CN111690982A - Method for growing single crystal graphene by using single crystal copper foil with any index surface - Google Patents
Method for growing single crystal graphene by using single crystal copper foil with any index surface Download PDFInfo
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- CN111690982A CN111690982A CN201910179967.3A CN201910179967A CN111690982A CN 111690982 A CN111690982 A CN 111690982A CN 201910179967 A CN201910179967 A CN 201910179967A CN 111690982 A CN111690982 A CN 111690982A
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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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- 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
- C30B25/10—Heating of the reaction chamber or the substrate
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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
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
Abstract
The invention provides a method for growing single crystal graphene by using single crystal copper foil with any index surface for the first time, which comprises the following steps: s1, preparing single crystal copper foil with any index surface; s2, selecting the single crystal copper foil as a substrate, and growing high-quality and oversized single crystal graphene on the substrate. According to the invention, large-size single crystal graphene grows on common crystal faces such as non-Cu (111), Cu (100) and the like for the first time, and continuous large-size single crystal graphene grows on single crystal copper foils successfully preparing crystal faces such as Cu (211), Cu (323), Cu (110), Cu (236), Cu (331), Cu (256), Cu (553), Cu (659), Cu (736), Cu (748), Cu (671) and the like; the graphene with uniform single layer and high quality is grown on the crystal faces.
Description
Technical Field
The invention relates to a method for preparing ultra-large size (meter-scale) single crystal graphene by using single crystal copper foil with any index surface as a substrate.
Background
Rouff et al, 2009, discovered that high quality single layer graphene can be obtained using Chemical Vapor Deposition (CVD) with copper foil as the substrate and catalyst. The method has the characteristics of simple and convenient operation, extremely low cost and the like, so that the CVD method is the most common method for obtaining the graphene at present and is the most possible breakthrough of the graphene which really goes to industrial-grade application.
However, common industrial polycrystalline copper foils are commonly used for preparing graphene at present, and different crystal orientations, defects, roughness and grain boundaries of the polycrystalline copper foils have great influence on the quality of the graphene, so that the large-size single crystal copper foil with few defects and no grain boundaries is the key point for growing a high-quality single crystal graphene sample; in recent years, this group has succeeded in obtaining single crystal Cu (111) by an appropriate annealing method and growing large-sized (meter-sized) graphene single crystals as a growth substrate. However, growing some unusual single-crystal copper foils with crystal face indexes (Cu (211), Cu (553)) to large sizes (e.g., meter size) still remains a great problem to be solved urgently in the industry, and further limits the growth of large-size (meter size) single-crystal graphene on these unusual single-crystal copper foils with crystal face indexes.
Disclosure of Invention
The invention firstly provides a method for preparing ultra-large-size single crystal graphene by using single crystal copper foils with any index planes as substrates (including some common single crystal copper foils with index planes, such as Cu (211) and Cu (553)), and using the substrates.
The invention provides a method for growing single crystal graphene by using single crystal copper foil with any index surface, which comprises the following steps:
s1, preparing single crystal copper foil with any index surface;
s2, selecting the single crystal copper foil as a substrate, and growing high-quality and oversized single crystal graphene on the substrate.
Preferably, step S1 specifically includes the following steps:
s11, placing the polycrystalline copper foil in a tube furnace, heating the tube furnace to 150-200 ℃ in air, and oxidizing the polycrystalline copper foil;
s12, introducing Ar gas and H into the tube furnace2Mixed gas of gases, Ar gas and H2The flow ratio of the gas is 10: 1-100: 1, then openThe temperature is raised to 950 ℃ and 1060 ℃, and the temperature raising process lasts for 60-120 min;
s13, when the temperature is increased to 950-1060 ℃, Ar gas and H2Keeping the gas flow unchanged, and carrying out an annealing process;
s14, after the annealing is finished, the heating power supply is closed, and Ar and H are added2And naturally cooling to room temperature as protective gas to obtain the single crystal copper foil.
Preferably, the oxidation time in step S11 is 30-120 min.
Preferably, Ar gas and H gas in step S122The flow rates of gas were 1000sccm and 20sccm, respectively.
Preferably, the duration of the annealing is 120-500 min.
Preferably, step S2 specifically includes the following steps:
s21, placing the single crystal copper foil obtained in the step S1 into a tube furnace, introducing argon Ar with the flow of 500sccm or more, and then heating for 50-70 min to 900-1060 ℃;
s22, when the temperature rises to 900-1060 ℃, introducing H2Gas, H2The flow is 5-500 sccm, the Ar flow is kept unchanged, the annealing process is carried out, the temperature is kept unchanged, and the annealing duration is 5-180 min;
s23, introducing CH after the annealing is finished4Mixed gas (CH) of Ar and4the content is 200-20000 ppm), the flow rate of the mixed gas is 0.2-50 sccm, and the growth time is 10 min-20 h;
s24, after the growth is finished, the heating power supply is closed, the CH4 gas is stopped being introduced, and Ar and H are added2And naturally cooling to room temperature for protecting gas, namely obtaining high-quality large-size single crystal graphene on the single crystal copper foil with any index surface.
