CN113652654B - Deformation-resistant oxygen-free copper backboard and preparation method thereof - Google Patents

Deformation-resistant oxygen-free copper backboard and preparation method thereof Download PDF

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Publication number
CN113652654B
CN113652654B CN202110919594.6A CN202110919594A CN113652654B CN 113652654 B CN113652654 B CN 113652654B CN 202110919594 A CN202110919594 A CN 202110919594A CN 113652654 B CN113652654 B CN 113652654B
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deformation
backboard
copper
preparation
copper ingot
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CN113652654A (en
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姚力军
潘杰
边逸军
王学泽
周敏
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002—Hybrid process, e.g. forging following casting
    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Forging (AREA)

Abstract

The invention provides a deformation-resistant oxygen-free copper backboard and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Preheating a copper ingot, and forging for at least 2 times, wherein the forging ratio is 1-3; (2) Cooling the copper ingot obtained in the step (1) after the first heat treatment; (3) rolling the copper ingot obtained in the step (2); (4) And (3) performing second heat treatment on the copper ingot obtained in the step (3) and then cooling to obtain the deformation-resistant oxygen-free copper backboard. The preparation method provided by the invention is particularly suitable for manufacturing the oxygen-free copper backboard, improves the deformation resistance and the dimensional accuracy of the backboard, and avoids the abnormal installation phenomenon.

