CN114411233A - Method for rapidly preparing (100) single crystal copper - Google Patents

Method for rapidly preparing (100) single crystal copper Download PDF

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CN114411233A
CN114411233A CN202210028237.5A CN202210028237A CN114411233A CN 114411233 A CN114411233 A CN 114411233A CN 202210028237 A CN202210028237 A CN 202210028237A CN 114411233 A CN114411233 A CN 114411233A
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crystal
twin
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CN114411233B (en
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黄明亮
张诗楠
武洋
詹莉昕
黄斐斐
任婧
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Dalian University of Technology
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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
    • 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
    • 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
    • C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • C30B30/02—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using electric fields, e.g. electrolysis

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Abstract

The invention provides a method for rapidly preparing (100) single crystal copper, which is characterized in that while annealing is carried out on a (111) preferred orientation nanometer twin crystal Cu film, an electric field is applied to the film and the film is kept for a certain time, so that crystal grains of the film grow rapidly, and finally the (111) preferred orientation nanometer twin crystal Cu is converted into (100) preferred orientation single crystal Cu. The method of the invention obviously improves the production efficiency of the single crystal Cu, and the prepared single crystal Cu with the (100) preferred orientation and large grain size has the advantages of excellent mechanical property, oxidation resistance, electromigration resistance, thermal stability and the like. The preparation method of the (100) single crystal copper is simple, efficient, low in cost, good in compatibility with the existing microelectronic packaging process and very suitable for large-scale industrial production.

Description

Method for rapidly preparing (100) single crystal copper
Technical Field
The invention relates to the technical field of microelectronic manufacturing, in particular to a method for rapidly preparing (100) single crystal copper.
Background
Copper (Cu) is the most widely used conductor material in current microelectronic packaging technology, and is applied to Under Bump Metallization (UBM), Redistribution Layer (RDL), chip interconnects, and wires, etc. With the development of semiconductor technology, microelectronic packaging technology continues to develop towards miniaturization, and advanced three-dimensional system-in-package puts new requirements on the used Cu interconnection material. With the reduction of the size and the improvement of the density, the current density in the microelectronic packaging structure is improved, the heat dissipation capability is weakened, and electromigration failure and high-temperature failure are more likely to occur; meanwhile, as the bump size is reduced, the number of grains of Intermetallic compounds (IMCs) and UBMs in the micro-bumps is continuously reduced, even only one grain is formed, so that the anisotropic characteristics of the IMCs and UBMs are more prominent, which may lead to early failure and reduced reliability of the micro-bumps. Conventional polycrystalline Cu cannot solve the above problems, and thus new materials are required to comprehensively replace polycrystalline Cu widely used in microelectronic packaging technology.
The single crystal copper has single preferred orientation, eliminates a crystal boundary structure serving as a diffusion channel, and therefore has better electromigration resistance than polycrystalline copper; meanwhile, the single crystal Cu can not generate grain growth and recrystallization, and has better thermal stability than the polycrystal Cu; in addition, IMC crystal grains generated by reaction of the UBM and the brazing filler metal alloy also have preferred orientation, and meanwhile, the formation of Kirkendall holes (Kirkendall Voids) can be reduced, and the reliability of micro welding spots is improved; the single crystal copper also has the advantages of excellent mechanical property, low resistivity and the like. Therefore, single crystal Cu is a highly desirable material for UBM, RDL, and wires, etc. in microelectronic packaging technology. In industry, single crystal Cu is generally prepared by a method of controlling a molten metal solidification process such as bridgman method, however, it is difficult to obtain a thin film structure having a fine pattern such as UBM, RDL, etc. required in a microelectronic packaging technology by this method, and a high temperature in a casting process may cause serious thermal damage to a semiconductor device, so that it has an important engineering practical value to develop a method of preparing single crystal Cu suitable for microelectronic packaging.
