CN114345389A - InN nano-particles with uniform carbon coating, and preparation method and application thereof - Google Patents

InN nano-particles with uniform carbon coating, and preparation method and application thereof Download PDF

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CN114345389A
CN114345389A CN202210028482.6A CN202210028482A CN114345389A CN 114345389 A CN114345389 A CN 114345389A CN 202210028482 A CN202210028482 A CN 202210028482A CN 114345389 A CN114345389 A CN 114345389A
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CN114345389B (en
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高山
黄涛
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Anhui University
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Abstract

The invention relates to the technical field of nano materials and electrocatalysis, and discloses a preparation method of InN nanosheet particles with uniform carbon coating, so that the electrocatalysis reduction of CO is improved2And (4) performance. The invention provides a preparation method of uniform carbon-coated InN nanosheet particles, which comprises the following steps of 1, preparation of a precursor, adding InCl 3.4H 2O into the precursorStirring in deionized water at room temperature for 20-40min, adding ammonia water, stirring for 6-14 hr to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze drying for 5-12 hr to obtain white powder; and 2, preparing the InN nanosheet. And 3, preparing the carbon-coated InN nanosheets. The method for calcining the InN nanosheets coated with the polyvinylpyrrolidone at a proper calcination temperature and for a proper calcination time under an argon atmosphere to obtain the carbon-coated InN nanosheets can realize mass synthesis, and has a wide application prospect in actual large-scale industrial application.

Description

InN nano-particles with uniform carbon coating, and preparation method and application thereof
Technical Field
The invention relates to the technical field of nano materials and electrocatalysis, in particular to InN nano particles with uniform carbon coating, a preparation method and application thereof.
Background
Currently, fossil fueled combustion releases large amounts of CO while providing energy2The problem of gases, and consequently greenhouse effect, has evolved into a global environmental problem. In recent years, researches show that carbon atoms in the fuel can be converted into hydrocarbon fuel to relieve CO2The environmental problem can create new value at the same time, so the method is concerned by extensive researchers. In the electrochemical reduction process of the carbon dioxide, the carbon dioxide molecules and water molecules are converted into valuable compounds by using electric energy generated by renewable energy sources such as wind energy, solar energy, tidal energy and the like, so that on one hand, the high-efficiency storage of the electric energy can be realized, on the other hand, the emission reduction of the carbon dioxide can be realized, and the electrochemical reduction process has wide application prospect. Due to CO2The chemical inertness of the molecule, electro-reduction, is limited to a large extent by the slow reaction kinetics and the huge activation barriers. Furthermore, the hydrogen evolution reaction is considered to be CO2The main competing reactions of electroreduction limit catalytic activity and selectivity. Therefore, to increase CO2The practicality of electroreduction, and the important significance of representing the high-efficiency, high-selectivity and high-stability catalyst on the premise that the exploration and development of the synthetic method are simple and the large-scale synthesis can be realized.
Based on previous studies, a large number of transition metal materials have been developed as highly efficient catalysts. In which InN is applied to electrocatalytic reactions due to its excellent electron transport properties and narrow energy band. However, for pure InN, the CO is reduced electrocatalytically2In the process, severe surface reconstruction occurs, so that the stability is poor, and the method is not favorable for practical application. With the development of scientific technology, researchers find that carbon coating is one of the most common material modification methods. Carbon coating of the material can improve the electrical conductivity of the material on the one hand and provide a stable chemical and electrochemical reaction interface on the other hand, and becomes an important strategy for modifying the catalyst at present. Research reports show that the carbon layer is coated on the surface of the catalyst, so that the catalyst junction can be effectively protectedThe structure is not damaged in the electrocatalysis process, and the unique interface formed between the carbon layer and the catalyst can change the electron transfer path of the catalyst, so that the catalyst has good catalytic activity and stability. In most of the preparation methods of carbon-coated materials reported at present, the synthesis conditions are harsh, the thickness of the obtained carbon layer is not uniform, the production cost is high, and further the catalytic performance of the carbon-coated material is limited. Therefore, the method for exploring the InN nanosheet catalyst with simple synthesis conditions, low production cost and uniform carbon layer thickness has certain challenges.
Disclosure of Invention
The invention aims to provide InN nano particles with uniform carbon coating, a preparation method and application thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a composite material having uniform carbon-coated InN nanoparticles, the InN nanoplatelets being overcoated with a layer of uniform carbon.
Furthermore, the carbon layer has uniform thickness and the thickness value is 3-5 nm.
