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Phosphorus and nitrogen co-doped iron monatomic carbon material as well as preparation method and application thereof

An atomic carbon and co-doping technology, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve the problems of limiting the large-scale use of noble metal single-atom catalysts, the reduction of catalyst activity and stability, and the high cost of noble metals. Achieve the effects of good battery power density, improved catalytic activity and stability, and improved catalytic activity

Active Publication Date: 2021-06-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the catalysts currently used in high-temperature fuel cell systems are still based on platinum carbon, but due to the competitive adsorption of phosphoric acid and oxygen at the active sites during the catalytic ORR reaction, and the existence of problems such as the corrosion of carbon substrates by toxic small molecules, Lead to passivation, detachment and burial of platinum components, which significantly reduces the activity and stability of the catalyst
[0005]At the same time, the high cost, limited reserves and easy poisoning of noble metals, which are non-renewable energy sources, severely limit the large-scale use of noble metal single-atom catalysts

Method used

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  • Phosphorus and nitrogen co-doped iron monatomic carbon material as well as preparation method and application thereof
  • Phosphorus and nitrogen co-doped iron monatomic carbon material as well as preparation method and application thereof
  • Phosphorus and nitrogen co-doped iron monatomic carbon material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] refer to figure 1 The flow chart of the preparation process is shown to illustrate the method of the present invention in detail.

[0051]Firstly, using formamide as nitrogen source and carbon source, adding the selected iron salt and zinc salt into formamide, and adding red phosphorus, sonicating until dissolved, and obtaining the hydrothermal reaction mother liquid. Wherein the iron salt is selected from anhydrous ferric chloride, and the zinc salt is selected from anhydrous zinc chloride, this is mainly because the self-polymerization of formamide cannot take place in the presence of water.

[0052] The purpose of adding zinc salt is to prevent metal elements from agglomerating. The added amount of the iron salt and the zinc salt is added in a ratio of 1 / 10 under the condition that a large amount of metal aggregates are not synthesized. Wherein said phosphorus powder selects red phosphorus, and its addition amount is equal to the molar concentration of iron salt. ...

Embodiment 2

[0056] This embodiment 2 provides a specific preparation method of nitrogen and phosphorus co-doped iron single-atom carbon material:

[0057] a: Take 30mL of formamide, add 0.04g of anhydrous ferric chloride, 0.204g of anhydrous zinc chloride and 0.0046g of red phosphorus into it, stir thoroughly and ultrasonically until dissolved.

[0058] b: transfer the solution obtained in a to a closed hydrothermal reactor, raise the temperature to 180° C., and react for 12 hours. After cooling, wash with water and ethanol three times respectively, and dry to obtain a solid material that successfully incorporates phosphorus and contains iron and zinc atoms.

[0059] c: Put the solid product obtained in b into a porcelain boat, and raise the temperature to 900°C at a rate of 5°C / min. At this temperature, react for 2 hours, and the zinc atoms will sublimate. After natural cooling, put the product at 80°C with The concentrated sulfuric acid oil bath was used for 6 hours to remove the iron ...

Embodiment 3

[0084] The nitrogen and phosphorus co-doped iron single-atom carbon material prepared in Example 2 was used for the preparation of a rotating disk electrode. The preparation method was as follows: take 5 mg of the catalyst material prepared in Example 2 and disperse it in 490 μ L DMF, add 10 μ L polytetrafluoroethylene Vinyl fluoride solution (20%, Aladdin's reagent), mix well, ultrasonic 30min. 10 μL of the prepared active material solution was evenly dropped on the glassy carbon electrode. The active material solution was dripped and dried before testing.

[0085] In addition, the nitrogen-doped iron single-atom carbon material prepared in Comparative Example 1 was used to prepare a rotating disk electrode, and the preparation method was as above.

[0086] Performance testing: test the CV and LSV polarization curves in 0.1M perchloric acid and 0.1M phosphoric acid solutions with the two electrodes prepared in Example 3 above and commercially available platinum carbon electr...

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Abstract

The invention belongs to the technical field of inorganic chemical industry, and particularly relates to a phosphorus and nitrogen co-doped iron monatomic carbon material as well as a preparation method and application thereof. The iron monatomic carbon material contains four elements of phosphorus, nitrogen, iron and carbon at the same time, iron is dispersed in an atomic scale, Fe atoms on a carbon-nitrogen substrate are averagely coordinated with four N atoms, and a P atom is averagely connected with the N atoms around each Fe-N4. The invention accidentally finds that by introducing the heteroelements N and P to regulate and control the electronic structure at the Fe-N4 active site, the stability of the active site can be improved while the activity of the catalyst is improved, and the tolerance of the catalyst to phosphoric acid is enhanced. Compared with an f-FeNC catalyst not doped with a P element and a commercially available platinum-carbon electrode, the ORR catalytic activity and stability of the synthesized f-FeNPC catalyst in a phosphoric acid system and a perchloric acid system are obviously improved, and when the synthesized f-FeNPC catalyst is used for preparing an oxyhydrogen fuel cell electrode material, the cell power density is high.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical industry, and in particular relates to a phosphorus-nitrogen co-doped iron single-atom carbon material and its preparation method and application. Background technique [0002] In 2011, Academician Zhang Tao from Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Professor Li Jun from Tsinghua University, and Professor Liu Jingyue from Arizona State University successfully synthesized a single-atom platinum (Pt) catalyst, and thus proposed the concept of "single-atom catalysis". Due to their unique physical and chemical properties and broad application prospects, single-atom catalysts have attracted extensive attention. Single-atom catalysts are considered ideal electrode materials due to their unique electronic structures, strong metal-support interactions, and unsaturated coordination structures that can achieve maximum metal utilization. [0003] However, the current...

Claims

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Application Information

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IPC IPC(8): C01B32/312H01M4/88H01M4/92
CPCC01B32/312H01M4/926H01M4/921H01M4/88Y02E60/50
Inventor 刘文李雅杰孙晓明曹子博
Owner BEIJING UNIV OF CHEM TECH
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