CN105441902B - A kind of preparation method of epitaxial silicon carbide graphene composite film - Google Patents
A kind of preparation method of epitaxial silicon carbide graphene composite film Download PDFInfo
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Abstract
The present invention relates to technical field of semiconductors, especially a kind of preparation method of epitaxial growth carborundum graphite alkene laminated film, it comprises the following steps：Pretreated substrate is placed in chemical vapor deposition chamber body, controls the vapor deposition chamber Absolute truth reciprocal of duty cycle to be higher than 10‑4Pa, 2~10 microns of silicon carbide epitaxial layers are grown in the substrate surface at 1500~1600 DEG C；The temperature of the chemical vapor deposition chamber body is controlled to be reduced to 1000 DEG C; 1600 DEG C are heated to from 1000 DEG C to the chemical vapor deposition chamber body under protective atmosphere; make the silicon carbide epitaxial layers STRUCTURE DECOMPOSITION and restructuring, obtain graphene composite bed on the substrate.This method can be not entirely dependent on expensive monocrystal SiC base material, but use high temperature chemical vapor deposition apparatus, realize the continuous growth of silicon carbide epitaxy layer graphene.
Description
Technical field
The invention belongs to semiconductor film material technical field, is related to a kind of preparation side of novel semi-conductor thin-film material
Method, it is exactly specifically continuous epitaxial growth larger area, the method for uniform graphene on silicon carbide epitaxial layers.
Background technology
Graphene is a kind of by the tightly packed carbon material into bi-dimensional cellular shape structure of single layer of carbon atom, because with uniqueness
Crystal and electronic band structure and possess very excellent mechanics, calorifics, optics, electricity and chemical property, such as the current-carrying of superelevation
Transport factor, the specific surface area of super large, perfect quantum tunneling effect, half-integer quantum hall effect etc..Britain is graceful within 2004
After the Chester university A.K.Geim and K.S.Novoselov graphene of discovery first, graphene rapidly becomes present material, thing
The international forward position of the research field such as reason, chemistry, semiconductor, microelectronics, biology, new energy and focus.Carborundum has stratiform knot
Structure, its basic Component units are the silicon-carbon diatomic layer that silicon atom and carbon atom form.During sic wafer is made, by
Can not accomplish in cutting knife it is complete fine, cause can not the edge weaker direction cleavage of Si-C associative keys between layers completely, and
It is to have individual angle with cleavage surface, so that after carrying out dicing operation, carborundum is along in a direction in step-like.Also just because of such as
This, the graphene of growing high quality is just possibly realized on its step.
Preparing graphene has a variety of methods, such as mechanical stripping method, liquid phase or gas phase dissociation method, oxidation-reduction method, cutting
Nanometer tube method, chemical vapour deposition technique, single-crystal metal epitaxy and SiC epitaxial growth methods etc..SiC epitaxial growth methods are certain
Vacuum under, SiC is heated to certain temperature, causes silicon atom to evaporate, remaining carbon atom is reconstructed to form graphene.By
It is semi-insulated in the substrate SiC of so growth graphene, it is numerous that the sample after growth need not carry out substrate corrosion, sample migration etc.
Trivial work, it can directly carry out the test of electricity.This reduces the defects of introducing in transfer process, the factor such as doping
Influence.It is most effective as realizing that graphene is applied in microelectronic that this also causes SiC substrate Epitaxial growths graphene
One of approach.
SiC extending and growing graphenes are all to use monocrystal SiC substrate, the SiC materials that traditional single crystal preparation method obtains at present
Expect that defect is more, it is difficult to control thickness and doping, often do not reach the requirement of manufacture device, and the monocrystal SiC substrate of high quality
It is again expensive.The step of needing to carry out hydrogen etching to substrate before extending and growing graphene in addition, because carborundum passes through
Surface can retain many cuts after crossing chemically mechanical polishing (CMP) PROCESS FOR TREATMENT, directly use it to graphite shape prepared by growth
Looks quality is all poor, and obtained sample topography is grown on uniform step and quality can be well a lot, and hydrogen etching is exactly one
Generally acknowledged feasible scheme the defects of can removing the cut of sample surfaces of kind.But improperly hydrogen etching can make on the contrary
SiC substrate surfaces form lattice defect, and can produce the compound deposition phenomenon of silicon, excessively cut down the enrichment of surface of SiC silicon, shadow
Ring the epitaxial growth of graphene.
