CN113604838A - Preparation method and application of nickel-cobalt bimetallic selenide heterostructure electrocatalyst - Google Patents
Preparation method and application of nickel-cobalt bimetallic selenide heterostructure electrocatalyst Download PDFInfo
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Abstract
The invention belongs to the field of nano materials, and discloses a preparation method and application of a nickel-cobalt double-metal selenide heterostructure electrocatalyst. Synthesizing a nickel-cobalt nanowire precursor through simple hydrothermal reaction, further generating Co-MOF particles on the surface of the nickel-cobalt nanowire precursor through a coprecipitation method, and finally carrying out N-phase synthesis on the nickel-cobalt nanowire precursor at low temperature2Calcining under atmosphere to obtain (Ni, Co) Se2/CoSe2/NF heterostructure electrocatalysts. The series of bimetallic selenides have lower charge transfer resistance and reaction barrier of hydrogen evolution and oxygen evolution reactions, and have excellent performance in electrocatalytic hydrogen evolution and oxygen evolution reactions. Meanwhile, the catalyst has low cost, simple and convenient synthesis operation, simple process and excellent catalytic performance,provides basic application research for the material in the field of electrocatalysis.
Description
Technical Field
The invention belongs to the field of nano materials, and relates to the field of electrocatalysts and preparation thereof. More particularly, relates to a preparation method and application of a layered double-metal selenide electrocatalyst for high-performance electrochemical decomposition of water to produce hydrogen and oxygen.
Technical Field
With the gradual exhaustion of non-renewable fossil fuels and the aggravation of environmental pollution, the search for new energy sources with high efficiency, low cost and environmental protection is urgent. Hydrogen has attracted much attention as a clean, pollution-free, renewable energy source with high energy density. In the existing hydrogen production technology, the electrochemical decomposition of water is considered to be one of the most promising hydrogen production methods at present due to the advantages of high energy conversion efficiency, zero emission, high hydrogen production purity and the like. Currently, noble metals Pt, Ru, etc. are still considered as the most effective hydrogen and oxygen evolution electrocatalysts, but their high cost and low resource reserves limit their large-scale commercial production. Therefore, the development of a high-efficiency, stable and rich non-noble metal electrocatalyst for replacing noble metals is an effective way for realizing the industrialization of the hydrogen production by electrolyzing water.
Transition metal selenides have found widespread use in the field of water splitting in recent years due to their unique physicochemical properties. This is mainly due to the low electronegativity of the Se element making OH-Diffusion to the active surface of the electrode is faster and more convenient. In addition, the lower electronegativity of Se allows the metal selenides to have stronger metalloid properties and higher conductivity and anionic selenium (Se)2-) Has larger size, can provide a proper band gap so as to improve the electrochemical activity of the transition metal selenide. In addition, compared with single metal selenide, the ternary bimetallic selenide has higher conductivity, and the effective synergistic effect between the two metals is beneficial to further improving the electrochemical performance. For example, Xia et al successfully produced (Ni, Co) on carbon fiber sheets by a simple two-step hydrothermal process0.85An array of Se nanotubes. With pure Co0.85Se phase, bimetallic selenide (Ni, Co)0.85Se has a unique structure and chemical composition and thus higher electrocatalytic activity and stability (j. mater. chem. a,2018,6, 7585-. On the other hand, Li et al successfully grown a novel CuCoSe nanotube array structure in situ on nickel foam by simple hydrothermal and subsequent selenization methods, and the results showed that the OER electrocatalytic activity of the bimetallic selenide CuCoSe is significantly better than that of pure CuSe and CoSe due to the synergistic effect of two different metal-based components (ChemElectrochem 2019,6, 331-335). However, although the above studies have achieved remarkable effects, the transition metal has a single structureSelenides are generally limited by insufficient active sites, slow reaction kinetics, etc., resulting in electrocatalytic activity that is still far lower than noble metal electrocatalysts. It is therefore meaningful and challenging to design and prepare bimetallic selenides with layered heterostructures for fully decomposing water in alkaline solutions.
