CN110438556A - A kind of preparation method of monocrystalline copper foil - Google Patents
A kind of preparation method of monocrystalline copper foil Download PDFInfo
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- CN110438556A CN110438556A CN201910710749.8A CN201910710749A CN110438556A CN 110438556 A CN110438556 A CN 110438556A CN 201910710749 A CN201910710749 A CN 201910710749A CN 110438556 A CN110438556 A CN 110438556A
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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
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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 present invention provides a kind of monocrystalline copper foil and preparation method thereof, this method includes that polycrystalline copper foil is placed in the region with multiple warm areas to anneal, and the monocrystalline copper foil is made；Wherein, in the region with multiple warm areas, the temperature difference of adjacent warm area is 5~200 DEG C.The method of an embodiment of the present invention, simple process obtain large area, the copper single crystal that monocrystalline degree is high, flatness is high in which can be convenient.
Description
Technical field
The present invention relates to the preparation of monocrystalline copper foil, specially a kind of method of static preparation large area monocrystalline copper foil.
Background technique
Industrial rolled copper foil or electrolytic copper foil are often polycrystalline copper foil, and the presence of crystal boundary will affect its electricity and mechanical property
Matter.And since scattering of the crystal boundary to electronics being not present in monocrystalline copper foil, thus there is higher electric conductivity；Single crystal Cu (111)
Crystal face can be used as graphene growth substrate, the same oriented epitaxial growth of graphene be realized, so as to prepare large area
Single crystal graphene sample.Therefore, people have extensive demand to the preparation of large area monocrystalline copper foil.
Currently, the reported method for preparing copper single crystal has:
1, high temperature long term annealing；This method may be implemented conversion of the polycrystalline copper foil to monocrystalline copper foil, but monocrystalline
Limited area；
2, copper foil one end is cut into tip, dynamic annealing then is carried out to copper foil；This method can prepare larger areas of copper
Foil monocrystalline, but annealing furnace device needs to wind and mechanical driving device, while the external force of mechanical traction can be introduced to copper foil, furthermore
There is particular/special requirement to the shape at copper foil tip, on the whole, the technique of this method, device are complex；
3, the unstressed annealing of static suspension, that is, vacantly place metal foil, it is outer to reduce to avoid the contact with substrate
Stress realizes the preparation of larger area copper foil monocrystalline；However, this method needs vacantly to place metal foil, and copper obtained
The area maximum of foil monocrystalline is at 32 square centimeters or so.
Summary of the invention
A primary object of the present invention is providing a kind of preparation method of monocrystalline copper foil, including polycrystalline copper foil is placed in tool
It anneals in the region for having multiple warm areas, the monocrystalline copper foil is made；Wherein, in the region with multiple warm areas,
The temperature difference of adjacent warm area is 5~200 DEG C.
According to an embodiment of the present invention, the temperature of at least one warm area is at 900 DEG C or more.
According to an embodiment of the present invention, the temperature of at least one warm area is at 980 DEG C or more.
According to an embodiment of the present invention, the temperature of the multiple warm area is 800~1080 DEG C.
According to an embodiment of the present invention, the multiple warm area includes the first warm area, the second warm area and third warm area.
According to an embodiment of the present invention, the temperature of first warm area is 980~1040 DEG C, the temperature of second warm area
Degree is 950~1020 DEG C, and the temperature of the third warm area is 850~1000 DEG C.
According to an embodiment of the present invention, the multiple warm area includes the first warm area, the second warm area, third warm area, the 4th
Warm area, the 5th warm area；The temperature of first warm area is 1000~1040 DEG C, and the temperature of second warm area is 980~1030
DEG C, the temperature of the third warm area is 950~1020 DEG C, and the temperature of four-temperature region is 900~1010 DEG C, the temperature of the 5th warm area
It is 850~1000 DEG C.
According to an embodiment of the present invention, the temperature difference of the adjacent warm area is 10~30 DEG C.
According to an embodiment of the present invention, the atmosphere in the annealing process is hydrogen, argon gas, helium, argon oxygen mix
One of gas is a variety of；And/or the annealing time is 5 minutes or more.
