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Method for synthesizing heterogeneous atom doped carbon material through one-step process

A technology of carbon materials and heterogeneous phases, applied in the field of materials, can solve problems such as complex synthesis steps, high cost, carbon material morphology, structure influence, etc., and achieve the effects of simple preparation conditions, easy operation, and good oxygen reduction performance

Inactive Publication Date: 2014-05-14
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In situ synthesis methods often require special equipment, high temperature, and precise condition control, so the cost is high and the synthesis steps are complicated; while post-processing methods often require toxic substances as heterogeneous atomic sources (for example, nitrogen doping requires pyridine, dopamine, etc.) etc.), and the post-processing method often has a great influence on the morphology and structure of carbon materials
Therefore, how to prepare heterogeneous atom-doped carbon materials on a large scale at low cost and achieve precise control of their structures and properties is still facing great challenges.

Method used

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  • Method for synthesizing heterogeneous atom doped carbon material through one-step process
  • Method for synthesizing heterogeneous atom doped carbon material through one-step process
  • Method for synthesizing heterogeneous atom doped carbon material through one-step process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] First, 0.1 g of carbon nanotubes was added to 35 ml of deionized water, and ultrasonically dispersed for 1 h. Then, 5 ml of ammonia water was added to the suspension of carbon nanotubes, and ultrasonic dispersion was continued for 1 h. Then the suspension was transferred to a 50ml hydrothermal kettle and placed in an oven at 180°C for 24h. After the reaction was completed, the suspension in the hydrothermal kettle was centrifuged and washed several times with deionized water. Finally, freeze-dry the obtained solid to obtain nitrogen-doped carbon nanotubes. Its element mapping diagram is as follows Figure 7 As shown, it shows that nitrogen atoms were successfully doped, and no other impurities were introduced. The SEM photos before (A) and after (B) of water heating are as follows figure 1 As shown, the pore size distribution is shown in figure 2 As shown, the nitrogen adsorption-desorption curve is as follows image 3 It can be seen from these figures that the n...

Embodiment 2

[0042] First, 0.1 g of mesoporous carbon was added to 40 ml of deionized water, and ultrasonically dispersed for 1 h. Then 2 g of boric acid was added to the suspension of mesoporous carbon, and ultrasonic dispersion was continued for 1 h. Then the suspension was transferred to a 50ml hydrothermal kettle and placed in an oven at 180°C for 24h. After the reaction was completed, the suspension in the hydrothermal kettle was centrifuged and washed several times with deionized water. Finally, the obtained solid is freeze-dried to obtain boron-doped mesoporous carbon. The boron-doped mesoporous carbon prepared by the method is consistent with the mesoporous carbon before the hydrothermal reaction in terms of specific surface area, pore size distribution, crystallinity and other properties. The CV curves of the as-prepared boron-doped mesoporous carbon in oxygen (solid line) or nitrogen (dashed line) saturated 0.1M KOH aqueous solution are as follows Figure 5 It can be seen that...

Embodiment 3

[0044] First, 0.1 g of carbon black was added to 30 ml of deionized water, and ultrasonically dispersed for 1 h. Then add 10ml1g ml to the suspension of carbon black -1 Sodium sulfide, and continue ultrasonic dispersion for 1h. Then the suspension was transferred to a 50ml hydrothermal kettle and placed in an oven at 180°C for 24h. After the reaction was completed, the suspension in the hydrothermal kettle was centrifuged and washed several times with deionized water. Finally, the obtained solid is freeze-dried to obtain sulfur-doped carbon black. The sulfur-doped carbon black prepared by the method is consistent with the carbon black before the hydrothermal reaction in terms of specific surface area, pore size distribution, crystallinity and the like. The CV curves of the prepared sulfur-doped carbon black in oxygen (solid line) or nitrogen (dashed line) saturated 0.1M KOH aqueous solution are as follows Image 6 It can be seen that it has good oxygen reduction performanc...

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Abstract

The invention relates to a method for synthesizing a heterogeneous atom doped carbon material through a one-step process. The method comprises the following steps of uniformly dispersing a carbon material and a heterogeneous atom source into water and / or ethanol to obtain a mixed solution, and carrying out hydrothermal reaction at 120-200 DEG C for 12-48 hours to prepare the heterogeneous atom doped carbon material, wherein a heterogeneous atom comprises at least one of N, S, B, P and F. The heterogeneous atom doped carbon material prepared according to the method disclosed by the invention is doped with the heterogeneous atom, keeps the original properties of the carbon material, namely surface area, aperture distribution, crystal structure and the like are basically unchanged, has good oxygen reduction property, hydrogen storage property, carbon dioxide adsorption property and the like and can be used for the fields of fuel-cell catalysts, lithium batteries, supercapacitors, absorption, gas storage and the like.

Description

technical field [0001] The invention relates to the field of materials, in particular to a method for preparing carbon materials doped with heterogeneous atoms (nitrogen, sulfur, boron, phosphorus, etc.) by a one-step hydrothermal method. Background technique [0002] Micro-nano carbon materials such as carbon nanotubes, graphene, and mesoporous carbon have excellent properties different from bulk materials due to their unique structures, so they are used in energy storage, adsorbents, sensors, storage materials, catalytic materials, Supercapacitors have broad application prospects. Both theoretical and experimental studies have shown that the doping of heterogeneous atoms can change the crystal structure and electronic structure of carbon materials to improve their electrochemical performance, adsorption, and catalytic performance. The synthesis methods of heterogeneous atom-doped carbon materials mainly include in-situ synthesis and post-processing. In situ synthesis met...

Claims

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Application Information

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IPC IPC(8): C01B31/02B01J27/24B01J21/18B01J27/04H01M4/90C01B32/05
CPCY02E60/50
Inventor 陈立松崔香枝王永霞王敏张玲霞吴玫颖施剑林
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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