Description

Deformation-resistant oxygen-free copper backboard and preparation method thereof
Technical Field
The invention belongs to the technical field of sputtering targets, relates to a backboard, and particularly relates to an anti-deformation oxygen-free copper backboard and a preparation method thereof.
Background
The quality of the sputter target is critical to semiconductor fabrication. Along with continuous innovation of chip design and development and continuous reduction of chip wiring width, the requirements of high-quality chips on uniformity, impurities and defects of the coating film are higher and higher. In order to meet the strict requirements of coating quality, the performance requirements of the sputtering target are correspondingly improved, and the sputtering target specifically comprises the microstructure, the component purity, the size strength, the installation matching degree and the like of the target.
In the semiconductor industry, most target assemblies consist of various high purity metal targets meeting sputtering performance requirements and backing plates with a certain supporting effect. The backboard not only plays a supporting role, but also has the effect of heat conduction. At present, the combination between the target and the backboard is mainly realized through welding, but in the welding process, the oxygen-free copper backboard is extremely easy to be subjected to thermal expansion deformation, so that dimensional deviation and abnormal installation are caused.
CN 111197148A discloses a method for manufacturing a target, which comprises the following steps: providing a copper-aluminum alloy ingot; performing a first forging process on the material ingot at least twice; after each first forging treatment, carrying out a first heat treatment process on the material ingot; calendering the forged and heat-treated material ingot; and carrying out a hot working process on the rolled material ingot. The grain structure in the material ingot is fine through a repeated forging process and a heat treatment process, so that the toughness of the material is greatly enhanced, the material ingot is rolled to ensure that the internal structure of the material ingot is uniform and reaches the thickness of a required target, then the copper-aluminum alloy target is manufactured through the heat treatment process, and the size of the internal grain size of the target is regulated through the heat treatment process parameters. However, the manufacturing process provided by the invention is only suitable for the target material, and cannot be sleeved in the manufacturing process of the backboard.
Therefore, how to provide a method for manufacturing the backboard is particularly suitable for the oxygen-free copper backboard, improves the deformation resistance and the dimensional accuracy of the backboard, avoids the abnormal installation phenomenon, and becomes the problem which needs to be solved by the current technicians in the field.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the deformation-resistant oxygen-free copper backboard and the preparation method thereof, and the preparation method is particularly suitable for manufacturing the oxygen-free copper backboard, so that the deformation resistance and the dimensional accuracy of the backboard are improved, and the abnormal installation phenomenon is avoided.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an anti-deformation oxygen-free copper back plate, the method comprising the steps of:
(1) Preheating a copper ingot, and forging for at least 2 times, wherein the forging ratio is 1-3;
(2) Cooling the copper ingot obtained in the step (1) after the first heat treatment;
(3) Calendering the copper ingot obtained in the step (2);
(4) And (3) performing second heat treatment on the copper ingot obtained in the step (3) and then cooling to obtain the deformation-resistant oxygen-free copper backboard.
According to the preparation method provided by the invention, the preheated copper ingot is forged for at least 2 times, the forging ratio is strictly controlled to be 1-3, so that original grains in the copper ingot are destroyed, and coarse grains are forged into fine and uniform grains. In addition, some brittle impurities in the copper ingot are crushed, and plastic impurities are gradually elongated along with the deformation of the material to form a fiber structure, so that the toughness of the material is greatly enhanced, and the subsequent heat treatment and calendaring of the copper ingot are facilitated. The rolling treatment ensures that the grains in the copper ingot are finer and more uniform; the heat treatment fully releases the stress in the crystal grains, so that the stability of the size and the state of the crystal grains is improved, the deformation resistance and the size precision of the backboard are further improved, and the abnormal installation phenomenon is avoided.
In the present invention, the copper ingot in step (1) is forged at least 2 times, for example, 2 times, 3 times, 4 times or 5 times, but the present invention is not limited to the recited values, and other non-recited values within the range are equally applicable.
In the present invention, the forging ratio in the step (1) is 1 to 3, and may be, for example, 1, 1.2, 1.4, 1.6, 1.8, 2, 2.2, 2.4, 2.6, 2.8 or 3, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In the invention, the forging ratio specifically refers to the ratio of the cross-sectional areas of the copper ingot before and after each forging deformation, and the ratio needs to be kept within a reasonable range. When the forging ratio is more than 3, excessive fiber tissues can be formed in the copper ingot, so that the plasticity index of the transverse mechanical property is rapidly reduced, and the obtained backboard is anisotropic; when the forging ratio is less than 1, the original crystal grains in the copper ingot cannot be effectively destroyed, and the obtained backboard cannot meet the performance requirement.
Preferably, the preheating of step (1) is performed in a resistive heating furnace.
The preheating in step (1) is preferably carried out at a temperature of 400 to 600 ℃, and may be, for example, 400 ℃, 420 ℃, 440 ℃, 460 ℃, 480 ℃, 500 ℃, 520 ℃, 540 ℃, 560 ℃, 580 ℃, or 600 ℃, but is not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the preheating time in the step (1) is 5-30min, for example, may be 5min, 6min, 8min, 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min or 30min, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, step (1) is performed for 2 forging times.
Preferably, the forging ratio in step (1) is 1.5-2.5, and may be, for example, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4 or 2.5, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the temperature of the first heat treatment in the step (2) is 200 to 500 ℃, for example, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, 450 ℃ or 500 ℃, but the temperature is not limited to the listed values, and other values not listed in the range of the values are equally applicable.
Preferably, the time of the first heat treatment in the step (2) is 60-180min, for example, 60min, 80min, 100min, 120min, 140min, 160min or 180min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the deformation of the rolling in the step (3) is 60% -85%, for example, 60%, 62%, 64%, 66%, 68%, 70%, 72%, 74%, 76%, 78%, 80%, 82%, 84% or 85%, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the temperature of the second heat treatment in the step (4) is 200 to 400 ℃, for example, 200 ℃, 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃, 320 ℃, 340 ℃, 360 ℃, 380 ℃ or 400 ℃, but not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the time of the second heat treatment in the step (4) is 120-240min, for example, 120min, 130min, 140min, 150min, 160min, 170min, 180min, 190min, 200min, 210min, 220min, 230min or 240min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the cooling manners in the step (2) and the step (4) are respectively and independently water cooling or air cooling.
Preferably, the cooling manners in the step (2) and the step (4) are respectively and independently water-cooling.
As a preferred technical solution of the first aspect of the present invention, the preparation method includes the following steps:
(1) Preheating a copper ingot in a resistance heating furnace at 400-600 ℃ for 5-30min, and forging for 2 times with the forging ratio of 1.5-2.5;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 200-500 ℃ for 60-180min, and then carrying out water cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 60% -85%;
(4) And (3) performing a second heat treatment on the copper ingot obtained in the step (3) at 200-400 ℃ for 120-240min, and then performing water cooling to obtain the deformation-resistant oxygen-free copper backboard.