An embodiment of the present invention provides a kind of monocrystalline copper foil, is made by above-mentioned method.
The method of an embodiment of the present invention, simple process obtain large area, monocrystalline degree height, flatness in which can be convenient
High copper single crystal.
Detailed description of the invention
Fig. 1 is the indicative of local optical picture of large area monocrystalline copper foil made from the embodiment of the present invention 1；
Fig. 2 is the XRD characterization result of (111) high preferred orientation copper foil monocrystalline made from the embodiment of the present invention 1；
Fig. 3 is the EBSD characterization result of (111) high preferred orientation copper foil monocrystalline made from the embodiment of the present invention 1；
Fig. 4 is the indicative of local optical picture of (111) high preferred orientation copper foil monocrystalline a piece of made from the embodiment of the present invention 3；
Fig. 5 is the EBSD characterization result of (111) high preferred orientation copper foil monocrystalline a piece of made from the embodiment of the present invention 3；
Fig. 6 is the optics picture of (106) high preferred orientation copper foil monocrystalline a piece of made from the embodiment of the present invention 5；
Fig. 7 is the EBSD characterization result of (106) high preferred orientation copper foil monocrystalline a piece of made from the embodiment of the present invention 5；
Fig. 8 is the XRD characterization result of (111) high preferred orientation copper foil monocrystalline a piece of made from the embodiment of the present invention 6.
Specific embodiment
The exemplary embodiment for embodying feature of present invention and advantage will describe in detail in the following description.It should be understood that
The present invention can have various variations in different embodiments, neither depart from the scope of the present invention, and theory therein
Bright and diagram inherently is illustrated as being used, rather than to limit the present invention.
An embodiment of the present invention provides a kind of preparation method of monocrystalline copper foil, including polycrystalline copper foil is placed in more
It anneals in the region (annealing region) of a warm area, monocrystalline copper foil is made；Wherein, in the region with multiple warm areas, phase
The temperature difference of adjacent warm area is 5~200 DEG C.
In an embodiment, in annealing process, polycrystalline copper foil is located at least two warm areas, that is, polycrystalline copper foil passes through
The intersection of two warm areas.
In an embodiment, polycrystalline copper foil is set to each warm area of entire annealing region.
In an embodiment, the temperature difference of adjacent warm area can be 5~200 DEG C in annealing region, may further be 5~
50 DEG C, it further can be 10~30 DEG C.Such as 6 DEG C, 8 DEG C, 10 DEG C, 12 DEG C, 14 DEG C, 15 DEG C, 16 DEG C, 18 DEG C, 20 DEG C, 25
DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 100 DEG C, 120 DEG C, 150 DEG C, 180 DEG C etc..
In an embodiment, annealing region includes connected multiple warm areas, such as two warm areas, three warm areas, four
Warm area, five warm areas, six warm areas etc.；Wherein, the temperature of at least one warm area is at 900 DEG C or more, and preferably 980 DEG C or more,
Such as 1000 DEG C, 1020 DEG C, 1050 DEG C, 1080 DEG C etc., so that part copper foil region is in surface and melts state in advance.
In an embodiment, the temperature of annealing region (multiple warm areas) is 800~1080 DEG C, for example, 820 DEG C, 840 DEG C,
850℃、870℃、880℃、900℃、920℃、940℃、950℃、960℃、980℃、1000℃、1020℃、1050℃、
1060 DEG C, 1080 DEG C etc..
In the application, the quantity of warm area is not limited, it can be depending on the structure of used annealing furnace body.
In an embodiment, multiple warm areas include connected the first warm area and the second warm area, and the first warm area can be
1000 DEG C, the second warm area can be 900 DEG C, 950 DEG C, 980 DEG C or 990 DEG C.
In an embodiment, multiple warm areas include the first warm area, the second warm area and third warm area being sequentially connected.
