CN1360071A - High-temp vacuum induction smelting and desulfurizing technology for preparing super-purity alloy - Google Patents
High-temp vacuum induction smelting and desulfurizing technology for preparing super-purity alloy Download PDFInfo
- Publication number
- CN1360071A CN1360071A CN00134346A CN00134346A CN1360071A CN 1360071 A CN1360071 A CN 1360071A CN 00134346 A CN00134346 A CN 00134346A CN 00134346 A CN00134346 A CN 00134346A CN 1360071 A CN1360071 A CN 1360071A
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- Prior art keywords
- desulfurization
- vacuum induction
- cao
- alloy
- refining
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 17
- 239000000956 alloy Substances 0.000 title claims abstract description 17
- 238000003723 Smelting Methods 0.000 title claims abstract description 8
- 230000006698 induction Effects 0.000 title claims abstract description 6
- 238000005516 engineering process Methods 0.000 title claims description 6
- 230000003009 desulfurizing effect Effects 0.000 title abstract description 4
- 238000005275 alloying Methods 0.000 claims abstract description 8
- 238000007670 refining Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000006477 desulfuration reaction Methods 0.000 claims description 12
- 230000023556 desulfurization Effects 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 239000011819 refractory material Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 230000003014 reinforcing effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 3
- 230000000887 hydrating effect Effects 0.000 abstract 1
- 229910000601 superalloy Inorganic materials 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000002498 deadly effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Classifications
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Manufacture And Refinement Of Metals (AREA)
- Treatment Of Steel In Its Molten State (AREA)
Abstract
An efficient desulfurizing process for high-temp vacuum induction smelting of alloy is characterized by that the refractory CaO material with higher purity (over 98.9%), high thermodynamic stability and low hydrating speed is used as crucible, and includes such steps as smelting, pre-refining, alloying by adding Al and Ca as strong desulfurizing element, and post-refining. Its advantages is low S content (less than 5 ppm).
Description
The invention belongs to the vacuum metallurgy field, be applicable to the nickel base superalloy of smelting ultrapure clean S content.
The vapour pressure that CaO is low, high basicity, good Thermodynamically stable may play a significant role it as refractory materials in the VIM of superalloy.Just, in industrial production, be difficult at present be applied because there is the deadly defect of easy aquation in CaO.Applicant at first works out anti-hydratability CaO refractory materials (patent of invention number: 97103854.6), use this refractory materials, and in conjunction with the desulfurization smelting technology of pureization of this patented invention, realized that melting superalloy S's is ultrapure clean preferably.
The technological process of melting super low sulfur desulfurization superalloy of the present invention is: concise phase of concise phase charging → melting period → preceding → alloying phase → back → casting, concrete operations are as follows:
1. in the disposable crucibles of packing into of main raw material such as the loading sequence of alloy: C, Ni, Cr, Co, W, Mo, Nb, Ta, the material alloying buckets of packing into such as Al, Ti, Ni-B, Ca.
2. alloy melting phase: melted alloy fusing main raw material under the high vacuum, realize that will there be good carbon deoxidation melting period.
3. the preceding concise phase: capacity after main raw materialization is clear, is warming up to 1600 ℃, concise time 10～15min less than the smelting of 200Kg alloy.Capacity is greater than the melting of the above alloy of 500Kg, but concise time proper extension, and this concise phase mainly acts on the carbon deoxidation that is.
4. alloying phase: preceding concise after date, molten steel are cooled to about 1380 ℃, add Al, Ti, add fashionable gradually preface and add, and the stirring of following simultaneously prevents the gravity segregation of Al, Ti.Al, Ti add, and logical Ar to 400mmHg adds Ca (total add-on is less than 0.1wt%) under protective atmosphere, stir molten steel.The strong sweetening agent Ca that alloying adds, effectively desulfurization.
5. the concise phase after: the main effect of concise phase of back is desulfurization.After adding Al, Ti, Ca, vacuumize, be warming up to 1650 ℃, concise 10～15min.Adopt higher refining temperature, utilize the good stirring of induction melting, increased the velocity of diffusion of S, reduce the boundary layer thickness of sulphur at the CaO crucible surface, make S accelerate, strengthened the thermodynamics and kinetics of desulfurization, improve desulfurization rate in the renewal speed of strong basicity CaO crucible surface, realization molten alloy S's is ultrapure clean
6. the cast of alloy: the concise phase of back finishes, and adjusts the temperature of molten steel, cast.
Below by embodiment in detail the present invention is described in detail.
