CN103382533A - Alloy purifying smelting method for nickel base superalloy return scraps - Google Patents
Alloy purifying smelting method for nickel base superalloy return scraps Download PDFInfo
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Abstract
The invention relates to an alloy purifying smelting method for nickel base superalloy return scraps. The method comprises following steps: (I) pre-treating the return scraps: removing the oil stains on the surfaces of the return scraps; (II) manufacturing primary vacuum induction ingots: putting the return scraps, which are generated during the production process of nickel base superalloy pipe materials, in a vacuum induction furnace, vacuum pumping and heating to refine while argon gas is blown from the bottom, subjecting the alloy solution to a cooling treatment after the refinement is over, reheating the solidified alloy solution, and casting into the primary vacuum induction ingots; (III) preparing for the secondary vacuum induction smelting: preparing the secondary vacuum induction smelting when the components of the vacuum induction ingots reach the requirements; (IV) performing the secondary vacuum induction smelting: putting the primary vacuum induction ingots in the vacuum induction furnace, vacuum pumping and electrifying while argon gas is blown from the bottom, subjecting the primary vacuum induction ingots to a cooling treatment after the refinement is over to make the surface of the alloy solution solidify; (V) obtaining the 617 B alloy. The nickel base superalloy prepared by the alloy purifying smelting method meets the requirements of the ASMESB-167 standard.
Description
Technical field
The invention belongs to the pure smelting process of alloy of nickel base superalloy returns, is specifically a kind of pure smelting process of alloy of nickel base superalloy 617B returns.
Background technology
A kind of Ni-Cr-Co-Mo solution strengthening of 617B alloy type nickel base superalloy has good corrosion-resistant, anti-oxidant and good mechanical property, is mainly used in Aeronautics and Astronautics, the energy and petrochemical industry.Enter 21 century, thermal power generation is constantly to the vapor pressure that improves boiler and temperature direction development, to advanced ultra supercritical (700 ℃) development transition, the 617B alloy is used as thermal power generation boiler superheater of new generation, reheater and the main candidate material of main steam line by present ultra supercritical (600 ℃).As the thermoelectricity Boiler Pipe, alloy will pass through the complicated technological process of productions such as vacuum induction smelting-esr-homogenizing-hammer cogging-hot extrusion-cold rolling-thermal treatment, and each step production link all will guarantee high quality.For example: vacuum ingot, ESR ingot, pipe need to carry out crop end, the surface strips off the skin and processes etc., therefore can produce a certain amount of returns in process of production, the overall recovery rate of alloy is 35 ~ 40%, and especially the Ni in superalloy, Cr, Co, Mo etc. belong to the rare expensive element of country.The 617B alloy is in the situation that output and use popularization, and the application of returns has become the task of top priority.
Returns reclaim and generally adopt virgin material directly to add the mixed smelting mode of returns at present; Perhaps adopt directly to become alloy pig with the returns smelting and pouring, then alloy pig is as adjusting the mode of material with the virgin material mixed smelting.Above returns recovery method certainly will have a negative impact to the metallurgical quality of final gained alloy pig because there is certain difference in virgin material and returns (perhaps returns smelting and pouring become alloy pig) purity.
Summary of the invention
In order to overcome the above-mentioned deficiency of the pure smelting process of alloy that has the nickel base superalloy returns now, the invention provides a kind of pure smelting process of alloy of nickel base superalloy 617B returns, smelting process of the present invention is smelted the nickel base superalloy 617B that and is reached the requirement of ASME SB-167 standard, and reaches for the manufacture of 700 ℃-100MPa/10
5The requirement of h ultra-supercritical boiler superheater and reheater material.
The pure smelting process of the alloy of this nickel base superalloy returns, different according to the per-cent of each composition of making a vacuum induction ingot casting, be divided into two kinds of smelting processes that common trait is arranged.
