CN112846660B - Processing method of thick-wall high-length-diameter-ratio high-purity copper pipe target - Google Patents
Processing method of thick-wall high-length-diameter-ratio high-purity copper pipe target Download PDFInfo
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- 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
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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
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The invention discloses a processing method of a thick-wall large-length-diameter ratio high-purity copper tube target, belonging to the technical field of target material manufacturing, which comprises the following steps: 1) preparing a high-purity copper ingot 2) preparing a high-purity copper pipe 3) preparing a high-purity copper pipe blank 4) processing a high-purity copper pipe target; and then the finished high-purity copper tube target is obtained through the subsequent cleaning, drying and packaging processes; the invention fundamentally solves the problems of low purity, high oxygen content, long processing flow, high production cost and difficult realization of batch production of the copper tube target produced by the traditional preparation process.
Description
Technical Field
The invention belongs to the technical field of target manufacturing, and particularly relates to a method for processing a thick-wall high-length-diameter-ratio high-purity copper pipe target.
Background
The sputtering target material is used as one of important matching materials in the manufacturing process of integrated circuit chips and devices, and is mainly used for preparing films of interconnection lines, barrier layers, through holes, back metallization layers and the like in the metallization process. The sputtering target mainly comprises ultrahigh pure titanium, tantalum, cobalt, gold, silver, platinum, aluminum and aluminum alloy, copper and copper alloy, tungsten and tungsten alloy and the like. The global sputtering target market presents an oligopolistic pattern, the industrial concentration is high, research and development and production are mainly concentrated on a few companies in the United states and Japan, target production enterprises have complete technology vertical integration capability from high-purity preparation of metal materials to target manufacturing production, and the main market of global high-end targets is controlled. According to SEMI data, the market size of sputtering targets for global semiconductor manufacturing was $ 7.3 billion in 2019, with a 7.2% reduction, which remained essentially stable in 2020, and a 8.1 billion dollar return to growth in 2021.
Enterprises engaged in the research, development and production of sputtering targets at home lags foreign target production enterprises in the key technical aspects of high purification, microstructure control, refined deep processing and the like. The development of the domestic high-purity metal target material industry can not only greatly drive the upgrading of the upstream traditional nonferrous metal material industry structure in China, but also promote the technical progress and the rapid development of the downstream electronic manufacturing industry. At present, the sputtering process developed at a high speed not only has high requirements on the purity of the target material, but also has strict requirements on the aspects of the grain size and texture orientation of the target material, the structural uniformity control of large-size block materials, the high-precision forming processing of large-size target materials and the like. The national high-purity metal target production and research and development organization needs to break through key core technologies such as high purification technology, microstructure control, texture regulation, precision machining and the like, forms a basic electronic industry system with optimized structure and complete matching, promotes industrial transformation and upgrading, fully meets the requirement of domestic high-purity metal targets, and has important influence on the international market.
As shown in tables 1 and 2, for the rotary target, the occupancy rate of the rotary target in the domestic target market is only 10%, and the occupancy rate in the international market is only 20%, and the planar target occupies most of the rotary target. At present, users of the rotary target have panda electronics, Jingdong, Suzhou Samsung and Huaxing photoelectricity at home, have well-known enterprises such as Samsung and LG at home, and have huge market prospects. For the planar target, due to the low utilization rate, after 8.5 generation, the rotary target with high utilization rate will gradually replace the planar target, the market share of the rotary target will gradually increase, which is expected to reach about 40%, and the rotary target has a wide increase space.
At present, mature rotary target material manufacturers are few, only east guan European Lai exists in China, the rotary target material is mainly and internationally concentrated in Korea, Japan and the like, enterprises comprising Korea east friend, Japan Hitachi metal, Japan steel and the like are provided, rotary target material processing and manufacturing are developed at the present stage, the rotary target material has great advantages, on one hand, the manufacturing level of the domestic rotary target material can be improved, the industrial development is promoted, on the other hand, the international market share can be seized, and the international influence is increased.