Disclosure of Invention
It is an object of the present invention to provide a high performance layered double metal selenide heterostructure electrocatalyst. The catalyst prepared by the method has the advantages of simple preparation method, lower overpotential and Tafel slope, and good conductivity, and the layered nano array structure can greatly improve the water decomposition efficiency of the catalyst. In addition, the selenide synthesized in situ by taking the foamed nickel as the substrate can shorten an ion/electron transmission path, accelerate charge transfer and further improve the conductive capability of the material, thereby improving the catalytic activity of the material. Therefore, the nickel-cobalt bimetallic selenide is synthesized in situ by taking the foamed nickel as a substrate material, is applied to electrochemical full-hydrolysis, and has better application prospect.
The technical scheme of the invention is as follows:
(1) cleaning the foamed nickel for later use
Ultrasonically cleaning commercial foam nickel by using hydrochloric acid, acetone, ethanol and deionized water in sequence, and drying to obtain clean foam nickel;
(2) preparing a nickel-cobalt nanowire precursor with foam Nickel (NF) as a substrate, namely NiCo NWs/NF;
weighing Ni (NO)3)2·6H2O、Co(NO3)2·6H2Adding deionized water, dissolving completely to obtain a precursor solution, and placing the precursor solution in a reaction kettle; immersing the foamed nickel cleaned in the step (1) in the precursor solution, transferring the reaction kettle to an oven for hydrothermal reaction, taking out the foamed nickel after the reaction is finished, washing with water and alcohol, and drying in vacuum overnight;
(3) preparing NiCo NWs/Co-MOF/NF with foamed Nickel (NF) as a substrate;
weighing Co (NO)3)2·6H2Dissolving O and 2-methylimidazole in methanol respectively, and stirring to obtain mixtureMixing the solution, namely putting the NiCo NWs/NF prepared in the step (2) into the solution for standing, taking out, washing with water and alcohol, and drying in vacuum overnight to obtain a precursor, namely NiCo NWs/Co-MOF/NF;
(4) preparation of foamed Nickel (NF) -based (Ni, Co) Se2/CoSe2/NF；
Placing the NiCo NWs/Co-MOF/NF prepared in the step (3) into an open porcelain boat, transferring the porcelain boat into a temperature rising tube furnace with automatic program temperature control, and putting the porcelain boat into an N2Calcining in atmosphere, naturally cooling to room temperature after calcining, and taking out to obtain the nickel-cobalt bimetallic selenide heterostructure electrocatalyst, namely (Ni, Co) Se2/CoSe2/NF。
In step (2), Ni (NO)3)2·6H2O、Co(NO3)2·6H2The molar ratio of O is 1: 2, in the precursor solution, Ni (NO)3)2·6H2The concentration of O is 0.017 mol.L-1，Co(NO3)2·6H2The concentration of O is 0.033 mol. L-1The size of the foam nickel is 2cm multiplied by 5 cm; the temperature of the hydrothermal reaction is 100 ℃, and the reaction time is 6 h.
In the step (3), Co (NO) is added into the mixed solution3)2·6H2The concentration of O is 0.052 mol.L-1The concentration of 2-methylimidazole is 0.810 mol.L-1And standing for 12 h.
In the step (4), the heating rate is 2 ℃/min, the calcining temperature is 450 ℃, and the calcining time is 2 h.
In the steps (1), (2) and (3), the drying temperature is 60 ℃, and the drying time is 12 h.
The nickel-cobalt bimetallic selenide heterojunction prepared by the invention can be applied to electrocatalysis full-hydrolysis under alkaline conditions.
The product was analyzed for composition morphology using an X-ray diffractometer (XRD), a Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM). A three-electrode reaction device is adopted, a platinum wire is used as a counter electrode, a mercury oxide (Hg/HgO) electrode is used as a reference electrode, and the electrochemical performance of the product is tested in a 1M KOH electrolyte.
