Preparation method of nitrogen-doped graphene

A nitrogen-doped graphene and precursor technology, applied in the field of nitrogen-doped graphene preparation, can solve problems such as environmental pollution, polluting products, and difficulty in mass production of nitrogen-doped graphene, and achieve excellent performance and appearance. uniform effect

Active Publication Date: 2014-12-24
QINGDAO HAIYUAN IND
5 Cites 42 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Among them, the CVD method needs to use a metal catalyst, which will pollute the product, and it is not easy to mass-produ...
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Abstract

The invention relates to a preparation method of nitrogen-doped graphene. The preparation method comprises the following steps: adding raw materials of citric acid and melamine into methanol, stirring, performing ultrasonic treatment and drying to obtain a precursor, and calcining the precursor in a tubular furnace by two stages to finally obtain the nitrogen-doped grapheme. Compared with the prior art, the preparation method has the following advantages: the raw materials are wide in source; the steps are simple; requirements on equipment are low; in the preparation process, a reducing agent is not required, so that environment pollution is low; the prepared nitrogen-doped graphene is thin in sheet, large in specific surface area, uniform in structure and good in reproducibility.

Technology Topic

Cvd grapheneTube furnace +10

Image

  • Preparation method of nitrogen-doped graphene
  • Preparation method of nitrogen-doped graphene
  • Preparation method of nitrogen-doped graphene

Examples

  • Experimental program(3)

Example Embodiment

[0018] Example 1
[0019] The first step, the specific steps of preparing the precursor are as follows: the precursor is prepared in the following way: take 1.1g of citric acid and 28.9g of melamine (molar ratio is 1:40), add it to 150ml of anhydrous methanol, and at room temperature with Stir at a rate of 1000 r/min for 10 min, put the sample into a probe-type ultrasonic processor, and sonicate for 10 min in an ice-water bath at a power of 20 kHz and 400 W. The ultrasonicated sample was taken out, heated in a water bath at 80°C and stirred at a rate of 1000 r/min until the sample had no obvious liquid water, moved into a blast drying oven, and dried at 80°C for 24 hours to obtain the desired precursor.
[0020] In the second step, the precursor calcination process is as follows: put the precursor sample obtained above into a boat-shaped crucible of 100 × 50 × 50 cm, cover it, and place it in a tube furnace under an inert gas atmosphere at a temperature of 6 °C/min. The heating rate was increased to 600 °C for 2 h, and then the heating rate was 7 °C/min to 1000 °C for 1 h, and it was cooled naturally.
[0021] In the third step, the calcined sample is taken out to obtain nitrogen-doped graphene.
[0022] like Figures 1 to 3 As shown, through XRD, SEM, BET, Raman, elemental analysis and other test analysis, the prepared sample is nitrogen-doped graphene with a pore size of 2.24 cm 3 /g, the specific surface area is 909m 2 /g, the nitrogen content is 11.3%.

Example Embodiment

[0023] Example 2
[0024] The first step, the specific steps of preparing the precursor are as follows: the precursor is prepared in the following way: take 1.2g of citric acid and 23.8g of melamine (molar ratio is 1:30), add it to 130ml of anhydrous methanol, and at room temperature with Stir at a rate of 800 r/min for 20 min, put the sample into a probe-type ultrasonic processor, sonicate for 15 min in an ice-water bath at a power of 20 kHz and 300 W. The sonicated sample was taken out, heated in a water bath at 70 °C and stirred at a rate of 800 r/min until the sample had no obvious liquid water, moved into a blast drying oven, and dried at 70 °C for 36 hours to obtain the desired precursor.
[0025] In the second step, the calcination process of the precursor is as follows: put the obtained precursor sample into a 100×50×50cm boat-shaped crucible, cover it, and place it in a tube furnace under an inert gas atmosphere at a temperature of 4°C/min. The heating rate was increased to 550 °C for 2.5 h, and then the heating rate was 5 °C/min to 900 °C for 1.5 h, and it was naturally cooled.
[0026] In the third step, the calcined sample is taken out to obtain nitrogen-doped graphene.
[0027] Through XRD, SEM, BET, Raman, elemental analysis and other tests and analysis, the prepared sample is nitrogen-doped graphene with an average pore volume of 1.05cm 3 /g, the specific surface area is 370m 2 /g, the nitrogen content is 25.5%.

Example Embodiment

[0028] Example 3
[0029] The first step, the specific steps of preparing the precursor are as follows: the precursor is prepared in the following manner: take 1.4g of citric acid and 18.6g of melamine (molar ratio of 1:20), add it to 100ml of anhydrous methanol, and at room temperature with Stir at a rate of 600 r/min for 30 min, put the sample into a probe-type ultrasonic processor, and sonicate for 20 min in an ice-water bath at a power of 20 kHz and 200 W. The ultrasonicated sample was taken out, heated in a water bath at 60 °C and stirred at a rate of 600 r/min until the sample had no obvious liquid water, moved into a blast drying oven, and dried at 60 °C for 48 hours to obtain the desired precursor.
[0030] In the second step, the precursor calcination process is as follows: put the obtained precursor sample into a 100 × 50 × 50 cm boat-shaped crucible, cover it, and place it in a tube furnace under an inert gas atmosphere at a temperature of 2 °C/min. The heating rate was increased to 500 °C for 3 h, and then the heating rate was 3 °C/min to 800 °C for 2 h, and it was cooled naturally.
[0031] In the third step, the calcined sample is taken out to obtain nitrogen-doped graphene.
[0032] Through XRD, SEM, BET, Raman, elemental analysis and other tests and analysis, the prepared sample is nitrogen-doped graphene with an average pore volume of 0.90cm 3 /g, the specific surface area is 423m 2 /g, the nitrogen content is 26.3%.
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PUM

PropertyMeasurementUnit
Average pore volume1.05cm³/g
Specific surface area370.0m²/g
Average pore volume0.9cm³/g
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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