CN116851753A - Preparation method of multi-principal element alloy target - Google Patents

Preparation method of multi-principal element alloy target Download PDF

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Publication number
CN116851753A
CN116851753A CN202211743620.5A CN202211743620A CN116851753A CN 116851753 A CN116851753 A CN 116851753A CN 202211743620 A CN202211743620 A CN 202211743620A CN 116851753 A CN116851753 A CN 116851753A
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powder
parts
alloy target
chromium
cobalt
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刘淑兰
刘惠
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Tangshan Normal University
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Tangshan Normal University
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/12Metallic powder containing non-metallic particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0483Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C18/00Alloys based on zinc
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C30/00Alloys containing less than 50% by weight of each constituent
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention belongs to the technical field of target processing, and particularly relates to a preparation method of a multi-principal-element alloy target, which comprises the following specific preparation steps: step one: the method comprises the steps of preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for standby, firstly mixing and preparing the multi-principal alloy target by iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder, and on the selected materials, the particle size range of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 10-20 microns, the purity is 99.9-99.999%, the oxygen content is 1-1800ppm, firstly mixing various metal material particles, then pouring the mixture into a vacuum hot press to prepare a target blank, and finally preparing the multi-principal alloy target by the process operation.

Description

Preparation method of multi-principal element alloy target
Technical Field
The invention relates to the technical field of target processing, in particular to a preparation method of a multi-principal element alloy target.
Background
The alloy target is a sputtering coating, which can be simply understood as a sputtering target bombarded by electrons or high-energy laser, and the surface components are sputtered out in the form of atomic groups or ions and finally deposited on the surface of a substrate, and the film is finally formed through a film forming process.
The sputtering coating is divided into a plurality of types, and the difference between the sputtering coating and the evaporation coating is that the sputtering rate becomes one of the main parameters, the uniformity of the components of the laser sputtering coating pld in the sputtering coating is easy to maintain, the uniformity of the thickness of the atomic scale is relatively poor, and the control of the crystal growth is relatively general.
However, in the existing alloy target production process, the hot isostatic pressing process has high cost and small target capacity, and is not suitable for large-scale production.
Disclosure of Invention
The invention aims to provide a preparation method of a multi-principal element alloy target, which aims to solve the problems that in the production process of the existing alloy target in the background technology, the hot isostatic pressing process has higher cost and small target capacity and is not suitable for large-scale production.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation method of the multi-principal-element alloy target comprises the following specific preparation steps of:
step one: preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for later use;
step two: pouring 5-6 parts of iron powder, 1-2 parts of cobalt powder, 3-4 parts of aluminum powder, 5-6 parts of silicon powder, 8-10 parts of chromium powder, 10-12 parts of zinc powder, 8-10 parts of titanium powder and 3-4 parts of nickel powder into a mixer, and continuously mixing and stirring for 10-20 minutes to obtain a mixture;
step three: pouring the product obtained in the third step into a vacuum hot press, firstly, performing a sintering stage, firstly, adjusting the temperature of the hot press to 800-1000 ℃ for continuous sintering for 80-100 minutes, then, adjusting the temperature of the hot press to 1850-2100 ℃ for continuous sintering for 100-120 minutes, cooling after sintering, and removing pressure after cooling to room temperature;
step four: and (3) carrying out machine treatment on the multi-element alloy target blank obtained in the step (III) to finally obtain the multi-element alloy target.
Preferably, in the first step, the particle size of the iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder is 10-20 microns, the purity of the iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder is 99.9-99.999%, and the oxygen content of the iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder is 1-1800ppm.
Preferably, the multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 5 parts of iron powder, 1 part of cobalt powder, 3 parts of aluminum powder, 5 parts of silicon powder, 8 parts of chromium powder, 10 parts of zinc powder, 8 parts of titanium powder and 3 parts of nickel powder.
Preferably, the multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 5.5 parts of iron powder, 1.5 parts of cobalt powder, 3.5 parts of aluminum powder, 5.5 parts of silicon powder, 9 parts of chromium powder, 11 parts of zinc powder, 9 parts of titanium powder and 3.5 parts of nickel powder.
Preferably, the multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 6 parts of iron powder, 2 parts of cobalt powder, 4 parts of aluminum powder, 6 parts of silicon powder, 10 parts of chromium powder, 12 parts of zinc powder, 10 parts of titanium powder and 4 parts of nickel powder.
Preferably, the vacuum hot press requires vacuum to be drawn to 0.0055-0.06Pa.