Embodiment
Adopt the art of this patent to smelt casting and wrought superalloy, capacity is from 10Kg to 350Kg, and the S content of alloy is all reduced to below the 10ppm, alloy performance high and stablize, the results are shown in Table 1.Now this technology can be smelted the superalloy of low S content in batches, and realization molten alloy S's is ultrapure clean.
The S content (ppm) and the performance of alloy under table 1 new desulfurization process
| Alloy | Capacity (Kg) | ????S | Senior middle school's temperature creep rupture life (hr) |
| ??DZ17G | ??20 | ????1 | 71 (standard: 980 ℃/216MPa 〉=32hr) 249 (760 ℃/725MPa) |
| ??DZ125 | ??20 | ????1.5 | 73,97.5 (standard: 980 ℃/216MPa 〉=32hr) 296 (760 ℃/800MPa) |
| ??IN738 | ??20 | ????1 | 114,151,130 (standard: 982 ℃/152MPa 〉=30hr) |
| The M17 returns | ??250 | ????7 | 198 (standard: 900 ℃/315MPa 〉=40hr) |
| Newly develop alloy | ??50 | ????5 |
Claims (1)
1. a vacuum induction is smelted the new technology of desulfurization, it is characterized in that: use purity higher (CaO＞98.9%), thermodynamic stability is good, hydration rate the is lower CaO refractory materials crucible material as vacuum induction melting; Smelting technology comprises: melting period, preceding refining period, alloying phase and back refining period, preceding refining period molten liquid steel have under the prerequisite of certain deoxidation, behind the alloying phase adding Al, improve the back refining temperature in refining period, the thermodynamics and kinetics condition of reinforcing desulfuration, carry out effective desulfurization at the CaO sidewall of crucible, the alloying phase adds strong desulfurization Elements C a simultaneously, by following reaction, further desulfurization, both combine, and the S content of virgin material alloy can be reduced to below the 5ppm, and the S content of returns is reduced to below the 10ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001343467A CN1137275C (en) | 2000-12-21 | 2000-12-21 | High-temp vacuum induction smelting and desulfurizing technology for preparing super-purity alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001343467A CN1137275C (en) | 2000-12-21 | 2000-12-21 | High-temp vacuum induction smelting and desulfurizing technology for preparing super-purity alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1360071A true CN1360071A (en) | 2002-07-24 |
| CN1137275C CN1137275C (en) | 2004-02-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001343467A Expired - Lifetime CN1137275C (en) | 2000-12-21 | 2000-12-21 | High-temp vacuum induction smelting and desulfurizing technology for preparing super-purity alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1137275C (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643876B (en) * | 2008-08-08 | 2011-02-02 | 中国科学院金属研究所 | Super-pure smelting method for industrially producing Incone1690 alloy |
| CN102296200A (en) * | 2011-08-30 | 2011-12-28 | 江苏大学 | Alloy for nickel-based high-temperature alloy refining and using method thereof |
| CN102534122A (en) * | 2010-12-08 | 2012-07-04 | 中国科学院金属研究所 | Ultrapure smelting method of low-alloy high-strength steel |
| CN102776378A (en) * | 2012-07-30 | 2012-11-14 | 攀钢集团江油长城特殊钢有限公司 | Desulfurization method of high temperature alloy smelted by vacuum induction furnace |
| CN103276231A (en) * | 2013-05-17 | 2013-09-04 | 中国航空工业集团公司北京航空材料研究院 | Method for removing S and O from cast superalloy by vacuum induction smelting |
| CN105624473A (en) * | 2016-03-30 | 2016-06-01 | 山东瑞泰新材料科技有限公司 | Vacuum smelting technology for high-temperature alloy |
| CN105803233A (en) * | 2016-03-30 | 2016-07-27 | 山东瑞泰新材料科技有限公司 | Melting technology of nickel-base alloy containing aluminum titanium boron zirconium |
| CN108559860A (en) * | 2018-06-11 | 2018-09-21 | 江苏集萃先进金属材料研究所有限公司 | A kind of device and method for nickel-base alloy vacuum induction melting high-efficiency desulfurization |
| CN108913922A (en) * | 2018-07-23 | 2018-11-30 | 江苏美特林科特殊合金股份有限公司 | The sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy |
| CN109423535A (en) * | 2017-08-29 | 2019-03-05 | 宝钢特钢有限公司 | A kind of technology of high-temperature alloy vacuum induction melting depth desulfurization |
