CN113458409A - Method for synthesizing nano alloy catalyst at room temperature - Google Patents

Method for synthesizing nano alloy catalyst at room temperature Download PDF

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CN113458409A
CN113458409A CN202110671409.6A CN202110671409A CN113458409A CN 113458409 A CN113458409 A CN 113458409A CN 202110671409 A CN202110671409 A CN 202110671409A CN 113458409 A CN113458409 A CN 113458409A
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room temperature
sodium borohydride
deionized water
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何荣幸
江永
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Southwest University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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    • 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
    • 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
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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

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Abstract

The invention discloses a method for synthesizing a nano alloy catalyst at room temperature, and relates to the technical field of nano powder preparation. A method for synthesizing a nano alloy catalyst at room temperature comprises the following steps: adding anhydrous ruthenium trichloride and iridium trichloride trihydrate into deionized water, carrying out ultrasonic treatment at a constant temperature of 25 ℃ for 1h, and carrying out magnetic stirring after metal salts in the solution are completely dissolved; dissolving sodium borohydride in deionized water, and dissolving by ultrasonic waves; and slowly dropwise adding a sodium borohydride solution into a metal salt solution, carefully observing the color of the mixed solution, stopping dropwise adding and stirring when the color is completely clear, washing with ethanol and deionized water, performing suction filtration to recover precipitates, and drying to obtain the RuIr alloy. The method has low requirement on synthesis conditions and mild reaction conditions, and the nano-alloy catalyst RuIr prepared by the method shows excellent effect in the application of electrochemical water decomposition and has super-good chemical stability.