In a second aspect, the present invention provides a deformation-resistant oxygen-free copper backsheet prepared by the preparation method according to the first aspect.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method provided by the invention, the preheated copper ingot is forged for at least 2 times, the forging ratio is strictly controlled to be 1-3, so that original grains in the copper ingot are destroyed, and coarse grains are forged into fine and uniform grains. In addition, some brittle impurities in the copper ingot are crushed, and plastic impurities are gradually elongated along with the deformation of the material to form a fiber structure, so that the toughness of the material is greatly enhanced, and the subsequent heat treatment and calendaring of the copper ingot are facilitated. The rolling treatment ensures that the grains in the copper ingot are finer and more uniform; the heat treatment fully releases the stress in the crystal grains, so that the stability of the size and the state of the crystal grains is improved, the deformation resistance and the size precision of the backboard are further improved, and the abnormal installation phenomenon is avoided.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments.
Example 1
The embodiment provides a deformation-resistant oxygen-free copper back plate and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Preheating a copper ingot in a resistance heating furnace at 500 ℃ for 20min, and forging for 2 times, wherein the forging ratio is 2;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 350 ℃ for 120min, and then carrying out water cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 75%;
(4) And (3) performing a second heat treatment on the copper ingot obtained in the step (3) at 300 ℃ for 180min, and then performing water cooling to obtain the deformation-resistant oxygen-free copper backboard.
The backboard obtained by the embodiment is used for welding the target assembly, and in the welding process, the backboard is not deformed due to thermal expansion, so that the deformation resistance and the dimensional accuracy of the backboard are improved, and the subsequent abnormal installation phenomenon is avoided.
Example 2
The embodiment provides a deformation-resistant oxygen-free copper back plate and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Preheating a copper ingot in a resistance heating furnace for 30min at 400 ℃, and forging for 2 times, wherein the forging ratio is 1.5;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 200 ℃ for 180min, and then carrying out water cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 60%;
(4) And (3) carrying out second heat treatment on the copper ingot obtained in the step (3) at 200 ℃ for 240min, and then carrying out water cooling to obtain the deformation-resistant oxygen-free copper backboard.
The backboard obtained by the embodiment is used for welding the target assembly, and in the welding process, the backboard is not deformed due to thermal expansion, so that the deformation resistance and the dimensional accuracy of the backboard are improved, and the subsequent abnormal installation phenomenon is avoided.
Example 3
The embodiment provides a deformation-resistant oxygen-free copper back plate and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Preheating a copper ingot in a resistance heating furnace for 5min at 600 ℃, and forging for 3 times, wherein the forging ratio is 2.5;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 500 ℃ for 60min, and then carrying out air cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 85%;
(4) And (3) performing a second heat treatment on the copper ingot obtained in the step (3) at 400 ℃ for 120min, and then performing air cooling to obtain the deformation-resistant oxygen-free copper backboard.
The backboard obtained by the embodiment is used for welding the target assembly, and in the welding process, the backboard is not deformed due to thermal expansion, so that the deformation resistance and the dimensional accuracy of the backboard are improved, and the subsequent abnormal installation phenomenon is avoided.
Example 4
The embodiment provides a deformation-resistant oxygen-free copper back plate and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Preheating a copper ingot in a resistance heating furnace at 500 ℃ for 20min, and then forging for 2 times, wherein the forging ratio is 1;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 350 ℃ for 120min, and then carrying out water cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 75%;
(4) And (3) performing a second heat treatment on the copper ingot obtained in the step (3) at 300 ℃ for 180min, and then performing water cooling to obtain the deformation-resistant oxygen-free copper backboard.
The backboard obtained by the embodiment is used for welding the target assembly, and in the welding process, the backboard is not deformed due to thermal expansion, so that the deformation resistance and the dimensional accuracy of the backboard are improved, and the subsequent abnormal installation phenomenon is avoided.
Example 5
The embodiment provides a deformation-resistant oxygen-free copper back plate and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Preheating a copper ingot in a resistance heating furnace at 500 ℃ for 20min, and forging for 2 times, wherein the forging ratio is 3;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 350 ℃ for 120min, and then carrying out water cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 75%;
(4) And (3) performing a second heat treatment on the copper ingot obtained in the step (3) at 300 ℃ for 180min, and then performing water cooling to obtain the deformation-resistant oxygen-free copper backboard.
The backboard obtained by the embodiment is used for welding the target assembly, and in the welding process, the backboard is not deformed due to thermal expansion, so that the deformation resistance and the dimensional accuracy of the backboard are improved, and the subsequent abnormal installation phenomenon is avoided.
Comparative example 1
The comparative example provides an oxygen-free copper back plate and a preparation method thereof, wherein the preparation method is the same as that of example 1 except that the copper ingot in step (1) is changed to 1 forging, so that the description thereof is omitted.
Compared with example 1, the back plate obtained in this comparative example has slight thermal expansion deformation phenomenon during the welding process with the target, and it is seen that too low forging times can result in reduced deformation resistance and dimensional accuracy of the obtained back plate.
Comparative example 2
The comparative example provides an oxygen-free copper back plate and a preparation method thereof, wherein the forging ratio in the step (1) is changed to 0.8, and other conditions are the same as those in the example 1, so that the description thereof is omitted.
Compared with example 1, the backboard obtained in the comparative example has obvious thermal expansion deformation phenomenon in the welding process with the target, and the too low forging ratio can cause the reduction of the deformation resistance and the dimensional accuracy of the backboard.
Comparative example 3
The comparative example provides an oxygen-free copper back plate and a preparation method thereof, wherein the forging ratio in the step (1) is changed to 3.5, and the other conditions are the same as those in the embodiment 1, so that the description thereof is omitted.
Compared with example 1, the backboard obtained in the comparative example has obvious thermal expansion deformation phenomenon in the welding process with the target, and the excessively high forging ratio can cause the reduction of the deformation resistance and the dimensional accuracy of the backboard.
Therefore, the preparation method provided by the invention forges the preheated copper ingot for at least 2 times, and strictly controls the forging ratio to be 1-3, so that the original crystal grains in the copper ingot are destroyed, and coarse crystal grains are forged into fine and uniform crystal grains. In addition, some brittle impurities in the copper ingot are crushed, and plastic impurities are gradually elongated along with the deformation of the material to form a fiber structure, so that the toughness of the material is greatly enhanced, and the subsequent heat treatment and calendaring of the copper ingot are facilitated. The rolling treatment ensures that the grains in the copper ingot are finer and more uniform; the heat treatment fully releases the stress in the crystal grains, so that the stability of the size and the state of the crystal grains is improved, the deformation resistance and the size precision of the backboard are further improved, and the abnormal installation phenomenon is avoided.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.