Method one
The pure smelting process of a kind of alloy of nickel base superalloy returns, it comprises following step:
I, the returns pre-treatment
Clout is expanded in the hot extrusion remainder material that produces in the block returns that a produces vacuum ingot, ESR ingot, pipe, hollow forging, cold rolled tube crop end in nickel base superalloy 617B tubing production process and hot extrusion process and hot reaming, block returns carry out shot-peening and sandblasting, and the cleaning oil pollution on returns surfaces is clean;
B carries out 200 ~ 300 ℃ to the turning returns of the vacuum ingot in nickel base superalloy 617B tubing production process, ESR ingot, pipe surface and heart section mechanical process, and the high bake of 2-4h is processed, and the surface and oil contaminant of turning returns is cleaned out;
Block returns and turning returns weight proportion are in (3 ~ 5): between 1:
II, make a vacuum induction ingot casting
Block returns in nickel base superalloy 617B tubing production process are placed in vacuum induction furnace, and the turning returns add during the phase at alloy melting as adding material in batches; Start vacuum apparatus and vacuumize, begin power transmission (power is restriction not, watches in real time material melting situation Modulating Power size in stove), the pressure≤5Pa of alloy melting phase vacuum tightness when the pressure of vacuum tightness≤1Pa; Improve power transmission power and (bring up to 250 ~ 350KW), when being warming up to 1550 ~ 1600 ℃, alloy molten solution begins refining, refining time is 30 ~ 40min, carry out the BOTTOM ARGON BLOWING operation in refining process, assist in removing gas and inclusion in alloy molten solution, and the pressure≤5Pa of control process vacuum tightness; Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies, this step operation helps further to remove the gas in alloy molten solution; The alloy molten solution of conjunctiva is reheated to 1470 ~ 1520 ℃, pour into the vacuum induction ingot casting one time;
III, prepare the secondary vacuum induction and smelt
Analyze the chemical composition of a vacuum induction ingot casting, the mass percent of the chemical composition of a vacuum induction ingot casting reaches:
Cr 21.5~23%； Co 11.5~12.5%； Mo 8.5~9.5%；Al 1.1~1.5%；
Ti 0.3~0.6%； C 0.03~0.06%； Zr 0.02~0.045%； B 0.003~0.005%；
When all the other are Ni, prepare the secondary vacuum induction and smelt;
IV, secondary vacuum induction smelts
A vacuum induction ingot casting is placed in vacuum induction furnace, starting vacuum apparatus vacuumizes, begin power transmission when the pressure of vacuum tightness≤1Pa, carry out alloy melting, alloy molten solution is warming up to 1550 ~ 1600 ℃ carries out refining, refining time is 30 ~ 40min, carries out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness.Refining is carried out the alloy molten solution freezing treatment after finishing equally, until the surperficial conjunctiva of alloy molten solution solidifies.
V, obtain the 617B alloy
Refining is finished the alloy molten solution that the rear surface conjunctiva solidifies be heated to 1470～1520 ℃, the pressure≤5Pa of vacuum tightness pours into the 617B alloy pig.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns is characterized in that: in step IV secondary vacuum induction smelting process, and the pressure≤5Pa of alloy melting phase vacuum tightness.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns is characterized in that: step
IIn the returns preprocessing process, the maximum linear dimension of block material is not less than the shot peening of carrying out of 50mm, less than the block material employing sandblasting of 50mm.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns is characterized in that: step
IIn the returns preprocessing process, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopts sandblasting less than φ 50mm equivalent size block material.
Method two
The pure smelting process of alloy of another kind of nickel base superalloy returns, it comprises following step:
I, the returns pre-treatment
Clout is expanded in the hot extrusion remainder material that produces in the block returns that a produces vacuum ingot, ESR ingot, pipe, hollow forging, cold rolled tube crop end in nickel base superalloy 617B tubing production process and hot extrusion process and hot reaming, block returns carry out shot-peening and sandblasting, and the cleaning oil pollution on returns surfaces is clean;
B carries out 200 ~ 300 ℃ to the turning returns of the vacuum ingot in nickel base superalloy 617B tubing production process, ESR ingot, pipe surface and heart section mechanical process, and the high bake of 2-4h is processed, and the surface and oil contaminant of turning returns is cleaned out;
Block returns and turning returns weight proportion are in (3 ~ 5): between 1:
II, make a vacuum induction ingot casting
Block returns in nickel base superalloy 617B tubing production process are placed in vacuum induction furnace, and the turning returns add during the phase at alloy melting as adding material in batches; Start vacuum apparatus and vacuumize, begin power transmission, the pressure≤5Pa of alloy melting phase vacuum tightness when the pressure of vacuum tightness≤1Pa; Improve power transmission power, begin refining when alloy molten solution is warming up to 1550 ~ 1600 ℃, refining time is 30 ~ 40min, carries out the BOTTOM ARGON BLOWING operation in refining process, assist in removing gas and inclusion in alloy molten solution, and the pressure≤5Pa of control process vacuum tightness; Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies, this step operation helps further to remove the gas in alloy molten solution; The alloy molten solution of conjunctiva is reheated to 1470 ~ 1520 ℃, pour into the vacuum induction ingot casting one time;
III, prepare the secondary vacuum induction and smelt
Analyze the chemical composition of a vacuum induction ingot casting, the mass percent of any in the Cr of a vacuum induction ingot casting, Co, Mo, Al, Ti, C, Zr or B exceeds:
Cr 21.5~23%； Co 11.5~12.5%； Mo 8.5~9.5%； Al 1.1~1.5%；
Ti 0.3~0.6%； C 0.03~0.06%； Zr 0.02~0.045%； B 0.003~0.005%；
All the other are the scope of Ni;
Use the minimum a kind of as regulating the composition materials of nickel, chromium, cobalt, molybdenum, aluminium, titanium, carbon, zirconium, ferro-boron, make the mass percent of composition of the vacuum induction ingot casting after adjusting in the mentioned component scope;
IV, secondary vacuum induction smelts
A vacuum induction ingot casting is placed in vacuum induction furnace, and will regulate the minimum a kind of of composition materials also adds in vacuum induction furnace, starting vacuum apparatus vacuumizes, begin power transmission when the pressure of vacuum tightness≤1Pa, carry out alloy melting, alloy molten solution is warming up to 1550 ~ 1600 ℃ carries out refining, refining time is 30 ~ 40min, carry out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness.Refining is carried out the alloy molten solution freezing treatment after finishing, until the surperficial conjunctiva of alloy molten solution solidifies.