In an embodiment, the temperature of the first warm area can be 980~1040 DEG C, such as 1000 DEG C, 1020 DEG C；Second
The temperature of warm area can be 950~1020 DEG C, such as 960 DEG C, 980 DEG C, 1000 DEG C etc.；The temperature of third warm area can be 850
~1000 DEG C, such as 870 DEG C, 900 DEG C, 920 DEG C, 950 DEG C, 980 DEG C etc..
In an embodiment, the first warm area, the second warm area and third warm area can be respectively 1020 DEG C, 1000 DEG C, 980
℃。
In an embodiment, the first warm area, the second warm area and third warm area can be respectively 1000 DEG C, 950 DEG C, 900
℃。
In an embodiment, the first warm area, the second warm area and third warm area can be respectively 1020 DEG C, 950 DEG C, 900
℃。
In an embodiment, the first warm area, the second warm area and third warm area can be respectively 850 DEG C, 1020 DEG C, 850
℃。
In an embodiment, the first warm area, the second warm area and third warm area can be respectively 980 DEG C, 1020 DEG C, 970
℃。
In an embodiment, multiple warm areas include the first warm area, the second warm area, third warm area, the 4th being sequentially connected
Warm area, the 5th warm area.
In an embodiment, the temperature of the first warm area can be 1000~1040 DEG C, for example, 1020 DEG C, 1030 DEG C etc.；
The temperature of second warm area can be 980~1030 DEG C, for example, 990 DEG C, 1000 DEG C, 1020 DEG C etc.；The temperature of third warm area can be with
It is 950~1020 DEG C, for example, 960 DEG C, 980 DEG C, 1000 DEG C, 1010 DEG C etc.；The temperature of four-temperature region can be 900~1010
DEG C, for example, 920 DEG C, 950 DEG C, 980 DEG C, 1000 DEG C etc.；The temperature of 5th warm area can be 850~1000 DEG C for example, 860 DEG C,
880 DEG C, 900 DEG C, 920 DEG C, 950 DEG C, 960 DEG C, 980 DEG C etc..
In an embodiment, multiple warm areas in annealing region are connected, and the temperature of each warm area is with identical or different
The temperature difference is sequentially increased or reduces；For example, the temperature of the first connected warm area, the second warm area, third warm area can be 1000 DEG C,
980 DEG C, 900 DEG C or 900 DEG C, 980 DEG C, 1000 DEG C.
In an embodiment, the temperature difference of adjacent warm area is identical in annealing region, that is, the temperature of multiple warm areas is in staged
Increasing or decreasing, such as with 10 DEG C, 20 DEG C or 50 DEG C for temperature difference increasing or decreasing, form static temperature gradient.
In an embodiment, the temperature in multiple warm areas being connected in annealing region is successively first increased and is reduced afterwards, for example,
Connected the first warm area, the second warm area, third warm area temperature can be 850 DEG C, 1020 DEG C, 850 DEG C respectively.
In an embodiment, the temperature in multiple warm areas being connected in annealing region successively first reduces to be increased afterwards, for example,
Connected the first warm area, the second warm area, third warm area temperature can be 1020 DEG C, 900 DEG C, 1000 DEG C respectively.
In an embodiment, the annealing process of polycrystalline copper foil can be completed in annealing furnace (such as tube furnace), pass through tune
The annealing region of multiple warm areas composition with the temperature difference is provided in the temperature of whole each warm area of annealing furnace.
In an embodiment, annealing furnace has one or more heating warm areas, different by the way that each heating warm area to be arranged
Temperature, and then be arranged and come out of the stove interior static temperature gradients region.
In an embodiment, when the annealing process of polycrystalline copper foil is completed in annealing furnace, annealing includes in annealing furnace
Warm area is heated, may also comprise the unheated zone other than heating warm area, that is, the temperature difference between heating warm area and unheated zone meets
Temperature difference restriction is stated, corresponding unheated zone also belongs to a part of annealing region.
In an embodiment, the annealing of polycrystalline copper foil is carried out using three-temperature-zone annealing furnace, three warm areas in annealing furnace
Temperature successively can be 1020 DEG C, 1000 DEG C, 980 DEG C or 1000 DEG C, 950 DEG C, 900 DEG C.
