CN108203806B - Method for manufacturing nickel target material - Google Patents

Method for manufacturing nickel target material Download PDF

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Publication number
CN108203806B
CN108203806B CN201611186151.6A CN201611186151A CN108203806B CN 108203806 B CN108203806 B CN 108203806B CN 201611186151 A CN201611186151 A CN 201611186151A CN 108203806 B CN108203806 B CN 108203806B
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nickel
cleaning
plate
square
centrifugal
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CN108203806A (en
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姚力军
潘杰
相原俊夫
王学泽
曹欢欢
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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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
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method for producing a nickel target, comprising: forming a nickel plate; polishing the nickel plate; and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material. Because the metal nickel has good mechanical strength and strong capability of resisting deformation and fracture when bearing external force, the metal nickel is suitable for processing modes such as polishing, grinding and the like. Oxide and impurities on the surface of the nickel plate can be effectively removed through a polishing mode, then the impurities on the surface of the nickel plate are further removed through a centrifugal grinding mode, and the cleanliness of the nickel target material is effectively improved through the polishing and centrifugal grinding combined mode.

Description

Method for manufacturing nickel target material
Technical Field
The invention relates to the field of target material manufacturing, in particular to a nickel target material manufacturing method.
Background
Physical Vapor Deposition (PVD) is a core technology in various industries such as the semiconductor industry. It mainly uses gas discharge to evaporate the target material and ionize the evaporated material and gas, and uses the accelerating action of electric field to make the evaporated material and its reaction product deposit on the workpiece. Therefore, the purity and cleanliness of the target material are of critical importance.
A general method of preparing a target product comprises: providing a metal that meets the target properties, such as high purity nickel (typically 99.99%); and carrying out processes such as preheating, extrusion forming, rough machining, finish machining and the like on the metal, and finally machining the metal into a target product with qualified size. However, the extrusion process, heat treatment, etc. tend to degrade the cleanliness of the metal, resulting in reduced performance of the formed target material.
Disclosure of Invention
The invention aims to provide a method for manufacturing a nickel target material so as to improve the cleanliness of the nickel target material.
In order to solve the above problems, the present invention provides a method for manufacturing a nickel target, including: forming a nickel plate; polishing the nickel plate; and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material.
Optionally, after polishing the nickel plate and before centrifugal grinding, the manufacturing method further includes: manufacturing the nickel plate into a nickel square sheet; pickling the nickel square sheet; and in the step of centrifugal grinding, the nickel square pieces after acid washing are subjected to centrifugal grinding.
Optionally, the step of centrifugal grinding is performed within a centrifugal grinder drum; the step of centrifugal grinding comprises: placing the nickel square pieces in a drum of a centrifugal grinder, wherein the drum charge is less than or equal to one third of the depth of the drum.
Optionally, the step of centrifugal grinding is performed within a centrifugal grinder drum; the step of centrifugal grinding comprises adding 30ml to 50ml of grinding agent into a roller of the centrifugal grinding machine.
Optionally, the rotation speed of the centrifugal grinding is 180-200 rpm, and the centrifugal grinding time is 10-20 minutes.
Optionally, after the centrifugal grinding, the nickel square pieces are dried.
Optionally, the drying step comprises: and screening and draining the nickel square sheets after centrifugal grinding, and drying the nickel square sheets after screening and draining by adopting an air gun.
Optionally, the step of pickling comprises: putting the nickel square sheet into aviation kerosene for first cleaning; transferring the nickel square sheet subjected to the first cleaning into an isopropanol solution, and performing second cleaning; transferring the nickel square sheets subjected to the second cleaning into an acid solution, and performing third cleaning; putting the nickel square slice subjected to the third cleaning into pure water for pure water cleaning; and drying the nickel square slice cleaned by the pure water.
Optionally, in the step of performing acid washing, the nickel square pieces are placed in a roller to perform the first washing, the second washing and the third washing; keeping the roller still in the step of performing the first cleaning and the second cleaning; in the step of performing the third washing, the drum is kept rolling.
