CN107354506A - A kind of method for preparing super smooth copper single crystal film - Google Patents
A kind of method for preparing super smooth copper single crystal film Download PDFInfo
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- CN107354506A CN107354506A CN201710522321.1A CN201710522321A CN107354506A CN 107354506 A CN107354506 A CN 107354506A CN 201710522321 A CN201710522321 A CN 201710522321A CN 107354506 A CN107354506 A CN 107354506A
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—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
- 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
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Abstract
The invention discloses a kind of method for preparing super smooth copper single crystal film.The method provided by the invention for preparing copper single crystal film, comprises the following steps：Using sapphire single-crystal as growth substrate, magnetron sputtering copper target, annealing, the copper single crystal film is obtained.The present invention uses epitaxial growth substrate of the sapphire as copper, using the method for magnetron sputtering, it deposited in c surface sapphire substrate surfaces and be orientated consistent Copper thin film, and in subsequent annealing process, it is orientated consistent copper curing and grows up into consistent single crystal Cu (111) film without twin in face of orientation.Single crystal Cu (111) film that this method is prepared, surface and its smooth, controlled diameter, repeatability is high, has very extensive application prospect in fields such as communication, electronics, graphene preparations.
Description
Technical field
The present invention relates to a kind of method for preparing super smooth copper single crystal film.
Background technology
In general, monocrystalline has the performances such as the electricity more excellent than polycrystalline, machinery, it is one very heavy to prepare monocrystal thin films
The material science research field wanted.Single crystal Cu has excellent because eliminating as the crystal boundary in resistance generating source and signal attenuation source
Combination property：Remarkable electricity and signal transmission performance, good plastic deformation ability；Excellent corrosion resistance；Significantly
Anti-fatigue performance；Reduce segregation, stomata, shrinkage cavity, the pressure casting flaw such as miscellaneous；Bright surface quality；Thus it is mainly used in
The fields such as national defence high-tech, civil electronic, communication and network.Copper thin film is a kind of widely used metallic film, in electronics
There is very extensive application in the fields such as interconnection, printed circuit board (PCB).Particularly in recent years, it has been found that growth base is used as using copper metal
Bottom being capable of the excellent graphene film of processability, especially copper (111) single crystal substrates, it is considered to be realizes high-quality graphene
The very excellent substrate of growth.
The preparation method of copper single crystal is mainly two methods at present：Czochralski method, hot-mold continuous cast method.Both approaches are all systems
The method of standby copper single crystal body material.The single crystal casting length of these methods production is limited by device and crucible size, can only
The limited bar of growth diameter, and be difficult to prepare large-sized film, seriously limit the application of Copper thin film.In addition, these sides
Bar prepared by method is in the field that some film applications use, it is necessary to extra cutting, and cutting may produce to copper single crystal
Certain damage.And these square law devices are expensive, therefore have not been able to realization and be widely applied.Therefore, development is a kind of cheap, big
The copper single crystal method for manufacturing thin film of area, for its electricity, anti-rotten, machinery, graphene prepare etc. field have it is of crucial importance
Meaning.
The content of the invention
It is an object of the invention to provide a kind of method for preparing super smooth copper single crystal film.
The method provided by the invention for preparing copper single crystal film, comprises the following steps：
Using sapphire single-crystal as growth substrate, magnetron sputtering copper target, annealing, the copper single crystal film is obtained.
In the above method, sapphire single-crystal used is the conventional sapphire single crystal substrate as GaN epitaxy, is purchased from river
Cloudy farsighted rich electronics new material Co., Ltd；Sapphire single-crystal is c faces (0001)；The thickness of sapphire single-crystal is unlimited, is usually
0.5mm or 0.65mm；Size is usually 2 inches or 4 inches.
Methods described also comprises the following steps：Before the magnetron sputtering step, growth substrate is cleaned.Cleaning
Purpose be the surface state for improving sapphire single-crystal, remove the defects of being produced in cutting process, fracture or impurity, cleaning
Condition be usually：Phosphoric acid：Sulfuric acid=3.1 (v/v), temperature：300 DEG C, scavenging period：1h；Then rinse in deionized water
For several times, finally dried up with nitrogen gun.
In the magnetron sputtering step, the sputter face of growth substrate is the sapphire Al2O3(0001) face, namely c
Face.
In the magnetron sputtering step, the purity of copper target is 99.999%；
Sputtering pressure is 4*10-4- 10Pa, concretely 4*10-4Pa；
Power is 300-600W, concretely 500W；
In the annealing steps, annealing atmosphere is reducing atmosphere, the mixed atmosphere being specially made up of hydrogen and argon gas；
In the mixed atmosphere being made up of hydrogen and argon gas, the flow-rate ratio of hydrogen and argon gas is 10-50:500；The hydrogen
The flow of gas is specially 10sccm；The flow of argon gas is specially 500sccm.
