CN103981372A - Method for removing trace impurity elements in high temperature alloy - Google Patents
Method for removing trace impurity elements in high temperature alloy Download PDFInfo
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- CN103981372A CN103981372A CN201410235863.7A CN201410235863A CN103981372A CN 103981372 A CN103981372 A CN 103981372A CN 201410235863 A CN201410235863 A CN 201410235863A CN 103981372 A CN103981372 A CN 103981372A
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Abstract
The invention relates to a method for removing trace impurity elements in a high temperature alloy and belongs to the field of electron beam smelting. The method for removing the trace impurity elements in the high temperature alloy is an electron beam smelting method and comprises a pre-impurity removal step, namely firstly a beam spot of an electron beam is expanded until the edge of the beam spot is tangent to the edge of a water cooling copper crucible while an alloy base material is not smelted by the electron beam, beam current is gradually increased at a rate of 4-17mA/s, and the beam spot of the electron beam is reduced; when the beam spot of the electron beam is reduced until the edge of the beam spot is a certain distance away from the center of the crucible, the beam spot of the electron beam is reversely expanded until the edge of the beam spot is tangent to the edge of the water cooling copper crucible, and the beam current is continuously and gradually increased; the process is repeated until the beam current of the electron beam is 250-1000mA. Continuous electron beam smelting can be realized, and trace elements can be removed from the alloy base material continuously, so that production efficiency is improved.
Description
Technical field
The present invention relates to a kind of method of removing micro impurity element in superalloy, belong to electron beam melting field.
Background technology
Superalloy is the important materials that heat-resistant part is manufactured in the industry such as Aeronautics and Astronautics, Nuclear Power System, domestic gas turbine.Trace element in superalloy is restricting its mechanical property.
Oxygen has a great impact the performance of nickel base superalloy, and oxide impurity is (as Al
2o
3deng) affect surrender, creep, creep rupture strength of single crystal casting etc.; High oxygen level due to the lattice defect of nucleogenesis, affects the yield strength of single crystal casting in mother alloy; Oxygen changes into nonmetallic impurity (as Al
2o
3), being mingled with is often germinating ground and the extended channel of fatigue cracking.These inclusiones can become core simultaneously, in monocrystalline part process of setting, develop into crystal grain defect, cause the castability of alloy poor; In the aircraft engine turbine disk, 50 microns or less oxide inclusion are determining its fatigue lifetime.
Sulphur can generate M with alloying element titanium, zirconium and carbon
2sC compound, these flaky compounds formation of crack often, for example, in M17 alloy, in the time that sulphur content is 0.002%, have Ti
5sC (γ phase) occurs.
In superalloy, contain strong close nitrogen element titanium, therefore nitrogen exists with nitride in superalloy, and these nitride can be used as the form of the nucleating center change MC carbide of MC carbide.Nitrogen content increases, and causes pore in alloy to increase, and nitride becomes bulk by Chinese character body shape, greatly reduces the mechanical property of alloy, and nitrogen content increases simultaneously, can impel the segregation of aluminium on crystal boundary, titanium, causes crystal boundary sclerosis and degradation property.Gas (nitrogen, oxygen) formation of inclusion in alloy is positioned at crystal boundary or interdendritic, poor with the bonding force of metallic matrix, and in use these compounds easily become formation of crack or for crack propagation provides passage, accelerate crack propagation.
Summary of the invention
The object of this invention is to provide a kind of method of removing micro impurity element in superalloy.
Removing a method for micro impurity element in superalloy, is electron-beam process, comprises the step of pre-removal of impurities and deep impurity-removing, and wherein, the step of described pre-removal of impurities is:
High pressure and the line of unlocking electronic rifle simultaneously, high pressure 25~35kV, line 50~500mA, when keeping alloy mother metal not by electron-beam melting, electron beam spot is expanded to make its edge and water jacketed copper crucible edge tangent, now increase gradually line with the speed of 4~17mA/s, simultaneously with
speed dwindle electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible center
time, oppositely with
speed expand electron beam spot to restrainting spot edge and water jacketed copper crucible edge is tangent, continuation increases line gradually with the speed of 4~17mA/s; Repeat said process until Electron Beam flow to 250~1000mA.
In technique scheme, described " keeping alloy mother metal not by electron-beam melting " can observe by the viewing window of electron-beam melting system, do not melt to ensure alloy mother metal by the size of controlling line.
