CN111705359A - Method for preparing graphene single crystal wafer on copper-based textured film substrate - Google Patents
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- CN111705359A CN111705359A CN202010620665.8A CN202010620665A CN111705359A CN 111705359 A CN111705359 A CN 111705359A CN 202010620665 A CN202010620665 A CN 202010620665A CN 111705359 A CN111705359 A CN 111705359A
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- 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
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for preparing a graphene single crystal wafer on a copper-based textured film substrate, which comprises the following steps: s1: providing a copper-based textured film substrate, and placing the copper-based textured film substrate in a chemical vapor deposition system for annealing treatment; and S2: and introducing a gaseous carbon source, and epitaxially growing a graphene single crystal wafer on the surface of the copper-based textured film substrate. According to the method for preparing the graphene single crystal wafer on the copper-based texture film substrate, provided by the invention, the problem of high cost caused by epitaxial growth of the single crystal graphene wafer on the single crystal substrate is solved, the large-scale application of the graphene single crystal wafer is facilitated, and the method has an important significance for realizing the wide application of graphene in the field of microelectronics.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for preparing a graphene single crystal wafer on a copper-based textured film substrate.
Background
Graphene has excellent photoelectric properties and has great application potential in various fields, thereby drawing wide attention in various social circles. Among the numerous applications of graphene, the most attractive one is in the field of microelectronics. Graphene as a channel material is an important candidate material to replace the existing silicon material due to its ultra-high carrier mobility and is expected to continue moore's law. The mass preparation of the graphene single crystal wafer is a precondition for large-scale application of the graphene single crystal wafer in the field of microelectronics in the future. The existing graphene single crystal wafer is mainly prepared by epitaxially growing a graphene wafer by taking a metal single crystal or a germanium single crystal as a substrate. However, the cost of the single crystal substrate is generally high and has a high preparation technology threshold, and the cost of the graphene wafer is greatly increased when the substrate is used for preparing the graphene wafer, which is not beneficial to the large-scale application of the graphene single crystal wafer. Therefore, the graphene single crystal wafer can be epitaxially grown on the surface of the non-single crystal metal substrate, and the method has important significance for realizing wide application of graphene in the field of microelectronics.
Disclosure of Invention
The invention aims to provide a method for preparing a graphene single crystal wafer on a copper-based textured film substrate, so as to solve the problem of high cost caused by epitaxial growth of the single crystal graphene wafer on the single crystal substrate in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
the method for preparing the graphene single crystal wafer on the copper-based textured film substrate comprises the following steps: s1: providing a copper-based textured film substrate, and placing the copper-based textured film substrate in a chemical vapor deposition system for annealing treatment; and S2: and introducing a gaseous carbon source, and epitaxially growing a graphene single crystal wafer on the surface of the copper-based textured film substrate.
In step S1, the copper-based textured thin film substrate is composed of a main element copper and an auxiliary element nickel, wherein copper is an essential element.
Preferably, the number of the auxiliary element nickel atoms accounts for 0-30% of the total atomic ratio of the copper-based textured film substrate. If the content exceeds 30%, the number of graphene layers may be non-uniform, resulting in the occurrence of multi-layer graphene.
In step S1, the copper-based textured film substrate is a copper-based (111) textured film, the out-of-plane orientation is (111) preferred orientation, and the in-plane crystal domains form an included angle of 60 degrees.
In step S1, the deposition method includes: magnetron sputtering, thermal evaporation, electron beam evaporation and molecular beam epitaxy.
Preferably, in step S1, the thickness of the copper-based textured thin film substrate is 10nm to 3000 nm. Too low a thickness may result in the alloy film being volatile or agglomerated at high temperatures, and too high a thickness may result in increased film production costs.
Preferably, in step S1, annealing is performed in an argon/hydrogen gas atmosphere, wherein the annealing temperature ranges from 300 ℃ to 1050 ℃, the annealing time ranges from 10min to 180min, and the flow ratio of argon to hydrogen is (50sccm to 500sccm) to (10sccm to 100 sccm). More preferably, the annealing temperature is 500-1000 deg.C, the annealing time is 60-120 min, and the flow ratio of argon and hydrogen is (100-300 sccm): 20-80 sccm.
Preferably, in step S2, the growth temperature of the graphene ranges from 300 ℃ to 1050 ℃, the growth time ranges from 10min to 180min, and the flow ratio of argon to hydrogen ranges from 50sccm to 500sccm to 10sccm to 100 sccm. More preferably, the growth temperature of the graphene is 500-1000 ℃, the growth time is 60-120 min, and the flow ratio of the argon to the hydrogen is (100-300 sccm): 20-80 sccm.
In step S2, the gaseous carbon source for growing graphene is one or any combination of methane, ethane, acetylene, and ethylene.
