CN113774337A - Preparation process of high-purity copper rotary tube target for plane display - Google Patents
Preparation process of high-purity copper rotary tube target for plane display Download PDFInfo
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- CN113774337A CN113774337A CN202110956453.1A CN202110956453A CN113774337A CN 113774337 A CN113774337 A CN 113774337A CN 202110956453 A CN202110956453 A CN 202110956453A CN 113774337 A CN113774337 A CN 113774337A
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- copper
- tube target
- purity copper
- rotary tube
- extrusion
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 176
- 239000010949 copper Substances 0.000 title claims abstract description 176
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 42
- 239000002994 raw material Substances 0.000 claims abstract description 37
- 238000007670 refining Methods 0.000 claims abstract description 24
- 238000003754 machining Methods 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 17
- 238000003723 Smelting Methods 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims abstract description 9
- 238000007872 degassing Methods 0.000 claims abstract description 9
- 239000000155 melt Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 65
- 238000001125 extrusion Methods 0.000 claims description 62
- 238000002844 melting Methods 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000003344 environmental pollutant Substances 0.000 claims description 8
- 231100000719 pollutant Toxicity 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 230000003746 surface roughness Effects 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 8
- 238000005477 sputtering target Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- 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 discloses a preparation process of a high-purity copper rotating tube target for plane display. It comprises the following steps: (1) cathode electrolytic copper is used as a raw material; (2) preheating the raw materials to 110-150 ℃, and preserving heat for 0.5-2 h; (3) smelting; (4) cooling to solidify the melt to remove gas; (5) primary refining; (6) cooling to solidify the refined copper melt and degassing again; (7) secondary refining; (8) casting; (9) continuously extruding to obtain a high-purity copper rotary tube target primary blank; (10) and machining to obtain the finished product of the high-purity copper rotary tube target. The high-purity copper rotary tube target prepared by the preparation process of the high-purity copper rotary tube target for the flat panel display can meet the requirements of the high-purity copper rotary tube target for the flat panel display, has smaller surface roughness and lower oxygen content, and is more suitable for the use of the flat panel display industry.
Description
Technical Field
The invention belongs to the technical field of target material manufacturing, and particularly relates to a preparation process of a high-purity copper rotary tube target for plane display.
Background
High purity copper sputtering target products are used mainly in the semiconductor industry and flat panel display industry.
Semiconductor industry: with the development of the semiconductor industry, high purity sputtering targets are growing up, and the integrated circuit industry has become one of the main application fields of high purity sputtering targets. With the rapid development of information technology, the integration degree of an integrated circuit needs to be improved, and the size of a unit device in the circuit needs to be reduced. The inside of each unit device is composed of a substrate, an insulating layer, a dielectric layer, a conductor layer and a protective layer, wherein the dielectric layer, the conductor layer and even the protective layer are all dependent on the sputtering coating technique, and thus the sputtering target is a core material for preparing an integrated circuit. The coatings used in the field of integrated circuits mainly comprise copper targets, aluminum targets, titanium targets, tantalum targets, tungsten targets, etc., which require high purity target materials, typically more than 5N (99.999%). With the increasing demand of semiconductor in terminal consumption fields such as smart phones, tablet computers, automotive electronics and the like, especially the tight combination of consumer electronics products with the Internet and the mobile Internet, network access terminals (such as mobile phones, tablet computers and smart televisions continue to be developed, further increasing the capacity of the semiconductor market.
Flat panel display industry (including touch screen industry): the flat panel display mainly includes a Liquid Crystal Display (LCD), a Plasma Display Panel (PDP), an electroluminescent display (EL), a Field Emission Display (FED), and the like. In recent years, Liquid Crystal Displays (LCDs) have gradually replaced cathode-ray tube displays (CRTs) and become the mainstream display technology in the world, and their major applications include high definition televisions, notebook computers, desktop computer displays and other electronic products. Flat panel displays are composed of a metal electrode, a transparent conductive electrode, an insulating layer and a light emitting layer, and in order to ensure uniformity of a thin film layer having a large area to improve productivity, a sputtering technique is increasingly used to prepare the thin film. And reduces the cost. The main types of targets for coating include chromium targets, molybdenum targets, aluminum targets, copper alloy targets and indium oxide targets with tin (ITO).
