Preparation method of monatomic metal-nitrogen doped carbon aerogel electrocatalyst

A carbon aerogel and electrocatalyst technology, which is applied to electrodes, circuits, electrolytic components, etc., can solve the problems of uneven distribution of iron, low activity, low electrocatalytic activity, etc., avoiding the pickling step, simple preparation method, Porous structure with high effect

Active Publication Date: 2021-11-02
NAT UNIV OF DEFENSE TECH
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Problems solved by technology

The patented mixture of ferric citrate and cyanamide is added to the alkaline phenolic resin sol, which is very easy to form iron hydroxide precipitation, which in turn leads to uneven distribution of iron and the formation of large iron particles, which catalyzes the acidic half wave of the oxygen reduction reaction. Potential less than 0.780V vs RHE, lower electrocatalytic activity
Pickling not only destroys some reactive sites, but also increases the complexity of the process
It has been reported that cracking resin aerogels to prepare metal-nitrogen-doped carbon aerogel materials mostly obtains metal nanoparticles, which do not have single-atom active sites, and the metal utilization rate is not high, and the active site distribution is low. Inhomogeneous and therefore less active, oxygen reduction half-wave potential below 0.700V vs RHE under acidic conditions and below 0.85V vs RHE under alkaline conditions

Method used

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  • Preparation method of monatomic metal-nitrogen doped carbon aerogel electrocatalyst
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  • Preparation method of monatomic metal-nitrogen doped carbon aerogel electrocatalyst

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preparation Embodiment 1

[0047] Such as figure 1 Shown, adopt the present invention to prepare embodiment 1 to comprise the following steps:

[0048] The first step, prepare organic solution or sol A, choose 1mol resorcinol ( figure 1 Organic matter in 2) and 2mol formaldehyde ( figure 1 The organic matter 1) in the solution was dissolved in 60mol deionized water and stirred until completely dissolved to form a uniform organic solution or sol A.

[0049] Second step, prepare metal complex solution or sol B, the iron chloride hexahydrate of 1 / 25mol ( figure 1 Inorganic metal salt in), be dissolved in dehydrated alcohol whose molar mass is 10 times, stir until completely dissolving, form ferric chloride inorganic salt solution ( figure 1 Inorganic metal salt solution). Select the epoxy chlorohydrin ( figure 1 The organic matter in 3) joins in the inorganic metal salt solution, continues to stir until the solution is clarified, prepares ferric chloride sol B ( figure 1 Metal complex solutions or so...

preparation Embodiment 2

[0057] Such as figure 1 Shown, adopt the present invention to prepare embodiment 2, comprise the following steps:

[0058] The first step, prepare organic solution or sol A, choose 1mol resorcinol (figure 1 Organic matter in 2) and 2mol formaldehyde ( figure 1 The organic matter 1) in the solution was dissolved in 60mol deionized water and stirred until completely dissolved to form a uniform organic solution or sol A.

[0059] Second step, prepare metal complex solution or sol B, the cobalt chloride hexahydrate of 1 / 25mol ( figure 1 Inorganic metal salt in), be dissolved in the dehydrated alcohol whose molar mass is 12 times, stir until completely dissolving, form the cobalt chloride inorganic salt solution ( figure 1 Inorganic metal salt solution). Choose epichlorohydrin whose molar mass is 8 times of the molar mass of cobalt chloride hexahydrate to join in the inorganic metal salt solution, continue to stir until the solution is clear, and prepare cobalt chloride sol B ( ...

Embodiment 2

[0065] The single-atom cobalt-nitrogen-doped carbon airgel electrocatalyst prepared in Example 2 has a very high catalytic oxygen evolution reaction activity, in 0.1mol / L potassium hydroxide solution, 10mA / cm 2 The corresponding potential is 1.635V vs RHE, and the half-wave potential difference with the oxygen reduction reaction is 0.710V. Figure 4 It is a spherical aberration transmission electron microscope photo of Example 2. The scale at the bottom of the electron microscope shows 2nm. The bright spot in the figure is the cobalt active site. The scale of the cobalt active site is much smaller than 1nm. It can be seen that it has an active catalytic site on a single-atom scale, and the utilization efficiency of cobalt is very high.

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Abstract

The invention discloses a preparation method of a monatomic metal-nitrogen doped carbon aerogel electrocatalyst, and aims to meet the urgent demand of the field of electrocatalysis on large-scale preparation of a low-cost and high-activity monatomic electrocatalyst. According to the technical scheme, the preparation method comprises the following steps: firstly, preparing an organic solution or sol A from aldehyde organic matters containing aldehyde groups, polyhydroxy benzene compounds or polyamino benzene compounds; preparing a metal complex solution or sol B from an inorganic metal salt and an organic matter which can generate a complex with the inorganic metal salt or can catalyze metal salt ions to form metal cation sol; mixing and heating A and B to obtain metal-doped organic matter gel C; removing liquid in the C to obtain metal-doped organic matter aerogel; and cracking the metal doped organic matter aerogel to obtain the monatomic metal-nitrogen doped carbon aerogel electrocatalyst. The acid pickling step is avoided, active sites are generated in one step in situ in the cracking process, the method is simple and low in cost, and the electrocatalyst prepared through the method is very high in catalytic activity.

Description

technical field [0001] The invention relates to the technical fields of carbon materials and electrochemistry, in particular to a method for preparing a single-atom metal-nitrogen-doped carbon airgel electrocatalyst. Background technique [0002] An electrocatalyst is a substance that changes the chemical reaction rate in an electrochemical reaction without changing the chemical balance, and its quality and chemical properties do not change before and after the chemical reaction. The operation of many energy storage and conversion devices is inseparable from the corresponding electrocatalysts. The cathodes of hydrogen fuel cells, methanol fuel cells, and metal-air batteries require electrocatalysts that catalyze the slow oxygen reduction reaction faster. The anode of the metal-air battery needs an electrocatalyst that catalyzes the reaction of water evolution to oxygen. Carbon dioxide electrolysis cells require carbon dioxide electroreduction electrocatalysts to reduce car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/04C25B1/04C25B3/26H01M4/88
CPCC25B11/04C25B1/04C25B3/26H01M4/8825Y02E60/50
Inventor 冯军宗冯坚罗燚姜勇刚李良军王鲁凯
Owner NAT UNIV OF DEFENSE TECH
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