The invention provides a preparation method of InN nano particles with uniform carbon coating, which comprises the following steps,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 20-40min, adding ammonia water, stirring for 6-14H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 5-12H to obtain white powder;
step 2, preparation of InN nanosheet
Putting the white powder obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tube furnace, carrying out temperature programming to 800 ℃ in an ammonia atmosphere, and calcining the quartz boat for 1h at the temperature of 800 ℃ in 600-;
step 3, preparation of carbon-coated InN nanosheet
Adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the black brown powder obtained in the step 2, stirring at room temperature for 7-13h to form a black brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 5-12h, placing the dried black powder in a quartz boat, placing the quartz boat in a tube furnace, raising the temperature to 400-600 ℃ in an argon atmosphere, and calcining at 400-600 ℃ for 0.5-2h to obtain black powder, wherein the argon is an inert gas, and the flow rate is 10-20 mL/min.
Furthermore, in step 1, under the premise of not changing the adding proportion of the three reactants, the large-scale synthesis can be realized by increasing the dosage of the reactants.
Further, when the mass synthesis is realized, the volume ratio of ammonia water to deionized water is 75-80:1, the mass ratio of InCl3 & 4H2O to deionized water is 1: 100.
Further, in the step 2, the average temperature increase rate of the ammonia gas atmosphere is 14 ℃/min.
Further, in the step 3, the average temperature increase rate of the argon atmosphere is 15 ℃/min.
The invention also provides application of the InN nano-particles with uniform carbon coating as a catalyst for electrocatalytic reduction of carbon dioxide.
The specific use method comprises the steps of weighing 5mg of the carbon-coated InN nanosheet catalyst obtained in the step 3 in the above example, dispersing the carbon-coated InN nanosheet catalyst in 300ul of a mixed solution of absolute ethyl alcohol and naphthol, wherein the volume ratio of the absolute ethyl alcohol to the naphthol is 6:19, and performing ultrasonic dispersion for 30min to obtain a uniformly dispersed mixed solution. 100uL of evenly dispersed mixed liquid is taken by a pipette with the measuring range of 100uL and is dripped and coated on the surface of 1 x 1cm in 2 times2The carbon cloth coated with the catalyst after pretreatment is dried and directly used as a working electrode, and an Ag/AgCl electrode is used as a reference electrode, 1 x 1cm2The platinum sheet electrode as a counter electrode, a three-electrode system was constructed, and then CO was added for 30 minutes after the gas had been injected2Carrying out electrocatalytic reduction of CO in the electrolyte2And (6) testing.
The invention has the beneficial effects that:
1. the method can obtain the InN nanosheets with uniform carbon layer thickness through proper calcination temperature and time under the argon atmosphere, can realize mass synthesis, and has wide application prospect in actual large-scale industrial application.
2. The method enables the nanosheet surface to contain a uniform carbon layer by adjusting the amount of reactants and a calcination technology, the carbon layer can effectively protect the structure of the catalyst from being damaged in an electrocatalysis process, and a unique interface formed between the carbon layer and the catalyst can change an electron transfer path of the catalyst, so that the catalyst has good catalytic activity and stability, and the catalyst has high-efficiency CO2Reduction performance.
3. The carbon-coated InN nanosheet catalyst prepared by the invention is used for electrocatalytic reduction of CO2The catalyst shows excellent catalytic activity and stability. When the potential is-1.1V, the corresponding current density reaches 90mA/cm2Higher than pure InN (70 mA/cm)2) (ii) a at-0.7V, the Faraday efficiency of the carbon-containing product can reach about 80 percent; in addition, the stability of the catalyst can reach 20 hours and is much longer than that of a pure InN catalyst. The catalyst with high activity and good stability has higher practical application value.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort. In the drawings:
fig. 1 is an optical photograph of a carbon-coated InN nanosheet catalyst prepared in accordance with the present invention, resulting in a large scale synthesis.
Fig. 2 is an X-ray diffraction (XRD) pattern of the carbon-coated InN nanosheet catalyst prepared in accordance with the present invention.
