CN109399620A - A method of preparing the silicon carbide-based grapheme material of high mobility - Google Patents
A method of preparing the silicon carbide-based grapheme material of high mobility Download PDFInfo
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- CN109399620A CN109399620A CN201811477126.2A CN201811477126A CN109399620A CN 109399620 A CN109399620 A CN 109399620A CN 201811477126 A CN201811477126 A CN 201811477126A CN 109399620 A CN109399620 A CN 109399620A
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- silicon carbide
- grapheme material
- high mobility
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- carbon source
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
Abstract
The invention discloses a kind of methods for preparing the silicon carbide-based grapheme material of high mobility, it is the growth for carrying out grapheme material by chemical vapor deposition on silicon carbide substrates, using hydrogen and argon gas as carrier gas, it is passed through gaseous carbon source, nitrogen and gaseous state ethyl alcohol, 1-100min is grown under 1400-1800 DEG C, 500-1000mbar pressure, the silicon carbide-based grapheme material of the high mobility is made.Grapheme material surface folding density made from the method for the present invention is low, and carrier mobility is high, and square resistance inhomogeneities is low.
Description
Technical field
The present invention relates to grapheme material preparation technical fields, and in particular to a kind of to prepare the silicon carbide-based graphite of high mobility
The method of alkene material.
Background technique
Mobility is the important parameter for reflecting carrier conductive capability in semiconductor, in a semiconductor material, by certain original
Because the carrier of generation is in random warm-up movement, upon application of a voltage, carrier is acted on by electric field force, does directed movement
Electric current is formed, mobility is bigger, and carrier moving is faster, and the conductivity of semiconductor material is also higher.
Graphene is the hexagonal structure being made of carbon atom, can be widely applied to nano electron device, ultrahigh speed
The multiple fields such as computer chip, efficient energy storage, solid-state gas sensor, field emmision material and microelectronics is integrated.Stone
There are many preparation method of black alkene, and wherein chemical vapor deposition (CVD) method is to prepare a kind of important means of graphene.CVD preparation
In the process, since the Enhancing Nucleation Density of graphene is not easy to control, the crystallite dimension of the graphene of preparation is usually in several hundred nanometers to several
Between hundred microns, moreover, graphene is easy to produce defect in forming core and growth course, these are all very big to affect mobility
And electric conductivity.As Chinese patent application 107500278A discloses a kind of growth side for preparing low corrugation density grapheme material
Method, by the flow etc. of gaseous carbon source in modulated growth processes, although material surface corrugation density can be reduced to 0.1/μ
m2, but its mobility is still lower, is only capable of reaching 5000cm2/ Vs or so.
Summary of the invention
The problems such as graphene mobility is lower is prepared for prior art CVD, and the present invention, which provides, a kind of prepares high mobility
The method of silicon carbide-based grapheme material.
To achieve the above object of the invention, present invention employs the following technical solutions:
A method of the silicon carbide-based grapheme material of high mobility is prepared, is on silicon carbide substrates by chemical gas
The growth that mutually deposition carries out grapheme material is passed through gaseous carbon source, nitrogen and gaseous state ethyl alcohol using hydrogen and argon gas as carrier gas,
1-100min is grown under 1400-1800 DEG C, 500-1000mbar pressure, the silicon carbide-based graphene material of the high mobility is made
Material.
Preferably, it is put into chemical vapor depsotition equipment after the cleaned drying of the insulating substrate, is evacuated to≤10- 4mbar。
Preferably, the cleaning and drying method of the insulating substrate are as follows: insulating substrate uses the concentrated sulfuric acid, chloroazotic acid and hydrofluoric acid respectively
Solution heating cleaning, deionized water are rinsed, and are placed in dust guard after nitrogen gun drying, are dried in an oven.
Preferably, vacuum environment is warming up to 500-1100 DEG C, to remove substrate surface adsorbed gas.
Preferably, argon flow 1-20L/min, hydrogen flowing quantity 1-20L/min.
Preferably, the gaseous carbon source is methane, ethane, ethylene, acetylene or propane, flow 0.001-0.2L/
min。
Preferably, the ratio between flow of gaseous carbon source and hydrogen is 0.01%-1%.