In an embodiment, polycrystalline copper foil can be put on carrier, by carrier be placed in annealing region (annealing furnace) into
Row high annealing, the structure of carrier can the existing carrier for annealing structure.
In an embodiment, the quantity of carrier can be one, be also possible to it is multiple, it is more for placing one or more pieces
Brilliant copper foil；When placing multiple polycrystalline copper foils using multiple carriers, the batch preparation of monocrystalline copper foil may be implemented.
In an embodiment, the atmosphere in annealing process can mix in gas for hydrogen, argon gas, helium, argon oxygen
It is one or more.
In an embodiment, the atmosphere of annealing process is 500sccm hydrogen.
In an embodiment, annealing time is 5 minutes or more, such as 10 minutes, 30 minutes, 60 minutes etc..
The preparation method of the monocrystalline copper foil of an embodiment of the present invention, includes the following steps:
S1: polycrystalline copper foil is placed on carrier；
S2: the carrier for being placed with copper foil is placed in annealing furnace；
S3: being warming up to assigned temperature for annealing furnace, form the annealing region with multiple warm areas, carries out to polycrystalline copper foil high
Temperature annealing；
S3: annealing furnace is cooled to room temperature, and obtains monocrystalline copper foil sample.
The method of an embodiment of the present invention can once move back multi-disc polycrystalline copper foil by configuring multiple carriers
Fire processing realizes that mass static state prepares monocrystalline copper foil.
The method of this embodiment, does not require the shape of polycrystalline copper foil specifically, the length and width of copper foil monocrystalline
Degree is limited only in the size of furnace body, thus large area mass production may be implemented.
The method of an embodiment of the present invention, without complicated mechanical driving device, without being hung to polycrystalline copper foil
The mass preparation of large area monocrystalline copper foil can be realized.
The method of an embodiment of the present invention, technique is more simple and convenient, and used device is simple, common tube furnace
Equal annealing furnaces can meet the preparation demand of monocrystalline copper foil；Machine driving and winding device, and the side of static annealing are not needed
Formula will not generate additional mechanical stretching to copper foil, and the monocrystalline copper foil made is more smooth.
Below in conjunction with preparation method of the drawings and the specific embodiments to the monocrystalline copper foil of an embodiment of the present invention carry out into
One step explanation.Wherein, used raw material is commercially available acquisition.
1 three-temperature-zone anneal of embodiment obtains monolithic monocrystalline copper foil
In the present embodiment, used annealing furnace is three-temperature-zone annealing furnace.The length of each warm area is 20cm.Three temperature
The temperature setting in area is successively are as follows: 1020 DEG C, 1000 DEG C, 980 DEG C.Specific step are as follows:
(1) monolithic industry copper foil is cut into 40cm long, is placed on copper foil carrier, copper foil carrier is placed in annealing furnace,
It is in copper foil in three warm areas；
(2) opening mechanical pump will anneal stove evacuation, then pass to 500sccm hydrogen；
(3) temperature of three warm areas of annealing furnace rises to the temperature of setting: 1020 DEG C, 1000 DEG C, 980 DEG C；
(4) copper foil is annealed at a set temperature 30 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, obtain larger areas of copper (111) monocrystalline sample
Product.The picture of local copper foil monocrystalline as shown in Fig. 1, the area size of copper foil monocrystalline are 182 square centimeters.
2 three-temperature-zone anneal of embodiment obtains multi-disc mass monocrystalline copper foil
In the present embodiment, used annealing furnace is three-temperature-zone annealing furnace.The length of each warm area is 20cm.Three temperature
The temperature setting in area is successively are as follows: 1020 DEG C, 1000 DEG C, 980 DEG C.Specific step are as follows:
(1) multi-disc industry copper foil is cut into 45cm long, is placed on a piece of copper foil carrier per a piece of copper foil, by copper foil
Carrier vertical stacking, is subsequently placed in annealing furnace, is in copper foil in three warm areas；
(2) opening mechanical pump will anneal stove evacuation, then pass to 500sccm hydrogen；
(3) temperature of three warm areas of annealing furnace rises to the temperature of setting: 1020 DEG C, 1000 DEG C, 980 DEG C；
(4) copper foil is annealed at a set temperature 30 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, it is single to obtain multi-disc larger areas of copper (111)
Brilliant sample.
