CN104291339A - Preparation method of ultra-thin silicon carbide material - Google Patents
Preparation method of ultra-thin silicon carbide material Download PDFInfo
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- CN104291339A CN104291339A CN201410511422.5A CN201410511422A CN104291339A CN 104291339 A CN104291339 A CN 104291339A CN 201410511422 A CN201410511422 A CN 201410511422A CN 104291339 A CN104291339 A CN 104291339A
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Abstract
The invention relates to a preparation method of an ultra-thin silicon carbide material. The preparation method comprises the following steps: placing a silicon source and a carbon source in a reaction furnace tube in a manner that the silicon source is 0-100cm away from the carbon source; raising the temperature to 600 DEG C -2300 DEG C at a speed of 1 DEG C/min-300 DEG C/min, vacuumizing the reaction furnace tube until the vacuum degree is 10<-5>-10<5>Pa and reacting for 1-2880 minutes under a protective atmosphere; and then cooling to room temperature at a speed of 1 DEG C/min-500 DEG C/min to obtain the ultra-thin silicon carbide material. The preparation method disclosed by the invention is simple, the prepared ultra-thin silicon carbide (of which the thickness is below 5nm) is a two-dimensional material which has wide band gap and can maintain stable and the production of the ultra-thin silicon carbide material overcomes the disadvantages that graphene is free of band gap and the single-layer disulfide molybdenum cannot maintain stable. The ultra-thin silicon carbide material can be widely applied in the technical fields of quantum light sources, photoelectricity, semiconductor prototype devices, microelectronic circuits, RF devices, integrated circuits, photocatalysis, desalination of seawater, nanometer energy, composite materials and the like.
Description
Technical field
The present invention relates to a kind of preparation method of ultra-thin carbofrax material, belong to carbofrax material preparing technical field.
Background technology
Graphene is monoatomic layer carbon crystal material, its discovery confirms the stable existence of two-dimensional material and opens new stage of the research of two-dimensional material, particularly the photoelectric properties of its excellence cause the interest of numerous scientists, and 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, single-layer graphene 2.3% is absorbed as to light, 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.Usually ways such as preparing graphene nanobelt to be adopted to open being with of Graphene, but size can be with all at 300 below meV.Therefore, scientist is finding other more superior two-dimensional material a kind of to replace Graphene, such as the molybdenumdisulphide of two dimension, and this is the two-dimensional material that a kind of energy gap can reach 1.5eV; But the molybdenumdisulphide of individual layer can not stable existence, and easily oxidation by air, this also makes its utilization receive certain restriction.Silicon carbide is as an important wide bandgap semiconductor, and have wide application at optoelectronic areas, but the growth of silicon carbide faces a major issue, namely silicon carbide has more than 200 kind of allotropic substance.If we can prepare ultra-thin silicon carbide, so we can obtain the silicon carbide of single-phase.And according to Theoretical Calculation, monolayer carbon SiClx is direct energy-gap semiconductor.At present, not yet someone obtains ultra-thin and even individual layer silicon carbide structure in the world.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ultra-thin carbofrax material.
The technical solution realizing foregoing invention is:
The preparation method of ultra-thin carbofrax material, comprises the steps:
1) be positioned in reaction boiler tube by silicon source and carbon source at a distance of 0-100cm, the mole ratio of silicon source and carbon source is 100:1-1:100;
2) with the ramp to 600 of 1 DEG C/min-300 DEG C/min DEG C-2300 DEG C, it is 10 that reaction boiler tube is evacuated to vacuum tightness
-5-10
5pa, then passes into protective atmosphere, under protective atmosphere, react 1-2880min;
3) be cooled to room temperature with the speed of 1 DEG C/min-500 DEG C/min, obtain ultra-thin carbofrax material.
