CN114400336B - Nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst, and preparation method and application thereof - Google Patents
Nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst, and preparation method and application thereof Download PDFInfo
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst, and a preparation method and application thereof, wherein an iron source, a nitrogen source, a chlorine source, a carbon source and a nickel source are placed in an acetone container, heated and stirred to be viscous, evaporated and dried to obtain a dried object, and then calcined, wherein the mass part ratio of the iron source to the nickel source is (1-2): 1.5-2, wherein the mass part ratio of the nitrogen source to the carbon source is 2-3:1-2, wherein the total mass part ratio of the iron source to the nickel source and the mass part ratio of the iron source to the carbon source are 7-8.5:20-25, wherein the total mass parts of the chlorine source and the iron source and the mass parts of the chlorine source and the carbon source are 3-4:7-8, the carrier loaded chlorine-doped iron-nickel oxide with the electro-catalytic oxygen evolution catalyst being nitrogen-doped carbon is prepared by the technical scheme, the oxygen evolution reaction efficiency can be effectively improved, and the concentration of the carrier loaded chlorine-doped iron-nickel oxide is 10mA cm ‑2 The overpotential in a 1M KOH aqueous solution is 0.226V, and after long-time stability test, the stability is better, and the large-scale production is easy.
Description
Technical Field
The invention relates to the technical field of electrocatalysts, in particular to a nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst, and a preparation method and application thereof.
Background
Non-noble metal oxygen evolution reaction electrocatalysts have attracted extensive research attention and made great scientific progress in recent decades. It was found that the catalytic performance for water splitting reaction is greatly improved by the bimetallic catalyst which balances the components between the transition metals. It is worth noting that the oxygen evolution reaction can show better performance due to the synergistic effect between iron and nickel. This is because the presence of iron improves the catalytic capacity of nickel, which is inefficient in generating oxygen radicals at the active sites of the oxygen evolution reaction. The doping of the iron can change the electronic structure and coordination environment of an active site and improve the transfer rate of electrons by reducing a kinetic barrier, thereby promoting the formation of an active phase on the surface of the oxygen evolution reaction catalyst.
However, iron and nickel elements are very active in daily environment, and the iron-nickel-based electrocatalyst in a pure gold state has a strong corrosion effect and often cannot be directly and stably exerted in an acidic or alkaline electrolyte.
Although the morphology and electronic structure of iron and nickel are modified by oxidation or oxidation of iron and nickel with hydrogen, the long-term durability due to irreversible side reactions cannot meet the requirements of industrial practical applications. Therefore, the iron-nickel catalyst with high stability and high activity can be produced in large quantity, and has more practical significance for the electro-catalytic oxygen evolution catalyst.
Disclosure of Invention
The invention provides a nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst, and a preparation method and application thereof.
The invention is realized by the following technical scheme:
a preparation method of a nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst comprises the steps of placing an iron source, a nitrogen source, a chlorine source, a carbon source and a nickel source in a container of acetone, heating and stirring the mixture to be viscous, evaporating and drying the mixture to obtain a dried object, and then calcining the dried object, wherein the mass part ratio of the iron source to the nickel source is (1-2): 1.5-2, wherein the mass part ratio of the nitrogen source to the carbon source is 2-3:1-2, the total mass portion of the iron source and the nickel source and the mass portion ratio of the iron source to the carbon source are 7-8.5:20-25, wherein the total mass parts of the chlorine source and the iron source and the mass parts of the chlorine source and the carbon source are 3-4:7-8.
Optionally, the mass part ratio of the iron source to the nickel source is 1:1.5, wherein the mass part ratio of the nitrogen source to the carbon source is 2:1, the total mass part ratio of the iron source to the nickel source and the mass part ratio of the iron source to the carbon source are 7:20, the total mass parts of the chlorine source and the iron source and the mass parts of the chlorine source and the carbon source are 3:7.
optionally, the nitrogen source and the chlorine source are both hydroxylamine hydrochloride, the carbon source is at least one of carbon black, carbon nanotubes and graphene, the iron source is at least one of ferric acetylacetonate, ferric oxalate and ferric chloride hydrate, and the nickel source is at least one of nickel acetylacetonate, nickel chloride and nickel nitrate.
Optionally, the iron source, the nitrogen source, the chlorine source, the carbon source and the nickel source are placed in a container of acetone, heated and stirred at 70-80 ℃ to be viscous.
