CN103695659A - Method for improving purity of nickel-based superalloy - Google Patents
Method for improving purity of nickel-based superalloy Download PDFInfo
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- CN103695659A CN103695659A CN201310719750.XA CN201310719750A CN103695659A CN 103695659 A CN103695659 A CN 103695659A CN 201310719750 A CN201310719750 A CN 201310719750A CN 103695659 A CN103695659 A CN 103695659A
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Abstract
The invention relates to a method for improving the purity of nickel-based superalloy, which belongs to the field of alloy smelting. The method for improving the purity of nickel-based superalloy comprises the following process steps: increasing a beam to 200 mA at a speed of 1 mA/s under a vacuum degree of less than 0.05 Pa in the furnace body of an electron beam smelting device and a vacuum degree of less than 0.005 Pa of an electron gun body, and bombarding the beam onto a nickel-based superalloy substrate until the alloy is completely smelted; after the nickel-based superalloy substrate is completely smelted, continuing to increase the electron gun beam to 400 mA at a speed of 2 mA/s, adjusting the beam spot radius of the electron beam to 15*15, smelting the alloy for 5 minutes, and then cooling. According to the method, O, N and S in the alloy as well as harmful impurity elements such as As, Sb, Si, Pb and Bi can be greatly reduced, thus improving the purity of the alloy in the aspect of reducing the contents of the harmful elements, and then improving the comprehensive performance of the nickel-based superalloy.
Description
Technical field
The present invention relates to a kind of method that improves nickel base superalloy purity, belong to alloy melting field.
Background technology
Nickel base superalloy is for the indispensable class important materials of the various high temperature component of aircraft engine, space rocket engine and industry gas turbine.Because it has good hot strength and antioxidant anticorrosive performance, excellent creep resistance, anti-fatigue performance and Duan Lie Ni, and the alloying level of superalloy is very high, thereby be also referred to as superalloy (Superalloy) at American-European countries's superalloy.Superalloy is widely used in each industrial circles such as Aeronautics and Astronautics, the energy, communications and transportation, chemical industry, in particular for making production aircraft engine and industry gas turbine aspect: as the four large component such as misfortune impeller blade, turning vane, misfortune wheel disc and combustion chamber almost make by superalloy.By the evaporative effect of element under high vacuum environment, can effectively remove the impurity element in alloy, thereby eliminate the metallurgical imperfection producing in fusion process, improve the comprehensive mechanical property of nickel base superalloy.But not yet find that relevant electron beam melting improves the report of alloy purity at present.
The method that tradition is prepared superalloy is to utilize vacuum induction melting and the preparation of vacuum arc remelting duplex technique.The shortcomings such as contaminating impurity that duplex technique itself has that production efficiency is low, process is loaded down with trivial details and introduces due to technique conversion, and in single melting technology, in vacuum induction melting process, there is the problem of introducing other impurity, mainly that refractory materials can increase oxide inclusion content with reacting also of melt, affect its purity, electric arc reflow process exists and can not remove sulphur and phosphorus in addition, and the size of inclusion is larger, there is dendroid and white-spot defects, the problem such as the surface quality of ingot casting is poor.Simultaneously in traditional preparation technology, the vacuum environment in fusion process is not enough to allow the impurity atoms removal of volatilizing from alloy melt, and this also makes alloy purity be difficult to be improved.
Summary of the invention
The object of this invention is to provide a kind of method that improves nickel base superalloy purity, the method adopts electron beam melting technology to carry out remelting to nickel-base alloy mother metal.
Improve a method for nickel base superalloy purity, described method is electron beam remelting method, specifically comprises following processing step:
In electron beam melting device body of heater, vacuum tightness is less than 5 * 10
-2pa, electron gun vacuum tightness is less than 5 * 10
-3pa, increases line to 200mA with 1mA/s speed, and sweep radius is 10 * 10, makes its bombardment to nickel base superalloy substrate until alloy melts completely; After nickel base superalloy substrate melts completely, continuing increases electron beam gun line to 400mA with 2mA/s speed, and electron beam spot radius is adjusted into 15 * 15, carries out alloy melting, and the time is 5min～10min, rear cooling.
Nickel base superalloy of the present invention can business be buied, and is preferably Inconel 718 alloys; Described substrate is preferably sheet material or bulk.
In aforesaid method, the radius of described electron beam spot is the circular electron beam bundle spot that 15 * 15 finger radiuses are 15mm.
In aforesaid method, in described electron beam melting device body of heater, vacuum tightness is less than 5 * 10
-2pa, electron gun vacuum tightness is less than 5 * 10
-3under Pa, this vacuum tightness is without lower limit requirement; In preferred electron bundle smelting apparatus body of heater, vacuum tightness is 5 * 10
-3pa～5 * 10
-2pa, electron gun vacuum tightness is 5 * 10
-4pa～5 * 10
-3pa.
