CN111644635A - Preparation method of highly-recessed nanoscale platinum-copper-nickel alloy frame material - Google Patents
Preparation method of highly-recessed nanoscale platinum-copper-nickel alloy frame material Download PDFInfo
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a preparation method of a highly concave nano-scale platinum-copper-nickel alloy frame material, which comprises the steps of adding precursor platinum salt, copper salt and nickel salt into oleylamine through an organic reduction solvent, then adding a surfactant, carrying out heat treatment reaction, carrying out centrifugal cleaning, and drying to obtain the highly concave nano-scale platinum-copper-nickel alloy frame material. The invention can be used for preparing the nano-scale platinum-copper-nickel alloy nano-frame material with stable structure, the obtained nano-scale platinum-copper-nickel alloy nano-frame material has good electrical conductivity and stable structure, can be used for preparing electrodes and catalytic materials, and provides technical support for development research and commercial application of novel energy batteries.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, relates to a solvothermal method and preparation of metal alloy, and particularly relates to a preparation method of a highly-recessed nano-scale platinum-copper-nickel alloy nano-frame.
Technical Field
The nanometer material mainly comprises single metal nanometer material and alloy nanometer material, the alloy nanometer material has more stable structure compared with the single metal material, and the conductivity and the hardness are also improved. Therefore, some researchers refer to nanomaterials as "third state crystalline materials" other than crystalline and amorphous materials. Due to the special properties of the nano material, the nano material science and technology generates four effects, namely a small-size effect, a quantum effect (including a macroscopic quantum tunneling effect), a surface effect and an interface effect, so that the nano material has physical and chemical properties which are not possessed by the traditional material, shows unique optical, electrical, magnetic, catalytic, chemical properties, superconducting properties and other properties, and has important application value in the fields of national defense, electronics, chemical industry, metallurgy, light industry, aviation, ceramics, nuclear technology, catalysts, medicine and the like.
However, the conventional metal material preparation method: the nanometer metal material is difficult to obtain through smelting, casting and rolling, forging and heat treatment and the like. The preparation method of the relatively mature nano metal material mainly comprises the following steps: inert gas evaporation, in-situ pressurization and high energy ball milling. However, these methods are difficult to realize uniform and well-crystallized alloy nano-materials. Thus, many challenges remain for the extensive preparation of nanoalloy materials.
Disclosure of Invention
The invention aims to improve the stability, the conductivity and the catalytic activity of metal alloy, create technical conditions for the development and the commercial application of a metal alloy nano-frame in the field of electrode and energy catalysis, and provide a preparation method for preparing a concave platinum-copper-nickel alloy nano-frame material.
The technical scheme of the invention is a preparation method of a highly-concave nano-scale platinum-copper-nickel alloy frame material, which is characterized by comprising the following steps.
1) And (3) adding precursor platinum salt, copper salt and nickel salt into oleylamine through an organic reduction solvent to obtain a mixed solution A.
2) To the obtained mixed solution a, a surfactant was added to obtain a mixed solution B.
3) And carrying out heat treatment reaction at the temperature of 160-200 ℃ to obtain a black solution C.
4) And centrifugally cleaning the black solution C, and drying to obtain the highly-recessed nano-scale platinum-copper-nickel alloy nano-framework material.
Further, the organic reducing solvent is one or more mixed solvents of oleylamine, oleic acid, dimethylformamide, ethylene glycol and triethylene glycol.
Furthermore, the dosage of the reducing solvent is 1/5-1/2 of the volume of the reaction lining.
Further, the platinum salt is one or more of chloroplatinic acid, potassium chloroplatinate and sodium chloroplatinate.
Further, the copper salt is one or more of copper nitrate, copper chloride, copper sulfate and copper acetate.
Further, the nickel salt is one or more of nickel nitrate, nickel chloride, nickel sulfate and nickel acetate.
Further, the molar ratio of the platinum salt to the copper salt to the nickel salt is 1:5: 1-5.
Further, the surfactant is one or more of dodecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, sodium citrate monohydrate and ascorbic acid.
Furthermore, the dosage of the surfactant is 10-50 times of the mass of platinum in the platinum salt.
