CN114836788B - N-Ni/N-CeO 2 Preparation method and application of nickel electrode - Google Patents
N-Ni/N-CeO 2 Preparation method and application of nickel electrode Download PDFInfo
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- CN114836788B CN114836788B CN202210491494.2A CN202210491494A CN114836788B CN 114836788 B CN114836788 B CN 114836788B CN 202210491494 A CN202210491494 A CN 202210491494A CN 114836788 B CN114836788 B CN 114836788B
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- C—CHEMISTRY; METALLURGY
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- 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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- C—CHEMISTRY; METALLURGY
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The application discloses a preparation method and application of an N-Ni/N-CeO 2/nickel electrode. A nitrogen-containing Ce-metal organic framework (Ce-MOF) is grown on foam Nickel (NF) by an in-situ growth mode, and then an N-Ni/N-CeO 2/nickel electrode self-supporting electrode is constructed by pyrolysis. According to the application, the N element is doped into the lattices of the metal Ni and CeO2 composing the Ni/CeO2 heterojunction for the first time so as to remarkably improve the electrocatalytic activity. The N-Ni/N-CeO2/NF can drive 100 and 500 mA cm < -2 > full hydrolysis current density in 1.0M KOH electrolyte only by 1.672V and 1.991V respectively, and the catalytic performance of the electrolytic water device is higher than that of a commercial noble metal Pt/C-RuO2 assembled, thus the electrolytic water device has potential industrial application value.
Description
Technical Field
The application relates to the field of inorganic synthesis and energy catalysis, in particular to a nitrogen (N) -doped Ni/CeO 2 Heterojunction (N-Ni/N-CeO) 2 ) Self-supporting electricityPolar material (N-Ni/N-CeO) 2 Nickel electrode) and its application in electrocatalytic full water splitting.
Background
Electrocatalytic water splitting to produce hydrogen can alleviate the current energy crisis and environmental problems, and is thus widely studied. However, the efficiency of water splitting is limited by the high overpotential of Hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER). The development of highly efficient electrocatalysts is critical to promote the widespread use of this energy conversion technology. Currently, commercial HER and OER catalysts are predominantly Pt, ru, ir and their compounds. However, the high cost of such noble metals limits their further large scale application. Thus, there is a great interest in preparing highly active non-noble metal electrocatalysts.
Non-noble metal electrocatalysts have been reported to include mainly transition metals, metal oxides, metal hydroxides, metal phosphides, metal sulfides, metal selenides, metal nitrides, and the like. Among them, metallic Ni has the advantage of being inexpensive and readily available and is being widely studied. However, the poor intrinsic activity and stability limit the further development of metallic Ni.
Disclosure of Invention
Recent researches show that on one hand, the heterostructure has the advantages of promoting electron transfer, increasing active surface area, optimizing adsorption/desorption energy of an electrocatalytic intermediate and the like, so that the catalytic activity is improved. CeO (CeO) 2 Has excellent oxidation-reduction characteristics, excellent ionic conductivity and oxygen-enriched vacancies, and is a good auxiliary accelerator for electrocatalysis. Thus, ni/CeO was constructed 2 The heterojunction can remarkably improve the electrocatalytic activity of the metal Ni. On the other hand, doping N element into the metal Ni crystal lattice can not only regulate the electronic structure of the catalytic center, but also enrich the active site of the catalyst, thereby further improving the catalytic property of the metal Ni. In addition, the catalyst is directly grown on the foam Nickel (NF) in situ, so that not only can expensive conductive polymer adhesive be avoided, but also abundant active sites can be exposed, and the catalyst has more excellent electrocatalytic activity and stability. The application synthesizes the N-Ni/N-CeO 2 Heterostructure and for the first timeN element is doped into metal Ni and CeO simultaneously 2 To significantly enhance its electrocatalytic activity. Synthesized self-supporting electrode N-Ni/N-CeO 2 The NF can drive 100 and 500 mA cm in 1.0M KOH electrolyte with low voltages of 1.672V and 1.991V respectively -2 The full hydrolysis current density of (C) has catalytic performance exceeding that of commercial noble metal Pt/C-RuO 2 The assembled water electrolysis device has potential industrial application value. The reason for the high activity can be attributed to (1) N-Ni/N-CeO 2 The heterojunction promotes charge transfer and optimizes the electronic structure of the Ni center; (2) N doping can further tune the electronic configuration of Ni and enrich the active sites of the catalyst. The inventors of the present application summarized the following technical scheme.
