Carbon-loaded multi-metal multistage material as well as preparation method and application thereof

A technology of multi-element metals and metals, applied in the field of carbon-supported multi-element metal multi-level materials and its preparation, can solve the problem that the distance between electrochemical performance and catalytic performance is insufficient to meet the actual needs, lack of preparation methods for carbon-supported multi-element metal multi-level materials, and lack of different Problems such as the universality of metal sulfide loading, to achieve the effect of abundant reaction sites, good electrochemical performance, and multi-level structure promotion

Active Publication Date: 2021-01-05
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this technical solution prepares a multi-element metal multi-level structure composite material, it does not support carbon, does not have the universality of different metal sulfide loading, and does not simply form a multi-level structure, and the distance between electrochemical performance and catalytic performance There are still insufficient actual needs
[0004] In summary, the prior art still lacks a method for preparing carbon-supported multi-element metal multi-level materials

Method used

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  • Carbon-loaded multi-metal multistage material as well as preparation method and application thereof
  • Carbon-loaded multi-metal multistage material as well as preparation method and application thereof
  • Carbon-loaded multi-metal multistage material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In this embodiment, the inner template is prepared by the following method: cobalt nitrate hexahydrate (Co(NO 3 ) 2 ·6H 2 O, 1 mmol) and cetyltrimethylammonium bromide (CTAB, 0.0137 mmol) were dissolved in 10 ml of deionized water to form solution A. Solution B was formed by dissolving 4.54 g of 2-methylimidazole (2-MeIm) in 70 ml of deionized water. Pour solution A into solution B and stir vigorously for 20 min. After centrifugation and washing with ethanol, it was dried naturally at room temperature to obtain a purple powder, which is the inner template ZIF-67. The scanning electron microscope image of the appearance of ZIF-67 is attached figure 1 shown. From figure 1It can be seen that the catalyst described in the examples has obvious nano-cubic characteristics, the side length is about 600nm, and the surface is smooth, which proves the successful synthesis of the material.

[0041] Prepare metal salt solution, disperse sodium bicarbonate (SB, 3mM) and sodium...

Embodiment 2

[0048] The difference between this embodiment and Embodiment 1 is that this embodiment also includes step (4) for vulcanization, as described below.

[0049] (1) Ultrasonic disperse 200mg of ZIF-67 in 35ml of ethanol, stir in a water bath at 33°C, pour into solution C, and form cobalt-tungsten metal precipitation;

[0050] (2) Disperse meta-aminophenol (mAP, 200mg) in 10ml ethanol solution to form solution D, dissolve formaldehyde (HCHO, 0.3ml) into 10ml aqueous solution to form solution E, add solution D and solution E to step (1 ) in the solution obtained, reacted for 9 hours, centrifuged, washed and dried at room temperature to obtain a purple powder, which is the cobalt-tungsten metal precipitate ZIF-67 / CCH-CT-PmAP wrapped in a polymer.

[0051] (3) Carbonize ZIF-67 / CCH-CT-PmAP, and calcinate ZIF-67 / CCH-CT-PmAP in a tube furnace under an atmosphere of argon (flow rate of 100 sccm), with a heating rate of 2°C / min , the carbonization temperature was 500° C., and the carboni...

Embodiment 3

[0056] The difference between this embodiment and Embodiments 1 and 2 is that the inner and outer carbon layers are different, the carbonization reaction rate is different, and a hollow structure is also formed. The details are as follows.

[0057] (1) Weigh 1g of melamine and mix 1ml of formaldehyde, 0.27g of polyvinyl alcohol and 45ml of deionized water, add 5ml of aqueous solution in a water bath at 80°C and mix with 10mM and 20mM zinc chloride. After the solution became turbid, react for 8-10min. Centrifugal washing obtains melamine formaldehyde resin.

[0058] (2) Redisperse 0.5g of melamine-formaldehyde resin in 50ml of aqueous solution, add 100mg of dopamine hydrochloride, 0.695g of ferrous sulfate and 0.297g of cobalt chloride in an aqueous solution and react in a water bath at 60°C for 24 hours. The surface is covered with a layer of polydopamine, and at the same time, two metal sources of cobalt and iron are mixed.

[0059] (3) Under an argon atmosphere, heat up t...

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Abstract

The invention belongs to the technical field of multi-stage structure composite materials, and particularly relates to a carbon-loaded multi-metal multi-stage material and a preparation method and application thereof. The preparation method comprises the following steps: (1) adding a solvent into an inner-layer template for dissolving, and adding a first metal salt and a second metal salt for chemical precipitation reaction to form a multiphase metal precipitate; (2) continuously adding a polymer reaction monomer, and carrying out a polymerization reaction on the surface of the multiphase metal precipitate to form a polymer-coated multiphase metal precipitate; and (3) carbonizing the polymer-coated multi-phase metal precipitate to obtain the carbon-supported multi-metal multistage material. The invention provides a carbon-loaded multi-component sulfide multistage composite material synthesized in a surface-assisted manner, the purpose of controllable micro-nano structure is achieved based on different thermal behaviors of surface and internal components, the prepared carbon-based material has the advantages of good conductivity, rich reaction sites and the like, and when the carbon-based material is used as an oxygen reduction and oxygen evolution electrocatalyst, good electrochemical properties are provided.

Description

technical field [0001] The invention belongs to the technical field of multi-level structure composite materials, and in particular relates to a carbon-supported multi-element metal multi-level material and its preparation method and application. Background technique [0002] Micro-nano hierarchical structure materials not only maintain the high specific surface area of ​​nano-materials, but also have the characteristics of easy separation and high recycling of micro-materials, so they have potential application prospects in the fields of catalysis and adsorption. At present, the commercial application of noble metal catalysts such as platinum and ruthenium in terms of oxygen reduction and oxygen evolution performance is still difficult to replace. However, its earth abundance is low, it is expensive and has poor stability. Therefore, in order to reduce the cost and improve the application value, transition metal carbon materials have received some attention in recent years...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88H01M4/90H01M12/06
CPCH01M4/8825H01M4/9075H01M4/9041H01M12/06
Inventor 肖军武谢倩如李斌
Owner HUAZHONG UNIV OF SCI & TECH
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