Preferably, the index surface of the single-crystal copper foil is Cu (211), Cu (323), Cu (110), Cu (236), Cu (331), Cu (256), Cu (553), Cu (659), Cu (736), Cu (748), or Cu (671).
Preferably, the prepared single crystal graphene has a radial dimension of 5-40 cm and a transverse dimension of 5-20 cm.
Preferably, the single crystal graphene prepared on any index plane has consistent orientation and can be spliced into a continuous film.
The invention also provides high-quality and ultra-large-size single crystal graphene, which is prepared by the method, and the prepared single crystal graphene has the radial size of 5-40 cm and the transverse size of 5-20 cm.
The method comprises the steps of using the existing single crystal copper foil with any index surface as a raw material, removing surface impurities by an annealing process, using the single crystal copper foil as a substrate, and obtaining the ultra-large-size high-quality single crystal graphene by using a normal-pressure chemical vapor deposition method.
The invention has the advantages that:
1. according to the method, the ultra-large-size single crystal graphene can be prepared only by taking the existing single crystal copper foil with any index surface as a growth substrate, other special treatment is not needed, and the growth process is simple;
2. according to the invention, large-size single crystal graphene grows on common crystal faces such as non-Cu (111) and Cu (100) for the first time, and large-size single crystal graphene grows on crystal faces such as Cu (211), Cu (323), Cu (110), Cu (236), Cu (331), Cu (256), Cu (553), Cu (659), Cu (736), Cu (748) and Cu (671);
3. the oversized single crystal graphene prepared on the single crystal copper substrate with any index surface by adopting a chemical vapor deposition method has the advantages of few defects, high quality and good application prospect;
4. the method is simple, efficient and low in cost, and is beneficial to promoting the practical application of large-size single crystal graphene in the industrial field.
Drawings
Fig. 1 is an optical photograph of graphene grown on a single-crystal copper foil having two crystal planes (Cu (211) and Cu (553)), and fig. 1a and 1b show the shape of graphene on the Cu (211) crystal plane, and fig. 1c and 1d show the shape of graphene on the Cu (553) crystal plane, and thus the orientation of graphene is very consistent.
Fig. 2 shows EBSD results of selected single crystal copper foils of two crystal planes, wherein fig. 2a shows EBSD results of Cu (211) crystal plane, and fig. 2b shows EBSD results of Cu (553) crystal plane.
Fig. 3 is a raman characterization result of graphene grown on a single crystal copper foil with 12 crystal planes, and the result shows that uniform and high-quality single-layer graphene is grown on the crystal planes.
FIG. 4 is single crystal graphene on large size single crystal copper, FIG. 4a is large size high quality single crystal graphene on Cu (211) crystal face single crystal copper foil, FIG. 4b is large size high quality single crystal graphene on Cu (553) crystal face single crystal copper foil, both pictures show that the graphene size on single crystal copper foil is 40X 20cm2The magnitude of the graphene is larger than that of the single crystal graphene; gr in the figure represents graphene (graphene).
Detailed Description
The present invention will be described in further detail with reference to specific examples, which are conventional unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
The first implementation mode comprises the following steps: a method for growing a single crystal copper foil with an uncommon index surface comprises the following steps:
putting commercial polycrystalline copper foil into a tube furnace, heating to 150-200 ℃ in air, and oxidizing for 60 min;
(II) introducing Ar gas and H2Gas with the flow rate of 1000sccm and 20sccm is heated to 1050 ℃ for 80 min;
thirdly, when the temperature rises to 1050 ℃, Ar gas and H2Keeping the gas flow unchanged, and carrying out an annealing process, wherein the annealing duration is 300 min;
(IV) after the annealing is finished, turning off the heating power supply, and using Ar and H2Naturally cooling to room temperature for protecting gas.
The uncommon index plane refers to crystal planes of Cu (211), Cu (323), Cu (110), Cu (236), Cu (331), Cu (256), Cu (553), Cu (659), Cu (736), Cu (748), Cu (671) and the like.
Conventionally, when a single crystal copper foil having a crystal face common to Cu (111), Cu (100), or the like is grown, an atmosphere in the temperature raising process is generally an inert gas, and a hydrogen gas is introduced at an annealing temperature. In the growing unusual index surface of the present inventionThe single crystal copper foil of (1) is oxidized by heating to a temperature of 200 ℃ or lower in air, and Ar gas and H gas are used at an annealing temperature2A gas. It should be noted that the above method for growing a single crystal copper foil with an unusual index plane can also be used for growing a single crystal copper foil with a usual crystal plane such as Cu (111) or Cu (100).