The application provides an N-Ni/N-CeO 2 A method of preparing a nickel electrode, the method comprising the steps of:
dissolving cerium salt and an organic ligand in water and N, N-Dimethylformamide (DMF), respectively, and stirring for a period of time to form a mixed solution;
transferring the mixed solution into a reaction kettle and placing a nickel electrode;
sealing the reaction kettle and reacting for a period of time at 80-120 ℃ to obtain a Ce-MOF/nickel electrode precursor;
placing the Ce-MOF/nickel electrode precursor in a tube furnace at 5% H 2 Pyrolyzing the precursor for a period of time under the flow rate of/Ar to obtain the N-Ni/N-CeO 2 Nickel electrode.
Further, the cerium salt is Ce (NH) 4 ) 2 (NO 3 ) 6 The organic ligand is 5-amino isophthalic acid and 1,3, 5-trimesic acid.
Further, the nickel material is foam nickel.
Further, the reaction kettle is sealed and reacts at the temperature of 80-120 ℃ for 15-120 min, preferably 30-60 min, more preferably 45 min.
Further, the pyrolysis temperature is 500-700 ℃, preferably 600 ℃.
Further, the pyrolysis time is 1-4 h.
Further, the stirring time is 30 min.
The application also provides the Ni/CeO containing catalyst 2 The use of/NF electrodes in electrocatalytic full water splitting reactions, namely electrocatalytic Hydrogen Evolution Reactions (HER) and Oxygen Evolution Reactions (OER) and other electrocatalytic energy conversion technologies.
Compared with the prior art, the application has the following beneficial effects:
(1) The N-Ni/N-CeO 2 The preparation method of the NF self-supporting electrode is simple, the raw materials are cheap and easy to obtain, the preparation time is short, and expensive conductive adhesives are not needed;
(2) The N-Ni/N-CeO 2 The preparation method of the/NF not only can prepare a heterostructure, but also can dope N element into metal Ni and CeO simultaneously 2 Thereby significantly enhancing the catalytic activity of the catalyst;
(3) The N-Ni/N-CeO 2 the/NF electrode shows excellent full-water decomposition catalytic performance, and can drive 100 and 500 mA cm in 1.0M KOH electrolyte only by low overpotential of 1.672V and 1.991V respectively -2 The catalytic performance of the catalyst exceeds the reference Pt/C and RuO in the prior art 2 The combined full hydrolysis system has potential industrial application value.
Drawings
FIG. 1 is a diagram of N-Ni/N-CeO according to the present application 2 X-ray powder diffraction pattern of/NF.
FIG. 2 is a diagram of N-Ni/N-CeO according to the present application 2 Scanning electron microscopy of/NF.
FIG. 3 is a diagram of N-Ni/N-CeO according to the present application 2 Transmission electron microscopy/NF.
FIG. 4 is a diagram of N-Ni/N-CeO according to the present application 2 Raman plot of/NF.
FIG. 5 is a diagram of N-Ni/N-CeO according to the present application 2 X-ray photoelectron spectroscopy (XPS) of NF.
FIG. 6 is a diagram of N-Ni/N-CeO according to the present application 2 /NF、Ni/CeO 2 HER linear sweep voltammetry plots of/NF, 20% @ Pt/C@NF and NF.
FIG. 7 is a diagram of N-Ni/N-CeO according to the present application 2 /NF、Ni/CeO 2 /NF、RuO 2 OER linear sweep voltammetry plots at NF and NF.
FIG. 8 is a diagram of N-Ni/N-CeO according to the present application 2 Linear sweep voltammetry graph of the total hydrolysis reaction of NF and noble metal catalyst.
