CN112609087A - Cold bed electron beam smelting method of high-purity nickel ingot - Google Patents
Cold bed electron beam smelting method of high-purity nickel ingot Download PDFInfo
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- CN112609087A CN112609087A CN202011394772.XA CN202011394772A CN112609087A CN 112609087 A CN112609087 A CN 112609087A CN 202011394772 A CN202011394772 A CN 202011394772A CN 112609087 A CN112609087 A CN 112609087A
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- 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
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
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- 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
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Abstract
The invention discloses a cold bed electron beam melting method of a high-purity nickel ingot, which comprises the following steps: s1, selecting a high-purity electrolytic nickel plate as a raw material, polishing, cleaning and drying the high-purity electrolytic nickel plate by using a cleaning solution, recording the weight, orderly placing the high-purity electrolytic nickel plate into a bin of an electron beam furnace for fixing, and vacuumizing the electron beam furnace; s2, preheating and powering the electron gun, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 2-4min, and making the nickel melt flow into an ingot casting crucible after the nickel melt is fully deflated to obtain a nickel ingot; s3, closing the electron gun and the vacuum system in sequence, opening the electron beam furnace, and taking out the nickel ingot prepared in the step S2. The method solves the problem of internal defects in the smelting process of the nickel ingot, and improves the product percent of pass and the production efficiency.
Description
Technical Field
The invention relates to the technical field of metal smelting, in particular to a cold bed electron beam smelting method of a high-purity nickel ingot.
Background
The high-purity nickel ingot is an important raw material of a sputtering nickel target material for semiconductors, and is mainly used as a coating material of integrated circuits and microelectronic thin film materials.
The conventional method adopts secondary smelting of nickel ingots, and the nickel ingots obtained by the secondary smelting of electron beams can remove most of defects in the ingots, but the secondary smelting has relatively high cost, long smelting time and low efficiency, and the nickel ingots need to be treated again after being discharged from a furnace, so that new polluted products are very easily introduced by lifting, installation and the like, and the quality of the products is not easy to keep stable.
Disclosure of Invention
The invention aims to provide a cold bed electron beam melting method of a high-purity nickel ingot aiming at the defects in the prior art, which solves the problem of internal defects of the nickel ingot in the melting process and improves the product percent of pass and the production efficiency.
In order to achieve the purpose, the invention adopts the technical scheme that:
the cold bed electron beam smelting process of high purity nickel ingot includes the following steps:
s1, selecting a high-purity electrolytic nickel plate as a raw material, polishing the high-purity electrolytic nickel plate, cleaning and drying the high-purity electrolytic nickel plate by using a cleaning solution, recording the weight of the high-purity electrolytic nickel plate, orderly placing the high-purity electrolytic nickel plate into a bin of an electron beam furnace for fixing, and vacuumizing the electron beam furnace;
s2, preheating an electron gun, adding 400KW of power 350KW, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 2-4min, and after the nickel melt is fully deflated, flowing the nickel melt into an ingot casting crucible with the power of 280KW and 300KW to prepare a nickel ingot;
s3, closing the electron gun and the vacuum system in sequence, opening the electron beam furnace, and taking out the nickel ingot prepared in the step S2.
Preferably, in S1, the electrolytic nickel plate has a purity of 99.95%.
Preferably, in S1, the cleaning solution contains dilute sulfuric acid.
Preferably, in S1, the high-purity electrolytic nickel plate is dried by using a vacuum drying oven.
Preferably, in S2, the electron gun power on the cooling bed is 350 KW.
Preferably, in S2, the power of the ingot crucible is 280 KW.
Preferably, in S3, the vacuum system is turned off 4h after the electron gun is turned off.
Preferably, in S3, the electron gun 12h is turned off and then the electron beam furnace is turned on.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the method can complete the smelting only once, so that the smelting cost is saved by half, the time is saved by half, and the efficiency is greatly improved; meanwhile, the smelting is carried out once, so that midway pollution is avoided, the product quality is more stable, the stay time of the raw materials on the cooling bed can be controlled, the raw materials are more fully deflated, and the internal defects of the nickel ingot can be completely avoided.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention provides a cold bed electron beam melting method of a high-purity nickel ingot, which comprises the following steps:
s1, selecting an electrolytic nickel plate with the purity of 99.95% as a raw material, polishing the high-purity electrolytic nickel plate, cleaning the high-purity electrolytic nickel plate by using a cleaning solution, drying the high-purity electrolytic nickel plate in a vacuum drying oven, recording the weight of the high-purity electrolytic nickel plate, orderly placing the high-purity electrolytic nickel plate into a bin of an electron beam furnace for fixing, and vacuumizing the electron beam furnace;
s2, preheating an electron gun and adding 400KW of power, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 2-4min, after the nickel melt is fully deflated, enabling the nickel melt to flow into an ingot casting crucible with the power of 280KW and 300KW, completing smelting for a small period, repeating for several times until all the high-purity electrolytic nickel plates in the bin are melted, and completing smelting to obtain a nickel ingot;
and S3, sequentially closing the electron guns, closing the vacuum system after 4 hours, opening the electron beam furnace after 12 hours, and taking out the nickel ingot prepared in the step S2.