V, obtain the 617B alloy
The alloy molten solution of conjunctiva after alloying is heated to 1470～1520 ℃, and the pressure≤5Pa of vacuum tightness then pours into the 617B alloy pig.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns is characterized in that: in step IV secondary vacuum induction smelting process, and the pressure≤5Pa of alloy melting phase vacuum tightness.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns is characterized in that: step
IIn the returns preprocessing process, the maximum linear dimension of block material is not less than the shot peening of carrying out of 50mm, less than the block material employing sandblasting of 50mm.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns is characterized in that: step
IIn the returns preprocessing process, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopts sandblasting less than φ 50mm equivalent size block material.
The pure smelting process of alloy of above-mentioned nickel base superalloy returns, it is characterized in that: in step IV secondary vacuum induction smelting process, refining finishes and carries out the alloy molten solution freezing treatment, until after alloy molten solution surface conjunctiva solidifies, the alloy molten solution of conjunctiva is reheated be warming up to 1550 ~ 1600 ℃, also add other raw material of remaining adjusting composition materials in vacuum induction furnace, refining time is no less than 8min, carry out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness is cooled to the surperficial conjunctiva of alloy molten solution again.
The present invention is the advantage that compares with prior art
Chemical composition analysis shows, adopts BOTTOM ARGON BLOWING+alloy molten solution freezing treatment technology in the vacuum induction smelting process, can make O in the 617B alloy of acquisition≤0.001%, and N≤0.0025% has obviously improved the purity of alloy.Show through overtesting production, the returns 617B alloy that adopts present method to obtain can satisfy production requirement fully, with the 617B mechanical properties of tubular goods of this returns manufacturing with adopt virgin material to prepare the 617B mechanical properties of tubular goods to be in same level, to satisfy ASME SB-167 standard.And reach for the manufacture of 700 ℃-100MPa/10
5The requirement of h ultra-supercritical boiler superheater and reheater material.
Specific embodiment
Below in conjunction with embodiment, technical scheme of the present invention is carried out clear, complete description.Described embodiment is several embodiments of the present invention, rather than limitation of the present invention.Those of ordinary skills do not have the pure smelting technical solution of alloy of the nickel base superalloy returns that obtain under the creative work prerequisite, all belong to protection scope of the present invention.
The weight purity of adding elemental nickel, chromium, cobalt, molybdenum, aluminium, titanium, carbon, zirconium, ferro-boron that adopts in the embodiment of the present invention is respectively: Ni in metallic nickel 〉=99.95%, Cr in chromium metal 〉=99.31%, Co in cobalt metal 〉=99.95%, Mo in metal molybdenum 〉=99.90%, Al in metallic aluminium 〉=99.75%, Ti in metal titanium 〉=99.75%, C in metal carbon 〉=99.50%, Zr in metal zirconium 〉=99.41%, B content 17～35% in ferro-boron.
The returns that adopt in the embodiment of the present invention are:
1) the block returns of clout are expanded in the hot extrusion remainder material that produces in the block returns that produce of vacuum ingot, ESR ingot, pipe, hollow forging, the cold rolled tube crop end in nickel base superalloy 617B tubing production process and hot extrusion process and hot reaming;
2) the turning returns of the vacuum ingot in nickel base superalloy 617B tubing production process, ESR ingot, pipe surface and heart section mechanical process.
Embodiment 1
The embodiment of the pure smelting process of alloy of this nickel base superalloy returns comprises following step successively:
1, returns pre-treatment
The block returns that produce in nickel base superalloy 617B tubing production process are carried out shot peening, block returns carry out shot-peening or sandblasting, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopt sandblasting less than φ 50mm equivalent size block material, the cleaning oil pollution on returns surfaces is clean;
The turning returns that produce in nickel base superalloy 617B tubing production process are carried out 200 ℃, and the high bake of 2h is processed, and the surface and oil contaminant of returns is cleaned out.
