CN104591168A - Preparation method of silicon-doped graphene material - Google Patents

Abstract

The invention discloses a preparation method of a silicon-doped graphene material. The preparation method of the silicon-doped graphene material comprises the following steps: positioning the graphene in a furnace tube, and pumping the furnace tube into the vacuum state, wherein the vacuum degree of the furnace tube is 10-5-105Pa; introducing protection atmosphere, and heating to 600-2300 DEG C at the heating speed of 1-300 DEG C/min; introducing silane into the furnace tube at the flow speed of 1-1000sccm, and reacting for 1-2880min; and cooling to room temperature and collecting the reaction product to obtain the silicon-doped graphene material. The silane is used as the silicon source, the reaction is carried out on the silane and the graphene under a cartain condition for preparing the silicon-doped graphene; compared with the zero band gap shortcomings of the graphene, the silicon-doped graphene can be used for opening the energy band of the graphene to be widely applied to the technical field of the micro and nano device and material preparation; the method is simple and is easy to realize.

Description

A kind of preparation method of silicon doping grapheme material

Technical field

The present invention relates to a kind of preparation method of silicon doping grapheme material, belong to technical field of material.

Background technology

The discovery of Graphene confirms the stable existence of two-dimensional material and opens new stage of the research of two-dimensional material, Graphene, as a kind of carbon material of monoatomic layer, has excellent photoelectric properties, causes the interest of scientist, such as its carrier mobility can reach 200,000 cm ²/ V.s, this electronics that can manufacture high-frequency operation for it provides the foundation, and single-layer graphene is absorbed as 2.3% to light, and this makes it can become a kind of important material of photoelectric device research.But while Graphene has excellent photoelectric characteristic, it has a very serious defect, and namely energy gap is zero, and this makes it there is certain restriction in the application of micro-nano opto-electronic device.In current experiment, ways such as preparing graphene nanobelt usually to be adopted to open being with of Graphene, but size can be with all at 300 below meV.In addition, scientists adopts the mode of doped graphene to regulate the fermi level of Graphene, thus changes electrical properties and the optical property of Graphene.In the mode of doping, usually adopt chemical doping and electrically doped mode, such as N doping, boron adulterate and add grid voltage doping etc.As time goes on the drawback of this kind of doping way can change in the character with the rear Graphene of doping, can not stable existence.Comparatively speaking, the displacement doping way that Siliciumatom substitutes the carbon atom in Graphene can keep the stable of doped graphene character more, and the Graphene of silicon doping not yet someone obtains at present.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of simple silicon doping grapheme material.

The technical solution realizing foregoing invention is:

The preparation method of silicon doping grapheme material, comprises the steps:

1) placing graphite alkene in boiler tube, it is 10 that reaction boiler tube is evacuated to vacuum tightness ^-5-10 ⁵pa.

2) continue to pass into shielding gas in boiler tube, with the ramp to 600 of 1 DEG C/min-300 DEG C/min DEG C-2300 DEG C, continue to pass into silane with the flow of 1-1000sccm in arrival temperature of reaction forward direction boiler tube, react after 1-2880 minute, stopping passes into silane;

3) be cooled to room temperature, collecting reaction product with the speed of 1 DEG C/min-500 DEG C/min, obtain silicon doping grapheme material.

Step 2 of the present invention) described in shielding gas can be one or several mixed gass in any proportion in argon gas, hydrogen, nitrogen and helium.

Preparation technology of the present invention is simple, easy to implement, the grapheme material stable performance of the silicon doping obtained, being with of Graphene can be opened by mixing Siliciumatom in Graphene, thus regulate electricity and the optical property of Graphene, and the stable in properties of Graphene of adulterating can be ensured, not passing in time and changing.Silicon doping Graphene prepared by the present invention can replace traditional metal catalyst in the reduction reaction such as oxygen reduction reaction, nitrogen protoxide, can also the micro-nano device such as widespread use and gas sensor field.