Preferably, the mixer in the second step is a three-dimensional mixer, before mixing, firstly, an electronic balance weighing device is used for weighing iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder, then the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder are poured into the mixer to be continuously mixed, and in the mixing process, protective gas is required to be added into the mixer to prevent the powder from being oxidized by oxygen in air in the mixing process.
Preferably, the protective gas added in the mixing process of the mixer is argon with the purity of 99.999 percent.
Compared with the prior art, the invention has the beneficial effects that:
the multi-principal element alloy target is prepared by mixing iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder, wherein the particle size range of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 10-20 microns, the purity is 99.9-99.999%, the oxygen content is 1-1800ppm, firstly, a plurality of metal material particles are mixed and then poured into a vacuum hot press to prepare a target blank, and finally, the multi-element alloy target is prepared through the vacuum hot press and the processing of the target blank.
Drawings
FIG. 1 is a flow chart of the preparation steps of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Referring to fig. 1, the present invention provides a technical solution: the preparation method of the multi-principal-element alloy target comprises the following specific preparation steps of:
step one: preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for later use;
step two: pouring 5-6 parts of iron powder, 1-2 parts of cobalt powder, 3-4 parts of aluminum powder, 5-6 parts of silicon powder, 8-10 parts of chromium powder, 10-12 parts of zinc powder, 8-10 parts of titanium powder and 3-4 parts of nickel powder into a mixer, and continuously mixing and stirring for 10-20 minutes to obtain a mixture;
step three: pouring the product obtained in the third step into a vacuum hot press, firstly, performing a sintering stage, firstly, adjusting the temperature of the hot press to 800-1000 ℃ for continuous sintering for 80-100 minutes, then, adjusting the temperature of the hot press to 1850-2100 ℃ for continuous sintering for 100-120 minutes, cooling after sintering, and removing pressure after cooling to room temperature;
step four: and (3) carrying out machine treatment on the multi-element alloy target blank obtained in the step (III) to finally obtain the multi-element alloy target.
In the first step, the particle size range of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 10-20 microns, the purity of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 99.9-99.999%, and the oxygen content of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 1-1800ppm.
The multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 5 parts of iron powder, 1 part of cobalt powder, 3 parts of aluminum powder, 5 parts of silicon powder, 8 parts of chromium powder, 10 parts of zinc powder, 8 parts of titanium powder and 3 parts of nickel powder.
The multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 5.5 parts of iron powder, 1.5 parts of cobalt powder, 3.5 parts of aluminum powder, 5.5 parts of silicon powder, 9 parts of chromium powder, 11 parts of zinc powder, 9 parts of titanium powder and 3.5 parts of nickel powder.
The multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 6 parts of iron powder, 2 parts of cobalt powder, 4 parts of aluminum powder, 6 parts of silicon powder, 10 parts of chromium powder, 12 parts of zinc powder, 10 parts of titanium powder and 4 parts of nickel powder.
The vacuum hot press needs to be vacuumized to 0.0055-0.06Pa.
The three-dimensional mixer is selected as the mixer in the second step, before mixing, an electronic balance weighing device is used for weighing iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder, and then the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder are poured into the mixer for continuous mixing, and protective gas is required to be added into the mixer in the mixing process to prevent the powder from being oxidized by oxygen in air in the mixing process.
The protective gas added in the mixing process of the mixer is argon with the purity of 99.999 percent.
Example 1:
the preparation method of the multi-principal element alloy target comprises the following specific preparation steps:
step one: preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for later use;
step two: 5 parts of iron powder, 1 part of cobalt powder, 3 parts of aluminum powder, 5 parts of silicon powder, 8 parts of chromium powder, 10 parts of zinc powder, 8 parts of titanium powder and 3 parts of nickel powder are poured into a mixer, and are continuously mixed and stirred for 10 minutes to obtain a mixture;
step three: pouring the product obtained in the third step into a vacuum hot press, firstly, performing a sintering stage, firstly, adjusting the temperature of the hot press to 800 ℃, continuously performing sintering for 80 minutes, then, adjusting the temperature of the hot press to 1850 ℃, continuously performing sintering for 100 minutes, cooling after the sintering is finished, and removing pressure after cooling to room temperature;
step four: performing machine treatment on the multi-element alloy target blank obtained in the step three to finally obtain a multi-element alloy target;
example 2:
the preparation method of the multi-principal element alloy target comprises the following specific preparation steps:
step one: preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for later use;
step two: pouring 5.5 parts of iron powder, 1.5 parts of cobalt powder, 3.5 parts of aluminum powder, 5.5 parts of silicon powder, 9 parts of chromium powder, 11 parts of zinc powder, 9 parts of titanium powder and 3.5 parts of nickel powder into a mixer, and continuously mixing and stirring for 15 minutes to obtain a mixture;
step three: pouring the product obtained in the third step into a vacuum hot press, firstly, performing a sintering stage, firstly, adjusting the temperature of the hot press to 900 ℃ for continuous sintering for 90 minutes, then, adjusting the temperature of the hot press to 1975 ℃ for continuous sintering for 110 minutes, cooling after the sintering is finished, and removing pressure after cooling to room temperature;