The annealing steps include：First it is warming up to be warming up to again after progress is once incubated and carries out secondary insulation, then drops naturally
Temperature arrives room temperature.
In incubation step, the temperature being once incubated is 400 DEG C -600 DEG C, concretely 500 DEG C；By room temperature liter
Time to the temperature being once incubated is 20-60 minutes, specially 30 minutes；The time being once incubated is 30-60 minutes, specifically
For 30 minutes；
In the secondary incubation step, the temperature of secondary insulation is 950 DEG C -1050 DEG C, concretely 1000 DEG C；By once
The time that the temperature of insulation rises to the temperature of secondary insulation is 20-60 minutes, specially 30 minutes；The time of secondary insulation is
30-60 minutes, specially 30 minutes；
The annealing is carried out in aumospheric pressure cvd tube furnace.
Methods described also includes：Before the magnetron sputtering step, sapphire is annealed.The purpose of high annealing
In the stress in sapphire process is discharged, and improve sapphire crystallinity.It is described that annealing step is carried out to sapphire
In rapid, annealing atmosphere is oxygen atmosphere or air atmosphere；
Annealing temperature is 1000-1100 DEG C；
Annealing time is 4-12 hours.
In addition, the copper single crystal film being prepared according to the method described above, falls within protection scope of the present invention.The copper list
Brilliant film is copper (111) monocrystal thin films.The thickness of the copper single crystal film is 500-800nm.
The present invention uses epitaxial growth substrate of the sapphire as copper, using the method for magnetron sputtering, in c surface sapphire bases
Basal surface, which deposited, is orientated consistent Copper thin film, and in subsequent annealing process, is orientated consistent copper curing and grows up into
Consistent single crystal Cu (111) film without twin in face of orientation.Single crystal Cu (111) film that this method is prepared, surface
And its smooth, controlled diameter, repeatability is high, before having very extensive application in fields such as communication, electronics, graphene preparations
Scape.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of present invention process；
Fig. 2 is the sapphire photo that the present invention is used to prepare；
Fig. 3 is the sapphire X-ray diffractogram that the present invention is used to prepare；
Fig. 4 is the photo of sapphire surface magnetron sputtering copper；
Fig. 5 is the atomic force microscopy of sapphire surface magnetron sputtering copper；
Fig. 6 is the X-ray diffractogram of sapphire surface magnetron sputtering copper after annealing；
In high-resolution X-ray diffraction faces of the Fig. 7 for sapphire surface magnetron sputtering copper after annealingScanning figure；
Fig. 8 is the electron micrograph of sapphire surface magnetron sputtering copper after annealing；
Fig. 9 is the atomic force microscopy of sapphire surface magnetron sputtering copper after annealing；
Figure 10 is as a comparison without in the high-resolution X-ray diffraction face after the sapphire sputtering copper by annealingScanning figure；
Figure 11 is as a comparison without the electron micrograph after the sapphire sputtering copper by annealing；
Figure 12 is as a comparison without the atomic force microscopy after the sapphire sputtering copper by annealing；
Embodiment
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.
Experimental method described in following embodiments, it is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1, magnetron sputtering prepare 4 inches of copper single crystals
Integrated artistic flow is as shown in Figure 1.
Step (1)：Using sapphire single-crystal, purchase from the farsighted rich electronics new material Co., Ltd in Jiangyin；Sapphire single-crystal is c
Face (0001)；The thickness of sapphire single-crystal is unlimited, usually 0.65mm, and size is 4 inches.Its photo is as shown in Figure 2.
Step (2)：Cleaning to improve sapphire surface state, remove the defects of being produced in cutting process, fracture or
Impurity, the condition of cleaning are：Phosphoric acid：Sulfuric acid=3.1 (v/v), temperature：300 DEG C, scavenging period：1h；Then in deionized water
Rinse for several times, finally dried up with nitrogen gun.Sapphire X-ray diffractogram after cleaning is as shown in Figure 3, it is seen that only Al2O3
(0006) peak, sapphire used in explanation are monocrystalline.
Step (3)：Stress in high annealing release sapphire process, and improve sapphire crystallinity.Make
Annealing conditions are：Oxygen atmosphere, 1100 DEG C, 4 hours.
Step (4)：Using the method sputtering plating Copper thin film of magnetron sputtering：Using high-purity copper target material (99.999%), Gao Zhen
Sky sputtering, the condition of magnetron sputtering are：Sputtering pressure 4*10-4Pa, power 500W.The sputter face of growth substrate is sapphire list
Brilliant Al2O3(0001) face.The copper on 4 inches sapphire surfaces after sputtering is as shown in Figure 4.The thickness of Copper thin film is 500nm.