The content of the invention
To solve the above problems, the present invention provides a kind of preparation method of epitaxial silicon carbide-graphene composite film, it is wrapped
Include following steps：
Step 1：Pretreated substrate is placed in chemical vapor deposition (CVD) cavity, controls the chemical vapor deposition
Product cavity Absolute truth reciprocal of duty cycle is higher than 10-4Pa, at 1500~1600 DEG C outside the carborundum that the substrate surface grows 2~10 microns
Prolong layer；
Step 2：The temperature of the chemical vapor deposition chamber body is controlled to be reduced to 1000 DEG C, to described under protective atmosphere
Chemical vapor deposition chamber body is heated to 1600 DEG C from 1000 DEG C, makes the silicon carbide epitaxial layers STRUCTURE DECOMPOSITION and restructuring,
Graphene composite bed is obtained in the substrate.
Wherein, the substrate is SiC.
Wherein, also include before the step 1：Grow 10~100nm thickness on the substrate using molecular beam epitaxy
Cushion.
Wherein, the substrate is GaN or Al2O3；The cushion is AlN.
Wherein, it is 1300~1600 to control the chemical vapor deposition chamber temperature in the step 2 under protective atmosphere
℃。
Wherein, the heating in the step 2 to the chemical vapor deposition chamber body takes staged to heat up, concrete operations
For：
Control the chemical vapor deposition chamber temperature to be increased to 1100 DEG C, and kept for 10 minutes；
Control the chemical vapor deposition chamber temperature to be increased to 1200 DEG C, and kept for 10 minutes；
The chemical vapor deposition chamber temperature rise is controlled up to 1300~1600 DEG C of scopes, and is kept for 30~50 minutes.
Further, the heating in the step 2 to the chemical vapor deposition chamber body takes staged to heat up, more
Preferable concrete operations are：
Control the chemical vapor deposition chamber temperature to be increased to 1100 DEG C, and kept for 10 minutes；
Control the chemical vapor deposition chamber temperature to be increased to 1200 DEG C, and kept for 10 minutes；
The chemical vapor deposition chamber temperature rise is controlled up to 1450~1600 DEG C of scopes, and is kept for 30~50 minutes.
Beneficial effects of the present invention：
(1) extending and growing graphene film is not entirely dependent on the carbide silicon base of costliness, but is directly growing
The preparation of graphene Heterogeneous Composite film is carried out continuously after silicon carbide epitaxial layers, and other hetero-substrates can also be grown in
On, further reduce cost.
(2) the silicon carbide epitaxial layers quality that chemical vapour deposition technique obtains is often higher, and can ensure faster life
Long speed and doping control, and are very suitable for the growth of high quality silicon carbide epitaxial layers-graphene composite film, while can also
Obtain the carbide-graphite alkene heterofilm of different doping types.
(3) the inventive method has cast out hydrogen etching substrate surface and then has made up the complex steps of surface silicon enrichment, obtains
Few layer graphene composite bed of high quality.
Brief description of the drawings
Fig. 1 a are AFM (AFM) surface two-dimensional appearance test chart of silicon carbide epitaxial layers of the present invention；Fig. 1 b are
AFM the topography analyzer figures.
Fig. 2 is the X-ray photoelectron spectroscopic analysis figure of epitaxial silicon carbide-graphene composite film of the present invention.
Fig. 3 a are the Raman spectrogram of epitaxial silicon carbide-graphene composite film of the present invention；Fig. 3 b are extension carbon of the present invention
The Raman spectroscopy scans image of SiClx-graphene composite film.
Embodiment
Below, the present invention will be elaborated in conjunction with specific embodiments.
Embodiment 1：
The substrate for epitaxial silicon carbide-graphene composite film that the present embodiment provides is the face-up 4H-SiC of silicon, specifically
Implementation steps are as follows：
Step 1：First the substrate is carried out cleaning pre- place using standard RCA clean method (a kind of wet chemical cleans method)
Reason, to eliminate oxide on surface and other impurity particles.
