CN101492835A - Method for extension of plumbago alkene with ultra-thin hexagonal phase silicon carbide membrane on insulated substrate - Google Patents
Method for extension of plumbago alkene with ultra-thin hexagonal phase silicon carbide membrane on insulated substrate Download PDFInfo
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- CN101492835A CN101492835A CNA2008100567276A CN200810056727A CN101492835A CN 101492835 A CN101492835 A CN 101492835A CN A2008100567276 A CNA2008100567276 A CN A2008100567276A CN 200810056727 A CN200810056727 A CN 200810056727A CN 101492835 A CN101492835 A CN 101492835A
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Abstract
The invention provides a method for preparing graphene by epitaxy of an ultrathin hexagonal phase silicon carbide film on an insulating substrate. The method is characterized by comprising the following steps: step one, taking the insulating substrate; step two, carrying out high-temperature etching pretreatement on the insulating substrate by hydrogen to remove surface scratch and other deficiencies so as to obtain flat surface; step three, carrying out high-temperature nitrogen treatment on the insulating substrate to activate the epitaxial surface so as to ensure that subsequent silicon carbide can be easily adhered on the surface of the substrate and maintain the same crystallographic orientation relationship with the substrate; step four, extending the hexagonal phase monocrystal silicon carbide on the insulating substrate; and step five, vaporizing silicon ions in the silicon carbide to complete preparation of the graphene on the insulating substrate.
Description
Technical field
The invention belongs to semi-conductor low-dimensional thin-film material preparation field, particularly relate to a kind of method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate.
Background technology
Graphene (Graphene) is a kind of by individual layer or the several layers of thin slice that (being lower than 100 layers) carbon atom is formed, two-dimentional graphite flake like this has been proved many superpower attributes, electronics as it transports in the trajectory mode in the submicron distance, do not have any scattering, have very attracting conductive capability, this provides condition for making super performance transistor.The Graphene transistor can at room temperature be worked, and has the prophesy graphene film may final substituted for silicon, and is because the Graphene transistor is more efficient than silicone tube, faster and power consumption is lower.
Graphene has brought a new opportunity to semicon industry, when the silicon processing procedure of following 65nm, 45nm even 32nm can not satisfy the semi-conductor industry demand, perhaps just should substitute it by Graphene.Present challenge is how to make this film with low cost and be suitable for large-scale application.Two kinds of typical graphene preparation methods are arranged, and a kind of is to scrape from the pyrolytic carbon of high orientation with mechanical means to clash individual layer or number layer graphene thin slice (K.S.Novoselov, science, 2004).Another kind method is to evaporate one or more layers (being lower than 100 layers) Siliciumatom in the thermal evaporation mode from the silicon carbide single-crystal surface of six side's phases, goes out Graphene (C.Berger, science, 2006) with this extension.Two kinds of methods by comparison, a kind of method in back helps preparing extensive Graphene, and it and current silicon planner technology compatibility mutually, thereby is expected to be applied in semicon industry.But a kind of method in back will be used the semi-insulating substrate of expensive silicon carbide, and this makes that the cost of epitaxial graphite alkene is too high, in addition, interaction between silicon carbide substrates and the Graphene, restricted the device performance (F.Varchon, Physical ReviewLetters, 2007) of Graphene.
The pros and cons of comprehensive above-mentioned graphene preparation method the present invention proposes a kind of new epitaxial graphite alkene preparation method.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of two-dimentional epitaxial graphite alkene, this method epitaxial graphite alkene does not rely on expensive semi-insulating silicon carbide substrate, but is prepared by the ultra-thin silicon carbide layer of extension by insulation cheap and easy to get six side's phase monocrystal substrates.
Another object of the present invention is to provide a kind of preparation method of two-dimentional epitaxial graphite alkene, the substrate of this method insulate fully, and the electrical property of epitaxial graphite alkene is not restricted by substrate;
Another purpose of the present invention is to provide a kind of preparation method of two-dimentional epitaxial graphite alkene, and the number of plies of this method epitaxial graphite alkene can design the number of plies of Graphene as required by the carbon silicon diatomic number of plies decision of ultra-thin silicon carbide film.
The technical solution used in the present invention is:
The invention provides a kind of method, it is characterized in that, comprise the steps: by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate
Step 1: get an insulating substrate;
Step 2: adopt hydrogen that insulating substrate is carried out the pre-treatment of high temperature etching, be used to remove defectives such as surface scratch, surface etch is smooth;
Step 3: insulating substrate is carried out high-temperature ammonolysis handle, be used to activate epitaxial surface, make follow-up silicon carbide be easy to keep identical crystal orientation relation attached to substrate surface and with substrate;
Step 4: extension six side's phase monocrystal attitude silicon carbide on insulating substrate;
Step 5: the Siliciumatom in the silicon carbide is evaporated, finish and on insulating substrate, prepare Graphene.
