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In situ embedding of binary transition metal nanoparticles into porous nitrogen-doped carbon spheres and its preparation method

A technology of transition metals and nanoparticles, applied in the direction of carbon preparation/purification, nanotechnology, nanotechnology, etc., can solve the problems of limiting the application of negative electrode materials, not being effectively used, and limitations, etc., to achieve universality and benefit Adsorption, low cost effect

Active Publication Date: 2020-08-07
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the current modification of phenolic resin carbon spheres is limited to the surface, such as the preparation of shell cores, cladding structures, etc., and most of the internal areas have not been effectively utilized, which limits their use as photo / electrocatalysts and lithium / sodium Application of negative electrode materials for ion batteries

Method used

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  • In situ embedding of binary transition metal nanoparticles into porous nitrogen-doped carbon spheres and its preparation method
  • In situ embedding of binary transition metal nanoparticles into porous nitrogen-doped carbon spheres and its preparation method
  • In situ embedding of binary transition metal nanoparticles into porous nitrogen-doped carbon spheres and its preparation method

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Embodiment 1

[0039] Step 1: Add transition metal nitrate cobalt nitrate and nickel nitrate in a molar ratio of 1:1 to the hydroalcoholic solution mixed with deionized water and absolute ethanol in a volume ratio of 1:0.4, and stir ultrasonically for 0.5h to obtain a concentration of 3mmol / L solution A;

[0040] Step 2: Take melamine and resorcinol with a mass ratio of 1:0.8, mix them evenly, add them to solution A, and stir magnetically at a stirring rate of 500r / min for 40min to obtain suspension B, wherein the mass-volume ratio of melamine to solution A is For 1g: 170mL;

[0041]Step 3: According to the volume ratio of formaldehyde solution and solution A is 1:80, take the formaldehyde solution and add it to the suspension B drop by drop at a rate of 2 s / drop, and stir while adding, at a rate of 100r / min Stir magnetically for 10 minutes to obtain suspension C. According to the volume ratio of ammonia water and formaldehyde solution of 1:0.9, take ammonia water and add it dropwise to sus...

Embodiment 2

[0050] Step 1: Add transition metal nitrate cobalt nitrate and ferric nitrate in a molar ratio of 1:1.2 to the hydroalcoholic solution mixed with deionized water and absolute ethanol in a volume ratio of 1:0.6, and stir ultrasonically for 1 hour to obtain a concentration of 8 mmol / L solution A;

[0051] Step 2: Take melamine and resorcinol with a mass ratio of 1:1.2, mix them evenly, add them to solution A, and magnetically stir at a stirring rate of 400r / min for 60min to obtain suspension B, wherein the mass-volume ratio of melamine to solution A For 1g: 150mL;

[0052] Step 3: According to the volume ratio of formaldehyde solution to solution A is 1:170, take formaldehyde solution and add it dropwise to suspension B at a rate of 3 s / drop, and stir while adding, at a rate of 200r / min Stir magnetically for 20 minutes to obtain suspension C. According to the volume ratio of ammonia water and formaldehyde solution as 1:2, take ammonia water and add it dropwise to suspension C ...

Embodiment 3

[0056] Step 1: Add transition metal nitrate cobalt nitrate and silver nitrate at a molar ratio of 1:0.9 to the hydroalcoholic solution mixed with deionized water and absolute ethanol at a volume ratio of 1:0.5, and stir ultrasonically for 0.8 hours to obtain a concentration of 5mmol / L solution A;

[0057] Step 2: Take melamine and resorcinol with a mass ratio of 1:1 and mix them evenly, then add them to solution A, stir magnetically at a stirring rate of 550r / min for 35min to obtain suspension B, wherein the mass-volume ratio of melamine to solution A For 1g: 120mL;

[0058] Step 3: According to the volume ratio of formaldehyde solution and solution A is 1:100, take the formaldehyde solution and add it to the suspension B drop by drop at a rate of 2 s / drop, and stir while adding, at a rate of 150r / min Stir magnetically for 15 minutes to obtain suspension C. According to the volume ratio of ammonia water and formaldehyde solution as 1:1, take ammonia water and add it dropwise ...

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Abstract

The invention relates to a porous nitrogen-doped carbon spheres in which binary transition metal nanoparticles are embedded in site and a preparation method of the carbon spheres. A mixed solution ofwater and alcohol is adopted as a solvent, two different transition metal nitrates are adopted as metal sources, melamine is adopted as a nitrogen source, and ammonia is adopted as a catalyst; in theprocess of a polycondensation reaction of resorcinol and formaldehyde, the binary transition metal nanoparticles and nitrogen are introduced in site, and by synergistically controlling the concentration, ratio, dropping rate and other parameters of the inary transition metal nanoparticles and nitrogen, a porous nitrogen-doped carbon sphere structure in which the binary transition metal nanoparticles are embedded in site is prepared. According to the method, the reaction process is simple and easy to control, large equipment and harsh reaction conditions are not needed, the universality is achieved, and the formation of the binary transition metal nanoparticles and the in-situ growth of the nanoparticles near and inside the nitrogen-doped carbon spheres in the reaction process can be directly achieved.

Description

technical field [0001] The invention relates to the field of nano-powder material preparation, in particular to a binary transition metal nanoparticle in-situ embedded porous nitrogen-doped carbon sphere and a preparation method thereof. Background technique [0002] As a cheap and controllable spherical carbon material, phenolic resin carbon spheres have been widely used in the field of photo / electrocatalysis and lithium / sodium ion batteries. However, their poor activity hinders their further development. At the same time, the introduction of non-metallic N and Non-precious metals can effectively improve their performance. Among numerous non-noble metal materials, transition metals (TM) such as Fe, Co, Ni, Mn, and Cu and their alloys are widely regarded as a promising class of noble metals due to their unique 3d electron orbitals and natural advantages of low price. candidate material. Incorporation of TMs into alloys not only preserves various advanced properties of diff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05C22C1/04B22F9/16B82Y30/00
CPCB22F9/16B22F2009/165B82Y30/00C01B32/05C22C1/0433
Inventor 李军奇宋倩茜李烀王少兰刘晓旭庞凌燕刘辉何选盟
Owner SHAANXI UNIV OF SCI & TECH
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