In the present invention, described silicon source can be silicon chip, Si powder, SiO 2 powder or silicon monoxide powder.Described carbon source can be graphene powder or graphite 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, and ultra-thin silicon carbide (below 5 nano thickness) a kind ofly has broad stopband and can the two-dimensional material of stable existence, and its birth overcomes Graphene does not have forbidden band and individual layer molybdenumdisulphide can not the shortcoming of stable existence.Ultra-thin two-dimension silicon carbide prepared by the present invention, has widespread use in multiple technical fields such as quantum light source, photoelectricity, semi-conductor antetype device, microelectronic circuit, radio-frequency devices, unicircuit, photochemical catalysis, sea water desaltination, the nanometer energy, matrix materials.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of ultra-thin silicon carbide under Electronic Speculum of embodiment 1;
Fig. 2 is the Raman spectrogram of the ultra-thin silicon carbide of embodiment 1;
Fig. 3 is the atomic force microscope figure of the ultra-thin silicon carbide of embodiment 1; Wherein: figure (a) is ultra-thin silicon carbide shape appearance figure under an atomic force microscope, figure (b) is the surface elevation curve of figure (a) cathetus position.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
1) Si powder mixed with graphene powder and be positioned in reaction boiler tube, the mole ratio of Si powder and graphene powder is 100:1;
2) with the ramp to 600 DEG C of 1 DEG C/min, it is 10 that reaction boiler tube is evacuated to vacuum tightness
-5pa, then passes into argon gas, reacts 10min under an argon atmosphere;
3) room temperature is cooled to the speed of 1 DEG C/min, sample is taken out, obtain ultra-thin carbofrax material, the shape appearance figure of the ultra-thin silicon carbide obtained under Electronic Speculum as shown in Figure 1, its Raman spectrogram as shown in Figure 2, atomic force microscope figure as shown in Figure 3, as seen from Figure 2, has obvious 796cm in the Raman spectrum of reaction product
-1peak position, the Raman peak position of corresponding silicon carbide, ultra-thin silicon carbide thickness is 1.5-2.5nm as seen from Figure 3.
Embodiment 2:
1) be positioned in reaction boiler tube by SiO 2 powder and graphene powder, the mole ratio of SiO 2 powder and graphene powder is 1:10, and both are at a distance of 10cm;
2) with the ramp to 1200 DEG C of 100 DEG C/min, it is 10 that reaction boiler tube is evacuated to vacuum tightness
-2pa, then passes into nitrogen, reacts 200min in a nitrogen atmosphere;
3) be cooled to room temperature with the speed of 100 DEG C/min, sample taken out, obtains the ultra-thin carbofrax material that thickness is 0.4nm.
Embodiment 3:
1) be positioned in reaction boiler tube by silicon monoxide powder and graphite, the mole ratio of silicon monoxide powder and graphite is 1:60, and both are at a distance of 60cm;
2) with the ramp to 1600 DEG C of 300 DEG C/min, it is 10 that reaction boiler tube is evacuated to vacuum tightness
-5pa, then passes into argon gas and hydrogen gas mixture, and mixed volume is than being 9:1; 1880min is reacted under argon gas and hydrogen atmosphere;
3) be cooled to room temperature with the speed of 400 DEG C/min, sample taken out, obtains the ultra-thin carbofrax material that thickness is 1.2nm.
Embodiment 4
1) be positioned in reaction boiler tube by silicon chip and graphite, the mole ratio of silicon chip and graphite is 1:100, and both are at a distance of 100cm;
3) with the ramp to 2000 DEG C of 200 DEG C/min, it is 10 that reaction boiler tube is evacuated to vacuum tightness
5pa, reacts and carries out under helium atmosphere, and the reaction times is 1440min;
4) be cooled to room temperature with the speed of 500 DEG C/min, sample taken out, obtains the ultra-thin carbofrax material that thickness is 1.6nm.