Optionally, heating and stirring at 70-80 deg.C to viscous state, evaporating and drying, specifically, evaporating and drying at 60-100 deg.C to obtain dried object.
Alternatively, the calcining treatment operation steps are as follows: the dried object obtained by evaporation and drying is heated to 450 ℃ under the action of protective gas, and is pyrolyzed for 1-5h at 450 ℃.
Optionally, the dried material is heated to 450 deg.C under the action of shielding gas at a heating rate of 1-10 deg.C for min -1 。
Optionally, the shielding gas is a mixture of at least one of nitrogen, helium, neon, argon, krypton, and xenon.
The technical scheme also provides an application of the oxygen evolution catalyst in an alkaline medium, namely the prepared electro-catalytic oxygen evolution catalyst is applied to the technical field of alkaline media.
The technical scheme also provides a nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst, wherein a nitrogen-doped carbon carrier is loaded with nitrogen-doped iron-nickel oxide, and the nitrogen-doped carbon carrier is formed by compounding nitrogen and carbon.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the prepared electro-catalytic oxygen evolution catalyst is a nitrogen-doped carbon carrier loaded chlorine-doped iron-nickel oxide, and can effectively improve the oxygen evolution reaction efficiency.
2. The preparation method in the technical scheme is mainly obtained by mixing a nitrogen source, a nickel source, an iron source, a chlorine source and a carbon source, and then carrying out heating stirring, evaporation drying and calcination treatment, and has strong overall operability and easy repeated operation.
3. The oxygen evolution catalyst prepared by the technical scheme is at 10mA cm -2 The overpotential in a 1M KOH aqueous solution is 0.226V, and after long-time stability test, the stability is better, and the large-scale production is easy.
Drawings
FIG. 1 is an X-ray diffraction pattern of the electrocatalytic oxygen evolution catalyst FeNi-Cl/NC obtained in example 1;
FIG. 2 is an X-ray photoelectron spectrum of the electrocatalytic oxygen evolution catalyst FeNi-Cl/NC obtained in example 1;
FIG. 3 is a graph showing the performance of the electrocatalytic oxygen evolution reaction of the electrocatalytic oxygen evolution catalyst FeNi-Cl/NC obtained in example 1 and commercially available iridium oxide;
FIG. 4 is a graph showing the electrocatalytic stability test performance of the electrocatalytic oxygen evolution catalyst FeNi-Cl/NC obtained in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1:
a preparation method of a nitrogen-doped loaded chlorine-doped iron-nickel oxide electrocatalytic oxygen evolution catalyst comprises the steps of weighing 0.29g of nickel acetylacetonate and 0.26g of iron acetylacetonate into a 20mL beaker, weighing 1.50g of hydroxylamine hydrochloride medicine into the beaker, weighing 30mL of acetone and 30mL of absolute ethyl alcohol into the beaker, and putting a mixed solution into an ultrasonic machine for mixing and ultrasonic treatment for 30min to obtain a deep red transparent solution.
The solution was transferred to a 80ml centrifuge tube and placed in an oil bath and heated to 70 ℃ with stirring, then 0.13g of carbon black was weighed in an analytical balance and added to the sonicated dark red clear solution until dry.
And then putting the sample into a blast drying oven, setting the temperature to be 60 ℃ for overnight drying the residual acetone and absolute ethyl alcohol, grinding the solid sample obtained after thorough drying into powder, and putting the powder into a porcelain boat.
And cleaning and drying the tubular quartz tube by using deionized water and alcohol, placing the tube furnace on which the porcelain boat filled with the sample is placed in the center of the quartz tube. After the air inlet flange and the air outlet flange are connected, the quartz tube is vacuumized, then high-purity argon is introduced to the normal pressure, after the step is repeated for three times, all argon in the quartz tube is ensured to be argon at the temperature of 10 ℃ for min -1 The temperature is raised to 450 ℃ at the temperature raising speed,keeping the constant temperature for 1h, and naturally cooling to room temperature. And finally, grinding the black solid obtained by calcination into powder by using an agate mortar to obtain a FeNi-Cl/NC catalyst sample.
Example 2:
a preparation method of a nitrogen-doped loaded chlorine-doped iron-nickel oxide electrocatalytic oxygen evolution catalyst comprises the steps of weighing 0.28g of nickel acetylacetonate and 0.25g of iron acetylacetonate into a 20mL beaker, weighing 1.4g of hydroxylamine hydrochloride medicine into the beaker, weighing 30mL of acetone and 30mL of absolute ethyl alcohol into the beaker, and putting a mixed solution into an ultrasonic machine for mixing and ultrasonic treatment for 30min to obtain a deep red transparent solution.
