CN105951179A - Method for selectable single-side growth of graphene on SiC substrate - Google Patents
Method for selectable single-side growth of graphene on SiC substrate Download PDFInfo
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- CN105951179A CN105951179A CN201610273844.2A CN201610273844A CN105951179A CN 105951179 A CN105951179 A CN 105951179A CN 201610273844 A CN201610273844 A CN 201610273844A CN 105951179 A CN105951179 A CN 105951179A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
Abstract
The invention relates to a method for selectable single-side growth of graphene on a SiC substrate. The method comprises the following steps: horizontally placing the SiC substrate in a graphite crucible, allowing the side of C to be downward or the side of Si to be downward, and overlaying a cover sheet on the upward side of the SiC substrate, wherein the cover sheet is a Si atom donor or a C atom absorber; vacuumizing the chamber of a heating furnace for heating, then introducing high-purity H2, and subjecting the surface of the SiC substrate to hydrogen etching so as to form a regular SiC step structure; and closing H2, introducing Ar gas, continuing heating the heating furnace to 1500 to 1800 DEG C, and maintaining the temperature so as to complete the growth of graphene. The graphene grown by using the method provided by the invention has greatly-improved quality and surface morphology, and can be extensively applied in the fields of logic circuits, laser Q modulation, high-frequency nanometer radio frequency devices, etc.
Description
Technical field
The method that the present invention relates to the growth of a kind of alternative one side based on SiC epitaxial graphene, belongs to microelectronic material skill
Art field.
Background technology
Graphene is a bright star in material with carbon element family.Shelled by Geim professor and professor Novoselov from 2004
Since preparing, lead the research boom of more than ten years.Graphene is by with sp2The netted list that is formed by connecting of hydbridized carbon atoms
The preferable two dimensional crystal of atom level, has impayable characteristic.Graphene has the intrinsic mobility of superelevation, about
200000cm2/ (v s), exceeds two orders of magnitude than typical silicon field-effect transistor electron mobility；Also have in known materials
High heat conductance [about 5000W/ (m K)], huge specific surface area (2630m2/ g), great Young's modulus (1.06TPa) and disconnected
Split stress (about 130GPa)；Additionally it also has good light transmission and pliability.These excellent characteristics make Graphene in pole
High frequency and UHF electronic device, Flexible Displays electronic device, optical communication, solaode, logical integrated circuit and super
The fields such as level electric capacity have huge application prospect.
The Graphene of preparation yet suffers from the defect in a lot of structure at present, and actual application test value and ideal value still have the biggest difference
Away from.The generally Graphene of growth is the polycrystal film structure that monodomain region is built-up, and the size in single farmland district is only capable of reaching centimetre
Substantial amounts of domain boundary and interlayer stacking provisions is there is between magnitude, and domain.The existence of these defect sturctures, on the one hand in defect
Adsorption effect can be formed so that carrier concentration increases at structure；On the other hand the scattering of carrier can be caused in transmitting procedure
Enhancement effect, thus reduce the carrier transport properties of Graphene.The quality of Graphene depends primarily on preparation method and preparation
During technology controlling and process.The main preparation methods of the existing Graphene that can be used for semiconductor device has: at catalytic effect
Chemical gaseous phase deposition (CVD) method on the other materials that metal substrate or lattice are adaptive, the mechanical stripping method of oriented graphite and
Pyrolytic silicon carbide (SiC) extending and growing graphene method.
Wherein SiC extending and growing graphene method has many merits relative to first two method: 1. without wanting in pyrolytic process
Add any auxiliary reagent, Graphene pure can be effectively ensured；2.SiC substrate itself has preferable insulation characterisitic and leads
Hot, the Graphene after having grown, without transfer, can avoid Graphene by secondary injury；3. partly can lead with existing
Body device technology is compatible, can directly use standard nanometer etching technology to carry out patterning and prepare electronic device.Such as
CN102373506A provides method and the graphene device of a kind of extending and growing graphene on sic substrates.
CN102051677A discloses a kind of method growing Graphene on major diameter 6H-SiC carbon face, by 6H-SiC wafer
Carbon faces up in the graphite pallet lain in heating furnace crucible, and suction is rapidly heated to 1700-1750 DEG C, is passed through
High-purity argon gas, is then to slowly warm up to 1750-1950 DEG C, is incubated 1-10min, completes the growth of Graphene.The method serves as a contrast
End not damaged layer, the Graphene grown is covered with two surfaces up and down of whole substrate, and the Graphene number of plies can be controlled in 1-10 layer.