The invention has the beneficial effects that:
(1) the preparation method disclosed by the invention is composed of simple hydrothermal reaction, normal-temperature standing and low-temperature calcining reaction, and has the advantages of simple steps, convenience in operation, environmental friendliness and strong repeatability;
(2) the layered nano array structure of the material increases the specific surface area of the electrode active material, provides more active sites, is beneficial to the permeation of electrolyte and the release of bubbles after reaction, and the synergistic effect between two different metal selenides regulates the electronic structure and improves the electron transmission efficiency, so the electrocatalytic activity can be further improved
(3) The material of the invention grows on the foam nickel in situ, avoids using polymer binder, reduces the indirect contact resistance between the material and the electrode, thereby enhancing the charge transfer efficiency and quickening the reaction kinetics. These factors synergistically enhance the electrocatalytic capacity of the material in water splitting reactions.
Drawings
FIG. 1 shows the prepared (Ni, Co) Se2/CoSe2XRD diffraction pattern of/NF electrocatalyst.
FIGS. 2a, b are prepared (Ni, Co) Se2/CoSe2Scanning electron micrographs of/NF electrocatalyst; FIG. 2c and d are (Ni, Co) Se2/CoSe2Transmission electron micrograph of/NF electrocatalyst.
FIGS. 3a and b are respectively prepared (Ni, Co) Se2/CoSe2Comparative plots of polarization curves for hydrogen evolution and oxygen evolution reactions under 1M KOH for NF and a series of comparative electrocatalysts.
FIGS. 4a and b are respectively prepared (Ni, Co) Se2/CoSe2Comparative plot of the TfServ curves for hydrogen evolution and oxygen evolution reactions under 1M KOH for NF and a series of comparative electrocatalysts.
Detailed Description
The invention will be further described with reference to the drawings and specific examples, but the scope of the invention is not limited thereto.
Comparative example 1
Preparation of NiCo NWs/NF electrocatalyst based on foam Nickel (NF):
ultrasonically cleaning foamed nickel with 3M hydrochloric acid, acetone, anhydrous ethanol and deionized water for 30min, and drying at 60 deg.C.
0.29g of Ni (NO) was weighed3)2·6H2O，0.58g Co(NO3)2·6H2Adding O and 0.6g of urea into 60mL of deionized water, stirring for 30 minutes to obtain a precursor solution, putting the foamed nickel (2cm multiplied by 5cm) into the precursor solution, transferring the precursor solution into a reaction kettle, carrying out hydrothermal treatment at 120 ℃ for 6 hours, taking out the foamed nickel after the reaction is finished, washing with water and alcohol, and drying at 60 ℃ for 12 hours to obtain NiCo NWs/NF.
Comparative example 2
Preparation of NiCo NWs/Co-MOF/NF electrocatalyst based on foam Nickel (NF):
0.60g of Co (NO) is weighed3)2·6H2O was dissolved in 20mL of methanol and stirred until a clear solution A was formed. 2.66g of 2-methylimidazole are weighed out and dissolved in 20mL of methanol and stirred until a clear solution B is formed. And pouring the solution B into the solution A, fully stirring to form a purple solution C, putting the NiCo NWs/NF into the solution C, standing for 12h, taking out the foamed nickel after the reaction is finished, washing with water and alcohol, and drying at 60 ℃ for 12h to obtain the NiCo NWs/Co-MOF/NF.
Comparative example 3
Preparation of Co-MOF/NF electrocatalyst based on foam Nickel (NF):
0.60g of Co (NO) is weighed3)2·6H2O was dissolved in 20mL of methanol and stirred until a clear solution A was formed. 2.66g of 2-methylimidazole are weighed out and dissolved in 20mL of methanol and stirred until a clear solution B is formed. And pouring the solution B into the solution A, fully stirring to form a purple solution C, putting the foamed nickel (2cm multiplied by 5cm) into the solution C, standing for 12h, taking out the foamed nickel after the reaction is finished, washing with water and alcohol, and drying at 60 ℃ for 12h to obtain Co-MOF/NF.
