CN113943949B - Platinum edge-modified nickel-based nano material and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a platinum edge modified nickel-based nano material and a preparation method and application thereof, belonging to the technical field of catalysts for hydrogen production by water electrolysis. The invention takes nickel nitrate as a precursor to prepare a two-dimensional nickel-based nano material, and adopts ethylene glycol as a reducing agent to obtain a composite material in which platinum nano particles are loaded to the edge of the two-dimensional nickel-based material in situ. In the composite material, the nickel-based two-dimensional nano material can adsorb oxygen/hydroxyl in a solution, the platinum nano particles can effectively adsorb hydrogen in water, meanwhile, the electro-catalytic hydrogen evolution reaction kinetics is accelerated, the electro-catalytic hydrogen production rate is accelerated, and the hydrogen production efficiency is improved. The invention also calculates the hydrogen evolution reaction path of the composite material through a density functional theory. The platinum edge modified nickel-based nano material provided by the invention can be used as a catalyst for hydrogen production by electrocatalytic decomposition of water, and the material has the advantages of simple preparation process, excellent catalytic performance and wide application prospect in the field of electrocatalytic hydrogen production.
Description
Technical Field
The invention belongs to the technical field of electrocatalytic water decomposition, and particularly relates to a platinum edge modified nickel-based nano material as well as a preparation method and application thereof.
Background
The hydrogen-oxygen fuel cell has the advantages of high energy conversion efficiency, high power density, good low-temperature performance, environmental friendliness and the like, and electrode reactions of the hydrogen-oxygen fuel cell comprise a cathode oxygen reduction reaction and an anode hydrogen oxidation reaction. Electrolytic hydrogen production is an important source of hydrogen gas, but it has a complex reaction path, a high activation energy barrier, which requires the use of catalysts to accelerate slow hydrogen evolution kinetics. The catalytic efficiency of the catalyst is closely related to the mechanism of the hydrogen evolution reaction. In an acidic medium, the mechanism of the hydrogen evolution reaction (H) + → c-H) only involve the adsorption and desorption reactions of hydrogen. The current research report shows that: hydrogen evolution from different metals in the same electrolyte solutionReactivity and hydrogen adsorption energy (. DELTA.G) H* ) There is a hill-shaped relationship curve, and the optimal catalytic activity appears in delta G H* Close to 0V, platinum (Pt) has an optimal electrocatalytic hydrogen evolution reaction activity. In an alkaline medium, hydrogen evolution reaction (H) 2 O+2e - →H 2 +2OH - ) Water molecules participate, and the catalytic mechanism of the method relates to the adsorption energy of hydrogen and hydroxyl. There are two views of the hydrogen evolution reaction mechanism in alkaline media: (1) The hydrogen evolution kinetics are only related to hydrogen adsorption energy, namely the hydrogen adsorption energy theory; (2) The kinetics of hydrogen evolution are related to the adsorption of hydrogen and hydroxyl groups, i.e. a bifunctional mechanism. At present, the law of the relationship between the hydrogen evolution reaction activity in alkaline media and the adsorption strength of electrode materials to hydrogen and hydroxyl groups is not clear. Under the background, an electrocatalytic material is urgently needed to be developed, the electrocatalytic hydrogen production efficiency is improved, meanwhile, the hydrogen production mechanism is researched, and theoretical and technical bases are laid for the design synthesis and the large-scale application of the hydrogen evolution battery catalyst which is efficient, stable and low in cost.
Disclosure of Invention
Aiming at the problems in the prior art, the first technical problem to be solved by the invention is to provide a platinum edge-modified nickel-based nanomaterial and a preparation method thereof. The second technical problem to be solved by the invention is to provide the application of the platinum edge modified nickel-based nanomaterial in the field of hydrogen production by electrocatalytic decomposition, and the platinum edge modified nickel-based nanomaterial has excellent electrocatalytic hydrogen production efficiency in the full pH value range. The third technical problem to be solved by the invention is to provide an electrolytic water reaction mechanism of the platinum edge modified nickel-based nano material under an alkaline condition.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a platinum edge modified nickel-based nano material comprises the following steps: respectively preparing a nickel nitrate aqueous solution and a urea aqueous solution, mixing, adding an ethylene glycol solution, adding into a reaction kettle, and preparing a nickel-based nano material by adopting a solvothermal method; and then respectively preparing the nickel-based nano material and a glycol solution of chloroplatinic acid, then mixing and uniformly stirring, heating in an oil bath, cooling, washing and drying the product to obtain the platinum edge modified nickel-based nano material.
