CN113026049A - Two-step solvothermal method for preparing NiFe (CN)5NO-Ni3S2-NF composite catalyst and application thereof - Google Patents
Two-step solvothermal method for preparing NiFe (CN)5NO-Ni3S2-NF composite catalyst and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of nano composite materials, relates to an electrolytic water oxygen evolution catalyst, and particularly relates to a two-step method for preparing NiFe (CN)5NO/Ni3S2a/NF hybrid catalyst comprising: the prepared mass percentage concentration is 1-5 mg mL‑1Transferring the thiourea deionized water solution into a reaction kettle, immersing the pretreated nickel foam into the solution, carrying out hydrothermal reaction at 120-180 ℃ for 3-10 h, naturally cooling to room temperature, taking out the solution, washing with deionized water, and carrying out vacuum drying at 60 ℃ for 12h to obtain Ni3S2/NF; according to the solid-to-liquid ratio of 1In a ratio of 00-300 mg to 20mL, adding Na2Fe(CN)5NO•2H2Dissolving O in ethylene glycol, transferring into a reaction kettle, and adding Ni3S2and/NF, carrying out solvothermal reaction for 6-12 h at 200 ℃, cooling to room temperature, taking out, washing with deionized water, and carrying out vacuum drying for 12h at 60 ℃ to obtain the catalyst. The synthetic method is simple and feasible, has low cost and is suitable for large-scale production. Benefit from Ni3S2And NiFe (CN)5The catalyst shows excellent OER electro-catalytic activity and stability due to the synergistic effect of NO and the excellent characteristics of the NF carrier, and is expected to be practically applied to electrolyzed water.
Description
Technical Field
The invention belongs to the technical field of nano composite material preparation, relates to an electrolytic water oxygen evolution catalyst, and particularly relates to a two-step method for preparing NiFe (CN)5NO-Ni3S2NF (i.e. NiFe (CN))5NO/Ni3S2/NF) composite catalyst and application thereof.
Background
In recent years, as the human society has been developed to depend on fossil fuels excessively, there are many problems that human beings have to pay attention to, such as environmental pollution and CO generation by using fossil fuels2Resulting in greenhouse effect, etc. Most importantly, fossil fuels are non-renewable energy sources, and with the excessive exploitation and use of human beings, the storage of fossil fuels is also becoming exhausted. On the other hand, common renewable energy sources such as wind energy, solar energy, tidal energy, geothermal energy, and the like cannot be widely applied due to factors such as the need for a special geographical environment.
The hydrogen energy is used as a pollution-free clean energy and has a very good application prospect in the fields of fuel cells and the like. There are many methods for producing hydrogen, and among them, the electrolysis of water to produce hydrogen is enthusiastic to researchers because of its simple process. The hydrogen production process by water electrolysis comprises two aspects: anodic Oxygen Evolution Reaction (OER) and cathodic Hydrogen Evolution Reaction (HER). In general, the two reactions have slower kinetic characteristics, require higher voltage for driving, and consume a large amount of electric energy. In order to solve the above problems, researchers need to develop an efficient electrocatalyst to reduce the reaction barrier and thus the driving voltage required for the reaction.
The current common commercial catalysts are noble metal-based catalysts such as Pt, Ru and Ir, are expensive and have scarce resource reserves on the earth, so that the wide application of the catalysts in the industry is limited. Therefore, it is necessary to develop a highly efficient and stable non-noble metal-based catalyst (such as transition metal-based catalyst of Fe, Co, Ni, etc.) instead of noble metal-based catalyst.
In recent years, transition metal compounds (such as oxides, borides, nitrides, sulfides, phosphides, etc.) of Fe, Co and Ni have been studied as alkaline electrolytic water catalysts because of their advantages such as structural diversity and low cost. Among them, transition metal sulfides are considered to be promising electrolytic water catalyst materials due to their higher electrical conductivity. In addition, the preparation of electrolytic water catalyst materials using Metal Organic Frameworks (MOFs) has been explored because of their advantages such as high specific surface area, special metal active sites and porosity.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to disclose a two-step solvothermal method for preparing NiFe (CN)5NO/Ni3S2a/NF composite catalyst.
