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Preparation method for electro-catalyst with shell-core structure

A technology of core-shell structure and electrocatalyst, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, structural parts, etc., can solve the problems of difficult catalyst cleaning process, cumbersome steps, environmental damage, etc., and achieve the convenience of large-scale production, The effect of simplifying the preparation process and reducing the preparation cost

Inactive Publication Date: 2017-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent 201210120922.7 discloses a method, using ethylene glycol, a high-boiling organic substance, as a solvent and a protective agent, and reducing platinum on the surface of carbon-supported palladium-copper nanoparticles at a temperature above 80°C. carbon-supported core-shell copper-palladium-platinum catalyst, but did not give the electrocatalytic performance test results
The steps are cumbersome, and the metal lost by alloying increases the cost and causes damage to the environment
U.S. Patent 2012 / 0135862A1 discloses a method, using amine-based organics as a reducing agent, ether-based organics as a solvent, the use of high-boiling point organics brings difficulties to the cleaning process of the catalyst; and the core of the core-shell structure must contain palladium, One of copper or iridium, the elements of the shell cannot exceed platinum, gold or iridium, limiting the elemental composition of the core-shell structure

Method used

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  • Preparation method for electro-catalyst with shell-core structure
  • Preparation method for electro-catalyst with shell-core structure
  • Preparation method for electro-catalyst with shell-core structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Take 50mg of Pd / C (BASF) in a three-necked flask, wherein the mass fraction of Pd is 20%; add 50.0mL of a mixed solution of deionized water and ethanol, wherein the volume ratio of water to ethanol is 3:1; stir and Sonicate until Pd / C is evenly dispersed in the solution.

[0034] 2. Pass H2 into the above solution with a flow rate of 100mL / min 2 / N 2 Mixed gas, where H 2 with N 2 The volume ratio is 5:95, while stirring at room temperature for 1 hour; add 1300 μL of 50.0 mM H 2 PtCl 6 aqueous solution, in H 2 / N 2 React under a mixed atmosphere for 24 hours, centrifuge, wash, and dry to obtain a Pd@Pt / C catalyst.

[0035] figure 1 It is the TEM figure of the Pd / C adopted in embodiment one; figure 2is the particle size distribution histogram of the corresponding Pd nanoparticles.

[0036] image 3 TEM image of Pd@Pt / C prepared for Example 1; Figure 4 is the particle size distribution histogram of the corresponding Pd@Pt nanoparticles.

Embodiment 2

[0044] 1. Take 70mg of Pd / C (BASF) in a three-neck flask, wherein the mass fraction of Pd is 20%; add 50.0mL of ethylene glycol; stir and sonicate until Pd / C is evenly dispersed in the solution.

[0045] 2. Into the above solution into the flow rate of 400mL / min H 2 / Ar mixed gas, where H 2 The volume ratio to Ar was 50:50 while stirring at 100 °C for 0.5 h; add 2600 μL of 50.0 mM K 2 PtCl 4 aqueous solution, in H 2 The reaction was carried out under a mixed atmosphere of Ar / Ar for 1 hour, centrifuged, washed and dried to obtain a Pd@Pt-2 / C catalyst.

[0046] Figure 10 and Figure 11 The cyclic voltammetry curves and oxygen reduction polarization curves of the Pd@Pt-2 / C prepared in Example 2 were obtained by the rotating disk electrode (RDE) test, respectively.

Embodiment 3

[0048] 1. Take 50mg of Pd / C (BASF) in a three-necked flask, wherein the mass fraction of Pd is 20%; add 50.0mL of deionized water; stir and sonicate until Pd / C is evenly dispersed in the solution.

[0049] 2. Into the above solution into the flow rate of 20mL / min H 2 / N 2 Mixed gas, where H 2 The volume ratio to Ar was 90:10 while stirring at room temperature for 0.2 h; add 1300 μL of 50.0 mM H 2 IrCl 6 aqueous solution, in H 2 / N 2 React under a mixed atmosphere for 1 hour, centrifuge, wash, and dry to obtain a Pd@Ir / C catalyst.

[0050] Figure 12 TEM image of Pd@Ir / C prepared for Example 2; Figure 13 is the particle size distribution histogram of the corresponding Pd@Ir nanoparticles.

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Abstract

The invention relates to a preparation method for an electro-catalyst with a shell-core structure. Specifically, shell-core structural metal nano-particles of which the surfaces are coated with platinum group metal are obtained by reducing one or more than one metal element, including the platinum group metal element, on the surfaces of the metal nano-particles which can adsorb the hydrogen with hydrogen as a reducing agent in a solution. The electro-catalyst material which is obtained by adopting the preparation method has a great application prospect in the aspect of proton exchange membrane fuel cells and electrolytic tanks.

Description

technical field [0001] The invention relates to a preparation method of an electrocatalyst with a core-shell structure. Background technique [0002] The core-shell structure is an effective way to reduce the loading of noble metals in the catalyst. In core-shell catalysts, the core is composed of non-noble metals and the shell is composed of noble metals, so that the reactive sites of noble metal atoms are fully exposed, the dispersion and utilization of noble metals are improved, and the content of noble metals in the catalyst is reduced. At present, the preparation methods of noble metal core-shell catalysts mainly include post-treatment method, replacement method, underpotential deposition method and seed growth method. [0003] Adzic et al. (L.Yang et.al., the Journal of Physical Chemistry C, 117(2013) 1748-1753) used the underpotential deposition method to deposit a single layer of copper on the surface of Ru nanoparticles, passing between K2PtCl4 and copper A single...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/46B01J23/89H01M4/92
CPCY02E60/50
Inventor 邵志刚曹龙生唐雪君秦晓平杨丽梦衣宝廉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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