Optionally, in the steps of performing the first cleaning, the second cleaning, and the pure water cleaning, the nickel square piece is subjected to ultrasonic oscillation.
Optionally, in the first cleaning step, the time for performing ultrasonic oscillation is 10 minutes to 20 minutes; in the second cleaning step, the time for ultrasonic oscillation is 5 to 15 minutes; in the step of pure water cleaning, the time for ultrasonic oscillation is 5 to 10 minutes.
Optionally, the acid solution is a nitric acid solution, wherein the mass ratio of nitric acid is 15-20%; the acid washing time is 3-5 minutes.
Optionally, the step of forming the nickel plate includes: providing as-cast nickel; forging the as-cast nickel; milling the forged cast nickel to manufacture a nickel ingot; and rolling the nickel ingot to manufacture a nickel plate.
Optionally, the forging step includes: forging and preheating the as-cast nickel; forging and molding the preheated as-cast nickel; and cooling the as-cast nickel after forging and forming.
Optionally, the preset temperature range of the forging preheating is 850-950 ℃.
Optionally, the forging deformation amount is between 30% and 60%.
Optionally, the step of cooling treatment includes placing the as-cast nickel in normal temperature water for cooling within 2 minutes after forging and forming.
Optionally, the step of calendering comprises: carrying out rough rolling on the nickel ingot to manufacture a rough rolled nickel plate; annealing heat treatment is carried out on the rough rolled nickel plate and cooling is carried out; slitting the rough rolled nickel plate; and carrying out finish rolling on the cut rough rolling aluminum plate to manufacture the nickel plate.
Optionally, the rough rolling step includes: and rolling the nickel ingot to a rough rolling nickel plate with the thickness of 5-7 mm, wherein the reduction of each pass of rough rolling is less than 1mm, and the rough rolling temperature is within the range of 500-600 ℃.
Optionally, the annealing heat treatment temperature is in a range of 500-600 ℃, the heat preservation time is in a range of 2-3 hours, and the cooling treatment method is to cool the rough rolled nickel plate in normal temperature water.
Optionally, the finish rolling step includes: and rolling the slit rough rolling aluminum plate to a nickel plate with the thickness of 1.8-2.2 mm, wherein the reduction of each pass of finish rolling is less than 1 mm.
Optionally, after the nickel target is manufactured, the method further includes the steps of placing the nickel target in a clean room for cleaning, drying before packaging, and packaging.
Optionally, the step of cleaning treatment includes: and placing the nickel target material in an isopropanol solution for ultrasonic oscillation for 5-10 minutes.
Optionally, the step of drying before packaging comprises: and carrying out vacuum drying on the nickel target material in a vacuum drying oven, wherein the vacuum degree of the vacuum drying oven is 0.01-0.03 pascal, the temperature is 60-80 ℃, and the drying time is 50-70 minutes.
Compared with the prior art, the technical scheme of the invention has the following advantages:
in the scheme of the invention, a nickel plate is formed; polishing the nickel plate; and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material. Because the metal nickel has good mechanical strength and strong capability of resisting deformation and fracture when bearing external force, the metal nickel is suitable for processing modes such as polishing, grinding and the like. Oxide and impurities on the surface of the nickel plate can be effectively removed through a polishing mode, then the impurities on the surface of the nickel plate are further removed through a centrifugal grinding mode, and the cleanliness of the nickel target material is effectively improved through the polishing and centrifugal grinding combined mode.
In the alternative, a step of acid washing the nickel square pieces is provided, and due to the high corrosion resistance of the metal nickel, the acid washing can remove oxides and other impurities on the surfaces of the nickel square pieces, and the metal nickel body cannot be damaged, so that the cleanliness of the nickel square pieces after acid washing is improved.
Drawings
FIG. 1 is a schematic flow chart of a method for producing a nickel target according to the present invention;
FIG. 2 is a schematic flow chart of step S1 of the embodiment shown in FIG. 1;
FIG. 3 is a schematic flow chart of step S12 of the embodiment shown in FIG. 2;
FIG. 4 is a schematic flow chart of step S14 of the embodiment shown in FIG. 2;
FIG. 5 is a flowchart illustrating the steps S3 after step S2 in the embodiment of FIG. 1;
fig. 6 is a schematic flow chart of step S22 in the embodiment shown in fig. 5.