Advantageous effects
The recessed platinum-copper-nickel nano frame material is prepared by a solvothermal technology in one step, the preparation method is simple and convenient, the reaction condition is mild, the prepared recessed platinum-copper-nickel nano frame material product is uniform and regular in shape, electron transfer and mass transmission in the reaction are facilitated, and the recessed platinum-copper-nickel nano frame material serving as a catalyst is applied to a fuel cell and has the advantages of excellent catalytic activity, stable circulation and the like.
Drawings
FIG. 1 is a schematic diagram of a highly recessed nanoscale platinum-copper-nickel alloy nano-framework structure.
Figure 2 mass activity and specific activity of highly recessed platinum copper nickel nano-frameworks and commercial platinum carbon in methanol oxidation.
Figure 3 is a graph of the performance parameters of a highly concave nano-scale platinum copper nickel nano-framework in an electrocatalytic methanol oxidation reaction.
Detailed Description
In order to make the technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples. It should be understood that the specific examples described herein are intended to be illustrative only and are not intended to be limiting.
In the embodiment of the invention, the concave nano-scale platinum-copper-nickel alloy nano-framework material is realized by a solvothermal method. The prepared alloy material has a highly open space structure, good conductivity, good stability and excellent catalytic activity, and is suitable for new energy materials.
The preparation method comprises the following steps.
1) Copper salt, nickel salt and surfactant are mixed in a reducing solvent at room temperature, then ultrasonic treatment is carried out for 30 minutes, platinum salt is added, and stirring is carried out for 10 minutes, so that the solvent and solute are fully mixed.
2) And transferring the fully stirred mixed solution into an inner liner of polytetrafluoroethylene, adding a magnetic stirrer, sleeving an outer liner of the reaction kettle, and screwing down a cover of the reaction kettle.
3) And transferring the screwed reaction kettle into an oil bath kettle with constant temperature of 160 ℃ for reaction for 18 hours. After the reaction is finished, the heating device is closed, and the reaction kettle is cooled to room temperature.
4) And taking out the black solution in the inner liner of the reaction kettle by using a rubber head dropper, transferring the black solution into a centrifugal tube, adding mixed cleaning solution of ethanol and n-hexane, carrying out ultrasonic centrifugal cleaning, and repeating the steps for a plurality of times.
5) Transferring the cleaned and centrifuged black product into a quartz boat, drying in a drying oven overnight, and then annealing in a 200 ℃ tube furnace for 1 hour under the air atmosphere to collect the concave nano-platinum-copper alloy nano-frame material.
The following description is given with reference to specific examples.
Example one.
The implementation flow of the preparation method of the highly concave nano-scale platinum-copper-nickel alloy nano-frame material in the embodiment is as follows.
At room temperature, copper salt, nickel salt and surfactant are fully mixed in 10 mL of reducing solvent oleylamine, the mixture is subjected to ultrasonic treatment for 30 minutes, then platinum salt is added, the mixture is fully mixed for 10 minutes, wherein the molar ratio of the platinum salt to the copper salt to the nickel salt is 1:5:1, the copper salt is copper acetate, the nickel salt is nickel acetate, the platinum salt is chloroplatinic acid, the amount of the copper acetate is 0.25mol, the amount of the nickel acetate is 0.05mol, the amount of the chloroplatinic acid is 0.05mol, and the surfactant is dodecyl trimethyl ammonium bromide, and the amount of the surfactant is 300 mg.
And transferring the fully stirred mixed solution into a polytetrafluoroethylene inner liner with the capacity of 20mL, adding a magnetic stirrer, sleeving an outer liner of the reaction kettle, and screwing down a cover of the reaction kettle.
Transferring the screwed reaction kettle into an oil bath kettle with constant temperature of 160 ℃, opening the magnetic stirring, continuously reacting for 18 hours, closing the heating device, and cooling the reaction kettle to room temperature.
And (3) taking out the black solution in the inner liner of the reaction kettle by using a rubber head dropper, transferring the black solution into a centrifugal tube, adding a mixed cleaning solution of ethanol and n-hexane in a ratio of 3:1, performing ultrasonic homogenization, centrifuging again, and repeating for 5 times to obtain a black metal alloy sample.
Transferring the cleaned and centrifuged black product into a quartz boat, drying in a drying oven overnight, and then annealing in a 200 ℃ tube furnace for 1 hour under the air atmosphere to collect the concave nano-platinum-copper alloy nano-frame material.