Further, the mass ratio of the platinum to the nickel-based nano material in the chloroplatinic acid is 1-5wt.%.
Further, the preparation method of the platinum edge modified nickel-based nano material comprises the following steps:
(1) Respectively preparing a nickel nitrate aqueous solution and a urea aqueous solution;
(2) Mixing the nickel nitrate aqueous solution prepared in the step (1) with a urea aqueous solution;
(3) Adding the ethylene glycol solution into the mixed solution in the step (2), and stirring until the mixed solution is clear;
(4) And (4) placing the mixed solution obtained in the step (3) into a reaction kettle, carrying out solvothermal treatment for 12 hours at the temperature of 160 ℃, cooling to room temperature, washing with water and ethanol, and carrying out centrifugal drying to obtain the nickel-based nano material.
(5) Preparing the nickel-based nano material and chloroplatinic acid in the step (4) into glycol solutions respectively;
(6) Mixing the chloroplatinic acid solution prepared in the step (5) with a nickel-based nano material glycol solution, and forming a uniform precursor solution under the action of magnetic stirring and ultrasound;
(7) And (3) placing the precursor mixed solution in the step (6) into a round-bottom flask, heating and stirring for 2 hours under the condition of oil bath at 120 ℃, cooling to room temperature, washing with water and ethanol, and centrifugally drying to obtain the nickel-based nanomaterial with the platinum edge modified.
Further, the preparation method of the nickel nitrate aqueous solution comprises the following steps: 0.2900-0.3000g Ni (NO) 3 ) 2 ·6H 2 And adding O into 4mL of deionized water, and stirring at a high speed until the O is completely dissolved to obtain a nickel nitrate aqueous solution.
Further, the preparation method of the urea aqueous solution comprises the following steps: 0.3600-0.3610g urea is added into 4mL deionized water, and the mixture is stirred at high speed until the urea is completely dissolved, so that a urea water solution is obtained.
Further, the nickel nitrate aqueous solution, the urea aqueous solution and the glycol solution are mixed according to the volume ratio of 1: 7, and are placed in a reaction kettle for solvothermal reaction.
Further, the preparation method of the chloroplatinic acid ethylene glycol solution comprises the following steps: 0.77-0.79mL H 2 PtCl 6 (ρ Pt ：6.38-6.40mg mL -1 ) The solution is poured into 95mL of glycol solution and stirred evenly to obtain chloroplatinic acid glycol solution.
Further, the preparation method of the nickel-based nano material ethylene glycol solution comprises the following steps: and dissolving 95mg of nickel-based nano material into 95mL of glycol solution, and uniformly stirring to obtain the glycol solution of the nickel-based nano material.
Further, the preparation method of the precursor solution comprises the following steps: mixing the chloroplatinic acid glycol solution and the nickel-based nano material glycol solution, performing ultrasonic treatment for 90min, and stirring for 90min to obtain a precursor solution.
The platinum edge-modified nickel-based nano material prepared by any one of the preparation methods.
The platinum edge modified nickel-based nano material is applied as a catalyst in hydrogen production by electrolyzing water.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) According to the invention, nickel nitrate is used as a precursor to prepare the two-dimensional nickel-based nano material, ethylene glycol is used as a reducing agent, and the composite material with platinum nanoparticles loaded on the edge of the two-dimensional nickel-based material in situ is obtained by a preparation method under certain conditions, so that the platinum loading capacity in the composite material with the structure is greatly reduced, and higher hydrogen production catalytic benefit is realized at lower cost;
(2) The two-dimensional nickel-based nano material in the composite material can adsorb oxygen/hydroxyl and the like in a solution, so that the activation energy required by water decomposition is reduced, the platinum nano particles can effectively adsorb hydrogen in water, the electro-catalytic hydrogen evolution reaction kinetics is accelerated, the electro-catalytic hydrogen production rate is accelerated, and the high-efficiency hydrogen production is realized in the full pH range;
(3) The composite material disclosed by the invention is simple in preparation process, excellent in catalytic performance and wide in application prospect in the field of electrocatalytic hydrogen production.