From the trend of the global lcd market, the growth of tablet computers is mainly driven by the growth of applications in the developed market (including north america, japan and western europe). Since the size of sputtering targets for liquid crystal displays is generally large, the steady and rapid growth in the volume of liquid crystal panel shipments will provide greater development space for sputtering target manufacturers. The applicant finds that the preparation of the high-purity copper rotary tube target for the plane display has higher market value and larger development space, and therefore, the research and development team is built to carry out deep research on the high-purity copper rotary tube target for the plane display.
The applicant finds that the high-purity copper rotating tube target prepared by the existing plane display high-purity copper rotating tube target preparation process has the defects of high surface roughness and high oxygen content.
Disclosure of Invention
The invention aims to provide a preparation process of a high-purity copper rotary tube target for planar display, which aims to solve the technical problems that the high-purity copper rotary tube target prepared by the preparation process of the high-purity copper rotary tube target for planar display in the prior art has high surface roughness and high oxygen content.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation process of a high-purity copper rotating tube target for plane display, which comprises the following steps:
(1) using cathode electrolytic copper as a raw material to remove dirt on the surface of the raw material;
(2) preheating the raw materials to 110-150 ℃, and preserving heat for 0.5-2 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1150-1250 ℃;
(4) keeping the vacuum degree in the vacuum melting device less than or equal to 3 multiplied by 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 600-700 ℃ at a heating rate of 25-35 ℃/h, and preserving heat for 1-2 h; then heating to 750-850 ℃ at a heating rate of 25-35 ℃/h, and preserving heat for 1-2 h to obtain refined copper melt;
(6) keeping the vacuum degree in the vacuum melting device less than or equal to 3 multiplied by 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain secondaryA copper solidification body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 900-1000 ℃ at a heating rate of 25-35 ℃/h, and keeping the temperature for 2-3 h; then heating to 1300-1400 ℃ at a heating rate of 25-35 ℃/h, and preserving heat for 1-2 h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-1.5 MPa to-0.5 MPa, the extrusion temperature is 860 to 900 ℃, the extrusion rate is 2 to 5m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm to obtain a high-purity copper rotary tube target finished product.
Further, in the step (1), the purity of the cathode electrolytic copper is 99.9% or more.
Further, in the step (2), the raw materials are preheated to 120-140 ℃, and heat preservation is carried out for 1-1.5 h.
Further, in the step (3), the used protective gas is argon or nitrogen.
Further, in the step (4), the vacuum degree is 2 × 10-2Pa。
Further, in the step (5), the temperature of the primary refining is increased to 700 ℃ at a temperature increasing rate of 30 ℃/h, and the temperature is kept for 1.5 h.
Further, in the step (7), the temperature of the secondary refining is increased to 900 ℃ at a temperature increasing rate of 30 ℃/h, and the temperature is kept for 2.5 h; then raising the temperature to 1350 ℃ at the temperature raising rate of 30 ℃/h and preserving the temperature for 1.5 h.
Further, in the step (9), the extrusion pressure is-1.0 MPa, the extrusion temperature is 880 ℃, and the extrusion rate is 3.5 m/s.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
the preparation process of the high-purity copper rotary tube target for the plane display, which is provided by the invention, takes cathode electrolytic copper as a raw material, and can improve the purity of a finished product of the high-purity copper rotary tube target and reduce the oxygen content of the finished product through twice refining and twice degassing; in the refining process, the adoption of the step-by-step heating mode is beneficial to reducing the grain size of the finished product of the high-purity copper rotary tube target, so that the surface roughness of the finished product is reduced; the high-purity copper rotating tube target prepared by the preparation process of the high-purity copper rotating tube target for the flat panel display can meet the requirements of the high-purity copper rotating tube target for the flat panel display, has smaller surface roughness and lower oxygen content, and is more suitable for the use of the flat panel display industry.
