CN110625135B - Method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies - Google Patents
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- 239000002159 nanocrystal Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 16
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
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- BIXNGBXQRRXPLM-UHFFFAOYSA-K ruthenium(3+);trichloride;hydrate Chemical compound O.Cl[Ru](Cl)Cl BIXNGBXQRRXPLM-UHFFFAOYSA-K 0.000 claims abstract description 6
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
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Abstract
The invention discloses a method for efficiently, simply and easily synthesizing Ru nanocrystals with different shapes, which comprises the steps of dissolving ruthenium trichloride hydrate and polyvinylpyrrolidone (PVP) in deionized water, stirring and mixing, adding a certain amount of potassium bromide or potassium iodide solid into the obtained mixed solution, stirring and mixing uniformly, then adding a formaldehyde solution, stirring the obtained mixed solution at room temperature for 0.5 h, sealing the solution, and placing the sealed solution in an oven with the temperature of 180-200 ℃ for reaction for 2 h. Naturally cooling to room temperature after the reaction is finished, adding acetone into the obtained black dispersion liquid for centrifugal separation, washing the obtained black precipitate with deionized water/acetone for three times, and finally dispersing in a mixed solution of water and ethanol for uniform dispersion by ultrasonic. The method adopts a hydrothermal method, utilizes halogen ions as micromolecule regulating agents, and controls and synthesizes the ruthenium nanocrystals with different shapes. The ruthenium nanocrystalline obtained by the invention can be used as a cathode material for water electrolysis, and shows good hydrogen production performance.
Description
Technical Field
The invention belongs to the technical field of photoelectric functional materials, relates to an electrocatalytic material, and particularly relates to a method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies.
Background
Energy and environmental issues are the focus of considerable attention in the modern times. The exploration of renewable and zero-pollution novel energy sources is imperative, and the most representative new energy sources comprise solar energy, wind energy, hydrogen energy and the like. At present, hydrogen production by means of water electrolysis is paid more and more attention by researchers worldwide. In the technical field of electrocatalytic hydrogen production, the catalyst Ru nanocrystalline is applied to a cathode material for water electrolysis due to the factors of low price, low overpotential, high current density, good stability and the like. In order to increase the efficiency of electrocatalytic hydrogen production, more demands are generally placed on the synthesized electrocatalytic material.
The cathode electrocatalyst is a key material of a water electrolysis hydrogen production system, and influences the efficiency of electrocatalytic hydrogen production. At present, ruthenium-based nano materials can be compared with commercial Pt/C catalysts in alkaline electrolyte, although the ruthenium-based nano materials are electrolytic water cathode materials with excellent performance and stability, ruthenium nano crystals with different crystal faces and different morphologies have different activity performances, and the controllable synthesis of the ruthenium nano crystals is the research direction. Aiming at the problem, micromolecule regulation can be adopted, and the formation and growth of ruthenium crystal nucleus can be controlled by utilizing the complexation of the micromolecule regulation and the ruthenium surface, so that the morphology of the ruthenium crystal nucleus is controlled. The controllable synthesis of the morphology of the nano material is a difficult point, and in the existing reports, the ruthenium (Ru) nanocrystalline synthesized in water phase or polyhydric alcohol is a random-morphology nano polyhedral small particle, and the controllable synthesis of the morphology of the Ru nanocrystalline still needs to be further explored.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the ruthenium nanocrystal with good water/ethanol phase dispersibility, uniform and controllable appearance and good electrocatalysis performance and the preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies comprises the following steps: dissolving a certain amount of ruthenium trichloride hydrate and polyvinylpyrrolidone (PVP) in deionized water, stirring and mixing, adding a certain amount of potassium bromide or potassium iodide solid into the obtained mixed solution, stirring and mixing uniformly, then adding a formaldehyde solution, stirring the obtained mixed solution at room temperature for 0.5 h, then transferring the solution into a 25 mL stainless steel reaction kettle containing a polytetrafluoroethylene lining, sealing, and placing in an oven at 180-200 ℃ for reaction for 2 h. Naturally cooling to room temperature after the reaction is finished, adding acetone into the obtained black dispersion liquid for centrifugal separation, washing the obtained black precipitate with deionized water/acetone for three times, and finally dispersing in a mixed solution of water and ethanol for uniform dispersion by ultrasonic. The method comprises the following specific steps:
(1) dissolving ruthenium trichloride hydrate and polyvinylpyrrolidone (PVP) in deionized water, and stirring to obtain a mixed solution;
(2) adding a certain amount of potassium bromide or potassium iodide into the mixed solution in the step (1);
(3) adding a certain amount of formaldehyde into the mixed solution obtained in the step (2), and stirring for 0.5 h;
(4) carrying out high-temperature hydrothermal reaction for 2 h;
(5) washing the black precipitate obtained in the step (4) with deionized water/acetone for three times, and finally uniformly dispersing the black precipitate in a mixed solution of water and ethanol by ultrasonic.
