CN115449767A - Preparation method of fine-grain high-purity nickel target material - Google Patents
Preparation method of fine-grain high-purity nickel target material Download PDFInfo
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- CN115449767A CN115449767A CN202211188785.0A CN202211188785A CN115449767A CN 115449767 A CN115449767 A CN 115449767A CN 202211188785 A CN202211188785 A CN 202211188785A CN 115449767 A CN115449767 A CN 115449767A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 204
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 102
- 239000013077 target material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 36
- 239000001257 hydrogen Substances 0.000 claims abstract description 36
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 230000008018 melting Effects 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 16
- 230000006698 induction Effects 0.000 claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 9
- 238000005097 cold rolling Methods 0.000 claims abstract description 9
- 238000005096 rolling process Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000003801 milling Methods 0.000 claims abstract description 6
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000008569 process Effects 0.000 description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 229910017604 nitric acid Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/06—Refining
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing 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
-
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention relates to a preparation method of a fine-grain high-purity nickel target material, belonging to the technical field of nickel target materials. The invention carries out vacuum melting on the high-purity nickel plate, and the vacuum degree reaches 1 multiplied by 10 0 When Pa is needed, introducing high-purity hydrogen, melting the hydrogen into a nickel melt in the hydrogen atmosphere, carrying out constant-temperature induction melting for more than 10min to fully dissolve the hydrogen into the nickel melt, and casting to obtain a nickel ingot; milling the surface of a nickel ingot, and then cold-rolling to obtain a cold-rolled nickel plate, wherein the total rolling deformation is 50-60%; and (3) uniformly heating the cold-rolled nickel plate to the temperature of 450-650 ℃, annealing for 0.5-2 h, and air cooling to room temperature to obtain the fine-grained high-purity nickel target material. The smelting under hydrogen atmosphere can removeThe metal nickel target material has the advantages of uniform structure and components, small grain size and remarkably reduced content of non-metallic impurities.
Description
Technical Field
The invention relates to a preparation method of a fine-grain high-purity nickel target material, belonging to the technical field of nickel target materials.
Background
With the development of industrial technology, thin film materials are widely applied in the fields of new energy, semiconductors and the like, and have high requirements on the quality of the thin film materials. Sputtering targets are a key material for forming thin films, and thus the technology for preparing targets with high quality requirements is becoming more important.
To obtain a high quality sputtered film, strict control is required on both the target purity and the grain size. In the aspect of purity, the target material purity can be applied to actual production only when the target material purity reaches more than 99.99 percent, because particles are formed on a wafer in the magnetron sputtering process when the impurity content in the target material is high, irreversible influence is caused on the quality of a film, and the service performance is seriously influenced. In terms of grain size: the grain size is below 100 μm to meet the requirement of high quality sputtering target, so repeated plastic deformation, heat treatment and other processes are required to accurately control the grain size. When the crystal grain of the target material is smaller, the higher the magnetron sputtering rate is, the better the quality of the film obtained by sputtering deposition is.
The two indexes of the material purity and the grain size are difficult to meet simultaneously in production, because the higher the purity of the pure metal material is, the fewer mechanisms for hindering the growth of grains are, the probability of heterogeneous nucleation is reduced in the metal solidification process, the pinning effect in the grain growth is weakened, and at the moment, the grains are easy to grow. Therefore, the method improves the purity of the target material and simultaneously realizes grain refinement, is the key for improving the sputtering performance and improving the coating quality, and is also the research focus of the research and development of the nickel-based target material at present.
Disclosure of Invention
The invention provides a preparation method of a fine-grain high-purity nickel target material aiming at the problem that the purity and the grain size are difficult to meet simultaneously in the preparation of the nickel target material.