Although the argon atmosphere in the method can suppress Si component rate of sublimation to a certain extent, but Si component still distils relatively
Hurry up, and the lateral transfer rate of surface C atom is relatively low, all there is Graphene, to follow-up point in two surfaces up and down of SiC simultaneously
Analysis causes difficulty.
The formation of Graphene and growth atmosphere have the biggest relation, and the surface of SiC being exposed to upward in Ar gas forms Graphene
Speed is higher than being attached to crucible bottom surface of SiC.Therefore, it is desirable to form Graphene at the aufwuchsplate selecting crucible bottom
Meanwhile, the graphene layer of thickness is formed the most over there.Up to now, based on SiC epitaxial in graphite crucible
The method of alkene available property one side growth has no report.
Summary of the invention
The technology of Graphene is concurrently formed based on SiC substrate C face and Si face under SiC substrate epitaxy process conditions for existing
A difficult problem, the invention provides a kind of alternative one side growth Graphene of carrying out on great diameter SiC substrate in graphite crucible
Method.
Term is explained:
SiC wafer (6H/4H-SiC) has two polar surface: silicon face (0001), carbon face (000-1), of the present invention can
Selectivity one side growth Graphene refer in C face, opposed polarity face or Si face, select one of them as graphene growth face,
Graphene on suppression another side generates simultaneously.
High-purity H2: refer to purity H more than 99.999%2。
4H/6H-SiC wafer: refer to 4H-SiC wafer or 6H-SiC wafer.
Technical scheme is as follows:
A kind of method of alternative one side growth Graphene in SiC substrate, including:
A piece of SiC substrate lies in center in graphite crucible, and the aufwuchsplate C of selection faces down or Si faces down,
Again by a cover plate imbrication on described SiC substrate face upward, cover graphite crucible upper cover；Described graphite crucible is positioned at heating
In furnace chamber；
Described cover plate is Si atom donor or C Atomic Absorption body；
By heating furnace chamber evacuation, in the way of heating, it is warming up to 1450～1750 DEG C, is passed through high-purity H2, to described SiC
Substrate surface carries out hydrogen etching, the SiC ledge structure of formation rule；
Close H2, it being passed through Ar gas, continuation rising furnace temperature, to 1500～1800 DEG C, is incubated 60-90min, completes Graphene
Growth.
According to currently preferred, described SiC substrate is selected from 4H-SiC or 6H-SiC.The preferably a diameter of 2-6 of SiC substrate
Inch.
According to currently preferred, the twin grinding of described SiC substrate, polishing, surface roughness is less than 0.5nm, smooth
Degree is less than 6 μm；The thickness of described SiC substrate is 300 μm～500 μm.
According to currently preferred, in described cover plate, Si atom donor is 4H/6H-SiC wafer, and C Atomic Absorption body is Ta
Sheet, Ta2C sheet or Ti sheet etc..Described cover plate diameter is identical with described SiC substrate or bigger.
According to the present invention, 4H/6H-SiC wafer selected by described cover plate, and the imbrication that faced down by the Si of 4H/6H-SiC wafer exists
In described SiC substrate.Preferably, the surface roughness in described cover plate 4H/6H-SiC wafer Si face is less than 3nm, flatness
Less than 15 μm；Described cover plate 4H/6H-SiC wafer thickness is 300 μm～500 μm.
According to the present invention, Ta sheet selected by described cover plate, and Ta sheet burnishing surface imbrication down is in described SiC substrate.Ta sheet
The surface roughness of burnishing surface is less than 3nm, and flatness is less than 15 μm；Described Ta sheet thickness is 0.5-3mm.Select Ta2C
Sheet or Ti sheet cover plate also with.
According to currently preferred, described heating furnace chamber evacuation, make vacuum reach (1～5) × 10-6mbar；It is passed through height
Pure H2Flow be 5～100sccm, Stress control is 600～900mbar.
Provide below the technical scheme that a kind of preferred preparation method is detailed.