The material is prepared by a solvothermal method, platinum, copper and nickel are directly formed into a ternary alloy, a sunken nano-framework material with a highly open structure is realized, and the obtained alloy nano-framework material is high in electric conductivity, good in stability and excellent in catalytic performance, and is suitable for application research in the field of novel energy. The preparation method is simple, convenient and stable, can optimize the alloying degree and the spatial structure of the material, and provides technical support and guarantee for the development and the commercial application of energy materials.
Example two.
The implementation flow of the preparation method of the highly concave nano-scale platinum-copper-nickel alloy nano-frame material in the embodiment is as follows.
At room temperature, copper salt, nickel salt and surfactant are fully mixed in 10 mL of reducing solvent oleylamine, the mixture is subjected to ultrasonic treatment for 30 minutes, then platinum salt is added, the mixture is fully mixed for 10 minutes, wherein the molar ratio of the platinum salt to the copper salt to the nickel salt is 1:5:2, the copper salt is copper acetate, the nickel salt is nickel acetate, the platinum salt is chloroplatinic acid, the amount of the copper acetate is 0.25mol, the amount of the nickel acetate is 0.10mol, the amount of the chloroplatinic acid is 0.05mol, and the surfactant is dodecyl trimethyl ammonium bromide, and the amount of the surfactant is 300 mg.
And transferring the fully stirred mixed solution into a polytetrafluoroethylene inner liner with the capacity of 20mL, adding a magnetic stirrer, sleeving an outer liner of the reaction kettle, and screwing down a cover of the reaction kettle.
Transferring the screwed reaction kettle into an oil bath kettle with constant temperature of 160 ℃, opening the magnetic stirring, continuously reacting for 18 hours, closing the heating device, and cooling the reaction kettle to room temperature.
And (3) taking out the black solution in the inner liner of the reaction kettle by using a rubber head dropper, transferring the black solution into a centrifugal tube, adding a mixed cleaning solution of ethanol and n-hexane in a ratio of 3:1, performing ultrasonic homogenization, centrifuging again, and repeating for 5 times to obtain a black metal alloy sample.
Transferring the cleaned and centrifuged black product into a quartz boat, drying in a drying oven overnight, and then annealing in a 200 ℃ tube furnace for 1 hour under the air atmosphere to collect the concave nano-platinum-copper alloy nano-frame material.
The material is prepared by a solvothermal method, platinum, copper and nickel are directly formed into a ternary alloy, a sunken nano-framework material with a highly open structure is realized, and the obtained alloy nano-framework material is high in electric conductivity, good in stability and excellent in catalytic performance, and is suitable for application research in the field of novel energy. The preparation method is simple, convenient and stable, can optimize the alloying degree and the spatial structure of the material, and provides technical support and guarantee for the development and the commercial application of energy materials.
Example three.
The implementation flow of the preparation method of the highly concave nano-scale platinum-copper-nickel alloy nano-frame material in the embodiment is as follows.
At room temperature, copper salt, nickel salt and surfactant are fully mixed in 10 mL of reducing solvent oleylamine, the mixture is subjected to ultrasonic treatment for 30 minutes, then platinum salt is added, the mixture is fully mixed for 10 minutes, wherein the molar ratio of the platinum salt to the copper salt to the nickel salt is 1:5:3, the copper salt is copper acetate, the nickel salt is nickel acetate, the platinum salt is chloroplatinic acid, the amount of the copper acetate is 0.25mol, the amount of the nickel acetate is 0.15 mol, the amount of the chloroplatinic acid is 0.05mol, and the surfactant is dodecyl trimethyl ammonium bromide, and the amount of the surfactant is 300 mg.
And transferring the fully stirred mixed solution into a polytetrafluoroethylene inner liner with the capacity of 20mL, adding a magnetic stirrer, sleeving an outer liner of the reaction kettle, and screwing down a cover of the reaction kettle.
Transferring the screwed reaction kettle into an oil bath kettle with constant temperature of 160 ℃, opening the magnetic stirring, continuously reacting for 18 hours, closing the heating device, and cooling the reaction kettle to room temperature.