Detailed Description
As can be seen from the background art, in the process of forming a target material in the prior art, the cleanliness of the metal is easily reduced by adopting the steps of extrusion forming process, heat treatment and the like, thereby causing the problem of reduced performance of the formed target material.
In order to solve the technical problem, the invention provides a method for manufacturing a nickel target, which comprises the following steps: forming a nickel plate; polishing the nickel plate; and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material.
The invention forms nickel plate; polishing the nickel plate; and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material. Because the metal nickel has good mechanical strength and strong capability of resisting deformation and fracture when bearing external force, the metal nickel is suitable for processing modes such as polishing, grinding and the like. Oxide and impurities on the surface of the nickel plate can be effectively removed through a polishing mode, then the impurities on the surface of the nickel plate are further removed through a centrifugal grinding mode, and the cleanliness of the nickel target material is effectively improved through the polishing and centrifugal grinding combined mode.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Referring to fig. 1, a flow chart of an embodiment of the method for manufacturing a nickel target according to the present invention is shown, wherein the method for manufacturing a nickel target includes the following basic steps:
step S1: forming a nickel plate;
step S2: polishing the nickel plate;
step S3: and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material.
In order to better illustrate the method for manufacturing the aluminum target according to the embodiment of the present invention, the following will further describe an embodiment of the present invention with reference to fig. 2 to 6.
Referring to fig. 2, a flow chart of step S1 of the embodiment shown in fig. 1 is shown.
The step of forming the nickel plate includes:
step S11: providing as-cast nickel;
step S12: forging the as-cast nickel;
step S13: milling the forged cast nickel to manufacture a nickel ingot;
step S14: and rolling the nickel ingot to manufacture a nickel plate.
The flow of S1 is further described below.
Step S11: as-cast nickel is provided. The as-cast nickel is used to form a target.
The as-cast nickel may be a portion cut from an ingot. The shape of the as-cast nickel may be any of circular, rectangular, annular, conical, or other similar shapes (including regular and irregular shapes) depending on the application environment, the actual requirements of the PVD apparatus. In this example, the purity of the as-cast nickel was 99.99%.
Step S12: forging the as-cast nickel.
Referring to fig. 3, a flow chart of step S12 of the embodiment shown in fig. 2 is shown.
The forging step includes:
step S110: forging and preheating the as-cast nickel;
step S111: forging and molding the preheated as-cast nickel;
step S112: and cooling the as-cast nickel after forging and forming.
The flow of step S12 is further described below.
Step S110: and forging and preheating the as-cast nickel. Through forging preheating treatment, the internal structure of the metal can be changed, so that the metal is relieved of stress and softened, the plasticity of the metal is improved, and a good foundation is laid for subsequent forging forming.
The preheating treatment comprises the following steps: the as-cast nickel is placed in a chamber of a heat treatment apparatus (e.g., a thermostatic furnace) having a protective atmosphere (e.g., an inert gas) therein, and specifically, the as-cast nickel is placed in a region capable of being uniformly heated, such as: placing as-cast nickel in a geometrically central region of the chamber; and raising the temperature in the chamber to a preset temperature and keeping the temperature at the preset temperature for a period of time to realize preheating. The preset temperature and time of the preheating treatment can be preset according to actual needs; and cooling the cast nickel to return to normal temperature.
If the predetermined temperature is too high, the as-cast nickel may cause heating defects and even waste. If the preheating temperature is too low, the plasticity of the as-cast nickel is reduced during deformation. In this embodiment, the predetermined temperature range of the forging preheating is 850 to 950 ℃.
Step S120: and forging and molding the preheated as-cast nickel. Through the forging forming process, the cast nickel can be deformed, and a nickel ingot which meets the size required by the subsequent rolling process is manufactured.