Present method electronic beam vacuum smelting technology used can be used for pure metal purifies and alloy melting, and it has melting under (1) high vacuum environment, and during melting, vacuum tightness is generally 10
-1～10
-3pa; (2) the concentrated feature of beam energy, makes molten bath reach very high temperature, is not only conducive to improve the effect of Refining, and can be used for melting refractory metal; (3) controllability of electron beam is good, so can control by controlling electron beam the heating position in molten bath, thereby guarantee that bath temperature is evenly distributed, be conducive to obtain surface quality and the good ingot metal of crystal structure, by electron beam remelting technology, and in conjunction with element the saturated vapor pressure relation under vacuum environment, formulate corresponding melting technology, effectively remove the impurity atoms in alloy, thereby improve preferably the purity of nickel base superalloy.
The method of raising nickel base superalloy purity of the present invention is described coolingly carry out as follows preferably: the speed with 1.35mA/s is down to zero by line, closes subsequently electron beam gun, after body of heater and the cooling 30min～60min of electron gun, and taking-up.
The preferred described method of method of raising nickel base superalloy purity of the present invention comprises the pretreated step of nickel base superalloy substrate, specific as follows:
Use sand paper to carry out surface finish processing to nickel base superalloy substrate, the use of sand paper is sequentially followed successively by: 200#, 600#, 1000#, 1500#; With being placed in deionized water, cleaning and dry, drying time is 3～5h, and bake out temperature is 50～80 degree.
Beneficial effect of the present invention is: the present invention is by the high-energy-density of electron beam, the melting characteristics of condition of high vacuum degree, the nickel-base alloy mother metal of having prepared is carried out to electron beam remelting, according to the relation of smelting time and monitor system, determine melting technology, can greatly reduce the content of O in alloy, N, from reducing the purity containing measuring angle raising alloy of harmful element, and then improve the over-all properties of nickel base superalloy.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of method described in embodiment 1;
Fig. 2 is is the schematic diagram of embodiment 1 electron beam melting device used;
Reference numeral is as follows: 1. diffusion pump 2. mechanical pump 3. nickel base superalloy 4. crucible holder 5. cooling water pipeline 6. electron beam gun 7. pneumavalve 8. electron beam 9. water jacketed copper crucible 10. lobe pumps
Said apparatus, is comprised of left and right sides electron beam gun 6, body of heater, water-cooling system, vacuum pump system, and wherein two electron beam gun 8 are connected with diffusion pump 1 and mechanical pump 2, to electron beam gun 6 is evacuated to 5 * 10
-3below.The bottom of body of heater is provided with for taking up the water jacketed copper crucible 9 of nickel base superalloy 3, and water jacketed copper crucible 9 is fixed on body of heater inside by crucible holder 4; Body of heater is connected with diffusion pump 1, lobe pump 10, mechanical pump 2 respectively, to its vacuum tightness is evacuated to 5 * 10
-2below.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Test method described in following embodiment, if no special instructions, is ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1
One, the pre-treatment of nickel base superalloy
1, choose commercially available nickel base superalloy Inconel 718 alloy cube matherials, use Wire EDM to be cut to the circular nickel-base alloy piece that is of a size of Φ 100mm * 8mm.
2, first on starting material, get sub-fraction and do composition detection;
3, use sand paper to carry out surface finish processing to nickel-base alloy piece, remove surperficial zone of oxidation and impurity enriched region, guarantee the purity of the front alloy of melting.Till treating the extremely clean light of sample surfaces polishing, the use of sand paper is sequentially followed successively by: 200#, 600#, 1000#, 1500#.With being placed in deionized water, cleaning and dry, drying time is 5h, and bake out temperature is 50 degree.
Two, electron beam remelting technology is removed impurity element atom
1, circular block nickel-base alloy is steadily positioned in the water jacketed copper crucible of electron beam melting device, unlocking electronic bundle smelting apparatus, startup mechanical pump, lobe pump, diffusion pump are evacuated to target vacuum state by body of heater and rifle body successively, wherein vacuum tightness 5 * 10 in body of heater
-3pa, electron gun vacuum tightness is less than 5 * 10
-4pa.
2, start electron beam gun after reaching target vacuum degree, with 1mA/s speed, slowly increase line to 200mA, sweep radius is 10 * 10, and adjust electron beam scanning pattern is circular spot simultaneously, and its bombardment is melted until alloy melts completely to Inconel718 superalloy substrate and slowly.
3, after alloy melts completely, continuing slowly increases electron beam gun line to 400mA with 2mA/s speed, and electron beam spot radius is adjusted into 15 * 15, carries out alloy melting, and the time is 5min.