The object of pre-removal step of the present invention is for by the impurity of each alloy mother metal surface and end face absorption, by the heating of water-cooled copper side, (water-cooled copper side temperature is minimum, easily make the each impurity of alloy mother metal surface adsorption), after heating along with electron beam spot radius dwindling gradually, impurity is collected to central zone, electron beam spot narrows down in certain limit, makes Heating Zone Temperature increase rapidly, foreign gas volumetric expansion, overflow alloy mother metal, discharged by vacuum system.Slowly increase electron beam line is in order to prevent that gas incorporates in alloy melt, the melt splash phenomena occurring because the fusing of alloy mother metal is too fast in the time of removal of impurities melting or alloy melting simultaneously.
In removal superalloy of the present invention, the step of the preferred described deep impurity-removing of method of micro impurity element is: increase Electron Beam with the speed of 10~20mA/s and flow to 300~2500mA, electron beam spot is R/2~3R/4, makes the fusing of alloy mother metal; Until alloy mother metal, all after fusing, maintaining electron beam line size is 200~2000mA, and electron beam spot size is adjusted to R/2~2R/3, make electron beam spot with
speed do and the interior tangent circumferential motion of water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, the circumferential motion time is 2~4min.
In removal superalloy of the present invention, the preferred described method of the method for micro impurity element comprises the pretreated step of alloy mother metal: alloy mother metal is cut, grinding process is carried out with the abrasive paper for metallograph of 240#, 320#, 600# successively alloy mother metal surface and end face in surface, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is packed in the water jacketed copper crucible of electron-beam melting system.
In removal superalloy of the present invention, the preferred described method of the method for micro impurity element comprises the step vacuumizing: close electron-beam melting system door, make body of heater vacuum tightness be less than 5 × 10
-2pa, gun chamber vacuum tightness is less than 5 × 10
-3pa.
In removal superalloy of the present invention, the preferred described method of the method for micro impurity element comprises the step of electron beam gun preheating: it is 25~35kV that high pressure is set, after high pressure preheating 5~10min, close high pressure, it is 70~200mA that electron beam gun line is set, line preheating 5~10min, closes electron beam gun line.
In removal superalloy of the present invention, the preferred described method of the method for micro impurity element comprises cooling step: close electron beam gun, alloy mother metal is cooling 20~40min in electron-beam melting system, close successively diffusion pump, lobe pump, mechanical pump, open purging valve, take out alloy mother metal.
The invention has the beneficial effects as follows:
1. the micro-speed in electron beam removal superalloy is fast; The method of main employing vacuum melting is removed Nitrogen Impurities, oxygen, the sulphur in alloy at present, and melting 35min at 1500 DEG C can remove 80ppmw by sulfur impurity, and oxygen is except arriving 90ppmw, and nitrogen is except arriving 20ppmw.And electron beam is removed the trace element in alloy, only need 5min, just can be by sulphur, oxygen, nitrogen element respectively except below 0.1ppmw.
2. electron beam melting can realize continuous smelting, and alloy mother metal is removed micro-processing serially, thereby enhances productivity.
Embodiment
Embodiment of the present invention is:
1. alloy mother metal pre-treatment: alloy mother metal is cut, grinding process is carried out with the abrasive paper for metallograph of 240#, 320#, 600# successively alloy mother metal surface and end face in surface, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is packed in the water jacketed copper crucible of electron-beam melting system;
2. vacuumize: close electron-beam melting system door, make body of heater vacuum tightness be less than 5 × 10-2Pa, gun chamber vacuum tightness is less than 5 × 10
-3pa;
3. electron beam gun preheating: it is 25~35kV that high pressure is set, and after high pressure preheating 5~10min, closes high pressure, it is 70~200mA that electron beam gun line is set, line preheating 5~10min, closes electron beam gun line;
4. the step of pre-removal of impurities is: high pressure and the line of unlocking electronic rifle simultaneously, high pressure 25~35kV, line 50~500mA, when keeping alloy mother metal not by electron-beam melting, electron beam spot is expanded to make its edge and water jacketed copper crucible edge tangent, now increase gradually line with the speed of 4~17mA/s, simultaneously with
speed dwindle electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible center
time, oppositely with
speed expand electron beam spot to restrainting spot edge and water jacketed copper crucible edge is tangent, continuation increases line gradually with the speed of 4~17mA/s; Repeat said process until Electron Beam flow to 250~1000mA;
5. deep impurity-removing: increase Electron Beam with the speed of 10~20mA/s and flow to 300~2500mA, electron beam spot is R/2~3R/4, makes the fusing of alloy mother metal; Until alloy mother metal, all after fusing, maintaining electron beam line size is 200~2000mA, and electron beam spot size is adjusted to R/2~2R/3, make electron beam spot with
speed do and the interior tangent circumferential motion of water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, the circumferential motion time is 2~4min;
6. cooling: close electron beam gun, alloy mother metal is cooling 20~40min in electron beam equipment, closes successively diffusion pump, lobe pump, mechanical pump, open purging valve, take out alloy mother metal.
