CN107904654A - A kind of preparation method of large size single crystal copper foil - Google Patents
A kind of preparation method of large size single crystal copper foil Download PDFInfo
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- CN107904654A CN107904654A CN201710020397.4A CN201710020397A CN107904654A CN 107904654 A CN107904654 A CN 107904654A CN 201710020397 A CN201710020397 A CN 201710020397A CN 107904654 A CN107904654 A CN 107904654A
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- copper foil
- tip
- single crystal
- large size
- polycrystalline
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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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- 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
Abstract
The present invention provides a kind of preparation method of large size single crystal copper foil.The method is cut into tip for polycrystalline copper foil as raw material, one end, and large size single crystal copper foil is prepared using special annealing technique.Method proposed by the present invention, solves the problems, such as that monocrystalline copper foil is expensive, by very simple method, realizes the preparation of large size single crystal copper foil.
Description
Technical field
The present invention relates to a kind of preparation method of large size single crystal copper foil.
Background technology
Copper is the non-ferrous metal very close with human relation, since it has good electric conductivity, thermal conductivity, extension
Property, corrosion resistance, be widely used in electrically, light industry, machine-building, building industry, the field such as national defense industry, have in China
Aluminium is only second in the consumption of non-ferrous metal material.Copper is a kind of red metal, while is also a kind of green metal.Its fusing point is relatively low,
Easy re-melting, smelt again, thus recycles considerably cheap.
Compared with polycrystalline copper, single crystal Cu has lot of advantages：1, due to no crystal boundary, the electric conductivity of single crystal Cu can be more preferable.
2, due to no crystal boundary, the mechanical performance of single crystal Cu also can be more preferable, can prevent the fracture on crystal boundary in actual processing production.3,
Single crystal Cu is more anti-oxidant more resistant to corrosion.4, the pliability of monocrystalline copper foil, hardness are than polycrystalline copper higher.
Copper single crystal is extraordinary substrate material, and more and more important work is played in terms of Surface Science, film preparation
With particularly the growth of graphene is ripe all the more on copper in recent years, and monocrystalline copper foil has important work for the quality for improving graphene
With.Therefore, how to improve the size of monocrystalline copper foil is an important problem in science.Monocrystalline copper foil price currently on the market is held high
Expensive, size is smaller, is increasingly difficult to meet the needs of people are to monocrystalline copper foil, is badly in need of a kind of simple, material benefit preparation method.
The content of the invention
Present invention firstly provides a kind of preparation method of large size single crystal copper foil, it is characterised in that by the one of polycrystalline copper foil
End is formed as tip, and annealing is carried out to polycrystalline copper foil and obtains monocrystalline copper foil.The monocrystalline copper foil is Cu (111), Cu (100), Cu
(110), the monocrystalline copper foil of the various crystal faces such as Cu (410), Cu (311).
A kind of large size single crystal copper foil, the large size single crystal copper foil are the large scales as prepared by above-mentioned method
The lengthwise dimension of monocrystalline copper foil is 0.1~50m.
The present invention prepares large size single crystal copper by the use of business polycrystalline copper foil as raw material using special annealing process
Paper tinsel.Method proposed by the present invention, solves the problems, such as that monocrystalline copper foil price is prohibitively expensive, by very simple method, realizes
The preparation of the large-sized monocrystalline copper foil of high quality.
The advantage of the invention is that：
1. present invention firstly provides the method that copper foil one end is cut into spike anneal, the system of large size single crystal copper foil is realized
It is standby；
2. the present invention selects the commercial polycrystalline copper foil that can be bought as raw material, it is not necessary to complicated table is carried out to copper foil
Face pre-processes, it is possible to prepares large size single crystal copper foil, greatly reduces manufacturing cost；
3. the present invention can prepare the various crystal faces such as Cu (111), Cu (100), Cu (110), Cu (410), Cu (311)
Monocrystalline copper foil.
4. the method for the present invention is simple, effective, cost is low, contributes to the practical application of large size single crystal copper foil and industrial metaplasia
Production.
Brief description of the drawings
Fig. 1 (a) is the optical picture that polycrystalline copper foil one end is cut into tip；Fig. 1 (b) is obtained copper after polycrystalline copper foil annealing
X-ray diffraction (XRD) result of paper tinsel.
Fig. 2 is backscattered electron diffraction (EBSD) result of monocrystalline Cu (111) copper foil prepared.