The state on its surface is characterized as shown in Figure 5 with AFM, it is seen that the copper surface very out-of-flatness after firm magnetron sputtering.
Step (5)：Copper/sapphire the annealing prepared to magnetron sputtering, way are：Aumospheric pressure cvd tubular type
Stove, hydrogen and argon gas mixed-gas atmosphere (500sccm Ar, 10sccm H2), carry out one to 500 DEG C by room temperature within 30 minutes
Secondary insulation 30 minutes；Then after being warming up to the secondary insulation of 1000 DEG C of progress 30 minutes by 500 DEG C in 30 minutes, then Temperature fall arrives
Room temperature.Copper after annealing is characterized using X-ray diffraction, scanning is as shown in Figure 6 outside its face, it is seen that copper takes outside face for 111
To.Copper after annealing is characterized using high-resolution X-ray diffraction, scanning is as shown in Figure 7 in its face, it is seen that copper only has in face
Three peaks occur, and this explanation copper is well without twin monocrystalline.Copper after annealing is characterized using electron microscope, such as Fig. 8
It is shown, it is seen that copper surface becomes very smooth after annealing.Copper after annealing is characterized using AFM, such as Fig. 9
It is shown, it is seen that copper surface becomes very smooth after annealing.
Embodiment 2, magnetron sputtering prepare the copper single crystal that twin be present
1) step is the same as the step 1) of embodiment 1；
2) step is the same as the step 2) of embodiment 1；
3) step：Sapphire single-crystal is not made annealing treatment
4) step is the same as the step 4) of embodiment 1；
5) step is the same as the step 5) of embodiment 1；Copper after stepping back is characterized using high-resolution X-ray diffraction, swept in its face
Retouch as shown in Figure 10, it is seen that copper there are 6 peaks to occur in face, and this explanation copper is the monocrystalline for existing twin.To the copper after annealing
Characterized using electron microscope, as shown in figure 11, it is seen that copper surface becomes very smooth after annealing, but twin boundary be present.
Copper after annealing being characterized using AFM, as shown in figure 12, it is seen that copper surface becomes very smooth after annealing,
But there is also some twin boundaries simultaneously.
Claims (10)
1. a kind of method for preparing copper single crystal film, comprises the following steps：
Using sapphire single-crystal as growth substrate, magnetron sputtering copper target, annealing, the copper single crystal film is obtained.
2. according to the method for claim 1, it is characterised in that：In the magnetron sputtering step, the sputter face of growth substrate
For the Al of the sapphire single-crystal2O3(0001) face.
3. method according to claim 1 or 2, it is characterised in that：In the magnetron sputtering step, the purity of copper target is
99.999%；
Sputtering pressure is 4*10-4-10Pa；
Power is 300-600W or 500W.
4. according to any described method in claim 1-3, it is characterised in that：In the annealing steps, annealing atmosphere is also
Originality atmosphere；The mixed atmosphere being specially made up of hydrogen and argon gas；
In the mixed atmosphere being made up of hydrogen and argon gas, the flow-rate ratio of hydrogen and argon gas is 10-50:500；The hydrogen
Flow is specially 10sccm；The flow of argon gas is specially 500sccm.
5. according to any described method in claim 1-4, it is characterised in that：The annealing steps include：First be warming up into
Row is warming up to again after being once incubated carries out secondary insulation, then Temperature fall is to room temperature.
6. according to the method for claim 5, it is characterised in that：In incubation step, the temperature being once incubated is
400 DEG C -600 DEG C or 500 DEG C；The time that the temperature being once incubated is risen to by room temperature is 20-60 minutes or 30 minutes；Once it is incubated
Time be 30-60 minutes；
In the secondary incubation step, the temperature of secondary insulation is 950 DEG C -1050 DEG C or 1000 DEG C；By the temperature being once incubated
The time for rising to the temperature of secondary insulation is 20-60 minutes or 30 minutes；The time of secondary insulation is 30-60 minutes；
The annealing is carried out in aumospheric pressure cvd tube furnace.
7. according to any described method in claim 1-6, it is characterised in that：Methods described also includes：Splashed in the magnetic control
Penetrate before step, sapphire is annealed.
8. according to the method for claim 7, it is characterised in that：It is described that sapphire is carried out in annealing steps, annealing atmosphere
For oxygen atmosphere or air atmosphere；
Annealing temperature is 1000-1100 DEG C；
Annealing time is 4-12 hours.
9. the copper single crystal film that any methods described is prepared in claim 1-8.