Detailed Description
First, preparation example
Example 1:
a preparation process of a high-purity copper rotating tube target for flat panel display comprises the following steps:
(1) cathode electrolytic copper with the purity of more than 99.9 percent is taken as a raw material, and dirt on the surface of the raw material is removed;
(2) preheating the raw materials to 130 ℃, and preserving heat for 1.2 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1150-1250 ℃; the used protective gas is argon;
(4) maintaining the vacuum degree in the vacuum melting apparatus at 2X 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 650 ℃ at a heating rate of 30 ℃/h, and preserving heat for 1.5 h; then heating to 800 ℃ at the heating rate of 30 ℃/h, and preserving the heat for 1.5h to obtain refined copper melt;
(6) maintaining the vacuum degree in the vacuum melting apparatus at 2X 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain a secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 950 ℃ at a heating rate of 30 ℃/h, and preserving heat for 2.5 h; then heating to 1350 ℃ at the heating rate of 30 ℃/h, and preserving heat for 1.5h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-1.0 MPa, the extrusion temperature is 880 ℃, the extrusion speed is 3.5m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm, and obtaining a high-purity copper rotary tube target finished product after machining.
Example 2:
a preparation process of a high-purity copper rotating tube target for flat panel display comprises the following steps:
(1) cathode electrolytic copper with the purity of more than 99.9 percent is taken as a raw material, and dirt on the surface of the raw material is removed;
(2) preheating the raw materials to 120 ℃, and preserving heat for 1.5 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1250 ℃; the protective gas used is nitrogen;
(4) maintaining the vacuum degree in the vacuum melting apparatus at 3X 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 700 ℃ at a heating rate of 35 ℃/h, and keeping the temperature for 1 h; then heating to 850 ℃ at the heating rate of 35 ℃/h, and preserving the heat for 1h to obtain refined copper melt;
(6) maintaining the vacuum degree in the vacuum melting apparatus at 3X 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and remove the solidified refined copper melt againGas is carried out to obtain secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 1000 ℃ at a heating rate of 35 ℃/h, and keeping the temperature for 2 h; then heating to 1400 ℃ at the heating rate of 35 ℃/h, and preserving the heat for 1h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-0.5 MPa, the extrusion temperature is 900 ℃, the extrusion speed is 5m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm, and obtaining a high-purity copper rotary tube target finished product after machining.
Example 3:
a preparation process of a high-purity copper rotating tube target for flat panel display comprises the following steps:
(1) cathode electrolytic copper with the purity of more than 99.9 percent is taken as a raw material, and dirt on the surface of the raw material is removed;
(2) preheating the raw materials to 140 ℃, and preserving heat for 1 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is 2.5 multiplied by 10- 2Pa, the smelting temperature is 1150 ℃; the used protective gas is argon;
(4) maintaining the vacuum degree in the vacuum melting apparatus at 2.5X 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 600 ℃ at a heating rate of 25 ℃/h, and keeping the temperature for 2 h; then heating to 750 ℃ at the heating rate of 25 ℃/h, and preserving the heat for 2h to obtain refined copper melt;
(6) maintaining the vacuum degree in the vacuum melting apparatus at 2.5X 10-2Pa，Cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain a secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 900 ℃ at a heating rate of 25 ℃/h, and preserving heat for 3 h; then heating to 1300 ℃ at the heating rate of 25 ℃/h, and preserving the heat for 2h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-1.5 MPa, the extrusion temperature is 860 ℃, the extrusion speed is 2m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm, and obtaining a high-purity copper rotary tube target finished product after machining.
Example 4:
a preparation process of a high-purity copper rotating tube target for flat panel display comprises the following steps:
(1) cathode electrolytic copper with the purity of more than 99.9 percent is taken as a raw material, and dirt on the surface of the raw material is removed;
(2) preheating the raw materials to 150 ℃, and preserving heat for 0.5 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1150-1250 ℃; the protective gas used is nitrogen;
(4) maintaining the vacuum degree in the vacuum melting apparatus at 2.8X 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 650 ℃ at a heating rate of 28 ℃/h, and keeping the temperature for 1.8 h; then heating to 800 ℃ at the heating rate of 28 ℃/h, and preserving the heat for 1.8h to obtain refined copper melt;
(6) keep trueThe vacuum degree in the air smelting device is 2.8 multiplied by 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain a secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 950 ℃ at a heating rate of 28 ℃/h, and preserving heat for 2.8 h; then heating to 1320 ℃ at the heating rate of 28 ℃/h, and preserving the heat for 1.8h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-1.2 MPa, the extrusion temperature is 870 ℃, the extrusion speed is 4m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm, and obtaining a high-purity copper rotary tube target finished product after machining.