A preparation method of a fine-grain high-purity nickel target material comprises the following specific steps:
(1) Vacuum smelting high-purity nickel plate to vacuum degree of 1 × 10 0 When Pa is needed, introducing high-purity hydrogen, melting the hydrogen into a nickel melt in the hydrogen atmosphere, carrying out constant-temperature induction melting for 10-20 min to fully dissolve the hydrogen into the nickel melt, and casting to obtain a nickel ingot;
(2) Milling the surface of a nickel ingot, and then cold-rolling to obtain a cold-rolled nickel plate, wherein the total rolling deformation is 50-60%;
(3) And (3) uniformly heating the cold-rolled nickel plate to the temperature of 450-650 ℃, annealing for 0.5-2 h, and air cooling to room temperature to obtain the fine-grained high-purity nickel target material.
The purity of the high-purity nickel plate in the step (1) is not lower than 99.99%;
the purity of the high-purity hydrogen in the step (1) is not lower than 99.999 percent;
the pressure of the hydrogen atmosphere in the step (1) is 5-20 KPa.
And (2) continuously carrying out constant-temperature induction melting in the casting process in the step (1), wherein the casting speed is 0.1-0.5 kg/s.
The cold rolling thickness deformation amount of the step (2) is 5-15%.
The constant temperature rise rate in the step (3) is 1-10 ℃/min.
The preparation principle of the fine-grain high-purity nickel target material is as follows: when pure nickel is smelted under the mixed hydrogen atmosphere, along with the increase of hydrogen partial pressure and the extension of heat preservation time, a part of hydrogen can be decomposed into hydrogen atoms, and the hydrogen atoms have extremely high reducibility and can react with impurities such as oxygen, carbon, sulfur and the like on the surface and in the metal to form gas and discharge the gas out of a melt, so that the effect of purifying the metal is achieved; hydrogen plays a certain role in dislocation, firstly, the hydrogen which is dissolved in nickel in a solid mode can reduce dislocation activation energy in the plastic deformation process, secondly, the hydrogen energy and impurity atoms form compound air mass, and the pinning effect of the impurity atoms on the dislocation is reduced, so that the starting of the dislocation is easier; the recrystallization process is accelerated, thereby obtaining the effect of grain refinement.
The beneficial effects of the invention are:
(1) The method has the advantages that the high-purity nickel is placed in the hydrogen atmosphere for induction melting, so that the non-metallic impurities in the melt can be effectively removed, particularly, the oxygen content is lower than 3ppm, and a nickel ingot with higher purity is obtained;
(2) The hydrogen dissolved in the nickel can reduce dislocation activation energy in the plastic deformation process, can obviously improve the plastic capability of the pure nickel, greatly relieves the edge crack phenomenon in the cold rolling process, and is easier to obtain fine and uniform recrystallized grains.
Drawings
FIG. 1 is a metallographic structure diagram of a high-purity fine-grained nickel target material according to example 1.
FIG. 2 is a metallographic structure diagram of a high-purity fine-grained nickel target material according to example 2.
FIG. 3 is a metallographic structure diagram of a high-purity fine-grained nickel target material according to example 3.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a preparation method of a fine-grain high-purity nickel target material comprises the following specific steps:
(1) Placing an anode nickel plate with the purity of 99.99% in a nitric acid solution for pickling for 3min to remove surface oxides and impurities, wherein the concentration of nitric acid is 15%; cleaning the acid liquor of the anode nickel plate by using distilled water, and removing the distilled water on the surface of the nickel plate by vacuum drying to obtain a pretreated nickel plate;
(2) Adding high-purity nickel plate into a vacuum furnace for vacuum melting, and when the vacuum degree reaches 1 multiplied by 10 0 When Pa is needed, introducing high-purity hydrogen with the purity of 99.999 percent to ensure that the hydrogen pressure in the vacuum furnace is 10Kpa, melting a nickel plate into a nickel melt in the hydrogen atmosphere, carrying out constant-temperature induction melting for 10min to ensure that the hydrogen is fully dissolved in the nickel melt, and casting the nickel melt into a graphite mold to obtain a nickel ingot; continuous constant-temperature induction smelting is carried out in the casting process, the power of the induction smelting is 40kW, and the casting speed is 0.3kg/s;
(3) The method comprises the following steps of milling the surface of a nickel ingot, then carrying out cold rolling to obtain a cold-rolled nickel plate, carrying out five-pass rolling, wherein the processing rates from the first pass to the fifth pass are respectively 5%, 10%, 15% and 15%, and the total rolling deformation is 50%;
(4) Uniformly heating the cold-rolled nickel plate to 500 ℃ at a heating rate of 5 ℃/min, annealing for 60min, and air-cooling to room temperature to obtain a fine-grain high-purity nickel target material;
the purity of the nickel plate in the embodiment is more than 99.99 percent, the metallographic structure diagram of the high-purity fine-grain nickel target material is shown in figure 1, and the average grain size is 51 mu m.