Fig. 3 is the EBSD results of monocrystalline Cu (100) copper foil prepared.
Fig. 4 is the XRD results of the polycrystalline copper foil prepared.
Embodiment
The present invention is described in further details with reference to specific embodiment, the raw material can unless otherwise instructed
Obtained from open commercial sources.
Embodiment one：A kind of method that monocrystalline copper foil is prepared by annealing to polycrystalline copper, includes the following steps：
(1), described polycrystalline copper foil one end is cut into tip to be flat on high temperature-resistant liner bottom, connects transmission device, being put into
Learn in vapor deposition apparatus, be passed through inert gas, inert gas flow is 300~500sccm, is then started to warm up, described
Inert gas is N2Or Ar；
(2), when temperature rises to 800~1100 DEG C, polycrystalline copper foil gradually passes through chemical vapor deposition since tip and sets
It is standby, start annealing process；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal copper foil.
Wherein, the tip is that elongated or rectangular copper foil is removed any one angle therein, or at the same time
Remove two adjacent angles along copper foil width and formed.The shape at tip does not have special requirement, can form one
A angle is the tip of acute angle or shape is the tip at obtuse angle at an angle, can also be to form a trapezoidal shape
Shape.The typical sizes of copper foil are 5-10cm wide, 0.1-50m long；Correspondingly, the typical sizes at tip are 5-10cm wide, 5-
20cm long.
Wherein, transmission device can be the transmission device as stated clearly in Chinese patent application CN201610191702.1, i.e.,
Including multiple first runners for being separately positioned on chemical vapor depsotition equipment both ends and multiple second runners.
Above-mentioned polycrystalline copper foil one end is cut into tip, optical picture is as shown in Figure 1a.Copper foil after annealing carries out XRD characterization,
As a result as shown in Figure 1 b.From Fig. 1 b, obverse and reverse only one direction, that is, Cu (111) of the copper foil after annealing spread out
Peak is penetrated, shows that the copper foil after annealing has integrally formed perfect Cu (111) monocrystalline.Backscattered electron diffraction (EBSD) can
Further to prove it as Cu (111) monocrystalline.It can be seen from the above that to polycrystalline copper foil one end is cut into tip, since Cu (111) is from point
End starts selective recrystallization, progressively grows up, so that large scale Cu (111) monocrystalline copper foil be prepared.
Cu (111) the monocrystalline copper foil width being prepared by the above method is 1~20cm, length direction for 0.1~
50m。
Experiment one：Polycrystalline copper foil one end is cut into tip by one kind of this experiment, and continuous annealing prepares monocrystalline Cu's (111)
Method is to carry out according to the following steps：
(1), described polycrystalline copper foil one end is cut into tip to be flat on high temperature-resistant liner bottom, connects transmission device, being put into
Learn in vapor deposition apparatus, be passed through inert gas, inert gas flow 500sccm, operating pressure is 1 × 105Pa, Ran Houkai
Begin to heat up, temperature-rise period continues 60min, and the inert gas is Ar；
(2), when temperature rises to 1000 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment, polycrystalline since tip
The speed that copper foil continues through heating region is 0.5cm/min, starts annealing process, annealing time 30min；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal Cu (111).
Experiment two：Polycrystalline copper foil one end is cut into tip by one kind of this experiment, and continuous annealing prepares monocrystalline Cu's (111)
Method is to carry out according to the following steps：
(1), described polycrystalline copper foil one end is cut into tip to be flat on high temperature-resistant liner bottom, connects transmission device, being put into
Learn in vapor deposition apparatus, be passed through inert gas, inert gas flow 500sccm, operating pressure is 1 × 105Pa, Ran Houkai
Begin to heat up, temperature-rise period continues 60min, and the inert gas is Ar；
(2), when temperature rises to 1050 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment, polycrystalline since tip
The speed that copper foil continues through heating region is 0.5cm/min, starts annealing process, annealing time 30min；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal Cu (111).
Experiment three：Polycrystalline copper foil one end is cut into tip by one kind of this experiment, and continuous annealing prepares monocrystalline Cu's (111)
Method is to carry out according to the following steps：
(1), described polycrystalline copper foil one end is cut into tip to be flat on high temperature-resistant liner bottom, connects transmission device, being put into
Learn in vapor deposition apparatus, be passed through inert gas, inert gas flow 500sccm, operating pressure is 1 × 105Pa, Ran Houkai
Begin to heat up, temperature-rise period continues 60min, and the inert gas is Ar；
(2), when temperature rises to 1000 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment, polycrystalline since tip
The speed that copper foil continues through heating region is 0.2cm/min, starts annealing process, annealing time 30min；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal Cu (111).
