Platinum-based intermetallic nanocrystal with ordered structure and low-temperature preparation and application thereof

Abstract

The invention relates to a platinum-based intermetallic nanocrystal with an ordered structure as well as low-temperature preparation and application of the platinum-based intermetallic nanocrystal, and belongs to the field of cathode materials of proton exchange membrane fuel cells. The method comprises the following steps: dispersing a platinum salt, a transition metal salt and a salt formed by a low-melting-point metal into an organic amine solution, and reducing the metal salt in the mixed solution to obtain a disordered ternary alloy nanocrystal; loading the obtained nanocrystalline on carbon, and carrying out medium and low temperature annealing treatment on the ternary alloy to obtain the platinum-based intermetallic nanocrystalline oxygen reduction catalyst. The preparation method disclosed by the invention is simple in process, the disordered-ordered phase transition temperature of the platinum-transition metal nanocrystal catalyst can be reduced by introducing the low-melting-point metal, the energy consumption is reduced, the energy is saved, the emission is reduced, the industrial batch production is easy, and the obtained platinum-based intermetallic nanocrystal oxygen reduction catalyst has good activity and durability, and can be applied to proton exchange membrane fuel cells.

Description

technical field

[0001] The invention belongs to the field of cathode materials for proton exchange membrane fuel cells, and more specifically relates to a structurally ordered platinum-based intermetallic nanocrystal and its medium and low temperature preparation and application, especially a platinum-based intermetallic nanocrystal oxygen reduction catalyst and its A preparation method, especially a preparation method for reducing the phase transition temperature of platinum-based intermetallic nanocrystals, a platinum-based intermetallic nanocrystal oxygen reduction catalyst for accelerating the oxygen reduction reaction rate of a fuel cell cathode, and a preparation method thereof. Background technique

[0002] Proton Exchange Membrane Fuel Cell (PEMFC) can convert the chemical energy stored in fuel / oxygen into electrical energy through an electrochemical process, which has the advantages of high conversion efficiency and high specific power, and its products are non-toxic...

Examples

Embodiment 1

[0045] S1: According to the molar ratio of 5:4:1, take platinum acetylacetonate, zinc acetylacetonate and dibutyl tin diacetylacetonate, and dissolve them in 5 mL of oleylamine solution to make the platinum precursor concentration 0.01mol / L The solution. Under the protection of argon, the solution was stirred at 110 °C for 20 minutes, and the precursor salt was fully dissolved and mixed.

[0046] S2: Subsequently, the temperature of the solution was raised to 320° C. at a heating rate of 10° C. / min, and the reaction was continued for 2 hours, followed by centrifugal washing to obtain disordered platinum-zinc-tin nanoparticles.

[0047] S3: Weigh a certain mass of carbon powder according to the metal loading of 15%, add a mixture of ethanol and hexane with a volume ratio of 2:1, and ultrasonically disperse, and then slowly drop into the disordered platinum-zinc-tin-tricarbonate obtained in step S2 meta-nanoparticles. After ultrasonication for a period of time, centrifuge, was...

Embodiment 2

[0050] S1: According to the molar ratio of 50:35:15, take platinum acetylacetonate, nickel acetylacetonate and dibutyl tin diacetylacetonate, and dissolve them in 5 mL of oleylamine solution to make the platinum precursor concentration 0.05 mol / L The solution. Under the protection of argon, the solution was stirred at 100 °C for 20 minutes, and the precursor salt was fully dissolved and mixed.

[0051] S2: Subsequently, at a heating rate of 5°C / min, the solution was heated to 260°C, and the reaction was continued for 1 hour, followed by centrifugal washing to obtain disordered platinum-nickel-tin ternary nanoparticles;

[0052] S3: Weigh a certain mass of carbon powder according to the metal loading of 20%, add a mixture of ethanol and hexane with a volume ratio of 2:1, and ultrasonically disperse, and then slowly drop into the disordered platinum nickel tin three meta-nanoparticles. After ultrasonication for a period of time, centrifuge, wash, and dry to obtain carbon-suppo...

Embodiment 3

[0055] S1: According to the molar ratio of 50:45:5, take platinum acetylacetonate, iron acetate and dibutyl tin diacetylacetonate, and dissolve them in 5 mL of oleylamine solution to make a platinum precursor concentration of 0.01mol / L solution. Under the protection of argon, the solution was stirred at 130 °C for 20 minutes, and the precursor salt was fully dissolved and mixed.