The solution was transferred to a 80ml centrifuge tube and placed in an oil bath and heated to 75 ℃ with stirring, then 0.12g of carbon black was weighed in an analytical balance and added to the dark red transparent solution after sonication until dry.
And then putting the mixture into a forced air drying oven, setting the temperature to 80 ℃ for overnight drying the residual acetone and absolute ethyl alcohol, grinding the solid sample obtained after complete drying into powder, and putting the powder into a porcelain boat.
And cleaning and drying the tubular quartz tube by using deionized water and alcohol, placing the tube furnace on which the porcelain boat filled with the sample is placed in the center of the quartz tube. After the gas inlet flange and the gas outlet flange are connected, the quartz tube is vacuumized, then high-purity argon is introduced to the normal pressure, the step is repeated for three times, all argon is ensured to be in the quartz tube, and the temperature is controlled to be 4 ℃ for min -1 The heating temperature is raised to 450 ℃ at a speed, the temperature is kept constant for 4 hours, and then the mixture is naturally cooled to room temperature. And finally, grinding the black solid obtained by calcination into powder by using an agate mortar to obtain a FeNi-Cl/NC catalyst sample.
Example 3:
a preparation method of a nitrogen-doped loaded chlorine-doped iron-nickel oxide electrocatalytic oxygen evolution catalyst comprises the steps of weighing 0.30g of nickel acetylacetonate and 0.27g of iron acetylacetonate into a 20mL beaker, weighing 1.7g of hydroxylamine hydrochloride medicine into the beaker, weighing 30mL of acetone and 30mL of absolute ethyl alcohol into the beaker, and putting a mixed solution into an ultrasonic machine for mixing and ultrasonic treatment for 30min to obtain a deep red transparent solution.
The solution was transferred to a 80ml centrifuge tube and placed in an oil bath and heated to 80 ℃ with stirring, then 0.15g of carbon black was weighed in an analytical balance and added to the sonicated dark red clear solution until dry.
And then putting the mixture into a forced air drying oven, setting the temperature to be 100 ℃ and drying the residual acetone and absolute ethyl alcohol overnight, grinding the solid sample obtained after complete drying into powder, and putting the powder into a porcelain boat.
And cleaning and drying the tubular quartz tube by using deionized water and alcohol, placing the quartz tube on a tubular furnace, and placing the ceramic boat filled with the sample in the center of the quartz tube. After the air inlet flange and the air outlet flange are connected, vacuumizing the quartz tube, then introducing high-purity argon to normal pressure, repeating the step for three times, ensuring that all argon is in the quartz tube at the temperature of 1 ℃ for min -1 The temperature is raised to 450 ℃ at the heating speed, kept at the constant temperature for 5 hours and then naturally cooled to the room temperature. And finally, grinding the black solid obtained by calcination into powder by using an agate mortar to obtain a FeNi-Cl/NC catalyst sample.
The oxygen evolution catalyst obtained in examples 1 to 3 is also called electrocatalytic oxygen evolution catalyst, and the protective gas introduced into the quartz tube in examples 1 to 3 may be at least one of nitrogen, helium, neon, krypton and xenon.
The electrocatalytic oxygen evolution catalyst prepared in the example 1 is subjected to oxygen evolution reaction performance test, the test method mainly adopts a three-electrode system, a working electrode is prepared by coating a prepared FeNi-Cl/NC catalyst sample on 1cm × 1cm of hydrophilic carbon paper in the form of ink and drying, a counter electrode is a carbon rod, a reference electrode is a mercury/mercury oxide electrode, an electrolyte is a 1M KOH aqueous solution, and the sweep speed of a polarization curve is 10mV/s.
The electro-catalytic oxygen evolution catalyst obtained by the preparation is shown in figure 1, and the phase diagram is an X-ray diffraction diagram, wherein a strong peak is obvious near an angle 35, and substances marked by the peak are iron oxide by analysis.
The valence diagram of the surface chemical elements of the prepared electrocatalytic oxygen evolution catalyst is shown in figure 2, and the existence of C, N, fe, ni, cl and O can be known from a diagram D, wherein a diagram A and a diagram B are respectively a Ni 2p and Fe 2p X ray photoelectron energy spectrogram, a diagram C is a Cl 2p X ray photoelectron energy spectrogram, and Ni is +2 through analysis; fe is +2 and +3 valence.