The invention uses foam Nickel (NF) with large specific surface area, good conductivity and high mechanical strength as a catalyst carrier and serves as a nickel source; the Ni is obtained by sulfurizing NF by hydrothermal method using non-toxic thiourea as sulfur source3S2/NF; then adding Na2Fe(CN)5NO•2H2O solvothermal method for Ni in ethylene glycol solution3S2Ion exchange of/NF to synthesize Ni loaded on foam nickel without binder3S2And NiFe (CN)5NO composite catalyst (expressed as NiFe (CN))5NO/Ni3S2/NF）。
Technical scheme
Two-step solvothermal method for preparing NiFe (CN)5NO/Ni3S2the/NF composite catalyst comprises the following steps:
(1) the prepared mass percentage concentration is 1-5 mg mL-1Preferably 2.5mg mL-1The thiourea deionized water solution is moved into a reaction kettle, the pretreated foam nickel is completely immersed, hydrothermal reaction is carried out for 3-10 h at 120-180 ℃, preferably reaction is carried out for 5 h at 150 ℃, natural cooling is carried out to room temperature, the solution is taken out and washed by deionized water, vacuum drying is carried out for 12h at 60 ℃, and Ni is obtained3S2/NF；
(2) And according to the solid-liquid ratio of 100-300 mg:20 mL, preferably 200 mg:20 mL of Na2Fe(CN)5NO•2H2And O is completely dissolved in ethylene glycol, transferred into a reaction kettle, and mixed according to the solid-liquid ratio of 200 mg:20 mL of Ni3S2/NF, carrying out solvothermal reaction at 200 ℃ for 6-12 h, preferably at 200 ℃ for 9 h, cooling to room temperature, taking out, washing with deionized water, and vacuum drying at 60 ℃ for 12h to obtain NiFe (CN)5NO/Ni3S2a/NF composite catalyst.
In a preferred embodiment of the present invention, the pretreated nickel foam comprises the following steps: soaking commercial nickel foam in 6M HCl for over 30min to remove surface oxides and impurities, and allowing the treated nickel foam to directly serve as a nickel source to participate in the reaction.
Ni produced by the invention3S2Ni in/NF3S2The nano-sheet array is closely attached to the surface of the foam nickel, and the final product is a rod-shaped NiFe (CN) assembled by nano-sheets5NO-Ni3S2Attached to the surface of the nickel foam.
NiFe (CN) prepared by the invention5NO/Ni3S2the/NF has a rod-shaped appearance formed by combining nano sheets, can provide more active sites, has lower electrochemical impedance to participate in electrochemical catalytic reaction, and can be applied to oxygen evolution reaction electrode catalysts.
Oxygen evolution experiment:
the obtained NiFe (CN)5NO/Ni3S2/NF shear area of 1 × 1 cm2The piece of (a) was used as a working electrode, a saturated silver/silver chloride electrode was used as a reference electrode, a carbon rod was used as a counter electrode, and a CV curve graph was measured in a 1M KOH solution using an electrochemical workstation (chenhua 760E).
As an oxygen evolution reaction electrode catalytic material, the excellent performance is shown to have lower initial over potential and smaller Tafel slope, and the current density is 10 mA cm in general-2Overpotential of time is used as a measure. Discovery with NiFe (CN)5NO/NF、Ni3S2comparative/NF, NiFe (CN)5NO/Ni3S2the/NF has more excellent catalytic performance in oxygen evolution reaction, obviously reduced over potential and Tafel slope and good stability.
Reagents and raw materials used: na (Na)2Fe(CN)5NO•2H2O (sodium nitrosoferricyanide), shanghai chemical agents ltd; HCl (hydrochloric acid), national chemical agents ltd; CN2H4S (thiourea), national chemical reagents ltd; (CH)2OH)2(ethylene glycol), national chemical agents, ltd; KOH (potassium hydroxide), national chemical agents ltd; are all analytically pure; nickel Foam (NF), chandeli new materials ltd.
Advantageous effects
Firstly, the foamed nickel is vulcanized to obtain Ni3S2/NF; then using solvothermal method to make Ni3S2/NF and Na2Fe(CN)5Ion exchange of NO to NiFe (CN)5NO/Ni3S2/NF oxygen evolution catalyst. The catalytic performance of the catalyst is higher than that of the commercial noble metal catalyst IrO2More excellent. The synthetic method is simple and feasible, has low cost and is suitable for large-scale production, and the prepared NiFe (CN)5NO/Ni3S2The NF electrolyzed water oxygen evolution catalyst has excellent performance and very high popularization and application values. Benefit from Ni3S2And NiFe (CN)5The synergistic effect of NO and the excellent characteristics of the NF carrier show excellent OER electrocatalytic activity and stability, and are expected to play a role in the practical application of water electrolysis.