Patent CN 105861999B discloses a method for preparing a high-purity fine-grain metallic nickel hot-extrusion rotary target material, which comprises melting raw material nickel into a high-purity nickel ingot by vacuum electron beams, heating the nickel ingot, directly extruding the heated nickel ingot, annealing the extruded nickel target, and finally performing necessary machining on the annealed nickel target to prepare the required rotary target material. The preparation method of the ingot used by the method is vacuum electron beam melting and traditional casting, while the preparation method adopted by the patent is vacuum induction melting and bottom casting type water-cooling copper mold casting, the production period is short, the efficiency is high, the cost is low, the surface of the ingot is flat and glossy, and the internal structure is compact and has no defects.
Patent CN 107267937A discloses a preparation process of a high-purity oxygen-free copper tube target material for sputtering, which mainly comprises the following steps: preheating, smelting, casting, heating, extruding, primary stretching, annealing, secondary stretching, bright annealing, finishing, checking mechanical property and warehousing. The method describes the processing process of the oxygen-free copper tube target in detail, but the method has more complex working procedures, needs to be subjected to multiple extrusion, stretching and annealing processes, and is not beneficial to batch production; the purity of the copper tube target obtained by the method is limited, the copper tube target can only be suitable for low-end flat panel display industry, and for high-end flat panel display industry of more than 8.5 generations, the oxygen content of 5ppm can not meet the requirement. The method that this patent adopted is vacuum induction melting, adopt "melting → solidification → secondary melting technology" to the abundant degasification of fuse-element, this patent adopts end casting formula water-cooling copper mold casting method, compare with traditional top tilting casting mode, the fuse-element disturbance is little in casting process, the possibility that gas was wrapped up in the clamp and gets into the mould reduces, consequently, the oxygen content in the ingot casting can reduce to below 1ppm, abnormal phenomena such as particle that can reduce the production in the sputtering process by a wide margin, and this patent processing procedure is simple, can realize mass production.
Patent CN 201722424U discloses a pipe target material subassembly, and this utility model constitutes pipe target material subassembly through threaded connection's mode, adopts the sealing washer to seal between flange and the pipe target base member, in order to prevent that target material subassembly from taking place gas leakage, the phenomenon of leaking water in the use, this method is very high to the machining precision of flange joint and the regional surface quality requirement of sealing, and this connected mode's intensity is limited moreover. For copper tube targets, a threaded connection is not suitable due to its own weight exceeding 250 kg. This patent adopts electron beam welding's mode to carry out flange joint, has produced the local fusion between flange and the pipe target base body, and welding strength is very high, and sealing performance is good. Compared with other connection modes, the electron beam welding has the following advantages: the deformation is small, and the precision welding can be performed after the precision machining before the welding; welding with complicated shapes or deep parts can be performed. The high-purity copper tube target in the invention has the length of more than 2500mm and the wall thickness of more than 20mm, and the problems of deformation and insufficient welding depth can be effectively solved by adopting an electron beam welding mode.
CN 103071791B and CN 105817627B disclose a method for forming a TiAl tube target material with a large length-diameter ratio and a method for preparing a tungsten tube target with a large length-diameter ratio by integral forming, wherein the tube target material is obtained by adopting a sheath design, powder forming and hot isostatic pressing, and the method is essentially different from the method.
