Carbon-supported spinel material and preparation method and application thereof

A spinel, carbon-supported technology, applied in nanotechnology for materials and surface science, chemical instruments and methods, nanocarbon, etc., can solve the problem of inability to effectively control element distribution and chemical properties, manganese cobalt spinel catalyst Insufficient catalytic oxygen reduction activity, inability to effectively control element distribution, etc., to achieve the effect of improving controllability

Active Publication Date: 2019-05-03
惠州市亿纬新能源研究院
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] CN102082270A discloses a preparation method of a class of manganese spinel nanomaterials, including Co x mn 3-x o 4 , MgMn 2 o 4 , Mn 3 o 4 Nanoparticles, ZnMn 2 o 4 Hollow nanospheres, hollow microspheres or nanosheets, which are prepared by reducing MnO 2 prepared by reduction; although this scheme can prepare spinel and control the microscopic morphology of the product, it cannot effectively control the element distribution on the surface of the prepared spinel nanoparticles
[0004] CN104810518A discloses a cobalt-manganese series spinel nanomaterial and a preparation method thereof, the chemical general formula of the cobalt-manganese series spinel nanomaterial is Co 3-x mn x o 4 , where 1≤x≤2, including cubic phase nanoparticles and tetragonal phase nanoparticles, the particle size of the nanoparticles is 5-15nm, and the molar ratio of Co to Mn is 0.4-2.2:1; the preparation method is: Under normal pressure air atmosphere, the two-step method of oxidation precipitation and embedded crystallization is used to control the crystal phase and composition, so as to obtain cobalt-manganese spinel nanomaterials. Although this method can prepare cobalt-manganese spinel n...

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  • Carbon-supported spinel material and preparation method and application thereof
  • Carbon-supported spinel material and preparation method and application thereof
  • Carbon-supported spinel material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0074] (1) Ultrasonically disperse 60mg of carbon carrier (solid carbon spheres with a particle size of 30nm) in 15mL of cobalt acetate aqueous solution with a concentration of 17.04mmol / L, then add 0.5mL of ammonia water with a concentration of 14mol / L dropwise, and stir in an air atmosphere 10min, obtain solution A;

[0075] (2) adding dropwise 15mL concentration in the solution A that step (1) obtains is 17.04mmol / L manganese acetate aqueous solution, obtains solution B;

[0076] (3) Aging solution B at 60°C for 120min, then adding it into a 35mL closed reaction kettle, and performing solvothermal reaction at 150°C for 3h;

[0077] (4) The product of step (3) is naturally cooled to room temperature, centrifuged, washed and dried to obtain the carbon-loaded spinel material, which is recorded as the surface manganese and cobalt elements evenly distributed Mn 1.5 co 1.5 o 4 / C.

[0078] In the carbon-supported spinel material prepared in this example, the mass ratio of car...

Embodiment 2

[0080] In this example, the aging temperature of step (3) in Example 1 is replaced by 40°C, and the other conditions are exactly the same as those in Example 1, and a carbon-supported spinel material is prepared, which is recorded as the surface manganese enriched Mn 1.5 co 1.5 o 4 / C.

[0081] In the carbon-supported spinel material prepared in this example, the mass ratio of carbon carrier to spinel is 0.67:1, and the spinel is Mn 1.5 co 1.5 o 4 The nanoparticle has an average particle diameter of 20nm; the surface of the spinel nanoparticle is rich in manganese, and the molar ratio of manganese to cobalt on the surface is 1.35:1.

Embodiment 3

[0083]In this example, the aging temperature of step (3) in Example 1 is replaced by 80°C, and the other conditions are exactly the same as those in Example 1, and a carbon-supported spinel material is prepared, which is recorded as surface cobalt enriched with Mn 1.5 co 1.5 o 4 / C.

[0084] In the carbon-supported spinel material prepared in this example, the mass ratio of carbon carrier to spinel is 0.67:1, and the spinel is Mn 1.5 co 1.5 o 4 The nanoparticles have an average particle size of 20nm; the surface of the spinel nanoparticles is enriched in cobalt, and the molar ratio of manganese to cobalt on the surface is 0.5:1.

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Abstract

The invention relates to a carbon-supported spinel material and a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing a carbon support and a cobalt salt-containing solution, and then adding ammonium hydroxide to obtain a solution A; (2) adding a manganese salt solution into the solution A obtained in the step (1) to obtain a solution B; and(3) heating and ageing the solution B, and then conducting solvothermal reaction to obtain the manganese-containing cobalt-containing carbon-supported spinel material. By means of the method, effective composition of the carbon support and spinel can be achieved, and meanwhile, surface element distribution and chemical property of spinel nanoparticles in the obtained carbon-supported spinel material are effectively adjusted and controlled, so that oxygen reduction half-wave potential of the carbon-supported spinel material, which is prepared through the method, with evenly-distributed surfacemanganese and cobalt is up to 0.872 V.

Description

technical field [0001] The invention relates to the field of new energy materials, in particular to a carbon-supported spinel material and its preparation method and application. Background technique [0002] Spinel materials containing manganese and cobalt have a wide range of sources, and can be obtained using a variety of synthetic methods at temperatures below 200 °C (F.Cheng, et al.Nat.Chem., 2011,3,79 ; C.Li, etal.Nat.Commun., 2015, 6, 7345), and its raw material cost and manufacturing cost are relatively cheap. [0003] CN102082270A discloses a preparation method of a class of manganese spinel nanomaterials, including Co x mn 3-x o 4 , MgMn 2 o 4 , Mn 3 o 4 Nanoparticles, ZnMn 2 o 4 Hollow nanospheres, hollow microspheres or nanosheets, which are prepared by reducing MnO 2 It is prepared by reduction; although this scheme can prepare spinel and control the microscopic morphology of the product, it cannot effectively control the element distribution on the na...

Claims

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Application Information

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IPC IPC(8): C01G51/00C01B32/15B82Y30/00B01J23/889C25B1/16C25B11/06
Inventor 汪瀛庄林袁中直刘金成
Owner 惠州市亿纬新能源研究院
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