Block returns and turning returns weight proportion are 4:1.
2, make a vacuum induction ingot casting
At first block returns are placed in vacuum induction furnace, start vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.7Pa, the pressure of alloy melting phase vacuum tightness is between 1 ~ 4Pa, and melting period is added the turning returns 2 times altogether.Improve power transmission power, alloy molten solution is warming up to 1600 ℃, refining 30min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1L/min, and the pressure of refining process vacuum tightness is between 2 ~ 3Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.The alloy molten solution of conjunctiva is reheated to 1490 ℃, pour into the vacuum induction ingot casting one time.
3, preparing the secondary vacuum induction smelts
The chemical composition of analyzing a vacuum induction ingot casting is Cr 21.9% by weight percentage; Co 12.1%; Mo 9.1%; Al 1.4%; Ti 0.4%; C 0.035%; Zr 0.022%; B 0.0033%, and surplus is Ni.This chemical composition all is positioned at the composition range of requirement, need not add and regulate the composition element material.
4, the secondary vacuum induction is smelted
A vacuum induction ingot casting is placed in vacuum induction furnace, starts vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.4Pa, the pressure of alloy melting phase vacuum tightness is between 1 ~ 3Pa.Improve power transmission power, alloy molten solution is warming up to 1590 ℃, refining 35min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1.2L/min, and the pressure of refining process vacuum tightness is between 2 ~ 4Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.
5, obtain the 617B alloy
The alloy molten solution of conjunctiva is reheated to 1500 ℃, and the pressure 3-4Pa of vacuum tightness pours into the 617B alloy pig.
The returns 617B alloy pig that obtains is carried out O, N gasometry, the O=0.0009% in alloy pig, N=0.0022%.The tubing that returns 617B alloy pig manufacturing is thus formed carries out Mechanics Performance Testing, room temperature condition lower yield strength 312MPa, tensile strength 713MPa, unit elongation 63%, relative reduction in area 48%.750 ℃ of hot conditions lower yield strength 270MPa, tensile strength 485MPa, unit elongation 68.5%, relative reduction in area 60%.Adopt the 617B tubing of virgin material preparation, room temperature condition lower yield strength 318MPa, tensile strength 711MPa, unit elongation 60.5%, relative reduction in area 46%.750 ℃ of hot conditions lower yield strength 255MPa, tensile strength 472MPa, unit elongation 66.5%, relative reduction in area 58.5%.Can find out, with the 617B mechanical properties of tubular goods of returns manufacturing with adopt virgin material to prepare the 617B mechanical properties of tubular goods to be in same level, also to satisfy ASME SB-167 standard.
Embodiment 2
The embodiment of the pure smelting process of alloy of this nickel base superalloy returns comprises following step successively:
1, returns pre-treatment
The block returns that produce in nickel base superalloy 617B tubing production process are carried out shot peening, block returns carry out shot-peening or sandblasting, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopt sandblasting less than φ 50mm equivalent size block material, the cleaning oil pollution on returns surfaces is clean;
The turning returns that produce in nickel base superalloy 617B tubing production process are carried out 240 ℃, and the high bake of 3h is processed, and the surface and oil contaminant of returns is cleaned out.
Block returns and turning returns weight proportion are 3:1.
2, make a vacuum induction ingot casting
At first block returns are placed in vacuum induction furnace, start vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.5Pa, the pressure of alloy melting phase vacuum tightness is between 1 ~ 3Pa, and melting period is added the turning returns 3 times altogether.Improve power transmission power, alloy molten solution is warming up to 1580 ℃, refining 40min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 0.8L/min, and the pressure of refining process vacuum tightness is between 1 ~ 3Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.The alloy molten solution of conjunctiva is reheated to 1470 ℃, pour into the vacuum induction ingot casting one time.
3, preparing the secondary vacuum induction smelts
1) chemical composition of a vacuum induction ingot casting of analysis is Cr 22.2% by weight percentage; Co 10.9%; Mo 9.0%; Al 1.67%; Ti 0.5%; C 0.52%; Zr 0.4%; B 0.0045%, and surplus is Ni.According to this chemical composition as seen, Co and Al need adjusting component all over composition range.
2) prepare cobalt, aluminium adjusting elemental composition materials, making a vacuum induction ingot casting composition that adds after adjusting is expected is Cr 21.9%; Co 11.7%; Mo 8.8%; Al 1.45%; Ti 0.46%; C 0.47%; Zr 0.35%; B 0.0039%, and surplus is Ni.