Disclosure of Invention
In order to solve the problems, the invention provides a processing method of a thick-wall high-length-diameter ratio high-purity copper tube target, which comprises the following steps:
1) preparing a high-purity copper ingot: adopting vacuum induction melting copper raw materials, and stopping heating after the melt is completely melted; vacuum degree is less than or equal to 3 multiplied by 10-2Pa, then cooling to solidify the melt so as to fully degas and obtain a solidified body; keeping for 1h under the condition; refining the solidified body at 1280 +/-10 ℃ to obtain refined copper melt, and casting by adopting a water-cooled copper mold to obtain a high-purity copper ingot;
2) preparing a high-purity copper pipe: carrying out hot extrusion deformation on the high-purity copper cast ingot by adopting a near constant temperature extrusion technology, and cooling to obtain a high-purity copper pipe; the extrusion temperature is 850 +/-10 ℃, the hot extrusion speed is 1-5m/s, water cooling is adopted in the cooling process, and the average grain size of the high-purity copper pipe is less than or equal to 70 mu m;
different variable speed extrusion processes are designed according to the allowable critical temperature range of the capacity and the surface quality of the extruder, so that the constant temperature extrusion of the outlet temperature is realized in the shortest extrusion stroke, and the method has the advantages of improving the tissue uniformity of the high-purity copper pipe in the length direction;
3) preparing a high-purity copper pipe blank: carrying out matching turning design on a high-purity copper pipe, an oxygen-free copper flange and an oxygen-free copper bottom plate, and connecting one end of the high-purity copper pipe with the oxygen-free copper flange and the other end with the oxygen-free copper bottom plate in an electron beam welding mode to obtain a thick-wall high-length-diameter-ratio high-purity copper pipe target blank with high supporting strength; carrying out matched turning design on a high-purity copper pipe, an oxygen-free copper flange and an oxygen-free copper bottom plate to obtain a high-purity copper pipe blank with close matching and a bright surface;
4) processing of the high-purity copper tube target: machining the high-purity copper pipe target blank by adopting a high-precision large-size lathe, wherein the machining precision is +/-0.1 mm, and thus obtaining a high-purity copper pipe target; the wall thickness of the high-purity copper pipe is 20-25mm, the length is 2500-3000mm, and the length-diameter ratio is not less than 17;
the step 4) is followed by a cleaning and packaging process of the high-purity copper tube target: the method comprises the following specific steps: designing and building a large-size rotary tube target cleaning, drying and packaging production line, and operating according to the process of preparation → ultrasonic cleaning → bubbling cleaning → drying → vacuum inner packaging → middle packaging → outer packaging → inspection → packing, wherein the surface quality meets the electronic grade requirement.
Step 1) before casting begins, argon is filled into a hearth, so that the surface quality of the high-purity copper cast ingot can be improved, and the cooling speed is increased; the casting process adopts a bottom casting type water-cooled copper mold, refined copper melt enters a bottom casting type water-cooled copper mold cavity through a crucible bottom guide pipe, and the melt is solidified into a high-purity copper cast ingot under the circulating water cooling effect; the high-purity copper cast ingot is clean and free of defects, and the oxygen content is less than or equal to 1 ppm.
The purity of the high-purity copper tube target is 99.99 percent (4N), 99.995 percent (4N5), 99.999 percent (5N) and 99.9999 percent (6N), and the oxygen content is less than or equal to 1 ppm.
The diameter of the high-purity copper ingot is
The high-purity copper pipe is extruded by a large-scale reverse extruder with the weight of 3500 tons or more.
And a synchronous supporting component is adopted to support the high-purity copper tube target blank and synchronously rotate with the high-purity copper tube target blank in the machining process, so that the high-purity copper tube target blank is ensured to be safely clamped, and the high-purity copper tube target blank is prevented from being deformed due to gravity. The machining precision is improved;
the inner package is used for realizing three-layer vacuum bag package on the vacuum packaging machine for the high-purity copper pipe target after vacuum drying so as to prevent oxidation; the middle package is to place the high-purity copper tube target subjected to the inner package in a customized PVC box to prevent collision; the outer package is to place the high-purity copper tube target packaged in the finished product into a customized wooden box to prevent collision in the transportation process.
Ultrasonic cleaning is carried out in an ultrasonic cleaning machine, and a proper cleaning agent is selected; and the vacuum drying is to send the cleaned tube target material into a vacuum oven, keep the temperature for a certain time at a proper temperature and then naturally cool the tube target material to room temperature in the vacuum oven.
The invention has the beneficial effects that:
1. the processing method is suitable for the preparation and processing of the high-purity copper rotary tube target for plane display, and solves the problems of low purity, high oxygen content, long processing flow, high production cost and difficulty in realizing batch production of the copper tube target produced by the traditional preparation process.
2. The preparation method adopted by the high-purity copper ingot provided by the invention is vacuum induction melting and bottom casting type water-cooling copper mold casting, and has the advantages of short production period, high efficiency, low cost, smooth and glossy ingot surface, compact and defect-free internal structure.