Example 2: a preparation method of a fine-grain high-purity nickel target material comprises the following specific steps:
(1) Placing an anode nickel plate with the purity of 99.99% in a nitric acid melt, and pickling for 4min to remove surface oxides and impurities, wherein the concentration of nitric acid is 14%; cleaning the acid liquor of the anode nickel plate by using distilled water, and removing the distilled water on the surface of the nickel plate by vacuum drying to obtain a pretreated nickel plate;
(2) Adding a high-purity nickel plate into a vacuum furnace for vacuum melting, and when the vacuum degree reaches 1 multiplied by 10 0 When Pa is needed, introducing high-purity hydrogen with the purity of 99.999 percent to ensure that the hydrogen pressure in the vacuum furnace is 20Kpa, melting a nickel plate into a nickel melt in the hydrogen atmosphere, carrying out constant-temperature induction melting for 15min to ensure that the hydrogen is fully dissolved in the nickel melt, and casting the nickel melt into a graphite mold to obtain a nickel ingot; continuous constant-temperature induction smelting is carried out in the casting process, the power of the induction smelting is 40kW, and the casting speed is 0.3kg/s;
(3) Milling the surface of a nickel ingot, then cold-rolling to obtain a cold-rolled nickel plate, and rolling in six passes, wherein the machining rates from the first pass to the sixth pass are respectively 5%, 10%, 15% and 15%, and the total rolling deformation is 60%;
(4) Uniformly heating the cold-rolled nickel plate to 450 ℃ at a heating rate of 8 ℃/min, annealing for 80min, and air-cooling to room temperature to obtain a fine-grain high-purity nickel target material;
the purity of the nickel plate of the embodiment is more than 99.99 percent, the metallographic structure diagram of the high-purity fine-grain nickel target material is shown in figure 2, and the average grain size is 37 mu m.
Example 3: a preparation method of a fine-grain high-purity nickel target material comprises the following specific steps:
(1) Placing an anode nickel plate with the purity of 99.99% in a nitric acid melt, and pickling for 5min to remove surface oxides and impurities, wherein the concentration of nitric acid is 12%; cleaning the acid liquor of the anode nickel plate by using distilled water, and removing the distilled water on the surface of the nickel plate by vacuum drying to obtain a pretreated nickel plate;
(2) Adding high-purity nickel plate into a vacuum furnace for vacuum melting, and when the vacuum degree reaches 1 multiplied by 10 0 When Pa is needed, introducing high-purity hydrogen with the purity of 99.999 percent to ensure that the pressure of the hydrogen in the vacuum furnace is 15Kpa, melting a nickel plate into a nickel melt in the hydrogen atmosphere, carrying out constant-temperature induction melting for 18min to ensure that the hydrogen is fully dissolved in the nickel melt, and casting the nickel melt into a graphite mold to obtain a nickel ingot; continuous constant-temperature induction smelting is carried out in the casting process, the power of the induction smelting is 35kW, and the casting speed is 0.2kg/s;
(3) The method comprises the following steps of milling the surface of a nickel ingot, then carrying out cold rolling to obtain a cold-rolled nickel plate, carrying out six-pass rolling, wherein the processing rates from the first pass to the sixth pass are respectively 5%, 10%, 15% and 15%, and the total rolling deformation is 55%;
(4) Uniformly heating the cold-rolled nickel plate to 600 ℃ at a heating rate of 6 ℃/min, annealing for 50min, and air-cooling to room temperature to obtain a fine-grain high-purity nickel target material;
the purity of the nickel plate of the embodiment is more than 99.99 percent, the metallographic structure diagram of the high-purity fine-grain nickel target material is shown in figure 3, and the average grain size is 34 mu m.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of a fine-grain high-purity nickel target material is characterized by comprising the following steps:
(1) Vacuum smelting high-purity nickel plate to vacuum degree of 1 × 10 0 When Pa is needed, introducing high-purity hydrogen, melting the hydrogen into a nickel melt in the hydrogen atmosphere, carrying out constant-temperature induction melting for more than 10min to fully dissolve the hydrogen into the nickel melt, and casting to obtain a nickel ingot;
(2) Milling the surface of a nickel ingot, and then cold-rolling to obtain a cold-rolled nickel plate, wherein the total rolling deformation is 50-60%;
(3) And (3) raising the temperature of the cold-rolled nickel plate to 450-650 ℃ at a constant speed, annealing for 0.5-2 h, and air cooling to room temperature to obtain the fine-grain high-purity nickel target material.