Wherein insulating substrate is the monocrystalline attitude, has six side's phase structures, and the epitaxial surface of insulating substrate is C (0001) face or R (1122) face.
Wherein epitaxial silicon carbide is to adopt high temperature chemical vapor deposition method extension on insulating substrate, and this silicon carbide is superthin layer.
Be to adopt NH when wherein insulating substrate is carried out the high-temperature ammonolysis processing
3Or N
2
Wherein during the insulating substrate epitaxial silicon carbide, the employing rare gas element is carrier gas.
Wherein during the insulating substrate epitaxial silicon carbide, adopting the single reaction thing of carbon containing and Siliciumatom is precursor.
Wherein during the insulating substrate epitaxial silicon carbide, adopting carbon source and silicon source mixed reactant is precursor.
Wherein during the insulating substrate epitaxial silicon carbide, the etching precursor when adopting the silicon source of HCl or chloride element to be epitaxy.
Wherein the insulating substrate epitaxial silicon carbide is the monocrystalline attitude, six side's phase structures, and thickness is 1～100 carbon silicon diatomic bed thickness.
Wherein the Siliciumatom in the silicon carbide being evaporated is the method that adopts thermal evaporation.
Wherein thermal evaporation temperature is 1100～1800 ℃, and air pressure is 10
-9～10
-4Handkerchief, the time is 0.2～5 hour.
The beneficial effect that the present invention has is:
(1) epitaxial graphite alkene does not rely on expensive semi-insulating silicon carbide substrate, but is prepared by the ultra-thin silicon carbide layer of extension by insulation cheap and easy to get six side's phase monocrystal substrates;
(2) substrate insulate fully, and the electrical property of epitaxial graphite alkene is not restricted by substrate;
(3) number of plies of epitaxial graphite alkene can design the number of plies of Graphene as required by the carbon silicon diatomic number of plies decision of ultra-thin silicon carbide film.
Description of drawings
For further specifying concrete technology contents of the present invention, below in conjunction with embodiment and accompanying drawing describes in detail as after, wherein:
Fig. 1 is the insulating substrate synoptic diagram that the present invention uses;
Fig. 2 is the device synoptic diagram of epitaxial silicon carbide superthin layer of the present invention;
Fig. 3 is a silicon carbide superthin layer synoptic diagram of the present invention;
Fig. 4 is the device synoptic diagram of epitaxial graphite alkene of the present invention;
Fig. 5 is an epitaxial graphite alkene synoptic diagram of the present invention
Among the figure:
10, insulating substrate
20, substrate bracket
30, inlet mouth
40, air outlet
50, chemical gas phase epitaxial apparatus
60, superthin layer silicon carbide
70, Graphene
Embodiment
The present invention be may further comprise the steps by super thin hexagonal phase silicon carbide membrane prepare epitaxial graphite alkene on the insulating substrate:
1) as shown in Figure 1, prepare insulating substrate 10, chemical rightenning epitaxy surface adopts the semiconductor wafer cleaning of standard to clean up, and epitaxial surface does not stain;
2) as shown in Figure 2, adopt chemical gas phase epitaxial apparatus 50 (being conventional device), carry out the high temperature chemical vapor deposition epitaxy of silicon carbide superthin layer.Insulating substrate 10 is placed in the insulating substrate holder 20, feed hydrogen toward inlet mouth 30, do-nothing system runs in air outlet 40, insulating substrate 10 surfaces are warmed up to assigned temperature, insulating substrate 10 is carried out the hydrogen etching, defective such as the surface scratch removing that is etched this moment, epitaxial surface is more smooth;
3) feed ammonia (or nitrogen) toward inlet mouth 30, air outlet 40 connects vacuum system, keep specified pressure in the growth chamber, insulating substrate 10 surfaces are warmed up to assigned temperature, insulating substrate 10 is carried out nitriding treatment, this moment, epitaxial surface fully activated, and follow-up silicon carbide diatomic layer is easy to have identical crystal orientation relation attached to substrate surface and with substrate;
4) close ammonia (or nitrogen), keep logical rare gas element (as hydrogen), air outlet 40 connects vacuum system, keep specified pressure in the growth chamber, insulating substrate 10 surfaces are warmed up to assigned temperature, feed carbon source and silicon source gas simultaneously and carry out 60 epitaxys of superthin layer silicon carbide, epitaxy defect is carried out the elimination of original position etching if the not chloride element of used silicon source gas then feeds HCl.The growth finish after as shown in Figure 3;
5) as shown in Figure 4, close all gas, air outlet 40 connects vacuum system, keep specified pressure in the growth chamber, insulating substrate 10 surfaces are warmed up to assigned temperature, and after insulation for some time, the silicon carbide 60 of insulating substrate 10 surperficial extensions all is converted into Graphene 70, the gained Graphene is two-dimentional crystalline structure, the growth finish after as shown in Figure 5.