Preferably, the flow of nitrogen is 0.05-1L/min.
Preferably, the flow of gaseous state ethyl alcohol is 0.001-1L/min
Preferably, after growth course, stop hydrogen, gaseous carbon source and nitrogen, continue to be passed through argon gas, keep pressure not
Become, drops to room temperature in ar gas environment.
The present invention is passed through gaseous state ethyl alcohol, hydrocarbon and water and institute is decomposed under high temperature during graphene growth
Gaseous carbon source interaction is stated, gaseous carbon source decomposition rate is influenced, controls graphene Enhancing Nucleation Density, adjusts grapheme material growth
The generation for the defects of global consistency can be effectively reduced material surface corrugation density, avoid hole in forming core and growth course,
Carrier mobility is improved, to improve the crystal quality and electrology characteristic of grapheme material.The present invention is on silicon carbide substrates
The grapheme material of CVD method growth is single layer p-type doped graphene, and with being not necessarily to, substrate is shifted, crystal quality is good, electrology characteristic
It is excellent and the advantages of easily combined with Si base semiconductor technique.
Specific embodiment
Technical solution in order to better illustrate the present invention is illustrated below by embodiment is further.
Embodiment 1
SiC substrate is selected, is rinsed respectively with the concentrated sulfuric acid, chloroazotic acid and hydrofluoric acid solution heating cleaning, deionized water, nitrogen gun
It is placed in dust guard after drying, dries in an oven.SiC substrate after cleaning-drying is put into CVD equipment, is evacuated to
≤10-4Mbar opens microwave power supply, and vacuum environment is warming up to 1100 DEG C, removes substrate surface adsorbed gas.It is passed through in reacting furnace
Hydrogen and argon gas are passed through propane as gaseous carbon source as carrier gas, and are passed through nitrogen and gaseous state ethyl alcohol, argon flow 3L/
Min, propane flow 0.022L/min, hydrogen flowing quantity 10L/min, C/H ratio be 0.22%, nitrogen flow 0.2L/min,
Gaseous state ethyl alcohol flow is 0.02L/min, and growth temperature is 1450 DEG C, growth pressure 900mbar, growth time 95min.It is raw
After length, microwave power supply is closed, stops hydrogen, gaseous carbon source and nitrogen, continues to be passed through argon gas, pressure keeps 900mbar not
Become, drops to room temperature in ar gas environment.The grapheme material of preparation is 1 layer, 0.1/μm of corrugation density <2, graphite Raman
2D peak width≤30cm-1, graphene mobility >=6,000cm2/ Vs, square resistance inhomogeneities≤5%.
Embodiment 2-3
Each control condition of embodiment 2-3 is as shown in the table, and not described part is same as Example 1.
| Condition | Embodiment 2 | Embodiment 3 |
| Carbon source | Methane | Ethylene |
| Temperature (DEG C) | 1400 | 1750 |
| Pressure (mbar) | 800 | 500 |
| Time (min) | 50 | 5 |
| Argon flow (L/min) | 18 | 10 |
| Carbon source flow (L/min) | 0.2 | 0.001 |
| Hydrogen flowing quantity (L/min) | 20 | 2 |
| C/H ratio | 1% | 0.05% |
| Nitrogen flow (L/min) | 0.95 | 0.05 |
| Gaseous state ethyl alcohol flow (L/min) | 0.9 | 0.002 |
Grapheme material made from embodiment 2 and embodiment 3 is respectively 3 layers and 1 layer, 0.1/μm of corrugation density <2, stone
Black alkene Raman 2D peak width≤30cm-1, graphene mobility >=6,000cm2/ Vs, square resistance inhomogeneities≤5%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of method for preparing the silicon carbide-based grapheme material of high mobility, it is characterised in that: pass through on silicon carbide substrates
The growth that chemical vapor deposition carries out grapheme material is passed through gaseous carbon source, nitrogen and gaseous state using hydrogen and argon gas as carrier gas
Ethyl alcohol grows 1-100min under 1400-1800 DEG C, 500-1000mbar pressure, and the high mobility silicon carbide foundation stone is made
Black alkene material.