In a kind of SiC substrate, the method for alternative one side growth Graphene, comprises the following steps that
(1) diameter 2-6 inch SiC substrate wafer is carried out twin grinding, polishing so that surface roughness is less than 0.5nm,
Flatness is less than 6 μm, and obtaining thickness is 200 μm～the SiC substrate of 800 μm.Subsequently surface is carried out, encapsulates and treat
With.
(2) diameter 2-6 inch SiC cover plate is carried out the grinding of Si face, polishing so that surface roughness is less than 3nm, smooth
Degree is less than 15 μm, and obtaining thickness is 200 μm～the SiC wafer of 800 μm.Subsequently surface is carried out, encapsulate stand-by.
Or, by diameter at 2-6 inch Ta sheet, Ta2C sheet or Ti sheet etc. are ground, polish, and obtain thickness 0.5-3mm's
Light Ta sheet, Ta2C sheet or Ti sheet.Subsequently surface is carried out, encapsulate stand-by.
(3) placing graphite crucible in vertical heater, the 4H/6H-SiC substrate that above-mentioned steps (1) prepared is a piece of to be kept flat
In graphite crucible center, C faces down or Si faces down, then 4H/6H-SiC above-mentioned steps (2) prepared is brilliant
The Ta sheet of sheet Si face or preparation, Ta2C sheet or Ti sheet wet look correspondence imbrication, on substrate, add a cover graphite crucible upper cover
Close；By heating furnace chamber evacuation, treat that vacuum arrives (1～5) × 10-6After mbar, it is rapidly heated to 1450～1750 DEG C,
Heating rate 10～50 DEG C/min, is passed through high-purity H2, H2Flow 5～100sccm, Stress control is 600～900mbar, right
Substrate surface carries out hydrogen etching, hydrogen etch period 10～40min, the SiC ledge structure of formation rule；
(4) H is closed2, it being passed through Ar gas, Ar throughput 10～1000sccm, Stress control is 800～900mbar；To add
Hot stove is warming up to 1500～1800 DEG C, heating rate 10～50 DEG C/min, is incubated 60～90min, completes the growth of Graphene.
Closing heating power supply after graphene growth, continue logical Ar gas, Ar throughput is 500～1000sccm, and Stress control exists
800mbar, cools to 500 DEG C；Closing Ar gas, Temperature fall is to room temperature.Subsequently, the Graphene sample in crucible is taken out.
Prepared the grapheme material of SiC substrate one side growth by the method, the coverage rate on SiC substrate surface is more than
90%, uniformity is preferable, 10 × 10mm2In the range of mobility at 1000-5000cm2/ v s, the Graphene number of plies is 1-2 layer.
Preferably, in step (1), the twin polishing to SiC substrate uses chemically mechanical polishing, cleans accepted standard wet method
Chemical cleaning technology；Can process that surface cleaning, roughness be little, the substrate surface of not damaged layer.
Preferably, in step (2), SiC wafer carries out Si face grinding and polishing, clear through over cleaning accepted standard wet chemistry
Wash technique；Surface cleaning, smooth coverslip surface can be processed.
Preferably, in step (2), Ta sheet is ground polishing, through over cleaning accepted standard wet chemical cleaning process；
Surface cleaning, smooth coverslip surface can be processed.
Preferably, in step (3) Si of SiC cover plate face down or Ta sheet burnishing surface down, imbrication growth Graphene
4H/6H-SiC substrate on, all cover plates are the most reusable.
Preferably, in step (3) growth furnace furnace chamber vacuum to 1 × 10-6Mbar, fast heating ramp rate at 30～50 DEG C/min,
Stress control is at 900mbar, hydrogen etch period 20～40min.
Preferably, in step (4), argon flow amount 30～50sccm, Stress control is at 900mbar；Heating furnace is warming up to
1650-1750 DEG C, heating rate 10-15 DEG C/min, it is incubated 60～80min.
The method of the present invention can obtain that large area, high-quality, the number of plies be controlled, the grapheme material of pattern uniform one side growth.
The coverage rate carrying out one side growth on aufwuchsplate selected on sic substrates is more than 90%, and Graphene step appearance is regular.?
Accurately controlling heating rate and under the conditions of the response time, the Graphene number of plies can be controlled in monolayer.
