CN114657398A - Large-size nickel-based high-temperature alloy ingot difficult to deform and preparation method thereof - Google Patents
Large-size nickel-based high-temperature alloy ingot difficult to deform and preparation method thereof Download PDFInfo
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Abstract
The application discloses a large-size nickel-based high-temperature alloy ingot difficult to deform and a preparation method thereof, wherein the preparation method comprises the following steps: triple smelting: carrying out triple smelting on a high-temperature alloy raw material through vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting to obtain a consumable ingot; homogenization treatment: carrying out multi-section homogenization treatment to preserve the heat of the consumable ingot; heating and preserving heat; heating and preserving heat; and heating, preserving heat and cooling to obtain the large-size nickel-based high-temperature alloy ingot which is difficult to deform. The method provided by the application can be used for stably preparing the phi 660 mm-specification hard-deformation nickel-based high-temperature alloy, the segregation of the prepared alloy ingot is low, the cracking problem of a large-size ingot is solved, the metallurgical quality of the hard-deformation high-temperature alloy is improved, the thermoplasticity is high, the later forging cogging cracking is further reduced, and a foundation is laid for preparing large-size bars and large-size disc forgings.
Description
Technical Field
The application relates to the technical field of high-temperature alloys, in particular to a large-size nickel-based high-temperature alloy ingot difficult to deform and a preparation method thereof.
Background
The turbine disk is a key hot end component of the engine, and the metallurgical quality and performance level of the turbine disk are decisive for improving the reliability, the safe life and the performance of the engine. With the development of high thrust/power-weight ratio engines, higher requirements are put on the temperature bearing capacity, high-temperature strength, long service life, toughness, fatigue property, reliability and durability of a turbine disc, and the nickel-based wrought superalloy for the turbine disc is required to have higher and higher alloying degree, higher and higher gamma' phase content and higher purity; meanwhile, the diameter of the turbine disc is also enlarged, and large-specification bars and large-ingot steel ingots are required, which continuously increase the difficulty in preparing alloys and the turbine disc.
GH4742 is Ni-based precipitation hardening type deformation high-temperature alloy, has higher endurance and creep strength and good comprehensive capability within the range of 650-800 ℃, has better structural stability and corrosion resistance, and is widely applied to manufacturing high-temperature bearing parts of aviation and aerospace engines and ship gas engines, such as turbine discs and the like.
At present, GH4742 alloy is mainly produced in large scale by a two-connection smelting process (vacuum induction furnace smelting (VIM) and vacuum consumable remelting smelting (VAR)), but because the alloy has high alloying degree and the VIM ingot and the VAR ingot have poor thermoplasticity, the prepared consumable ingot is easy to crack, and especially the cracking of a large ingot is more obvious; meanwhile, electrodes prepared by VIM often have cracks and deep shrinkage holes, VAR smelting is directly carried out, fluctuation of a smelting curve is large, dendrite segregation is difficult to control, the risk of metallurgical defects is increased, and the metallurgical quality of consumable ingots is seriously influenced. Therefore, in order to control the dendrite segregation degree of the alloy and prevent the steel ingot from cracking, the maximum size of the consumable ingot of the alloy is phi 508mm abroad. Because the consumable ingot is small in size, large-size bar and large-size disc forgings are required to be prepared, the process is complex, cracking is easy to occur, the dendrite segregation degree is high, impurities are more, the cost is high, and the popularization and the application of the alloy are influenced.
Disclosure of Invention
In order to prepare a large-size nickel-based high-temperature alloy ingot with higher metallurgical quality and difficult deformation, the application provides the large-size nickel-based high-temperature alloy ingot with difficult deformation and a preparation method thereof.
In a first aspect, the application provides a preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform, which adopts the following technical scheme:
a preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform comprises the following steps:
triple smelting: smelting a high-temperature alloy raw material by a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting to obtain a consumable ingot;
homogenizing: carrying out multi-stage homogenization treatment, and preserving the temperature of the consumable ingot at 830 ℃ -; then heating to 1115-1125 ℃, and preserving heat; heating to 1130-1140 deg.c and maintaining; heating to 1170-1190 deg.c, maintaining and cooling to obtain large scale hard-to-deform Ni-base high temperature alloy ingot.
By adopting the technical scheme, the ternary smelting process is adopted in the method, the nickel-based high-temperature alloy consumable ingot which is difficult to deform and has the specification of phi 660mm can be prepared, the dendritic crystal segregation degree of the obtained consumable ingot is low, the multi-section homogenization treatment of the consumable ingot is combined, the consumable ingot is subjected to low-temperature pretreatment at first, a low-melting-point phase appearing at a crystal boundary is dissolved, then high-temperature diffusion is carried out, the dendritic crystal segregation is further eliminated, the component segregation and the structure segregation of the obtained large-specification consumable ingot are obviously improved, the obtained ingot is uniform in structure, the thermoplasticity of the ingot is improved, the hot working window of the ingot is expanded, the ingot is further prevented from cracking, the large-specification nickel-based high-temperature alloy ingot can be stably prepared, and a foundation is laid for preparing large-specification bars and large-size disc forgings.