2. the method for preparing the silicon carbide-based grapheme material of high mobility as described in claim 1, it is characterised in that: described exhausted
It is put into chemical vapor depsotition equipment after the cleaned drying of edge substrate, is evacuated to≤10-4mbar。
3. the method for preparing the silicon carbide-based grapheme material of high mobility as claimed in claim 2, it is characterised in that: described exhausted
The cleaning and drying method of edge substrate are as follows: insulating substrate uses the concentrated sulfuric acid, chloroazotic acid and hydrofluoric acid solution heating cleaning, deionized water respectively
It rinses, is placed in dust guard after nitrogen gun drying, dries in an oven.
4. the method for preparing the silicon carbide-based grapheme material of high mobility as claimed in claim 3, it is characterised in that: by vacuum
Environment is warming up to 500-1100 DEG C, to remove substrate surface adsorbed gas.
5. the method for preparing the silicon carbide-based grapheme material of high mobility as described in claim 1, it is characterised in that: argon gas stream
Amount is 1-20L/min, hydrogen flowing quantity 1-20L/min.
6. the method for preparing the silicon carbide-based grapheme material of high mobility as described in claim 1, it is characterised in that: the gas
State carbon source is methane, ethane, ethylene, acetylene or propane, flow 0.001-0.2L/min.
7. the method for preparing the silicon carbide-based grapheme material of high mobility as claimed in claim 6, it is characterised in that: C/H ratio
For 0.01%-1%, C/H ratio is the ratio between gaseous carbon source and the flow of hydrogen.
8. the method for preparing the silicon carbide-based grapheme material of high mobility as described in claim 1, it is characterised in that: nitrogen
Flow is 0.05-1L/min.
9. the method for preparing the silicon carbide-based grapheme material of high mobility as described in claim 1, it is characterised in that: gaseous state second
The flow of alcohol is 0.001-1L/min.
10. the method for preparing the silicon carbide-based grapheme material of high mobility as described in claim 1, it is characterised in that: growth
After process, stop hydrogen, gaseous carbon source and nitrogen, be passed through argon gas, keeps pressure constant, drop to room in ar gas environment
Temperature.
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| CN201811477126.2A CN109399620B (en) | 2018-12-05 | 2018-12-05 | Method for preparing high-mobility silicon carbide-based graphene material |
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| CN201811477126.2A CN109399620B (en) | 2018-12-05 | 2018-12-05 | Method for preparing high-mobility silicon carbide-based graphene material |
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| CN109399620B CN109399620B (en) | 2020-10-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102891074A (en) * | 2012-10-22 | 2013-01-23 | 西安电子科技大学 | SiC substrate-based graphene CVD (Chemical Vapor Deposition) direct epitaxial growth method and manufactured device |
| CN103708448A (en) * | 2014-01-03 | 2014-04-09 | 中国科学院化学研究所 | Atmospheric pressure controlled growth method for graphene |
| CN107026259A (en) * | 2016-02-01 | 2017-08-08 | 北京大学 | A kind of graphene combination electrode material and preparation method and application |
| CN107500560A (en) * | 2017-09-30 | 2017-12-22 | 北京碳世纪科技有限公司 | The method for preparing Graphene glass |
| CN107601473A (en) * | 2017-09-30 | 2018-01-19 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) for the grapheme material for preparing uniformity |
-
2018
- 2018-12-05 CN CN201811477126.2A patent/CN109399620B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102891074A (en) * | 2012-10-22 | 2013-01-23 | 西安电子科技大学 | SiC substrate-based graphene CVD (Chemical Vapor Deposition) direct epitaxial growth method and manufactured device |
| CN103708448A (en) * | 2014-01-03 | 2014-04-09 | 中国科学院化学研究所 | Atmospheric pressure controlled growth method for graphene |
| CN107026259A (en) * | 2016-02-01 | 2017-08-08 | 北京大学 | A kind of graphene combination electrode material and preparation method and application |
| CN107500560A (en) * | 2017-09-30 | 2017-12-22 | 北京碳世纪科技有限公司 | The method for preparing Graphene glass |
| CN107601473A (en) * | 2017-09-30 | 2018-01-19 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) for the grapheme material for preparing uniformity |
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