According to a preferred scheme of the invention, the copper-based texture film substrate is prepared by deposition on the surface of sapphire at normal temperature by adopting a magnetron sputtering method.
According to the method provided by the invention, the copper-based texture film is used as the substrate, and annealing treatment and graphene growth are sequentially carried out, so that the graphene single crystal wafer is epitaxially grown on the surface of the non-single crystal substrate. The method overcomes the defect that a single crystal substrate is required for the growth of the graphene single crystal wafer in the prior art, and the single crystal substrate has high technical threshold and higher cost, so the method reduces the manufacturing cost of the graphene single crystal wafer. In addition, the morphology and single crystal property of the graphene are characterized by adopting an optical microscope, a scanning electron microscope, an atomic force microscope, Raman and low-energy electron diffraction, and the graphene single crystal prepared by the method is high in growth speed, consistent in orientation and good in crystallinity, so that the graphene single crystal has ultrahigh quality.
In a word, according to the method for preparing the graphene single crystal wafer on the copper-based texture film substrate, provided by the invention, the problem of high cost caused by epitaxial growth of the single crystal graphene wafer on the single crystal substrate is solved, the large-scale application of the graphene single crystal wafer is facilitated, and the method has important significance for realizing the wide application of graphene in the field of microelectronics.
Drawings
Fig. 1 is an optical microscope image of a graphene single crystal wafer according to a first embodiment;
fig. 2 is a picture of a scanning electron microscope of a graphene single crystal wafer according to an embodiment;
FIG. 3 is an atomic force microscope image of a single crystal graphene wafer according to one embodiment;
FIG. 4 is an XRD structure orientation of the Cu-Ni alloy thin film in the first example;
fig. 5 is a raman spectrum of a graphene single crystal wafer according to the first embodiment;
FIG. 6 is a low energy electron diffraction pattern of a single crystal graphene wafer according to one embodiment;
fig. 7 is a raman spectrum of the graphene single crystal wafer according to the second embodiment;
FIG. 8 is a low-energy electron diffraction pattern of a graphene single crystal wafer according to a second embodiment;
fig. 9 is a raman spectrum of the graphene single crystal wafer according to the third embodiment;
FIG. 10 is a low-energy electron diffraction pattern of a single-crystal graphene wafer according to the third embodiment;
fig. 11 is a raman spectrum of the graphene single crystal wafer according to the fourth embodiment;
FIG. 12 is a low-energy electron diffraction pattern of a graphene single crystal wafer according to the fourth embodiment;
fig. 13 is an optical microscope image of graphene prepared in example five on a silicon oxide surface.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example one
And depositing on the surface of the sapphire at normal temperature by adopting a magnetron sputtering method to form an 800nm copper-based textured film, wherein copper is a main element, nickel is an auxiliary element, and the content of the nickel element is 15%, so that the preparation of the copper-based textured film substrate is realized. Then, the copper-based texture thin film substrate is placed in a chemical vapor deposition system, annealing treatment is carried out in the protective atmosphere of argon and hydrogen, the flow ratio of argon to hydrogen is 300sccm:80sccm, the annealing temperature is 1000 ℃, the annealing time is 60min, then 10sccm methane is introduced, the growth temperature of the graphene thin film is 1000 ℃, and the graphene single crystal wafer grows for 10min, so that the graphene single crystal wafer grows on the surface of the copper-based texture thin film substrate in an epitaxial mode.
FIG. 1 is a topography of an optical microscope for graphene on the surface of a copper-based textured film, and it can be seen from the topography that the surface of other places except the crystal boundary of a substrate is flat; FIG. 2 is a scanning electron microscope image of graphene on the surface of a copper-based textured film, which shows that a large number of grain boundaries exist on the surface of a substrate film, the surface of other areas is flat, and fluctuation and wrinkles of the graphene cannot be observed; FIG. 3 is an AFM topography of graphene on the surface of a copper-based textured film, and the surface of the graphene can be seen to be flat; FIG. 4 is an XRD orientation diagram in the plane of the copper-based textured film, and the XRD diagram shows that the alloy film has 2 sets of diffraction peaks, which shows that the copper-based textured film has 2 crystal domains in the plane and the angle of the crystal domains is 60 degrees; as shown in fig. 5, a raman peak of graphene is not shown by a defect peak; as shown in fig. 6, LEED diffraction spots of graphene on the surface of the copper-based textured film in the first example show that the graphene is uniformly oriented as a single crystal film.
Example two
The difference between this embodiment and the first embodiment is: the content of nickel element in the copper-based textured film substrate prepared in the first embodiment is adjusted from 15% to 10%, the flow ratio of argon to hydrogen is 200sccm:50sccm, the annealing temperature is 800 ℃, the annealing time is 100min, the growth temperature of the graphene film is 300 ℃, and the rest process parameters are the same as those of the first embodiment. As shown in FIG. 7, the Raman spectrum of the inside of the crystal domain was analyzed at-1600 cm-1And-2700 cm-1And a characteristic peak of graphene appears, and the absence of a defect peak proves that the grown graphene is high in quality. As shown in fig. 8, the LEED diffraction spots of the graphene on the surface of the copper-nickel alloy thin film in the second example show that the graphene is uniformly oriented and is a single crystal thin film.