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
1. alloy mother metal pre-treatment: Inconel740 alloy mother metal is cut, grinding process is carried out with the abrasive paper for metallograph of 240#, 320#, 600# successively alloy mother metal surface and end face in surface, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is packed in the water jacketed copper crucible of electron-beam melting system into water jacketed copper crucible inside radius R=100mm;
2. vacuumize: close electron-beam melting system door, make body of heater vacuum tightness be less than 5 × 10
-2pa, gun chamber vacuum tightness is less than 5 × 10
-3pa;
3. electron beam gun preheating: it is 25kV that high pressure is set, and after high pressure preheating 10min, closes high pressure, it is 70mA that electron beam gun line is set, line preheating 10min, closes electron beam gun line;
4. the step of pre-removal of impurities is: high pressure and the line of unlocking electronic rifle simultaneously, high pressure 25kV, line increases to 50mA, when keeping alloy mother metal not by electron-beam melting, by electron beam spot expand to make its edge and water jacketed copper crucible edge tangent, simultaneously increase gradually line with the speed of 4mA/s, simultaneously with
speed dwindle electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot dwindles Zhi Ju center, its edge
time, oppositely with
speed expand electron beam spot to restrainting spot edge and water jacketed copper crucible edge is tangent, continuation increases line gradually with the speed of 4mA/s; Repeat said process until electron beam line increases to 50mA;
5. deep impurity-removing: increase Electron Beam with the speed of 10mA/s and flow to 300mA, electron beam spot is R/2, makes the fusing of alloy mother metal; After alloy mother metal all melts, maintain electron beam line size for 200mA, electron beam spot size is adjusted to R/2, electron beam spot is done and the interior tangent circumferential motion of water jacketed copper crucible inwall with the speed of C/4/s, wherein C is water jacketed copper crucible inwall circumferential size, and the circumferential motion time is 2min;
6. cooling: close electron beam gun, alloy mother metal is cooling 20min in electron beam equipment, closes successively diffusion pump, lobe pump, mechanical pump, open purging valve, take out alloy mother metal.
The initial O concentration of Inconel740 alloy 25ppmw, S concentration 15ppmw, N concentration 15ppmw, processes below rear O concentration 0.05ppmw, below S concentration 0.1ppmw, below N concentration 0.1ppmw.
Embodiment 2
1. alloy mother metal pre-treatment: GH2984 alloy mother metal is cut, grinding process is carried out with the abrasive paper for metallograph of 240#, 320#, 600# successively alloy mother metal surface and end face in surface, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is packed in the water jacketed copper crucible of electron-beam melting system into water jacketed copper crucible inside radius R=400mm;
2. vacuumize: close electron-beam melting system door, make body of heater vacuum tightness be less than 5 × 10
-2pa, gun chamber vacuum tightness is less than 5 × 10
-3pa;
3. electron beam gun preheating: it is 35kV that high pressure is set, and after high pressure preheating 5min, closes high pressure, it is 200mA that electron beam gun line is set, line preheating 5min, closes electron beam gun line;
4. the step of pre-removal of impurities is: high pressure and the line of unlocking electronic rifle simultaneously, high pressure 35kV, line increases to 500mA, when keeping alloy mother metal not by electron-beam melting, by electron beam spot expand to make its edge and water jacketed copper crucible edge tangent, now increase gradually line with the speed of 17mA/s, simultaneously with
speed dwindle electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to apart from center
time, oppositely with
speed expand electron beam spot to restrainting spot edge and water jacketed copper crucible edge is tangent, continuation increases line gradually with the speed of 17mA/s; Repeat said process until electron beam line increases to 500mA;
5. deep impurity-removing: increase Electron Beam with the speed of 20mA/s and flow to 2500mA, electron beam spot is 3R/4, makes the fusing of alloy mother metal; After alloy mother metal all melts, maintain electron beam line size for 2000mA, electron beam spot size is adjusted to 2R/3, electron beam spot is done and the interior tangent circumferential motion of water jacketed copper crucible inwall with the speed of C/10/s, wherein C is water jacketed copper crucible inwall circumferential size, and the circumferential motion time is 4min;
6. cooling: close electron beam gun, alloy mother metal is cooling 40min in electron beam equipment, closes successively diffusion pump, lobe pump, mechanical pump, open purging valve, take out alloy mother metal.