Then the high temperature chemical vapor deposition for pretreated substrate being placed in sensing heating reacts (Chemical
VaporDeposition, abbreviation CVD) in cavity, first vacuumize so that Absolute truth reciprocal of duty cycle is higher than 10-4Pa.It is continually fed into flow
For 7slm H2, utilize H2Etching removes oxide on surface and surface scratch.Meanwhile heating cavity by cavity temperature from room temperature by
Step rises to 1600 DEG C.Keep being used as the pregrown stage in 10 minutes at 1600 DEG C.
Then said temperature and pressure are kept, is passed through SiH4And C3H8, flow is respectively that 9sccm and 2sccm carries out carborundum
The growth of epitaxial layer.After reaction 60 minutes, the temperature of the chemical vapor deposition chamber body is down to 1000 DEG C, while be passed through flow
Protected for 1slm Ar, now form 2~10 microns of thick SiC epitaxial layers in substrate surface.Using AFM
The surface topography quality of silicon carbide epitaxial layers is characterized, as shown in Figure 1.Wherein, Fig. 1 a can be seen that gives birth to by silicon carbide epitaxial layers
After length, SiC surface topography starts to become orderly, forms well-regulated step striped, comparatively facilitates the growth of graphene.Figure
The step that 1b can be seen that SiC rises and falls in 10nm or so.By AFM software analysis, the root mean square roughness rate of surface of SiC is
2.4nm.Compared with the surface of SiC of hydrogen etching, effect is more preferable.
Step 2：The lasting flow that is passed through in chemical vapor deposition chamber body is protected for 1slm Ar, and adjustment pressure is protected
Hold 5Torr (using atmospheric pressure equivalent to 760 mmhg pressures as reference standard, 1Torr is 1/760 millimetres of mercury
Atmospheric pressure), staged heating then is carried out to the chemical vapor deposition chamber body, it is heated to 1300 from 1000 DEG C~
1550 DEG C of scope.Concrete operations are：The cavity temperature is first risen to 1100 DEG C from 1000 DEG C, stablized 10 minutes；Then
Cavity temperature is risen to 1200 DEG C from 1100 DEG C, and kept for 10 minutes；Cavity temperature is risen to 1550 DEG C from 1200 DEG C again, and protected
Hold 30 minutes.Wherein, Fig. 3 a are the Raman spectrum of the graphene of direct heteroepitaxial growth after epitaxial growth 4H-SiC, number
According to the peak value carried out when the growth temperature after normalized is respectively 1300 DEG C, 1450 DEG C and 1550 DEG C.It can be seen that
At 1300 DEG C, Raman (Raman) spectrum does not have obvious G peaks and 2D peaks, illustrates that also no graphene is formed on substrate.Work as temperature
When degree is increased to about 1450 DEG C, there is graphene significantly to be formed, show as occurring G peaks (1587cm simultaneously-1) and 2D
(2695cm-1) peak.D peaks (1344cm-1) show impurity or defect in graphene lattice structure be present more by force.As temperature is entered
When one step is increased to 1550 DEG C, the G peaks and 2D peak-to-peak signals of graphene are more obvious, show to be influenceed by SiC substrate less and less.D
Peak is fainter to show that impurity and defect are less.Fig. 3 b are the Raman 2D peaks scanning imagery in 1550 DEG C of extending and growing graphenes
Figure, scope is 25 μm of 25 μ m, and stepping is 0.5 μm of 0.5 μ m.It can be seen that large area color is more consistent in scanning imagery,
Show that the graphene number of plies is more uniform, and the monocrystalline area of the more explanation SiC epitaxial graphene in middle border is smaller.So
In staged temperature-rise period, final stage warming temperature preferably controls temperature more than 1450 DEG C；Also, temperature is higher, stone
The impurity and lattice defect of black alkene are smaller, and the quality of graphene is also higher.