Comparative example 4
(Ni, Co) Se based on Nickel Foam (NF)2Preparation of NF electrocatalyst:
weighing0.5gSe powder is placed at the upstream of a semi-closed crucible, the NiCo NWs/NF is placed at the downstream of the semi-closed crucible, the crucible is transferred to an automatic program temperature control heating tube furnace, and the temperature is raised to 450 ℃ at the heating rate of 2 ℃/min to be calcined for 2 h; naturally cooling to room temperature, taking out to obtain (Ni, Co) Se2/NF。
Comparative example 5
CoSe based on Nickel Foam (NF)2Preparation of NF electrocatalyst:
weighing 0.5gSe powder, placing the powder on the upstream of a semi-closed crucible, placing the Co-MOF/NF on the downstream of the semi-closed crucible, transferring the crucible to a temperature-rising tubular furnace with automatic program temperature control, and rising the temperature to 450 ℃ at the temperature-rising rate of 2 ℃/min to calcine for 2 hours; naturally cooling to room temperature, taking out to obtain CoSe2/NF。
Example 1
(Ni, Co) Se based on Nickel Foam (NF)2/CoSe2Preparation of NF electrocatalyst:
weighing 0.5gSe powder, placing the powder on the upstream of a semi-closed crucible, placing the NiCo NWs/Co-MOF/NF on the downstream of the semi-closed crucible, transferring the crucible to an automatic program temperature control heating tube furnace, heating to 450 ℃ at a heating rate of 2 ℃/min, and calcining for 2 h; naturally cooling to room temperature, taking out to obtain (Ni, Co) Se2/CoSe2/NF。
Electrocatalytic activity experiment of nickel-cobalt double-metal selenide electrode material
KOH solution with the concentration of 1 mol per liter is used as electrolyte, a three-electrode reaction device is adopted, a platinum wire is used as a counter electrode, Hg/HgO is used as a reference electrode, the scanning speed is 5mV/s, and the electrocatalytic decomposition water performance of the nickel-cobalt double-metal selenide electrode material in the solution is tested.
EXAMPLES characterization analysis of Nickel cobalt Bi-Metal selenide catalysts
FIG. 1 shows the prepared (Ni, Co) Se2/CoSe2XRD diffraction pattern of/NF electrocatalyst, from which (Ni, Co) Se can be seen2/CoSe2The diffraction peaks in/NF correspond well to (Ni, Co) Se2Standard card of (PDF #29-1417), and CoSe2Standard card of/NF(PDF#89-2002)。
FIGS. 2a, b are prepared (Ni, Co) Se2/CoSe2Scanning electron micrographs of/NF electrocatalyst, (Ni, Co) Se can be seen in FIGS. 2a, b2/CoSe2the/NF is a closely arranged nano array structure; FIG. 2c and d are (Ni, Co) Se2/CoSe2The transmission electron microscope photo of the/NF electrocatalyst shows that the thickness of the nano sheet is thinned after nitridation and small particles are arranged on the surface of the nano sheet from the pictures of fig. 2c and d; FIG. 2e, f are CoMoNxTransmission Electron micrograph of-500 NSAs/NF electrocatalyst
FIGS. 3a and b are respectively prepared (Ni, Co) Se2/CoSe2Comparative plots of polarization curves for hydrogen evolution and oxygen evolution reactions under 1M KOH for NF and a series of comparative electrocatalysts. From the figure, it can be seen that (Ni, Co) Se2/CoSe2The best performance is/NF, the current density is 10mA cm-2The corresponding hydrogen evolution and oxygen evolution overpotentials were 65mV and 255mV, respectively.
FIGS. 4a and b are respectively prepared (Ni, Co) Se2/CoSe2Comparative plot of the TfServ curves for hydrogen evolution and oxygen evolution reactions under 1M KOH for NF and a series of comparative electrocatalysts. From the figure, (Ni, Co) Se2/CoSe2the/NF electrocatalyst has a specific (Ni, Co) Se ratio2/NF、CoSe2Smaller Tafel slopes of/NF, NiCo NWs/Co-MOF/NF, NiCo NWs/NF, and Co-MOF/NF.