Fig. 3a is a transmission electron microscopy micrograph of pure InN nanoplates of the present invention;
fig. 3b is a Transmission Electron Microscope (TEM) image of carbon-coated InN nanoplates;
fig. 3c is a High Resolution Transmission Electron Microscope (HRTEM) photograph of carbon-coated InN nanoplates;
FIG. 4a is an X-ray photoelectron spectroscopy (XPS) plot of a carbon-coated InN nanosheet catalyst prepared in accordance with the present invention
FIG. 4b is an XPS spectrum of a carbon-coated InN nanosheet catalyst prepared in accordance with the present invention;
FIG. 5a shows the carbon-coated InN nanosheet catalyst prepared in the present invention at 0.2M (K)2CO3):0.8M(KHCO3) Linear voltammetric sweep profile (LSV) in electrolyte
FIG. 5b shows the preparation of a carbon-coated InN nanosheet catalyst at 0.2M (K) according to the present invention2CO3):0.8M(KHCO3) Faraday efficiency diagrams at different potentials in the electrolyte;
FIG. 5c is a graph of current density versus time (it) at constant potential.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the embodiments of the present application, it should be noted that the indication of orientation or positional relationship is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship which is usually placed when the product of the application is used, or the orientation or positional relationship which is usually understood by those skilled in the art, or the orientation or positional relationship which is usually placed when the product of the application is used, and is only for the convenience of describing the application and simplifying the description, but does not indicate or imply that the indicated device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the application. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
In the description of the embodiments of the present application, it should also be noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," and "connected" are to be construed broadly, and may for example be fixedly connected, detachably connected, or integrally connected; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
Example 1
A preparation method of InN nano-particles with uniform carbon coating comprises the following steps,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 20min, adding ammonia water, stirring for 6H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 5H to obtain white powder (precursor);
step 2, preparation of InN nanosheet
Putting the white powder (namely the precursor) obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tubular furnace, carrying out programmed heating to 600 ℃ in an ammonia atmosphere, and calcining for 1h at 600 ℃ to obtain black brown powder, wherein the flow rate of ammonia is 10-20 mL/min;
step 3, preparation of carbon-coated InN nanosheet
And (2) adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the black brown powder obtained in the step (2), stirring at room temperature for 7 hours to form a black brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 5 hours, putting the dried black powder into a quartz boat, placing the quartz boat in a tubular furnace, raising the temperature to 400 ℃ by program in an argon atmosphere, and calcining at 400 ℃ for 0.5 hour to obtain black powder, wherein the flow rate of argon is 10-20 mL/min.
Example 2
A preparation method of InN nano-particles with uniform carbon coating comprises the following steps,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 30min, adding ammonia water, stirring for 10H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 8H to obtain white powder (precursor);
step 2, preparation of InN nanosheet
Putting the white powder (namely the precursor) obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tubular furnace, carrying out programmed temperature rise to 700 ℃ in an ammonia atmosphere, and calcining the quartz boat for 1h at the temperature of 700 ℃ to obtain black brown powder, wherein the flow rate of ammonia is 10-20 mL/min;
step 3, preparation of carbon-coated InN nanosheet
And (2) adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the black brown powder obtained in the step (2), stirring at room temperature for 10 hours to form a black brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 8 hours, putting the dried black powder into a quartz boat, placing the quartz boat in a tubular furnace, raising the temperature to 450 ℃ by programming in an argon atmosphere, and calcining at 450 ℃ for 1 hour to obtain black powder, wherein the inert gas argon flows at 10-20 mL/min.
Example 3
A preparation method of InN nano-particles with uniform carbon coating comprises the following steps,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 40min, adding ammonia water, stirring for 14H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 12H to obtain white powder (precursor);
step 2, preparation of InN nanosheet
Putting the white powder (namely the precursor) obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tubular furnace, carrying out programmed heating to 800 ℃ in an ammonia atmosphere, and calcining for 1h at 800 ℃ to obtain black brown powder, wherein the flow rate of ammonia is 10-20 mL/min;
step 3, preparation of carbon-coated InN nanosheet
And (2) adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the black brown powder obtained in the step (2), stirring at room temperature for 13 hours to form a black brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 12 hours, putting the dried black powder into a quartz boat, placing the quartz boat in a tubular furnace, raising the temperature to 600 ℃ by programming in an argon atmosphere, and calcining at 600 ℃ for 2 hours to obtain black powder, wherein the inert gas argon flows at 10-20 mL/min.
Example 4
The invention provides a preparation method of InN nano-particles with uniform carbon coating, which comprises the following steps,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 20min, adding ammonia water, stirring for 6H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 5H to obtain white powder (precursor);
step 2, preparation of InN nanosheet
Putting the white powder (namely the precursor) obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tubular furnace, carrying out programmed temperature rise to 700 ℃ in an ammonia atmosphere, and calcining the quartz boat for 1h at the temperature of 700 ℃ to obtain black brown powder, wherein the flow rate of ammonia is 10-20 mL/min;
step 3, preparation of carbon-coated InN nanosheet
And (2) adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the black brown powder obtained in the step (2), stirring at room temperature for 3 hours to form a black brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 12 hours, putting the dried black powder into a quartz boat, placing the quartz boat in a tube furnace, heating to 600 ℃ in an argon atmosphere, and calcining at the temperature of 400-600 ℃ for 2 hours to obtain black powder, wherein the argon is an inert gas at the flow rate of 10-20 mL/min.