10. copper single crystal film according to claim 9, it is characterised in that：The thickness of the copper single crystal film is 500-
800nm。
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108447773A (en) * | 2018-03-26 | 2018-08-24 | 北京石墨烯研究院 | Graphene monocrystal thin films and preparation method thereof |
| CN108754608A (en) * | 2018-06-22 | 2018-11-06 | 中国科学院上海微系统与信息技术研究所 | A kind of ambrose alloy（111）The preparation method of alloy monocrystalline film and thus obtained ambrose alloy（111）Alloy monocrystalline film |
| CN108878058A (en) * | 2018-06-25 | 2018-11-23 | 湖北雄华科技有限公司 | Three-decker transparent conductive film and preparation method thereof for dimming glass |
| CN108950684A (en) * | 2018-06-08 | 2018-12-07 | 中国科学院物理研究所 | A method of preparing single-crystal metal foil |
| CN110387575A (en) * | 2018-04-17 | 2019-10-29 | 浙江大学 | A method of to prepare the copper-based bottom of two-dimensional material industrialized production surface single crystalization |
| CN110616454A (en) * | 2019-03-07 | 2019-12-27 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on monocrystal two-dimensional material/monocrystal copper |
| WO2020053102A1 (en) | 2018-09-10 | 2020-03-19 | Centre National De La Recherche Scientifique | Process for preparing single-crystal thin films |
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| CN111621845A (en) * | 2020-05-26 | 2020-09-04 | 中国人民解放军国防科技大学 | Preparation method of inch-grade single crystal film and single crystal film |
| CN111705359A (en) * | 2020-06-30 | 2020-09-25 | 中国科学院上海微系统与信息技术研究所 | Method for preparing graphene single crystal wafer on copper-based textured film substrate |
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| CN115595658A (en) * | 2022-10-27 | 2023-01-13 | 松山湖材料实验室（Cn） | Low-transmission-loss single crystal copper material and preparation method thereof, PCB (printed circuit board) and preparation method thereof, and electronic component |
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| CN108950684B (en) * | 2018-06-08 | 2022-02-11 | 中国科学院物理研究所 | Method for preparing single crystal metal foil |
| CN108950684A (en) * | 2018-06-08 | 2018-12-07 | 中国科学院物理研究所 | A method of preparing single-crystal metal foil |
| CN108754608A (en) * | 2018-06-22 | 2018-11-06 | 中国科学院上海微系统与信息技术研究所 | A kind of ambrose alloy（111）The preparation method of alloy monocrystalline film and thus obtained ambrose alloy（111）Alloy monocrystalline film |
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| CN108878058B (en) * | 2018-06-25 | 2019-11-22 | 湖北雄华科技有限公司 | Three-decker transparent conductive film and preparation method thereof for dimming glass |
| WO2020053102A1 (en) | 2018-09-10 | 2020-03-19 | Centre National De La Recherche Scientifique | Process for preparing single-crystal thin films |
| CN110616454A (en) * | 2019-03-07 | 2019-12-27 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on monocrystal two-dimensional material/monocrystal copper |
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| CN112095151B (en) * | 2019-07-30 | 2021-09-03 | 财团法人交大思源基金会 | Large-grain quasi-single crystal film and preparation method thereof |
| CN111424309A (en) * | 2020-05-15 | 2020-07-17 | 中国科学院重庆绿色智能技术研究院 | Single crystal metal foil and preparation method thereof |
| CN111621845A (en) * | 2020-05-26 | 2020-09-04 | 中国人民解放军国防科技大学 | Preparation method of inch-grade single crystal film and single crystal film |
| CN111705359A (en) * | 2020-06-30 | 2020-09-25 | 中国科学院上海微系统与信息技术研究所 | Method for preparing graphene single crystal wafer on copper-based textured film substrate |
| CN111705359B (en) * | 2020-06-30 | 2022-07-05 | 中国科学院上海微系统与信息技术研究所 | Method for preparing graphene single crystal wafer on copper-based textured film substrate |
| US11466385B2 (en) | 2020-07-27 | 2022-10-11 | National Yang Ming Chiao Tung University | Large grain quasi-single-crystal film and manufacturing method thereof |
| CN114836828A (en) * | 2021-02-01 | 2022-08-02 | 北京石墨烯研究院 | Preparation method of large domain graphene single crystal |
| CN114836828B (en) * | 2021-02-01 | 2023-08-29 | 北京石墨烯研究院 | Preparation method of large domain graphene single crystal |
| CN114411233A (en) * | 2022-01-11 | 2022-04-29 | 大连理工大学 | Method for rapidly preparing (100) single crystal copper |
| CN115595658A (en) * | 2022-10-27 | 2023-01-13 | 松山湖材料实验室（Cn） | Low-transmission-loss single crystal copper material and preparation method thereof, PCB (printed circuit board) and preparation method thereof, and electronic component |
| CN115595658B (en) * | 2022-10-27 | 2024-07-02 | 松山湖材料实验室 | Low-transmission-loss monocrystalline copper material and preparation method thereof, PCB and preparation method thereof, and electronic component |
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