CN114589212B - Hot extrusion forming method for ultra-high purity copper target - Google Patents
Hot extrusion forming method for ultra-high purity copper target Download PDFInfo
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- CN114589212B CN114589212B CN202210280060.8A CN202210280060A CN114589212B CN 114589212 B CN114589212 B CN 114589212B CN 202210280060 A CN202210280060 A CN 202210280060A CN 114589212 B CN114589212 B CN 114589212B
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- purity copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 72
- 239000010949 copper Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000001192 hot extrusion Methods 0.000 title claims abstract description 33
- 238000001125 extrusion Methods 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000000465 moulding Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000011282 treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000003064 anti-oxidating effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000110 cooling liquid Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000013077 target material Substances 0.000 description 10
- 229910000881 Cu alloy Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000002265 prevention Effects 0.000 description 5
- 238000000137 annealing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000009718 spray deposition Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C25/00—Profiling tools for metal extruding
- B21C25/02—Dies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C23/00—Extruding metal; Impact extrusion
- B21C23/02—Making uncoated products
- B21C23/04—Making uncoated products by direct extrusion
- B21C23/14—Making other products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C29/00—Cooling or heating work or parts of the extrusion press; Gas treatment of work
- B21C29/003—Cooling or heating of work
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a hot extrusion molding method of an ultra-high purity copper target, which comprises the following steps: heating the ultra-high-purity copper rod to 750-850 ℃, and then sequentially performing hot extrusion and cooling to obtain an ultra-high-purity copper target; the extrusion die for hot extrusion is a five-stage stepped expansion deformation channel; the heating temperature of the extrusion die is 650-700 ℃; the expansion thickness of each stage of the five-stage stepped expansion deformation channel is the same. According to the invention, the copper target is manufactured through one-time hot extrusion molding, and the designed extrusion die enables the copper plate blank to deform more uniformly, so that the grain size distribution is more uniform, and the molding is facilitated; the method has the advantages of low cost, simple process and high efficiency, the grain size of the prepared copper plate blank is 20-30 mu m, and the grains are uniform.
Description
Technical Field
The invention belongs to extrusion molding technology, and particularly relates to a hot extrusion molding method for an ultra-high purity copper target.
Background
The thin film transistor liquid crystal display has the characteristics of light weight, flattening, low power consumption, no radiation, excellent display quality and the like, and is widely applied to industries of liquid product screens, liquid product televisions and the like. With the increasing development of very large scale integrated circuits, the chip size for semiconductors has been reduced to the nanometer level, the RC delay and electromigration phenomenon of metal interconnect lines become main factors affecting the performance of the chip, and conventional aluminum and aluminum alloy interconnect lines have not been able to meet the requirements of the process of the very large scale integrated circuits. Compared with aluminum, high-purity copper and copper alloy are used as interconnection line materials due to high electromigration resistance and low resistance, and have important significance for reducing the resistance of chip interconnection lines and improving the operation speed of the chip interconnection lines. Accordingly, high-purity copper targets for sputtering used for copper film formation have been studied.
CN110578126B discloses a preparation method of a multi-specification high-purity copper target, which comprises the following steps: heating the high-purity copper ingot blank to 700-950 ℃; then carrying out multi-pass hot rolling on the heated high-purity copper ingot, and cooling to room temperature; leveling the cooled copper target blank by adopting a leveling machine; cutting the leveled copper target blank according to the requirement, and then sequentially carrying out rough machining and finish machining to obtain the high-purity copper target material. The preparation method adopts multiple hot rolling treatments to control the crystal grains, and has high cost.
CN110318024B discloses a preparation method of silver-copper alloy target, which comprises the following steps: smelting copper and silver in a protective atmosphere to obtain a liquid alloy; performing spray deposition treatment on the obtained liquid alloy to obtain a silver-copper alloy cast ingot; then sequentially carrying out homogenizing annealing, ECAP extrusion, low-temperature annealing, upsetting deformation and rolling treatment to obtain a silver-copper alloy coarse ingot; and carrying out recrystallization annealing treatment on the obtained silver-copper alloy coarse ingot to obtain the silver-copper alloy target. The preparation method adopts the traditional copper target preparation method, mainly adopts a metallurgical method to prepare an ultra-high purity copper cast ingot by vacuum smelting, and then adopts upsetting and rolling to carry out plastic deformation on the ultra-high purity copper cast ingot, and the preparation method has relatively complicated working procedures, long manufacturing period and higher manufacturing cost.