EXAMPLE III
The difference between this embodiment and the first embodiment is: the content of nickel element in the copper-based textured film substrate in the first embodiment is adjusted to be 5%, the flow ratio of argon to hydrogen is 100sccm:20sccm, the annealing temperature is 500 ℃, the annealing time is 120min, the growth temperature of the graphene film is 500 ℃, and the rest process parameters are the same as those in the first embodiment. As shown in FIG. 9, the Raman spectrum of the inside of the crystal domain was analyzed at-1600 cm-1And-2700 cm-1A characteristic peak of graphene appears, and a defect peak of the graphene is not observed, so that the quality of the grown graphene is high; fig. 10 is a LEED diffraction pattern of graphene on the surface of the alloy textured thin film in this example, and the result shows that the graphene on the surface of the copper-nickel textured thin film is uniformly oriented and is a single crystal thin film.
Example four
The difference between this embodiment and the first embodiment is: the content of nickel element in the copper-based textured film substrate in the first embodiment is adjusted to 0%, the flow ratio of argon to hydrogen is 100sccm:20sccm, the annealing temperature is 300 ℃, the annealing time is 180min, the growth temperature of the graphene film is 800 ℃, and the rest process parameters are the same as those in the first embodiment. As shown in FIG. 11, the Raman spectrum of the inside of the crystal domain was analyzed at-1600 cm-1And-2700 cm-1A characteristic peak of graphene appears at 1400cm-1No hair nearbyThe defect peak of the graphene proves that the quality of the grown graphene is high; as shown in fig. 12, the LEED diagram of graphene on the surface of the copper-based textured film in this example shows that the graphene is uniformly oriented and is a single crystal film.
EXAMPLE five
The difference between this embodiment and the first embodiment is: the content of nickel element in the copper-based textured film substrate in the first embodiment is adjusted to 40%, and the rest of the process parameters are the same as those in the first embodiment. As shown in fig. 13, when the grown graphene was transferred to the surface of silicon oxide, many double-layer graphene domains were observed. The uniformity of the graphene is relatively poor, and the multilayer graphene is easily obtained during growth.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
1. A method for preparing a graphene single crystal wafer on a copper-based textured film substrate is characterized by comprising the following steps:
s1: providing a copper-based textured film substrate, and placing the copper-based textured film substrate in a chemical vapor deposition system for annealing treatment; and
s2: and introducing a gaseous carbon source, and epitaxially growing a graphene single crystal wafer on the surface of the copper-based textured film substrate.
2. The method according to claim 1, wherein in step S1, the copper-based textured thin film substrate is composed of a main element copper and an auxiliary element nickel, wherein copper is an essential element.
3. The method according to claim 2, wherein the number of atoms of the auxiliary element nickel is in the range of 0 to 30% of the total number of atoms of the copper-based textured thin film substrate.
4. The method according to claim 1, wherein in step S1, the copper-based textured film substrate is a copper-based (111) textured film, the out-of-plane orientation is a (111) preferred orientation, and the in-plane domains form an included angle of 60 degrees.
5. The method of claim 1, wherein the depositing in step S1 comprises: magnetron sputtering, thermal evaporation, electron beam evaporation and molecular beam epitaxy.
6. The method of claim 1, wherein in step S1, the thickness of the copper-based textured thin film substrate is 10nm to 3000 nm.
7. The method as claimed in claim 1, wherein in step S1, the annealing process is performed in an argon/hydrogen atmosphere at an annealing temperature ranging from 300 ℃ to 1050 ℃, for an annealing time ranging from 10min to 180min, and at an argon/hydrogen flow ratio ranging from 50sccm to 500sccm to 10sccm to 100 sccm.
8. The method as claimed in claim 1, wherein in step S2, the graphene is grown at a temperature ranging from 300 ℃ to 1050 ℃, for a time ranging from 10min to 180min, and at a flow ratio of argon to hydrogen ranging from 50sccm to 500sccm to 10sccm to 100 sccm.
9. The method according to claim 1, wherein in step S2, the gaseous carbon source for growing graphene is one or any combination of methane, ethane, acetylene and ethylene.
10. The method according to claim 1, wherein the copper-based textured thin film substrate is prepared by deposition on the surface of sapphire at normal temperature by using a magnetron sputtering method.
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| CN114525581A (en) * | 2022-02-11 | 2022-05-24 | 中国科学院上海微***与信息技术研究所 | Preparation method of double-layer 30-degree torsion angle graphene single crystal wafer |
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