The method for preparing single crystal Cu in the microelectronic packaging technology in the prior art mainly comprises the following steps:
international patent application publication No. WO2020006761 discloses a method for preparing a (100) single crystal Cu thin film by electrodeposition, which uses a specific apparatus and an electroplating solution to cause potential oscillation between electrodes during the process of electrodeposition of Cu, thereby depositing the (100) single crystal Cu thin film. However, the plating solution used in the method contains various additives, on one hand, the stability of the plating solution is difficult to ensure due to complex components, and on the other hand, the additives can be remained in the Cu film as impurities to influence the performance of the film; meanwhile, in the electroplating process of the method, higher stirring speed of the plating solution is needed, the stirring speed can be achieved only by using a rotating disc electrode, and the electroplating area of the rotating disc electrode is very small, so that the method is difficult to deposit a large-area (100) single crystal Cu film, has low efficiency and is not suitable for industrial production; in addition, the single crystal Cu crystal grain prepared by the method is about 10-20 μm, which means that the single crystal Cu crystal grain still has more crystal boundaries, so that the conductivity, the mechanical property, the electromigration resistance and the like of the single crystal Cu crystal grain are influenced.
There is also a technique of obtaining a (100) single crystal Cu pillar or film by subjecting the produced nano twin crystal Cu pillar or film having a preferred orientation of (111) to high temperature annealing for a long time. However, semiconductor chips and devices cannot withstand long-term high-temperature annealing, and serious thermal damage can be generated; and the problems of chip and substrate warping and the like can be caused by too long annealing time; in addition, the process time is long, the process cost is increased, and the production efficiency is low. Therefore, the economy for industrial production is not high.
In summary, the existing single crystal Cu preparation method suitable for microelectronic packaging technology has the problems of complicated preparation device, large thermal damage, low quality of the prepared single crystal and the like, so that the single crystal Cu is still difficult to be applied to the microelectronic packaging technology in a large scale. Therefore, it is necessary to provide a method for preparing single crystal Cu with high efficiency and high quality with simple manufacturing equipment and little influence on chips and devices, so that the single crystal Cu can be applied to the field of microelectronic manufacturing.
Disclosure of Invention
According to the technical problems of complexity, low quality of the manufactured single crystal, large thermal damage and the like of the single crystal Cu preparation method in the existing microelectronic packaging technology, the method for quickly preparing the (100) single crystal copper is provided. The invention mainly applies an electric field in the annealing process of the (111) preferred orientation nanometer twin crystal Cu, generates stress and strain in the (111) direction nanometer twin crystal Cu under the action of current, promotes the nucleation and growth of the (100) direction crystal grain in the nanometer twin crystal Cu, and rapidly forms the (100) preferred orientation single crystal Cu. The method takes current as additional energy input, and the rate of converting (111) nano twin crystal Cu into (100) single crystal Cu is remarkably accelerated at a lower process temperature.
The technical means adopted by the invention are as follows:
a method for rapidly preparing (100) single crystal copper is characterized in that a (111) preferentially oriented nano-twin crystal Cu is provided, the nano-twin crystal Cu is annealed, a current density is directly/indirectly applied to the nano-twin crystal Cu, the nano-twin crystal Cu is kept for a certain time, crystal grains of the nano-twin crystal Cu grow rapidly and are converted into (100) preferentially oriented single crystal Cu, and finally the (111) preferentially oriented nano-twin crystal Cu is converted into the (100) preferentially oriented single crystal Cu.
Further, the method specifically comprises the following steps:
the method comprises the following steps: providing a nanometer twin crystal Cu, wherein crystal grains are columnar and have (111) preferred orientation;
step two: connecting the nano twin crystal Cu of the step one with a current source to form a complete path;
step three: heating the nanometer twin crystal Cu of the connected wire in the second step for annealing, simultaneously directly/indirectly applying a certain direct current or pulse current, and keeping constant temperature and current density for a period of time until the nanometer twin crystal Cu is completely converted into single crystal Cu; wherein, the single crystal Cu is formed by rapid growth of crystal grains in the annealing process of the nanometer twin crystal Cu and is in single (100) preferred orientation.
The single crystal Cu is formed by rapid growth of crystal grains in the annealing process of the nanometer twin crystal Cu, and under the condition of no change of other conditions, the higher the applied current density is, the higher the speed of forming the single crystal Cu by the nanometer twin crystal Cu is.