Therefore, there is a need to develop a method for preparing ultra-high purity copper targets with low cost, relatively simple manufacturing process and easy industrial production,
disclosure of Invention
The invention aims to provide a hot extrusion molding method for an ultra-high purity copper target, which is characterized in that the copper target is manufactured through one-time hot extrusion molding, and a designed extrusion die enables copper plate blanks to deform more uniformly, and the grain size distribution is more uniform, so that the molding is facilitated; the method has the advantages of low cost, simple process and high efficiency.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the invention provides a hot extrusion molding method of an ultra-high purity copper target, which comprises the following steps: and heating the ultra-high-purity copper rod to 750-850 ℃, and then sequentially performing hot extrusion and cooling to obtain the ultra-high-purity copper target.
In the present invention, the ultra-high purity copper rod may be heated at a temperature of 750 to 850 ℃, for example, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, 800 ℃, 810 ℃, 820 ℃, 830 ℃, 840 ℃, 850 ℃ or the like, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are applicable.
In the present invention, the ultra-high purity means that the purity is 99.9999% or more.
The method for hot extrusion molding of the ultra-high purity copper target material prepares the copper target material through one-time hot extrusion molding, has low cost, simple process and high efficiency, and the copper target material molded by the method has fine and uniform crystal grains and has no defect of internal tissues of a copper plate blank molded by extrusion.
In a preferred embodiment of the present invention, the diameter of the ultra-high purity copper rod is 10 to 20mm, for example, 10mm, 11mm, 12mm, 13mm, 14mm, 15mm, 16mm, 17mm, 18mm, 19mm, or 20mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
As a preferable technical scheme of the invention, the speed of the hot extrusion is 220-380mm/min, for example, 220mm/min, 240mm/min, 260mm/min, 280mm/min, 300mm/min, 320mm/min, 340mm/min, 360mm/min or 380mm/min and the like, but the hot extrusion is not limited to the listed values, and other non-listed values in the numerical range are applicable.
In the invention, the hot extrusion is carried out by adopting a 3000-ton hot extruder.
Preferably, the cooling temperature is 20 to 30 ℃, for example, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ or 30 ℃, etc., but not limited to the recited values, other non-recited values within the range of values are equally applicable.
Preferably, the cooling liquid used for cooling is a mixed liquid of industrial alcohol and water.
Preferably, the concentration of the industrial alcohol is 5-10%, for example, 5%, 6%, 7%, 8%, 9% or 10%, etc., but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
As a preferable technical scheme of the invention, an anti-oxidation treatment is further included between the hot extrusion and the cooling.
Preferably, the oxidation prevention treatment is to pass the hot extruded ultra-high purity copper slab through a vacuum oxidation prevention device.
As a preferable technical scheme of the invention, the extrusion die for hot extrusion is a five-stage stepped expansion deformation channel.
The heating temperature of the extrusion die is preferably 650 to 700 ℃, and may be, for example, 650 ℃, 655 ℃, 660 ℃, 665 ℃, 670 ℃, 675 ℃, 680 ℃, 685 ℃, 690 ℃, 695 ℃, 700 ℃, or the like, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the expansion thickness of each stage of the five-stage stepped expansion deformation channel is the same.
According to the invention, the extrusion die is a five-stage stepped expansion deformation channel, so that the purity of the material is not polluted, the full thermoplastic deformation of the copper rod is facilitated, each stage of deformation channel can ensure the full dynamic recrystallization of the material, the prepared target material has fine and uniform crystal grains, the expansion thickness of each stage is the same, the deformation of the copper plate blank is more uniform, the grain size distribution is more uniform, and the forming is facilitated.
As a preferable technical scheme of the invention, the expansion angle of the first-stage expansion deformation channel of the five-stage stepped expansion deformation channel is 30-40 degrees, the expansion height is 10-15mm, the expansion width is 20-30mm, and the expansion thickness is 30-40mm.
