CN103981372B - A kind of method removing micro impurity element in superalloy - Google Patents

A kind of method removing micro impurity element in superalloy Download PDF

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CN103981372B
CN103981372B CN201410235863.7A CN201410235863A CN103981372B CN 103981372 B CN103981372 B CN 103981372B CN 201410235863 A CN201410235863 A CN 201410235863A CN 103981372 B CN103981372 B CN 103981372B
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electron beam
mother metal
line
edge
alloy mother
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CN103981372A (en
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谭毅
姜大川
王登科
石爽
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Dalian University of Technology
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Abstract

The present invention relates to a kind of method removing micro impurity element in superalloy, belong to electron beam melting field. A kind of method removing micro impurity element in superalloy, for electron-beam process, comprise pre-removal step: first keep alloy mother metal not expanded to by electron beam spot while electron-beam melting and make its edge and water jacketed copper crucible edge tangent, now increase line gradually with the speed of 4��17mA/s, reduce electron beam spot simultaneously; When electron beam spot is contracted to its edge far from crucible center certain distance, oppositely expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continue to increase line gradually; Repeat said process until electron beam line to 250��1000mA. Electron beam melting can realize continuous melting, alloy mother metal can carry out removing the process of trace element continuously, thus improve production efficiency.

Description

A kind of method removing micro impurity element in superalloy
Technical field
The present invention relates to a kind of method removing micro impurity element in superalloy, belong to electron beam melting field.
Background technology
Superalloy is the important materials that the industry such as aviation, space flight, Nuclear Power System, domestic gas turbine manufacture heat-resistant part. Trace element in superalloy governs its mechanical property.
The performance of nickel base superalloy is had a great impact by oxygen, and oxide impurity is (such as Al2O3Deng) affect the surrender of single crystal casting, creep, creep rupture strength 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 (such as Al2O3), be mingled be often fatigue cracking germinating ground and extended channel. These inclusiones can become core simultaneously, develops into crystal grain defect, cause the castability of alloy poor in monocrystalline part process of setting; In aircraft engine turbine disk, the oxide inclusion of 50 microns or less decides its fatigue lifetime.
Sulphur can generate M with alloying element titanium, zirconium and carbon2SC compound, these flaky compounds formation of crack often, such as, in M17 alloy, when sulphur content is 0.002%, namely has Ti5SC (�� phase) occurs.
Containing strong close nitrogen element titanium in superalloy, therefore nitrogen exists with nitride in superalloy, and these nitride can change the form of MC carbide as the Xing He center of MC carbide. Nitrogen content increases, and causes pore in alloy to increase, and nitride becomes block 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 hardening and degradation property. Gas (nitrogen, oxygen) in the alloy the formation of inclusion be positioned at crystal boundary or interdendritic, poor with the bonding force of metallic matrix, in use these compounds easily become formation of crack or be crack propagation provide passage, accelerate crack propagation.
Summary of the invention
It is an object of the invention to provide a kind of method removing micro impurity element in superalloy.
Removing a method for micro impurity element in superalloy, be electron-beam process, comprise the step of pre-removal of impurities and deep impurity-removing, wherein, the step of described pre-removal of impurities is:
The simultaneously high pressure of unlocking electronic rifle and line, high pressure 25��35kV, line 50��500mA, keep alloy mother metal not expanded to by electron beam spot while electron-beam melting and make its edge and water jacketed copper crucible edge tangent, now increase line gradually with the speed of 4��17mA/s, simultaneously withSpeed reduce electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible centerTime, oppositely with Speed to expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continuation increases line gradually with the speed of 4��17mA/s; Repeat said process until electron beam line to 250��1000mA.
In technique scheme, described " keeping alloy mother metal not by electron-beam melting " can be observed by the viewing window of electron beam melting equipment, non-fusible to ensure alloy mother metal by controlling the size of line.
