WO2020173012A1 - 一种克隆生长单晶金属的方法 - Google Patents

一种克隆生长单晶金属的方法 Download PDF

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WO2020173012A1
WO2020173012A1 PCT/CN2019/089912 CN2019089912W WO2020173012A1 WO 2020173012 A1 WO2020173012 A1 WO 2020173012A1 CN 2019089912 W CN2019089912 W CN 2019089912W WO 2020173012 A1 WO2020173012 A1 WO 2020173012A1
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copper foil
single crystal
polycrystalline
crystal copper
annealing
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刘开辉
张志斌
吴慕鸿
俞大鹏
王恩哥
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Peking University
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Peking University
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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
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64—Flat crystals, e.g. plates, strips or discs
    • 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
    • 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
    • C30B1/04—Isothermal recrystallisation
    • 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

Definitions

  • the invention relates to a method for clonal growth of single crystal metal, in particular to a method for clonal growth of rice-level single crystal copper foil using single crystal copper with any crystal face index.
  • Copper as one of the earliest metals used in human history, still has an extremely wide range of applications today with the rapid development of information.
  • copper is the most common conductive connection metal; also, due to its superior thermal conductivity, using copper fins to dissipate heat is currently the most common and optimal heat dissipation solution in mobile phones and computers. Due to its price-friendliness and superior performance, the role of copper in the information age will receive more attention. Therefore, obtaining large-area (meter-level) copper foil has an extremely important position in industrial development.
  • the widely used industrial copper foil is mostly polycrystalline copper, which has the shortcomings of small crystal grains, many grain boundaries, and high defect density. These defects greatly reduce their electrical and thermal conductivity, making the superior performance of copper foil unable to be completely It will be greatly reduced in industrial applications.
  • single crystal copper has large crystal domains, no grain boundaries, and low defect density. It completely overcomes these shortcomings of polycrystalline copper. Therefore, a large area (meter level) ) Single crystal copper foil plays a very important role in the industrial application of copper.
  • the present invention provides a method for clonal growth of single crystal metal. Taking copper as an example, the method includes the following steps:
  • the method includes the following steps:
  • the first polycrystalline copper foil is transformed into the same crystal face index as the first single crystal copper foil
  • the second single crystal copper foil which completes the process of clonal growth of single crystal copper foil.
  • the clone matrix is a single crystal copper foil with any crystal plane, including but not limited to Cu(111), Cu(110), Cu(211), Cu(345), Cu(346), Cu(335) ), Cu(236), Cu(124), Cu(553), Cu(122), Cu(255), Cu(256) and other crystal planes.
  • the shape of the small triangle is a right triangle, and the length of the hypotenuse is 1-5 cm.
  • the first single crystal copper foil when the first single crystal copper foil is placed on the first polycrystalline copper foil, a flattening process is performed to make the first single crystal copper foil fully contact the first polycrystalline copper foil.
  • the size of the first polycrystalline copper foil is 39cm*18cm. As the volume of the tube furnace used becomes larger, the size of the first polycrystalline copper foil may become larger.
  • the annealing time is adjusted to ensure that the crystal plane of the second single crystal copper foil is consistent with the crystal plane of the first single crystal copper foil.
  • the area of the first single crystal copper foil is 1%-50% of the area of the first polycrystalline copper foil.
  • the present invention also provides a single crystal copper foil, which is the second single crystal copper foil prepared by the above method.
  • the size of the single crystal copper foil prepared by the above method is 39cm*18cm and above.
  • the present invention utilizes the existing single crystal copper foil with any exponent plane, is placed on the copper foil that needs to be single crystallized, and is processed by annealing process to clone and obtain a large area (meter-level) single crystal copper foil with the same crystal plane index of the parent body.
  • the method proposed by the present invention solves the problem that single crystal copper foil is difficult to prepare. Through annealing process, a large size or large area ( ⁇ 700cm 2 ) can be obtained by cloning of a very small size ( ⁇ 0.25cm 2 ) single crystal copper foil matrix The area of single crystal copper foil has expanded by about 3000 times!
  • the present invention is a method for clonal growth of single crystal metal, including but not limited to single crystal copper foil;
  • the present invention uses commercially available polycrystalline copper foil as the raw material, and does not require complicated surface pretreatment of the copper foil, and can prepare super-large single crystal copper foil with any exponential surface, which greatly reduces the production cost ;
  • the present invention proposes for the first time a method for preparing single crystal copper foil by clonal growth.
  • the prepared single crystal copper foil has large size, few defects and superior performance, and has good application prospects.
  • the method of the present invention is simple, effective and low in cost, which is helpful for the practical application and industrial production of large-size single crystal copper foil.
  • Figure 1 shows the use of single crystal copper (Cu(xyz)) with any crystal face as the parent body.
  • the polycrystalline copper foil below is transformed into a single crystal copper foil with the same exponential surface (Cu( xyz)) process diagram.
  • Figure 2 shows the process of cloning a single crystal Cu(211) with the Cu(211) crystal plane as an example.
  • a triangular matrix with a hypotenuse of 2cm and a 9cm*5cm polycrystalline copper Take the foil as an example. After 180 minutes of annealing treatment, 98% of the entire polycrystalline copper foil in Figure 2(c) is converted into Cu(211).
  • Figure 3(a) is the EBSD result of Cu(211) parent
  • Figure 3(b) is the EBSD result of Cu(211) induced after cloning.
  • Figure 4 shows the large-area single crystal Cu(211) obtained after the cloning is completed.
  • the methods are conventional methods unless otherwise specified; the raw materials can be obtained from open commercial channels unless otherwise specified.
  • Embodiment 1 A method for clonal growth of single crystal metal, including the following steps:
  • the single crystal copper foil prepared by the clone in this experiment is shown in Figure 2(b). It can be seen that after a 90-minute annealing process, the single crystal Cu(211) has a crystal plane that is consistent with the parent body. The different colors represent With different crystal planes, we can see that we have obtained the crystal plane Cu(211) consistent with the parent body through the method of cloning, and it extends to 1/4 of the entire copper foil.
  • Embodiment 2 A method for clonal growth of single crystal metal, including the following steps:
  • Embodiment 3 A method for clonal growth of single crystal metal, including the following steps:
  • FIG. 4 The single crystal copper foil prepared by this experimental clone is shown in Figure 4.
  • Figure 3(a) is the EBSD of the cloned parent
  • Figure 3(b) is the EBSD of the large single crystal copper induced. Both EBSDs proved to be single crystal Cu(211), which also confirmed the reliability of the single crystal cloning method. It can be seen that we obtained the Cu(211) crystal plane consistent with the parent body through the method of cloning, that is, a large area (meter-level) single crystal copper foil was prepared.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