Drawings
FIG. 1 NiFe (CN) prepared in example 15NO/Ni3S2X-ray diffraction (XRD) pattern of/NF composite material;
FIG. 2 NiFe (CN) prepared in example 15NO/Ni3S2A field emission Scanning Electron Microscope (SEM) picture of the/NF composite material;
FIG. 3 NiFe (CN) prepared in example 15NO/Ni3S2Energy spectrum (EDS) diagram of the/NF composite, wherein the abscissa is energy in Ke V and the ordinate is intensity in cps;
FIG. 4 NiFe (CN) prepared in examples 1 to 55NO/Ni3S2CV half-curve diagram of the/NF composite measured in a 1M KOH solutionThe test temperature is 25 ℃, after full activation by cyclic voltammetry scanning for 100 circles, the voltage range is 0-0.7V (Vvs Ag/AgCl) was subjected to CV curve test at a sweep rate of 5 mV s-1. The abscissa is voltage in units of V; the ordinate is the current density in mA cm-2；
FIG. 5 NiFe (CN) prepared in example 15NO/Ni3S2Tafel graph of/NF composite material as electrolyzed water oxygen evolution catalyst in 1M KOH solution, wherein the abscissa is current density (unit is mA cm)-2) The logarithm of (d); the ordinate is the overpotential in V;
FIG. 6 NiFe (CN) prepared in example 15NO/Ni3S2the/NF composite material is used as an electrolytic water oxygen evolution catalyst and is in the electrolyte of 1M KOH at 10 mA cm-2In which the abscissa is time in h and the ordinate is voltage in V, the voltage is plotted against time in 17 h.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
Adding 200 mg of Na2Fe(CN)5NO•2H2Dissolving O in 20mL of ethylene glycol, stirring for 30min, putting the solution into a 30 mL reaction kettle liner, and then adding Ni3S2the/NF is also put into the reaction kettle and reacts in an oven at the temperature of 200 ℃ for 9 hours. After the reaction is finished, washing the nickel foam with deionized water for a plurality of times, then putting the reacted nickel foam into a vacuum oven to be dried at 60 ℃, and finally obtaining NiFe (CN)5NO/Ni3S2a/NF composite material.
FIG. 1 is an XRD diagram of the product, in which all diffraction peaks except the signal peak of metallic nickel foam are in a cubic phase of NiFe (CN)5NO•5H2Standard card of O (JCPDS, number 43-0772) and Ni in cubic phase3S2Is consistent with the standard card (JCPDS, number 44-1418), indicating that the target product NiFe (CN) is successfully prepared5NO/Ni3S2/NF。
FIG. 2 is an SEM image of the product, from which it can be seen that the product NiFe (CN)5NO/Ni3S2the/NF is a rod formed by combining nano sheets and attached to the surface of the foam nickel.
FIG. 3 is the EDS spectrum of the product, the sample contains Fe, Ni, C, N, O and S elements.
As can be seen from the CV half-curve in FIG. 4, NiFe (CN)5NO/Ni3S2/NF Current Density of 10 mA cm-2The overpotential is 162 mV, has the most excellent performance and the performance is similar to that of commercial IrO2The comparison is more excellent.
As can be seen from the Tafel curve in FIG. 5, NiFe (CN)5NO/Ni3S2Tafel slope of/NF was 26 mV dec-1Which shows that it has superior oxygen evolution kinetics.
FIG. 6 is NiFe (CN)5NO/Ni3S2Voltage vs time curves of the NF catalyst in 1M KOH solution. The catalyst was tested for stability at 10 mA cm-2After the electrolysis is carried out for 17 hours under the constant current density, the good catalytic activity is still kept, which shows that the synthesized material has good stability.
Example 2
Adding 100 mg of Na2Fe(CN)5NO•2H2Dissolving O in 20mL of ethylene glycol, stirring for 30min, putting the solution into a 30 mL reaction kettle liner, and then adding Ni3S2the/NF is also put into the reaction kettle and reacts in an oven at the temperature of 200 ℃ for 9 hours. After the reaction is finished, washing the nickel foam with deionized water for a plurality of times, then putting the reacted nickel foam into a vacuum oven for drying at 60 ℃, and finally obtaining NiFe (CN)5NO/Ni3S2a/NF composite material.
