CN114606512B - Ru doped W 4.6 N 4 Particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst - Google Patents
Ru doped W 4.6 N 4 Particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst Download PDFInfo
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- CN114606512B CN114606512B CN202210333124.6A CN202210333124A CN114606512B CN 114606512 B CN114606512 B CN 114606512B CN 202210333124 A CN202210333124 A CN 202210333124A CN 114606512 B CN114606512 B CN 114606512B
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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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- 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
- C25B11/065—Carbon
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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
- C25B11/073—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 invention discloses a Ru doped W 4.6 N 4 Particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst. Ru-doped WO is grown in situ on a nitrogen-doped graphene tube carrier by a hydrothermal method x Heating the precursor to 700 ℃ in a tube furnace, introducing ammonia gas, nitriding for 2 hours to obtain the nitrogen-doped graphene tube and Ru-doped W grown on the surface of the nitrogen-doped graphene tube in situ 4.6 N 4 Nanoparticle-composed hydrogen evolution electrocatalyst. W is doped based on Ru 4.6 N 4 The electrocatalyst has excellent electrocatalytic activity and stability in alkaline medium, and has the synergistic effect of effective regulation and control of electronic structure, good conductivity of nitrogen doped graphene tube carrier and the like.
Description
Technical Field
The invention belongs to the field of electrocatalytic water splitting, and particularly relates to a Ru-doped W 4.6 N 4 Particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst and preparation method thereof.
Background
Hydrogen energy is an important component of the energy system of future countries. According to the production mode of hydrogen, the method can be divided into three types of ash hydrogen, blue hydrogen and green hydrogen, which respectively refer to fossil energy hydrogen production, fossil energy hydrogen production provided with carbon dioxide trapping and sealing facilities and renewable energy water electrolysis hydrogen production. According to the plan, the country gradually increases the green hydrogen ratio of the hydrogen production by water electrolysis. The hydrogen production by electrolysis of water involves two half reactions: both cathodic Hydrogen Evolution (HER) and anodic Oxygen Evolution (OER) reactions are achieved depending on highly efficient electrocatalysts. To date, pt-and Ir/Ru-oxide based catalysts have remained considered ideal electrocatalysts for HER and OER. However, their large-scale commercial application is hampered by the expensive cost and relatively low reserves. Therefore, developing a catalyst for hydrogen production by water electrolysis which is low in cost, efficient and stable becomes a key for reducing the hydrogen production cost.
Transition metal nitrides, by virtue of their low electrical resistance, broad d-band, excellent corrosion resistance and good mechanical strength, are becoming ideal materials for hydrogen evolution electrocatalysts, such as single metal nitrides (CoN, ni 3 N, etc.), bimetallic nitrides (CoFeN, niMoN, etc.). Doping proves to be a strategy for effectively improving the performance of the catalyst, and hetero atoms are introduced into the transition metal nitride crystal lattice, so that the electronic structure of the main catalyst can be accurately regulated and controlled, thereby optimizing the adsorption and desorption behaviors of intermediates in the reaction process, and further improving the catalytic activity of the transition metal nitride. Ceng et al successfully synthesized a ruthenium doped bimetallic phosphide catalyst (Ru-NiCoP) by a multi-step hydrothermal reaction, ion exchange and phosphating process, showing excellent hydrogen and oxygen evolution properties (Cen J, shen P K, zeng Y., J Colloid Interface Sci.,2022, 610:213-20). In addition, in order to improve the overall conductivity of the catalyst, it is an effective method to introduce a carbon material having excellent conductivity as a skeleton. The carbon material skeleton can avoid the agglomeration of active components in the catalytic process, and increase the exposed active sites, thereby improving the catalytic activity.
According to the invention, the nitrogen-doped graphene tube with excellent conductivity is used as a carrier, and the nitrogen-doped graphene tube and Ru-doped W grown on the surface of the nitrogen-doped graphene tube in situ are prepared by a hydrothermal nitriding method 4.6 N 4 Nanoparticle-composed hydrogen evolution electrocatalyst. The catalyst shows high-efficiency and stable electrocatalytic activity in alkaline medium, and generates 10mA cm -2 Only 38mV overpotential was required and exhibited excellent stability.