In the present invention, the expansion angle of the first-stage expansion deformation channel is 30 ° to 40 °, for example, 30 °, 31 °, 32 °, 33 °, 34 °, 35 °, 36 °, 37 °, 38 °, 39 °, or 40 °, etc., but the expansion angle is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
In the present invention, the expansion height of the first-stage expansion deformation channel is 10-15mm, for example, 10mm, 11mm, 12mm, 13mm, 14mm or 15mm, etc., but the expansion height is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion width of the first-stage expansion deformation channel is 20-30mm, for example, 20mm, 21mm, 22mm, 23mm, 24mm, 25mm, 26mm, 27mm, 28mm, 29mm or 30mm, etc., but the expansion width is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion thickness of the first-stage expansion deformation channel is 30-40mm, for example, 30mm, 31mm, 32mm, 33mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm or 40mm, etc., but the expansion thickness is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
As a preferable technical scheme of the invention, the expansion angle of the second-stage expansion deformation channel of the five-stage stepped expansion deformation channel is 95-105 degrees, the expansion height is 10-20mm, the expansion width is 80-100mm, and the expansion thickness is 30-40mm.
In the present invention, the expansion angle of the second-stage expansion deformation channel is 95 to 105 °, for example, 95 °, 96 °, 97 °, 98 °, 99 °, 100 °, 101 °, 102 °, 103 °, 104 ° or 105 °, etc., but the present invention is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
In the present invention, the expansion height of the second-stage expansion deformation channel is 10-20mm, for example, 10mm, 11mm, 12mm, 13mm, 14mm, 15mm, 16mm, 17mm, 18mm, 19mm or 20mm, etc., but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion width of the second-stage expansion deformation channel is 80-100mm, for example, 80mm, 82mm, 84mm, 86mm, 88mm, 90mm, 92mm, 94mm, 96mm, 98mm or 100mm, etc., but the expansion width is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion thickness of the second-stage expansion deformation channel is 30-40mm, for example, 30mm, 31mm, 32mm, 33mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm or 40mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
As a preferable technical scheme of the invention, the expansion angle of the third-stage expansion deformation channel of the five-stage stepped expansion deformation channel is 150-160 degrees, the expansion height is 10-20mm, the expansion width is 180-230mm, and the expansion thickness is 30-40mm.
In the present invention, the expansion angle of the third-stage expansion deformation channel is 150 ° to 160 °, for example, 150 °, 151 °, 152 °, 153 °, 154 °, 155 °, 156 °, 157 °, 158 °, 159 °, or 160 °, etc., but the present invention is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
In the present invention, the expansion height of the third-stage expansion deformation channel is 10 to 20mm, for example, 10mm, 11mm, 12mm, 13mm, 14mm, 15mm, 16mm, 17mm, 18mm, 19mm or 20mm, etc., but the expansion height is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion width of the third stage expansion deformation channel is 180-230mm, for example, 180mm, 185mm, 190mm, 195mm, 200mm, 205mm, 210mm, 215mm, 220mm, 225mm or 230mm, etc., but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion thickness of the third-stage expansion deformation channel is 30-40mm, for example, 30mm, 31mm, 32mm, 33mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm or 40mm, etc., but the expansion thickness is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
As a preferable technical scheme of the invention, the expansion angle of the fourth-stage expansion deformation channel of the five-stage stepped expansion deformation channel is 155-165 degrees, the expansion height is 10-20mm, the expansion width is 350-400mm, and the expansion thickness is 30-40mm.
In the present invention, the expansion angle of the fourth-stage expansion deformation channel is 155 to 165 °, for example, 155 °, 156 °, 157 °, 158 °, 159 °, 160 °, 161 °, 162 °, 163 °, 164 °, 165 °, or the like, but the present invention is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
In the present invention, the expansion height of the fourth-stage expansion deformation channel is 10-20mm, for example, 10mm, 11mm, 12mm, 13mm, 14mm, 15mm, 16mm, 17mm, 18mm, 19mm or 20mm, etc., but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In the present invention, the expansion width of the fourth-stage expansion deformation channel is 350-400mm, for example, 350mm, 355mm, 360mm, 365mm, 370mm, 375mm, 380mm, 385mm, 390mm, 395mm or 400mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
In the present invention, the expansion thickness of the fourth-stage expansion deformation channel is 30-40mm, for example, 30mm, 31mm, 32mm, 33mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm or 40mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
As a preferable technical scheme of the invention, the expansion angle of the fifth-stage expansion deformation channel of the fifth-stage stepped expansion deformation channel is 100-110 degrees, the expansion height is 25-35mm, the expansion width is 400-480mm, and the expansion thickness is 30-40mm.