3 three-temperature-zone anneal of embodiment obtains multi-disc mass monocrystalline copper foil
In the present embodiment, annealing furnace is three-temperature-zone annealing furnace.The length of each warm area is 20cm.The temperature of three warm areas
Setting is successively are as follows: 1020 DEG C, 950 DEG C, 900 DEG C.The present embodiment the difference from example 2 is that, the temperature setting of three warm areas
Difference, to make the of different sizes of the adjacent warm area temperature difference.Specific step are as follows:
(1) multi-disc industry copper foil is cut into 45cm long, is placed on a piece of copper foil carrier per a piece of copper foil, by copper foil
Carrier vertical stacking, is subsequently placed in annealing furnace, is in copper foil in three warm areas；
(2) opening mechanical pump will anneal stove evacuation, then pass to 500sccm hydrogen；
(3) temperature of three warm areas of annealing furnace rises to the temperature of setting: 1020 DEG C, 950 DEG C, 900 DEG C；
(4) copper foil is annealed at a set temperature 30 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, it is single to obtain multi-disc larger areas of copper (111)
Brilliant sample.
It should be understood that, due to setting the biggish temperature difference, some regional temperature is lower than in the present embodiment
The pre- of copper foil melts temperature, thus the crystal region length of the copper foil sample prepared can be less than embodiment 2, but will not be to list
Crystalline substance has an impact.
Fig. 4 is the indicative of local optical picture of a piece of (111) high preferred orientation copper foil monocrystalline made from embodiment 3, due to there is one
The temperature of point copper foil is lower, therefore it is apparent that crystal region (left side) and poly-region (right side) line of demarcation.
4 single temperature zone anneal of embodiment obtains multi-disc mass monocrystalline copper foil
In the present embodiment, used annealing furnace is single temperature zone annealing furnace, and the length of warm area is 30cm.The temperature of warm area
Setting are as follows: 1020 DEG C.Specific step are as follows:
(1) multi-disc industry copper foil is cut into 40cm long, is placed on a piece of copper foil carrier per a piece of copper foil, by copper foil
Carrier vertical stacking, is subsequently placed in annealing furnace.Since copper foil length is longer than warm area length, foil section region, which is located at, is moved back
Except the heating warm area of stove；
(2) opening mechanical pump will anneal stove evacuation, then pass to 500sccm hydrogen or 500sccm argon gas；
(3) annealing furnace Heating Zone Temperature is warming up to the temperature of setting: 1020 DEG C, the temperature at copper foil both ends except heating zone
About 850 DEG C；
(4) copper foil is annealed at a set temperature 30 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, it is single to obtain multi-disc larger areas of copper (111)
Brilliant sample.
5 three-temperature-zone anneal of embodiment obtains multi-disc mass monocrystalline copper foil
In the present embodiment, used annealing furnace is three-temperature-zone annealing furnace, and the temperature setting of three warm areas is successively are as follows:
1020℃,950℃,900℃.In the present embodiment, other crystal face copper foil monocrystalline in addition to (111) crystal face are illustrated.
Specific step are as follows:
(1) multi-disc industry copper foil is cut into 45cm long, is placed on a piece of copper foil carrier per a piece of copper foil.By copper foil
Carrier vertical stacking, is subsequently placed in annealing furnace, is in copper foil in three warm areas；
(2) opening mechanical pump will anneal stove evacuation, then pass to 500sccm hydrogen；
(3) furnace temperature that will anneal is warming up to the temperature of setting: 1020 DEG C, 950 DEG C, 900 DEG C；
(4) copper foil is annealed at a set temperature 60 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, it is single to obtain multi-disc larger areas of copper (106)
Brilliant sample.
Fig. 6 is the optics picture of a piece of (106) high preferred orientation copper foil monocrystalline made from embodiment 5, it is apparent that
The line of demarcation of crystal region (left side) and poly-region (right side).The area of the local copper foil monocrystalline shown in the present embodiment attached drawing 4
It is 53 square centimeters.