Disclosure of Invention
The invention aims to provide a nitrogen-doped graphene tube and Ru-doped W grown on the surface of the nitrogen-doped graphene tube in situ 4.6 N 4 Nanoparticle-composed hydrogen evolution electrocatalyst. The specific invention comprises the following steps:
1. the nitrogen-doped graphene tube is used as a carrier, and the nitrogen-doped graphene tube and Ru-doped W grown on the surface of the nitrogen-doped graphene tube in situ are obtained through a hydrothermal nitridation method 4.6 N 4 The hydrogen evolution electrocatalyst composed of the nano particles is prepared by the following method:
(1) The concentration was set to 0.72 mmol/l -1 Ammonium tungstate aqueous solution with concentration of 4.8-28.4 mmol.l -1 Mixing the two solutions according to the volume ratio of 5:1, and transferring to the reactionImmersing a nitrogen-doped graphene tube growing on a graphite sheet in a reaction kettle at the same time, performing hydrothermal reaction at a reaction temperature of 200 ℃ for 2 hours, washing and drying the product to obtain Ru-doped WO loaded on the nitrogen-doped graphene tube x A precursor;
(2) Placing the product obtained in the step (1) into a tubular furnace, heating to 700 ℃ in an argon atmosphere, closing argon, introducing ammonia gas for 2 hours at the set temperature, and cooling to room temperature to obtain the Ru-doped W 4.6 N 4 Hydrogen evolution electrocatalyst of nitrogen doped graphene tubes.
2. The Ru is doped with W 4.6 N 4 The hydrogen evolution electrocatalyst of the @ nitrogen-doped graphene tube shows excellent hydrogen evolution performance in alkaline medium, and can reach 10mA cm only by using 38mV overpotential -2 And exhibits excellent stability.
The invention discloses a Ru doped W 4.6 N 4 Compared with the prior art, the hydrogen evolution electrocatalyst of the nitrogen doped graphene tube has the advantages that:
(1) Heterogeneous atom Ru is introduced into the electrocatalyst to accurately regulate and control host material W 4.6 N 4 Thereby optimizing the adsorption and desorption actions of the intermediate in the reaction process and further improving the activity of the catalyst;
(2) The nitrogen doped graphene tube with excellent conductivity is introduced as a carrier, so that the overall conductivity of the catalyst can be improved, agglomeration of active ingredients in the catalytic process can be avoided, and exposed active sites can be increased, and the hydrogen evolution performance is improved.
Drawings
FIG. 1 shows Ru-doped W obtained in example 1 4.6 N 4 SEM photograph of hydrogen evolution electrocatalyst of @ nitrogen doped graphene tube, (a) 1 μm, (b) 500nm;
FIG. 2 shows Ru-doped W obtained in example 1 4.6 N 4 (a) a TEM photograph of a nitrogen doped graphene tube hydrogen evolution electrocatalyst, (b) a HRTEM photograph;
FIG. 3 shows the Ru-doped W obtained in example 1 4.6 N 4 Hydrogen evolution of @ nitrogen doped graphene tubeXRD spectrum of electrocatalyst;
FIG. 4 shows the Ru-doped W obtained in example 1 4.6 N 4 XPS spectrum of hydrogen evolution electrocatalyst of nitrogen doped graphene tube, (a) W4 f spectrum, (b) N1 s spectrum, and (c) Ru 3p spectrum;
FIG. 5 shows the Ru-doped W obtained in example 1 4.6 N 4 Hydrogen evolution reaction performance diagram of hydrogen evolution electrocatalyst of nitrogen doped graphene tube in 1mol/L KOH solution, (a) LSV graph, (b) Tafel slope diagram, and (c) stability test diagram.
Detailed Description
The present invention is described in further detail below in connection with specific examples, which, however, do not limit the scope of the invention in any way.
Example 1
Ru-doped W according to the present embodiment 4.6 N 4 The preparation method of the hydrogen evolution electrocatalyst of the @ nitrogen-doped graphene tube comprises the following steps:
(1) The concentration was set to 0.72 mmol/l -1 Ammonium tungstate aqueous solution with concentration of 24 mmol.l -1 Mixing the two solutions according to the volume ratio of 5:1, transferring into a reaction kettle, immersing a nitrogen-doped graphene tube growing on a graphite sheet into the reaction kettle, performing hydrothermal reaction at the reaction temperature of 200 ℃ for 2 hours, washing and drying the product to obtain Ru-doped WO loaded on the nitrogen-doped graphene tube x A precursor;
(2) Placing the product obtained in the step (1) into a tubular furnace, heating to 700 ℃ in an argon atmosphere, closing argon, introducing ammonia gas for 2 hours at the set temperature, and cooling to room temperature to obtain the Ru-doped W 4.6 N 4 Hydrogen evolution electrocatalyst of nitrogen doped graphene tubes.