FIG. 9 is a diagram of N-Ni/N-CeO according to the present application 2 /NF、Ni/CeO 2 HER tafel plot of/NF and 20% @ Pt/c@nf.
FIG. 10 shows N-Ni/N-CeO according to the present application 2 /NF、Ni/CeO 2 NF and RuO 2 OER tafel plot at NF.
FIG. 11 is a diagram of N-Ni/N-CeO according to the present application 2 /NF、Ni/CeO 2 HER electrochemical impedance spectra of/NF and NF.
FIG. 12 is a diagram of N-Ni/N-CeO according to the present application 2 /NF、Ni/CeO 2 OER electrochemical impedance spectra of/NF and NF.
FIG. 13 is a diagram of N-Ni/N-CeO according to the present application 2 The NF is respectively 10 and 100 mA cm -2 HER constant current electrolysis plot at current density.
FIG. 14 is a diagram of N-Ni/N-CeO according to the present application 2 The NF is respectively 10 and 100 mA cm -2 OER constant current electrolysis plot at current density.
Description of the embodiments
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this application belongs.
In the application, firstly, a certain amount of 0.5M tetravalent cerium salt water solution and DMF solution of organic ligand are respectively added, stirred for a period of time, transferred to a reaction kettle, added with nickel material with certain specification, reacted for a period of time at a certain temperature, and the nickel material with Ce-MOF grown is taken outDrying, carbonizing at a certain temperature to obtain N-Ni/N-CeO 2 Nickel electrode.
In particular embodiments, the method of the present application may comprise the steps of: washing NF with 1M hydrochloric acid solution to remove surface oxide and impurities, and preparing Ce (NH) 4 ) 2 (NO 3 ) 6 Aqueous solution and 5-aminoisophthalic acid (5-AIPI), 1,3, 5-benzenetricarboxylic acid (H) 3 BTC), mixing uniformly, placing the cleaned NF in the solution, reacting for a period of time at a certain temperature, drying the nickel material with Ce-MOF, and finally carbonizing to obtain CeO 2 A NF self-supporting electrode.
Example 1: N-Ni/N-CeO 2 Preparation of self-supporting NF electrode
Ultrasonic cleaning NF (thickness: 1.7. 1.7 mm) in acetone, 1.0. 1.0M hydrochloric acid solution and ultrapure water for 30 minutes; next, the prepared 0.5M Ce (NH) 4 ) 2 (NO 3 ) 6 Aqueous solution and 0.16M H 3 Mixing BTC and 5-AIPI uniformly; then placing the cleaned NF in a uniform solution, transferring the solution into a reaction kettle, and reacting for 45 min at 100 ℃; finally, carbonizing NF with Ce-MOF to obtain N-Ni/N-CeO 2 An X-ray diffraction diagram of the product of the NF self-supporting electrode is shown in figure 1; scanning electron microscopy is shown in figure 2; the transmission electron microscope image is shown in FIG. 3, illustrating N-Ni/N-CeO 2 Is a heterojunction structure. FIG. 4 is a Raman diagram of the product, and analysis shows that N element is doped with CeO 2 The method comprises the steps of carrying out a first treatment on the surface of the FIG. 5 is an XPS diagram of a product in which a high resolution XPS diagram of N reveals the presence of Ni-N bonds and Ce-N bonds in the catalyst, confirming that the N element is doped with Ni and CeO 2 Is defined in the crystal lattice of (a).
Example 2: N-Ni/N-CeO obtained in example 1 2 Electrocatalytic HER performance test of/NF
N-Ni/N-CeO obtained in example 1 2 Electrocatalytic HER performance testing of/NF was performed on the CHI760E electrochemical workstation. The electrolyte was a 1.0M KOH aqueous solution. Using N-Ni/N-CeO 2 the/NF, hg/HgO and Pt plates were used as the working, reference and counter electrodes, respectively. The linear sweep voltammetry graph shown in FIG. 6 is at 5.0Obtained at the scanning speed of mV/s, N-Ni/N-CeO is shown in FIG. 6 2 NF drive 100 and 500 mA cm -2 The overpotential required for the current density is 142 and 290 mV, respectively. The Taphillips plot shown in FIG. 9 is calculated from FIG. 6, and it can be seen that N-Ni/N-CeO 2 Tafil slope of/NF 93 mV-dec -1 . FIG. 13 shows a constant voltage electrolytic diagram of N-Ni/N-CeO control, respectively 2 The NF is 10, 100 mA cm -2 45-h by electrolysis under current density, N-Ni/N-CeO 2 the/NF maintains good catalytic stability at different current densities.