In the present invention, the expansion angle of the fifth-stage expansion deformation channel is 100 ° to 110 °, for example, 100 °, 101 °, 102 °, 103 °, 104 °, 105 °, 106 °, 107 °, 108 °, 109 ° or 110 °, etc., but the present invention is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
In the present invention, the expansion height of the fifth-stage expansion deformation channel is 25-35mm, for example, 25mm, 26mm, 27mm, 28mm, 29mm, 30mm, 31mm, 32mm, 33mm, 34mm or 35mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
In the present invention, the expansion width of the fifth stage expansion deformation channel is 400-480mm, for example, 400mm, 410mm, 420mm, 430mm, 440mm, 450mm, 460mm, 470mm or 480mm, etc., but the present invention is not limited to the recited values, and other non-recited values in the numerical range are equally applicable.
In the present invention, the expansion thickness of the fifth-stage expansion deformation channel is 30-40mm, for example, 30mm, 31mm, 32mm, 33mm, 34mm, 35mm, 36mm, 37mm, 38mm, 39mm or 40mm, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the following beneficial effects:
according to the hot extrusion molding method of the ultra-high purity copper target, the copper target is manufactured through one-time hot extrusion molding, and the designed extrusion die enables copper plate blanks to be deformed more uniformly, and the grain size distribution is more uniform, so that the molding is facilitated; the method has the advantages of low cost, simple process and high efficiency, the grain size of the prepared copper plate blank is 20-30 mu m, and the grains are uniform.
Drawings
FIG. 1 is a cross-sectional view of an extrusion die for hot extrusion;
wherein, the expansion angle of A1-first level, the expansion height of H1-first level, the expansion width of W1-first level, the expansion thickness of T1-first level, the expansion angle of A2-second level, the expansion height of H2-second level, the expansion width of W2-second level, the expansion thickness of T2-second level, the expansion angle of A3-third level, the expansion height of H3-third level, the expansion width of W3-third level, the expansion thickness of T3-third level, the expansion angle of A4-fourth level, the expansion height of H4-fourth level, the expansion width of W4-fourth level, the expansion thickness of T4-fourth level, the expansion angle of A5-fifth level, the expansion height of H5-fifth level, the expansion width of W5-fifth level, the expansion thickness of T5-fifth level.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a hot extrusion molding method of an ultra-high purity copper target, wherein a cross section of an extrusion die is shown in fig. 1, and the method comprises the following steps: heating an ultra-high purity copper rod with the diameter of 15mm to 800 ℃, heating an extrusion die to 670 ℃ before extrusion, performing hot extrusion at the speed of 300mm/min by adopting a 3000T hot extruder to obtain an ultra-high purity copper plate blank, then passing through a vacuum oxidation prevention pipe, and finally cooling to 25 ℃ by adopting a mixed solution of 7% industrial alcohol and water to obtain the ultra-high purity copper target.
The extrusion die is a five-stage stepped expansion deformation channel, and the expansion thickness of each stage is 35mm; wherein, the expansion angle A1 of the first-stage expansion deformation channel is 35 degrees, the expansion height H1 is 13mm, and the expansion width W1 is 25mm; the expansion angle A2 of the second-stage expansion deformation channel is 100 degrees, the expansion height H2 is 15mm, and the expansion width W2 is 90mm; the expansion angle A3 of the third-stage expansion deformation channel is 155 degrees, the expansion height H3 is 15mm, and the expansion width W3 is 200mm; the expansion angle A4 of the fourth-stage expansion deformation channel is 160 degrees, the expansion height H4 is 15mm, and the expansion width W4 is 370mm; the expansion angle A5 of the fifth-stage expansion deformation channel is 106 degrees, the expansion height H5 is 30mm, and the expansion width W5 is 440mm.
Example 2
The embodiment provides a hot extrusion molding method of an ultra-high purity copper target, which comprises the following steps: heating an ultra-high purity copper rod with the diameter of 10mm to 750 ℃, heating an extrusion die to 650 ℃ before extrusion, performing hot extrusion at the speed of 220mm/min by adopting a 3000T hot extruder to obtain an ultra-high purity copper plate blank, then passing through a vacuum oxidation prevention pipe, and finally cooling to 30 ℃ by adopting a mixed solution of 5% industrial alcohol and water to obtain the ultra-high purity copper target.
