CN106587066A - Preparation method of ultrathin two-dimensional silicon carbide material - Google Patents

Preparation method of ultrathin two-dimensional silicon carbide material Download PDF

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Publication number
CN106587066A
CN106587066A CN201611048694.1A CN201611048694A CN106587066A CN 106587066 A CN106587066 A CN 106587066A CN 201611048694 A CN201611048694 A CN 201611048694A CN 106587066 A CN106587066 A CN 106587066A
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silicon carbide
thin
dimension
ultra
ultrathin
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林时胜
徐文丽
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention relates to a preparation method of an ultrathin two-dimensional silicon carbide material. The method includes the steps of: a) placing a clean silicon chip in a reaction furnace tube, increasing the temperature to 1200-1400 DEG C and vacuumizing the reaction furnace tube to 10<-5>-10<5> Pa, and feeding methane under a protective atmosphere to perform a reaction for 10-180 s; b) cooling the product to room temperature; c) dispersing the product in isopropanol and performing ultrasonic treatment for 10-30 min; and d) dropping the solution after the ultrasonic treatment on a copper mesh and air-drying the solution to form the ultrathin two-dimensional silicon carbide material. The method has simple processes. The ultrathin two-dimensional silicon carbide can reach 2-3 nm in thickness and 2 [mu]m in size. The two-dimensional silicon carbide has wide forbidden band and can stably exist; compared with graphene which has zero band gap and MoS2 that cannot stably exist, the ultrathin two-dimensional silicon carbide may provides a breakthrough for application in the technical fields of photoelectric detectors, solar cells and other photoelectric devices and nano-materials and the like.