The direct/indirect current application means that the nano-twin crystal Cu can be directly connected with a current source through a lead, or the nano-twin crystal Cu is used as a UBM to form metallurgical connection with the UBM on the other side through a solder and then is connected with the current source through the lead.
Further, the current density is defined as I/S, I is the current value passing through the nano-twin Cu, and S is the sectional area of the nano-twin Cu perpendicular to the current direction.
Further, the direction of the current is parallel to, perpendicular to or at any angle with the (111) crystal plane of the nano twin crystal Cu.
Further, the current density value of the current is 1 × 103～5×105A/cm2Preferably 5X 103～105A/cm2。
Further, the atmosphere condition of the annealing process is vacuum, inert gas protection, nitrogen protection or air atmosphere.
Further, in the annealing process, the annealing temperature is 125-275 ℃, preferably 150-180 ℃ or 225-250 ℃. At a lower temperature, the thermal stress in the semiconductor device is smaller, and the problems of warping, cracking, tearing and the like caused by the thermal stress are not easy to occur; meanwhile, the atom mobility is weakened along with the reduction of the temperature, and the failure caused by the diffusion of atoms in the semiconductor device can be effectively avoided.
Furthermore, the annealing time, namely the time for keeping constant temperature and current, is 5-25 min, preferably 10-20 min, and the reduction of the annealing time can effectively reduce the thermal damage of the semiconductor device.
Further, the nano twin crystal Cu is prepared on a metal substrate or a non-metal substrate by a direct current or pulse plating method, the shape of the nano twin crystal Cu is not particularly limited, and the nano twin crystal Cu can be columnar, linear, thin film, irregular shape and the like, and the area of the nano twin crystal Cu is 1-107μm2The thickness of the film is 0.1 to 100 μm, preferablyIs selected to be 20-80 μm.
The average diameter of the nano twin Cu columnar crystal is larger than 3 mu m, the nano twin Cu columnar crystal has a high-density twin boundary, and the twin boundary distance is 1-100 nm, preferably 10-50 mu m. The nano-twin Cu substrate material may be silicon, glass, quartz, a printed circuit board, a metal, and an alloy thereof, but is not particularly limited.
Further, in the connection process in the second step, the nano-twin Cu and the lead may be connected by soldering, clamping with a metal clamp, or the like, and the connection method is not limited to the above method.
Further, the single crystal Cu is single (100) preferred orientation with an average grain size greater than 50 μm.
Compared with the prior art, the invention has the following advantages:
in the annealing process of the nanometer twin crystal Cu, an electric field is applied to the nanometer twin crystal Cu as additional energy input, a mode of applying current to promote crystal grain transformation is adopted, and the applied current can provide energy for a matrix to replace part of energy provided at high temperature, so that the process temperature is reduced and the process time is shortened under the condition of equivalent effect. When the material is subjected to a large current (the current density is more than 1 multiplied by 10)3A/cm2) During the annealing process, stress and strain are generated in the material, and the magnitude of the stress and the strain is increased along with the increase of the current density, so that on one hand, the internal energy of the material is increased, and the growth of crystal grains and the de-twinning of the crystal grains are easier to occur, thereby reducing the temperature required for transforming the nano-twin crystal Cu into the single crystal Cu in the annealing process; on the other hand, more defects such as vacancies, dislocations and the like can be generated in the material, nucleation sites are provided for new grains, and the more nucleation sites can ensure that the time for growing single crystal Cu grains and replacing all nanometer twin crystal Cu grains is shortened. It should be noted that although the larger the current applied during annealing, the stronger the effect of promoting the transformation of nano-twin Cu into single-crystal Cu, the current density cannot be increased without limitation, and when the current density is more than 5 × 105A/cm2The current density value selected by the invention is that the current-induced atom directional migration will cause the pores to appear in the microstructure of CuIs 103～5×105A/cm2。
The method provided by the invention realizes the rapid preparation of the single crystal Cu suitable for electronic packaging, and has small thermal damage to semiconductor chips and devices in the process; the production efficiency of preparing the single crystal Cu is high; the prepared single crystal Cu has preferred orientation in the (100) direction, large grain size, good mechanical property, oxidation resistance, electromigration resistance, thermal stability and the like; when the prepared single crystal Cu reacts with the brazing filler metal, the preferred orientation of intermetallic compounds can be regulated and controlled, and the generation of Cokendall holes can be inhibited.
