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Preparation method of embedded porous Fe-Nx@Pd-NC nanorod, nanorod prepared by preparation method, and application of nanorod

An embedded and nanorod technology, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problem of not having high temperature resistance, difficult to construct Pd active centers synchronously, and Pd surface active sites Issues such as point count reduction

Active Publication Date: 2021-04-30
NANJING NORMAL UNIVERSITY
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  • Description
  • Claims
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Problems solved by technology

[0004] However, how to combine Pd-based nanomaterials and Fe-N x The high catalytic activity of -C nanomaterials is combined, and the design and synthesis have both Fe-N x Nanomaterials with Pd active centers still face great challenges
This is due to Fe-N x The preparation of -C nanomaterials often requires a high-temperature reduction method to obtain (>300°C), while most Pd nanomaterials often do not have high temperature resistance characteristics, and Pd nanoparticles are prone to agglomeration and reconstruction under high temperature conditions. and combined, resulting in a significant reduction in the number of active sites on the Pd surface
Therefore, it is difficult to realize Fe-N in the same synthesis system x and the simultaneous construction of the Pd active center

Method used

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  • Preparation method of embedded porous Fe-Nx@Pd-NC nanorod, nanorod prepared by preparation method, and application of nanorod
  • Preparation method of embedded porous Fe-Nx@Pd-NC nanorod, nanorod prepared by preparation method, and application of nanorod
  • Preparation method of embedded porous Fe-Nx@Pd-NC nanorod, nanorod prepared by preparation method, and application of nanorod

Examples

Experimental program
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Effect test

Embodiment 1

[0039] An embedded porous Fe-N X The preparation method of @Pd-NC nanorod, comprises the following steps:

[0040] 1) Preparation of metal precursor complex: weigh 0.15g naphthylamine (C 10 h 9 N), added to 30mL of water and ethanol mixed solvent (the ratio of water and ethanol is 10:1), fully ultrasonic to dissolve; then add 4mL 0.05mol L -1 PdCl 2 Aqueous solution, mix evenly, after standing still, centrifuge to remove the liquid and dry to get yellow flaky Pd(II)-naphthylamine complex powder (observed under a 200nm scale electron microscope, the product is flaky, and the product is yellow), and the product is tested by icp The mass fraction of Pd in ​​the medium is 10.1%;

[0041] 2) Preparation of the green rod-shaped intermediate product FePc@Pd-NC: Weigh 20 mg of the yellow powder prepared in step 1), and at the same time weigh 10 mg of FePc and disperse them in 40 mL of THF, stir for 24 hours, evaporate the solvent, and centrifuge to remove the liquid and dry it, th...

Embodiment 2

[0044] An embedded porous Fe-N X The preparation method of @Pd-NC nanorod, comprises the following steps:

[0045] 1) Preparation of metal precursor complex: weigh 0.15g naphthylamine (C 10 h 9 N), added to 30mL of water and ethanol mixed solvent (the ratio of water and ethanol is 10:1), fully ultrasonic to dissolve; then add 4mL 0.05mol L -1 PdCl 2 Aqueous solution, mixed evenly, centrifuged to remove liquid after standing and dried to obtain yellow flake Pd(II)-naphthylamine complex;

[0046] 2) Preparation of the green rod-shaped intermediate product FePc@Pd-NC: Weigh 20 mg of the yellow powder prepared in step 1), and at the same time weigh 20 mg of FePc and disperse them in 40 ml THF, stir for 24 hours, evaporate the solvent, and centrifuge to remove the liquid and dry it, that is Green rod-shaped intermediate product FePc@Pd-NC powder can be obtained;

[0047] 3) Embedded porous Fe-N X Preparation of @Pd-NC nanorods: the green powder prepared in step 1) was heated ...

Embodiment 3

[0049] An embedded porous Fe-N X The preparation method of @Pd-NC nanorod, comprises the following steps:

[0050] 1) Preparation of metal precursor complex: weigh 0.15g naphthylamine (C 10 h 9 N), added to 30mL of water and ethanol mixed solvent (the ratio of water and ethanol is 10:1), fully ultrasonic to dissolve; then add 4mL 0.05mol L -1 PdCl 2 Aqueous solution, mixed evenly, centrifuged to remove liquid after standing and dried to obtain yellow flake Pd(II)-naphthylamine complex;

[0051] 2) Preparation of the green rod-shaped intermediate product FePc@Pd-NC: Weigh 20 mg of the yellow powder obtained in step 1), and at the same time weigh 30 mg of FePc and disperse them in 40 ml of THF, stir for 24 hours, evaporate the solvent, and centrifuge to remove the liquid and dry it, that is Green rod-shaped intermediate product FePc@Pd-NC powder can be obtained;

[0052] 3) Embedded porous Fe-N X Preparation of @Pd-NC nanorods: the green powder prepared in step 1) was heat...

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Abstract

The invention discloses a preparation method of an embedded porous Fe-NX@Pd-NC nanorod, the prepared nanorod and application of the nanorod. The preparation method comprises the following steps: adding PdCl2 and naphthylamine into an ethanol aqueous solution, uniformly mixing, standing to generate a complex, dispersing the complex and FePc powder into a THF solvent, stirring, centrifugally drying, collecting solid powder, calcining at high temperature, and cooling to obtain the embedded porous Fe-NX@Pd-NC nanorod. The method is simple and easy to implement and low in raw material cost, large-scale production can be achieved, and the prepared Fe-NX@Pd-NC nanorod has the structural advantages of being large in specific surface area, good in electrical conductivity, high in permeability, resistant to high temperature and the like; and two high-activity metal sites, namely Fe-Nx and Pd, are simultaneously provided for driving the alkaline oxygen reduction reaction. Therefore, the Fe-NX@Pd-NC shows excellent catalytic activity and stability as an oxygen reduction cathode catalyst.

Description

technical field [0001] The invention belongs to oxygen reduction catalyst technology, in particular to a method for preparing embedded porous Fe-NX@Pd-NC nanorods and the prepared embedded porous Fe-N X @Pd-NC nanorods and applications. Background technique [0002] The cathode oxygen reduction reaction (ORR) is one of the important chemical reactions in clean energy devices, and its efficiency directly determines the electrochemical conversion efficiency of the entire device. At present, platinum-based catalysts have the highest catalytic activity for the cathode oxygen reduction reaction. However, platinum-based nanomaterials have disadvantages such as scarce resources, high price, susceptibility to methanol poisoning and loss of activity, and poor stability, which greatly hinder their large-scale commercial application. Based on this, the research and development of non-platinum electrocatalysts with high activity and high stability has broad application prospects and h...

Claims

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Application Information

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IPC IPC(8): H01M4/88H01M4/92B82Y30/00
CPCH01M4/926H01M4/8878B82Y30/00Y02E60/50
Inventor 邱晓雨林梓楠李佳甜唐亚文
Owner NANJING NORMAL UNIVERSITY
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