In the present embodiment, the forging deformation amount ranges from 30% to 60%.
Step S130: and cooling the as-cast nickel after forging and forming. In this embodiment, the step of cooling includes placing the as-cast nickel in normal temperature water for cooling within 2 minutes after forging and forming. In other embodiments of the present invention, cooling by air cooling, pit cooling, or furnace cooling may be employed.
With continued reference to fig. 2, step S13: and milling the forged cast nickel to prepare a nickel ingot. The milling process is used for removing surface oxide layers, folds, wrinkles and the like after forging.
Step S14: and rolling the nickel ingot to manufacture a nickel plate.
Referring to fig. 4, a flowchart of step S14 of the embodiment shown in fig. 2 is shown.
The calendering step comprises:
step S210: carrying out rough rolling on the nickel ingot to manufacture a rough rolled nickel plate;
step S220: annealing heat treatment is carried out on the rough rolled nickel plate and cooling is carried out;
step S230: slitting the rough rolled nickel plate;
step S240: and carrying out finish rolling on the cut rough rolling aluminum plate to manufacture the nickel plate.
The flow of step S14 is further described below.
Step S210: and carrying out rough rolling on the nickel ingot to manufacture a rough rolled nickel plate.
Specifically, the rough rolling step includes: and rolling the nickel ingot to a rough rolling nickel plate with the thickness of 5-7 mm, wherein the reduction of each pass of rough rolling is less than 1mm, and the rough rolling temperature is within the range of 500-600 ℃.
Step S220: and carrying out annealing heat treatment on the rough rolled nickel plate and cooling.
Specifically, the heat treatment temperature of the annealing heat treatment is within the range of 500-600 ℃, the heat preservation time is within the range of 2-3 hours, and the cooling treatment method is to place the rough rolled nickel plate in normal temperature water for cooling.
Step S230: and slitting the rough rolled nickel plate. And slitting the rough rolled nickel plate to a size meeting the requirement of subsequent finish rolling.
Step S240: and carrying out finish rolling on the cut rough rolling aluminum plate to manufacture the nickel plate.
Specifically, the finish rolling step includes: and rolling the slit rough rolling aluminum plate to a nickel plate with the thickness of 1.8-2.2 mm, wherein the reduction of each pass of finish rolling is less than 1 mm.
With continued reference to fig. 1, step S2: and polishing the nickel plate. The polishing is used for removing an oxide layer and other attachments formed on the surface of the nickel plate after finish rolling.
Because the metal nickel has good mechanical strength and strong capability of resisting deformation and fracture when bearing external force, the polishing processing mode is suitable to be adopted. The oxide and impurities on the surface of the nickel plate can be effectively removed through a polishing mode, so that the cleanliness of the nickel target material is effectively improved.
Referring to FIG. 5, a flowchart of the embodiment shown in FIG. 1 is shown after step S2 and step S3.
After the nickel plate is polished and before centrifugal grinding, the manufacturing method further comprises the following steps:
step S21: manufacturing the nickel plate into a nickel square sheet;
step S22: pickling the nickel square sheet;
step S23: and in the step of centrifugal grinding, the nickel square pieces after acid washing are subjected to centrifugal grinding.
The flow after step S2 and step S3 is further described below.
Step S21: and manufacturing the nickel plate into a nickel square sheet. The nickel square sheet is prepared for subsequent pickling, so that the pickling process is easier to operate.
The method for forming the nickel square piece includes: putting the nickel plate into a punch die, and punching and blanking to form a nickel square sheet. In the present embodiment, since the gauge of the produced nickel target material is 10mm × 10mm, the gauge of the nickel square piece in the step of forming the nickel square piece by pressing is 10mm × 10 mm.
Step S22: and carrying out acid washing on the nickel square sheet. The acid washing can effectively remove oxides and other impurities on the surface of the nickel square piece.
Referring to fig. 6, a flow chart of step S22 in the embodiment shown in fig. 5 is shown.