4, after said process, with the speed of 1.35mA/s, line is down to zero, closes subsequently electron beam gun, after body of heater and the cooling 60min of rifle body, reach the abundant state of cooling, take out sample, detect micro-atom O, N in alloy.
Utilize electron beam remelting technology can reduce significantly the content of impurity element atom, O, N constituent content in Inconel 718 alloys are brought down below respectively 0.0005%, 0.0146% by 0.005%, 0.0201%.
One, the pre-treatment of nickel base superalloy
1, choose commercially available nickel base superalloy Inconel 718 alloy cube matherials, use Wire EDM to be cut to the circular nickel-base alloy piece that is of a size of Φ 100mm * 8mm.
2, first on starting material, get sub-fraction and do composition detection;
3, use sand paper to carry out surface finish processing to nickel-base alloy piece, remove surperficial zone of oxidation and impurity enriched region, guarantee the purity of the front alloy of melting.Till treating the extremely clean light of sample surfaces polishing, the use of sand paper is sequentially followed successively by: 200#, 600#, 1000#, 1500#.With being placed in deionized water, cleaning and dry, drying time is 4h, and bake out temperature is 65 degree.
Two, electron beam remelting technology is removed impurity element atom
1, circular block nickel-base alloy is steadily positioned in the water jacketed copper crucible of electron beam melting device, unlocking electronic bundle smelting apparatus, startup mechanical pump, lobe pump, diffusion pump are evacuated to target vacuum state by body of heater and rifle body successively, wherein vacuum tightness 3 * 10 in body of heater
-2pa, electron gun vacuum tightness is less than 3 * 10
-3pa.
2, start electron beam gun after reaching target vacuum degree, with 1mA/s speed, slowly increase line to 200mA, sweep radius is 10 * 10, and adjust electron beam scanning pattern is circular spot simultaneously, and its bombardment is melted until alloy melts completely to Inconel718 superalloy substrate and slowly.
3, after alloy melts completely, continuing slowly increases electron beam gun line to 400mA with 2mA/s speed, and electron beam spot radius is adjusted into 15 * 15, carries out alloy melting, and the time is 8min.
4, after said process, with the speed of 1.35mA/s, line is down to zero, closes subsequently electron beam gun, after body of heater and the cooling 45min of rifle body, reach the abundant state of cooling, take out sample, detect micro-atom O, N in alloy.
Utilize electron beam remelting technology can reduce significantly the content of impurity element atom, O, N constituent content in Inconel 718 alloys are brought down below respectively 0.0004%, 0.0147% by 0.005%, 0.0201%.
One, the pre-treatment of nickel base superalloy
1, choose commercially available nickel base superalloy Inconel 718 alloy cube matherials, use Wire EDM to be cut to the circular nickel-base alloy piece that is of a size of Φ 100mm * 8mm.
2, first on starting material, get sub-fraction and do composition detection;
3, use sand paper to carry out surface finish processing to nickel-base alloy piece, remove surperficial zone of oxidation and impurity enriched region, guarantee the purity of the front alloy of melting.Till treating the extremely clean light of sample surfaces polishing, the use of sand paper is sequentially followed successively by: 200#, 600#, 1000#, 1500#.With being placed in deionized water, cleaning and dry, drying time is 3h, and bake out temperature is 80 degree.
Two, electron beam remelting technology is removed impurity element atom
1, circular block nickel-base alloy is steadily positioned in the water jacketed copper crucible of electron beam melting device, unlocking electronic bundle smelting apparatus, startup mechanical pump, lobe pump, diffusion pump are evacuated to target vacuum state by body of heater and rifle body successively, wherein vacuum tightness 5 * 10 in body of heater
-2pa, electron gun vacuum tightness is less than 5 * 10
-3pa.
2, start electron beam gun after reaching target vacuum degree, with 1mA/s speed, slowly increase line to 200mA, sweep radius is 10 * 10, and adjust electron beam scanning pattern is circular spot simultaneously, and its bombardment is melted until alloy melts completely to Inconel718 superalloy substrate and slowly.
3, after alloy melts completely, continuing slowly increases electron beam gun line to 400mA with 2mA/s speed, and electron beam spot radius is adjusted into 15 * 15, carries out alloy melting, and the time is 10min.
4, after said process, with the speed of 1.35mA/s, line is down to zero, closes subsequently electron beam gun, after body of heater and the cooling 30min of rifle body, reach the abundant state of cooling, take out sample, detect micro-atom O, N in alloy.
Utilize electron beam remelting technology can reduce significantly the content of impurity element atom, O, N constituent content in Inconel 718 alloys are brought down below respectively 0.0003%, 0.0148% by 0.005%, 0.0201%.