The present invention uses the graphene growth of non-selection in bi-material in-situ control SiC substrate, and a class material is with SiC
Sheet is representative, but is not limited to this, and this type of material can provide the Si atomic composition of SiC substrate surface sublimation, by suppression or
Weaken the loss of Si atom, suppress the formation of Graphene；Equations of The Second Kind material is as representative with tantalum (Ta) sheet, but is not limited to
This, this type of material is the shape being suppressed Graphene by the active C atom stayed after absorbing the Si atom distillation of SiC substrate surface
Become.Mechanism based on SiC substrate thermal decomposition epitaxy growth Graphene, the invention proposes two kinds of suppression Graphenes and is formed
Mode, the method successfully realizing on great diameter SiC substrate alternative one side growth Graphene, the method not only improves
Improve the quality of growth Graphene, overcome again the deficiency of prior art, simple and easy to do.
Technical characterstic and the excellent results of the present invention are:
1, present invention SiC substrate extension in graphite crucible prepares Graphene, by adding SiC class cover plate or Ta class in situ
Cover plate can suppress the generation of two-sided Graphene effectively.
2, the cover plate used in the inventive method is reusable, it is not necessary to midway is changed；If surface carbonation is serious, can be through again
Reuse after grinding and polishing, greatly reduce use cost.
3, in the inventive method, optional a kind of polar surface (C face or Si face) carries out one side growth Graphene, only needs non-
Growth selection face is with ready cover plate imbrication, simple to operation.
4, the Graphene quality of the inventive method growth, surface topography are improved largely, can be at logic circuit, laser Q-switching
Extensively apply with fields such as high-frequency radio frequency devices.
Accompanying drawing explanation
Fig. 1 is the embodiment 1 Raman (Raman) spectrogram at the 4H-SiC silicon face substrate epitaxial growth Graphene of 2 inches.
Abscissa is Raman shift, and vertical coordinate is intensity (arbitrary unit)；Wherein,
(a) be growth selection face be 9 Raman test figures in Si face；
B () is the Raman figure after corresponding diagram (a) deducts SiC substrate peak, can be clear that sharp-pointed Graphene 2D in figure
With G characteristic peak, 2D peak with the unimodal matching of long-range navigation thatch and can't see D peak, can show the monolayer higher for quality of growth
Graphene；
C () is 9 test figures in non-selection aufwuchsplate C face；
D () deducts the Raman figure behind SiC substrate peak for corresponding (c), can't see the peak of any Graphene, show C in figure
Face does not forms Graphene.
Fig. 2 is the embodiment 1 atomic force microscope (Atomic at the 4H-SiC Si face substrate epitaxial growth Graphene of 2 inches
Force Microscope, atomic force microscope) shape appearance figure, demonstrate the surface topography of rule stepped profile, test area
10μm×10μm。
Fig. 3 is the device schematic diagram of SiC substrate epitaxial graphene selectivity one side growth in graphite crucible, and cover plate 4 is tight
Ground imbrication is on growth substrates 2；Wherein, 1, heating coil, 2, SiC substrate wafer, 3, graphite crucible, 4,
Graphite crucible upper cover, 5, cover plate.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the growing method of the present invention is described further, but is not limited to this.
In embodiment use SiC substrate, conduction type is semi-insulating, and surface orientation is forward, misorientation ± 0.3 degree it
In, a diameter of 2-6 inch, thickness 200 μm-800 μm.Vertical heat growth stove used is commercial general heating stove.
Embodiment 1
The method of a kind of available property one side based on SiC epitaxial graphene growth, comprises the steps:
(1) 2 inches diameter 4H-SiC substrate wafer is carried out twin grinding, polishing so that surface roughness is less than 0.5nm,
Flatness is less than 6 μm, obtains the 4H-SiC substrate that thickness is 400 μm.Then surface is carried out the cleaning of standard.
(2) 2 inches diameter 4H-SiC cover plate is carried out the grinding of Si face, polishing so that surface roughness is less than 3nm, flat
Whole degree is less than 15 μm, obtains the 4H-SiC wafer that thickness is 500 μm.Subsequently surface is carried out the cleaning of standard.