The object of pre-removal step of the present invention is in order to by the impurity on each for 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 alloy each impurity of mother metal surface adsorption), along with electron beam spot radius reducing gradually after heating, impurity is collected to central zone, electron beam spot narrows down in certain limit, makes Heating Zone Temperature rise rapidly, foreign gas volumetric expansion, overflow alloy mother metal, discharged by vacuum system. Slowly increase electron beam line is that gas incorporates in alloy melt, the melt splash phenomena occurred when removal of impurities melting or alloy melting in order to prevent owing to the fusing of alloy mother metal is too fast simultaneously.
In removal superalloy of the present invention, the step of the preferred described deep impurity-removing of the method for micro impurity element is: increasing electron beam line to 300��2500mA with the speed of 10��20mA/s, electron beam spot is R/2��3R/4, and alloy mother metal is melted; After alloy mother metal all melts, maintain electron beam line size be 200��2000mA, electron beam spot size is adjusted to R/2��2R/3, make electron beam spot withSpeed do and tangent circumferential motion in water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, and 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: cut by alloy mother metal, alloy mother metal surface and end face are carried out grinding process by the abrasive paper for metallograph of surface 240#, 320#, 600# successively, the impurity such as scale removal, clean with alcohol afterwards, by the water jacketed copper crucible cleaning rear alloy mother metal loading electron beam melting equipment.
In removal superalloy of the present invention, the preferred described method of the method for micro impurity element comprises the step vacuumized: closes electron beam melting equipment door, makes body of heater vacuum tightness be less than 5 �� 10-2Pa, electron beam gun room 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: arranging high pressure is 25��35kV, after high pressure preheating 5��10min, close high pressure, arranging electron beam gun line is 70��200mA, 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 the step of cooling: close electron beam gun, alloy mother metal cools 20��40min in electron beam melting equipment, close diffusion pump, lobe pump, mechanical pump successively, open purging valve, take out alloy mother metal.
The invention has the beneficial effects as follows:
1. the speed of the trace element in electron beam removal superalloy is fast; The method of main employing vacuum melting removes the impurity nitrogen in alloy, oxygen, sulphur, melting 35min at 1500 DEG C at present, can by sulfur impurity except to 80ppmw, oxygen is except arriving 90ppmw, and nitrogen is except to 20ppmw. And electron beam removes the trace element in alloy, it is only necessary to 5min, just can by sulphur, oxygen, nitrogen element respectively except to below 0.1ppmw.
2. electron beam melting can realize continuous melting, alloy mother metal can carry out removing the process of trace element continuously, thus improve production efficiency.
Embodiment
The present invention's embodiment is:
1. alloy mother metal pre-treatment: alloy mother metal is cut, alloy mother metal surface and end face are carried out grinding process by the abrasive paper for metallograph of surface 240#, 320#, 600# successively, the impurity such as scale removal, clean with alcohol afterwards, by the water jacketed copper crucible cleaning rear alloy mother metal loading electron beam melting equipment;
2. vacuumize: closing electron beam melting equipment door, make body of heater vacuum tightness be less than 5 �� 10-2Pa, electron beam gun room vacuum tightness is less than 5 �� 10-3Pa;
3. electron beam gun preheating: arranging high pressure is 25��35kV, after high pressure preheating 5��10min, closes high pressure, and arranging electron beam gun line is 70��200mA, line preheating 5��10min, closes electron beam gun line;
4. the step of pre-removal of impurities is: the high pressure of unlocking electronic rifle and line simultaneously, high pressure 25��35kV, line 50��500mA, keeping alloy mother metal not expanded to by electron beam spot while electron-beam melting makes its edge and water jacketed copper crucible edge tangent, now increase line gradually with the speed of 4��17mA/s, simultaneously withSpeed reduce electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible centerTime, oppositely withSpeed to expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continuation increases line gradually with the speed of 4��17mA/s; Repeat said process until electron beam line to 250��1000mA;
5. deep impurity-removing: increasing electron beam line to 300��2500mA with the speed of 10��20mA/s, electron beam spot is R/2��3R/4, and alloy mother metal is melted; After alloy mother metal all melts, maintain electron beam line size be 200��2000mA, electron beam spot size is adjusted to R/2��2R/3, make electron beam spot withSpeed do and tangent circumferential motion in water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, and the circumferential motion time is 2��4min;