Example 3: N-Ni/N-CeO obtained in example 1 2 Electrocatalytic OER Performance test of/NF
N-Ni/N-CeO obtained in example 1 2 Electrocatalytic OER performance testing of/NF was performed on the CHI760E electrochemical workstation. The electrolyte was a 1.0M KOH aqueous solution. Using N-Ni/N-CeO 2 the/NF, hg/HgO and Pt plates were used as the working, reference and counter electrodes, respectively. The linear sweep voltammetry graph of FIG. 7 was obtained at a sweep rate of 10 mV/s, where N-Ni/N-CeO is known 2 NF drive 100 and 500 mA cm -2 The overpotential required for the current density is 323 and 388 mV, respectively. The Taphillips plot shown in FIG. 10 is calculated from FIG. 6, and it can be seen that N-Ni/N-CeO 2 Tafil slope of/NF was 82 mV. Dec -1 . FIG. 14 shows a constant voltage electrolytic diagram of N-Ni/N-CeO control, respectively 2 The NF is 10, 100 mA cm -2 45 h by electrolysis at a current density, from which N-Ni/N-CeO can be seen 2 the/NF maintains good catalytic stability at different current densities.
Example 4: N-Ni/N-CeO obtained in example 1 2 Electrocatalytic full water splitting performance test of/NF
N-Ni/N-CeO obtained in example 1 2 Electrocatalytic full water splitting performance testing of/NF was performed on the CHI760E electrochemical workstation. The electrolyte is 1.0M KOH aqueous solution, N-Ni/N-CeO are respectively added 2 the/NF is carried out as anode and cathode. The linear sweep voltammetry graph shown in FIG. 8 was obtained at a sweep rate of 10 mV/s, and N-Ni/N-CeO is shown in FIG. 8 2 NF drive 100 and 500 mA cm -2 The overpotential required for the current density is 1.672V and 1.992V, respectively，N-Ni/N-CeO 2 The overpotential required for/NF-driven total water splitting is lower than that required for noble metals Pt-C and RuO 2 An electrocatalytic full water splitting device as an assembly of cathode and anode catalysts.
EXAMPLE 5N-Ni/N-CeO obtained in example 1 2 Electrochemical impedance spectroscopy/NF test
Electrochemical Impedance Spectroscopy (EIS) measurements were performed at a frequency range of 0.5 Hz to 100 kHz. The electrochemical impedance spectrum is shown in FIG. 11 and FIG. 12, and illustrates N-Ni/N-CeO 2 the/NF catalyst has good conductivity.
Comparative example 1: n-free Ni/CeO 2 Preparation of self-supporting NF electrode
Ultrasonic cleaning NF (thickness: 1.7. 1.7 mm) in acetone, 1.0. 1.0M hydrochloric acid solution and ultrapure water for 30 minutes; next, the prepared 0.5M Ce (NH) 4 ) 2 (NO 3 ) 6 Aqueous solution and 0.16M H 3 Uniformly mixing DMF solution of BTC; then placing the cleaned NF in a uniform solution, transferring the solution into a reaction kettle, and reacting for 45 min at 100 ℃; finally, carbonizing the foam nickel with the Ce-MOF to obtain Ni/CeO without N 2 A NF self-supporting electrode.