GH2984 alloy, initial O concentration 20ppmw, S concentration 20ppmw, N concentration 15ppmw, processes below rear O concentration 0.01ppmw, below S concentration 0.1ppmw, below N concentration 0.05ppmw.
Embodiment 1 and 2 alloy compositions used see the following form:
Claims (6)
1. removing a method for micro impurity element in superalloy, is electron-beam process, it is characterized in that: comprise the step of pre-removal of impurities and deep impurity-removing, wherein, the step of described pre-removal of impurities is:
High pressure and the line of unlocking electronic rifle simultaneously, high pressure 25~35kV, line 50~500mA, when keeping alloy mother metal not by electron-beam melting, electron beam spot is expanded to make its edge and water jacketed copper crucible edge tangent, now increase gradually line with the speed of 4~17mA/s, simultaneously with
speed dwindle electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible center
time, oppositely with
speed expand electron beam spot to restrainting spot edge and water jacketed copper crucible edge is tangent, continuation increases line gradually with the speed of 4~17mA/s; Repeat said process until Electron Beam flow to 250~1000mA.
2. method according to claim 1, is characterized in that: the step of described deep impurity-removing is: increase Electron Beam with the speed of 10~20mA/s and flow to 300~2500mA, electron beam spot is R/2~3R/4, makes the fusing of alloy mother metal; Until alloy mother metal, all after fusing, maintaining electron beam line size is 200~2000mA, and electron beam spot size is adjusted to R/2~2R/3, make electron beam spot with
speed do and the interior tangent circumferential motion of water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, the circumferential motion time is 2~4min.
3. method according to claim 1, it is characterized in that: described method comprises the pretreated step of alloy mother metal: alloy mother metal is cut, grinding process is carried out with the abrasive paper for metallograph of 240#, 320#, 600# successively alloy mother metal surface and end face in surface, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is packed in the water jacketed copper crucible of electron-beam melting system.
4. method according to claim 3, is characterized in that: described method comprises the step vacuumizing: close electron-beam melting system door, make body of heater vacuum tightness be less than 5 × 10
-2pa, gun chamber vacuum tightness is less than 5 × 10
-3pa.
5. method according to claim 1, is characterized in that: described method comprises the step of electron beam gun preheating: it is 25~35kV that high pressure is set, after high pressure preheating 5~10min, close high pressure, it is 70~200mA that electron beam gun line is set, and line preheating 5~10min, closes electron beam gun line.
6. method according to claim 1, it is characterized in that: described method comprises cooling step: close electron beam gun, alloy mother metal is cooling 20~40min in electron-beam melting system, closes successively diffusion pump, lobe pump, mechanical pump, open purging valve, take out alloy mother metal.
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Cited By (3)
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CN105331833A (en) * | 2014-08-07 | 2016-02-17 | 有研稀土新材料股份有限公司 | Refining device and method for high-purity rare earth metal |
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 |
CN110423918A (en) * | 2019-08-01 | 2019-11-08 | 大连理工大学 | A kind of method that electron beam-induced refining casting technique prepares high-purity nickel base superalloy |
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CN110423918A (en) * | 2019-08-01 | 2019-11-08 | 大连理工大学 | A kind of method that electron beam-induced refining casting technique prepares high-purity nickel base superalloy |
CN110423918B (en) * | 2019-08-01 | 2020-09-29 | 大连理工大学 | Method for preparing high-purity nickel-based high-temperature alloy by electron beam induced refining casting technology |
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