In conclusion, the method provided by the invention overcomes the defects of large thermal damage, low single crystal quality, poor economy and the like in the prior art, so that the single crystal Cu can be quickly prepared at a lower process temperature, and the method is very suitable for preparing the under bump metallization layer, the heavy wiring layer, the chip interconnection line or the wire and the like made of the single crystal Cu material.
The method is simple, efficient, low in cost, good in compatibility with the existing microelectronic packaging process and very suitable for large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 shows the results of X-ray diffraction (XRD) detection of nano-twin Cu used in examples 1 and 2 of the present invention.
Fig. 2 is a photograph of back scattered electron diffraction (EBSD) of nano-twin Cu used in examples 1 and 2 of the present invention.
FIG. 3 is a schematic view of embodiment 1 of the present invention.
Fig. 4 is a schematic view of embodiment 2 of the present invention.
FIG. 5 is a photograph of single-crystal Cu obtained in example 1 of the present invention after argon ion etching.
FIG. 6 is an EBSD photograph of single-crystal Cu obtained in example 1 of the present invention.
FIG. 7 shows XRD detection results of single crystal Cu obtained in example 2 of the present invention.
FIG. 8 is an EBSD photograph of single crystal Cu obtained in example 2 of the present invention.
FIG. 9 is a photograph of single crystal Cu obtained in example 2 of the present invention after Focused Ion Beam (FIB) etching.
FIG. 10 is an XRD detection result of nano twin crystal Cu after annealing obtained by a comparative example.
Fig. 11 is an EBSD photograph of nano-twin Cu obtained by the comparative example after annealing.
In the figure: 10. a substrate; 20. (111) preferentially orienting nano twin crystal Cu; 30. solder bumps; 40. an Under Bump Metallization (UBM).
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
Example 1
As shown in fig. 3, a method for rapidly preparing (100) single crystal copper according to the present invention can be realized by the following specific process steps:
the method comprises the following steps: a nano twin crystal Cu 20 (shown in FIG. 1 and FIG. 2) is provided, which has a high density twin boundary, a columnar crystal grain with a (111) preferred orientation, and a columnar crystal average diameter of 8 μm. The nano-twin crystal Cu is prepared on a substrate 10 by a direct current or pulse plating method, and the substrate is rolled polycrystalline Cu. The thickness of the nano twin crystal Cu is 30 μm.
Step two: and (3) taking the nano twin crystal Cu as the UBM in the step one, forming metallurgical connection with the UBM40 on the other side by using the brazing filler metal 30 to form a combination, and connecting the combination with a current source to form a complete path.
Step three: heating the assembly in the second step to 225 ℃, and simultaneously applying direct current to the nano-twin crystal Cu to ensure that the current density passing through the nano-twin crystal Cu is 1 multiplied by 104A/cm2And the direction of current flow is perpendicular toThe surface of the nano-twin crystal Cu, namely the (111) plane vertical to the nano-twin crystal Cu, is kept at the temperature and the current density for 15min, and the nano-twin crystal Cu is completely converted into the single crystal Cu.
As shown in fig. 5 and 6, the single crystal Cu formed is (100) preferred orientation with a grain size >50 μm.
Example 2
As shown in fig. 4, a method for rapidly preparing (100) single crystal copper according to the present invention can be realized by the following specific process steps:
the method comprises the following steps: a nano twin crystal Cu 20 is provided, which has a high density twin boundary, a columnar crystal grain with a preferred orientation of (111), and a columnar crystal average diameter of 8 μm. The nanometer twin crystal Cu is prepared on the substrate 10 by a direct current or pulse plating method, and the shape of the nanometer twin crystal Cu is strip-shaped. The thickness of the nano twin crystal Cu is 30 μm.
Step two: and (3) connecting the nano twin crystal Cu in the step one with a current source to form a complete path.
