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Preparation method for water phase of nitrogen-doped graphene

A nitrogen-doped graphene, water-phase preparation technology, applied in graphene, nano-carbon and other directions, can solve the problems of small specific surface area of ​​the product, high preparation difficulty and high cost, and achieves easy control of the reaction process and simple and easy preparation method. , the effect of low cost

Inactive Publication Date: 2012-08-01
NANJING UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of high toxicity and dangerous chemical reagents used in the current preparation method of nitrogen-doped graphene, high preparation difficulty, high cost, and small specific surface area of ​​the product, the present invention proposes a low-cost, fast, and large specific surface area of ​​the product. A new method for preparing nitrogen-doped graphene in aqueous phase

Method used

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  • Preparation method for water phase of nitrogen-doped graphene
  • Preparation method for water phase of nitrogen-doped graphene
  • Preparation method for water phase of nitrogen-doped graphene

Examples

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Embodiment 1

[0022] 1) Preparation method of raw material graphene oxide: analyze pure natural graphite powder after pre-oxidation and oxidation by improved Hummers' method (see: 1. Kovtyukhova, N.I.; Ollivier, P.J.; Martin, B.R.; Mallouk, T.E.; Chizhik, S.A.; Buzaneva, E.V.; ​​Gorchinskiy, A.D. Layer-by-Layer Assembly of Ultrathin Composite Films from Micron-Sized Graphite Oxide Sheets and Polycations. Chem. Mater. 1999, 11, 771-778; and 2. Hummers, W.S.; Offeman, R.E.Preparation of Graphic Oxide.J.Am.Chem.Soc.1958, 80, 1339~1339.), filtered and washed, the remaining viscous solid was put into dialysis bags, dialyzed until the pH value was close to neutral, and the obtained product was dried That is graphene oxide. Take 0.0300g of oxidized graphite and ultrasonically disperse it in 20mL of water to make a suspension of oxidized graphene with a concentration of 1.5mg / mL

[0023] 2) Mix and dissolve the oxidized graphene and urea at a mass ratio of 0.3, move it into a stainless steel react...

Embodiment 2

[0025] The preparation method of this example is the same as that of Example 1, but the hydrothermal reaction in step 2 is 150°C for 20 hours. Under the same conditions, a black product is also obtained—nitrogen-doped graphene with a nitrogen doping amount of 5.31 %.

Embodiment 3

[0027] The preparation method of this example is the same as that of Example 1. The mass ratio of the oxidized graphene suspension and urea in step 2 is 0.1. Under the same conditions, a black product is also obtained - nitrogen-doped graphene, nitrogen-doped The amount is 8.47%.

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Abstract

A preparation method for a water phase of nitrogen-doped graphene (NG) is characterized in that the preparation method comprises the following steps: mixing 0.5-5mg / mL oxidized graphene water suspension and solid urea as raw materials and dissolving, wherein the mass ratio of the oxidized graphene to the urea is 1 to 0.01; transferring the mixture into a stainless steel reaction kettle; feeding the stainless steel reaction kettle in a drying oven and carrying out constant temperature hydrothermal reaction at the reaction temperature of 150-200DEG C for 5-20 hours; naturally reducing the temperature to room temperature; taking out a sample and soaking or dialyzing with secondary deionized water; and removing the un-reacted urea; freezing and drying to obtain the nitrogen-doped graphene, wherein the nitrogen doping amount is 2.05-8.47 percent and the specific surface area is 450-550m<2> / g. According to the preparation method disclosed by the invention, the control over effective reduction of the nitrogen-doped graphene and the nitrogen doping ratio in the product can be realized by regulating and controlling the conditions such as the reaction temperature, the time, the ratio of a reactant and the like according to the requirement on the properties of products.

Description

technical field [0001] The invention relates to an aqueous phase preparation method of nitrogen-doped graphene, in particular to a method for preparing nitrogen-doped graphene with a large specific surface area by constant temperature hydrothermal reaction. Background technique [0002] Graphene is a zero-gap semiconductor material, and its application in microelectronic devices requires adjustment of its band gap or carrier concentration. Chemical doping is an effective way to adjust the physical and chemical properties of materials. For example, chemically doping graphene materials with electron-rich or electron-deficient elements or molecules can adjust the carrier concentration of graphene, thereby realizing its energy efficiency. Modulation of physical and chemical properties such as band width and catalytic properties. Theoretical research results show that the introduction of heteroatoms such as N and B into graphene sheets can effectively transform graphene from a z...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184
Inventor 夏兴华郑波
Owner NANJING UNIV
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