[go: up one dir, main page]

CN107354506B - A kind of method for preparing ultra-flat copper single crystal thin film - Google Patents

A kind of method for preparing ultra-flat copper single crystal thin film Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
copper
annealing
single crystal
temperature
sapphire
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710522321.1A
Other languages
Chinese (zh)
Other versions
CN107354506A (en
Inventor
彭海琳
邓兵
刘忠范
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Peking University
Original Assignee
Peking University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Peking University filed Critical Peking University
Priority to CN201710522321.1A priority Critical patent/CN107354506B/en
Publication of CN107354506A publication Critical patent/CN107354506A/en
Application granted granted Critical
Publication of CN107354506B publication Critical patent/CN107354506B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • 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
    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

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

A method of preparing super smooth copper single crystal film
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)

1.一种制备铜单晶薄膜的方法，包括如下步骤：1. a method for preparing a copper single crystal film, comprising the steps: 以蓝宝石单晶作为生长基底，磁控溅射铜靶，退火，所述退火步骤中，退火气氛为还原性气氛；所述退火步骤包括：先升温至进行一次保温后再升温至进行二次保温，再自然降温到室温；所述一次保温步骤中，一次保温的温度为400℃-600℃；由室温升至一次保温的温度的时间为20-60分钟；一次保温的时间为30-60分钟；所述二次保温步骤中，二次保温的温度为950℃-1050℃；由一次保温的温度升至二次保温的温度的时间为20-60分钟；二次保温的时间为30-60分钟；得到所述铜单晶薄膜；Using a sapphire single crystal as a growth substrate, magnetron sputtering a copper target, and annealing, in the annealing step, the annealing atmosphere is a reducing atmosphere; the annealing step includes: firstly heating up to perform a first thermal insulation, and then heating up to a secondary thermal insulation , and then naturally cool down to room temperature; in the first heat preservation step, the temperature of one heat preservation is 400°C-600°C; the time from room temperature to the temperature of one heat preservation is 20-60 minutes; the time of one heat preservation is 30-60 minutes; in the secondary insulation step, the temperature of the secondary insulation is 950 ℃-1050 ℃; the time from the temperature of the primary insulation to the temperature of the secondary insulation is 20-60 minutes; the time of the secondary insulation is 30- 60 minutes; obtaining the copper single crystal thin film; 所述方法还包括：在所述磁控溅射步骤之前，对蓝宝石进行退火；The method further includes: annealing the sapphire before the magnetron sputtering step; 所述对蓝宝石进行退火步骤中，退火气氛为氧气气氛或空气气氛；In the step of annealing the sapphire, the annealing atmosphere is an oxygen atmosphere or an air atmosphere; 退火温度为1000-1100℃；Annealing temperature is 1000-1100℃; 退火时间为4-12小时。Annealing time is 4-12 hours. 2.根据权利要求1所述的方法，其特征在于：所述磁控溅射步骤中，生长基底的溅射面为所述蓝宝石单晶的Al2O3(0001)面。2 . The method according to claim 1 , wherein in the magnetron sputtering step, the sputtering surface of the growth substrate is the Al 2 O 3 (0001) surface of the sapphire single crystal. 3 . 3.根据权利要求1或2所述的方法，其特征在于：所述磁控溅射步骤中，铜靶的纯度为99.999%；3. The method according to claim 1 or 2, characterized in that: in the magnetron sputtering step, the purity of the copper target is 99.999%; 溅射压强为4*10-4-10Pa；The sputtering pressure is 4*10 -4 -10Pa; 功率为300-600W。The power is 300-600W. 4.根据权利要求3所述的方法，其特征在于：所述功率为500W。4. The method according to claim 3, wherein the power is 500W. 5.根据权利要求1所述的方法，其特征在于：对磁控溅射制备的铜/蓝宝石的退火气氛为由氢气和氩气组成的混合气氛；5. method according to claim 1, is characterized in that: the annealing atmosphere to the copper/sapphire prepared by magnetron sputtering is the mixed atmosphere that is made up of hydrogen and argon; 所述由氢气和氩气组成的混合气氛中，氢气和氩气的流量比为10-50:500。In the mixed atmosphere composed of hydrogen and argon, the flow ratio of hydrogen and argon is 10-50:500. 6.根据权利要求5所述的方法，其特征在于：所述氢气的流量为10sccm；氩气的流量为500sccm。6 . The method according to claim 5 , wherein the flow rate of the hydrogen gas is 10 sccm; the flow rate of the argon gas is 500 sccm. 7 . 7.根据权利要求1所述的方法，其特征在于：对磁控溅射制备的铜/蓝宝石的退火是在常压化学气相沉积管式炉中进行。7. The method according to claim 1, wherein the annealing of the copper/sapphire prepared by magnetron sputtering is carried out in a normal pressure chemical vapor deposition tube furnace. 8.根据权利要求1所述的方法，其特征在于：所述一次保温的温度为500℃；由室温升至一次保温的温度的时间为30分钟；8. method according to claim 1, is characterized in that: the temperature of described one insulation is 500 ℃; The time that rises from room temperature to the temperature of one insulation is 30 minutes; 所述二次保温的温度为1000℃；由一次保温的温度升至二次保温的温度的时间为30分钟。The temperature of the second heat preservation is 1000°C; the time from the temperature of the first heat preservation to the temperature of the second heat preservation is 30 minutes. 9.权利要求1-8中任一所述方法制备得到的铜单晶薄膜。9. The copper single crystal thin film prepared by the method in any one of claims 1-8. 10.根据权利要求9所述的铜单晶薄膜，其特征在于：所述铜单晶薄膜的厚度为500-800nm。10 . The copper single crystal thin film according to claim 9 , wherein the thickness of the copper single crystal thin film is 500-800 nm. 11 .
CN201710522321.1A 2017-06-30 2017-06-30 A kind of method for preparing ultra-flat copper single crystal thin film Active CN107354506B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710522321.1A CN107354506B (en) 2017-06-30 2017-06-30 A kind of method for preparing ultra-flat copper single crystal thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710522321.1A CN107354506B (en) 2017-06-30 2017-06-30 A kind of method for preparing ultra-flat copper single crystal thin film