Claims (2)

1. The preparation method of the deformation-resistant oxygen-free copper backboard is characterized by comprising the following steps of:
(1) Preheating a copper ingot in a resistance heating furnace at 400-600 ℃ for 5-30min, and forging for 2 times with the forging ratio of 1.5-2.5;
(2) Carrying out first heat treatment on the copper ingot obtained in the step (1) at 200-500 ℃ for 60-180min, and then carrying out water cooling;
(3) Rolling the copper ingot obtained in the step (2), wherein the rolling deformation is 60% -85%;
(4) And (3) performing a second heat treatment on the copper ingot obtained in the step (3) at 200-400 ℃ for 120-240min, and then performing water cooling to obtain the deformation-resistant oxygen-free copper backboard.
2. A deformation-resistant oxygen-free copper backsheet prepared by the method of claim 1.
CN202110919594.6A 2021-08-11 2021-08-11 Deformation-resistant oxygen-free copper backboard and preparation method thereof Active CN113652654B (en)

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CN114043180A (en) * 2021-12-15 2022-02-15 宁波江丰电子材料股份有限公司 Preparation method of semiconductor high-purity titanium target material assembly
CN117230393A (en) * 2023-09-15 2023-12-15 宁波江丰电子材料股份有限公司 Preparation method of oxygen-free copper backboard

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103510055A (en) * 2012-06-27 2014-01-15 宁波江丰电子材料有限公司 Preparation method of high-purity copper target material
CN111197148A (en) * 2018-11-20 2020-05-26 宁波江丰电子材料股份有限公司 Method for manufacturing target material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103510055A (en) * 2012-06-27 2014-01-15 宁波江丰电子材料有限公司 Preparation method of high-purity copper target material
CN111197148A (en) * 2018-11-20 2020-05-26 宁波江丰电子材料股份有限公司 Method for manufacturing target material

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