Further, in the step (1), the dosage of the hydrated ruthenium trichloride is 0.06 mmol, the dosage of the PVP is 100 mg, and the dosage of the deionized water is 13 mL.
Further, in the step (2), the dosage of the potassium bromide is 3 mmol, and the dosage of the potassium iodide is 0.1 mmol.
Further, in the step (3), the amount of formaldehyde used is 0.4 mL.
Further, in the step (4), the reaction temperature is 180-200 ℃.
The invention has the beneficial effects that: the method adopts a hydrothermal method, utilizes halogen ions as micromolecule regulating agents, and controls and synthesizes the ruthenium nanocrystals with different shapes. The halogen ion and the reducing agent formaldehyde solution have specific input amount, and the formation and growth of ruthenium crystal nucleus are controlled by utilizing the coordination of the halogen ion and a certain crystal face of metal. Finally, the ruthenium nano-crystals with different morphologies and uniform dispersion are obtained. The ruthenium nanocrystalline obtained by the invention can be used as a cathode material for water electrolysis, and shows good hydrogen production performance.
The ruthenium nanosheet and the nanoparticles prepared by the method can be used as electrocatalytic hydrogen production materials, and are 10 mA cm in 1M KOH electrolyte-2The overpotential at the current density of (1) is 67 and 29 mV, respectively, the Tafel slopeDec of 104 and 37 mV, respectively-1。
Drawings
FIG. 1 is an XRD pattern of a ruthenium nanocrystal of the invention;
FIG. 2 is a TEM image of a ruthenium nanocrystal of the present invention;
FIG. 3 is the LSV curve and Tafel curve of the ruthenium nanocrystal in water electrolysis and hydrogen production in 1M KOH electrolyte.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
A method for efficiently and simply synthesizing Ru nanosheets (Ru-1) comprises the following steps:
(1) dissolving 0.06 mmol of ruthenium trichloride hydrate and 100 mg of polyvinylpyrrolidone (PVP, 24000) in 13mL of deionized water, and stirring to obtain a mixed solution;
(2) adding 3 mmol of potassium bromide into the mixed solution;
(3) adding 0.4 mL of formaldehyde solution into the mixed solution, and stirring the obtained mixed solution for 0.5 h;
(4) carrying out high-temperature hydrothermal reaction at 180 ℃ for 2 h;
(5) the obtained black precipitate was washed three times with deionized water/acetone, and finally dispersed uniformly in a mixed solution of water and ethanol by ultrasound.
Example 2
A method for efficiently and simply synthesizing Ru nanoparticles (Ru-2) comprises the following steps:
(1) dissolving 0.06 mmol of ruthenium trichloride hydrate and 100 mg of polyvinylpyrrolidone (PVP, 24000) in 13mL of deionized water, and stirring to obtain a mixed solution;
(2) adding 0.1 mmol of potassium iodide into the mixed solution;
(3) adding 0.4 mL of formaldehyde solution into the mixed solution, and stirring the obtained mixed solution for 0.5 h;
(4) carrying out high-temperature hydrothermal reaction at 200 ℃ for 2 h;
(5) the obtained black precipitate was washed three times with deionized water/acetone, and finally dispersed uniformly in a mixed solution of water and ethanol by ultrasound.