Description

A kind of preparation method of ultra-thin two-dimension carbofrax material
Technical field
The present invention relates to a kind of preparation method of ultra-thin two-dimension carbofrax material, belongs to carbofrax material technology of preparing neck Domain.
Background technology
Graphene is a kind of cellular crystal structure of carbon atom of monolayer, is found to for the first time now from it, it The applied research of various electronic devices has been achieved for very big progress.Excellent performance, such as its load due to its uniqueness Stream transport factor can reach 200000cm2/ V*s, and not temperature influence, this is provided for preparation high-speed electronic components can Can property.Single-layer graphene is absorbed as 2.3% to light for another example, and this can become to it in photoelectric device research is important Material has played conclusive effect, and it is considered as to be expected to replace silicon materials always that these intentional performances all allow Graphene, is become The basic material of next generation's integrated circuit development.But Graphene has special band structure, its energy gap is zero, this Its application in optoelectronic devices is seriously constrained just.In recent years, many scientists open Graphene by various methods Band gap, wherein just including preparing graphene nanobelt and being doped Graphene.But these methods are to opening Graphene Can be with most can only also arrive 250meV, this data is to wanting that it is far from enough that Graphene is further applied in electronic device 's.Then, many scholars also actively seek in addition to Graphene the two-dimensional material of other excellent performances, it is desirable to equally can be with Among applying to field of optoelectronic devices research, such as molybdenum bisuphide and carborundum.But can reach compared to energy gap 1.5eV, is but easily oxidized, it is impossible to which the monolayer molybdenum bisuphide of stable existence, carborundum are partly led as a kind of important broad stopband Body, has obvious advantage.Likewise, studying the growth that the great problem for facing is exactly carborundum at present.If energy Ultra-thin two-dimentional silicon carbide structure is prepared enough, this would is that an extremely important breakthrough.
The content of the invention
It is an object of the invention to provide a kind of preparation method of simple ultra-thin two-dimension carbofrax material.
Realize that technical solution of the invention is：
The preparation method of the ultra-thin two-dimension carbofrax material of the present invention, it is characterised in that comprise the following steps：
1) it is Wafer Cleaning is clean, after removing the oxide layer of silicon chip surface, it is placed in reacting furnace；
2) with the ramp of 10 DEG C/min-30 DEG C/min to 1300 DEG C -1400 DEG C, the vacuum in reaction boiler tube is evacuated to 10-5-105Pa, is passed through methane under the atmosphere of protective gas hydrogen, reacts 3s-3min；
3) reacting furnace is cooled to by room temperature with the speed of 1 DEG C/min-500 DEG C/min；
4) product for obtaining is placed in isopropanol, ultrasonic disperse；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.
In above-mentioned technical proposal, further, described step 2) in the flow proportional of methane and hydrogen can be 1 to 2.
Further, described step 4) in the product for obtaining is placed in isopropanol, concentration can be arrived in 1mg/L 10mg/L。
Further, described step 3) in ultrasonic time can be 10min to 30min.
The present invention is had an advantageous effect in that compared with background technology：
Preparation process is simple of the present invention, obtained ultra-thin two-dimension carbonization silicon thickness can reach 2-3nm, and size can reach 2 μm. And prepared two-dimentional carborundum be it is a kind of with broad stopband and can stable existence material, compare Graphene zero band gap and Molybdenum bisuphide is unable to the shortcoming of stable existence, and the birth of ultra-thin two-dimension carborundum is that two-dimentional carborundum is applied to photodetection The technical field such as the photoelectric devices such as device, solaode and nano material provides foundation.
Description of the drawings
Fig. 1 is shape appearance figure of the ultra-thin two-dimension carborundum of embodiment 1 under Electronic Speculum；
Fig. 2 is the Raman spectrogram of the ultra-thin two-dimension carborundum of embodiment 1；
Fig. 3 is the atomic force microscopy diagram of the ultra-thin two-dimension carborundum of embodiment 1；Wherein scheme (a) to exist for ultra-thin carborundum Shape appearance figure under atomic force microscope, schemes (b) to scheme the apparent height curve of (a) cathetus position.
Specific embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1：
1) it is Wafer Cleaning is clean, use HF/H2(volume ratio is 1 to O:20) oxide layer of silicon chip surface, juxtaposition are thoroughly removed In the middle of reacting furnace；
2) with the ramp of 10 DEG C/min to 1300 DEG C, the vacuum in reaction boiler tube is evacuated to 10-5Pa, with 35sccm's Flow is passed through protective gas hydrogen, under this atmosphere is passed through methane with the flow of 50sccm, reacts 3s；
3) reacting furnace is cooled to by room temperature with the speed of 100 DEG C/min；
4) product for obtaining is scattered in isopropanol, solution is put into into ultrasound 20min in ultrasonic machine；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.
Fig. 1 is shape appearance figure of the ultra-thin two-dimension carborundum for obtaining under Electronic Speculum, and Fig. 2 is the Raman spectrogram of sample, from drawing What in graceful spectrogram, we can be apparent sees 797cm-1And 970cm-1Peak position, respectively it is corresponding be carborundum in TO and The Raman peak position of LO both directions, Fig. 3 is then the atomic force microscopy diagram of ultra-thin two-dimension carborundum, has (b) figure in Fig. 3 can be with Find out silicon carbide sample thickness be 2-3nm.
Embodiment 2：
1) it is Wafer Cleaning is clean, use HF/H2(volume ratio is 1 to O:20) oxide layer of silicon chip surface, juxtaposition are thoroughly removed In the middle of reacting furnace；
2) with the ramp of 20 DEG C/min to 1350 DEG C, the vacuum in reaction boiler tube is evacuated to 10-5Pa, with 30sccm's Flow is passed through protective gas hydrogen, under this atmosphere is passed through methane with the flow of 40sccm, reacts 8s；
3) reacting furnace is cooled to by room temperature with the speed of 150 DEG C/min；
4) product for obtaining is scattered in isopropanol, solution is put into into ultrasound 20min in ultrasonic machine；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.
Embodiment 3：
1) it is Wafer Cleaning is clean, use HF/H2(volume ratio is 1 to O:20) oxide layer of silicon chip surface, juxtaposition are thoroughly removed In the middle of reacting furnace；
2) with the ramp of 10 DEG C/min to 1400 DEG C, the vacuum in reaction boiler tube is evacuated to 10Pa, with 30sccm's Flow is passed through protective gas hydrogen, under this atmosphere is passed through methane with the flow of 60sccm, reacts 10s；
3) reacting furnace is cooled to by room temperature with the speed of 100 DEG C/min；
4) product for obtaining is scattered in isopropanol, solution is put into into ultrasound 30min in ultrasonic machine；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.
Embodiment 4：
1) it is Wafer Cleaning is clean, use HF/H2(volume ratio is 1 to O:20) oxide layer of silicon chip surface, juxtaposition are thoroughly removed In the middle of reacting furnace；
2) with the ramp of 30 DEG C/min to 1300 DEG C, the vacuum in reaction boiler tube is evacuated to 10Pa, with 50sccm's Flow is passed through protective gas hydrogen, under this atmosphere is passed through methane with the flow of 70sccm, reacts 60s；
3) reacting furnace is cooled to by room temperature with the speed of 100 DEG C/min；
4) product for obtaining is scattered in isopropanol, solution is put into into ultrasound 30min in ultrasonic machine；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.
Embodiment 5：
1) it is Wafer Cleaning is clean, use HF/H2(volume ratio is 1 to O:20) oxide layer of silicon chip surface, juxtaposition are thoroughly removed In the middle of reacting furnace；
2) with the ramp of 15 DEG C/min to 1350 DEG C, the vacuum in reaction boiler tube is evacuated to 10-1Pa, with 40sccm's Flow is passed through protective gas hydrogen, under this atmosphere is passed through methane with the flow of 60sccm, reacts 60s；
3) reacting furnace is cooled to by room temperature with the speed of 150 DEG C/min；
4) product for obtaining is scattered in isopropanol, solution is put into into ultrasound 20min in ultrasonic machine；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.