2. The method for preparing the fine-grained high-purity nickel target material according to claim 1, characterized by comprising the following steps: the pressure of the hydrogen atmosphere in the step (1) is 5-20 KPa.
3. The method for preparing the fine-grained high-purity nickel target material according to claim 1, characterized by comprising the following steps: and (2) continuously carrying out constant-temperature induction melting in the casting process in the step (1), wherein the casting speed is 0.1-0.5 kg/s.
4. The method for preparing the fine-grained high-purity nickel target material according to claim 1, characterized by comprising the following steps: and (3) the cold rolling single-pass thickness deformation amount in the step (2) is 5-15%.
5. The method for preparing the fine-grained high-purity nickel target material according to claim 1, characterized by comprising the following steps: the constant temperature rise rate in the step (3) is 1-10 ℃/min.
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| CN202211188785.0A CN115449767A (en) | 2022-09-28 | 2022-09-28 | Preparation method of fine-grain high-purity nickel target material |
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| CN202211188785.0A CN115449767A (en) | 2022-09-28 | 2022-09-28 | Preparation method of fine-grain high-purity nickel target material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0790398A (en) * | 1993-09-27 | 1995-04-04 | Minoru Isshiki | Production of high purity metal |
| JP2000038622A (en) * | 1998-07-23 | 2000-02-08 | Minoru Isshiki | Purification and refinement of transition metal |
| WO2003062488A1 (en) * | 2002-01-24 | 2003-07-31 | Nikko Materials Company, Limited | High-purity nickel or nickel alloy sputtering target, and its manufacturing method |
| CN101307429A (en) * | 2008-07-14 | 2008-11-19 | 中南大学 | Process for preparing high-purity metallic nickel target of superfine crystal particle |
| 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 |
| CN113387336A (en) * | 2021-06-15 | 2021-09-14 | 中南大学 | Method for removing selenium from tellurium ingot |
-
2022
- 2022-09-28 CN CN202211188785.0A patent/CN115449767A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0790398A (en) * | 1993-09-27 | 1995-04-04 | Minoru Isshiki | Production of high purity metal |
| JP2000038622A (en) * | 1998-07-23 | 2000-02-08 | Minoru Isshiki | Purification and refinement of transition metal |
| WO2003062488A1 (en) * | 2002-01-24 | 2003-07-31 | Nikko Materials Company, Limited | High-purity nickel or nickel alloy sputtering target, and its manufacturing method |
| CN101307429A (en) * | 2008-07-14 | 2008-11-19 | 中南大学 | Process for preparing high-purity metallic nickel target of superfine crystal particle |
| 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 |
| CN113387336A (en) * | 2021-06-15 | 2021-09-14 | 中南大学 | Method for removing selenium from tellurium ingot |
Non-Patent Citations (1)
| Title |
|---|
| 北京钢铁学院 等: "《金属学及热处理》", vol. 1, 中国工业出版社, pages: 298 - 299 * |
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