Preparation method of Cu-Ir alloy polyhedral nano cage

A technology of polyhedron and nanocage, which is applied in the field of preparation of Cu-Ir alloy nanocage particles, can solve the problems of high price and catalytic activity limitation, and achieve the effect of electrocatalytic activity of high oxygen generation reaction

Inactive Publication Date: 2016-06-15
JILIN UNIV
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Problems solved by technology

But IrO 2 The high price and limited catalytic activity limit its practical application

Method used

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  • Preparation method of Cu-Ir alloy polyhedral nano cage
  • Preparation method of Cu-Ir alloy polyhedral nano cage
  • Preparation method of Cu-Ir alloy polyhedral nano cage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: Preparation of elemental copper nanocrystals

[0036] Put 0.2mmol copper acetylacetonate and 5mL oleylamine into a round-bottomed three-neck flask, and gradually raise the temperature to 270°C under magnetic stirring and nitrogen protection. During the heating process, the color of the solution changes from dark green to orange. When 270°C was reached, it turned into a wine-red cloudy solution, indicating the formation of copper nanocrystals, and was then held at 270°C for 15 minutes. figure 1 , figure 2 and image 3 They are the X-ray diffraction pattern, the transmission electron microscope image and the high-resolution transmission electron microscope image of the elemental Cu nanocrystals prepared in this example, respectively. It can be seen that the obtained Cu templates are nearly spherical single crystal nanoparticles with a particle diameter of about 14 nm.

Embodiment 2

[0037] Example 2: Hollow Porous Structure Cu 1.1 Preparation of Ir nanocages

[0038] First, prepare a solution of iridium chloride oleylamine with a concentration of 0.2mol / L. The specific operation process is as follows: mix 0.2mmol iridium chloride powder and 1mL oleylamine into a 50mL round-bottomed three-necked bottle, and raise the temperature to 120°C under the protection of nitrogen. °C for 30 minutes.

[0039] According to Example 1, copper acetylacetonate was reacted in oleylamine at 270°C for 15 minutes and then rapidly dropped to 250°C, and then 1 mL of iridium chloride oleylamine solution with a prepared concentration of 0.2mol / L was taken out with a syringe and quickly injected into In the round-bottomed three-neck flask of Example 1, keep 250 DEG C for 2 hours, at this moment, the mixed solution turns into a black turbid liquid, indicating that the hollow Cu 1.1 Formation of Ir nanocage structures. Figure 4 , Figure 5 , Figure 6 and Figure 7 Respective...

Embodiment 3

[0040] Example 3: Cu with core-shell structure 1.4 Ir and Cu 2 Preparation of Ir nanoparticles

[0041] By changing the molar ratio (3:1 or 3:2) of the precursor copper acetylacetonate and iridium chloride, the preparation of Cu core Cu-Ir alloy shell nanoparticles can be realized. When the molar ratio of precursor copper acetylacetonate and iridium chloride is 3:1, Cu with core-shell structure is obtained 2 Ir, Figure 11 and Figure 12 Its transmission electron micrographs and high-resolution transmission electron micrographs. It can be seen that the obtained Cu 2 The particle size of Ir nanoparticles is uniform, there is a layer of Cu-Ir alloy shell on the surface and there are obvious etched pits. When the molar ratio of the precursor copper acetylacetonate and iridium chloride is 3:2, Cu with core-shell structure is obtained 2 Ir, Figure 13 and Figure 14 Its transmission electron micrographs and high-resolution transmission electron micrographs. It can be seen...

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Abstract

The invention belongs to the technical field of noble metal nano particle synthesis and especially relates to a preparation method of a Cu-Ir alloy polyhedral nano cage having high catalytic activity in water electrolysis for producing oxygen. The method includes the steps of adding copper acetylacetonate in oleamine, increasing the temperature gradually to 270 DEG C under magnetic stirring with protection by nitrogen gas, maintaining the temperature for 15 min, reducing the temperature to an injection temperature, injecting an oleamine solution of iridium chloride, and maintaining the injection temperature for 2 h to obtain the Cu-Ir alloy polyhedral nano cage. The method is simple and convenient. The Cu-Ir alloy polyhedral nano cage has high electrically catalytic activity in an oxygen production reaction.

Description

technical field [0001] The invention belongs to the technical field of noble metal nanoparticle synthesis, in particular to a method for preparing Cu-Ir alloy nanocage particles with high catalytic activity for electrolyzing water to produce oxygen. Background technique [0002] Using renewable intermittent power generation technologies, such as solar power and wind power, to electrolyze water is a very good way to produce hydrogen. Hydrogen produced in this way could store more electrical energy and reduce the use of fossil fuels. However, water electrolysis requires a high overpotential due to the high thermodynamic stability of water. Since the slow four-electron transfer process of the oxygen generation reaction in the electrolysis of water greatly reduces the efficiency of water splitting, in order to improve the electrolysis efficiency of water, it is very critical to prepare high-efficiency electrocatalysts for the oxygen generation reaction. In addition, acidic pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/02B22F9/24C25B1/04B82Y30/00B82Y40/00
CPCY02E60/36
Inventor 隋永明王超邹勃
Owner JILIN UNIV
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