By staged temperature-rise period, silicon carbide epitaxial layers carry out a series of reconstruct, are finally dropped naturally under Ar protections
Temperature, obtain forming the graphene composite bed in the stabilization of substrate surface, after the cavity temperature is reduced to 1000 DEG C, close
Ar is inputted；After the cavity temperature is reduced to room temperature, Ar is passed through to atmospheric pressure is recovered to when the cavity, opens cavity
Take out epitaxial silicon carbide-graphene composite film product that the present embodiment obtains.
Using the formation (referring to Fig. 2) of x-ray photoelectron power spectrum checking graphene composite bed, concrete operations are：By graphite
The C (1s) of alkene composite bed sample and the graph of a relation and curve A of combination energy are fitted, and obtain B, C, D peaks.(283.5eV) is at D peaks
Come from SiC substrate peak.High combination can locate C peaks (284.5eV) and be approached with graphite C-sp2 key positions, so C peaks are graphene
Composition, graphene can be obtained with the experimental method so as to further demonstrate.B peaks (284.9eV) combine energy position and connect very much
The position of nearly diamond C-sp3 keys, may be cushion carbon atom.
Verify that epitaxial silicon carbide-graphene composite film that the present embodiment obtains has preferable crystal using Raman spectrum
Quality, the number of plies of graphene composite bed is controlled below 4 layers, and has good uniformity (referring to Fig. 3).
Embodiment 2：
The substrate for epitaxial silicon carbide-graphene heterofilm that the present embodiment provides is Al2O3, specific implementation step is as follows：
Step 1：The substrate is first subjected to cleaning pretreatment using standard RCA clean method, with eliminate oxide on surface and
Other impurity particles.
Using pretreated substrate be placed in growth a layer thickness is 10nm in molecular beam epitaxy (MBE) AlN films as
Cushion.Then the substrate that growth has cushion is placed into the high temperature CVD stoves of sensing heating, first vacuumized so that definitely
Vacuum is higher than 10-4Pa.It is continually fed into 9slm H2, utilize H2Etching removes oxide on surface and surface scratch.By cavity temperature
Degree progressively rises to 1600 DEG C from room temperature, keeps being used as the pregrown stage in 10 minutes at 1600 DEG C.
Then pass to SiH4And C3H8, flow is respectively the growth that 10sccm and 3sccm carries out silicon carbide epitaxial layers.Reaction
After 60 minutes, the temperature of the chemical vapor deposition chamber body is down to 1000 DEG C, while is passed through the Ar that flow is 1slm and is protected
Shield, now form 2~10 microns of thick SiC epitaxial layers in substrate surface.
Step 2：The lasting flow that is passed through in chemical vapor deposition chamber body is protected for 2slm Ar, and adjustment pressure is protected
Hold in 10Torr, staged heating then is carried out to the chemical vapor deposition chamber body, 1500 DEG C are heated to from 1000 DEG C.
Concrete operations are：The cavity temperature is first risen to 1100 DEG C from 1000 DEG C, stablized 10 minutes；Then by cavity temperature from
1100 DEG C rise to 1200 DEG C, and are kept for 10 minutes；Cavity temperature is risen to 1500 DEG C from 1200 DEG C again, and kept for 40 minutes.Through
Staged temperature-rise period is crossed, silicon carbide epitaxial layers carry out a series of reconstruct, and finally the Temperature fall under Ar protections, is formed
In the graphene composite bed of the stabilization of substrate surface, after the cavity temperature is reduced to 1000 DEG C, Ar inputs are closed；Work as institute
State cavity temperature to be reduced to after room temperature, be passed through Ar to atmospheric pressure is recovered to when the cavity, open cavity and take out this implementation
Epitaxial silicon carbide-graphene heterofilm product that example obtains.
The surface topography quality of epitaxial silicon carbide is characterized using AFM, using x-ray photoelectron power spectrum and drawing
The formation and its crystal mass of graceful spectrum checking graphene, the number of plies and uniformity.