Claims (10)
1. A preparation method of a nickel-cobalt bimetallic selenide heterostructure electrocatalyst is characterized by comprising the following steps:
(1) cleaning the foamed nickel, and drying for later use;
(2) preparing a nickel-cobalt nanowire precursor with foam Nickel (NF) as a substrate, namely NiCo NWs/NF;
weighing Ni (NO)3)2·6H2O、Co(NO3)2·6H2Adding deionized water, dissolving completely to obtain a precursor solution, and placing the precursor solution in a reaction kettle; then immersing the foamed nickel cleaned in the step (1) in the precursor solution, transferring the reaction kettle to an oven for hydrothermal reaction, and finishing the reactionTaking out the foamed nickel, washing with water and alcohol, and vacuum drying overnight;
(3) preparing NiCo NWs/Co-MOF/NF with foamed Nickel (NF) as a substrate;
weighing Co (NO)3)2·6H2Adding methanol into O and 2-methylimidazole respectively, dissolving, stirring to obtain a mixed solution, placing the NiCo NWs/NF prepared in the step (2) into the solution, standing, taking out, washing with water, washing with alcohol, and drying overnight in vacuum to obtain a precursor, namely NiCo NWs/Co-MOF/NF;
(4) preparation of foamed Nickel (NF) -based (Ni, Co) Se2/CoSe2/NF；
Placing the NiCo NWs/Co-MOF/NF prepared in the step (3) into an open porcelain boat, transferring the porcelain boat into a temperature rising tube furnace with automatic program temperature control, and putting the porcelain boat into an N2Calcining in atmosphere, naturally cooling to room temperature after calcining, and taking out to obtain the nickel-cobalt bimetallic selenide heterostructure electrocatalyst, namely (Ni, Co) Se2/CoSe2/NF。
2. The method of preparing a nickel cobalt bimetallic selenide heterostructure electrocatalyst according to claim 1, wherein in step (1), the cleaning nickel foam is: and ultrasonically cleaning the commercial foamed nickel by using hydrochloric acid, acetone, ethanol and deionized water in sequence.
3. The method of preparing a nickel cobalt bimetallic selenide heterostructure electrocatalyst according to claim 1, in which in step (2), Ni (NO)3)2·6H2O、Co(NO3)2·6H2The molar ratio of O is 1: 2, in the precursor solution, Ni (NO)3)2·6H2The concentration of O is 0.017 mol.L-1，Co(NO3)2·6H2The concentration of O is 0.033 mol. L-1。
4. The method of preparing a nickel cobalt bimetallic selenide heterostructure electrocatalyst according to claim 1, wherein in step (2), the dimensions of the nickel foam are 2cm x 5 cm; the temperature of the hydrothermal reaction is 100 ℃, and the reaction time is 6 h.
5. The method of preparing a nickel cobalt double metal selenide heterostructure electrocatalyst according to claim 1, wherein in step (3), in the mixed solution, Co (NO) is present3)2·6H2The concentration of O is 0.052 mol.L-1The concentration of 2-methylimidazole is 0.810 mol.L-1。
6. The method of preparing a nickel cobalt bimetallic selenide heterostructure electrocatalyst according to claim 1, in which in step (3) the resting time is 12 h.
7. The method of preparing a nickel cobalt bimetallic selenide heterostructure electrocatalyst according to claim 1, wherein in step (4), the temperature rise rate is 2 ℃/min, the calcination temperature is 450 ℃, and the calcination time is 2 h.
8. The method of preparing a nickel cobalt bimetallic selenide heterostructure electrocatalyst according to claim 1, wherein the drying temperature in steps (1), (2) and (3) is 60 ℃ and the drying time is 12 h.
9. A nickel-cobalt bimetallic selenide heterostructure electrocatalyst, characterized in that it is prepared by the preparation method of any one of claims 1 to 8.
10. The application of the nickel-cobalt double-metal selenide heterostructure electrocatalyst synthesized by the synthesis method according to any one of claims 1 to 8 in electrocatalytic full-hydrolysis under alkaline conditions.
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