Accompanying drawing explanation

Fig. 1 is the Raman spectrogram of the Graphene of the silicon doping of embodiment 1;

Fig. 2 is the Raman spectrum of the original Graphene of embodiment 1;

Fig. 3 is the shape appearance figure of Graphene under transmission electron microscope of the silicon doping of embodiment 1;

Fig. 4 is the energy spectrogram of the Graphene of the silicon doping of embodiment 1.

Embodiment

The present invention is further illustrated below in conjunction with embodiment and accompanying drawing.

Embodiment 1

1) placing graphite alkene in boiler tube, it is 10 that reaction boiler tube is evacuated to vacuum tightness ^-5pa.

2) continue to pass into argon shield gas, with the ramp to 600 DEG C of 1 DEG C/min, then continue to pass into the silane that flow is 1sccm, after reaction 1min, stop passing into silane;

3) room temperature is cooled to the speed of 1 DEG C/min, obtain silicon doping grapheme material, the Raman spectrogram of the Graphene of the silicon doping obtained as shown in Figure 1, the Raman spectrum of original Graphene as shown in Figure 2, as can be seen from Fig. 1 and Fig. 2, (peak position is at 1354cm at the D peak of the Raman spectrum of the rear Graphene of reaction ^-1) intensity obviously become large, prove that Graphene is doped.As shown in Figure 3, energy spectrogram as shown in Figure 4, as can be seen from the figure, has the existence of silicon to the shape appearance figure of reaction product under transmission electron microscope in Graphene.

Embodiment 2:

1) placing graphite alkene in boiler tube, it is 10Pa that reaction boiler tube is evacuated to vacuum tightness.

2) continue to pass into hydrogen-argon-mixed, with the ramp to 1300 DEG C of 30 DEG C/min, then continue to pass into silane, the flow of silane is 100sccm, stops passing into silane after reaction 880min;

3) be cooled to room temperature with the speed of 30 DEG C/min, obtain silicon doping grapheme material.

Embodiment 3:

1) placing graphite alkene in boiler tube, it is 10 that reaction boiler tube is evacuated to vacuum tightness ²pa.

2) continue to pass into hydrogen, with the ramp to 1600 DEG C of 100 DEG C/min, then continue to pass into silane, the flow of silane is 300sccm, stops passing into silane after reaction 1440min;

3) be cooled to room temperature with the speed of 400 DEG C/min, obtain silicon doping grapheme material.

Embodiment 4

1) placing graphite alkene in boiler tube, it is 10 that reaction boiler tube is evacuated to vacuum tightness ⁴pa.

2) continue to pass into helium, with the ramp to 2000 DEG C of 300 DEG C/min, then continue to pass into silane, the flow of silane is 800sccm, stops passing into silane after reaction 2880min;

3) be cooled to room temperature with the speed of 500 DEG C/min, obtain silicon doping grapheme material.

Embodiment 5

1) placing graphite alkene in boiler tube, it is 10 that reaction boiler tube is evacuated to vacuum tightness ⁵pa.

2) continue to pass into helium protective atmosphere, with the ramp to 2300 DEG C of 15 DEG C/min, then continue to pass into silane, the flow of silane is 1000sccm, stops passing into silane after reaction 1200min;

3) be cooled to room temperature with the speed of 500 DEG C/min, obtain silicon doping grapheme material.

Claims (2)

1. a preparation method for silicon doping grapheme material, is characterized in that comprising the steps:

1) be placed in boiler tube by Graphene, being evacuated to vacuum tightness is 10 ^-5-10 ⁵pa;

2) continue to pass into shielding gas in boiler tube, with the ramp to 600 of 1 DEG C/min-300 DEG C/min DEG C-2300 DEG C, continue to pass into silane with the flow of 1-1000sccm in arrival temperature of reaction forward direction boiler tube, react after 1-2880 minute, stopping passes into silane;

3) be cooled to room temperature, collecting reaction product with the speed of 1 DEG C/min-500 DEG C/min, obtain silicon doping grapheme material.

2. the preparation method of silicon doping grapheme material according to claim 1, is characterized in that described shielding gas is one or several mixed gass in any proportion in argon gas, hydrogen, nitrogen and helium.