CN107354506B - A method of preparing super smooth copper single crystal film - Google Patents
A method of preparing super smooth copper single crystal film Download PDFInfo
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- CN107354506B CN107354506B CN201710522321.1A CN201710522321A CN107354506B CN 107354506 B CN107354506 B CN 107354506B CN 201710522321 A CN201710522321 A CN 201710522321A CN 107354506 B CN107354506 B CN 107354506B
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- 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 methods for preparing super smooth copper single crystal film.The method provided by the invention for preparing copper single crystal film includes the following steps: using sapphire single-crystal as growth substrate, magnetron sputtering copper target, anneals, obtains the copper single crystal film.The present invention uses epitaxial growth substrate of the sapphire as copper, using the method for magnetron sputtering, it deposited the consistent Copper thin film of orientation in c surface sapphire substrate surface, and in subsequent annealing process, it is orientated consistent copper curing and grows up into single crystal Cu (111) film for being orientated twin in consistent no face.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 methods for preparing super smooth copper single crystal film.
Background technique
In general, monocrystalline has the performances such as electricity, the machinery more excellent than polycrystalline, preparing monocrystal thin films is one very heavy
The material science research field wanted.Single crystal Cu has excellent because eliminating the crystal boundary as resistance generating source and signal decaying source
Comprehensive performance: brilliant electricity and signal transmission performance, good plastic deformation ability；Excellent corrosion resistance；Significantly
Anti-fatigue performance；Reduce segregation, stomata, shrinkage cavity, press the casting flaws such as miscellaneous；Bright surface quality；Thus it is mainly used for
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.Especially in recent years, it has been found that using copper metal as growth base
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 methods is all system
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
The bar of method preparation needs additional cutting in the field that certain film applications use, and copper single crystal may be generated by cutting
Certain damage.And these square law devices are expensive, therefore have not been able to realize and be widely applied.Therefore, develop a kind of cheap, big
The copper single crystal method for manufacturing thin film of area has in fields such as electricity, anti-rotten, mechanical, graphene preparations it of crucial importance
Meaning.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing super smooth copper single crystal film.
The method provided by the invention for preparing copper single crystal film, includes the following steps:
Using sapphire single-crystal as growth substrate, magnetron sputtering copper target, annealing obtains the copper single crystal film.
In the above method, sapphire single-crystal used is the common sapphire single crystal substrate as GaN epitaxy, is purchased from river
The farsighted rich electronics new material Co., Ltd of yin；Sapphire single-crystal is the face c (0001)；The thickness of sapphire single-crystal is unlimited, usually
0.5mm or 0.65mm；Size is usually 2 inches or 4 inches.
The method also includes following steps: before the magnetron sputtering step, cleaning to growth substrate.Cleaning
Purpose be to improve the surface state of sapphire single-crystal, remove the defect, fracture or the impurity that generate in cutting process, cleaning
Condition it is usual are as follows: phosphoric acid: sulfuric acid=3.1 (v/v), temperature: 300 DEG C, scavenging period: 1h；Then it rinses in deionized water
For several times, it is 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 of hydrogen and argon gas；
In the mixed atmosphere being made 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 to be warming up to be warming up to again after progress is once kept the temperature to carry out secondary heat preservation, then drop naturally
Temperature arrives room temperature.
In incubation step, the temperature once kept the temperature is 400 DEG C -600 DEG C, concretely 500 DEG C；By room temperature liter
Time to the temperature once kept the temperature is 20-60 minutes, specially 30 minutes；The time once kept the temperature is 30-60 minutes, specifically
It is 30 minutes；
In the secondary incubation step, the temperature of secondary heat preservation is 950 DEG C -1050 DEG C, concretely 1000 DEG C；By primary
The time that the temperature of heat preservation rises to the temperature of secondary heat preservation is 20-60 minutes, specially 30 minutes；The time of secondary heat preservation is
30-60 minutes, specially 30 minutes；
The annealing carries out in aumospheric pressure cvd tube furnace.
The method also includes: before the magnetron sputtering step, anneal to sapphire.The purpose of high annealing
It is to discharge the stress in sapphire process, and improves 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, also belongs to protection scope of the present invention.The copper list
Brilliant film is copper (111) monocrystal thin films.The copper single crystal film with a thickness of 500-800nm.
The present invention uses epitaxial growth substrate of the sapphire as copper, using the method for magnetron sputtering, in c surface sapphire base
Bottom surface deposited the consistent Copper thin film of orientation, and in subsequent annealing process, is orientated consistent copper curing and grows up into
It is orientated single crystal Cu (111) film of twin in consistent no face.Single crystal Cu (111) film that this method is prepared, surface
And its smooth, controlled diameter, repeatability is high, before the fields such as communication, electronics, graphene preparation have very extensive application
Scape.
Detailed description of the invention
Fig. 1 is the flow diagram 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；
Fig. 7 be annealing after sapphire surface magnetron sputtering copper high-resolution X-ray diffraction face inScanning 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；
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1, magnetron sputtering prepare 4 inches of copper single crystals
Integrated artistic process is as shown in Figure 1.
Step (1): using sapphire single-crystal, purchases 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, having a size of 4 inches.Its photo is as shown in Figure 2.