4, the secondary vacuum induction is smelted
Cobalt in the adjusting materials of vacuum induction ingot casting and above-mentioned preparation is placed in vacuum induction furnace, starts vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.6Pa, the pressure of alloy melting phase vacuum tightness is between 1 ~ 3Pa.Improve power transmission power, alloy molten solution is warming up to 1580 ℃, refining 30min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1.1L/min, and the pressure of refining process vacuum tightness is between 1 ~ 3Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.The alloy molten solution of conjunctiva is reheated to 1490 ℃, add the aluminium of regulating in materials, BOTTOM ARGON BLOWING 10min, argon flow amount are 0.5L/min, and the pressure of vacuum tightness is cooled to the surperficial conjunctiva of alloy molten solution again between 3 ~ 4Pa.
5, obtain the 617B alloy
The alloy molten solution of conjunctiva is reheated to 1490 ℃, and the pressure 3-4Pa of vacuum tightness pours into the 617B alloy pig.
The returns 617B alloy pig that obtains is carried out O, N gasometry, the O=0.0007% in alloy pig, N=0.0020%.The tubing that returns 617B alloy pig manufacturing is thus formed carries out Mechanics Performance Testing, room temperature condition lower yield strength 330MPa, tensile strength 725MPa, unit elongation 61%, relative reduction in area 47%.750 ℃ of hot conditions lower yield strength 266MPa, tensile strength 487MPa, unit elongation 66.5%, relative reduction in area 61%.Adopt the 617B tubing of virgin material preparation, room temperature condition lower yield strength 318MPa, tensile strength 711MPa, unit elongation 60.5%, relative reduction in area 46%.750 ℃ of hot conditions lower yield strength 255MPa, tensile strength 472MPa, unit elongation 66.5%, relative reduction in area 58.5%.Can find out, with the 617B mechanical properties of tubular goods of returns manufacturing with adopt virgin material to prepare the 617B mechanical properties of tubular goods to be in same level, also to satisfy ASME SB-167 standard.
Embodiment 3
The embodiment of the pure smelting process of alloy of this nickel base superalloy returns comprises following step successively:
1, returns pre-treatment
The block returns that produce in nickel base superalloy 617B tubing production process are carried out shot peening, block returns carry out shot-peening or sandblasting, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopt sandblasting less than φ 50mm equivalent size block material, the cleaning oil pollution on returns surfaces is clean;
The turning returns that produce in nickel base superalloy 617B tubing production process are carried out 300 ℃, and the high bake of 4h is processed, and the surface and oil contaminant of returns is cleaned out.
Block returns and turning returns weight proportion are 5:1.
2, make a vacuum induction ingot casting
At first block returns are placed in vacuum induction furnace, start vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.8Pa, the pressure of alloy melting phase vacuum tightness is between 3 ~ 5Pa, and melting period is added the turning returns 2 times altogether.Improve power transmission power, alloy molten solution is warming up to 1560 ℃, refining 40min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1.0L/min, and the pressure of refining process vacuum tightness is between 2 ~ 4Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.The alloy molten solution of conjunctiva is reheated to 1500 ℃, pour into the vacuum induction ingot casting one time.
3, preparing the secondary vacuum induction smelts
1) chemical composition of a vacuum induction ingot casting of analysis is Cr 22.5% by weight percentage; Co 12.0%; Mo 8.1%; Al 1.41%; Ti 0.25%; C 0.47%; Zr 0.28%; B 0.0038%, and surplus is Ni.According to this chemical composition as seen, Mo and Ti need adjusting component all over composition range.
2) prepare nickel, chromium, cobalt, molybdenum, aluminium, titanium, carbon, zirconium, ferro-boron as adjusting composition materials, making a vacuum induction ingot casting composition that adds after adjusting is expected is Cr 22.0%; Co 11.7%; Mo 9.2%; Al 1.40%; Ti 0.40%; C 0.50%; Zr 0.32%; B 0.0030%, and surplus is Ni.
4, the secondary vacuum induction is smelted
Nickel, chromium, cobalt, molybdenum in the adjusting materials of vacuum induction ingot casting and above-mentioned preparation are placed in vacuum induction furnace, start vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.5Pa, the pressure of alloy melting phase vacuum tightness is between 2 ~ 3Pa.Improve power transmission power, alloy molten solution is warming up to 1590 ℃, refining 35min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1.3L/min, and the pressure of refining process vacuum tightness is between 3 ~ 5Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.
The alloy molten solution of conjunctiva is reheated to 1500 ℃, add aluminium, titanium, carbon, zirconium, the ferro-boron regulated in materials, BOTTOM ARGON BLOWING 8min, argon flow amount is 0.8L/min, vacuum tightness is between 2 ~ 4Pa.Again be cooled to the surperficial conjunctiva of alloy molten solution.