一种克隆生长单晶金属的方法，以铜为例，利用已有的任意指数面小尺寸单晶铜箔，放置在需要单晶化的铜箔上，通过退火工艺处理，克隆得到与母体晶面指数相同的大面积(米级)单晶铜箔。该方法解决了大面积单晶铜箔难以制备的问题，通过退火工艺处理，利用极小尺寸(～0.25cm 2)的单晶铜箔母体可以克隆制得大面积(～700cm 2)的单晶铜箔，面积扩大了约3000倍。

Description

一种克隆生长单晶金属的方法 技术领域
本发明涉及一种克隆生长单晶金属的方法，尤其涉及一种用任意晶面指数的单晶铜克隆生长米级单晶铜箔的方法。
背景技术
铜，作为人类历史上最早使用的金属之一，在信息高速发达的今天，仍然有着极其广泛的应用。例如：在手机、电脑等电子产品中，铜是最常见的导电连接金属；同样，由于其优越的导热性质，使用铜片散热是目前手机、电脑中最常见也是最优的散热解决方案。由于价格友好，性能优越，铜在信息时代所起的作用还将会得到更多的关注，因此获得大面积(米级)铜箔在工业发展中具有极其重要的地位。
而目前广泛使用的工业铜箔多为多晶铜，具有晶粒小，晶界多，缺陷密度高等缺点，这些缺陷大大地降低了他们的导电导热性能，使得铜箔优越的性能不能得以完全的发挥，在工业应用上会大打折扣，而与之相反的是，单晶铜晶畴大，无晶界，缺陷密度低，完全克服了多晶铜的这些缺点，因此，获得大面积(米级)单晶铜箔在铜的工业应用上起着非常重要的作用。
发明内容
本发明提出一种克隆生长单晶金属的方法，以铜为例，所述方法包括如下步骤：
提供第一单晶铜箔和第一多晶铜箔；
将所述第一单晶铜箔放置于所述第一多晶铜箔上；
退火，利用小尺寸的所述第一单晶铜箔作为克隆母体，将所述第一多晶铜箔克隆成与所述第一单晶铜箔晶面指数一致的大尺寸第二单晶铜箔。
优选的是，所述方法包括如下步骤：
(一)、使用任意晶面的单晶铜箔作为克隆母体；
(二)、将克隆母体剪成小三角形形状作为所述第一单晶铜箔，放置于需要单晶化的第一多晶铜箔之上；
(三)、将叠置的第一多晶铜箔和第一单晶铜箔放置于加热炉当中，通入Ar，流量为300sccm以上，然后开始升温，升温过程持续60～100min；
(四)、温度升至1010～1050℃时，通入H 2气体，H 2流量为10～500sccm，Ar流量保持不变，进行退火过程，退火持续时间为120min～300min；
(五)、退火结束后，关闭加热炉电源，以Ar和H 2为保护气体，自然冷却至室温，所述第一多晶铜箔转化为与所述第一单晶铜箔晶面指数一致的第二单晶铜箔，即完成克隆生长单晶铜箔的过程。
优选的是，所述克隆母体为任意晶面的单晶铜箔，包括但不限于Cu(111)、Cu(110)、Cu(211)、Cu(345)、Cu(346)、Cu(335)、Cu(236)、Cu(124)、Cu(553)、Cu(122)、Cu(255)、Cu(256)等晶面。
优选的是，所述小三角形形状为直角三角形，斜边长度为1-5cm。
优选的是，所述第一单晶铜箔放置于第一多晶铜箔之上时，进行做压平处理以使第一单晶铜箔与所述第一多晶铜箔充分接触。
在本发明的一些具体实施例中，所述第一多晶铜箔尺寸为39cm*18cm。随所用管式炉容积的变大，所述第一多晶铜箔的尺寸可以变大。
优选的是，调整所述退火的时间以保证第二单晶铜箔的晶面都与第一单晶铜箔的晶面一致。
优选的是，所述第一单晶铜箔的面积为所述第一多晶铜箔的面积的1％-50％。
本发明还提供一种单晶铜箔，该单晶铜箔为由上述方法制备的第二单晶铜箔。
优选的是，上述方法制备的所述单晶铜箔的尺寸在39cm*18cm及以上。
本发明利用已有的任意指数面单晶铜箔，放置在需要单晶化的铜箔上，通过退火工艺处理，克隆得到与母体晶面指数相同的大面积(米级)单晶铜箔。本发明提出的方法解决了单晶铜箔难以制备的问题，通过退火工艺处理，利用极小尺寸(～0.25cm 2)的单晶铜箔母体克隆制得了大尺寸或大面积(～700cm 2)的单晶铜箔，面积扩大了约3000倍！
本发明的优点在于：
1.本发明为一种克隆生长单晶金属的方法，包括但不限于单晶铜箔；