3. The high-purity copper pipe is prepared by adopting a near constant temperature extrusion technology, and has the advantage of improving the tissue uniformity of the high-purity copper pipe in the length direction.
4. The high-purity copper pipe blank related by the invention realizes the connection of the oxygen-free copper flange, the oxygen-free copper base plate and the high-purity copper pipe by adopting an electron beam welding mode, local fusion is generated between the flange and the pipe target substrate, the welding strength is very high, and the sealing performance is good. Compared with other connection modes, the method has the advantages of small deformation and deep welding.
Drawings
FIG. 1 is a microstructure of a high purity copper pipe material according to example 1.
Fig. 2 shows the matching size of the oxygen-free copper flange of the high-purity copper pipe blank in the example 1.
FIG. 3 shows the oxygen-free copper bottom plate matching size of the high-purity copper pipe blank in example 1.
FIG. 4 shows the fitting dimensions of the high purity copper pipe blank in example 1.
FIG. 5 is a microstructure of a high purity copper pipe material of example 2.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
To produce 4N5 pure
The high-purity copper tube target:
smelting: the raw material adopts a high-purity electrolytic copper plate, the purity is more than or equal to 99.999 percent, the oxygen content is less than or equal to 5ppm, and the surface is clean and has no oxidation and oil stain. Gradually heating the electrolytic copper plate in a vacuum induction melting furnace to full melting according to the power supply power of 20-40-60-100 kw; then the power supply is turned off to stop heating, so that the melt is cooled and solidified, and the gas is fully removed; and (4) after the power is cut off for 1 hour, the power supply is turned on again for heating, the mixture is heated to full melting by 120kw, and refining is carried out for 10 +/-2 min.
Casting: filling argon into the hearth, opening a flow guide pipe at the bottom of the crucible, and transferring the refined high-purity copper melt to a water-cooled copper mold cavityIn the process, the mixture is solidified and formed under the action of circulating water cooling, and the specification of the cast ingot is
Heating: and heating the ingot blank by using a power frequency heating furnace, wherein the heating temperature is 800 +/-20 ℃, the heating time is 3 +/-0.2 h, and the time is counted when the temperature is reached.
Extruding: and extruding the heated ingot casting blank by using a 3500 ton extruding machine and a matched mould to process the ingot casting blank into a high-purity copper pipe, and gradually lifting the extruding speed according to the ratio of 5 → 4 → 3 → 2 → 1.5 → 1m/s and cooling by water. The outer diameter of the high-purity copper pipe is 172mm, the wall thickness is 26mm, and the length is 3000 mm. The metallographic microstructure of the high-purity copper pipe material is shown in FIG. 1, and the average grain size is 48 μm.
And (3) finishing: and performing mechanical finishing on the extruded high-purity copper pipe.
Welding: and (3) carrying out matching and turning design on the oxygen-free copper flange, the oxygen-free copper bottom plate and the high-purity copper pipe, wherein the matching and turning sizes of the three are respectively shown in figures 2-4, so that a blank with tight matching and a bright surface is obtained, and a welding joint is qualified through a helium leak detection test.
Machining: a high-precision large-size lathe is utilized, a synchronous supporting component is adopted to support the tube target and synchronously rotate with the tube target in the processing process, the high-purity copper tube blank is processed to the finished product size,
cleaning, drying and packaging: according to the process operation of preparation → ultrasonic cleaning → bubbling cleaning → drying → vacuum inner packaging → middle packaging → outer packaging → inspection → boxing, the surface quality of the finished product of the high-purity copper pipe target meets the requirement of electronic grade.
Example 2
To produce a product having a purity of 6N
The high-purity copper tube target:
smelting: the raw material adopts a high-purity electrolytic copper plate, the purity is more than or equal to 99.999 percent, the oxygen content is less than or equal to 5ppm, and the surface is clean and has no oxidation and no oil stain. Gradually heating the electrolytic copper plate in a vacuum induction melting furnace to full melting according to the power supply power of 20-40-60-100 kw; then the power supply is turned off to stop heating, so that the melt is cooled and solidified, and the gas is fully removed; and (4) after the power is cut off for 1 hour, the power supply is turned on again for heating, the mixture is heated to full melting by 120kw, and refining is carried out for 10 +/-2 min.