(3) placing the graphite crucible of 2 inches in vertical heat growth stove, 4H-SiC above-mentioned steps (1) prepared serves as a contrast
End Si faces down and lies in graphite crucible center, then 4H-SiC wafer Si face above-mentioned steps (2) prepared is corresponding
Imbrication, above substrate, is added a cover graphite crucible upper cover and is closed；By heating furnace chamber evacuation, treat that vacuum is to 1 × 10-6Mbar,
It is rapidly heated to 1500 DEG C, 30 DEG C/min of heating rate, it is passed through high-purity H2, H2Flow 30sccm, Stress control at 900mbar,
Substrate surface is carried out hydrogen etching, hydrogen etch period 30min, the SiC ledge structure of formation rule；
(5) H is closed2, it being passed through Ar gas, Ar throughput 200sccm, Stress control is at 800mbar；Furnace chamber is warming up to
1600 DEG C, 15 DEG C/min of heating rate, it is incubated 90min, completes the growth of Graphene.
Closing heating power supply after graphene growth, continue logical Ar gas, Ar throughput is 800sccm, Stress control at 800mbar,
Cool to 500 DEG C；Closing Ar gas, Temperature fall is to room temperature.Subsequently, the Graphene sample in crucible is taken out.
The pattern of the grapheme material obtained is uniform, and the number of plies is monolayer, and its Hall mobility has reached 1300cm2/v·s.Survey
Raman spectrogram such as Fig. 1 of examination, it can be seen that the number of plies of Graphene is monolayer, 9 tests show the distribution of the Graphene number of plies all
Even, see Fig. 1 (b)；And can be seen that C face upward generates without any Graphene, see Fig. 1 (d).Atomic Mechanics
The pattern rule of the bright Graphene of microscope (AFM) image table, step are uniform, and test area is 10 × 10 μm2。
Embodiment 2
The method of a kind of available property one side based on SiC epitaxial graphene growth, according to graphite same as in Example 1
Alkene growing method, its difference is, being faced down by process 2 inches of 4H-SiC substrate C lies in growth furnace earthenware
In crucible, growth temperature controls at 1550 DEG C.Use Raman spectrum and atomic force microscope to characterize and obtain grapheme material, stone
Ink alkene pattern is uniform；Hall mobility is 3500cm2/v·s。
Embodiment 3
The method of a kind of available property one side based on SiC epitaxial graphene growth, according to graphite same as in Example 1
Alkene growing method, its difference is, process 3 inches of 4H-SiC substrate Si being faced down lies in growth furnace earthenware
In crucible, use polished Ta sheet imbrication above substrate.Test characterizes the Graphene of growth, and the number of plies is monolayer；Hall moves
Shifting rate is 1500cm2/v·s。
By the description of embodiment 1-3, the characterization result of grapheme material is it can be seen that this inventive method can in conjunction with the embodiments
Effectively to suppress the formation of non-selection aufwuchsplate Graphene, eliminate the measurement error that the two-sided Graphene of substrate produces；Growth
Graphene quality, uniformity and mobility be all improved, be beneficial to SiC substrate epitaxial graphene electronic device lead
The application in territory.
Claims (10)
1. a method for alternative one side growth Graphene in SiC substrate, including:
A piece of SiC substrate lies in center in graphite crucible, and C faces down or Si faces down, then is folded by a cover plate
Cover on described SiC substrate face upward, cover graphite crucible upper cover；It is indoor that described graphite crucible is positioned at heating furnace chamber；
Described cover plate is Si atom donor or C Atomic Absorption body；
By heating furnace chamber evacuation, to be heated to 1450～1750 DEG C, it is passed through high-purity H2, to described SiC substrate table
Face carries out hydrogen etching, the SiC ledge structure of formation rule；
Close H2, it being passed through Ar gas, continuation rising furnace temperature, to 1500～1800 DEG C, is incubated 60-90min, completes Graphene
Growth.
2. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 1, it is characterised in that institute
State SiC substrate selected from 4H-SiC or 6H-SiC；Preferably, the twin grinding of described SiC substrate, polishing, rough surface
Degree is less than 6 μm less than 0.5nm, flatness；The thickness of the most described SiC substrate is 300 μm～500 μm.
3. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 1, it is characterised in that institute
Stating in cover plate, Si atom donor is 4H/6H-SiC wafer, and C Atomic Absorption body is Ta sheet, Ta2C sheet or Ti sheet or other
There is the thin slice that this acts on.
4. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 1, it is characterised in that institute
State cover plate and select 4H/6H-SiC wafer, the Si of 4H/6H-SiC wafer is faced down imbrication in described SiC substrate；Excellent
Choosing, the surface roughness in described cover plate 4H/6H-SiC wafer Si face is less than 3nm, and flatness is less than 15 μm.
5. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 1, it is characterised in that institute
Stating cover plate and select Ta sheet, Ta sheet burnishing surface imbrication down is in described SiC substrate；Preferably, the table of Ta sheet burnishing surface
Surface roughness is less than 3nm, and flatness is less than 15 μm；The most described Ta sheet thickness is 1-3mm.
6. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 1, it is characterised in that institute
State heating furnace chamber evacuation, make vacuum reach (1～5) × 10-6mbar；It is passed through high-purity H2Flow be 5～100sccm,
Stress control is 600～900mbar.
7. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 1, it is characterised in that step
As follows:
(1) diameter 2-6 inch SiC substrate wafer is carried out twin grinding, polishing so that surface roughness is less than 0.5nm,
Flatness is less than 6 μm, and obtaining thickness is 300 μm～the SiC substrate of 500 μm；Clean stand-by；
(2) diameter 2-6 inch SiC cover plate is carried out the grinding of Si face, polishing so that surface roughness is less than 3nm, smooth
Degree is less than 15 μm, and obtaining thickness is 300 μm～the SiC wafer of 500 μm；Clean stand-by；Or,
By diameter at 2-6 inch Ta sheet, Ta2C sheet or Ti sheet are ground, polish, and obtain the bright Ta of thickness 1-3mm
Sheet, Ta2C sheet or Ti sheet；Clean stand-by；
(3) placing graphite crucible in heating furnace, the 4H/6H-SiC substrate that above-mentioned steps (1) prepared is a piece of lies in stone
Ink crucible center, C faces down or Si faces down, then 4H/6H-SiC wafer Si above-mentioned steps (2) prepared
Face or Ta sheet, Ta2The wet look correspondence imbrication of C sheet or Ti sheet, on substrate, is added a cover graphite crucible upper cover and is closed；
By heating furnace chamber evacuation, treat that vacuum arrives (1～5) × 10-6Mbar, is rapidly heated to 1450～1750 DEG C, heating rate
10～50 DEG C/min, it is passed through high-purity H2, H2Flow 5～100sccm, substrate surface, 800～900mbar, is entered by Stress control
Row hydrogen etches, hydrogen etch period 10～40min, the SiC ledge structure of formation rule；
(4) H is closed2, it being passed through Ar gas, Ar throughput 10～1000sccm, Stress control is 800～900mbar；To add
Hot stove is warming up to 1500～1800 DEG C, heating rate 10～50 DEG C/min, is incubated 60～90min, completes the growth of Graphene.
8. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 7, it is characterised in that step
Suddenly in (3) heating stove furnace chamber vacuum to 1 × 10-6Mbar, fast heating ramp rate exists at 30～50 DEG C/min, Stress control
900mbar, hydrogen etch period 20～40min；Preferably, described in step (3), the height of the SiC step of rule is nanometer
Magnitude, step width is micron dimension.
9. the method for alternative one side growth Graphene in SiC substrate as claimed in claim 7, it is characterised in that step
Suddenly, in (4), argon flow amount 30～50sccm, Stress control is at 900mbar；Heating furnace is warming up to 1650-1750 DEG C,
Heating rate 10-15 DEG C/min, is incubated 60～80min.
10. the grapheme material of the SiC substrate one side growth that any one of claim 1-9 prepares, it is characterised in that
The coverage rate on SiC substrate surface is more than 90%, 10 × 10mm2In the range of mobility at 1000-5000cm2/ v s, graphene layer
Number is 1-2 layer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610273844.2A CN105951179B (en) | 2016-04-28 | 2016-04-28 | A kind of method of alternative single side growth graphene in SiC substrate |
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| CN201610273844.2A CN105951179B (en) | 2016-04-28 | 2016-04-28 | A kind of method of alternative single side growth graphene in SiC substrate |
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| CN105951179A true CN105951179A (en) | 2016-09-21 |
| CN105951179B CN105951179B (en) | 2019-01-11 |
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| CN106517165A (en) * | 2016-11-07 | 2017-03-22 | 山东大学 | Method for growing graphene by metal-assisted internal/external carbon sources combination mode on 6H/4H-SiC silicon surface |
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| CN115849352A (en) * | 2023-02-27 | 2023-03-28 | 太原理工大学 | Method for efficiently preparing laminated graphene |
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