Example 5:
a preparation process of a high-purity copper rotating tube target for flat panel display comprises the following steps:
(1) cathode electrolytic copper with the purity of more than 99.9 percent is taken as a raw material, and dirt on the surface of the raw material is removed;
(2) preheating the raw materials to 110 ℃, and preserving heat for 2 hours;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1150-1250 ℃; the used protective gas is argon;
(4) maintaining the vacuum degree in the vacuum melting apparatus at 2.5X 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 680 ℃ at a heating rate of 32 ℃/h, and preserving heat for 1.2 h; then heating to 820 ℃ at a heating rate of 32 ℃/h, and preserving the heat for 1-2 h to obtain a refined copper melt;
(6) maintaining the vacuum degree in the vacuum melting apparatus at 2.5X 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain a secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 980 ℃ at a heating rate of 32 ℃/h, and preserving heat for 2.2 h; then heating to 1380 ℃ at the heating rate of 32 ℃/h and preserving the heat for 1.2h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-0.8 MPa, the extrusion temperature is 890 ℃, the extrusion speed is 3m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm, and obtaining a high-purity copper rotary tube target finished product after machining.
Example 6:
a preparation process of a high-purity copper rotating tube target for flat panel display comprises the following steps:
(1) cathode electrolytic copper with the purity of more than 99.9 percent is taken as a raw material, and dirt on the surface of the raw material is removed;
(2) preheating the raw materials to 140 ℃, and preserving heat for 0.9 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1150-1250 ℃; the protective gas used is nitrogen;
(4) maintaining the vacuum degree in the vacuum melting apparatus at 3X 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 700 ℃ at a heating rate of 30 ℃/h, and keeping the temperature for 2 h; then heating to 850 ℃ at the heating rate of 30 ℃/h, and preserving the heat for 2h to obtain refined copper melt;
(6) maintaining the vacuum degree in the vacuum melting apparatus at 3X 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain a secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 900 ℃ at a heating rate of 30 ℃/h, and preserving heat for 2.8 h; then heating to 1300 ℃ at the heating rate of 30 ℃/h, and preserving the heat for 2h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-1.5 MPa, the extrusion temperature is 900 ℃, the extrusion speed is 5m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm, and obtaining a high-purity copper rotary tube target finished product after machining.
Second, experimental example:
1. the GBT 39158-:
TABLE 1 results of testing target performance of high-purity copper rotary tube in examples 1-6
As can be seen from table 1, the high purity copper rotary tube targets prepared in examples 1 to 6 all meet the detection standard of the high purity copper rotary tube target for flat panel display, have smaller surface roughness and lower oxygen content, and are more suitable for use in the flat panel display industry.