6 five warm area annealing furnace of embodiment prepares monocrystalline copper foil
In the present embodiment, used annealing furnace is five warm area annealing furnaces, and the length of each warm area is 30cm.
The temperature setting of five warm areas is successively are as follows: 1040 DEG C, 1025 DEG C, 1005 DEG C, 990 DEG C, 975 DEG C.
Specific step are as follows:
(1) multi-disc industry copper foil is cut into 150cm long, is placed on a piece of copper foil carrier per a piece of copper foil.By copper
Foil carrier vertical stacking, is subsequently placed in annealing furnace, is in copper foil in five warm areas；
(2) opening mechanical pump will anneal stove evacuation, then pass to 2000sccm hydrogen；
(3) furnace temperature that will anneal is warming up to the temperature of setting: 1040 DEG C, 1025 DEG C, 1005 DEG C, 990 DEG C, 975 DEG C；
(4) copper foil is annealed at a set temperature 60 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, it is single to obtain multi-disc larger areas of copper (111)
Brilliant sample.
7 three-temperature-zone anneal of embodiment obtains monolithic monocrystalline copper foil
In the present embodiment, used annealing furnace is three-temperature-zone annealing furnace.The length of each warm area is 20cm.Three temperature
The temperature setting in area is successively are as follows: 980 DEG C, 1020 DEG C, 970 DEG C.One of the present embodiment and the difference of embodiment 1 are: this implementation
In example in three warm areas intermediate warm area temperature setting highest.Specific step are as follows:
(1) monolithic industry copper foil is cut out into 50cm long, is placed on copper foil carrier, copper foil carrier is placed in annealing furnace, is made
Copper foil is in three warm areas；
(2) opening mechanical pump will anneal stove evacuation, then pass to 500sccm hydrogen and 500sccm argon gas；
(3) temperature of three warm areas of annealing furnace rises to the temperature of setting: 1020 DEG C, 1000 DEG C, 980 DEG C；
(4) copper foil is annealed at a set temperature 60 minutes；
(5) after furnace temperature to be annealed is reduced to room temperature, turn off gas, be connected to atmosphere, obtain copper single crystal sample.
Unless limited otherwise, term used herein is the normally understood meaning of those skilled in the art.
Embodiment described in the invention is merely for exemplary purpose, the protection scope being not intended to limit the invention,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention is not limited to
Above embodiment, and be only defined by the claims.
Claims (10)
1. a kind of preparation method of monocrystalline copper foil, anneals including being placed in polycrystalline copper foil in the region with multiple warm areas,
The monocrystalline copper foil is made；Wherein, in the region with multiple warm areas, the temperature difference of adjacent warm area is 5~200 DEG C.
2. according to the method described in claim 1, wherein, the temperature of at least one warm area is at 900 DEG C or more.
3. according to the method described in claim 2, wherein, the temperature of at least one warm area is at 980 DEG C or more.
4. according to the method described in claim 1, wherein, the temperature of the multiple warm area is 800~1080 DEG C.
5. method according to claim 1 to 4, wherein the multiple warm area includes the first warm area, the second temperature
Area and third warm area.
6. described second is warm according to the method described in claim 5, wherein, the temperature of first warm area is 980~1040 DEG C
The temperature in area is 950~1020 DEG C, and the temperature of the third warm area is 850~1000 DEG C.
7. according to the method described in claim 5, further including four-temperature region and the 5th warm area wherein.
8. according to the method described in claim 7, wherein, the temperature of first warm area is 1000~1040 DEG C, described second
The temperature of warm area is 980~1030 DEG C, and the temperature of the third warm area is 950~1020 DEG C, the temperature of four-temperature region is 900~
1010 DEG C, the temperature of the 5th warm area is 850~1000 DEG C.
9. method according to claim 1 to 4, wherein the temperature difference of the adjacent warm area is 10~30 DEG C.
10. a kind of monocrystalline copper foil, the method as described in any one of claims 1 to 9 are made.
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| 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 |
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