It is an object of the invention to provide a kind of side of continuous growth compound (heterogeneous) film of silicon carbide epitaxy-graphene
Method.This method can be not entirely dependent on expensive monocrystal SiC base material, but use the sensing heating of independent research
High temperature CVD equipment, realize the continuous growth of silicon carbide epitaxial layers-graphene.The SiC epitaxial layer quality that CVD obtains often compared with
Height, and can ensure that faster growth rate and doping control, it is different to be very suitable for high quality silicon carbide epitaxial layers-graphene
The growth of matter laminated film.The step of other this method has cast out hydrogen etching substrate surface and then has made up surface silicon enrichment,
Few layer graphene of high quality is obtained.
Although the present invention is disclosed above with preferred embodiment, so it is not limited to the present invention, any affiliated technology
Have in field with city skill, without departing from the spirit and scope of the present invention, when a little change and retouching, therefore this can be done
The protection domain of invention is defined when what the scope of the claim depending on the present invention was defined.
Claims (5)
1. a kind of preparation method of epitaxial silicon carbide-graphene composite film, it comprises the following steps：
Step 1：Pretreated substrate is placed in chemical vapor deposition chamber body, controls the chemical vapor deposition chamber body
Absolute truth reciprocal of duty cycle is more than 10-4Pa, 2~10 microns of silicon carbide epitaxial layers are grown in the substrate surface at 1500~1600 DEG C；
Step 2：The temperature of the chemical vapor deposition chamber body is controlled to be reduced to 1000 DEG C, to the chemistry under protective atmosphere
Vapor deposition chamber takes staged heat temperature raising, makes the silicon carbide epitaxial layers STRUCTURE DECOMPOSITION and restructuring, on the substrate
Obtain graphene composite bed；
The concrete operations of the staged heat temperature raising are：
Control the chemical vapor deposition chamber temperature to be increased to 1100 DEG C, and kept for 10 minutes；
Control the chemical vapor deposition chamber temperature to be increased to 1200 DEG C, and kept for 10 minutes；
The chemical vapor deposition chamber temperature rise is controlled up to 1300~1600 DEG C of scopes, and is kept for 30~50 minutes.
2. preparation method according to claim 1, it is characterised in that the substrate is SiC.
3. preparation method according to claim 1, it is characterised in that also include before the step 1：
Grow the thick cushions of 10~100nm on the substrate using molecular beam epitaxy.
4. preparation method according to claim 3, it is characterised in that the substrate is GaN or Al2O3；The cushion is
AlN。
5. preparation method according to claim 1, it is characterised in that to the chemical vapor deposition chamber in the step 2
The heating of body takes staged to heat up, and concrete operations are：
Control the chemical vapor deposition chamber temperature to be increased to 1100 DEG C, and kept for 10 minutes；
Control the chemical vapor deposition chamber temperature to be increased to 1200 DEG C, and kept for 10 minutes；
The chemical vapor deposition chamber temperature rise is controlled up to 1450~1600 DEG C of scopes, and is kept for 30~50 minutes.
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| CN106584968A (en) * | 2016-12-28 | 2017-04-26 | 镇江博昊科技有限公司 | Graphene composite material high in heat dissipation property |
| GB201809206D0 (en) * | 2018-06-05 | 2018-07-25 | Pontificia Univ Catolica Madre Y Maestra Autopista Duarte Km 1 1/2 | Sp3-bonded carbon materials, methods of manufacturing and uses thereof |
| CN110670138A (en) * | 2018-07-03 | 2020-01-10 | 中国科学院物理研究所 | Composite seed crystal for aluminum nitride single crystal growth and preparation method thereof |
| CN110648855B (en) * | 2019-09-26 | 2021-12-07 | 武汉理工大学 | Silicon carbide/graphene composite nano forest film material and preparation method and application thereof |
| CN112919456B (en) * | 2021-02-23 | 2023-09-22 | 南京大学 | Flat graphene growth method with uniform layer thickness and single-layer or double-layer graphene film |
| CN114314569B (en) * | 2022-01-10 | 2024-01-09 | 厦门大学 | Method for forming graphene on substrate |
| CN115537768B (en) * | 2022-12-01 | 2023-07-07 | 浙江晶越半导体有限公司 | Silicon carbide chemical vapor deposition method and multi-heat source horizontal wall heating type reactor |
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