The pickling step comprises:
step S310: putting the nickel square sheet into aviation kerosene for first cleaning;
step S320: transferring the nickel square sheet subjected to the first cleaning into an isopropanol solution, and performing second cleaning;
step S330: transferring the nickel square sheets subjected to the second cleaning into an acid solution, and performing third cleaning;
step S340: putting the nickel square slice subjected to the third cleaning into pure water for pure water cleaning;
step S350: and drying the nickel square slice cleaned by the pure water.
The flow of step S22 will be further described below.
Step S310: and putting the nickel square sheet into aviation kerosene for first cleaning. The first cleaning is used for removing oil stains remained on the nickel square sheets in the stamping and blanking process. In other embodiments of the present invention, the nickel square piece may be immersed in a cleaning agent such as a detergent or pure water.
In the step of performing the acid washing, the nickel square pieces are placed in a drum to perform the first washing; in the step of performing the first washing, the drum is kept stationary.
In this embodiment, in the step of performing the first cleaning, the nickel square pieces are subjected to ultrasonic oscillation; the time for performing the ultrasonic oscillation is 10 to 20 minutes.
Step S320: and transferring the nickel square sheet subjected to the first cleaning into an isopropanol solution, and carrying out second cleaning. The second cleaning is used for removing the aviation kerosene remained on the nickel square pieces in the first cleaning process. In other embodiments of the present invention, the aviation kerosene may be removed by using a cleaning agent such as alcohol.
In the present embodiment, in the step of performing the acid washing, the nickel square pieces are placed in a drum to perform the second washing, and the drum is kept still. In other embodiments of the present invention, the rollers may also be kept rolling.
In this embodiment, in the second cleaning step, the nickel square pieces are subjected to ultrasonic oscillation; the ultrasonic oscillation is carried out for 5 to 15 minutes.
Step S330: and transferring the nickel square pieces subjected to the second cleaning into acid liquor, and carrying out third cleaning. The third cleaning is used for further removing the oxide and other impurities on the surface of the nickel square piece. In the embodiment, the acid solution is a nitric acid solution, wherein the mass ratio of nitric acid is 15-20%; the acid washing time is 3-5 minutes.
In the present embodiment, in the step of performing the acid washing, the nickel square pieces are placed in a roller and the third cleaning is performed, so that the roller is kept rolling.
Because the corrosion resistance of the metal nickel is high, the oxide and other impurities on the surface of the nickel square piece can be removed by acid washing, and the metal nickel body can not be damaged, so that the cleanliness of the nickel square piece after acid washing is improved.
Step S340: and placing the nickel square slice subjected to the third cleaning in pure water for pure water cleaning. The pure water cleaning is used for removing acid liquor residues on the surfaces of the nickel square pieces.
In the step of performing the pure water cleaning, the nickel square pieces are subjected to ultrasonic oscillation for 5 to 10 minutes.
Step S350: and drying the nickel square slice cleaned by the pure water. In this embodiment, the nickel square piece is dried by an air gun. In other embodiments of the invention, drying can also be carried out in a drying or natural air drying manner.
With continued reference to fig. 5, step S23: and in the step of centrifugal grinding, the nickel square pieces after acid washing are subjected to centrifugal grinding. The centrifugal grinding is used for polishing the surface of the nickel square piece to remove surface color difference.
Because the metal nickel has good mechanical strength and strong capability of resisting deformation and fracture when bearing external force, the metal nickel is suitable for processing modes such as grinding and the like. Impurities on the surface of the nickel plate are further removed in a centrifugal grinding mode, and the cleanliness of the nickel target material is effectively improved in a polishing and centrifugal grinding combined mode.
In particular, the step of centrifugal grinding is performed within a centrifugal grinder bowl. The step of centrifugal grinding comprises: placing the nickel square pieces in a roller of a centrifugal grinder.
The roller feed cannot be too much, and if too much, overheating and uneven stirring of the material and the grinding sleeve are easily caused. Thus, the drum charge is less than or equal to one third of the drum depth.
Specifically, the step of centrifugal grinding comprises adding 30-50 ml of grinding agent into the roller of the centrifugal grinding machine.