The extrusion die is a five-stage stepped expansion deformation channel, and the expansion thickness of each stage is 30mm; wherein, the expansion angle A1 of the first-stage expansion deformation channel is 30 degrees, the expansion height H1 is 10mm, and the expansion width W1 is 20mm; the expansion angle A2 of the second-stage expansion deformation channel is 95 degrees, the expansion height H2 is 10mm, and the expansion width W2 is 80mm; the expansion angle A3 of the third-stage expansion deformation channel is 150 degrees, the expansion height H3 is 10mm, and the expansion width W3 is 180mm; the expansion angle A4 of the fourth-stage expansion deformation channel is 155 degrees, the expansion height H4 is 10mm, and the expansion width W4 is 350mm; the expansion angle A5 of the fifth-stage expansion deformation channel is 100 degrees, the expansion height H5 is 25mm, and the expansion width W5 is 400mm.
Example 3
The embodiment provides a hot extrusion molding method of an ultra-high purity copper target, which comprises the following steps: heating an ultra-high purity copper rod with the diameter of 20mm to 850 ℃, heating an extrusion die to 700 ℃ before extrusion, performing hot extrusion at the speed of 380mm/min by adopting a 3000T hot extruder to obtain an ultra-high purity copper plate blank, then passing through a vacuum oxidation prevention pipe, and finally cooling to 20 ℃ by adopting a mixed solution of 10% industrial alcohol and water to obtain the ultra-high purity copper target.
The extrusion die is a five-stage stepped expansion deformation channel, and the expansion thickness of each stage is 40mm; wherein, the expansion angle A1 of the first-stage expansion deformation channel is 40 degrees, the expansion height H1 is 15mm, and the expansion width W1 is 30mm; the expansion angle A2 of the second-stage expansion deformation channel is 105 degrees, the expansion height H2 is 20mm, and the expansion width W2 is 100mm; the expansion angle A3 of the third-stage expansion deformation channel is 160 degrees, the expansion height H3 is 20mm, and the expansion width W3 is 230mm; the expansion angle A4 of the fourth-stage expansion deformation channel is 165 degrees, the expansion height H4 is 20mm, and the expansion width W4 is 400mm; the expansion angle A5 of the fifth-stage expansion deformation channel is 110 degrees, the expansion height H5 is 35mm, and the expansion width W5 is 480mm.
Example 4
This example differs from example 1 only in that the extrusion die was heated to 620 ℃ prior to extrusion, with the other conditions being the same as example 1.
Example 5
This example differs from example 1 only in that the extrusion die was heated to 720 ℃ prior to extrusion, and the other conditions were the same as in example 1.
Example 6
The difference between this example and example 1 is that the expansion thickness of each layer of the extrusion die is different, the expansion thickness of the first stage expansion deformation channel is 30mm, the expansion thickness of the other stages expansion deformation channels is 40mm, and other conditions are the same as those of example 1.
Example 7
The difference between this embodiment and embodiment 1 is that the expansion thicknesses of the layers of the extrusion die are different, the expansion thicknesses of the first-stage expansion deformation channel and the second-stage expansion deformation channel are both 30mm, the expansion thicknesses of the remaining expansion deformation channels are both 40mm, and other conditions are the same as those of embodiment 1.
Example 8
The difference between this embodiment and embodiment 1 is that the expansion thicknesses of the layers of the extrusion die are different, the expansion thicknesses of the first-stage expansion deformation channels, the second-stage expansion deformation channels and the third-stage expansion deformation channels are all 30mm, the expansion thicknesses of the other expansion deformation channels are all 40mm, and other conditions are the same as those of embodiment 1.
Example 9
The difference between this embodiment and embodiment 1 is that the expansion thicknesses of the layers of the extrusion die are different, the expansion thicknesses of the first-stage expansion deformation channel and the second-stage expansion deformation channel are both 30mm, the expansion thicknesses of the remaining expansion deformation channels are both 35mm, and other conditions are the same as those of embodiment 1.
Comparative example 1
This comparative example differs from example 1 only in that the ultra-high purity copper rod was heated to 720 ℃, with the other conditions being the same as example 1.
Comparative example 2
This comparative example differs from example 1 only in that the ultra-high purity copper rod was heated to 870 ℃, with the other conditions being the same as example 1.
The ultra-high purity copper targets prepared in examples 1-9 and comparative examples 1-2 were subjected to performance tests for grain size and internal structure uniformity, as follows:
(1) Grain size: the determination is carried out according to a section method disclosed in national standard GB/T6394-2017, metal average grain size determination method;
(2) Uniformity of internal tissue of target: firstly, taking a visual standard sample as a standard, and then precisely processing, wherein the surface is clean, the color and luster are uniform, and no bunchy or punctiform spots appear, so that the internal structure is uniform, and no segregation phenomenon appears.