Claims (8)
1. A preparation process of a high-purity copper rotating tube target for flat panel display is characterized by comprising the following steps:
(1) using cathode electrolytic copper as a raw material to remove dirt on the surface of the raw material;
(2) preheating the raw materials to 110-150 ℃, and preserving heat for 0.5-2 h;
(3) putting the preheated raw materials in the step (2) into a vacuum melting device for melting, wherein the vacuum degree is less than or equal to 3 multiplied by 10-2Pa, the smelting temperature is 1150-1250 ℃;
(4) keeping the vacuum degree in the vacuum melting device less than or equal to 3 multiplied by 10-2Pa, cooling to solidify the melt to fully remove the gas and obtain a copper solidified body;
(5) carrying out primary refining on the copper solidified body obtained in the step (4), heating to 600-700 ℃ at a heating rate of 25-35 ℃/h, and preserving heat for 1-2 h; then heating to 750-850 ℃ at a heating rate of 25-35 ℃/h, and preserving heat for 1-2 h to obtain refined copper melt;
(6) keeping the vacuum degree in the vacuum melting device less than or equal to 3 multiplied by 10-2Pa, cooling to solidify the refined copper melt obtained in the step (5) and degassing again to obtain a secondary copper solidified body;
(7) carrying out secondary refining on the secondary copper solidified body obtained in the step (6), heating to 900-1000 ℃ at a heating rate of 25-35 ℃/h, and keeping the temperature for 2-3 h; then heating to 1300-1400 ℃ at a heating rate of 25-35 ℃/h, and preserving heat for 1-2 h to obtain refined copper melt;
(8) casting the refined copper melt obtained in the step (7) by adopting a water-cooling copper mold to obtain a high-purity copper ingot;
(9) extruding the high-purity copper ingot obtained in the step (8) by using a vacuum extrusion device, and before the extrusion process, peeling the surface of the high-purity copper ingot to remove surface oxides and other pollutants; performing nitrogen protection during extrusion, wherein the extrusion pressure is-1.5 MPa to-0.5 MPa, the extrusion temperature is 860 to 900 ℃, the extrusion rate is 2 to 5m/s, water cooling is adopted in the cooling process, and a high-purity copper rotary tube target primary blank is obtained after extrusion;
(10) and (4) machining the high-purity copper rotary tube target blank obtained in the step (9) to the machining precision of +/-0.1 mm to obtain a high-purity copper rotary tube target finished product.
2. The process for preparing a high purity copper rotary tube target for flat panel display according to claim 1, wherein the purity of the cathode electrolytic copper in the step (1) is 99.9% or more.
3. The process for preparing a high-purity copper rotary tube target for flat panel display according to claim 1, wherein in the step (2), the raw material is preheated to 120-140 ℃ and is kept warm for 1-1.5 hours.
4. The process for preparing a rotary tube target of high purity copper for flat panel display according to claim 1, wherein the protective gas used in the step (3) is argon or nitrogen.
5. The process for preparing a high purity copper rotary tube target for flat panel display as claimed in claim 1, wherein in the step (4), the degree of vacuum is 2 x 10-2Pa。
6. The process for preparing a rotary tube target of high purity copper for flat panel display as claimed in claim 1, wherein in the step (5), the primary refining is carried out by raising the temperature to 700 ℃ at a temperature raising rate of 30 ℃/h for 1.5 h.
7. The process for preparing a high purity copper rotary tube target for flat panel display as claimed in claim 1, wherein in the step (7), the secondary refining is performed by raising the temperature to 900 ℃ at a temperature raising rate of 30 ℃/h and keeping the temperature for 2.5 h; then raising the temperature to 1350 ℃ at the temperature raising rate of 30 ℃/h and preserving the temperature for 1.5 h.
8. The process for producing a high purity copper rotary tube target for flat panel display according to claim 1, wherein in the step (9), the extrusion pressure is-1.0 MPa, the extrusion temperature is 880 ℃, and the extrusion rate is 3.5 m/s.
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| CN105132873A (en) * | 2015-09-08 | 2015-12-09 | 有研亿金新材料有限公司 | Au-Sn alloy sputtering target material and preparation method thereof |
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| CN112846660A (en) * | 2020-12-31 | 2021-05-28 | 有研亿金新材料有限公司 | Processing method of thick-wall high-length-diameter-ratio high-purity copper pipe target |
| CN112981335A (en) * | 2021-02-09 | 2021-06-18 | 洛阳高新四丰电子材料有限公司 | Preparation method of high-purity copper tube target |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105132873A (en) * | 2015-09-08 | 2015-12-09 | 有研亿金新材料有限公司 | Au-Sn alloy sputtering target material and preparation method thereof |
| CN105734507A (en) * | 2016-04-05 | 2016-07-06 | 基迈克材料科技（苏州）有限公司 | Fine grain nickel alloy rotary target capable of achieving even film forming and hot extrusion optimizing preparation method thereof |
| CN112846660A (en) * | 2020-12-31 | 2021-05-28 | 有研亿金新材料有限公司 | Processing method of thick-wall high-length-diameter-ratio high-purity copper pipe target |
| CN112981335A (en) * | 2021-02-09 | 2021-06-18 | 洛阳高新四丰电子材料有限公司 | Preparation method of high-purity copper tube target |
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