Example 3
Adding 300mg of Na2Fe(CN)5NO•2H2Dissolving O in 20mL of ethylene glycol, stirring for 30min, putting the solution into a 30 mL reaction kettle liner, and then adding Ni3S2the/NF is also put into the reaction kettle and is reacted in an ovenThe temperature is 200 ℃ and the time is 9 h. After the reaction is finished, washing the nickel foam with deionized water for a plurality of times, then putting the reacted nickel foam into a vacuum oven to be dried at 60 ℃, and finally obtaining NiFe (CN)5NO/Ni3S2a/NF composite material.
Example 4
Adding 200 mg of Na2Fe(CN)5NO•2H2Dissolving O in 20mL of ethylene glycol, stirring for 30min, putting the solution into a 30 mL reaction kettle liner, and then adding Ni3S2the/NF is also put into the reaction kettle and reacts in an oven at the temperature of 200 ℃ for 6 hours. After the reaction is finished, washing the nickel foam with deionized water for a plurality of times, then putting the reacted nickel foam into a vacuum oven to be dried at 60 ℃, and finally obtaining NiFe (CN)5NO/Ni3S2a/NF composite material.
Example 5
Adding 200 mg of Na2Fe(CN)5NO•2H2Dissolving O in 20mL of ethylene glycol, stirring for 30min, putting the solution into a 30 mL reaction kettle liner, and then adding Ni3S2the/NF is also put into the reaction kettle and reacts in an oven at the temperature of 200 ℃ for 12 hours. After the reaction is finished, washing the nickel foam with deionized water for a plurality of times, then putting the reacted nickel foam into a vacuum oven to be dried at 60 ℃, and finally obtaining NiFe (CN)5NO/Ni3S2a/NF composite material.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (9)
1. Two-step solvothermal method for preparing NiFe (CN)5NO/Ni3S2the/NF composite catalyst is characterized by comprising the following steps:
(1) the prepared mass percentage concentration is 1-5 mg mL-1Transferring the thiourea solution into a reaction kettle, and pre-treatingCompletely immersing foamed nickel, carrying out hydrothermal reaction at 120-180 ℃ for 3-10 h, naturally cooling to room temperature, taking out, washing with deionized water, and carrying out vacuum drying at 60 ℃ for 12h to obtain Ni3S2/NF；
(2) And according to the solid-liquid ratio of 100-300 mg:20 mL of Na2Fe(CN)5NO•2H2And O is completely dissolved in ethylene glycol, transferred into a reaction kettle, and mixed according to the solid-liquid ratio of 200 mg:20 mL of Ni3S2and/NF, carrying out solvothermal reaction for 6-12 h at 200 ℃, cooling to room temperature, taking out, washing with deionized water, and carrying out vacuum drying for 12h at 60 ℃ to obtain the catalyst.
2. The two-step solvothermal method of preparing NiFe (CN)' according to claim 15NO/Ni3S2the/NF composite catalyst is characterized in that: the preparation mass percentage concentration in the step (1) is 2.5mg mL-1Deionized water solution of thiourea.
3. The two-step solvothermal method of preparing NiFe (CN)' according to claim 15NO/Ni3S2the/NF composite catalyst is characterized in that: carrying out hydrothermal reaction at 150 ℃ for 5 h in the step (1).
4. The two-step solvothermal method of preparing NiFe (CN)' according to claim 15NO/Ni3S2the/NF composite catalyst is characterized in that: the pretreated foamed nickel in the step (1) is treated by soaking commercial foamed nickel in 6M HCl for over 30min to remove surface oxides and impurities, and the treated foamed nickel is directly used as a nickel source to participate in the reaction.
5. The two-step solvothermal method of preparing NiFe (CN)' according to claim 15NO/Ni3S2the/NF composite catalyst is characterized in that: in the step (2), the solid-to-liquid ratio is 200 mg:20 mL of Na2Fe(CN)5NO•2H2O is completely dissolved in ethylene glycol.
6. The two-step solvothermal method of preparing NiFe (CN)' according to claim 15NO/Ni3S2the/NF composite catalyst is characterized in that: and (3) carrying out solvothermal reaction at 200 ℃ for 9 h in the step (2).
7. NiFe (CN) produced by the method according to any one of claims 1 to 65NO/Ni3S2a/NF composite catalyst.
8. The NiFe (CN) of claim 75NO/Ni3S2the/NF composite catalyst is characterized in that: the rod-shaped appearance assembled by the nano sheets is attached to the surface of the foam nickel.
9. A process according to claim 7 or 8 wherein said NiFe (CN)5NO/Ni3S2The application of the/NF composite catalyst is characterized in that: it is applied to an oxygen evolution reaction electrode catalyst.
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