Claims (3)
1. a method that improves nickel base superalloy purity, is characterized in that: described method is electron beam remelting method, specifically comprises following processing step:
In electron beam melting device body of heater, vacuum tightness is less than 5 * 10
-2pa, electron gun vacuum tightness is less than 5 * 10
-3pa, increases line to 200mA with 1mA/s speed, and sweep radius is 10 * 10, makes its bombardment to nickel base superalloy substrate until alloy melts completely; After nickel base superalloy substrate melts completely, continuing increases electron beam gun line to 400mA with 2mA/s speed, and electron beam spot radius is adjusted into 15 * 15, carries out alloy melting, and the time is 5min～10min, rear cooling.
2. according to the method for claim 1, it is characterized in that: described coolingly carry out as follows: the speed with 1.35mA/s is down to zero by line, closes subsequently electron beam gun, after body of heater and the cooling 30min～60min of electron gun, taking-up.
3. according to the method for claim 1, it is characterized in that: described method comprises the pretreated step of nickel base superalloy substrate, specific as follows: use sand paper to carry out surface finish processing to nickel base superalloy substrate, the use of sand paper is sequentially followed successively by: 200#, 600#, 1000#, 1500#; With being placed in deionized water, cleaning and dry, drying time is 3～5h, and bake out temperature is 50～80 degree.
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| CN103981380A (en) * | 2014-05-29 | 2014-08-13 | 大连理工大学 | Method for preparing cobalt-based high-temperature alloy |
| CN103981372A (en) * | 2014-05-29 | 2014-08-13 | 大连理工大学 | Method for removing trace impurity elements in high temperature alloy |
| CN107164639A (en) * | 2017-06-27 | 2017-09-15 | 大连理工大学 | A kind of electron beam covers the method that formula solidification technology prepares high temperature alloy |
| CN107267788A (en) * | 2017-07-12 | 2017-10-20 | 大连理工大学 | A kind of electron beam melting purification is combined the method for preparing high-purity nickel base superalloy with low-temperature receiver gettering |
| CN107607567A (en) * | 2017-09-28 | 2018-01-19 | 华南理工大学 | The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder |
| CN107893214A (en) * | 2017-10-31 | 2018-04-10 | 宝鸡众有色金属材料有限公司 | The technique of impurity and elemental gas defect in a kind of elimination nickel plate target |
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| CN103981380A (en) * | 2014-05-29 | 2014-08-13 | 大连理工大学 | Method for preparing cobalt-based high-temperature alloy |
| CN103981372A (en) * | 2014-05-29 | 2014-08-13 | 大连理工大学 | Method for removing trace impurity elements in high temperature alloy |
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| CN107164639A (en) * | 2017-06-27 | 2017-09-15 | 大连理工大学 | A kind of electron beam covers the method that formula solidification technology prepares high temperature alloy |
| CN107164639B (en) * | 2017-06-27 | 2019-01-15 | 大连理工大学 | A kind of electron beam covers the method that formula solidification technology prepares high temperature alloy |
| CN107267788B (en) * | 2017-07-12 | 2018-11-09 | 大连理工大学 | A kind of electron beam melting purification is combined the method for preparing high-purity nickel base superalloy with low-temperature receiver gettering |
| CN107267788A (en) * | 2017-07-12 | 2017-10-20 | 大连理工大学 | A kind of electron beam melting purification is combined the method for preparing high-purity nickel base superalloy with low-temperature receiver gettering |
| CN107607567A (en) * | 2017-09-28 | 2018-01-19 | 华南理工大学 | The quantitatively characterizing method of non-metallic inclusion in a kind of Ni-base Superalloy Powder |
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| CN107893214A (en) * | 2017-10-31 | 2018-04-10 | 宝鸡众有色金属材料有限公司 | The technique of impurity and elemental gas defect in a kind of elimination nickel plate target |
| CN110423931A (en) * | 2019-08-01 | 2019-11-08 | 大连理工大学 | A kind of electron-beam smelting homogenizes the method for preparing Ti-Zr-Hf-Nb-Ta infusibility high-entropy alloy |
| WO2021017661A1 (en) * | 2019-08-01 | 2021-02-04 | 大连理工大学 | Method for preparing high-purity nickel-based high-temperature alloy using electron beam induced refining and casting technology |
| US11981978B2 (en) | 2019-08-01 | 2024-05-14 | Dalian University Of Technology | Method for preparing high-purity nickel-based superalloy by electron beam induced refining and casting technology |
| CN112095019A (en) * | 2020-08-11 | 2020-12-18 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
| CN112095019B (en) * | 2020-08-11 | 2021-07-30 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
| CN112746180A (en) * | 2020-12-28 | 2021-05-04 | 大连理工大学 | Method for promoting electron beam refining nickel-based high-temperature alloy desulfurization through slagging |
| CN112746180B (en) * | 2020-12-28 | 2022-02-11 | 大连理工大学 | Method for promoting electron beam refining nickel-based high-temperature alloy desulfurization through slagging |
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