Example 5
The invention provides a preparation method of InN nano particles with uniform carbon coating, which comprises the following steps,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 40min, adding ammonia water, stirring for 14H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 12H to obtain white powder (precursor);
step 2, preparation of InN nanosheet
Putting the white powder (namely the precursor) obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tubular furnace, carrying out programmed temperature rise to 700 ℃ in an ammonia atmosphere, and calcining the quartz boat for 1h at the temperature of 700 ℃ to obtain black brown powder, wherein the flow rate of ammonia is 10-20 mL/min;
step 3, preparation of carbon-coated InN nanosheet
And (2) adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the black brown powder obtained in the step (2), stirring at room temperature for 7 hours to form a black brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 5 hours, putting the dried black powder into a quartz boat, placing the quartz boat in a tubular furnace, heating to 400 ℃ in an argon atmosphere, and calcining at 400 ℃ for 0.5 hour to obtain black powder, wherein the argon is an inert gas at the flow rate of 10-20 mL/min.
For the analysis of the product obtained in the above example, as can be seen from fig. 2, phase analysis is performed on the carbon-coated InN nanosheet catalyst prepared in the present invention by using XRD, and all diffraction peaks obtained by performing phase analysis on the carbon-coated InN nanosheet catalyst can be matched with a card with the number of JCPDS: 50-1239, indicating that the material synthesized by the present invention is indium nitride.
As can be seen from the TEM photograph of FIG. 3b, the size of the carbon-coated InN nanosheet synthesized in the present invention is about 100-200 nm; furthermore, with respect to the pure InN in fig. 3a, it is evident that there is a ring of carbon layers around the periphery; in addition, the high-resolution TEM photograph, specifically see fig. 3c, shows that the lattice spacing of the nanosheets is 0.31nm, which corresponds to the (100) plane of indium nitride, and we can clearly observe the carbon layer structure at the periphery of the carbon-coated nanosheets, which also indicates that we successfully synthesized the InN catalyst with the carbon-coated structure.
From XPS full spectrum (fig. 4a), it can be seen that In, N, and C elements are present In the carbon-coated InN nanosheet catalyst, and further from XPS spectrum (fig. 4b) of In elements, it can be seen that In 3d binding energy of carbon-coated InN species moves In a high energy direction relative to pure InN, indicating that the carbon-coated InN obtained by the present invention has electron movement from InN to a carbon layer, and that there is interaction between the carbon layer and InN.
According to the invention, all the characterization results are integrated, the metal indium ions and ammonia water are coordinated to form a precursor through simple stirring, and then the carbon-coated InN nanosheet with uniform carbon layer thickness can be obtained through proper calcination temperature and time in different atmospheres.
Example 6
The implementation steps are the same as those of the embodiment 2, the ratio of ammonia to deionized water in the step 1 is 75-80:1, and the mass ratio of InCl 3.4h2O to deionized water is 1:100, except that the use amount of each raw material in the embodiment is increased by 2-100 times, and the rest conditions are unchanged, so that the corresponding multiple increase of the obtained product can be realized, therefore, by increasing the raw materials of the carbon-coated InN nanosheet catalyst, a large amount of catalyst can be obtained, as shown by combining the optical photograph of the attached drawing 1, by increasing the raw materials of the carbon-coated InN nanosheet catalyst prepared by the present invention, the method for preparing the carbon-coated InN nanosheet catalyst is simple, and a large amount of synthesis can be realized.
Example 7
The InN nanoplate particles prepared in examples 1-5 were subjected to application testing. Namely, the carbon-coated InN nanosheet catalyst is applied to the electrocatalytic reduction of CO2Detailed description of the inventionAs follows.
