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A nanoporous copper/platinum core-shell structure catalytic electrode and its preparation method

A technology of nanoporous copper and core-shell structure, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, electrodes, etc. Difficulty in transfer and use, etc., to achieve the effect of simple preparation method, controllable size and continuous film structure

Active Publication Date: 2017-11-24
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The prior art discloses the preparation of Pt-based binary alloys by means of mechanical ball milling and vacuum stripping, and then dealloying and corroding the active components to obtain a nanoporous platinum-based structure (such as: CN103055895A), but the preparation process of this method Complicated and high energy consumption is not suitable for large-scale use
There are also some patents (such as: CN 100571865 C) to first prepare an aluminum-copper alloy precursor alloy, then dealloy and corrode the aluminum components to obtain nanoporous copper, and then soak and replace in platinum salt to obtain a copper / platinum core-shell structure. Although the method is simple to operate, the transfer and use of the obtained catalyst are difficult, discontinuous, and cannot be used in large blocks and on a large scale

Method used

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  • A nanoporous copper/platinum core-shell structure catalytic electrode and its preparation method
  • A nanoporous copper/platinum core-shell structure catalytic electrode and its preparation method
  • A nanoporous copper/platinum core-shell structure catalytic electrode and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1: the preparation of alloy precursor thin film

[0046] The alloy precursor thin film is prepared by magnetron sputtering. The equipment used is the TRP-450 high vacuum three-target magnetron coating system produced by Shenyang Scientific Instruments, Chinese Academy of Sciences. The coating quality is good and the operation is simple; the annealing equipment is Shenyang, Chinese Academy of Sciences. The scientific instrument TRP-450 high vacuum three-target magnetron coating system has its own substrate heating function.

[0047] Concrete preparation steps are as follows:

[0048] (1) The commercial copper foil substrate (with a copper content of more than 96%) was ultrasonically cleaned with acetone for 5 minutes to remove residual organic matter on the surface, and then ultrasonically cleaned with 20-fold concentrated hydrochloric acid for 5 minutes to remove surface oxides. Finally, anhydrous Ethanol removes residual solution ions on the surface and dri...

Embodiment 2

[0053] Embodiment 2: the preparation of nanoporous copper matrix

[0054] Cut the alloy precursor film prepared in Example 1 into a size of 1.0×0.5cm (it can be cut into different quantities according to needs), and put it into the prepared 1mol / L hydrochloric acid solution. The volume of the solution can be measured as needed , you need to pass N before putting in 2 Remove residual oxygen in the solution for 5 minutes, and then corrode in a water bath at 25°C for 12 hours. The obtained sample is cleaned with deionized water to obtain a nanoporous copper matrix.

[0055] The SEM image of the nanoporous copper matrix prepared in this embodiment is as follows Figure 4a and Figure 4b As shown, it can be seen from the figure that the diameter of the average nanopore of nanoporous copper is about 220nm, the film thickness of nanoporous copper is about 500nm, and the pore size distribution is uniform and the structure is continuous. decisive role.

Embodiment 3

[0056] Example 3: Preparation of nanoporous copper / platinum core-shell catalyst

[0057] The nanoporous copper matrix prepared in Example 2 is soaked in 0.5g / L of H 2 PtCl 6 In a platinum salt solution composed of 3g / L HCl, the soaking reaction time is 50min; after the reaction is completed, the sample is taken out, washed, and dried to prepare a nanoporous copper / platinum core-shell catalyst.

[0058] Material characterization and compositional analysis: the catalyst material prepared in this embodiment observes the microstructure with a scanning electron microscope (SEM), and uses an energy dispersive spectrometer (EDS) attached to the SEM to characterize the presence of platinum nuclei. The results are as follows: Figure 5a , Figure 5b and Figure 6 as shown, Figure 5a -b shows the formed core-shell structure. Compared with the original nanoporous copper structure, it will be found that the original dendrite and strip structure has become a spherical structure. It ca...

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Abstract

The invention discloses a method for preparing a nanoporous copper / platinum core-shell structure catalyst. The steps are as follows: (1) Preparing an alloy precursor film using a magnetron sputtering method. In the alloy precursor film, the Cu atomic percentage is 65 -70%, Al atomic percentage is 35-30%; (2) Place the prepared alloy precursor film in a hydrochloric acid solution, and dealloy it for 10-15h at a temperature of 20-30°C to obtain a nanoporous copper matrix ; (3) Soak the prepared nanoporous copper matrix in a platinate solution composed of 0.4-0.6g / L H2PtCl6 and 2-4g / L HCl. The soaking reaction time is 30-60min; after the reaction is completed, take out the sample , clean and dry, and a nanoporous copper / platinum core-shell structure catalyst is prepared. The invention also discloses the application of the catalyst in preparing catalytic electrodes. The nanoporous copper / platinum core-shell structure catalytic electrode of the present invention has a simple preparation method, excellent hydrogen evolution effect, and has commercial application prospects.

Description

technical field [0001] The invention belongs to the technical field of nano-metal material preparation, and in particular relates to a nano-porous copper / platinum core-shell structure catalytic electrode and a preparation method thereof. Background technique [0002] Noble metal platinum nanomaterials have excellent catalytic activity. In order to reduce costs and improve the use efficiency of noble metal catalytic electrodes, most noble metal catalytic electrodes are currently based on nanoporous material substrates to support noble metal catalysts, because nanoporous material substrates have a large ratio Surface area, good conductivity, such as porous conductive carbon, metal oxides, metal nano-nano balls, nanowires, etc. However, the core-shell structure of these catalytic electrodes is relatively complicated to manufacture, and their stability and controllability are poor, which limits their use to a certain extent. [0003] The method of chemical corrosion and electro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J35/02C25B11/08B01J35/00
CPCB01J23/8926C25B11/097B01J35/00B01J35/30
Inventor 司鹏超孙挥
Owner SHANDONG UNIV
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