Step three: heating the nanometer twin crystal Cu of the connected wire in the second step to 160 ℃, and simultaneously applying pulse current T to the nanometer twin crystal Cuon/Toff1, 200 Hz, and the current density passing through the nanometer twin crystal Cu is 1 multiplied by 105A/cm2And the current direction is parallel to the surface of the nano-twin crystal Cu, namely parallel to the (111) surface of the nano-twin crystal Cu, the constant temperature and the constant current density are kept for 15min, and the nano-twin crystal Cu is completely converted into the single crystal Cu.
As shown in fig. 7, 8 and 9, the single crystal Cu formed is (100) preferred orientation with a grain size >50 μm.
Comparative example
In this comparative example, no current was applied to the nano-twin Cu, i.e., annealing was performed by heating only at an annealing temperature of 300 ℃, for an annealing time of 1 hour, and other steps, materials, process conditions, etc. were the same as in example 2, and as a result, (111) the preferentially oriented nano-twin Cu was not converted into (100) single-crystal Cu, as shown in fig. 10 and 11.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for rapidly preparing (100) single crystal copper is characterized in that a (111) preferentially oriented nano-twin crystal Cu is provided, annealing is carried out on the nano-twin crystal Cu, a current is directly/indirectly applied to the nano-twin crystal Cu and is kept for a certain time, crystal grains of the nano-twin crystal Cu grow rapidly and are converted into (100) preferentially oriented single crystal Cu, and finally the (111) preferentially oriented nano-twin crystal Cu is converted into the (100) preferentially oriented single crystal Cu.
2. The method for the rapid production (100) of single-crystal copper according to claim 1, characterized in that it comprises in particular the following steps:
the method comprises the following steps: providing a nanometer twin crystal Cu, wherein crystal grains are columnar and have (111) preferred orientation;
step two: connecting the nano twin crystal Cu of the step one with a current source to form a complete path;
step three: and (2) heating the nano-twin crystal Cu of the connected wire in the step two for annealing, simultaneously directly/indirectly applying a certain direct current or pulse current, and keeping constant temperature and current density for a period of time until the nano-twin crystal Cu is completely converted into single crystal Cu, wherein the single crystal Cu is formed by rapid growth of crystal grains in the annealing process of the nano-twin crystal Cu and has single (100) preferred orientation.
3. The method for rapidly preparing (100) single-crystal copper according to claim 1 or 2, wherein the current density is defined as I/S, I is a current value passing through the nano-twin Cu, and S is a sectional area of the nano-twin Cu perpendicular to a current direction.
4. The method for rapidly preparing (100) single crystal copper according to claim 3, wherein the current direction is parallel to, perpendicular to or at any angle with respect to the (111) crystal plane of the nano twin crystal Cu.
5. The method for rapid production (100) of single-crystal copper according to claim 4, characterized in that the current density value of the current is 1 x 103～5×105A/cm2。
6. The method for rapid production (100) of single-crystal copper according to claim 1 or 2, characterized in that the annealing process atmosphere conditions are vacuum, inert gas blanket, nitrogen blanket or air atmosphere.
7. The method for rapidly preparing (100) single crystal copper according to claim 6, wherein the annealing temperature is 125-275 ℃ during the annealing process.
8. The method for rapid production (100) of single-crystal copper according to claim 7, wherein the annealing time, that is, the time for maintaining the constant temperature and current density, is 5 to 25 min.
9. The method for rapidly preparing (100) single crystal copper according to claim 1 or 2, wherein the nano twin crystal Cu is prepared on a metal substrate or a non-metal substrate by a direct current or pulse plating method, and the area of the nano twin crystal Cu is 1-10%7μm2The thickness is 0.1 to 100 μm; the average diameter of the nano twin Cu columnar crystal is larger than 3 mu m, the nano twin Cu columnar crystal has a high-density twin boundary, and the twin boundary spacing is 1-100 nm.
10. The method for rapid production (100) of single-crystal copper according to claim 1 or 2, characterized in that the single-crystal Cu has a single (100) preferred orientation with an average grain size of more than 50 μ ι η.
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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

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