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Monatomic iron-based carbon material and preparation method and electrocatalytic application thereof

A carbon material, iron-based technology, used in circuits, electrical components, battery electrodes, etc., can solve the problems of complex process, low product yield, poor controllability of product morphology, etc., and achieves simple synthesis means and preparation technology. Simple, highly repeatable effects

Inactive Publication Date: 2019-03-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In summary, the disadvantages of the existing preparation of single-atom catalysts are that the process is complicated and special processes are used, and the many variable factors in the preparation process lead to poor controllability of product morphology, which limits the repeatability of experimental synthesis and the product yield. The rate is low, which is not conducive to the macro preparation of materials

Method used

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  • Monatomic iron-based carbon material and preparation method and electrocatalytic application thereof
  • Monatomic iron-based carbon material and preparation method and electrocatalytic application thereof
  • Monatomic iron-based carbon material and preparation method and electrocatalytic application thereof

Examples

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Effect test

Embodiment 1

[0038] Weigh 60mg of ferric ammonium citrate and dissolve it in 20mL of deionized water, then add 1.0g of ZIF-7, stir vigorously for 16 hours, centrifuge, wash and dry to obtain a yellow powder, then place 0.5g of the yellow powder in a horizontal Tube furnace, in argon atmosphere 50mL min -1 At flow rate, at 3°C ​​min -1 Raise the temperature to 600°C and keep it for 2 hours, then take it out after naturally cooling to room temperature. The resulting black solid was dissolved in 0.5mol L -1 HClO 4 solution, treated at 80°C for 10 hours, filtered, washed and dried to obtain a monoatomic iron-based carbon material with a product yield of 65%. The electron microscope appearance of the catalyst is as follows: figure 1 As shown in the figure, the product in this example does not have iron nanoparticles to generate, which proves that the anchoring effect of ZIF-7 on ferric ammonium citrate effectively avoids the accumulation of iron elements in the pyrolysis process, so that the...

Embodiment 2

[0041] Weigh 240 mg ferric ammonium citrate and dissolve it in 20 mL deionized water, then add 1.0 g ZIF-7, stir vigorously for 4 hours, centrifuge, wash and dry to obtain a yellow powder. Then 0.6g of yellow powder was placed in a horizontal tube furnace equipped with a quartz tube, in a helium atmosphere of 30mL min -1 At flow rate, at 5°C min -1 Raise the temperature to 900°C and keep it for 4 hours, then take it out after naturally cooling to room temperature. The resulting black solid was dissolved in 3mol L -1 h 2 SO 4 solution, treated at 70°C for 8 hours, filtered and washed with water, and dried to obtain a monoatomic iron-based carbon material catalyst with a product yield of 53%. The electron microscope appearance of the catalyst is as follows: image 3 It can be seen that even in the case of high ferric ammonium citrate feed, the molecular level dispersion of iron element can still be achieved, and the mass fraction of iron element corresponding to the catalyst...

Embodiment 3

[0043] Weigh 12 mg of ferric ammonium citrate and dissolve it in 20 mL of deionized water, then add 1.0 g of ZIF-7, stir vigorously for 24 hours, then centrifugally wash and dry to obtain a yellow powder. Then 0.5g of yellow powder was placed in a horizontal tube furnace equipped with a quartz tube, in a nitrogen atmosphere of 100mL min -1 At flow rate, at 3°C ​​min -1 Raise the temperature to 1100°C and keep it for 6 hours, then take it out after naturally cooling to room temperature. The resulting black solid was dissolved in 0.1mol L -1 HClO 4 solution, treated at 70°C for 12 hours, filtered, washed and dried to obtain a monoatomic iron-based carbon material with a product yield of 45%. The electron microscope appearance of the catalyst is as follows: Figure 4 As shown, although the pyrolysis temperature is as high as 1100 ° C, no iron nanoparticles appear, and the white bright spots in the figure illustrate the uniform dispersion of metal species, that is, the method p...

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Abstract

The invention discloses a monatomic iron-based carbon material and a preparation method and electrocatalytic application thereof. The preparation method includes dissolving ammonium iron acetate powder of certain mass in deionized water of specific volume, adding zeolite imidazole framework structural material ZIF-7, stirring violently for 4-24 hours, washing centrifugally, and drying to obtain yellow solid powder; placing the yellow solid powder of certain mass into a quartz boat, and placing the quartz boat into a horizontal tubular furnace with a quartz tube; heating to 600-1100 DEG C in aninert atmosphere, holding the temperature for 2-12 hours, and cooling naturally to room temperature; treating with an acid solution at the temperature of less than 90 DEG C for 8-25 hours, filtering,washing with water, and drying to obtain the monatomic iron-based carbon material. a precursor used herein has a wide range of origins; the preparation process is simple; batched macroscopic preparation can be carried out.

Description

technical field [0001] The invention relates to a method for preparing a single-atom iron-based carbon material through high-temperature pyrolysis and acid treatment processes, and its electrocatalytic application. Background technique [0002] Compared with traditional metal nanoparticle compounds, single-atom materials have a highly dispersed atomic structure, which makes them exhibit different characteristics in the field of electrochemistry and traditional catalysis. With the help of the rich specific surface area, pore structure and excellent electrical and thermal conductivity of the carbon substrate, single-atom iron-based carbon materials have broad application prospects in gas separation and adsorption, catalytic reactions, and electrochemical energy conversion processes. Research in related fields is increasing year by year. . Existing methods for preparing single-atom materials mainly include impregnation method, co-precipitation method, and template method. Thes...

Claims

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Application Information

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IPC IPC(8): H01M4/96H01M4/90H01M4/88
CPCH01M4/88H01M4/9041H01M4/96Y02E60/50
Inventor 汪国雄叶益凡阎程程包信和
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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