Embodiment 1
Adopt monocrystalline sapphire substrate (α-Al
2O
3) (insulating substrate 10), C (0001) handles through chemical rightenning on the surface, put into growth furnace after cleaning up, feed hydrogen the monocrystalline sapphire substrate surface is carried out the etching polishing, hydrogen flowing quantity is 3000sccm during etching, monocrystalline sapphire substrate surface temperature is 1350 ℃, and growth room's pressure is normal pressure, etching 30 minutes.The intact back substrate surface of etching can see the planeness of atom level not having defectives such as cut at microscopically.Feed ammonia then the monocrystalline sapphire substrate surface is carried out nitriding treatment, ammonia flow is 1sccm during nitrogenize, and monocrystalline sapphire substrate surface temperature is 1500 ℃, 40 holders of growth room's pressure, nitriding treatment 10 minutes.Keep feeding hydrogen, close ammonia, feed C simultaneously
3H
8And SiHCl
3Carry out the superthin layer silicon carbide epitaxial growth, monocrystalline sapphire substrate surface temperature is 1500 ℃ during growth, growth room's pressure 10
-2Handkerchief, C
3H
8And SiHCl
3Flow is respectively 0.1sccm and 0.3sccm, growth time 5 minutes.The silicon carbide of preparation has identical crystal formation and crystal orientation relation with substrate.Close all gas, keeping monocrystalline sapphire substrate surface temperature is 1500 ℃, and growth room's pressure is adjusted into 10
-7Handkerchief kept 30 minutes, the silicon carbide of extension all can be converted into the Graphene of two-dimentional crystalline state.
Though the present invention discloses as above with preferred embodiment; right its is not in order to limit the present invention; have in the technical field under any and know the knowledgeable usually; without departing from the spirit and scope of the present invention; when can doing a little change and retouching, thus protection scope of the present invention when look claim of the present invention scope defined is as the criterion.
Claims (11)
1, a kind of method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate is characterized in that, comprises the steps:
Step 1: get an insulating substrate;
Step 2: adopt hydrogen that insulating substrate is carried out the pre-treatment of high temperature etching, be used to remove defectives such as surface scratch, surface etch is smooth;
Step 3: insulating substrate is carried out high-temperature ammonolysis handle, be used to activate epitaxial surface, make follow-up silicon carbide be easy to keep identical crystal orientation relation attached to substrate surface and with substrate;
Step 4: extension six side's phase monocrystal attitude silicon carbide on insulating substrate;
Step 5: the Siliciumatom in the silicon carbide is evaporated, finish and on insulating substrate, prepare Graphene.
2, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that wherein insulating substrate is the monocrystalline attitude, has six side's phase structures, and the epitaxial surface of insulating substrate is C (0001) face or R (1122) face.
3, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, wherein epitaxial silicon carbide is to adopt high temperature chemical vapor deposition method extension on insulating substrate, and this silicon carbide is superthin layer.
4, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, is to adopt NH when wherein insulating substrate is carried out the high-temperature ammonolysis processing
3Or N
2
5, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, wherein during the insulating substrate epitaxial silicon carbide, the employing rare gas element is carrier gas.
6, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, wherein during the insulating substrate epitaxial silicon carbide, adopting the single reaction thing of carbon containing and Siliciumatom is precursor.
7, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, wherein during the insulating substrate epitaxial silicon carbide, adopting carbon source and silicon source mixed reactant is precursor.
8, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, wherein during the insulating substrate epitaxial silicon carbide, and the etching precursor when adopting the silicon source of HCl or chloride element to be epitaxy.
9, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that wherein the insulating substrate epitaxial silicon carbide is the monocrystalline attitude, six side's phase structures, and thickness is 1～100 carbon silicon diatomic bed thickness.
10, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 1 is characterized in that, wherein the Siliciumatom in the silicon carbide being evaporated is the method that adopts thermal evaporation.
11, the method by super thin hexagonal phase silicon carbide film epitaxial graphite alkene on the insulating substrate according to claim 11 is characterized in that wherein thermal evaporation temperature is 1100～1800 ℃, and air pressure is 10
-9～10
-4Handkerchief, the time is 0.2～5 hour.
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