Experiment four：Polycrystalline copper foil one end is cut into tip by one kind of this experiment, and continuous annealing prepares monocrystalline Cu's (100)
Method is to carry out according to the following steps：
(1), described polycrystalline copper foil one end is cut into tip to be flat on high temperature-resistant liner bottom, connects transmission device, being put into
Learn in vapor deposition apparatus, be passed through Ar and H2Gas, Ar flows are 500sccm, H2Flow is 50sccm, operating pressure for 1 ×
105Pa, then starts to warm up, and temperature-rise period continues 60min；
(2), when temperature rises to 1000 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment, polycrystalline since tip
The speed that copper foil continues through heating region is 0.5cm/min, starts annealing process, annealing time 30min；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal Cu (100).
The results are shown in Figure 3 by the EBSD for the monocrystalline Cu (100) that the method for above-mentioned experiment four is prepared, it can be seen that passes through
Different growth atmospheres are adjusted, the monocrystalline copper foil of various crystal faces can be prepared in this way.
It should be noted that the method for above-mentioned experiment one to experiment four uses identical transmission device.The tip is
Elongated or rectangular copper foil is removed into any one angle therein, or removes along copper foil width two at the same time
Adjacent angle and formed.The shape at tip does not have special requirement, can be the tip that shape is at an angle acute angle, can also
It is the tip that shape is at an angle obtuse angle, can also be to form a trapezoidal shape.The typical sizes of copper foil are 5-10cm
Width, 0.1-50m cm long；Correspondingly, the typical sizes at tip are 5-10cm wide, 5-20cm long.In addition, Cu (110), Cu
(410), the monocrystalline copper foil of the various crystal faces such as Cu (311) can use the method for above-mentioned similar step to be prepared, herein not
Repeat again.
Comparative example：Anneal to the polycrystalline copper foil that one end is not cut into tip, carry out according to the following steps：
(1), the polycrystalline copper foil that no one end is cut into tip is flat on high temperature-resistant liner bottom, is connected transmission device, is put into
In chemical vapor depsotition equipment, inert gas, inert gas flow 500sccm are passed through, operating pressure is 1 × 105Pa, then
Start to warm up, temperature-rise period continues 60min, and the inert gas is Ar；
(2), when temperature rises to 1000 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment, and polycrystalline copper foil continuously leads to
The speed for crossing heating region is 0.2cm/min, starts annealing process, annealing time 30min；
(3), after growing, it is cooled to room temperature, that is, the copper foil prepared.
XRD characterization is carried out to the copper foil after above-mentioned annealing, the results are shown in Figure 4.As shown in Figure 4, copper foil after annealing
Obverse and reverse includes the diffraction maximum of multiple copper crystal faces, shows copper single crystal particle therein there are multiple orientations and is orientated simultaneously
It is inconsistent.If annealed again it can be seen from the above that one end of copper foil is not cut into tip, copper foil can not recrystallize to form big ruler
Very little monocrystalline copper foil.
Claims (10)
1. a kind of preparation method of large size single crystal copper foil, it is characterised in that one end of polycrystalline copper foil is formed as into tip, to more
Brilliant copper foil carries out annealing and obtains monocrystalline copper foil.
2. according to the method described in claim 1, it is characterized in that, one end of polycrystalline copper foil is cut into tip, continue through plus
Thermal region.
3. according to the method described in claim 2, it is characterized in that, polycrystalline copper foil continues through heating region since tip
Speed is 0.01~10cm/min.
4. according to the method described in claim 1, it is characterized in that, the monocrystalline copper foil is Cu (111), Cu (100), Cu
(110), the monocrystalline copper foil of Cu (410) or Cu (311) crystal face.
5. according to the method described in claim 1, it is characterized in that, the tip is by elongated or rectangular polycrystalline copper
Paper tinsel removes any one angle therein, or removes two adjacent angles along copper foil width at the same time and formed.
6. according to the method described in claim 5, it is characterized in that, it is the tip of acute angle, one that the shape at tip, which is an angle,
Tip or a trapezoidal shape of a angle for obtuse angle；Preferably, tip is 5-10cm wide, 5-20cm long.