[0056] S2: Subsequently, at a heating rate of 5°C / min, the temperature of the solution was raised to 260°C, the reaction was continued for 1 hour, and then centrifuged and washed to obtain disordered platinum-iron-tin ternary nanoparticles;

[0057] S3: Weigh a certain mass of carbon powder according to the metal loading of 10%, add a mixture of ethanol and hexane with a volume ratio of 2:1, and ultrasonically disperse, then slowly drop into the disordered platinum-iron-tin tricarbonate obtained in step S2 meta-nanoparticles. After ultrasonication for a period of time, centrifuge, wash, and dry to ...

technical field

[0001] The invention belongs to the field of cathode materials for proton exchange membrane fuel cells, and more specifically relates to a structurally ordered platinum-based intermetallic nanocrystal and its medium and low temperature preparation and application, especially a platinum-based intermetallic nanocrystal oxygen reduction catalyst and its A preparation method, especially a preparation method for reducing the phase transition temperature of platinum-based intermetallic nanocrystals, a platinum-based intermetallic nanocrystal oxygen reduction catalyst for accelerating the oxygen reduction reaction rate of a fuel cell cathode, and a preparation method thereof. Background technique

[0002] Proton Exchange Membrane Fuel Cell (PEMFC) can convert the chemical energy stored in fuel / oxygen into electrical energy through an electrochemical process, which has the advantages of high conversion efficiency and high specific power, and its products are non-toxic...

Examples

Embodiment 1

[0045] S1: According to the molar ratio of 5:4:1, take platinum acetylacetonate, zinc acetylacetonate and dibutyl tin diacetylacetonate, and dissolve them in 5 mL of oleylamine solution to make the platinum precursor concentration 0.01mol / L The solution. Under the protection of argon, the solution was stirred at 110 °C for 20 minutes, and the precursor salt was fully dissolved and mixed.

[0046] S2: Subsequently, the temperature of the solution was raised to 320° C. at a heating rate of 10° C. / min, and the reaction was continued for 2 hours, followed by centrifugal washing to obtain disordered platinum-zinc-tin nanoparticles.

[0047] S3: Weigh a certain mass of carbon powder according to the metal loading of 15%, add a mixture of ethanol and hexane with a volume ratio of 2:1, and ultrasonically disperse, and then slowly drop into the disordered platinum-zinc-tin-tricarbonate obtained in step S2 meta-nanoparticles. After ultrasonication for a period of time, centrifuge, was...

Embodiment 2

[0050] S1: According to the molar ratio of 50:35:15, take platinum acetylacetonate, nickel acetylacetonate and dibutyl tin diacetylacetonate, and dissolve them in 5 mL of oleylamine solution to make the platinum precursor concentration 0.05 mol / L The solution. Under the protection of argon, the solution was stirred at 100 °C for 20 minutes, and the precursor salt was fully dissolved and mixed.

[0051] S2: Subsequently, at a heating rate of 5°C / min, the solution was heated to 260°C, and the reaction was continued for 1 hour, followed by centrifugal washing to obtain disordered platinum-nickel-tin ternary nanoparticles;

[0052] S3: Weigh a certain mass of carbon powder according to the metal loading of 20%, add a mixture of ethanol and hexane with a volume ratio of 2:1, and ultrasonically disperse, and then slowly drop into the disordered platinum nickel tin three meta-nanoparticles. After ultrasonication for a period of time, centrifuge, wash, and dry to obtain carbon-suppo...

Embodiment 3

[0055] S1: According to the molar ratio of 50:45:5, take platinum acetylacetonate, iron acetate and dibutyl tin diacetylacetonate, and dissolve them in 5 mL of oleylamine solution to make a platinum precursor concentration of 0.01mol / L solution. Under the protection of argon, the solution was stirred at 130 °C for 20 minutes, and the precursor salt was fully dissolved and mixed.

[0056] S2: Subsequently, at a heating rate of 5°C / min, the temperature of the solution was raised to 260°C, the reaction was continued for 1 hour, and then centrifuged and washed to obtain disordered platinum-iron-tin ternary nanoparticles;

[0057] S3: Weigh a certain mass of carbon powder according to the metal loading of 10%, add a mixture of ethanol and hexane with a volume ratio of 2:1, and ultrasonically disperse, then slowly drop into the disordered platinum-iron-tin tricarbonate obtained in step S2 meta-nanoparticles. After ultrasonication for a period of time, centrifuge, wash, and dry to ...

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