step four: performing machine treatment on the multi-element alloy target blank obtained in the step three to finally obtain a multi-element alloy target;
example 3:
the preparation method of the multi-principal element alloy target comprises the following specific preparation steps:
step one: preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for later use;
step two: pouring 6 parts of iron powder, 2 parts of cobalt powder, 4 parts of aluminum powder, 6 parts of silicon powder, 10 parts of chromium powder, 12 parts of zinc powder, 10 parts of titanium powder and 4 parts of nickel powder into a mixer, and continuously mixing and stirring for 20 minutes to obtain a mixture;
step three: pouring the product obtained in the third step into a vacuum hot press, firstly, performing a sintering stage, firstly, adjusting the temperature of the hot press to 1000 ℃ for continuous sintering for 100 minutes, then, adjusting the temperature of the hot press to 2100 ℃ for continuous sintering for 120 minutes, cooling after the sintering is finished, and removing pressure after cooling to room temperature;
step four: and (3) carrying out machine treatment on the multi-element alloy target blank obtained in the step (III) to finally obtain the multi-element alloy target.
While the fundamental and principal features of the invention and advantages of the invention have been shown and described, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but may be embodied in other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. The preparation method of the multi-principal-element alloy target is characterized by comprising the following specific preparation steps of:
step one: preparing corresponding powder of iron, cobalt, aluminum, silicon, chromium, zinc, titanium and nickel for later use;
step two: pouring 5-6 parts of iron powder, 1-2 parts of cobalt powder, 3-4 parts of aluminum powder, 5-6 parts of silicon powder, 8-10 parts of chromium powder, 10-12 parts of zinc powder, 8-10 parts of titanium powder and 3-4 parts of nickel powder into a mixer, and continuously mixing and stirring for 10-20 minutes to obtain a mixture;
step three: pouring the product obtained in the third step into a vacuum hot press, firstly, performing a sintering stage, firstly, adjusting the temperature of the hot press to 800-1000 ℃ for continuous sintering for 80-100 minutes, then, adjusting the temperature of the hot press to 1850-2100 ℃ for continuous sintering for 100-120 minutes, cooling after sintering, and removing pressure after cooling to room temperature;
step four: and (3) carrying out machine treatment on the multi-element alloy target blank obtained in the step (III) to finally obtain the multi-element alloy target.
2. The method for preparing the multi-principal element alloy target according to claim 1, wherein the method comprises the following steps: in the first step, the particle size range of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 10-20 microns, the purity of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 99.9-99.999%, and the oxygen content of the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder is 1-1800ppm.
3. The method for preparing the multi-principal element alloy target according to claim 1, wherein the method comprises the following steps: the multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 5 parts of iron powder, 1 part of cobalt powder, 3 parts of aluminum powder, 5 parts of silicon powder, 8 parts of chromium powder, 10 parts of zinc powder, 8 parts of titanium powder and 3 parts of nickel powder.
4. The method for preparing the multi-principal element alloy target according to claim 1, wherein the method comprises the following steps: the multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 5.5 parts of iron powder, 1.5 parts of cobalt powder, 3.5 parts of aluminum powder, 5.5 parts of silicon powder, 9 parts of chromium powder, 11 parts of zinc powder, 9 parts of titanium powder and 3.5 parts of nickel powder.
5. The method for preparing the multi-principal element alloy target according to claim 1, wherein the method comprises the following steps: the multi-principal element alloy target comprises the following specific raw material components in percentage by weight: 6 parts of iron powder, 2 parts of cobalt powder, 4 parts of aluminum powder, 6 parts of silicon powder, 10 parts of chromium powder, 12 parts of zinc powder, 10 parts of titanium powder and 4 parts of nickel powder.
6. The method for preparing the multi-principal element alloy target according to claim 1, wherein the method comprises the following steps: the vacuum hot press needs to be vacuumized to 0.0055-0.06Pa.
7. The method for preparing the multi-principal element alloy target according to claim 1, wherein the method comprises the following steps: the three-dimensional mixer is selected as the mixer in the second step, before mixing, an electronic balance weighing device is used for weighing iron powder, cobalt powder, aluminum powder, silicon powder, chromium powder, zinc powder, titanium powder and nickel powder, and then the iron powder, the cobalt powder, the aluminum powder, the silicon powder, the chromium powder, the zinc powder, the titanium powder and the nickel powder are poured into the mixer for continuous mixing, and protective gas is required to be added into the mixer in the mixing process to prevent the powder from being oxidized by oxygen in air in the mixing process.
8. The method for preparing the multi-principal element alloy target according to claim 7, wherein the method comprises the following steps: the protective gas added in the mixing process of the mixer is argon with the purity of 99.999 percent.
CN202211743620.5A 2022-12-22 2022-12-22 Preparation method of multi-principal element alloy target Pending CN116851753A (en)

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Application Number Priority Date Filing Date Title
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