The specific test results are shown in table 1.
TABLE 1
From table 1, the following points can be found:
(1) The hot extrusion molding method of the copper target material can effectively control the grain size of the copper target material, the grain size of the copper target material is 20-30 mu m, the grains are fine and uniform, and the requirement of an integrated circuit process on the grain size is met;
(2) Comparing example 1 with examples 4-5, when the heating temperature of the extrusion die is lower than 650 ℃, the prepared copper target material has fine and uniform crystal grains, but causes great loss and easy cracking of the extrusion die; when the heating temperature of the extrusion die is higher than 700 ℃, the prepared copper target material has fine and uniform crystal grains, but the energy consumption is increased, and the cost is increased;
(3) Comparing the embodiment 1 with the embodiments 6-9, the copper plate blank is deformed unevenly, the crystal grains are uneven, layering occurs in the thickness direction and internal defects are caused due to the fact that the expansion thicknesses of all stages of the extrusion die are inconsistent;
(4) Comparing example 1 with comparative examples 1-2, when the ultra-high purity copper rod heating temperature is below 750 ℃, although the grain size of the prepared copper target is 21.8 μm, the extrusion is difficult, the thermoplastic deformation is insufficient, and the grains are uneven and the internal defects are caused; when the heating temperature of the ultra-high-purity copper rod is higher than 850 ℃, the ultra-high-purity copper rod becomes soft and cannot be extruded smoothly due to the fact that the heating temperature is too high.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (11)
1. The hot extrusion molding method of the ultra-high purity copper target is characterized by comprising the following steps of: heating the ultra-high-purity copper rod to 750-850 ℃, and then sequentially performing hot extrusion, anti-oxidation treatment and cooling to obtain an ultra-high-purity copper target;
the extrusion die for hot extrusion is a five-stage stepped expansion deformation channel, the heating temperature of the extrusion die is 650-700 ℃, and the expansion thickness of each stage of the five-stage stepped expansion deformation channel is the same;
the anti-oxidation treatment is to pass the ultra-high purity copper plate blank formed by hot extrusion through a vacuum anti-oxidation device.
2. The method of claim 1, wherein the ultra-high purity copper rod has a diameter of 10-20mm.
3. The method according to claim 1, wherein the speed of the hot extrusion is 220-380mm/min.
4. The method of claim 1, wherein the cooling is at a temperature of 20-30 ℃.
5. The method according to claim 1, wherein the cooling liquid used for cooling is a mixed liquid of industrial alcohol and water.
6. The method of claim 5, wherein the industrial alcohol is present in a concentration of 5-10%.
7. The method of claim 1, wherein the expansion angle of the first stage expansion deformation channel of the five stage ladder expansion deformation channel is 30-40 °, the expansion height is 10-15mm, the expansion width is 20-30mm, and the expansion thickness is 30-40mm.
8. The method of claim 1, wherein the expansion angle of the second stage expansion deformation channel of the five stage ladder expansion deformation channel is 95-105 °, the expansion height is 10-20mm, the expansion width is 80-100mm, and the expansion thickness is 30-40mm.
9. The method of claim 1, wherein the expansion angle of the third stage expansion deformation channel of the five stage ladder expansion deformation channel is 150-160 °, the expansion height is 10-20mm, the expansion width is 180-230mm, and the expansion thickness is 30-40mm.
10. The method of claim 1, wherein the expansion angle of the fourth stage expansion deformation channel of the five stage ladder expansion deformation channel is 155-165 °, the expansion height is 10-20mm, the expansion width is 350-400mm, and the expansion thickness is 30-40mm.
11. The method of claim 1, wherein the expansion angle of the fifth stage expansion deformation channel of the five stage ladder expansion deformation channel is 100-110 °, the expansion height is 25-35mm, the expansion width is 400-480mm, and the expansion thickness is 30-40mm.
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| CN113846297A (en) * | 2020-06-26 | 2021-12-28 | 东方铜业有限公司 | Method for producing copper cylinder target for sputtering film coating by hot extrusion technology |
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| CN101992223A (en) * | 2010-11-12 | 2011-03-30 | 西南铝业（集团）有限责任公司 | Processing method of porous round bar die |
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