Preparation method of sulfur-containing carbon material as well as sulfur-containing carbon material prepared by using same

A technology of carbon materials and sulfur content, applied in the preparation/purification of carbon, nano-carbon, graphene, etc., can solve the problem of low sulfur content in sulfur doping

Active Publication Date: 2013-11-20
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sulfur-doped sulfur they obtained is still relatively low, and there is still a lot of work to be done in terms of preparation methods and product properties.

Method used

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  • Preparation method of sulfur-containing carbon material as well as sulfur-containing carbon material prepared by using same
  • Preparation method of sulfur-containing carbon material as well as sulfur-containing carbon material prepared by using same
  • Preparation method of sulfur-containing carbon material as well as sulfur-containing carbon material prepared by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0097] Sulfur-containing graphene was prepared by chemical vapor deposition using basic magnesium sulfate whiskers as a template.

[0098] Basic magnesium sulfate whiskers were prepared by the method described in the document Journal of Inorganic Materials 2004, 19, 784, and 13.00 g of basic magnesium sulfate whiskers were calcined at 750°C for 1 hour as a template, and then poured into a vertical fluidization chamber with a diameter of 50 mm The bed reactor was fed with 0.4L / min argon and heated to 900°C at a rate of 15°C / min. L / min methane flow for 10 minutes, the molar ratio of argon to methane is 1:1. Take out the reaction product after naturally cooling to room temperature, and pickle the reaction product with hydrochloric acid solution (60% volume of concentrated hydrochloric acid + 40% volume of deionized water) at 50-100°C to remove the template agent and the metal oxidation generated during the reaction. The product was finally washed with deionized water until neutr...

Embodiment 2

[0101] Sulfur-containing graphene was prepared by using calcined basic magnesium sulfate whiskers as a template and chemical vapor deposition.

[0102] Basic magnesium sulfate whiskers were prepared by the method described in the document Journal of Inorganic Materials 2004, 19, 784, and then the basic magnesium sulfate whiskers were calcined at 750° C. for 1 h. The pore size distribution is between 1-100nm, and the whisker specific surface area is 58.2m 2 / g, the length of the whiskers is 30-90 μm, the width of the whiskers is 0.2-1.0 μm, and the aspect ratio of the whiskers is 30-450. Weigh 10.0 g of the calcined basic magnesium sulfate whisker template, feed 0.4 L / min argon into a vertical fluidized bed reactor with a diameter of 50 mm and raise the temperature to 900 °C at a rate of 15 °C / min, and the reactor Operate under normal pressure conditions, add template agent to the vertical fluidized bed reactor, then pass through 0.4L / min methane gas flow for 10 minutes, then ...

Embodiment 3

[0106] Sulfur-containing graphene was prepared by chemical vapor deposition using ethylene as the carbon source gas.

[0107] Adopt the process described in embodiment 2 to prepare calcined basic magnesium sulfate template agent, take by weighing 10.00g template agent, pass into 0.8L / min argon gas to the vertical fluidized bed reactor of 50mm diameter and 15 ℃ The temperature was raised to 650°C at a rate of 1 / min, and the reactor was operated under normal pressure conditions. The templating agent was added to the vertical fluidized bed reactor, and then 0.4L / min ethylene flow was introduced to react for 10 minutes, and then naturally cooled to room temperature. The reaction product was taken out, the acid washing and purification steps were the same as in Example 1, and 0.09 g of the final product was obtained after drying.

[0108] Figure 7b , Figure 8c and Figure 8d The scanning and transmission electron microscope pictures of the sulfur-containing graphene produced b...

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Abstract

The invention relates to a preparation method of a sulfur-containing carbon material as well as the sulfur-containing carbon material prepared by using the preparation method. The preparation method comprises the following steps of: with sulfate, sulfite or a calcined product of the sulfate or the sulfite as a template agent, and reacting with a carbon source through a gas phase chemical deposition method or a groove liquid phase impregnation method so as to prepare sulfur-containing graphene or porous carbon. The sulfur content of the prepared sulfur-containing graphene or porous carbon is 0.1-30% in percentage by mass. By using the gas phase chemical deposition method or the groove liquid phase impregnation method, sulfur-containing graphene or porous carbon can be prepared in batch. The operation condition of the method is easy to control and the operation cost is low.

Description

technical field [0001] The invention belongs to the technical field of preparation of novel carbon materials, and in particular relates to a method for preparing sulfur-containing carbon materials and the prepared sulfur-containing carbon materials. Background technique [0002] In recent years, more and more scientific workers have conducted in-depth research on the doping of carbon materials. For example, the important reason why graphene can be applied to microelectronic devices is the tunability of its carrier concentration and carrier polarity, and chemical doping is just an important way to achieve this regulation. Wei et al. adopted CH 4 and NH 3 As the raw material, nitrogen-doped few-layer graphene was grown on the surface of copper film at 800°C by chemical vapor deposition. Electrical measurements showed that N-doped graphene exhibited n-type semiconductor behavior. Dai Hongjie and others used the electrothermal reaction method to dope N atoms on the boundaries...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B31/04C01B32/05C01B32/184C01B32/186
Inventor 宁国庆马新龙高金森
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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