FIG. 3 is a graph showing the performance of the electrocatalytic oxygen evolution reaction of the electrocatalytic oxygen evolution catalyst (FeNi-Cl/NC) obtained in example 1 and commercially available iridium oxide, and it can be seen that the FeNi-Cl/NC catalyst in the alkaline state is 10mA cm -2 The maximum current density is stronger than that of iridium oxide.
FIG. 4 is a graph showing the electrocatalytic stability test performance of the electrocatalytic oxygen evolution catalyst (FeNi-Cl/NC) obtained in example 1, with a graph of the curve under 100h stability test, after which there is only a 10mV decay.
The electrocatalytic oxygen evolution catalyst prepared in example 1-example 3 was used for oxygen evolution performance in alkaline medium. Can exert stable performance in alkaline electrolyte.
The above-mentioned embodiments, which further illustrate the objects, technical solutions and advantages of the present invention, should be understood that the above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the nitrogen-doped carbon-loaded chlorine-doped iron-nickel oxide oxygen evolution catalyst is characterized by placing an iron source, a nitrogen source, a chlorine source, a carbon source and a nickel source in an acetone container, heating and stirring the mixture to be viscous, evaporating and drying the mixture to obtain a dried object, and calcining the dried object, wherein the mass part ratio of the iron source to the nickel source is 1-2:1.5-2, wherein the mass part ratio of the nitrogen source to the carbon source is 2-3:1-2, the total mass portion of the iron source and the nickel source and the mass portion ratio of the iron source to the carbon source are 7-8.5:20-25, wherein the total mass parts of the chlorine source and the iron source and the mass parts of the chlorine source and the carbon source are 3-4:7-8.
2. The preparation method of the nitrogen-doped carbon-supported chlorine-doped iron-nickel oxide oxygen evolution catalyst according to claim 1, wherein the mass part ratio of the iron source to the nickel source is 1:1.5, wherein the mass part ratio of the nitrogen source to the carbon source is 2:1, the total mass part of the iron source and the nickel source and the mass part ratio of the iron source to the nickel source to the carbon source are 7:20, the total mass parts of the chlorine source and the iron source and the mass parts of the chlorine source and the carbon source are 3:7.
3. the method for preparing the nitrogen-doped carbon-supported chlorine-doped iron-nickel oxide oxygen evolution catalyst according to claim 1, wherein the nitrogen source and the chlorine source are both hydroxylamine hydrochloride, the carbon source is at least one of carbon black, carbon nanotubes and graphene, the iron source is at least one of iron acetylacetonate, iron oxalate and iron chloride hydrate, and the nickel source is at least one of nickel acetylacetonate, nickel chloride and nickel nitrate.
4. The method for preparing the nitrogen-doped carbon-supported chlorine-doped iron-nickel oxide oxygen evolution catalyst according to claim 1, wherein an iron source, a nitrogen source, a chlorine source, a carbon source and a nickel source are placed in an acetone container, and heated and stirred at 70-80 ℃ to be viscous.
5. The preparation method of the nitrogen-doped carbon-supported chlorine-doped iron-nickel oxide oxygen evolution catalyst according to claim 4, characterized in that the catalyst is heated and stirred at 70-80 ℃ to be viscous and then evaporated and dried, and the specific operation is to evaporate and dry at 60-100 ℃ to obtain a dry object.
6. The preparation method of the nitrogen-doped carbon-supported chlorine-doped iron-nickel oxide oxygen evolution catalyst according to claim 5, characterized in that the calcination treatment operation steps are as follows: the dried object is heated to 450 ℃ under the action of protective gas and pyrolyzed at 450 ℃ for 1-5h.
7. The method for preparing the nitrogen-doped carbon-supported chlorine-doped iron-nickel oxide oxygen evolution catalyst according to claim 6, wherein a dry object is heated to 450 ℃ under the action of a protective gasHeating rate of 1-10 deg.C for min -1 。
8. The method as claimed in claim 7, wherein the shielding gas is at least one of nitrogen, helium, neon, argon, krypton and xenon.
9. An oxygen evolution catalyst produced by the production method according to any one of claims 1 to 8, characterized in that a nitrogen-doped carbon support carrying a nitrogen-doped iron nickel oxide is formed by compounding nitrogen and carbon.
10. Use of the oxygen evolution catalyst according to any of the claims 1 to 8, characterized in that it is used in the field of alkaline media technology.
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