Step (2): cleaning to improve sapphire surface state, remove the defect generated in cutting process, fracture or
Impurity, the condition of cleaning are as follows: phosphoric acid: sulfuric acid=3.1 (v/v), and temperature: 300 DEG C, scavenging period: 1h；Then in deionized water
It rinses for several times, is 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 illustrates that sapphire used is monocrystalline.
Step (3): high annealing discharges the stress in sapphire process, and improves sapphire crystallinity.Make
Annealing conditions are as follows: 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 as follows: 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.Copper thin film with a thickness of 500nm.
The state on its surface atomic force microscope characterizes as shown in Figure 5, it is seen that the copper surface very out-of-flatness after rigid magnetron sputtering.
Step (5): copper/sapphire annealing to magnetron sputtering preparation, way are as follows: aumospheric pressure cvd tubular type
Furnace, hydrogen and argon gas mixed-gas atmosphere (500sccm Ar, 10sccm H2), one is carried out to 500 DEG C by room temperature within 30 minutes
Secondary heat preservation 30 minutes；Then after being warming up to the secondary heat preservation 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, is scanned outside face as shown in Figure 6, it is seen that copper is 111 to take outside face
To.Copper after annealing is characterized using high-resolution X-ray diffraction, scanning is as shown in Figure 7 in face, it is seen that copper only has in face
Three peaks occur, this illustrates that 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 atomic force microscope, such as Fig. 9
It is shown, it is seen that copper surface becomes very smooth after annealing.
Embodiment 2, there are the copper single crystals of twin for magnetron sputtering preparation
1) step is the same as 1 step 1) of embodiment；
2) step is the same as 1 step 2) of embodiment；
3) step: sapphire single-crystal is not made annealing treatment
4) step is the same as 1 step 4) of embodiment；
5) step is the same as 1 step 5) of embodiment；Copper after stepping back is characterized using high-resolution X-ray diffraction, is swept in face
It retouches as shown in Figure 10, it is seen that copper has 6 peaks to occur in face, this illustrates that copper is the monocrystalline there are twin.To the copper after annealing
It is characterized using electron microscope, as shown in figure 11, it is seen that copper surface becomes very smooth after annealing, but there are twin boundaries.
Copper after annealing being characterized using atomic force microscope, 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, includes the following steps:
Using sapphire single-crystal as growth substrate, magnetron sputtering copper target is annealed, and in the annealing steps, annealing atmosphere is reduction
Property atmosphere；The annealing steps include: first to be warming up to be warming up to again after progress is once kept the temperature to carry out secondary heat preservation, then Temperature fall
To room temperature；In incubation step, the temperature once kept the temperature is 400 DEG C -600 DEG C；The temperature once kept the temperature is risen to by room temperature
The time of degree is 20-60 minutes；The time once kept the temperature is 30-60 minutes；In the secondary incubation step, the temperature of secondary heat preservation
Degree is 950 DEG C -1050 DEG C；It is 20-60 minutes by the time that the temperature once kept the temperature rises to the temperature of secondary heat preservation；Secondary heat preservation
Time be 30-60 minutes；Obtain the copper single crystal film；
The method also includes: before the magnetron sputtering step, anneal to sapphire；
Described to carry out in annealing steps to sapphire, annealing atmosphere is oxygen atmosphere or air atmosphere；
Annealing temperature is 1000-1100 DEG C；
Annealing time is 4-12 hours.
2. according to the method described in claim 1, it is characterized by: 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.
4. according to the method described in claim 3, it is characterized by: the power is 500W.
5. according to the method described in claim 1, it is characterized by: the copper/sapphire annealing atmosphere prepared to magnetron sputtering
For the mixed atmosphere being made of hydrogen and argon gas；
In the mixed atmosphere being made of hydrogen and argon gas, the flow-rate ratio of hydrogen and argon gas is 10-50:500.
6. according to the method described in claim 5, it is characterized by: the flow of the hydrogen is 10sccm；The flow of argon gas is
500sccm。
7. according to the method described in claim 1, it is characterized by: to magnetron sputtering preparation copper/it is sapphire annealing be
It is carried out in aumospheric pressure cvd tube furnace.
8. according to the method described in claim 1, it is characterized by: the temperature once kept the temperature is 500 DEG C；It is risen to by room temperature
The time of the temperature once kept the temperature is 30 minutes；
The temperature of the secondary heat preservation is 1000 DEG C；It is 30 points by the time that the temperature once kept the temperature rises to the temperature of secondary heat preservation
Clock.
9. the copper single crystal film that any the method is prepared in claim 1-8.
10. copper single crystal film according to claim 9, it is characterised in that: the copper single crystal film with a thickness of 500-
800nm。
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| WO2020053102A1 (en) | 2018-09-10 | 2020-03-19 | Centre National De La Recherche Scientifique | Process for preparing single-crystal thin films |
| CN110616454B (en) * | 2019-03-07 | 2020-10-09 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on monocrystal two-dimensional material/monocrystal copper |
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| CN103378235B (en) * | 2012-04-25 | 2015-12-02 | 清华大学 | Light-emitting diode |
| CN104532206A (en) * | 2014-12-12 | 2015-04-22 | 中国科学院重庆绿色智能技术研究院 | Preparation method of graphene doped film growing on insulating substrate in in-situ growth mode |
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