2.本发明选用商业上可以购买的多晶铜箔作为原料，不需要对铜箔进行复杂的表面预处理，就可以制备出超大尺寸的任意指数面的单晶铜箔，极大地降低制备成本；
3.本发明首次提出了一种克隆生长制备单晶铜箔的方法，制备出的单晶铜箔尺寸大、缺陷少、性能优越，具有良好的应用前景。
4.本发明方法简单、有效、成本低，有助于大尺寸单晶铜箔的实际应用及工业化生产。
附图说明
图1为用任意晶面的单晶铜(Cu(xyz))作为母体，在管式炉退火过程中，通过克隆使得下面的多晶铜箔转变为同样指数面的单晶铜箔(Cu(xyz))的过程示意图。
图2为以Cu(211)晶面为例，克隆得到单晶Cu(211)过程，在此过程图2(a)中，以斜边为2cm的三角形母体，以9cm*5cm的多晶铜箔为例，经过180分钟的退火处理，图2(c)整个多晶铜箔的98％的区域都转化为Cu(211)。
图3(a)为Cu(211)母体的EBSD结果，图3(b)是经过克隆之后诱导出的Cu(211)的EBSD结果。
图4是克隆完成之后，得到的大面积单晶Cu(211)。
具体实施方式
下面结合具体实施例对本发明做进一步详细说明，但本方法并不限于以下实例。
下述实施的方式中，所述方法如无特别说明均为常规方法；所述原材料如无特别说明均能从公开商业途径而得。
实施方式一：一种克隆生长单晶金属的方法，包括如下步骤：
(一)、使用任意晶面的单晶铜箔作为克隆的母体，此处选用单晶Cu(211)；
(二)、将得到的母体剪成标准的小直角三角形形状，斜边尺寸为2cm，放置于需要单晶化的多晶铜箔之上，尺寸为9cm*5cm；
(三)、将该铜箔放置于管式炉当中，通入Ar气体，流量为800sccm，然后开始升温，升温过程持续80min；
(四)、温度升至1030℃时，通入H 2气体，流量为50sccm，Ar流量保持不变，进行退火过程，退火持续时间为90min；
(五)、退火结束后，关闭加热电源，以Ar和H 2为保护气体，自然冷却至室温。
本试验克隆制备的单晶铜箔如图2(b)所示，可以看到，经过90分钟的退火过程，单晶Cu(211)周围克隆出与母体一致的晶面，由于不同的颜色代表着不同的晶面，可知，我们通过克隆的方法，得到了与母体一致的晶面Cu(211)，并延伸至整个铜箔1/4的区域。
实施方式二：一种克隆生长单晶金属的方法，包括如下步骤：
(一)、使用任意晶面的单晶铜箔作为克隆的母体，此处选用单晶Cu(211)；
(二)、将得到的母体剪成标准的小直角三角形形状，斜边尺寸为2cm，放置于需要单晶化的多晶铜箔之上，尺寸为9cm*5cm；
(三)、将该铜箔放置于管式炉当中，通入Ar气体，流量为800sccm，然后开始升温，升温过程持续80min；
(四)、温度升至1030℃时，通入H 2气体，流量为50sccm，Ar流量保持不变，进行退火过程，退火持续时间为180min；
(五)、退火结束后，关闭加热电源，以Ar和H 2为保护气体，自然冷却至室温。
本试验克隆制备的单晶铜箔如图2(c)所示，可以看到，经过180分钟的退火过程，我们通过克隆的方法，得到了与母体一致的晶面Cu(211)，并延伸至整个铜箔大于98％的区域。
实施方式三：一种克隆生长单晶金属的方法，包括如下步骤：
(一)、使用任意晶面的单晶铜箔作为克隆的母体，此处选用单晶Cu(211)；
(二)、将得到的母体剪成标准的小直角三角形形状，斜边尺寸为1cm，放置于需要单晶化的多晶铜箔之上，尺寸为39cm*18cm；
(三)、将该铜箔放置于管式炉当中，通入Ar气体，流量为800sccm，然后开始升温，升温过程持续80min；
(四)、温度升至1030℃时，通入H 2气体，流量为50sccm，Ar流量保持不变，进行退火过程，退火持续时间为300min；
(五)、退火结束后，关闭加热电源，以Ar和H 2为保护气体，自然冷却至室温。
本试验克隆制备的单晶铜箔如图4所示。而图3(a)是克隆母体的EBSD，图3(b)是诱导出的大单晶铜的EBSD。两个EBSD均证明是单晶Cu(211)，也证实了单晶克隆方法的可靠性。可以看到，我们通过克隆的方法，得到了与母体一致的晶面Cu(211)，即制备得了大面积(米级)单晶铜箔。