Through the test operation, the single crystal copper foils with different crystal faces can be obtained for the growth of the following graphene.
The second embodiment: a method for growing single crystal graphene by using single crystal copper foil with any index surface comprises the following steps:
test one:
putting the Cu (211) single-crystal copper foil obtained in the first embodiment into a tube furnace, introducing argon gas at the flow rate of 500sccm, and then heating for 70min to 1010 ℃;
(II) when the temperature rises to 1010 ℃, introducing H2Gas, H2The flow is 10sccm, the Ar flow is kept unchanged, the annealing process is carried out, the temperature is kept unchanged, and the annealing duration is 40 min;
(III) after the annealing is finished, introducing CH4Mixed gas (CH) of Ar and4the content is 200-20000 ppm), the flow rate of the mixed gas is 1sccm, and the growth time is 1 h;
(IV) after the growth is finished, closing the heating power supply and stopping introducing CH4Gas with Ar and H2And naturally cooling to room temperature for protecting gas, namely obtaining the high-quality single crystal graphene with discrete domains on the single crystal Cu (211).
The EBSD of the single crystal copper foil used in this test is shown in fig. 2a, which demonstrates perfect single crystal Cu (211); as shown in the optical diagrams of fig. 1a and 1b, the prepared single crystal graphene sample has strong orientation consistency among graphene domains grown on a single crystal Cu (211) substrate; meanwhile, raman of fig. 3 indicates that the graphene is of single-layer high quality.
And (2) test II:
putting the Cu (553) single crystal copper foil obtained in the first embodiment into a tube furnace, introducing argon gas at the flow rate of 500sccm, and then heating for 70min to 1010 ℃;
(II) when the temperature rises to 1010 ℃, introducing H2Gas, H2The flow is 10sccm, the Ar flow is kept unchanged, the annealing process is carried out, the temperature is kept unchanged, and the annealing duration is 40 min;
(III) after the annealing is finished, introducing CH4Mixed gas (CH) of Ar and4the content is 200-20000 ppm), the flow rate of the mixed gas is 1sccm, and the growth time is 1 h;
(IV) after the growth is finished, closing the heating power supply and stopping introducing CH4Gas with Ar and H2And naturally cooling to room temperature for protecting gas, namely obtaining the single crystal graphene with high quality discrete domains on the single crystal Cu (553).
The EBSD of the single crystal copper foil used in this test is shown in fig. 2b, and is proved to be perfect single crystal Cu (553); as shown in the optical diagrams of fig. 1c and 1d, the prepared single crystal graphene samples have strong orientation consistency among graphene domains grown on a single crystal Cu (553) substrate; meanwhile, raman of fig. 3 indicates that the graphene is of single-layer high quality.
And (3) test III:
putting the twelve single crystal copper foils with different index surfaces obtained in the first embodiment into a tube furnace, introducing argon gas at the flow rate of 500sccm, and then heating for 70min to 1010 ℃;
(II) when the temperature rises to 1010 ℃, introducing H2Gas, H2The flow is 10sccm, the Ar flow is kept unchanged, the annealing process is carried out, the temperature is kept unchanged, and the annealing duration is 40 min;
(III) after the annealing is finished, introducing CH4Mixed gas (CH) of Ar and4the content is 200-20000 ppm), the flow rate of the mixed gas is 1sccm, and the growth time is 1 h;
(IV) after the growth is finished, closing the heating power supply and stopping introducing CH4Gas with Ar and H2And naturally cooling to room temperature for protecting gas, namely obtaining the high-quality single crystal graphene in discrete domains on the copper foil with any index surface.
After the growth is finished, raman characterization is performed, and fig. 3 shows raman on the twelve crystal planes, and the result shows that high-quality single-layer graphene is obtained on all the twelve crystal planes.
The twelve crystal planes include crystal planes of Cu (111), Cu (211), Cu (323), Cu (110), Cu (236), Cu (331), Cu (256), Cu (553), Cu (659), Cu (736), Cu (748), Cu (671), and the like.
The third embodiment is as follows: method for growing large-size single crystal graphene by using large-size single crystal copper foil with any index surface
The test was carried out as follows:
respectively putting the large-size single crystal Cu obtained in the first embodiment into a tube furnace, wherein the size of the large-size single crystal Cu is 39 x 18cm2Introducing argon at the flow rate of 500sccm, and heating to 1010 ℃ for 70 min;
(II) when the temperature rises to 1010 ℃, introducing H2Gas, H2The flow is 10sccm, the Ar flow is kept unchanged, the annealing process is carried out, the temperature is kept unchanged, and the annealing duration is 40 min;
(III) after the annealing is finished, introducing CH4Mixed gas (CH) of Ar and4the content is 200-20000 ppm), the flow rate of the mixed gas is 1sccm, and the growth time is 5 hours;
(IV) after the growth is finished, closing the heating power supply and stopping introducing CH4Gas with Ar and H2And naturally cooling to room temperature for protecting gas, namely obtaining the continuous single crystal graphene film on the large-size single crystal copper foil with any index surface.