In S1, the cleaning solution contains dilute sulfuric acid to clean the oxide film and the dirt on the surface of the electrolytic nickel plate, so as to prevent the introduction of the dirt from affecting the product quality.
As a preferred embodiment, in S2, the electron gun power on the cooling bed is 350 KW; the power of the ingot casting crucible is 280KW, so that the electrolytic nickel plate is uniformly and stably heated in the process of bombarding the electrolytic nickel plate.
The method can complete the smelting only once, so that the smelting cost is saved by half, the time is saved by half, and the efficiency is greatly improved; meanwhile, the smelting is carried out once, so that midway pollution is avoided, the product quality is more stable, the stay time of the raw materials on the cooling bed can be controlled, the raw materials are more fully deflated, and the internal defects of the nickel ingot can be completely avoided.
Example 1
The embodiment provides a cold bed electron beam melting method of a high-purity nickel ingot, which comprises the following steps:
s1, selecting an electrolytic nickel plate with the purity of 99.95% as a raw material, polishing the high-purity electrolytic nickel plate, cleaning the high-purity electrolytic nickel plate by using a cleaning solution and drying the high-purity electrolytic nickel plate in a vacuum drying oven, wherein the cleaning solution contains dilute sulfuric acid, so that an oxide film and dirt on the surface of the electrolytic nickel plate are removed completely, the introduction of the pollutants is prevented from influencing the product quality, the high-purity electrolytic nickel plate is orderly placed in a bin of an electron beam furnace to be fixed after the weight of the high-purity electrolytic nickel plate is recorded, and the electron beam furnace is vacuumized;
s2, preheating an electron gun, applying 350KW of power, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 2min, after the nickel melt is fully deflated, enabling the nickel melt to flow into an ingot casting crucible, wherein the power of the ingot casting crucible is 280KW, completing smelting for a small period, repeating for several times until all the high-purity electrolytic nickel plates in the bin are completely melted, and completing smelting to obtain a nickel ingot;
and S3, sequentially closing the electron guns, closing the vacuum system after 4 hours, opening the electron beam furnace after 12 hours, and taking out the nickel ingot prepared in the step S2.
Example 2
The embodiment provides a cold bed electron beam melting method of a high-purity nickel ingot, which comprises the following steps:
s1, selecting an electrolytic nickel plate with the purity of 99.95% as a raw material, polishing the high-purity electrolytic nickel plate, cleaning the high-purity electrolytic nickel plate by using a cleaning solution and drying the high-purity electrolytic nickel plate in a vacuum drying oven, wherein the cleaning solution contains dilute sulfuric acid, so that an oxide film and dirt on the surface of the electrolytic nickel plate are removed completely, the introduction of the pollutants is prevented from influencing the product quality, the high-purity electrolytic nickel plate is orderly placed in a bin of an electron beam furnace to be fixed after the weight of the high-purity electrolytic nickel plate is recorded, and the electron beam furnace is vacuumized;
s2, preheating an electron gun and applying 380KW of power, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 3min, after the nickel melt is fully deflated, enabling the nickel melt to flow into an ingot casting crucible with the power of 290KW, finishing smelting for a small period, repeating for several times until all the high-purity electrolytic nickel plates in the bin are completely melted, and finishing smelting to obtain a nickel ingot;
and S3, sequentially closing the electron guns, closing the vacuum system after 4 hours, opening the electron beam furnace after 12 hours, and taking out the nickel ingot prepared in the step S2.