And (3) taking out the black solution in the inner liner of the reaction kettle by using a rubber head dropper, transferring the black solution into a centrifugal tube, adding a mixed cleaning solution of ethanol and n-hexane in a ratio of 3:1, performing ultrasonic homogenization, centrifuging again, and repeating for 5 times to obtain a black metal alloy sample.
Transferring the cleaned and centrifuged black product into a quartz boat, drying in a drying oven overnight, and then annealing in a 200 ℃ tube furnace for 1 hour under the air atmosphere to collect the concave nano-platinum-copper alloy nano-frame material.
The material is prepared by a solvothermal method, platinum, copper and nickel are directly formed into a ternary alloy, a sunken nano-framework material with a highly open structure is realized, and the obtained alloy nano-framework material is high in electric conductivity, good in stability and excellent in catalytic performance, and is suitable for application research in the field of novel energy. The preparation method is simple, convenient and stable, can optimize the alloying degree and the spatial structure of the material, and provides technical support and guarantee for the development and the commercial application of energy materials.
Example four.
The implementation flow of the preparation method of the highly concave nano-scale platinum-copper-nickel alloy nano-frame material in the embodiment is as follows.
At room temperature, copper salt, nickel salt and surfactant are fully mixed in 10 mL of reducing solvent oleylamine, the mixture is subjected to ultrasonic treatment for 30 minutes, then platinum salt is added, the mixture is fully mixed for 10 minutes, wherein the molar ratio of the platinum salt to the copper salt to the nickel salt is 1:5:4, the copper salt is copper acetate, the nickel salt is nickel acetate, the platinum salt is chloroplatinic acid, the amount of the copper acetate is 0.25mol, the amount of the nickel acetate is 0.20 mol, the amount of the chloroplatinic acid is 0.05mol, and the surfactant is dodecyl trimethyl ammonium bromide, and the amount of the surfactant is 300 mg.
And transferring the fully stirred mixed solution into a polytetrafluoroethylene inner liner with the capacity of 20mL, adding a magnetic stirrer, sleeving an outer liner of the reaction kettle, and screwing down a cover of the reaction kettle.
Transferring the screwed reaction kettle into an oil bath kettle with constant temperature of 160 ℃, opening the magnetic stirring, continuously reacting for 18 hours, closing the heating device, and cooling the reaction kettle to room temperature.
And (3) taking out the black solution in the inner liner of the reaction kettle by using a rubber head dropper, transferring the black solution into a centrifugal tube, adding a mixed cleaning solution of ethanol and n-hexane in a ratio of 3:1, performing ultrasonic homogenization, centrifuging again, and repeating for 5 times to obtain a black metal alloy sample.
Transferring the cleaned and centrifuged black product into a quartz boat, drying in a drying oven overnight, and then annealing in a 200 ℃ tube furnace for 1 hour under the air atmosphere to collect the concave nano-platinum-copper alloy nano-frame material.
The material is prepared by a solvothermal method, platinum, copper and nickel are directly formed into a ternary alloy, a sunken nano-framework material with a highly open structure is realized, and the obtained alloy nano-framework material is high in electric conductivity, good in stability and excellent in catalytic performance, and is suitable for application research in the field of novel energy. The preparation method is simple, convenient and stable, can optimize the alloying degree and the spatial structure of the material, and provides technical support and guarantee for the development and the commercial application of energy materials.
Example five.
The implementation flow of the preparation method of the highly concave nano-scale platinum-copper-nickel alloy nano-frame material in the embodiment is as follows.
At room temperature, copper salt, nickel salt and surfactant are fully mixed in 10 mL of reducing solvent oleylamine, the mixture is subjected to ultrasonic treatment for 30 minutes, then platinum salt is added, the mixture is fully mixed for 10 minutes, wherein the molar ratio of the platinum salt to the copper salt to the nickel salt is 1:5:5, the copper salt is copper acetate, the nickel salt is nickel acetate, the platinum salt is chloroplatinic acid, the amount of the copper acetate is 0.25mol, the amount of the nickel acetate is 0.25mol, the amount of the chloroplatinic acid is 0.05mol, and the surfactant is dodecyl trimethyl ammonium bromide, and the amount of the surfactant is 300 mg.
And transferring the fully stirred mixed solution into a polytetrafluoroethylene inner liner with the capacity of 20mL, adding a magnetic stirrer, sleeving an outer liner of the reaction kettle, and screwing down a cover of the reaction kettle.