5, obtain the 617B alloy
The alloy molten solution of conjunctiva is reheated to 1480 ℃, and the pressure 3-4Pa of vacuum tightness pours into the 617B alloy pig.
The returns 617B alloy pig that obtains is carried out O, N gasometry, the O=0.0008% in alloy pig, N=0.0021%.The tubing that returns 617B alloy pig manufacturing is thus formed carries out Mechanics Performance Testing, room temperature condition lower yield strength 311MPa, tensile strength 739MPa, unit elongation 58%, relative reduction in area 49.5%.750 ℃ of hot conditions lower yield strength 245MPa, tensile strength 466MPa, unit elongation 66%, relative reduction in area 57%.Adopt the 617B tubing of virgin material preparation, room temperature condition lower yield strength 318MPa, tensile strength 711MPa, unit elongation 60.5%, relative reduction in area 46%.750 ℃ of hot conditions lower yield strength 255MPa, tensile strength 472MPa, unit elongation 66.5%, relative reduction in area 58.5%.Can find out, with the 617B mechanical properties of tubular goods of returns manufacturing with adopt virgin material to prepare the 617B mechanical properties of tubular goods to be in same level, also to satisfy ASME SB-167 standard.
Embodiment 4
The embodiment of the pure smelting process of alloy of this nickel base superalloy returns comprises following step successively:
1, returns pre-treatment
The block returns that produce in nickel base superalloy 617B tubing production process are carried out shot peening, block returns carry out shot-peening or sandblasting, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopt sandblasting less than φ 50mm equivalent size block material, the cleaning oil pollution on returns surfaces is clean;
The turning returns that produce in nickel base superalloy 617B tubing production process are carried out 200 ℃, and the high bake of 3h is processed, and the surface and oil contaminant of returns is cleaned out.
Block returns and turning returns weight proportion are 4:1.
2, make a vacuum induction ingot casting
At first block returns are placed in vacuum induction furnace, start vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.5Pa, the pressure of alloy melting phase vacuum tightness is between 2 ~ 5Pa, and melting period is added the turning returns 3 times altogether.Improve power transmission power, alloy molten solution is warming up to 1590 ℃, refining 40min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1.2L/min, and the pressure of refining process vacuum tightness is between 2 ~ 5Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.The alloy molten solution of conjunctiva is reheated to 1520 ℃, pour into the vacuum induction ingot casting one time.
3, preparing the secondary vacuum induction smelts
1) chemical composition of a vacuum induction ingot casting of analysis is Cr 23.8% by weight percentage; Co 12.2%; Mo 9.3%; Al 1.45%; Ti 0.5%; C 0.35%; Zr 0.29%; B 0.0048%, and surplus is Ni.According to this chemical composition as seen, Cr surpasses composition range, needs adjusting component.
2) preparing chromium is Cr 22.7% as regulating the composition materials, make a vacuum induction ingot casting composition that adds after adjusting is expected; Co 12.0%; Mo 9.1%; Al 1.41%; Ti 0.43%; C 0.33%; Zr 0.24%; B 0.0042%, and surplus is Ni.
4, the secondary vacuum induction is smelted
Chromium in the adjusting materials of vacuum induction ingot casting and above-mentioned preparation is placed in vacuum induction furnace, starts vacuum apparatus and vacuumize, begin power transmission when the pressure of vacuum tightness is 0.6Pa, the pressure of alloy melting phase vacuum tightness is between 1 ~ 3Pa.Improve power transmission power, alloy molten solution is warming up to 1600 ℃, refining 30min carries out the BOTTOM ARGON BLOWING operation in refining process, and argon flow amount is 1.0L/min, and the pressure of refining process vacuum tightness is between 1 ~ 4Pa.Refining stops power transmission after finishing, and carries out the alloy molten solution freezing treatment, until the surperficial conjunctiva of alloy molten solution solidifies.
5, obtain the 617B alloy
The alloy molten solution of conjunctiva is reheated to 1510 ℃, and the pressure 3-4Pa of vacuum tightness pours into the 617B alloy pig.