Weighing 5mg of the carbon-coated InN nanosheet catalyst obtained in the step 3 in the above example, dispersing the carbon-coated InN nanosheet catalyst in 300ul of a mixed solution of absolute ethyl alcohol and naphthol, wherein the volume ratio of the absolute ethyl alcohol to the naphthol is 6:19, and performing ultrasonic dispersion for 30min to obtain a uniformly dispersed mixed solution. 100uL of evenly dispersed mixed liquid is taken by a pipette with the measuring range of 100uL and is dripped and coated on the surface of 1 x 1cm in 2 times2The carbon cloth coated with the catalyst after pretreatment is dried and directly used as a working electrode, and an Ag/AgCl electrode is used as a reference electrode, 1 x 1cm2The platinum sheet electrode as a counter electrode, a three-electrode system was constructed, and then CO was added for 30 minutes after the gas had been injected2Carrying out electrocatalytic reduction of CO in the electrolyte2Test in which the electrolyte had a raw material composition of 0.2M (K)2CO3):0.8M(KHCO3). In the test, Linear Sweep Voltammetry (LSV) is adopted to probe the electrocatalytic activity of the catalyst, and the change of current with time under different potentials is tested by a potentiostatic method to show the Faraday efficiency and the stability of the catalyst. And the performance of the carbon-coated InN catalyst prepared in the invention is compared with that of pure InN.
As shown by the LSV test results of fig. 5a, at 0.2M K2CO3:0.8M KHCO3In the electrolyte, the carbon-coated InN nanosheet catalyst prepared by the invention is used for carrying out electrocatalytic reduction on CO2When the potential is-1.1V, the corresponding current density is 90mA/cm2Higher than pure InN (70 mA/cm)2)。
Figure 5b shows faradaic efficiencies at different potentials. The test result shows that the faradaic efficiency of the carbon-containing product can reach about 80 percent at-0.7V.
In addition, the results of the current density time-dependent curve test at constant potential in fig. 5c show that the stability of the catalyst can reach 20 hours and is much longer than that of the pure InN catalyst (4.5 h).
The electrochemical test results show that the carbon-coated InN nanosheet prepared by the method can be well applied to electrocatalytic reduction of CO2The catalytic activity and stability are higher than those of pure InN, and the catalyst has higher practical application value. The catalytic effect is obvious.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. An InN nanoparticle with uniform carbon coating, characterized by: and the InN nano-sheet particles are coated with a layer of composite material with a uniform carbon layer.
2. An InN nanoplate particle according to claim 1, wherein: the carbon layer has uniform thickness and the thickness value is 3-5 nm.
3. A method of preparing the nanoparticles of claim 1 or 2 having a uniform carbon coating InN, wherein: comprises the following steps of (a) carrying out,
step 1, preparation of precursor
Adding InCl3 & 4H2O into deionized water, stirring at room temperature for 20-40min, adding ammonia water, stirring for 6-14H to form white precipitate, washing the precipitate with deionized water and ethanol, and freeze-drying for 5-12H to obtain white powder;
step 2, preparation of InN nanosheet
Putting the white powder obtained after drying in the step 1 into a quartz boat, placing the quartz boat in a tube furnace, carrying out temperature programming to 800 ℃ in an ammonia atmosphere, and calcining the quartz boat for 1h at 800 ℃ in 600-;
step 3, preparation of carbon-coated InN nanosheet
Adding polyvinylpyrrolidone into deionized water to form a transparent solution, adding the blackish brown powder obtained in the step 2, stirring at room temperature for 7-13h to form a blackish brown precipitate, washing the precipitate with deionized water and ethanol, then drying in vacuum for 5-12h, placing the dried black powder in a quartz boat, placing the quartz boat in a tube furnace, raising the temperature to 400-600 ℃ in an argon atmosphere, and calcining at 400-600 ℃ for 0.5-2h to obtain the black powder.
4. The production method according to claim 3, characterized in that: in step 1, under the premise of not changing the adding proportion of the three reactants, the large-scale synthesis can be realized by increasing the dosage of the reactants.
5. The method of claim 4, wherein: when the mass synthesis is realized, the volume ratio of ammonia water to deionized water is 75-80:1, the mass ratio of InCl3 & 4H2O to deionized water is 1: 100.
6. The production method according to claim 3, characterized in that: in the step 2, the average temperature increase rate of the ammonia gas atmosphere is 14 ℃/min.
7. The production method according to claim 3, characterized in that: in the step 3, the average heating rate of the argon atmosphere is 15 ℃/min.
8. The use of the uniformly carbon coated InN nanoparticles as claimed in claim 1 or 2 as a catalyst for the electrocatalytic reduction of carbon dioxide.
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CN115430450B (en) * 2022-08-30 2024-05-14 上海交通大学 Preparation method and application of Rh nanoparticle modified III-group nitrogen oxide Si catalyst

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