Description

Method for synthesizing nano alloy catalyst at room temperature
Technical Field
The invention belongs to the technical field of nano powder preparation, and particularly relates to a method for synthesizing a nano alloy catalyst at room temperature.
Background
The metal accounts for more than 75% of the periodic table of elements, and is widely applied to the fields of photonics, catalysis, energy storage and conversion, electronics, medicine and the like. In particular, metals in a finely divided state, known as nanocrystals, often exhibit chemical properties that are distinct from bulk materials. The characteristics of metal nanocrystals mainly derive from surface effects and quantum size effects, which can be manipulated in terms of size, shape, composition, structure, and crystal, etc. Despite some advances in this regard, in practical applications, metal nanocrystals typically do not meet all of the requirements, and are expected to have high activity, high chemical and structural stability, and high selectivity. To potentially meet all of these requirements, there has been increasing interest in recent years in developing multi-metallic nanocrystals with good properties. Multi-metallic nanocrystals composed of different metallic elements have unique physicochemical properties that are superior to single-metallic nanocrystals in certain applications due to synergistic effects with different metals. In general, the addition of another metal to form bimetallic alloys can significantly change their electronic structure and spatial arrangement pattern, further contributing to a significant improvement in performance. The metal alloy catalyst has great application prospect in the aspects of catalyst, lithium battery, hydrogen storage, electrochemistry and the like due to the unique chemical property and the special microstructure.
The main preparation methods of the current alloy material mainly comprise a high-temperature oil bath auxiliary reduction method, a seed-mediated growth method, a co-reduction method, an electrochemical replacement method and an oxidation corrosion method, or adopt a hydrothermal method for preparation. These methods generally have the following problems: the synthesis conditions are harsh, high-temperature auxiliary synthesis is needed, a surfactant is needed to participate, oil bath reaction is needed under the high-temperature condition, the pretreatment of the synthetic product is complicated, the loss of the final collected product is high, the yield is limited, and impurities which are not removed completely are easily mixed on the target substance. Moreover, the reaction period required by the methods is long, and part of experimental processes involve hydrothermal and high-temperature oil bath and have certain dangerousness.
Disclosure of Invention
The invention provides a method for synthesizing a nano alloy catalyst at room temperature, which has lower requirements on synthesis conditions and milder reaction conditions.
The invention firstly relates to a synthesis method of a room-temperature reduction metal alloy, which is characterized by comprising the following synthesis steps: s1, adding anhydrous ruthenium trichloride and iridium trichloride trihydrate into deionized water, carrying out ultrasonic treatment for 1h at a constant temperature of 25 ℃, and carrying out magnetic stirring at a stirring speed of 200rpm after metal salts in the solution are completely dissolved;
s2, dissolving sodium borohydride in deionized water, and ultrasonically dissolving;
s3, slowly dripping the sodium borohydride solution prepared in the step S2 into the metal salt solution of the step S1, carefully observing the color of the mixed solution, stopping dripping and stirring when the color is completely clear, then washing with ethanol and deionized water, performing suction filtration to recover precipitates, and drying to obtain RuIr.
Furthermore, the purity of the anhydrous ruthenium trichloride, the iridium trichloride trihydrate and the sodium borohydride is 99.999 percent.
Furthermore, the volume of the deionized water is 100-200 mL.
Further, the mass to total metal mass ratio of sodium borohydride is 1-1.5: 1.
Further, the amount of anhydrous ruthenium trichloride was 10mg, and the amount of iridium trichloride trihydrate was 10 mg.
Further, the dosage of the sodium borohydride is 20-30 mg.
Compared with the prior art, the invention has the beneficial effects that:
1. the method can perform reduction synthesis at room temperature, has low synthesis requirement and mild reaction condition, does not need to perform complex high-temperature reaction, greatly shortens the synthesis period, and is simple and convenient to collect samples and controllable in amount;
2. the alloy prepared by the method has lasting stability, certain universality, uniform appearance, pure substance and no impurity phase.
2. The alloy prepared by the method can be applied to electrochemical water decomposition reaction, has good electrochemical effect, greatly reduces the time required by the reaction by a room-temperature stirring auxiliary reduction method, can obtain products in a short time, and finally has controllable yield and less loss.
Drawings
FIG. 1 is a 15k scanning electron microscope image of a nano-alloy catalyst RuIr prepared according to a first embodiment of the present invention;
FIG. 2 is a 20k scanning electron microscope image of a nano-alloy catalyst RuIr prepared according to the first embodiment of the present invention;
FIG. 3 is an X-ray diffraction diagram of RuIr, a nano-alloy catalyst prepared according to a first embodiment of the present invention;
FIG. 4 is an LSV curve of the nano-alloy catalyst RuIr prepared by the present invention in an acidic environment HER;
FIG. 5 is an LSV curve of the nano-alloy catalyst RuIr prepared by the present invention in alkaline environment HER;
FIG. 6 is an LSV curve of a nano-alloy catalyst RuIr prepared by the present invention in an acidic environment OER;
FIG. 7 is an LSV curve of the nano-alloy catalyst RuIr prepared by the present invention in the alkaline environment OER;
FIG. 8 is a current density curve with time of the nano-alloy catalyst RuIr prepared by the invention under an acidic environment.
Detailed Description
The invention is described in further detail below with reference to the following figures and detailed description:
the invention discloses a method for synthesizing a nano alloy catalyst at room temperature, which comprises the following steps:
s1, adding anhydrous ruthenium trichloride and iridium trichloride trihydrate into deionized water, carrying out ultrasonic treatment for 1h at a constant temperature of 25 ℃, and carrying out magnetic stirring at a stirring speed of 200rpm after metal salts in the solution are completely dissolved;
s2, dissolving sodium borohydride in deionized water, and ultrasonically dissolving;
s3, slowly adding the sodium borohydride solution prepared in the step S2 into the metal salt solution of the step S1 in a dropwise manner, wherein the mass-to-total metal mass ratio of the sodium borohydride is 1-1.5: 1, carefully observing the color of the mixed solution, stopping dropwise adding and stirring when the color is completely clear, washing with ethanol and deionized water, performing suction filtration to recover precipitates, and drying to obtain RuIr.
In the method, the purities of anhydrous ruthenium trichloride, iridium trichloride trihydrate and sodium borohydride are all 99.999%, the volume of deionized water is 100-200 mL, and the mass of sodium borohydride is 20-30 mg.
Example one
Preparation of nano alloy catalyst
Weighing 10mg of anhydrous ruthenium trichloride and 10mg of iridium trichloride trihydrate, dissolving the anhydrous ruthenium trichloride and the iridium trichloride trihydrate in deionized water, performing ultrasonic treatment for 1 hour at a constant temperature of 25 ℃, and stirring by using a magnetic stirrer after the anhydrous ruthenium trichloride and the iridium trichloride trihydrate are completely dissolved, wherein the stirring speed is 200 rpm; and then weighing 20mg of sodium borohydride, dissolving the sodium borohydride in deionized water, performing ultrasonic treatment to fully dissolve the sodium borohydride, slowly dropwise adding the prepared sodium borohydride solution into a metal salt solution, carefully observing the color of the mixed solution when the sodium borohydride solution is dropwise added, reducing the dropwise adding speed when the color of the mixed solution is transited from dark color to gray color, stopping dropwise adding when the color of the mixed solution is completely clear, stopping stirring simultaneously, washing with ethanol and deionized water, performing suction filtration to recover precipitates, and drying the precipitates to obtain RuIr.
The prepared RuIr nano alloy catalyst is used for electrochemical water decomposition reaction under the condition of wide pH range. Characterization of RuIr nanoalloy catalyst
SEM test
Fig. 1 and 2 are scanning electron micrographs of the nano-alloy catalyst prepared in the first embodiment of the present invention, and as shown in the figure, the prepared RuIr nano-alloy catalyst has uniformly distributed particles with a small size of 2-5 nm.
XRD analysis
Fig. 3 is an X-ray powder diffraction pattern of the nano-alloy catalyst RuIr prepared in the first embodiment of the present invention, wherein the X-ray powder diffraction pattern of the RuIr alloy has a peak shape same as that of elemental ruthenium, which indicates that the purity of the material phase is higher, but due to the influence of alloying, the X-ray diffraction pattern of the RuIr alloy is slightly shifted from that of the standard.
LSV curve analysis
First, the invention is usedMethod for synthesizing nano alloy catalyst RuIr with mass ratio of Ru to Ir being 1:11:1And Ru and Ir in a mass ratio of 1:21:2Then, the HER performance and OER performance of the catalyst were tested under acidic and basic environments respectively with iR correction using a typical three-electrode system, the HER/OER performance of the catalyst was evaluated with LSV with iR correction, and for comparison, the HER performance of commercial Pt/C and commercial RuO were also investigated2The OER performance of (1) is shown in FIG. 4, FIG. 5, FIG. 6 and FIG. 7, and the hydrogen evolution and oxygen evolution are at 0.5M H2SO4And 1.0M KOH respectively shows ultralow potentials of 13 mV, 35 mV, 251 mV and 268mV, and the nano alloy catalyst RuIr prepared by the method has excellent effect on the aspect of electrochemical water decomposition, wherein the hydrogen evolution effect is far superior to that of a commercial Pt/C catalyst, and the oxygen evolution effect is also similar to that of a commercial RuO2Can be compared with each other, and can be electrolyzed in a wide pH range.
The alloy catalyst prepared by the method has excellent chemical stability in the process of electrochemically decomposing water, and as shown in figure 8, the catalyst is not obviously dissolved after being continuously operated for 60 hours under high current density.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.