6. cool: closing electron beam gun, alloy mother metal cools 20��40min in electron beam equipment, closes diffusion pump, lobe pump, mechanical pump successively, open purging valve, take out alloy mother metal.
Following non-limiting example can make the those of ordinary skill of this area more fully understand the present invention, 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, alloy mother metal surface and end face are carried out grinding process by the abrasive paper for metallograph of surface 240#, 320#, 600# successively, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is loaded in the water jacketed copper crucible of electron beam melting equipment, water jacketed copper crucible inside radius R=100mm;
2. vacuumize: close electron beam melting equipment door, make body of heater vacuum tightness be less than 5 �� 10-2Pa, electron beam gun room vacuum tightness is less than 5 �� 10-3Pa;
3. electron beam gun preheating: arranging high pressure is 25kV, after high pressure preheating 10min, closes high pressure, and arranging electron beam gun line is 70mA, line preheating 10min, closes electron beam gun line;
4. the step of pre-removal of impurities is: the high pressure of unlocking electronic rifle and line simultaneously, high pressure 25kV, line increases to 50mA, keep alloy mother metal not by while electron-beam melting, electron beam spot is expanded to and makes its edge and water jacketed copper crucible edge tangent, simultaneously increase line gradually with the speed of 4mA/s, simultaneously withSpeed reduce electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot reduces its edge to apart from centerTime, oppositely withSpeed to expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continuation increases line gradually with the speed of 4mA/s; Repeat said process until electron beam line increases to 50mA;
5. deep impurity-removing: increasing electron beam line to 300mA with the speed of 10mA/s, electron beam spot is R/2, and alloy mother metal is melted; After alloy mother metal all melts, maintaining electron beam line size is 200mA, electron beam spot size is adjusted to R/2, electron beam spot is done and tangent circumferential motion in 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. cool: closing electron beam gun, alloy mother metal cools 20min in electron beam equipment, closes diffusion pump, lobe pump, mechanical pump successively, open purging valve, take out alloy mother metal.
The initial O concentration 25ppmw of Inconel740 alloy, S concentration 15ppmw, N concentration 15ppmw, below O concentration 0.05ppmw, S below concentration 0.1ppmw, N below concentration 0.1ppmw after process.
Embodiment 2
1. alloy mother metal pre-treatment: GH2984 alloy mother metal is cut, alloy mother metal surface and end face are carried out grinding process by the abrasive paper for metallograph of surface 240#, 320#, 600# successively, the impurity such as scale removal, clean with alcohol afterwards, alloy mother metal after cleaning is loaded in the water jacketed copper crucible of electron beam melting equipment, water jacketed copper crucible inside radius R=400mm;
2. vacuumize: close electron beam melting equipment door, make body of heater vacuum tightness be less than 5 �� 10-2Pa, electron beam gun room vacuum tightness is less than 5 �� 10-3Pa;
3. electron beam gun preheating: arranging high pressure is 35kV, after high pressure preheating 5min, closes high pressure, and arranging electron beam gun line is 200mA, line preheating 5min, closes electron beam gun line;
4. the step of pre-removal of impurities is: the high pressure of unlocking electronic rifle and line simultaneously, high pressure 35kV, line increases to 500mA, keep alloy mother metal not by while electron-beam melting, electron beam spot is expanded to and makes its edge and water jacketed copper crucible edge tangent, now increase line gradually with the speed of 17mA/s, simultaneously withSpeed reduce electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to apart from centerTime, oppositely withSpeed to expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continuation increases line gradually with the speed of 17mA/s; Repeat said process until electron beam line increases to 500mA;
5. deep impurity-removing: increasing electron beam line to 2500mA with the speed of 20mA/s, electron beam spot is 3R/4, and alloy mother metal is melted; After alloy mother metal all melts, maintaining electron beam line size is 2000mA, electron beam spot size is adjusted to 2R/3, electron beam spot is done and tangent circumferential motion in 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. cool: closing electron beam gun, alloy mother metal cools 40min in electron beam equipment, closes diffusion pump, lobe pump, mechanical pump successively, open purging valve, take out alloy mother metal.
GH2984 alloy, initial O concentration 20ppmw, S concentration 20ppmw, N concentration 15ppmw, below O concentration 0.01ppmw, S below concentration 0.1ppmw, N below concentration 0.05ppmw after process.
Embodiment 1 and 2 alloy compositions used sees the following form:

Claims (6)

1. remove a method for micro impurity element in superalloy, it be electron-beam process, it is characterised in that: the step comprising pre-removal of impurities and deep impurity-removing, wherein, the step of described pre-removal of impurities is:
I. the simultaneously high pressure of unlocking electronic rifle and line, high pressure 25��35kV, final line 50��500mA;
Ii. keep alloy mother metal not expanded to by electron beam spot while electron-beam melting and make its edge and water jacketed copper crucible edge tangent, now increase line gradually with the speed of 4��17mA/s, while withSpeed reduce electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible centerTime, withSpeed to expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continue to increase line gradually with the speed of 4��17mA/s, repetition said process is until electron beam line is to 50mA;
The step of described deep impurity-removing is: increasing electron beam line to 300��2500mA with the speed of 10��20mA/s, electron beam spot is R/2��3R/4, and alloy mother metal is melted; After alloy mother metal all melts, maintain electron beam line size be 200��2000mA, electron beam spot size is adjusted to R/2��2R/3, make electron beam spot withSpeed do and tangent circumferential motion in water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, and the circumferential motion time is 2��4min.
2. remove a method for micro impurity element in superalloy, it be electron-beam process, it is characterised in that: the step comprising pre-removal of impurities and deep impurity-removing, wherein, the step of described pre-removal of impurities is:
I. the simultaneously high pressure of unlocking electronic rifle and line, high pressure 25��35kV, final line 50��500mA;
Ii. keep alloy mother metal not expanded to by electron beam spot while electron-beam melting and make its edge and water jacketed copper crucible edge tangent, now increase line gradually with the speed of 4��17mA/s, while withSpeed reduce electron beam spot, wherein, R is water jacketed copper crucible inwall radius; When electron beam spot is contracted to its edge far from crucible centerTime, withSpeed to expand electron beam spot tangent to bundle spot edge and water jacketed copper crucible edge, continue to increase line gradually with the speed of 4��17mA/s, repetition said process is until electron beam line is to 500mA;
The step of described deep impurity-removing is: increasing electron beam line to 300��2500mA with the speed of 10��20mA/s, electron beam spot is R/2��3R/4, and alloy mother metal is melted; After alloy mother metal all melts, maintain electron beam line size be 200��2000mA, electron beam spot size is adjusted to R/2��2R/3, make electron beam spot withSpeed do and tangent circumferential motion in water jacketed copper crucible inwall, wherein C is water jacketed copper crucible inwall circumferential size, and the circumferential motion time is 2��4min.
3. method according to claim 1 and 2, it is characterized in that: described method comprises the pretreated step of alloy mother metal: cut by alloy mother metal, alloy mother metal surface and end face are carried out grinding process by the abrasive paper for metallograph of surface 240#, 320#, 600# successively, scale removal impurity, clean with alcohol afterwards, by the water jacketed copper crucible cleaning rear alloy mother metal loading electron beam melting equipment.
4. method according to claim 3, it is characterised in that: described method carries out the step vacuumized after being included in alloy mother metal pre-treatment step: close electron beam melting equipment door, make body of heater vacuum tightness be less than 5 �� 10-2Pa, electron beam gun room vacuum tightness is less than 5 �� 10-3Pa��
5. method according to claim 1 and 2, it is characterized in that: described method is included in the step carrying out electron beam gun preheating after vacuumizing step: arranging high pressure is 25��35kV, after high pressure preheating 5��10min, close high pressure, arranging electron beam gun line is 70��200mA, line preheating 5��10min, closes electron beam gun line.
6. method according to claim 1 and 2, it is characterized in that: described method comprises the step of cooling: closing electron beam gun, alloy mother metal cools 20��40min in electron beam melting equipment, closes diffusion pump, lobe pump, mechanical pump successively, open purging valve, take out alloy mother metal.
CN201410235863.7A 2014-05-29 2014-05-29 A kind of method removing micro impurity element in superalloy Expired - Fee Related CN103981372B (en)

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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
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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