The returns 617B alloy pig that obtains is carried out O, N gasometry, the O=0.0006% in alloy pig, N=0.0024%.The tubing that returns 617B alloy pig manufacturing is thus formed carries out Mechanics Performance Testing, room temperature condition lower yield strength 317MPa, tensile strength 716MPa, unit elongation 62.5%, relative reduction in area 53%.750 ℃ of hot conditions lower yield strength 242MPa, tensile strength 458MPa, unit elongation 67.5%, relative reduction in area 54%.Adopt the 617B tubing of virgin material preparation, room temperature condition lower yield strength 318MPa, tensile strength 711MPa, unit elongation 60.5%, relative reduction in area 46%.750 ℃ of hot conditions lower yield strength 255MPa, tensile strength 472MPa, unit elongation 66.5%, relative reduction in area 58.5%.Can find out, with the 617B mechanical properties of tubular goods of returns manufacturing with adopt virgin material to prepare the 617B mechanical properties of tubular goods to be in same level, also to satisfy ASME SB-167 standard.
In above-mentioned four embodiment, in step
IIn the returns preprocessing process, also can take the maximum linear dimension of block material to be not less than the shot peening of carrying out of 50mm, maximum linear dimension adopts sandblasting less than the block material of 50mm.
Claims (9)
1. the pure smelting process of the alloy of nickel base superalloy returns, it comprises following step:
IThe returns pre-treatment
Clout is expanded in the hot extrusion remainder material that produces in the block returns that a produces vacuum ingot, ESR ingot, pipe, hollow forging, cold rolled tube crop end in nickel base superalloy 617B tubing production process and hot extrusion process and hot reaming, block returns carry out shot-peening and sandblasting, and the cleaning oil pollution on returns surfaces is clean;
B carries out 200 ~ 300 ℃ to the turning returns of the vacuum ingot in nickel base superalloy 617B tubing production process, ESR ingot, pipe surface and heart section mechanical process, and the high bake of 2 ~ 4h is processed, and the surface and oil contaminant of turning returns is cleaned out;
Block returns and turning returns weight proportion are in (3 ~ 5): between 1:
II, make a vacuum induction ingot casting
Block returns in nickel base superalloy 617B tubing production process are placed in vacuum induction furnace, and the turning returns add during the phase at alloy melting as adding material in batches; Start vacuum apparatus and vacuumize, begin power transmission, the pressure≤5Pa of alloy melting phase vacuum tightness when the pressure of vacuum tightness≤1Pa; Improve power transmission power, begin refining when alloy molten solution is warming up to 1550 ~ 1600 ℃, refining time is 30 ~ 40min, carries out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness; After refining finishes, stop power transmission, carry out the alloy molten solution freezing treatment, until alloy molten solution surface conjunctiva solidifies, the alloy molten solution of conjunctiva is reheated to 1470 ~ 1520 ℃, pour into the vacuum induction ingot casting one time;
III, prepare the secondary vacuum induction and smelt
Analyze the chemical composition of a vacuum induction ingot casting, the mass percent of the chemical composition of a vacuum induction ingot casting reaches:
Cr 21.5~23%； Co 11.5~12.5%； Mo 8.5~9.5%；Al 1.1~1.5%；
Ti 0.3~0.6%； C 0.03~0.06%； Zr 0.02~0.045%； B 0.003~0.005%；
When all the other are Ni, prepare the secondary vacuum induction and smelt;
IV, secondary vacuum induction smelts
A vacuum induction ingot casting is placed in vacuum induction furnace, starting vacuum apparatus vacuumizes, begin power transmission when the pressure of vacuum tightness≤1Pa, carry out alloy melting, alloy molten solution is warming up to 1550 ~ 1600 ℃ carries out refining, refining time is 30 ~ 40min, carries out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness; Refining is carried out the alloy molten solution freezing treatment after finishing equally, until the surperficial conjunctiva of alloy molten solution solidifies;
V, obtain the 617B alloy
Refining is finished the alloy molten solution that the rear surface conjunctiva solidifies be heated to 1470～1520 ℃, the pressure≤5Pa of vacuum tightness pours into the 617B alloy pig.
2. the pure smelting process of the alloy of nickel base superalloy returns according to claim 1 is characterized in that: in step IV secondary vacuum induction smelting process, and the pressure≤5Pa of alloy melting phase vacuum tightness.
3. the pure smelting process of the alloy of nickel base superalloy returns according to claim 1 and 2, is characterized in that: step
IIn the returns preprocessing process, the maximum linear dimension of block material is not less than the shot peening of carrying out of 50mm, less than the block material employing sandblasting of 50mm.
4. the pure smelting process of the alloy of nickel base superalloy returns according to claim 1 and 2, is characterized in that: step
IIn the returns preprocessing process, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopts sandblasting less than φ 50mm equivalent size block material.
