprises the following steps: respectively ultrasonically cleaning foam iron nickel in acetone, absolute ethyl alcohol and deionized water in sequence, and then drying; urea and foam iron-nickel after cleaning and drying are heated to 200-600 ℃ in a protective gas atmosphere to carry out surface nitrogen treatment, and then the surface nitrogen doped electrode is obtained; the protective gas is nitrogen or hydrogen.
2. The method of claim 1, wherein the surface nitrogen treatment is: placing urea and foam iron-nickel after cleaning and drying in a container, and then placing in a tube furnace; introducing protective gas to remove air, heating to 200-600deg.C, and maintaining for 1-3 hr; and naturally cooling in a protective gas atmosphere to obtain the surface nitrogen doped electrode.
3. The method according to claim 2, wherein the ratio of the surface area of the foam iron-nickel material to the amount of urea is (2-4) cm 2 /(0.5-3)g。
4. The method according to claim 3, wherein the ratio of the surface area of the foam iron-nickel material to the amount of urea is (2-4) cm 2 /0.5g。
5. The method of claim 2, wherein the air-out time is 2 hours.
6. The method according to claim 2, wherein the temperature rise rate is 5 ℃ per minute, and the temperature is raised to 200 ℃ and maintained for 2 hours.
7. The method according to claim 1, wherein the foam iron-nickel electrode body is ultrasonically cleaned in acetone, absolute ethyl alcohol and deionized water for 20-30 min, respectively.
8. The method of 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.
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CN105107540B (en) * 2015-09-06 2017-04-12 太原理工大学 Nitrogen-doped carbon nanotube nickel-iron coated oxygen evolution catalytic material for water electrolysis and application
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