Embodiment 5
1) be positioned in reaction boiler tube by silicon chip and graphite, the mole ratio of silicon chip and graphite is 5:1, and both are at a distance of 50cm;
2) with the ramp to 2300 DEG C of 300 DEG C/min, it is 1000Pa that reaction boiler tube is evacuated to vacuum tightness, then passes into, nitrogen and hydrogen gas mixture, and mixed volume is than being 5:1; 1440min is reacted under nitrogen and hydrogen atmosphere;
3) be cooled to room temperature with the speed of 400 DEG C/min, sample taken out, obtains the ultra-thin carbofrax material that thickness is 2.0nm.
Claims (4)
1. a preparation method for ultra-thin carbofrax material, is characterized in that comprising the steps:
1) be positioned in reaction boiler tube by silicon source and carbon source at a distance of 0-100cm, the mole ratio of silicon source and carbon source is 100:1-1:100;
2) with the ramp to 600 of 1 DEG C/min-300 DEG C/min DEG C-2300 DEG C, it is 10 that reaction boiler tube is evacuated to vacuum tightness
-5-10
5pa, then passes into protective atmosphere, under protective atmosphere, react 1-2880min;
3) be cooled to room temperature with the speed of 1 DEG C/min-500 DEG C/min, obtain ultra-thin carbofrax material.
2. the preparation method of ultra-thin carbofrax material according to claim 1, is characterized in that described silicon source is silicon chip, Si powder, SiO 2 powder or silicon monoxide powder.
3. the preparation method of ultra-thin carbofrax material according to claim 1, is characterized in that described carbon source is graphene powder or graphite material.
4. the preparation method of ultra-thin carbofrax 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.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777124A (en) * | 2016-02-29 | 2016-07-20 | 中原工学院 | Method for preparing graphene in-situ growth silicon-carbide nanometer materials |
| CN107082415A (en) * | 2017-02-28 | 2017-08-22 | 杭州格蓝丰纳米科技有限公司 | A kind of preparation method of Ge-doped grapheme material |
| CN109954509A (en) * | 2018-12-04 | 2019-07-02 | 山东科技大学 | A kind of preparation method and application of silicon carbide-based photochemical catalyst |
| CN109999870A (en) * | 2019-03-21 | 2019-07-12 | 武汉工程大学 | A kind of silicon carbide/graphene nano sheet composite material and preparation method |
| CN110182808A (en) * | 2019-05-24 | 2019-08-30 | 武汉楚能电子有限公司 | A kind of method that silicon-carbon alkene preparation method and its photodegradation vapor water prepare hydrogen |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777124A (en) * | 2016-02-29 | 2016-07-20 | 中原工学院 | Method for preparing graphene in-situ growth silicon-carbide nanometer materials |
| CN105777124B (en) * | 2016-02-29 | 2018-03-30 | 中原工学院 | A kind of preparation method of graphene growth in situ silicon carbide nano material |
| CN107082415A (en) * | 2017-02-28 | 2017-08-22 | 杭州格蓝丰纳米科技有限公司 | A kind of preparation method of Ge-doped grapheme material |
| CN109954509A (en) * | 2018-12-04 | 2019-07-02 | 山东科技大学 | A kind of preparation method and application of silicon carbide-based photochemical catalyst |
| CN109999870A (en) * | 2019-03-21 | 2019-07-12 | 武汉工程大学 | A kind of silicon carbide/graphene nano sheet composite material and preparation method |
| CN109999870B (en) * | 2019-03-21 | 2022-01-11 | 武汉工程大学 | Silicon carbide/graphene nano sheet composite material and preparation method thereof |
| CN110182808A (en) * | 2019-05-24 | 2019-08-30 | 武汉楚能电子有限公司 | A kind of method that silicon-carbon alkene preparation method and its photodegradation vapor water prepare hydrogen |
| CN110182808B (en) * | 2019-05-24 | 2022-06-10 | 武汉楚能电子有限公司 | Preparation method of silicon-carbon alkene and method for preparing hydrogen by photolysis of water vapor |
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| CN104291339B (en) | 2016-08-17 |
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