5. the pure smelting process of the alloy of nickel base superalloy returns, it comprises following step:
IThe returns pre-treatment
Clout is expanded in the hot extrusion remainder material that produces in the block returns that a produces vacuum ingot, ESR ingot, pipe, hollow forging, cold rolled tube crop end in nickel base superalloy 617B tubing production process and hot extrusion process and hot reaming, block returns carry out shot-peening and sandblasting, and the cleaning oil pollution on returns surfaces is clean;
B carries out 200 ~ 300 ℃ to the turning returns of the vacuum ingot in nickel base superalloy 617B tubing production process, ESR ingot, pipe surface and heart section mechanical process, and the high bake of 2 ~ 4h is processed, and the surface and oil contaminant of turning returns is cleaned out;
Block returns and turning returns weight proportion are in (3 ~ 5): between 1:
II, make a vacuum induction ingot casting
Block returns in nickel base superalloy 617B tubing production process are placed in vacuum induction furnace, and the turning returns add during the phase at alloy melting as adding material in batches; Start vacuum apparatus and vacuumize, begin power transmission, the pressure≤5Pa of alloy melting phase vacuum tightness when the pressure of vacuum tightness≤1Pa; Improve power transmission power, begin refining when alloy molten solution is warming up to 1550 ~ 1600 ℃, refining time is 30 ~ 40min, carries out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness; After refining finishes, stop power transmission, carry out the alloy molten solution freezing treatment, until alloy molten solution surface conjunctiva solidifies, the alloy molten solution of conjunctiva is reheated to 1470 ~ 1520 ℃, pour into the vacuum induction ingot casting one time;
III, prepare the secondary vacuum induction and smelt
Analyze the chemical composition of a vacuum induction ingot casting, the mass percent of any in the Cr of a vacuum induction ingot casting, Co, Mo, Al, Ti, C, Zr or B exceeds:
Cr 21.5~23%； Co 11.5~12.5%； Mo 8.5~9.5%； Al 1.1~1.5%；
Ti 0.3~0.6%； C 0.03~0.06%； Zr 0.02~0.045%； B 0.003~0.005%；
All the other are the scope of Ni;
Use the minimum a kind of as regulating the composition materials of nickel, chromium, cobalt, molybdenum, aluminium, titanium, carbon, zirconium, ferro-boron, make the mass percent of composition of the vacuum induction ingot casting after adjusting in the mentioned component scope;
IV, secondary vacuum induction smelts
A vacuum induction ingot casting is placed in vacuum induction furnace, and will regulate the minimum a kind of of composition materials also adds in vacuum induction furnace, starting vacuum apparatus vacuumizes, begin power transmission when the pressure of vacuum tightness≤1Pa, carry out alloy melting, alloy molten solution is warming up to 1550 ~ 1600 ℃ carries out refining, refining time is 30 ~ 40min, carry out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness; Refining is carried out the alloy molten solution freezing treatment after finishing, until the surperficial conjunctiva of alloy molten solution solidifies;
V, obtain the 617B alloy
The alloy molten solution of conjunctiva after alloying is heated to 1470～1520 ℃, and the pressure≤5Pa of vacuum tightness then pours into the 617B alloy pig.
6. the pure smelting process of the alloy of nickel base superalloy returns according to claim 5 is characterized in that: in step IV secondary vacuum induction smelting process, and the pressure≤5Pa of alloy melting phase vacuum tightness.
7. the pure smelting process of the alloy of according to claim 5 or 6 described nickel base superalloy returns, it is characterized in that: in step IV secondary vacuum induction smelting process, refining finishes and carries out the alloy molten solution freezing treatment, until after alloy molten solution surface conjunctiva solidifies, the alloy molten solution of conjunctiva is reheated be warming up to 1550 ~ 1600 ℃, also add other raw material of remaining adjusting composition materials in vacuum induction furnace, refining time is no less than 8min, carry out the BOTTOM ARGON BLOWING operation in refining process, and the pressure≤5Pa of control process vacuum tightness, again be cooled to the surperficial conjunctiva of alloy molten solution.
8. the pure smelting process of the alloy of according to claim 5 or 6 described nickel base superalloy returns, is characterized in that: step
IIn the returns preprocessing process, the maximum linear dimension of block material is not less than the shot peening of carrying out of 50mm, less than the block material employing sandblasting of 50mm.
9. the pure smelting process of the alloy of according to claim 5 or 6 described nickel base superalloy returns, is characterized in that: step
IIn the returns preprocessing process, the block material size is not less than the shot peening of carrying out of φ 50mm equivalent size, adopts sandblasting less than φ 50mm equivalent size block material.
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| CN104532063A (en) * | 2014-12-09 | 2015-04-22 | 抚顺特殊钢股份有限公司 | Method for smelting low-carbon hyperpure nickel-based alloy from high-Al and Ti returns as raw materials |
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| CN111823063A (en) * | 2020-07-17 | 2020-10-27 | 江苏美特林科特殊合金股份有限公司 | Surface treatment method and application of high-temperature alloy return |
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