The results obtained in this embodiment show that by prolonging the growth time, a continuous single crystal graphene film can be prepared on a large-size single crystal copper foil of any index surface. FIG. 4a is a photograph of large size single crystal graphene on single crystal Cu (211) with dimensions 39X 18.5cm2FIG. 4b is a photograph of large size single crystal graphene on single crystal Cu (553) with dimensions 39 × 21cm2. Large-size single crystalline graphene that can be obtained on single crystalline copper includes, but is not limited to, these two crystal planes.
Claims (10)
1. A method for growing single crystal graphene by using single crystal copper foil with any index surface is characterized by comprising the following steps:
s1, preparing single crystal copper foil with any index surface;
s2, selecting the single crystal copper foil as a substrate, and growing high-quality and oversized single crystal graphene on the substrate.
2. The method according to claim 1, wherein step S1 specifically comprises the steps of:
s11, placing the polycrystalline copper foil in a tube furnace, heating the tube furnace to 150-200 ℃ in air, and oxidizing the polycrystalline copper foil;
s12, introducing Ar gas and H into the tube furnace2Mixed gas of gases, Ar gas and H2The flow ratio of the gas is 10: 1-100: 1, then starting to heat to 950-1060 ℃, and continuing the heating process for 60-120 min;
s13, when the temperature is increased to 950-1060 ℃, Ar gas and H2Keeping the gas flow unchanged, and carrying out an annealing process;
s14, after the annealing is finished, the heating power supply is closed, and Ar and H are added2And naturally cooling to room temperature as protective gas to obtain the single crystal copper foil.
3. The method as claimed in claim 2, wherein the oxidation time in step S11 is 30-120 min.
4. The method of claim 2, wherein the Ar gas and the H gas in step S122The flow rates of gas were 1000sccm and 20sccm, respectively.
5. The method as claimed in claim 2, wherein the annealing duration in step S13 is 120-500 min.
6. The method according to claim 1, wherein step S2 specifically comprises the steps of:
s21, placing the single crystal copper foil obtained in the step S1 into a tube furnace, introducing argon Ar with the flow of 500sccm or more, and then heating for 50-70 min to 900-1060 ℃;
s22, when the temperature rises to 900-1010 ℃, introducing H2Gas, H2The flow is 5-500 sccm, the Ar flow is kept unchanged, the annealing process is carried out, the temperature is kept unchanged, and the annealing duration is 5-180 min;
s23, introducing CH after the annealing is finished4Mixed gas (CH) of Ar and4the content is 200-20000 ppm), the flow rate of the mixed gas is 0.2-50 sccm, and the growth time is 10 min-20 h;
s24, after the growth is finished, the heating power supply is closed, the CH4 gas is stopped being introduced, and Ar and H are added2And naturally cooling to room temperature for protecting gas, namely obtaining high-quality large-size single crystal graphene on the single crystal copper foil with any index surface.
7. The method according to any one of claims 1 to 6, wherein the index face of the single-crystal copper foil is Cu (211), Cu (323), Cu (110), Cu (236), Cu (331), Cu (256), Cu (553), Cu (659), Cu (736), Cu (748), or Cu (671).
8. The method according to any one of claims 1 to 6, wherein the prepared single-crystal graphene has a radial dimension of 5 to 40cm and a transverse dimension of 5 to 20 cm.
9. The method according to any one of claims 1 to 6, wherein the single crystal graphene prepared on any index plane has consistent orientation and can be spliced into a continuous film.
10. A high-quality ultra-large-sized single crystal graphene prepared by the method of any one of claims 1 to 9, wherein the prepared single crystal graphene has a radial dimension of 5-40 cm and a transverse dimension of 5-20 cm.
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| CN112301429A (en) * | 2020-10-10 | 2021-02-02 | 哈尔滨工业大学 | Tubular furnace refitting device and method for preparing single crystal metal foil and two-dimensional material |
| CN114447340A (en) * | 2020-11-06 | 2022-05-06 | 松山湖材料实验室 | Anti-cracking copper foil and battery |
| CN114717654A (en) * | 2022-04-06 | 2022-07-08 | 北京石墨烯研究院 | Method for controlling grain boundary angle of two-dimensional material and application thereof |
| WO2023083055A1 (en) * | 2021-11-09 | 2023-05-19 | 北京大学 | Method for infiltration growth of carbon film |
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