Transferring the screwed reaction kettle into an oil bath kettle with constant temperature of 160 ℃, opening the magnetic stirring, continuously reacting for 18 hours, closing the heating device, and cooling the reaction kettle to room temperature.
And (3) taking out the black solution in the inner liner of the reaction kettle by using a rubber head dropper, transferring the black solution into a centrifugal tube, adding a mixed cleaning solution of ethanol and n-hexane in a ratio of 3:1, performing ultrasonic homogenization, centrifuging again, and repeating for 5 times to obtain a black metal alloy sample.
Transferring the cleaned and centrifuged black product into a quartz boat, drying in a drying oven overnight, and then annealing in a 200 ℃ tube furnace for 1 hour under the air atmosphere to collect the concave nano-platinum-copper alloy nano-frame material.
The material is prepared by a solvothermal method, platinum, copper and nickel are directly formed into a ternary alloy, a sunken nano-framework material with a highly open structure is realized, and the obtained alloy nano-framework material is high in electric conductivity, good in stability and excellent in catalytic performance, and is suitable for application research in the field of novel energy. The preparation method is simple, convenient and stable, can optimize the alloying degree and the spatial structure of the material, and provides technical support and guarantee for the development and the commercial application of energy materials.
Claims (9)
1. A preparation method of a highly-recessed nano-scale platinum-copper-nickel alloy frame material is characterized by comprising the following steps:
1) adding precursor platinum salt, copper salt and nickel salt into oleylamine through an organic reduction solvent to obtain a mixed solution A;
2) adding a surfactant into the obtained mixed solution A to obtain a mixed solution B;
3) carrying out heat treatment reaction at the temperature of 160-200 ℃ to obtain a black solution C;
4) and centrifugally cleaning the black solution C, and drying to obtain the highly-recessed nano-scale platinum-copper-nickel alloy framework material.
2. The method according to claim 1, wherein the organic reducing solvent is a mixed solvent of one or more of oleylamine, oleic acid, dimethylformamide, ethylene glycol and triethylene glycol.
3. The method according to claim 1 or 2, wherein the reducing solvent is used in an amount of 1/5 to 1/2% by volume of the reaction lining.
4. The method of claim 1, wherein the platinum salt is one or more of chloroplatinic acid, potassium chloroplatinate, and sodium chloroplatinate.
5. The method of claim 1, wherein the copper salt is one or more of copper nitrate, copper chloride, copper sulfate and copper acetate.
6. The method of claim 1, wherein the one or more of nickel nitrate, nickel chloride, nickel sulfate, and nickel acetate are used.
7. The method according to any one of claims 1, 5, 6 or 7, wherein the molar ratio of the platinum salt, the cuprous salt and the nickel salt is 1:5:1 to 5.
8. The method of claim 1, wherein the surfactant is one or more of dodecyltrimethylammonium chloride, dodecyltrimethylammonium bromide, sodium citrate monohydrate, and ascorbic acid.
9. The method according to claim 1, wherein the amount of the surfactant is 10 to 50 times the mass of platinum in the platinum salt.
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| CN105470531A (en) * | 2015-11-19 | 2016-04-06 | 中山大学 | Eight-legged transparent frame structure alloy electrocatalyst and preparation method thereof |
| CN105478794A (en) * | 2015-12-11 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Platinum-copper alloy nano particle and preparation method thereof |
| CN108247080A (en) * | 2018-02-08 | 2018-07-06 | 厦门大学 | A kind of platinoid nickel ternary alloy nano material and preparation method thereof |
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2020
- 2020-06-02 CN CN202010487550.6A patent/CN111644635A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010192172A (en) * | 2009-02-16 | 2010-09-02 | Noritake Co Ltd | Method of manufacturing alloy catalyst electrode for fuel cell |
| CN105470531A (en) * | 2015-11-19 | 2016-04-06 | 中山大学 | Eight-legged transparent frame structure alloy electrocatalyst and preparation method thereof |
| CN105478794A (en) * | 2015-12-11 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Platinum-copper alloy nano particle and preparation method thereof |
| CN108247080A (en) * | 2018-02-08 | 2018-07-06 | 厦门大学 | A kind of platinoid nickel ternary alloy nano material and preparation method thereof |
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Application publication date: 20200911 |