As shown in FIG. 1, X-ray powder diffraction shows that the phases of the prepared ruthenium nanocrystals are allhcpAnd (4) phase(s). Corresponding to JCPDS card number 06-0663, no impurity peak appears, which indicates that the product purity is higher.
As shown in fig. 2, the transmission electron microscope shows that when potassium bromide is used as the small molecule regulator, the ruthenium nanocrystal with the morphology of a nanosheet structure is obtained, and when potassium iodide is used as the small molecule regulator, the ruthenium nanoparticle is obtained. The ruthenium nanosheet and the nanoparticles prepared in the embodiment are used as a material for producing hydrogen by electrolyzing water, and the electrocatalysis performance of the material is tested, and the specific method comprises the following steps: firstly, carrying out ICP-OES quantification on mixed Ru nanocrystal dispersion liquid of water and ethanol, then diluting the same mass of ruthenium nanocrystal dispersion liquid to 1 mL (diluted by a mixed solvent with the volume ratio of water to ethanol being 3: 7), adding 30 mu L of an Afion (5 wt.%) solution, carrying out ultrasonic treatment for about 1 h to uniformly disperse the ruthenium nanocrystal dispersion liquid, taking 5 mu L of dispersed liquid drops, and naturally drying the 5 mu L of dispersed liquid drops on a 3 mm glassy carbon electrode, thereby taking the Ru nanocrystal dispersion liquid as a working electrode. The electrochemical hydrogen evolution test adopts a three-electrode system, Ag/AgCl (saturated potassium chloride) is used as a reference electrode, and a graphite rod is used as a counter electrode. The hydrogen evolution reaction polarization curve is obtained by a Linear Sweep Voltammetry (LSV) test, and the potential test range is-0.9 to-1.5V (vsAg/AgCl), the scanning speed was 5 mV/s. The potential values are fitted to the Reversible Hydrogen Electrode (RHE) potential according to the nernst equation.
E RHE = E Ag/AgCl + 0.059×pH + E θ Ag/AgCl (0.197)
As shown in FIG. 3, LSV and Tafel curves of the ruthenium nanoplates and nanoparticles prepared in this example were obtained in a 1M KOH electrolyte, and FIG. 3 shows the LSV curve and Tafel curve at 10 mA cm-2The overpotential at the current density of (1) is 67 and 29 mV, respectively, and the Tafel slope is 104 and 37 mV dec-1.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. A method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies is characterized by comprising the following steps:
(1) dissolving 0.06 mmol of ruthenium trichloride hydrate and 100 mg of polyvinylpyrrolidone (PVP) in 13mL of deionized water, and stirring to obtain a mixed solution;
(2) adding 3 mmol of potassium bromide or 0.1 mmol of potassium iodide into the mixed solution in the step (1);
(3) adding 0.4 mL of formaldehyde into the mixed solution obtained in the step (2), and stirring for 0.5 h;
(4) carrying out hydrothermal reaction for 2 hours at 180-200 ℃;
(5) washing the black precipitate obtained in the step (4) with deionized water/acetone for three times, and finally uniformly dispersing the black precipitate in a mixed solution of water and ethanol by ultrasonic;
the obtained Ru nanocrystal phases are allhcpPhase (1);
when 3 mmol of potassium bromide is added, Ru nanosheets are obtained, and the Ru nanosheets are 10 mA cm in 1M KOH electrolyte-2The overpotential at the current density of (1) is 67 mV, and the Tafel slope is 104 mV dec-1；
When 0.1 mmol of potassium iodide is added, Ru nanoparticles are obtained, and the Ru nanoparticles are dissolved in a KOH electrolyte solution of 1M at 10 mA cm-2The overpotential at the current density of (1) is 29 mV, and the Tafel slope is 37 mV dec-1。
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