Preparation method of monodisperse platinum-series high-entropy alloy nanoparticle catalyst

A high-entropy alloy and nanoparticle technology, which is applied in the field of material chemistry, can solve the problems of element distribution not reaching the chemical distribution of elements, high synthesis temperature, and uneven particle size of high-entropy alloys, and achieve low cost, uniform element distribution, and preparation The effect of simple method

Active Publication Date: 2020-05-08
CHONGQING UNIV
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AI Technical Summary

Problems solved by technology

It has been reported in the literature that the high-entropy alloy was loaded on graphene for the first time by mechanical ball milling, and CoCrCuFeNi high-entropy alloy nanoparticles with a diameter of 9 nm immobilized on graphene were synthesized, but the high-entropy alloy synthesized by ball milling The particle size is not uniform, and the element distribution does not meet the target chemical distribution of the elements
[0004] However, another document reported that the metal precursor salt solution was reduced at a high temperature of 2000K, and PtPdNiAuFeCoCuSn high-entropy alloy nanoparticles with a diameter of 10nm were prepared by rapid annealing. The high-entropy alloy elements synthesized by this method were uniformly dispersed and the particle size distribution Uniform, but the synthesis temperature is too high to produce nanoparticles immobilized on conductive, surface-oxidized carbon support materials

Method used

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  • Preparation method of monodisperse platinum-series high-entropy alloy nanoparticle catalyst
  • Preparation method of monodisperse platinum-series high-entropy alloy nanoparticle catalyst
  • Preparation method of monodisperse platinum-series high-entropy alloy nanoparticle catalyst

Examples

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preparation example Construction

[0047] Wherein the preparation method of hard template silicon dioxide photonic crystal is as follows:

[0048] Mix deionized water and ethanol at a volume ratio of 1:6 in a round-bottomed flask, and add ammonia solution with a volume ratio of 1:0.5 to water, and continuously stir the resulting solution at 30°C for 30 min. Subsequently, tetraethyl orthosilicate with a volume ratio of 1:1 to water was added to the above mixed solution and continued to stir for 12 hours to obtain a milky white solution.

[0049] Take tetraethyl orthosilicate and ethanol with a volume ratio of 1:1, mix and transfer it to a constant pressure dropping funnel, and control the mixed solution to slowly drip into the above milky white solution at a rate of one drop every 3 seconds, and then further continuously Stir for 12 hours, and finally centrifuge wash the obtained product with a mixed solution of water and ethanol at a speed of 7000r for 7 minutes. After washing three times, disperse in the ethan...

Embodiment 1

[0054] A method for preparing a monodisperse platinum-based high-entropy alloy nanoparticle catalyst, comprising the following steps:

[0055] Step 1: According to the mass ratio of platinum acetylacetonate, nickel acetylacetonate, bis(iron dicarbonylcyclopentadienyl), copper stearate, zinc zirdene, and ethyl cobalt bis-salicylamido is 5:4:4:4:3 :3 Weigh and dissolve in tetrahydrofuran (THF) and CHCl 3 in the mixed solution.

[0056] Step 2: Weigh the block copolymer F127 with a mass ratio of 1:1:1, the carbon precursor solution and tetraethyl orthosilicate, prepare a hydrochloric acid solution with a substance amount of 0.7 mmol, and then add the obtained in step 1 in sequence The mixed solution was stirred for 30 min to obtain a transparent solution.

[0057] Step 3: Pour the transparent solution obtained in step 2 into a silica photonic crystal template, then place it in a vacuum oven at 30°C for 24 hours, then raise the temperature to 110°C for 11 hours, and then raise t...

Embodiment 2～8

[0061] The preparation methods of Examples 2-8 are the same as those of Example 1, except that, as shown in Table 1, the platinum precursors, other metal precursors, protonic acid solutions and process parameters used are different.

[0062] Wherein in embodiment 2, the mass ratio of platinum acetylacetonate, ruthenium acetylacetonate, iridium acetylacetonate, nickel acetylacetonate, two (iron dicarbonyl cyclopentadienyl), copper stearate, zinc zirdene, bis-salicylamidoethyl cobalt 5:2:3:3:4:4:4:3.

[0063] Platinum acetylacetonate, ruthenium acetylacetonate, iridium acetylacetonate, rhodium acetylacetonate, tin chloride acetylacetonate, nickel acetylacetonate, bis(iron dicarbonyl cyclopentadienyl), copper stearate, zinc zirdene, bis The mass ratio of ethyl cobalt salicylamide is 4:4:3:3:2:3:6:3:6:4.

[0064] Table 1

[0065]

[0066]

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Abstract

The invention relates to the technical field of material chemistry, and particularly discloses a preparation method of a monodisperse platinum-series high-entropy alloy nanoparticle catalyst. The preparation method comprises the steps: preparing a silicon dioxide photonic crystal template, preparing a carbon precursor solution, and dissolving a platinum precursor and at least four other metal precursors in THF and CHCl3 to obtain a mixed solution; mixing a block copolymer F127, a carbon precursor solution and tetraethyl orthosilicate, respectively adding the mixture and a protonic acid solution into the mixed solution, and stirring to obtain a transparent solution; adding the transparent solution into the silicon dioxide photonic crystal template, drying, heating and curing to obtain a purple brown solid; calcining the purple brown solid to obtain a gray solid; and etching the gray solid by adopting strong base or strong acid, filtering and drying. The monodisperse platinum-series high-entropy alloy nanoparticle catalyst with the advantages of controllable particle size, good dispersity, excellent performance and the like is obtained by adopting the preparation method disclosed bythe invention.

Description

technical field [0001] The invention relates to the technical field of material chemistry, in particular to a method for preparing a monodisperse platinum-based high-entropy alloy nanoparticle catalyst. Background technique [0002] Proton exchange membrane fuel cells (PEMFCs) have attracted extensive attention due to their high energy density and environmental friendliness. At present, the cost of fuel cells has been high in the application process. The reason is that the cathode oxygen reduction reaction (ORR) requires a large amount of Pt noble metal catalysts to accelerate the reaction process. Therefore, reducing the amount of Pt and improving the utilization of Pt is the solution to this problem. best solution to the problem. In order to achieve this goal, on the one hand, Pt is highly dispersed in the form of nano-scale particles on carbon supports to improve the utilization of Pt; on the other hand, replacing part of Pt with other metals (M) to prepare various Pt-ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/10
CPCB01J23/8953B01J35/0033B01J35/1004
Inventor 魏子栋张文静毛占鑫李静宋乐乐毛清蓉孙德恩
Owner CHONGQING UNIV
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