Claims (4)

1. a kind of preparation method of ultra-thin two-dimension carbofrax material, it is characterised in that comprise the following steps：
1) it is Wafer Cleaning is clean, after removing the oxide layer of silicon chip surface, it is placed in reacting furnace；
2) with the ramp of 10 DEG C/min-30 DEG C/min to 1300 DEG C -1400 DEG C, the vacuum in reaction boiler tube is evacuated to 10-5- 105Pa, is passed through methane under the atmosphere of protective gas hydrogen, reacts 3s-3min；
3) reacting furnace is cooled to by room temperature with the speed of 1 DEG C/min-500 DEG C/min；
4) product for obtaining is placed in isopropanol, ultrasonic disperse；
5) solution after ultrasound is dripped and is dried on copper mesh, obtain ultra-thin two-dimension carbofrax material.
2. the preparation method of ultra-thin two-dimension carbofrax material according to claim 1, it is characterised in that described step 2) Middle methane is 1-2 with the flow proportional of hydrogen.
3. the preparation method of ultra-thin two-dimension carbofrax material according to claim 1, it is characterised in that described step 4) Middle product is placed in isopropanol, and concentration is 1mg/L-10mg/L.
4. the preparation method of ultra-thin two-dimension carbofrax material according to claim 1, it is characterised in that described step 3) Middle ultrasonic time is 10min to 30min.
CN201611048694.1A 2016-11-23 2016-11-23 Preparation method of ultrathin two-dimensional silicon carbide material Pending CN106587066A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108715450A (en) * 2018-08-09 2018-10-30 中国电子科技集团公司第十三研究所 The preparation method of two-dimentional SiC material layer
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
WO2021242509A1 (en) * 2020-05-26 2021-12-02 Unm Rainforest Innovations Two-dimensional silicon carbide materials and fabrication methods thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942696A (en) * 2010-07-15 2011-01-12 四川大学 Si-base reversed extension 3C-SiC monocrystal film and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942696A (en) * 2010-07-15 2011-01-12 四川大学 Si-base reversed extension 3C-SiC monocrystal film and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
S.S.LIN: "Light-Emitting Two-Dimensional Ultrathin Silicon Carbide", 《J.PHYS.CHEM.C》 *
SHISHENG LIN ET AL.: "Quasi-Two-Dimensional SiC and SiC2: Interaction of Silicon and Carbon at Atomic Thin Lattice Plane", 《J. PHYS. CHEM. C》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108715450A (en) * 2018-08-09 2018-10-30 中国电子科技集团公司第十三研究所 The preparation method of two-dimentional SiC material layer
CN108715450B (en) * 2018-08-09 2020-09-22 中国电子科技集团公司第十三研究所 Preparation method of two-dimensional SiC material layer
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
CN109954509B (en) * 2018-12-04 2021-11-02 山东科技大学 Preparation method and application of silicon carbide-based photocatalyst
WO2021242509A1 (en) * 2020-05-26 2021-12-02 Unm Rainforest Innovations Two-dimensional silicon carbide materials and fabrication methods thereof

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