Comparative example 2: comparative example 1 Ni/CeO 2 Electrocatalytic HER performance test of/NF
Comparative example 1 different Ni/CeO 2 Electrocatalytic HER performance testing of/NF was performed on the CHI760E electrochemical workstation. The electrolyte was a 1.0M KOH aqueous solution. Using Ni/CeO 2 the/NF, hg/HgO and Pt plates were used as the working, reference and counter electrodes, respectively. The linear sweep voltammetry graph shown in FIG. 10 was obtained at a sweep rate of 10 mV/s, and it was found that N-Ni/N-CeO containing nitrogen 2 the/NF electrode has the best hydrogen evolution catalysis performance and is superior to Ni/CeO 2 HER catalytic performance of/NF.
Comparative example 3: comparative example 1 Ni/CeO 2 Electrocatalytic OER Performance test of/NF
Comparative example 1 Ni/CeO 2 Electrocatalytic OER performance testing of/NF was performed on the CHI760E electrochemical workstation. The electrolyte was a 1.0M KOH aqueous solution. Using Ni/CeO 2 the/NF, hg/HgO and Pt plates are respectively used as working electricityA pole, a reference electrode and a counter electrode. The linear sweep voltammetry graph shown in FIG. 11 was obtained at a sweep rate of 10 mV/s, indicating N-Ni/N-CeO containing nitrogen 2 the/NF electrode has the best oxygen evolution catalysis performance and is superior to Ni/CeO 2 OER catalytic performance of/NF.
The application loads CeO on NF by in-situ growth carbonization method 2 And carefully explore the N-doped p-N-Ni/N-CeO of hetero atoms 2 Influence of NF total water splitting performance. Benefiting from CeO 2 Heterojunction with Ni and N atom pair CeO 2 Regulating and controlling Ni to prepare N-Ni/N-CeO 2 The NF self-supporting electrode has excellent catalytic activity and good stability, and thus, shows excellent full-water decomposition electrocatalytic performance. N-Ni/N-CeO 2 The NF can drive 100, 500 mA cm in 1.0M KOH only by 1.672V and 1.992V overpotential respectively -2 Has potential industrial application value.
The above embodiments are only for illustrating the present application, not for limiting the present application, and various changes and modifications may be made by one of ordinary skill in the relevant art without departing from the spirit and scope of the present application, and therefore all equivalent technical solutions are also within the scope of the present application, which is defined by the claims.
Claims (6)
1. N-Ni/N-CeO 2 The preparation method of the nickel electrode comprises the following steps:
dissolving cerium salt and an organic ligand in water and N, N-Dimethylformamide (DMF), respectively, and stirring for a period of time to form a mixed solution;
transferring the mixed solution into a reaction kettle and placing a nickel electrode;
sealing the reaction kettle and reacting for a period of time at 80-120 ℃ to obtain a Ce-MOF/nickel electrode precursor;
placing the Ce-MOF/nickel electrode precursor in a tube furnace at 5% H 2 Pyrolyzing the precursor for a period of time under the flow rate of/Ar to obtain the N-Ni/N-CeO 2 Nickel electrode;
wherein the ceriumThe salt is Ce (NH) 4 ) 2 (NO 3 ) 6 The organic ligand is 5-amino isophthalic acid and 1,3, 5-trimesic acid, and the nickel electrode is foam nickel; the pyrolysis temperature is 500-700 ℃, and the pyrolysis time is 1-4 h.
2. The method according to claim 1, characterized in that: and sealing the reaction kettle and reacting for 15-120 min at the temperature of 80-120 ℃.
3. The method according to claim 1, characterized in that: the stirring time is 30 min.
4. An N-Ni/N-CeO obtained by the method according to any one of claims 1 to 3 2 Nickel electrode, characterized in that: the N-Ni/N-CeO 2 Is of a heterojunction structure, and N element is doped with metal Ni and CeO simultaneously 2 Is defined in the crystal lattice of (a).
5. The N-Ni/N-CeO according to claim 4 2 Use of nickel electrodes in the field of electrocatalysis.
6. The use according to claim 5, characterized in that: the N-Ni/N-CeO 2 The nickel electrode was used for the total water splitting reaction.
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| CN113005476A (en) * | 2021-02-06 | 2021-06-22 | 江西师范大学 | Preparation method and application of nickel hydroxide/nickel electrode |
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