Publications (2)

Publication Number Publication Date
CN107354506A CN107354506A (en) 2017-11-17
CN107354506B true CN107354506B (en) 2019-06-18

Family

ID=60273343

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710522321.1A Active CN107354506B (en) 2017-06-30 2017-06-30 A kind of method for preparing ultra-flat copper single crystal thin film

Country Status (1)

Country Link
CN (1) CN107354506B (en)

Families Citing this family (19)

* Cited by examiner, † Cited by third party
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 single crystal film and preparation method thereof
CN110387575A (en) * 2018-04-17 2019-10-29 浙江大学 A method for the industrial production of surface monocrystalline copper substrates for the preparation of two-dimensional materials
CN108950684B (en) * 2018-06-08 2022-02-11 中国科学院物理研究所 A kind of method for 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
CN108878058B (en) * 2018-06-25 2019-11-22 湖北雄华科技有限公司 Three-layer transparent conductive film for dimming glass and preparation method thereof
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 A method for vertical heteroepitaxial single crystal metal thin film based on single crystal two-dimensional material/single crystal copper
TWI726777B (en) 2020-07-27 2021-05-01 國立陽明交通大學 Large grain quasi-single-crystal film and manufacturing method thereof
TWI743525B (en) 2019-07-30 2021-10-21 國立陽明交通大學 Quasi-single-crystal film and manufacturing method thereof
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
CN112837993B (en) * 2019-11-25 2025-03-04 中国科学院上海微系统与信息技术研究所 A nickel-copper (111) twin film with an in-plane angle of 60° and a preparation method thereof
CN111424309B (en) * 2020-05-15 2021-07-09 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
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 A method for preparing graphene single crystal wafer on copper-based textured film substrate
CN114836828B (en) * 2021-02-01 2023-08-29 北京石墨烯研究院 A kind of preparation method of large-domain graphene single crystal
CN115961258A (en) * 2021-10-12 2023-04-14 北京石墨烯研究院 Metal wafer and preparation method thereof
CN115961253A (en) * 2021-10-12 2023-04-14 北京石墨烯研究院 Metal substrate and method for producing the same
CN114411233B (en) * 2022-01-11 2023-05-26 大连理工大学 A method for rapidly preparing (100) single crystal copper
CN115595658B (en) * 2022-10-27 2024-07-02 松山湖材料实验室 Low transmission loss single crystal copper material and preparation method thereof, PCB board and preparation method thereof, and electronic component

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8697230B2 (en) * 2009-08-31 2014-04-15 Kyushu University Graphene sheet and method for producing the same
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

Also Published As

Publication number Publication date
CN107354506A (en) 2017-11-17

Similar Documents

Publication Publication Date Title
CN107354506B (en) A kind of method for preparing ultra-flat copper single crystal thin film
CN108950684B (en) A kind of method for preparing single crystal metal foil
CN108447773A (en) Graphene single crystal film and preparation method thereof
CN107190315A (en) A kind of method for preparing super smooth corrugationless graphene monocrystalline
CN106868469B (en) A kind of method for preparing graphene without metal catalyst on silicon base
CN106835260A (en) The preparation method of oversize multilayer single crystal graphene and large size single crystal corronil
CN112831768B (en) Preparation method and application of hafnium nitride film with high crystallization quality
CN110273176B (en) Method for preparing large-area copper Cu (111) single crystal
CN101230454A (en) A kind of preparation method of cubic boron nitride film
CN111826714B (en) Method for enhancing CVD diamond heteroepitaxial nucleation by applying bias voltage based on radio frequency power supply
CN101740358A (en) Method for preparing P type poly-silicon thin film on glass substrate
CN101665905A (en) Aluminum-induced low temperature preparation method of large grain size polysilicon film
CN110896024B (en) Silicon carbide epitaxial gallium oxide film method and silicon carbide epitaxial gallium oxide film structure
CN116575121B (en) Monocrystalline Cr with high orientation 2 AlC material and preparation method thereof
CN114717654B (en) Method for controlling grain boundary angle of two-dimensional material and application thereof
CN110067027B (en) Method for improving yield of bulk hexagonal phase boron nitride single crystal
CN108149198A (en) A kind of WC hard alloy film and its gradient layer technology room temperature preparation method
CN101235539A (en) Epitaxy growing method for La1-xCaxMnO3 single crystal thin film
CN112831766B (en) Method for preparing zirconium metal film on silicon substrate by utilizing magnetron sputtering and application
CN113584446A (en) Metal hafnium film prepared on silicon substrate by utilizing magnetron sputtering, method and application
CN101250705B (en) Method for manufacturing nickel-cuprum metallic baseband layer of highly oriented double-shaft texture
CN112299399B (en) Multilayer graphene and growth method thereof
CN114717657B (en) Method for growing nickel oxide monocrystal film based on plasma-assisted laser molecular beam epitaxy
CN110724922A (en) A kind of epitaxial AZO thin film with controllable crystal orientation and polarity on flexible substrate and preparation method thereof
CN107059119B (en) Method for preparing polycrystalline SiC film through sapphire substrate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant