CN108754608A - A kind of ambrose alloy（111）The preparation method of alloy monocrystalline film and thus obtained ambrose alloy（111）Alloy monocrystalline film - Google Patents
A kind of ambrose alloy（111）The preparation method of alloy monocrystalline film and thus obtained ambrose alloy（111）Alloy monocrystalline film Download PDFInfo
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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Abstract
The present invention relates to a kind of ambrose alloys（111）The preparation method of alloy monocrystalline film, includes the following steps：S1 provides sapphire substrate；S2, in the crystal face Al of sapphire substrate2O3(0001) metallic film that 50-5000nm thickness is deposited on, obtaining deposition has the Sapphire Substrate of monel, wherein the metallic film is the alloy firm of the 1-40% that nickle atom accounts for total atom number being made of nickle atom and copper atom；Sapphire Substrate is put into chemical vapor deposition stove by S3, is made annealing treatment in the atmosphere of argon gas and hydrogen, obtains the monocrystal thin films of (111) crystal orientation.The invention further relates to a kind of ambrose alloy (111) alloy monocrystalline films obtained according to above-mentioned preparation method.Ambrose alloy (111) alloy monocrystalline film that preparation in accordance with the present invention obtains, greatlys improve the performance of graphene, lays the foundation for application of the next step graphene in field of microelectronics.
Description
Technical field
The present invention relates to alloy monocrystalline films, relate more specifically to a kind of preparation side of ambrose alloy (111) alloy monocrystalline film
Method and thus obtained ambrose alloy (111) alloy monocrystalline film.
Background technology
There are grapheme material excellent photoelectric properties, future to have in fields such as microelectronics, the energy, biological detections important
Application, cause the extensive concern of all circles.And the growth material of graphene is mainly metal copper foil material at present.Due to metallic copper
Foil rough surface, fluctuating is big, catalytic capability is weaker, so in the graphene poor quality that copper foil substrate surface is grown, sternly
Its following application in field of microelectronics of important place limitation.
Invention content
Graphene poor quality caused by growth material in order to solve the problems, such as above-mentioned graphene of the existing technology,
The present invention is intended to provide the preparation method and thus obtained ambrose alloy (111) alloy of a kind of ambrose alloy (111) alloy monocrystalline film
Monocrystal thin films.
The present invention provides a kind of preparation method of ambrose alloy (111) alloy monocrystalline film, includes the following steps：S1 provides indigo plant
Sapphire substrates；S2, in the crystal face Al of sapphire substrate2O3(0001) metallic film that 50-5000nm thickness is deposited on, is deposited
Have the Sapphire Substrate of monel, wherein the metallic film be the 1-40% that nickle atom accounts for total atom number by nickle atom and
The alloy firm of copper atom composition；Sapphire Substrate is put into chemical vapor deposition stove by S3, in the gas atmosphere of argon gas and hydrogen
It is made annealing treatment in enclosing, obtains the monocrystal thin films of (111) crystal orientation.
Sapphire substrate in preparation in accordance with the present invention can be carried out with the extension of the alloy atom of metallic film
Matching；Metallic film in preparation in accordance with the present invention is selected as specific ambrose alloy atomic ratio, it can be ensured that alloy is thin
The catalytic performance of film；Metallic film in preparation in accordance with the present invention is selected as specific thickness, it can be ensured that metal
The single crystallization for ensuring to realize alloy firm while breakage will not occur in annealing for film；Preparation side according to the present invention
Chemical vapor deposition in method is selected as specific atmosphere, it can be ensured that realize the single crystallization of alloy firm, particularly,
It can play and protect alloy firm not oxidized in annealing process and improve the kinetic energy of ambrose alloy atomic motion.
Wherein, Al2O3(0001) what is referred to is exactly the sapphire faces C, also referred to as sapphire (0001).Experiment shows Lan Bao
The faces R or the faces A of stone cannot achieve the single crystallization of alloy firm.
Wherein, the purity of the nickel in the metallic film and copper atom is 99.999%.That is, copper and mickel total atom number
Account for the 99.999% of metallic film total atom number.
The step S1 includes：Sapphire sheet is provided；Sapphire sheet is cleaned；And by the sapphire sheet after cleaning
It is put into Muffle furnace and carries out high annealing, to obtain sapphire substrate.Preferably, it is 2- which, which is catercorner length,
6 inches of sheet material.
The temperature of the high annealing carried out in Muffle furnace is 1100 DEG C.
The step S2 includes：While sapphire substrate is heated to 100 DEG C~900 DEG C with 0.1nm/min~
The rate of 100nm/min is deposited.Preferably, the mode heated to sapphire substrate is that radiant heating or resistance add
Heat.
The step S2 is specially：It is deposited by magnetron sputtering, thermal evaporation, electron beam evaporation or molecular beam epitaxy.
The step S2 is specially：Deposit ambrose alloy atom simultaneously；Or first deposit redeposited copper atom after nickle atom；Or
First redeposited nickle atom after deposition copper atom.
The annealing carried out in chemical vapor deposition stove includes holding stage, annealing stage and temperature-fall period.Preferably,
Holding stage can greatly improve film crystalline quality, and annealing stage can ensure to realize the single crystallization of film.
The temperature range of holding stage is 200 DEG C~600 DEG C, and soaking time is 10min~240min；The temperature of annealing stage
Ranging from 600 DEG C~1100 DEG C of degree, annealing time are 10min~240min.
It is 0.1 DEG C/min~50 DEG C/min by the heating rate of room temperature to holding stage；Annealing is warming up to by holding stage
The heating rate in stage is 0.1 DEG C/min~50 DEG C/min；By annealing stage be cooled to room temperature rate of temperature fall be 0.01 DEG C/
Min~100 DEG C/min.
Room temperature rises to the argon gas of holding stage and hydrogen ratio is (10~1000sccm)：(1~500sccm)；Holding stage
Argon gas and hydrogen ratio be (10~1000sccm)：(1~300sccm)；Holding stage is warming up to the argon gas and hydrogen of annealing stage
Gas ratio is (10~1000sccm)：(1~300sccm)；Argon gas and the hydrogen ratio of annealing stage are (10~1000sccm)：(1~
100sccm)；Argon gas and the hydrogen ratio of temperature-fall period are (10~1000sccm)：(1~50sccm).
The present invention also provides a kind of ambrose alloy (111) alloy monocrystalline films obtained according to above-mentioned preparation method.
Preparation in accordance with the present invention prepares ambrose alloy monocrystal thin films, the ambrose alloy of acquisition using the method for sapphire extension
(111) alloy monocrystalline film has atomic-level flatness (waviness be not higher than 0.5nm), to by the smooth substrate come
Ensure that the graphene of growth not will produce fold, so that it is guaranteed that the electricity magnetic performance and heat conductivility of graphene will not be due to pleats
The presence of wrinkle and reduce, improve graphene quality.In addition, ambrose alloy (111) alloy list that preparation in accordance with the present invention obtains
Brilliant film under lower temperature decomposes the organic gas such as methane, ethane, acetylene by the nickle atom in alloy to provide
Superelevation catalytic capability, to realize the high efficiency catalytic growth of graphene.Particularly, graphene is in preparation side according to the present invention
The growth on ambrose alloy (111) alloy monocrystalline film that method obtains can be carried out at 800 DEG C or less, less than the minimum growth temperature on copper
900 DEG C of degree.In short, ambrose alloy (111) alloy monocrystalline film that preparation in accordance with the present invention obtains, greatlys improve graphene
Performance, lay the foundation for application of the next step graphene in field of microelectronics.
Description of the drawings
Fig. 1 is the photo of ambrose alloy (111) alloy monocrystalline film that first embodiment according to the present invention obtains；
Fig. 2 is the scanning optical microphotograph of ambrose alloy (111) alloy monocrystalline film that first embodiment according to the present invention obtains
Mirror photo；
Fig. 3 is the scanning electron microscopy of ambrose alloy (111) alloy monocrystalline film that first embodiment according to the present invention obtains
Mirror photo；
Fig. 4 is the atomic force microscope of ambrose alloy (111) alloy monocrystalline film that first embodiment according to the present invention obtains
Photo；
Fig. 5 is that X-ray is spread out outside the face of ambrose alloy (111) alloy monocrystalline film that first embodiment according to the present invention obtains
Penetrate figure；
Fig. 6 is that the face internal X-ray of ambrose alloy (111) alloy monocrystalline film that first embodiment according to the present invention obtains spreads out
Penetrate figure；
Fig. 7 is the photo of ambrose alloy (111) the alloy monocrystalline film obtained according to the second embodiment of the present invention；
Fig. 8 is the photo of ambrose alloy (111) the alloy monocrystalline film according to the third embodiment of the invention obtained.
Specific implementation mode
Below in conjunction with the accompanying drawings, presently preferred embodiments of the present invention is provided, and is described in detail.
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
Step a：Select 2 inches of sapphire sheet.
Step b：Sapphire sheet is cleaned, ultrasound 30min in deionized water is put into, is purged with High Purity Nitrogen air gun dry
Only；It is put into ultrasound 30min in acetone soln, is purged with High Purity Nitrogen air gun clean.
Step c：Sapphire sheet is put into Muffle furnace and carries out high annealing, 1100 DEG C of annealing temperature is annealed 12 hours,
It is naturally cooling to room temperature, obtains sapphire substrate.
Step d：Using the method for magnetron sputtering, in the crystal face Al of sapphire substrate2O3(0001) 600nm thickness is deposited on
Metallic film, sapphire substrate are heated to 200 DEG C of temperature, sputter rate (deposition rate) 20nm/min, argon gas 0.5pa, work(
Rate 400w, obtaining deposition has the Sapphire Substrate (ambrose alloy/sapphire) of monel.
Step e：Ambrose alloy/sapphire is made annealing treatment.Sapphire Substrate is put into chemical vapor deposition stove and is carried out
Annealing.600 DEG C are risen to the heating rate of 10 DEG C/min, and the ratio of argon gas and hydrogen is 500sccm：40sccm；600
Keep the temperature 60min under the conditions of DEG C, the ratio of argon gas and hydrogen is 500sccm：20sccm；By 600 DEG C with 10 DEG C/min heating rates
Rise to 1000 DEG C, the ratio of argon gas and hydrogen is 500sccm：20sccm；It anneals under the conditions of 1000 DEG C 60min, argon gas and hydrogen
The ratio of gas is 500sccm：10sccm；With the near room temperature of the rate of temperature fall of 4 DEG C/min after annealing, the ratio of argon gas and hydrogen is
500sccm：5sccm obtains ambrose alloy (111) alloy monocrystalline film.
Pattern is characterized：
The pattern of ambrose alloy (111) alloy monocrystalline film of gained is characterized, wherein Fig. 1 is the ambrose alloy (111) of gained
The photo of alloy monocrystalline film；Fig. 2 is the scanning optical microscope photo of ambrose alloy (111) alloy monocrystalline film of gained, in figure
It can be seen that the surface of substrate is a wide range of interior very smooth；Fig. 3 is the scanning of ambrose alloy (111) alloy monocrystalline film of gained
Electron micrograph, in figure it can be seen that in the case of high magnification numbe, alloy firm surface is very smooth, does not find crystalline substance
Boundary；Fig. 4 is the atomic force microscopy of ambrose alloy (111) alloy monocrystalline film of gained, and it is flat to can see alloy substrate in figure
It is whole, surface undulation degree 0.5nm.
It follows that ambrose alloy (111) alloy monocrystalline film that preparation in accordance with the present invention obtains, flat with atom level
Whole degree, to ensure that the graphene of growth not will produce fold by the smooth substrate, so that it is guaranteed that the electricity of graphene
Performance will not be reduced due to the presence of fold, improve graphene quality.
It is characterized to monocrystalline：
Monocrystalline characterizing to ambrose alloy (111) alloy monocrystalline film of gained, wherein Fig. 5 is the ambrose alloy of gained
(111) X-ray diffractogram outside the face of alloy monocrystalline film, in figure it can be seen that the peak at 43.5 ° be ambrose alloy (111) alloy
It is orientated peak, shows that the alloy firm is (111) alignment films, wherein (111) face is the original in the six sides rice pile structure of nickel alloy
Son arranges most close face, and atomic arrangement lattice and the mismatch of graphene lattice are relatively low, being capable of epitaxial growth stone well
Black alkene；And its catalytic performance is all stronger than other faces；Fig. 6 is that the face internal X-ray of ambrose alloy (111) alloy monocrystalline film of gained spreads out
Figure is penetrated, three peaks that can see in figure are in mutually hexagonal angle, are three-fold symmetries, to illustrate that the alloy firm is monocrystalline nickel
The face of copper (111) film, film is (111) face.
Embodiment 2
Step a：Select 2 inches of sapphire sheet.
Step b：Sapphire sheet is cleaned, ultrasound 30min in deionized water is put into, is purged with High Purity Nitrogen air gun dry
Only；It is put into ultrasound 30min in acetone soln, is purged with High Purity Nitrogen air gun clean.
Step c：Sapphire sheet is put into Muffle furnace and carries out high annealing, 1100 DEG C of annealing temperature is annealed 12 hours,
It is naturally cooling to room temperature, obtains sapphire substrate.
Step d：Using the method for molecular beam epitaxy (MBE), deposited on the crystal face Al2O3 (0001) of sapphire substrate
The metallic film of 50nm thickness, the ratio that wherein nickle atom accounts for total atom number is 1%, and sapphire substrate is heated to 100 DEG C of temperature,
Sputter rate 0.1nm/min, obtaining deposition has the Sapphire Substrate (ambrose alloy/sapphire) of monel.
Step e：Ambrose alloy/sapphire is made annealing treatment.Sapphire Substrate is put into chemical vapor deposition stove and is carried out
Annealing.200 DEG C are risen to the heating rate of 0.1 DEG C/min, and the ratio of argon gas and hydrogen is 10sccm：1sccm；200
Keep the temperature 10min under the conditions of DEG C, the ratio of argon gas and hydrogen is 10sccm： 1sccm；By 200 DEG C with 0.1 DEG C/min heating rates
Rise to 600 DEG C, the ratio of argon gas and hydrogen is 10sccm：1sccm；Anneal 10min under the conditions of 600 DEG C, argon gas and hydrogen
Ratio is 500sccm：10sccm；With the near room temperature of the rate of temperature fall of 0.01 DEG C/min after annealing, the ratio of argon gas and hydrogen is
10sccm：50sccm obtains ambrose alloy (111) alloy monocrystalline film.
Fig. 7 is the photo of ambrose alloy (111) alloy monocrystalline film of gained, and the surface that substrate is can see in figure is very flat
It is whole.
Embodiment 3
Step a：Select 6 inches of sapphire sheet.
Step b：Sapphire sheet is cleaned, ultrasound 30min in deionized water is put into, is purged with High Purity Nitrogen air gun dry
Only；It is put into ultrasound 30min in acetone soln, is purged with High Purity Nitrogen air gun clean.
Step c：Sapphire sheet is put into Muffle furnace and carries out high annealing, 1100 DEG C of annealing temperature is annealed 12 hours,
It is naturally cooling to room temperature, obtains sapphire substrate.
Step d：Using the method for magnetron sputtering, in the crystal face Al of sapphire substrate2O3(0001) it is thick that 5000nm is deposited on
Metallic film, the ratio that wherein nickle atom accounts for total atom number is 40%, and sapphire substrate is heated to 900 DEG C of temperature, sputtering
Rate 100nm/min, argon gas 0.5pa, power 50w, obtaining deposition has the Sapphire Substrate (ambrose alloy/sapphire) of monel.
Step e：Ambrose alloy/sapphire is made annealing treatment.Sapphire Substrate is put into chemical vapor deposition stove and is carried out
Annealing.600 DEG C are risen to the heating rate of 50 DEG C/min, and the ratio of argon gas and hydrogen is 1000sccm：500sccm；?
Keep the temperature 240min under the conditions of 600 DEG C, the ratio of argon gas and hydrogen is 1000sccm：300sccm；By 600 DEG C with 50 DEG C/min liters
Warm rate rises to 1100 DEG C, and the ratio of argon gas and hydrogen is 1000sccm：300sccm；Anneal 240min under the conditions of 1100 DEG C,
The ratio of argon gas and hydrogen is 1000sccm：100sccm；With the near room temperature of the rate of temperature fall of 100 DEG C/min after annealing, argon gas and
The ratio of hydrogen is 1000sccm：50sccm obtains ambrose alloy (111) alloy monocrystalline film.
Fig. 8 is the photo of ambrose alloy (111) alloy monocrystalline film of gained, and the surface that substrate is can see in figure is very flat
It is whole.
Above-described, only presently preferred embodiments of the present invention is not limited to the scope of the present invention, of the invention is upper
Stating embodiment can also make a variety of changes.Made by i.e. every claims applied according to the present invention and description
Simply, equivalent changes and modifications fall within the claims of patent of the present invention.The not detailed description of the present invention is
Routine techniques content.
Claims (11)
1. a kind of preparation method of ambrose alloy (111) alloy monocrystalline film, which is characterized in that include the following steps：
S1 provides sapphire substrate；
S2, in the crystal face Al of sapphire substrate2O3(0001) metallic film that 50-5000nm thickness is deposited on, obtaining deposition has ambrose alloy
The Sapphire Substrate of alloy, wherein the metallic film is the 1-40% that nickle atom accounts for total atom number by nickle atom and copper atom
The alloy firm of composition；
Sapphire Substrate is put into chemical vapor deposition stove by S3, is made annealing treatment in the atmosphere of argon gas and hydrogen,
Obtain the monocrystal thin films of (111) crystal orientation.
2. preparation method according to claim 1, which is characterized in that the step S1 includes：Sapphire sheet is provided；To indigo plant
Jewel piece is cleaned；And the sapphire sheet after cleaning is put into Muffle furnace and carries out high annealing, to obtain sapphire
Substrate.
3. preparation method according to claim 2, which is characterized in that the temperature of the high annealing carried out in Muffle furnace is
1100℃。
4. preparation method according to claim 1, which is characterized in that the step S2 includes：Add by sapphire substrate
Heat is deposited to while 100 DEG C~900 DEG C with the rate of 0.1nm/min~100nm/min.
5. preparation method according to claim 4, which is characterized in that the step S2 is specially：Pass through magnetron sputtering, heat
Evaporation, electron beam evaporation or molecular beam epitaxy are deposited.
6. preparation method according to claim 4, which is characterized in that the step S2 is specially：Ambrose alloy original is deposited simultaneously
Son；Or first deposit redeposited copper atom after nickle atom；Or first deposit redeposited nickle atom after copper atom.
7. preparation method according to claim 1, which is characterized in that the annealing packet carried out in chemical vapor deposition stove
Include holding stage, annealing stage and temperature-fall period.
8. preparation method according to claim 7, which is characterized in that the temperature range of holding stage is 200 DEG C~600
DEG C, soaking time is 10min~240min；The temperature range of annealing stage is 600 DEG C~1100 DEG C, annealing time 10min
~240min.
9. preparation method according to claim 7, which is characterized in that by room temperature to holding stage heating rate be 0.1
DEG C/min~50 DEG C/min；The heating rate that annealing stage is warming up to by holding stage is 0.1 DEG C/min~50 DEG C/min；By moving back
The rate of temperature fall that the fiery stage is cooled to room temperature is 0.01 DEG C/min~100 DEG C/min.
10. preparation method according to claim 7, which is characterized in that room temperature rises to the argon gas and hydrogen ratio of holding stage
For (10~1000sccm)：(1~500sccm)；Argon gas and the hydrogen ratio of holding stage are (10~1000sccm)：(1~
300sccm)；Holding stage is warming up to the argon gas of annealing stage and hydrogen ratio is (10~1000sccm)：(1~300sccm)；It moves back
Argon gas and the hydrogen ratio in fiery stage are (10~1000sccm)：(1~100sccm)；Argon gas and the hydrogen ratio of temperature-fall period are (10
~1000sccm)：(1~50sccm).
11. ambrose alloy (111) alloy monocrystalline film that a kind of preparation method according to claim 1-10 obtains.
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| 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 |
| CN111188086A (en) * | 2020-02-27 | 2020-05-22 | 北京大学 | Preparation method of ultrahigh-conductivity multilayer single crystal laminated copper material and copper material |
| 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 |
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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***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***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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| CN114481101B (en) * | 2021-12-15 | 2023-09-29 | 中南大学 | Metal material obtained by method for regulating and controlling crystal face orientation of metal coating and application |
| CN116206948A (en) * | 2023-02-20 | 2023-06-02 | 湖北九峰山实验室 | Method for extending graphene on substrate and prepared graphene epitaxial wafer |
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