Drawings
FIG. 1 is a structural representation diagram of the NHC-Pt-3 nanomaterial of the present invention: transmission electron micrograph of nanomaterial at 20nm (1 a); high resolution transmission electron microscopy images of nanomaterials at 5nm (1 b); EDS elemental map of nanomaterials including C, ni, O, pt (1C);
FIG. 2 is an X-ray photoelectron spectrum of (2 a) Ni 2p, (2 b) Pt 4f, (2C) C1 s and (2 d) O1 s in NHC-Pt-3, NHC and Pt/C materials of the present invention; pt L-edge (2 e) XANES and (2 f) EXAFS spectra of NHC-Pt-3 and Pt-foil materials;
FIG. 3 is the electrocatalytic hydrogen evolution performance test chart of different nanomaterials of the invention (3 a) in 1M KOH solution; (3 b) Tafel performance graphs of different materials; (3c) The different nanometer materials are 0.5M H 2 SO 4 An electrocatalytic hydrogen evolution performance test chart in the solution; (3d) Electrocatalytic hydrogen evolution performance test patterns of different nano materials in 1M PBS (phosphate buffer solution); (3e) Comparison of mass activity of different catalysts under 50mV conditions; (3f) The stability characterization chart of the NHC-Pt-3 catalyst in different solutions;
FIG. 4 shows the optimized hydroxyl radical adsorption of the present invention on (4 a) Ni (HCO) 3 ) 2 (001) Crystal plane, (4 b) NiO (111) crystal plane, (4 c) NOOH (001) crystal plane, (4 d) NiCoO (001) crystal plane and (4 e) Ni (OH) 2 (001) Crystal plane diagram, (4 f) is the mechanism diagram of hydrogen evolution reaction.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1: preparation and synthesis of platinum edge modified nickel-based nano material
A preparation method of a platinum edge-modified nickel-based nano material comprises the following steps:
(1) 0.2908gNi (NO) 3 ) 2 ·6H 2 And adding O into 4mL of deionized water, and stirring at a high speed until the O is completely dissolved to obtain a nickel nitrate aqueous solution.
(2) 0.3602g urea is added into 4mL deionized water and stirred at high speed until completely dissolved, thus obtaining a urea aqueous solution.
(3) Mixing the nickel nitrate aqueous solution, the urea aqueous solution and the glycol solution according to the volume of 4mL,4mL and 28mL, placing the mixture in a 50mL reaction kettle, carrying out solvothermal treatment for 12 hours at the temperature of 160 ℃, cooling the mixture to room temperature, washing the mixture with water and ethanol, and carrying out centrifugal drying to obtain the nickel-based nanomaterial.
(4) 0.78mL of H 2 PtCl 6 (ρ Pt ：6.39mg mL -1 ) The solution is poured into 95mL of glycol solution and is stirred uniformly to obtain chloroplatinic acid glycol solution.
(5) Dissolving 95mg of nickel-based nano material into 95mL of glycol solution, and uniformly stirring to obtain the nickel-based nano material glycol solution;
(6) And mixing the obtained chloroplatinic acid glycol solution and the nickel-based nano material glycol solution, performing ultrasonic treatment for 90min, and stirring for 90min to obtain a precursor solution.
(7) Adding the precursor solution into a 250mL round-bottom flask, stirring for 2h in an oil bath at 120 ℃, respectively centrifugally washing with ethanol and water for 6 times, and vacuum-drying at 60 ℃ to obtain a platinum-modified nickel-based nanomaterial with a Pt content of 5wt.%;
(8) The mass ratio of platinum to nickel-based nano material in the chloroplatinic acid ethylene glycol solution and the nickel nano material ethylene glycol solution is regulated to obtain 1wt.%,2wt.%,3wt.% and 5wt.% of platinum edge modification nickel-based nano material which is named as NHC-Pt-1, NHC-Pt-2, NHC-Pt-3 and NHC-Pt-5 respectively.
The platinum nanoparticles can be observed to be loaded on the edge of the two-dimensional nickel-based nano material through a transmission electron microscope; the elements such as platinum, nickel, oxygen and the like can be seen through the element mapping (figure 1); the interaction between the platinum and the nickel-based carrier can be analyzed through X-ray photoelectron spectroscopy and synchrotron radiation, and the formation of Pt-O bonds can reduce the energy barrier of hydrogen evolution reaction and promote the adsorption of hydrogen and the formation of hydrogen-hydrogen bonds, thereby being beneficial to improving the performance of hydrogen production by water decomposition (figure 2).
Example 2: application of platinum edge modified nickel-based nano material
(1) The practical application performance of the invention is tested on an electrochemical workstation of a Shanghai Chenghua CHI 760E three-electrode system;
(2) Graphite rods and Reversible Hydrogen Electrodes (RHE) were used as counter and reference electrodes, respectively, 2.0mg of catalyst and 1mg of Vulcan XC-72 were added to 0.2mL of Nafion/isopropyl alcohol (1 ‰) to prepare catalyst ink, and 20 μ L of catalyst ink was slowly dropped on a Rotating Disk Electrode (RDE) and naturally dried to prepare a working electrode.
(3) In the potential range of-0.2-0.1V (vs RHE), at N 2 Saturated 1M KOH,0.5M H 2 SO 4 1M PBS solution at 5mV s -1 And a rotation speed of 1600rpm, a polarization curve of the electrolytic water hydrogen evolution reaction was obtained (fig. 3).
The catalytic benefit of the material for producing hydrogen by electrocatalytic decomposition of water is 1M KOH,0.5M H 2 SO 4 The test of practical application performance in 1M PBS solution shows that NHC-Pt-3 has excellent performance and high platinum utilization rate (FIG. 3).
Density functional theory calculations indicate that the adsorption of hydroxyl groups is the rate controlling step in alkaline media, and the gradual desorption process can be further described as: ni-OH → Ni-OOH → Ni … OH → OH - (FIG. 4).
Claims (4)
1. A preparation method of a platinum edge-modified nickel-based nano material is characterized by comprising the following steps:
(1) 0.2900-0.3000gNi (NO) 3 ) 2 ·6H 2 Adding O into 4mL of deionized water, and stirring at a high speed until the O is completely dissolved to obtain a nickel nitrate aqueous solution;
(2) Adding 0.3600-0.3610g of urea into 4mL of deionized water, and stirring at a high speed until the urea is completely dissolved to obtain a urea aqueous solution;
(3) Mixing the ethylene glycol solution with the prepared nickel nitrate aqueous solution and urea aqueous solution according to the volume ratio of 7;
(4) Placing the mixed solution obtained in the step (3) in a reaction kettle, heating the mixed solution with a solvent at 160 ℃ for 12 hours, cooling to room temperature, washing the mixed solution with water and ethanol, and centrifugally drying to obtain the nickel-based nano material;
(5) Respectively preparing the nickel-based nano material and chloroplatinic acid in the step (4) into glycol solutions, wherein the mass ratio of platinum to the nickel-based nano material in the chloroplatinic acid is 1-5wt.%;
(6) Mixing the chloroplatinic acid solution prepared in the step (5) with a nickel-based nano material glycol solution, and forming a uniform precursor solution under the action of magnetic stirring and ultrasound;
(7) And (3) placing the precursor mixed solution in the step (6) into a round-bottom flask, heating and stirring for 2 hours under the condition of oil bath at 120 ℃, cooling to room temperature, washing with water and ethanol, and centrifugally drying to obtain the nickel-based nanomaterial with the platinum edge modified.
2. The method for preparing the platinum edge-modified nickel-based nanomaterial according to claim 1, wherein the method for preparing the chloroplatinic acid ethylene glycol solution comprises the following steps: mixing 0.77-0.79mL of rho Pt ：6.38-6.40mg mL -1 H 2 PtCl 6 The solution is poured into 95mL of glycol solution and is stirred uniformly to obtain chloroplatinic acid glycol solution.
3. The platinum edge-modified nickel-based nanomaterial obtained by the preparation method of any one of claims 1-2.
4. The use of the platinum edge-modified nickel-based nanomaterial of claim 3 as a catalyst in the production of hydrogen by electrolysis of water.
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