Claims (10)

  1. 一种克隆生长单晶金属的方法，其特征在于，所述方法包括如下步骤：
    提供第一单晶铜箔和第一多晶铜箔；
    将所述第一单晶铜箔放置于所述第一多晶铜箔上；
    退火，利用小尺寸的所述第一单晶铜箔作为克隆母体，将所述第一多晶铜箔克隆成与所述第一单晶铜箔晶面指数一致的大尺寸第二单晶铜箔。
  2. 根据权利要求1所述的方法，其特征在于，所述方法包括如下步骤：
    (一)使用任意晶面的单晶铜箔作为克隆母体；
    (二)将所述克隆母体剪成小三角形形状作为第一单晶铜箔，放置于需要单晶化的第一多晶铜箔之上；
    (三)将叠置的第一多晶铜箔和第一单晶铜箔放置于加热炉当中，通入Ar，流量为300sccm以上，然后开始升温，升温过程持续60～100min；
    (四)温度升至1010～1050℃时，通入H 2气体，H 2流量为10～500sccm，Ar流量保持不变，进行退火过程，退火持续时间为120min～300min；
    (五)退火结束后，关闭加热炉电源，以Ar和H 2为保护气体，自然冷却至室温，所述第一多晶铜箔转化为与所述第一单晶铜箔晶面指数一致的第二单晶铜箔，即完成克隆生长单晶铜箔的过程。
  3. 根据权利要求2所述的方法，其特征在于，所述克隆母体的晶面包括但不限于Cu(111)、Cu(110)、Cu(211)、Cu(345)、Cu(346)、Cu(335)、Cu(236)、Cu(124)、Cu(553)、Cu(122)、Cu(255)、Cu(256)。
  4. 根据权利要求2所述的方法，其特征在于，所述小三角形形状为直角三角形，斜边长度为1-5cm。
  5. 根据权利要求2所述的方法，其特征在于，步骤(二)将第一单晶铜箔放置于第一多晶铜箔之上时，进行压平处理以使所述第一单晶铜箔与所述第一多晶铜箔充分接触。
  6. 根据权利要求2所述的方法，其特征在于，所述第一多晶铜箔尺寸为39cm*18cm或以上。
  7. 根据权利要求1所述的方法，其特征在于，调整所述退火的时间以保证第二单晶铜箔的晶面都与第一单晶铜箔的晶面一致。
  8. 根据权利要求1所述的方法，其特征在于，所述第一单晶铜箔的面积为所述第一多晶铜箔的面积的1％-50％。
  9. 一种单晶铜箔，其特征在于，所述单晶铜箔为由权利要求1-8任一项所述的方法制备的第二单晶铜箔。
  10. 根据权利要求9所述的单晶铜箔，其特征在于，所述单晶铜箔的尺寸为39cm*18cm或以上。
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