Casting: filling argon into the hearth, opening a guide pipe at the bottom of the crucible, transferring the refined high-purity copper melt into a water-cooling copper mold cavity, and solidifying and forming under the action of circulating water cooling, wherein the specification of the ingot is
Heating: and heating the ingot blank by using a power frequency heating furnace, wherein the heating temperature is 830 +/-20 ℃, the heating time is 3 +/-0.2 h, and timing when the temperature is reached.
Extruding: and (3) extruding the heated ingot casting blank by using a 3500 ton extruding machine and a matched mould to process the ingot casting blank into a high-purity copper pipe, wherein the extruding speed is 5 → 3 → 1m/s, and water cooling is carried out. The outer diameter of the high-purity copper pipe is 172mm, the wall thickness is 26mm, and the length is 3000 mm. The metallographic microstructure of the high purity copper pipe material is shown in FIG. 5, and the average grain size is 60 μm.
And (3) finishing: and performing mechanical finishing on the extruded high-purity copper pipe.
Welding: and carrying out matching and turning design on the oxygen-free copper flange, the oxygen-free copper bottom plate and the high-purity copper pipe to obtain a blank with tight matching and a bright surface, wherein the welded joint is qualified through a helium leak detection test.
Machining: a high-precision large-size lathe is utilized, a synchronous supporting component is adopted to support the tube target and synchronously rotate with the tube target in the processing process, the high-purity copper tube blank is processed to the finished product size,
cleaning, drying and packaging: according to the process operation of preparation → ultrasonic cleaning → bubbling cleaning → drying → vacuum inner packaging → middle packaging → outer packaging → inspection → boxing, the surface quality of the finished product of the high-purity copper pipe target meets the requirement of electronic grade.
TABLE 1 target utilization ratio table
| Type of target | Planar target material | Rotary target material |
| Utilization rate | 30％ | 80％ |
| Recovery rate | 70％ | 70％ |
| Overall efficiency of use | 21％ | 56％ |
TABLE 2 Flat display manufacturer Capacity summaries
Claims (7)
1. The processing method of the thick-wall large-length-diameter ratio high-purity copper tube target is characterized by comprising the following steps of:
1) preparing a high-purity copper ingot: smelting a copper raw material by vacuum induction, and stopping heating after a melt is completely melted; vacuum degree is less than or equal to 3 multiplied by 10-2Pa, then cooling to solidify the melt to fully degas to obtain a solidified body; under the condition thatKeeping for 1 h; refining the solidified body at 1280 +/-10 ℃ to obtain refined copper melt, and casting by adopting a water-cooled copper mold to obtain a high-purity copper ingot;
2) preparing a high-purity copper pipe: carrying out hot extrusion deformation on the high-purity copper cast ingot by adopting a near constant temperature extrusion technology, and cooling to obtain a high-purity copper pipe; the extrusion temperature is 850 +/-10 ℃, the hot extrusion speed is 1-5m/s, water cooling is adopted in the cooling process, and the average grain size of the high-purity copper pipe is less than or equal to 70 mu m;
3) preparing a high-purity copper pipe blank: carrying out matching turning design on a high-purity copper pipe, an oxygen-free copper flange and an oxygen-free copper bottom plate, and connecting one end of the high-purity copper pipe with the oxygen-free copper flange and the other end with the oxygen-free copper bottom plate in an electron beam welding mode to obtain a thick-wall high-length-diameter-ratio high-purity copper pipe target blank with high supporting strength;
4) processing of the high-purity copper tube target: machining the high-purity copper pipe target blank by adopting a high-precision large-size lathe, wherein the machining precision is +/-0.1 mm, and thus obtaining a high-purity copper pipe target; the wall thickness of the high-purity copper pipe is 20-25mm, the length is 2500-3000mm, and the length-diameter ratio is not less than 17;
the step 4) is followed by a cleaning and packaging process of the high-purity copper tube target: the method comprises the following specific steps: designing and building a large-size rotary tube target cleaning, drying and packaging production line, and operating according to the process of preparation → ultrasonic cleaning → bubbling cleaning → drying → vacuum inner packaging → middle packaging → outer packaging → inspection → packing, wherein the surface quality meets the electronic grade requirement; the high-purity copper cast ingot is clean and free of defects, and the oxygen content is less than or equal to 1 ppm.