7. according to any methods of claim 1-6, it is characterised in that described method includes following steps：
(1), described polycrystalline copper foil one end is formed as tip to be flat on high temperature-resistant liner bottom, connects transmission device, be put into chemistry
In vapor deposition apparatus, inert gas is passed through, inert gas flow is 300~500sccm, is then started to warm up, described is lazy
Property gas is N2Or Ar；
(2), when temperature rises to 800~1100 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment since tip, opens
Beginning annealing process；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal copper foil.
8. the method according to the description of claim 7 is characterized in that described method includes following steps：
(1), described polycrystalline copper foil one end is formed as tip to be flat on high temperature-resistant liner bottom, connects transmission device, be put into chemistry
In vapor deposition apparatus, inert gas is passed through, inert gas flow is 300~500sccm, is then started to warm up, temperature-rise period
Continue 50~70min, the inert gas is N2Or Ar；
(2), when temperature rises to 800~1100 DEG C, polycrystalline copper foil gradually passes through chemical vapor depsotition equipment since tip, more
The speed that brilliant copper foil continues through heating region is 0.01~10cm/min, starts annealing process, and annealing time is more than 1min；
(3), after growing, it is cooled to room temperature, that is, obtains large size single crystal copper foil.
9. according to claim 1-6 any one of them methods, it is characterised in that the length direction ruler for the monocrystalline copper foil prepared
Very little is 0.1~50m.
10. a kind of large size single crystal copper foil, it is characterised in that the large size single crystal copper foil is by any one of claim 1-9
Prepared by the method, the lengthwise dimension of the large size single crystal copper foil is 0.1~50m.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109537043A (en) * | 2018-12-28 | 2019-03-29 | 北京大学 | Control the preparation method of the monocrystalline copper foil of crystal face exposure orientation |
| CN109949964A (en) * | 2019-03-07 | 2019-06-28 | 北京大学 | A kind of method for reducing high-frequency circuit loss of based single crystal copper |
| 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 |
| CN110438556A (en) * | 2019-08-02 | 2019-11-12 | 北京石墨烯研究院 | A kind of preparation method of monocrystalline copper foil |
| CN110607550A (en) * | 2019-07-30 | 2019-12-24 | 财团法人交大思源基金会 | Quasi-single crystal thin film and method for producing same |
| 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 |
| CN110616458A (en) * | 2019-03-07 | 2019-12-27 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on 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 |
| WO2020173012A1 (en) * | 2019-02-27 | 2020-09-03 | 北京大学 | Method for clonal-growth of single-crystal metal |
| CN111663175A (en) * | 2019-03-07 | 2020-09-15 | 北京大学 | Method for preparing single crystal metal by grafting |
| CN111690982A (en) * | 2019-03-11 | 2020-09-22 | 北京大学 | Method for growing single crystal graphene by using single crystal copper foil with any index surface |
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| US11466385B2 (en) | 2020-07-27 | 2022-10-11 | National Yang Ming Chiao Tung University | Large grain quasi-single-crystal film and manufacturing method thereof |
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| CN112144116A (en) * | 2020-07-22 | 2020-12-29 | 郑州大学 | Method for simply and selectively preparing single crystal copper foil |
| CN112144116B (en) * | 2020-07-22 | 2021-09-14 | 郑州大学 | Method for simply and selectively preparing single crystal copper foil |
| US11466385B2 (en) | 2020-07-27 | 2022-10-11 | National Yang Ming Chiao Tung University | Large grain quasi-single-crystal film and manufacturing method thereof |
| CN111876703A (en) * | 2020-07-28 | 2020-11-03 | 江南大学 | Method for preparing graphene-grown single crystal copper substrate through stepping motor in vacuum |
| CN112795876A (en) * | 2020-12-31 | 2021-05-14 | 松山湖材料实验室 | Copper target material and preparation method thereof |
| CN112795876B (en) * | 2020-12-31 | 2023-08-08 | 松山湖材料实验室 | Copper target and preparation method thereof |
| CN112899768A (en) * | 2021-01-20 | 2021-06-04 | 南方科技大学 | Method for preparing single crystal copper |
| CN115029769A (en) * | 2022-06-28 | 2022-09-09 | 江苏科技大学 | Preparation method for transforming nano twin crystal copper film into single crystal copper film |
| CN115029769B (en) * | 2022-06-28 | 2023-11-21 | 江苏科技大学 | Preparation method for converting nano twin crystal copper film into single crystal copper film |
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