Example 3
The embodiment provides a cold bed electron beam melting method of a high-purity nickel ingot, which comprises the following steps:
s1, selecting an electrolytic nickel plate with the purity of 99.95% as a raw material, polishing the high-purity electrolytic nickel plate, cleaning the high-purity electrolytic nickel plate by using a cleaning solution and drying the high-purity electrolytic nickel plate in a vacuum drying oven, wherein the cleaning solution contains dilute sulfuric acid, so that an oxide film and dirt on the surface of the electrolytic nickel plate are removed completely, the introduction of the pollutants is prevented from influencing the product quality, the high-purity electrolytic nickel plate is orderly placed in a bin of an electron beam furnace to be fixed after the weight of the high-purity electrolytic nickel plate is recorded, and the electron beam furnace is vacuumized;
s2, preheating an electron gun, applying 400KW of power, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 4min, after the nickel melt is fully deflated, enabling the nickel melt to flow into an ingot casting crucible with the power of 300KW, finishing smelting for a small period, repeating for several times until all the high-purity electrolytic nickel plates in the bin are completely melted, and finishing smelting to obtain a nickel ingot;
and S3, sequentially closing the electron guns, closing the vacuum system after 4 hours, opening the electron beam furnace after 12 hours, and taking out the nickel ingot prepared in the step S2.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A cold bed electron beam melting method of high-purity nickel ingots is characterized by comprising the following steps:
s1, selecting a high-purity electrolytic nickel plate as a raw material, polishing the high-purity electrolytic nickel plate, cleaning and drying the high-purity electrolytic nickel plate by using a cleaning solution, recording the weight of the high-purity electrolytic nickel plate, orderly placing the high-purity electrolytic nickel plate into a bin of an electron beam furnace for fixing, and vacuumizing the electron beam furnace;
s2, preheating an electron gun, adding 400KW of power 350KW, starting a material pushing mechanism after the electron gun is stabilized, sequentially pushing the high-purity electrolytic nickel plates in the bin fixed in the step S1 into a cooling bed to be completely melted to form a nickel melt, staying the nickel melt on the cooling bed for 2-4min, and after the nickel melt is fully deflated, flowing the nickel melt into an ingot casting crucible with the power of 280KW and 300KW to prepare a nickel ingot;
s3, closing the electron gun and the vacuum system in sequence, opening the electron beam furnace, and taking out the nickel ingot prepared in the step S2.
2. The cold bed electron beam melting method of a high purity nickel ingot as claimed in claim 1, wherein the purity of the electrolytic nickel plate in S1 is 99.95%.
3. The method for cold bed electron beam melting of a high purity nickel ingot according to claim 1, wherein in S1, the cleaning solution contains dilute sulfuric acid.
4. The cold bed electron beam melting method of a high purity nickel ingot as claimed in claim 1, wherein in S1, the high purity electrolytic nickel plate is dried by using a vacuum drying oven.
5. The cold bed electron beam melting method of high purity nickel ingot as claimed in claim 1, wherein in S2, the electron gun power on the cold bed is 350 KW.
6. The cold bed electron beam melting method of high purity nickel ingot as claimed in claim 1, wherein in S2, the ingot crucible power is 280 KW.
7. The method for cold bed electron beam melting of a high purity nickel ingot as claimed in claim 1, wherein in S3, the vacuum system is turned off 4 hours after the electron gun is turned off.
8. The cold bed electron beam melting method of high purity nickel ingot as claimed in claim 1, wherein in S3, the electron beam furnace is opened after the electron gun is turned off for 12 hours.
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Citations (7)
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CN103484691A (en) * | 2013-09-13 | 2014-01-01 | 攀枝花云钛实业有限公司 | Nickel and nickel alloy EB furnace smelting method |
CN104190885A (en) * | 2014-08-28 | 2014-12-10 | 云南钛业股份有限公司 | Method for producing huge high-purity nickel ingot square billets through four-gun electron beam cold bed furnace |
CN106399721A (en) * | 2016-08-27 | 2017-02-15 | 宝鸡众有色金属材料有限公司 | Preparation technique of high-purity nickel ingot for semiconductor target |
CN106702176A (en) * | 2015-07-17 | 2017-05-24 | 宁波创润新材料有限公司 | Melting method for bottom ingot used in electron beam cold hearth |
CN106987727A (en) * | 2016-01-20 | 2017-07-28 | 宁波创润新材料有限公司 | Method of smelting |
CN109014088A (en) * | 2017-06-12 | 2018-12-18 | 宁波创润新材料有限公司 | Method of smelting |
CN110578061A (en) * | 2018-06-07 | 2019-12-17 | 湖南稀土金属材料研究院 | Electron beam melting continuous ingot casting method for high-purity rare earth metal |
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2020
- 2020-12-02 CN CN202011394772.XA patent/CN112609087A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103484691A (en) * | 2013-09-13 | 2014-01-01 | 攀枝花云钛实业有限公司 | Nickel and nickel alloy EB furnace smelting method |
CN104190885A (en) * | 2014-08-28 | 2014-12-10 | 云南钛业股份有限公司 | Method for producing huge high-purity nickel ingot square billets through four-gun electron beam cold bed furnace |
CN106702176A (en) * | 2015-07-17 | 2017-05-24 | 宁波创润新材料有限公司 | Melting method for bottom ingot used in electron beam cold hearth |
CN106987727A (en) * | 2016-01-20 | 2017-07-28 | 宁波创润新材料有限公司 | Method of smelting |
CN106399721A (en) * | 2016-08-27 | 2017-02-15 | 宝鸡众有色金属材料有限公司 | Preparation technique of high-purity nickel ingot for semiconductor target |
CN109014088A (en) * | 2017-06-12 | 2018-12-18 | 宁波创润新材料有限公司 | Method of smelting |
CN110578061A (en) * | 2018-06-07 | 2019-12-17 | 湖南稀土金属材料研究院 | Electron beam melting continuous ingot casting method for high-purity rare earth metal |
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