Claims (6)

1. A synthesis method of a room-temperature reduction metal alloy is characterized by comprising the following synthesis steps: s1, adding anhydrous ruthenium trichloride and iridium trichloride trihydrate into deionized water, carrying out ultrasonic treatment for 1h at a constant temperature of 25 ℃, and carrying out magnetic stirring at a stirring speed of 200rpm after metal salts in the solution are completely dissolved;
s2, dissolving sodium borohydride in deionized water, and ultrasonically dissolving;
s3, slowly dripping the sodium borohydride solution prepared in the step S2 into the metal salt solution of the step S1, carefully observing the color of the mixed solution, stopping dripping and stirring when the color is completely clear, then washing with ethanol and deionized water, performing suction filtration to recover precipitates, and drying to obtain RuIr.
2. A method of synthesizing a room temperature reducing metal alloy as claimed in claim 1, wherein: the purities of the anhydrous ruthenium trichloride, the iridium trichloride trihydrate and the sodium borohydride are all 99.999%.
3. A method of synthesizing a room temperature reducing metal alloy as claimed in claim 1, wherein: the volume of the deionized water is 100-200 mL.
4. A method of synthesizing a room temperature reducing metal alloy as claimed in claim 1, wherein: the mass to total metal mass ratio of the sodium borohydride is 1-1.5: 1.
5. A method of synthesizing a room temperature reducing metal alloy as claimed in claim 1, wherein: the dosage of the anhydrous ruthenium trichloride is 10mg, and the dosage of the iridium trichloride trihydrate is 10 mg.
6. A method of synthesizing a room temperature reducing metal alloy as claimed in claim 1, wherein: the dosage of the sodium borohydride is 20-30 mg.
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Cited By (1)

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CN117564289A (en) * 2024-01-12 2024-02-20 中国科学技术大学 Iridium ruthenium gold core-shell structure nano material and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117564289A (en) * 2024-01-12 2024-02-20 中国科学技术大学 Iridium ruthenium gold core-shell structure nano material and preparation method and application thereof
CN117564289B (en) * 2024-01-12 2024-05-17 中国科学技术大学 Iridium ruthenium gold core-shell structure nano material and preparation method and application thereof

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Application publication date: 20211001