| CN110872653A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院金属研究所 | Smelting method for controlling nitrogen content in Inconel690 alloy |
| CN112522541A (en) * | 2019-09-17 | 2021-03-19 | 东北大学 | Nickel-based alloy desulfurizing agent and preparation method thereof |
| CN114317891A (en) * | 2022-01-05 | 2022-04-12 | 任超群 | Vacuum induction melting desulfurization process for alloy steel |
| CN115323117A (en) * | 2022-07-28 | 2022-11-11 | 中国科学院金属研究所 | Smelting method for deep desulfurization of high-temperature alloy |
-
2000
- 2000-12-21 CN CNB001343467A patent/CN1137275C/en not_active Expired - Lifetime
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643876B (en) * | 2008-08-08 | 2011-02-02 | 中国科学院金属研究所 | Super-pure smelting method for industrially producing Incone1690 alloy |
| CN102534122A (en) * | 2010-12-08 | 2012-07-04 | 中国科学院金属研究所 | Ultrapure smelting method of low-alloy high-strength steel |
| CN102534122B (en) * | 2010-12-08 | 2013-08-21 | 中国科学院金属研究所 | Ultrapure smelting method of low-alloy high-strength steel |
| CN102296200A (en) * | 2011-08-30 | 2011-12-28 | 江苏大学 | Alloy for nickel-based high-temperature alloy refining and using method thereof |
| CN102776378A (en) * | 2012-07-30 | 2012-11-14 | 攀钢集团江油长城特殊钢有限公司 | Desulfurization method of high temperature alloy smelted by vacuum induction furnace |
| CN102776378B (en) * | 2012-07-30 | 2014-04-30 | 攀钢集团江油长城特殊钢有限公司 | Desulfurization method of high temperature alloy smelted by vacuum induction furnace |
| CN103276231A (en) * | 2013-05-17 | 2013-09-04 | 中国航空工业集团公司北京航空材料研究院 | Method for removing S and O from cast superalloy by vacuum induction smelting |
| CN105803233A (en) * | 2016-03-30 | 2016-07-27 | 山东瑞泰新材料科技有限公司 | Melting technology of nickel-base alloy containing aluminum titanium boron zirconium |
| CN105624473A (en) * | 2016-03-30 | 2016-06-01 | 山东瑞泰新材料科技有限公司 | Vacuum smelting technology for high-temperature alloy |
| CN105624473B (en) * | 2016-03-30 | 2017-10-13 | 山东瑞泰新材料科技有限公司 | The vacuum metling technique of high temperature alloy |
| CN109423535A (en) * | 2017-08-29 | 2019-03-05 | 宝钢特钢有限公司 | A kind of technology of high-temperature alloy vacuum induction melting depth desulfurization |
| CN108559860A (en) * | 2018-06-11 | 2018-09-21 | 江苏集萃先进金属材料研究所有限公司 | A kind of device and method for nickel-base alloy vacuum induction melting high-efficiency desulfurization |
| CN108913922A (en) * | 2018-07-23 | 2018-11-30 | 江苏美特林科特殊合金股份有限公司 | The sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy |
| CN110872653A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院金属研究所 | Smelting method for controlling nitrogen content in Inconel690 alloy |
| CN110872653B (en) * | 2018-09-04 | 2021-08-10 | 中国科学院金属研究所 | Smelting method for controlling nitrogen content in Inconel690 alloy |
| CN112522541A (en) * | 2019-09-17 | 2021-03-19 | 东北大学 | Nickel-based alloy desulfurizing agent and preparation method thereof |
| CN114317891A (en) * | 2022-01-05 | 2022-04-12 | 任超群 | Vacuum induction melting desulfurization process for alloy steel |
| CN115323117A (en) * | 2022-07-28 | 2022-11-11 | 中国科学院金属研究所 | Smelting method for deep desulfurization of high-temperature alloy |
| CN115323117B (en) * | 2022-07-28 | 2024-01-19 | 中国科学院金属研究所 | Smelting method for deep desulfurization of high-temperature alloy |
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| Publication number | Publication date |
|---|---|
| CN1137275C (en) | 2004-02-04 |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Danyang Precision Alloy Factory Co., Ltd. Assignor: Institute of metal research, Chinese Academy of Sciences Contract fulfillment period: 2007.1.18 to 2012.1.18 Contract record no.: 2008320001061 Denomination of invention: High-temp vacuum induction smelting and desulfurizing technology for preparing super-purity alloy Granted publication date: 20040204 License type: Exclusive license Record date: 20081027 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.1.18 TO 2012.1.18; CHANGE OF CONTRACT Name of requester: DANYANG CITY PRECISE ALLOY FACTORY CO., LTD. Effective date: 20081027 |
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Granted publication date: 20040204 |