Specifically, the rotation speed of the centrifugal grinding is 180-200 revolutions per minute, and the centrifugal grinding time is 10-20 minutes.
In this example, the nickel square pieces were dried after the centrifugal grinding.
Specifically, the drying step includes: and screening and draining the nickel square sheets after centrifugal grinding, and drying the nickel square sheets after screening and draining by adopting an air gun.
In this embodiment, after the nickel target is manufactured, the method further includes the steps of placing the nickel target in a clean room for cleaning, drying before packaging, and packaging. Therefore, impurities on the surface of the nickel square piece are further removed, and the nickel target with high cleanliness is obtained.
Specifically, the cleaning treatment includes: and placing the nickel target material in an isopropanol solution for ultrasonic oscillation for 5-10 minutes.
Specifically, the step of drying before packaging comprises: and carrying out vacuum drying on the nickel target material in a vacuum drying oven, wherein the vacuum degree of the vacuum drying oven is 0.01-0.03 pascal, the temperature is 60-80 ℃, and the drying time is 50-70 minutes.
In conclusion, the scheme of the invention forms the nickel plate; polishing the nickel plate; and (4) carrying out centrifugal grinding on the polished nickel plate to prepare the nickel target material. Because the metal nickel has good mechanical strength and strong capability of resisting deformation and fracture when bearing external force, the metal nickel is suitable for processing modes such as polishing, grinding and the like. Oxide and impurities on the surface of the nickel plate can be effectively removed through a polishing mode, then the impurities on the surface of the nickel plate are further removed through a centrifugal grinding mode, and the cleanliness of the nickel target material is effectively improved through the polishing and centrifugal grinding combined mode.
In addition, the scheme of the invention provides a step of pickling the nickel square sheets, and the pickling can remove oxides and other impurities on the surfaces of the nickel square sheets due to the high corrosion resistance of the metal nickel, and can not damage the metal nickel body, so that the cleanliness of the pickled nickel square sheets is improved.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (19)

1. A method for producing a nickel target, comprising:
forming a nickel plate;
polishing the nickel plate;
carrying out centrifugal grinding on the polished nickel plate to manufacture a nickel target material; the step of centrifugal grinding is performed within a centrifugal grinder drum; the step of centrifugal grinding comprises adding 30-50 ml of grinding agent into a roller of the centrifugal grinder; the rotation speed of the centrifugal grinding is 180-200 r/min, and the centrifugal grinding time is 10-20 min;
after the nickel plate is polished and before centrifugal grinding, the manufacturing method further comprises the following steps: manufacturing the nickel plate into a nickel square sheet; pickling the nickel square sheet; in the step of centrifugal grinding, the nickel square sheets after acid cleaning are subjected to centrifugal grinding;
the pickling step comprises:
putting the nickel square sheet into aviation kerosene for first cleaning;
transferring the nickel square sheet subjected to the first cleaning into an isopropanol solution, and performing second cleaning;
transferring the nickel square sheets subjected to the second cleaning into an acid solution, and performing third cleaning; the acid solution is nitric acid solution, wherein the mass ratio of nitric acid is 15-20%; the pickling time is 3 to 5 minutes;
putting the nickel square slice subjected to the third cleaning into pure water for pure water cleaning;
and drying the nickel square slice cleaned by the pure water.
2. The method of manufacturing of claim 1, wherein the step of centrifugal grinding is performed within a centrifugal grinder bowl; the step of centrifugal grinding comprises: placing the nickel square pieces in a drum of a centrifugal grinder, wherein the drum charge is less than or equal to one third of the depth of the drum.
3. The method of claim 1, wherein the nickel square pieces are dried after the centrifugal grinding.
4. The method of claim 3, wherein the step of drying comprises: and screening and draining the nickel square sheets after centrifugal grinding, and drying the nickel square sheets after screening and draining by adopting an air gun.
5. The method according to claim 1, wherein in the step of performing acid washing, the nickel square piece is placed in a roller to perform the first washing, the second washing, and the third washing; keeping the roller still in the step of performing the first cleaning and the second cleaning; in the step of performing the third washing, the drum is kept rolling.