From SEM pictures of different magnifications of FIGS. 1 (a), (b) in the drawings of the specification, it can be seen that the support material is uniformly tubular with a diameter of 150-200 nm and Ru doped with W 4.6 N 4 Is granular and uniformly anchored on the surface of the nitrogen-doped graphene tube. As is clear from the TEM photograph of FIG. 2 (a), ru-W 4.6 N 4 The particle size is 5-10 nm; from the HRTEM photograph of FIG. 2 (b), it is clear that two kinds of stripes having different interplanar spacings d are observed, wherein a lattice stripe having a d value of 0.208nm corresponds to W 4.6 N 4 The (104) crystal face of the graphene, the lattice fringes with d value of 0.370nm correspond to the (002) crystal face of the graphene, and the result proves that the catalyst Ru is doped with W 4.6 N 4 Successful preparation of @ nitrogen doped graphene tubes. The XRD patterns are shown in figure 3, and the characteristic peaks at 35.2 degrees, 36.3 degrees, 46.9 degrees and 64.4 degrees are matched with W 4.6 N 4 The (0 00 6), (1 0 1), (1 0 5) and (1 1 0) crystal planes are identical (JCDF # 77-2001). The XPS spectra of FIGS. 4 (a), (b) and (c) characterize the surface composition and chemical valence of the hydrogen evolution electrocatalyst, which can confirm the successful incorporation of Ru element into W 4.6 N 4 Is a kind of medium.
The electrocatalytic performance test of the product adopts a three-electrode system, and is loaded with the Ru doped W 4.6 N 4 The graphite sheet of the @ nitrogen-doped graphene tube electrocatalyst is used as a working electrode, a Pt electrode (oxygen evolution reaction), a graphite electrode (hydrogen evolution reaction) is used as a counter electrode, a Hg/HgO electrode is used as a reference electrode, a KOH aqueous solution of 1mol/L is used as an electrolyte, and a CHI 760E electrochemical workstation is used for testing the catalytic activity and stability of the hydrogen evolution reaction of the product. FIG. 5 (a), (b) and (c) are the Ru-doped W catalysts prepared according to this example 4.6 N 4 Performance graph of @ nitrogen doped graphene tube for electrocatalytic decomposition water hydrogen evolution reaction, from which it can be seen that the catalyst has a current density of 10mA cm -2 At the time of hydrogen evolution reaction, the overpotential was 38mV and the Tafel slope was 43mV dec -1 And at 10mA cm -2 The lower part can be kept for 28 hours without obvious change of current density, which shows that the catalyst has good hydrogen evolution stability.
Claims (4)
1. Ru doped W 4.6 N 4 The particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst is characterized in that a Ru doped W formed by nitrogen doped graphene tube and in-situ grown on the surface of the nitrogen doped graphene tube is obtained by a hydrothermal nitridation method 4.6 N 4 Nanoparticle-composed hydrogen evolution electrocatalyst, characterized by being prepared by the following method：
(1) The concentration was set to 0.72 mmol/l -1 Mixing the ammonium tungstate aqueous solution and the ruthenium trichloride aqueous solution with set concentration according to the volume ratio of 5:1, transferring the mixed solution to a reaction kettle, immersing a nitrogen-doped graphene tube growing on a graphite sheet into the reaction kettle for hydrothermal reaction at the reaction temperature of 200 ℃ for 2 hours, and washing and drying the product to obtain Ru-doped WO loaded on the nitrogen-doped graphene tube x A precursor;
(2) Placing the product obtained in the step (1) into a tubular furnace, heating to a set temperature in an argon atmosphere, closing argon, introducing ammonia at the set temperature for a certain time, and cooling to room temperature to obtain the Ru-doped W 4.6 N 4 Particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst.
2. A Ru-doped W as claimed in claim 1 4.6 N 4 The particle @ nitrogen doped graphene tube hydrogen evolution electrocatalyst is characterized in that RuCl used in the step (1) is 3 The concentration of (C) is 4.8-28.4 mmol.l -1 。
3. A Ru-doped W as claimed in claim 1 4.6 N 4 The particle@nitrogen doped graphene tube hydrogen evolution electrocatalyst is characterized in that the heating rate in the step (2) is 5 ℃/min, the set temperature is 700 ℃, and the ammonia gas inlet time is 2 hours.
4. A Ru-doped W as claimed in claim 1 4.6 N 4 The particle@nitrogen doped graphene tube hydrogen evolution electrocatalyst is characterized in that the electrocatalyst shows excellent hydrogen evolution performance in alkaline medium, and can reach 10mA cm only by 38mV overpotential -2 Is characterized by a Tafel slope of 43mV dec -1 And at 10mA cm -2 Is maintained for 28 hours without obvious change of current density, and shows good stability.
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