2. The method for processing the high-purity copper tube target with the thick wall and the large length-diameter ratio as claimed in claim 1, wherein before the casting in the step 1), argon gas is filled into a hearth, so that the surface quality of the high-purity copper cast ingot can be improved, and the cooling speed is increased; and in the casting process, a bottom casting type water-cooled copper mold is adopted, refined copper melt enters a cavity of the bottom casting type water-cooled copper mold through a flow guide pipe at the bottom of the crucible, and the melt is solidified into a high-purity copper cast ingot under the action of circulating water cooling.
3. The method as claimed in claim 1, wherein the purity of the high-purity copper tube target is 99.99% (4N), 99.995% (4N5), 99.999% (5N), 99.9999% (6N), and the oxygen content is less than or equal to 1 ppm.
4. The method for processing the high-purity copper pipe target with the thick wall and the large length-diameter ratio as claimed in claim 1, wherein the diameter of the high-purity copper ingot is as follows
5. The method for processing the thick-wall high-length-diameter ratio high-purity copper tube target as claimed in claim 1, wherein the high-purity copper tube is extruded by a large-scale backward extrusion machine with the weight of 3500 tons or more.
6. The method for processing the high-purity copper tube target with the thick wall and the large length-diameter ratio according to claim 1, wherein a synchronous supporting assembly is adopted to support the high-purity copper tube target blank and synchronously rotate with the high-purity copper tube target blank during the processing process, so that the high-purity copper tube target blank is safely clamped, and the high-purity copper tube target blank is prevented from being deformed due to gravity.
7. The processing method of the thick-wall large-length-diameter ratio high-purity copper tube target as claimed in claim 1, wherein the inner package is a three-layer vacuum bag package of the vacuum-dried high-purity copper tube target on a vacuum packaging machine to prevent oxidation; the middle package is to place the high-purity copper tube target subjected to the inner package in a customized PVC box to prevent collision; the outer package is to place the high-purity copper tube target packaged in the finished product into a customized wooden box to prevent collision in the transportation process.
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| CN113529027A (en) * | 2021-05-31 | 2021-10-22 | 洛阳科威钨钼有限公司 | Preparation method of high-purity oxygen-free copper sputtering coating target material |
| CN113649509B (en) * | 2021-08-13 | 2024-03-22 | 宁波江丰电子材料股份有限公司 | Copper target and preparation method thereof |
| CN113774337B (en) * | 2021-08-19 | 2023-11-17 | 四川华赐科技有限公司 | Preparation process of high-purity copper rotary tube target for flat panel display |
| CN113774228A (en) * | 2021-08-19 | 2021-12-10 | 虹华科技股份有限公司 | Forming processing method of high-purity copper |
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| CN109940066A (en) * | 2019-03-18 | 2019-06-28 | 东莞市欧莱溅射靶材有限公司 | A kind of semi-automatic aligning method of high purity copper rotary target welding end |
| CN111451314A (en) * | 2020-04-01 | 2020-07-28 | 东莞市欧莱溅射靶材有限公司 | Preparation method of high-purity copper rotary target |
| CN111590279A (en) * | 2020-06-03 | 2020-08-28 | 福建阿石创新材料股份有限公司 | High-purity metal rotary target material and preparation method thereof |
| CN111604651A (en) * | 2020-06-28 | 2020-09-01 | 沈阳有色金属加工有限公司 | Preparation method of large-size high-purity copper rotary target material |
| CN112128177A (en) * | 2020-08-27 | 2020-12-25 | 中联重科股份有限公司 | Method for dynamically adjusting engineering machinery power |
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