6. The manufacturing method according to claim 1, wherein ultrasonic oscillation is performed on the nickel square piece in the steps of performing the first cleaning, the second cleaning, and the pure water cleaning.
7. The method according to claim 6, wherein in the first cleaning step, the ultrasonic oscillation is performed for 10 to 20 minutes; in the second cleaning step, the time for ultrasonic oscillation is 5 to 15 minutes; in the step of pure water cleaning, the time for ultrasonic oscillation is 5 to 10 minutes.
8. The method of manufacturing of claim 1, wherein the step of forming the nickel plate comprises: providing as-cast nickel;
forging the as-cast nickel;
milling the forged cast nickel to manufacture a nickel ingot;
and rolling the nickel ingot to manufacture a nickel plate.
9. The method of claim 8, wherein the step of forging comprises:
forging and preheating the as-cast nickel;
forging and molding the preheated as-cast nickel;
and cooling the as-cast nickel after forging and forming.
10. The method of claim 9, wherein the predetermined temperature range of the forging preheat is 850 degrees celsius to 950 degrees celsius.
11. The method of claim 9, wherein the forging strain is between 30% and 60%.
12. The method of claim 9, wherein the step of cooling comprises cooling the as-cast nickel in water at room temperature within 2 minutes after forging and forming.
13. The method of manufacturing of claim 8, wherein said step of calendering comprises:
carrying out rough rolling on the nickel ingot to manufacture a rough rolled nickel plate;
annealing heat treatment is carried out on the rough rolled nickel plate and cooling is carried out;
slitting the rough rolled nickel plate;
and carrying out finish rolling on the cut rough rolling aluminum plate to manufacture the nickel plate.
14. The method of manufacturing of claim 13, wherein the step of rough rolling comprises: and rolling the nickel ingot to a rough rolling nickel plate with the thickness of 5-7 mm, wherein the reduction of each pass of rough rolling is less than 1mm, and the rough rolling temperature is within the range of 500-600 ℃.
15. The manufacturing method according to claim 13, wherein the annealing heat treatment is performed at a heat treatment temperature in a range of 500 to 600 degrees celsius and a holding time in a range of 2 to 3 hours, and the cooling treatment is performed by cooling the rough rolled nickel plate in normal temperature water.
16. The method of claim 13, wherein said step of finish rolling comprises: and rolling the slit rough rolling aluminum plate to a nickel plate with the thickness of 1.8-2.2 mm, wherein the reduction of each pass of finish rolling is less than 1 mm.
17. The method of claim 1, wherein after the nickel target is produced, the method further comprises the steps of placing the nickel target in a clean room for cleaning, drying before packaging, and packaging.
18. The method of manufacturing of claim 17, wherein the step of cleaning comprises: and placing the nickel target material in an isopropanol solution for ultrasonic oscillation for 5-10 minutes.
19. The method of claim 17, wherein the step of pre-packaging drying comprises: and carrying out vacuum drying on the nickel target material in a vacuum drying oven, wherein the vacuum degree of the vacuum drying oven is 0.01-0.03 pascal, the temperature is 60-80 ℃, and the drying time is 50-70 minutes.
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CN87213371U (en) * 1987-09-16 1988-10-05 江苏省无锡县机械厂 Horizontal centrifugal grinder

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US8556681B2 (en) * 2007-01-29 2013-10-15 Tosoh Smd, Inc. Ultra smooth face sputter targets and methods of producing same
WO2009123055A1 (en) * 2008-04-03 2009-10-08 日鉱金属株式会社 Low particulate-generating sputtering target
CN102864421A (en) * 2011-07-05 2013-01-09 北京有色金属研究总院 Method for producing fine grain high-purity Ni target

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JPS61113759A (en) * 1984-11-09 1986-05-31 Matsushita Electric Ind Co Ltd Target for sputtering
CN87213371U (en) * 1987-09-16 1988-10-05 江苏省无锡县机械厂 Horizontal centrifugal grinder

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