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ZIFs derived metal nitride/carbon composite material and preparation method and application thereof

A carbon composite material and composite material technology, applied in the field of ZIFs-derived metal nitride/carbon composite material and its preparation, can solve the problems of poor electrical conductivity, limited amplification and industrialization, long preparation cycle, etc. The effect of improving the content and performance indicators

Active Publication Date: 2019-10-18
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, limited by the structure and composition of the nitride itself, most of the nitrides prepared by conventional methods are bulk, with poor electrical conductivity. The synthesis conditions of high temperature and high pressure also pose great challenges to production equipment and energy consumption. And the preparation cycle is long, which limits the scale-up and industrialization

Method used

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  • ZIFs derived metal nitride/carbon composite material and preparation method and application thereof
  • ZIFs derived metal nitride/carbon composite material and preparation method and application thereof
  • ZIFs derived metal nitride/carbon composite material and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0055] A kind of preparation method of ZIFs derived metal nitride / carbon composite material, such as figure 1 Shown is a schematic diagram of the synthesis of ZIFs-derived metal nitride / carbon composites prepared in Example 1 of the present invention, including: Synthetic NiCo 2 o 4 , then NiCo 2 o 4 Co in the high-temperature molten state is assembled with 2-methylimidazole to form ZIF-67, and then further nitrided, the specific steps are as follows:

[0056] (1) Weigh 248.84mg (1mM) of nickel acetate tetrahydrate, 498.12mg (2mM) of cobalt acetate tetrahydrate and 2.37g (30mM) of ammonium bicarbonate, respectively, and disperse them in a mixed solution of 15mL deionized water and 35mL ethylene glycol , add a stirrer, and use a magnetic stirrer to stir evenly for 30 minutes at room temperature;

[0057] (2) Put the uniformly mixed solution into a 50mL polytetrafluoroethylene reactor, set the oven parameters to 200°C, and conduct a hydrothermal reaction for 12 hours. After...

Embodiment 2

[0067] A kind of preparation method of ZIFs derived metal nitride / carbon composite material, such as Figure 4 As shown, it is a schematic diagram of the synthesis of ZIFs-derived metal nitride / carbon composite material (Ni-CoN / NC in the figure) prepared in Example 2 of the present invention, and the steps (1)-(3) to prepare NiCo 2 o 4 The same as the preparation process of Example 1, the difference is:

[0068] (4) Weigh 200mg NiCo 2 o 4 1. 5g polyvinylpyrrolidone (PVP), put into a beaker with 50mL methanol, add a stir bar, and stir at room temperature for 30min on a magnetic stirrer;

[0069] (5) Weigh 0.8924g of zinc nitrate hexahydrate and dissolve it in 10mL of methanol, weigh 4g of 2-methylimidazole and dissolve it in 30mL of methanol, and quickly pour the methanol solution of 2-methylimidazole into the methanol of zinc nitrate hexahydrate In the solution, stir at room temperature for 30 minutes and then let it stand for 3 hours, then pour it into the methanol soluti...

Embodiment 3

[0082] A method for preparing a ZIFs-derived metal nitride / carbon composite material is basically the same as in Example 2, except that in step (5), 1.7848 g of zinc nitrate hexahydrate and 8 g of 2-methylimidazole are used. The obtained ZIFs-derived metal nitride / carbon composite is designated as sample 3.

[0083] Such as Figure 15 Shown is the oxygen reduction performance comparison chart of the samples prepared in Example 1, Example 2 and Example 3. It can be seen from the figure that the onset potential of sample 2 is about 0.95V (vs.RHE), and the half-wave potential is 0.77 V(vs.RHE), the limiting current density is about 5.0mA cm -2 , showing optimal oxygen reduction activity, indicating that an appropriate proportion of nitrogen reacts with metals in this example to obtain metal nitrides, and adding an appropriate proportion of 2-methylimidazole forms nitrogen-doped carbon compounds with abundant pore structures. To a certain extent, the number of active sites is in...

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Abstract

The invention discloses a ZIFs derived metal nitride / carbon composite material and a preparation method and application thereof. The method comprises the steps: NiCo2O4 nano-spheres and 2-methylimidazole are mixed and ground and sintered at the temperature of 700-900 DEG C in the mixture gas of ammonia and inert gas so as to obtain the composite material; or a zinc salt and the 2-methylimidazole are added to a methanol solution to obtain a ZIFs precursor, the ZIFs precursor is added the methanol solution of the NiCo2O4 -spheres and the dispersant to be stirred and separated to obtain the solid, the solid is heated to 700-900 DEG C under the protection of the inert gas and sintered in the mixture gas of ammonia and the inert gas and then cooled under the protection of the inert gas after sintering and thus the composite material is obtained. The method effectively avoids the agglomeration of metal particles and the structural collapse of ZIFs in the nitriding process, significantly speeds up the electron conduction rate and improves the reaction efficiency.

Description

technical field [0001] The invention relates to a metal nitride / carbon composite material and a preparation method thereof, in particular to a ZIFs (Zeolitic Imidazolate Frameworks, zeolitic imidazolate framework material) derived metal nitride / carbon composite material and a preparation method thereof. Background technique [0002] A fuel cell is a device that can directly convert the chemical energy of fuel into electrical energy. It has a relatively high energy conversion rate and is highly efficient and environmentally friendly during operation. It has been successfully applied to the energy supply of portable mobile devices and vehicles. The cathode oxygen reduction reaction (ORR) of the fuel cell has relatively high requirements on the catalyst. Whether the reaction process is a 4-electron or 2-electron process mainly depends on the inherent electrocatalytic properties of the catalyst. For a given electrocatalyst, a highly selective 4-electron process leads to better e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/86H01M4/88
CPCH01M4/8878H01M4/8647Y02E60/50
Inventor 王瑞林张洁陈金伟王刚罗艳
Owner SICHUAN UNIV
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