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An embedded porous fe-n x Preparation method of @pd-nc nanorods and its prepared nanorods and applications

An embedded and nanorod technology, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problem that Pd nanoparticles are prone to agglomeration, reconstruction and merger, and it is difficult to construct Pd active centers synchronously , the reduction of the number of active sites on the surface of Pd, etc., to achieve excellent catalytic activity and stability, low cost of raw materials, and simple and easy methods

Active Publication Date: 2022-06-17
NANJING NORMAL UNIVERSITY
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  • Abstract
  • 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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  • An embedded porous fe-n <sub>x</sub> Preparation method of @pd-nc nanorods and its prepared nanorods and applications
  • An embedded porous fe-n <sub>x</sub> Preparation method of @pd-nc nanorods and its prepared nanorods and applications
  • An embedded porous fe-n <sub>x</sub> Preparation method of @pd-nc nanorods and its prepared nanorods and applications

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Experimental program
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Effect test

Embodiment 1

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

[0040] 1) Preparation of metal precursor complex: Weigh 0.15 g of naphthylamine (C 10 H 9 N), added to 30mL mixed solvent of water and ethanol (the ratio of water and ethanol is 10:1), fully ultrasonicated to dissolve; then add 4mL 0.05mol L -1 PdCl 2 Aqueous solution, mixed evenly, and centrifuged to remove the liquid after standing to dry to obtain a yellow flake Pd(II)-naphthylamine complex powder (observed under a 200nm electron microscope, the product was flake-like, and the product was yellow), and the product was tested by icp The mass fraction of Pd is 10.1%;

[0041] 2) Preparation of green rod-shaped intermediate FePc@Pd-NC: Weigh 20 mg of the yellow powder obtained in step 1), and simultaneously weigh 10 mg of FePc and disperse them in 40 mL of THF. After stirring for 24 h, the solvent was evaporated, and the liquid was removed by centrifugation. The green...

Embodiment 2

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

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

[0046] 2) Preparation of green rod-shaped intermediate product FePc@Pd-NC: Weigh 20 mg of the yellow powder obtained in step 1), and simultaneously weigh 20 mg of FePc and disperse them in 40 ml of THF. The green rod-like intermediate FePc@Pd-NC powder can be obtained;

[0047] 3) Embedded porous Fe-N X Preparation of @Pd-NC nanorods: The green powder obtained in step 1) was heated at 5 °C for min under nitrogen atmosphere. -1 Program the temperature to 600 °C for heat treat...

Embodiment 3

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

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

[0051] 2) Preparation of green rod-shaped intermediate product FePc@Pd-NC: Weigh 20 mg of the yellow powder obtained in step 1), and simultaneously weigh 30 mg of FePc and disperse them in 40 ml of THF. The green rod-like intermediate FePc@Pd-NC powder can be obtained;

[0052] 3) Embedded porous Fe-N X Preparation of @Pd-NC nanorods: The green powder obtained in step 1) was heated at 5 °C for min under nitrogen atmosphere. -1 Program the temperature to 600 °C for heat treat...

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Abstract

The invention discloses an embedded porous Fe-N X The preparation method of @Pd‑NC nanorods and the prepared nanorods and applications thereof, the preparation method comprises: adding PdCl to ethanol aqueous solution 2 and naphthylamine, mixed evenly and left to form a complex, dispersed with FePc powder in THF solvent and stirred, then centrifuged and dried, the solid powder was collected and calcined at high temperature, and embedded porous Fe-N could be obtained after cooling X @Pd‑NC nanorods. The method is simple and easy, the raw material cost is low, and large-scale production can be realized, and the prepared Fe-N X @Pd‑NC nanorods not only have structural advantages such as large specific surface area, good electrical conductivity, strong permeability, and high temperature resistance; but also have two highly active metal sites of Fe‑Nx and Pd to drive the basic oxygen reduction reaction. Therefore, Fe‑N X @Pd‑NC exhibits excellent catalytic activity and stability as an oxygen reduction cathode catalyst.

Description

technical field [0001] The invention belongs to the technology of oxygen reduction catalyst, and in particular relates to a preparation method of embedded porous Fe-NX@Pd-NC nanorods and the prepared embedded porous Fe-N X @Pd-NC nanorods and applications. Background technique [0002] 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 cathodic oxygen reduction reaction. However, platinum-based nanomaterials have disadvantages such as low resources, high price, inactivation due to methanol poisoning, and poor stability, which greatly hinder their large-scale commercial applications. Based on this, research and development of non-platinum electrocatalysts with high activity and high stability have broad application prospects and have bec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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