Preferably, in the homogenization treatment step, the temperature of the consumable ingot is raised to 1120 +/-10 ℃ and then is kept for 10-14 h; heating the consumable ingot to 1135 +/-10 ℃, and then preserving heat for 22-26 h;
and heating the consumable ingot to 1180 +/-20 ℃, and then preserving the temperature for 62-66 h.
Preferably, in the homogenization treatment step, the heating rate of the temperature rise to 1120 +/-10 ℃ is (45-60) DEG C/h;
the heating rate of heating to 1135 +/-10 ℃ is (4-10) DEG C/h;
the heating rate is (3-6) DEG C/h when the temperature is increased to 1180 +/-20 ℃.
By adopting the technical scheme, a multi-section homogenization system is implemented on the consumable ingot obtained by triple smelting in the method, the consumable ingot is heated to 1120 +/-10 ℃ and then is subjected to heat preservation, so that the low-melting-point phase sigma of the high-temperature alloy difficult to deform is dissolved back in a solid solution mode, then the temperature is heated to 1135 +/-10 ℃ at the heating rate of (4-10) DEG C and is subjected to heat preservation, the low-melting-point phase eta and boride are continuously dissolved back, and the excessively large internal and external temperature difference caused by the excessively fast heating and the excessively slow heating can be prevented from causing the excessively long process time and the increase of the fuel cost by adopting the heating rate of (4-10) DEG C/h. And finally, heating to 1180 +/-20 ℃ at the heating rate of (3-6) DEG C/h, accelerating the diffusion of elements, reducing microsegregation, and finally adopting the multi-section homogenization system in the application to obviously reduce the component segregation and the structure segregation of the consumable ingot, thereby obtaining the ingot with a uniform structure and improving the plasticity of the ingot.
Preferably, the vacuum induction smelting in the triple smelting step comprises the following steps:
s1-1, smelting the high-temperature alloy raw material in a vacuum induction furnace, wherein the smelting in the vacuum induction furnace comprises full melting, refining and tapping, the full melting temperature is 1480-1580 ℃, and the vacuum degree of the full melting is 0-50 Pa; the refining temperature is 1500-;
s1-2, pouring in vacuum, pouring the molten steel into an ingot mold which is heated to 200 and 500 ℃ in advance to obtain a VIM electrode rod;
s1-3, transferring the obtained VIM electrode rod into an annealing furnace within 2 hours for stress relief annealing, wherein the annealing temperature is 800-1200 ℃, and the temperature is kept for more than 10 hours to obtain the annealed VIM electrode rod.
By adopting the technical scheme, the GH4742 alloy induction ingot has qualified components, the internal stress is obviously reduced, and no crack is generated according to the standard requirement
Preferably, in the triple smelting step, the protective atmosphere electroslag remelting comprises the following steps:
s2-1, obtaining the annealed VIM electrode bar after vacuum induction melting, performing car polishing treatment on the surface, then performing electrode welding, and performing preparation work of protective atmosphere electroslag remelting;
s2-2, selecting a slag system;
s2-3: selecting a crystallizer, introducing argon for protection, wherein the filling ratio of the VIM electrode bar to the crystallizer is 0.5-0.9, the whole argon flow is 30-120L/min, and performing the working procedures of slagging, arcing, remelting, feeding, cooling and demolding to obtain a P-ESR electrode bar;
s2-4, performing stress relief annealing on the obtained P-ESR electrode rod within 2 hours, wherein the annealing temperature is 800-1180 ℃, and preserving the heat for 18 hours to obtain the annealed P-ESR electrode rod.
By adopting the technical scheme, the electrode prepared by the protective atmosphere electroslag remelting (P-ESR) has the advantages of compact structure, good plasticity and high purity, the cracking problem of the large-size steel ingot of the alloy is solved by combining with proper process parameter matching control, and a foundation is laid for realizing the preparation of the consumable steel ingot with the diameter of 660 mm.
Preferably, in the step of electroslag remelting in a protective atmosphere, the electroslag selected in S2-2 comprises the following components in percentage by weight: CaF2：36-60％；Al2O3: 13 to 30 percent; CaO: 12 to 35 percent; MgO: 1 to 15 percent; the balance being TiO2More preferably, Al2O3The addition amount of (B) is 13-15%.
By adopting the technical scheme, the proportion of the electroslag components in the protective atmosphere electroslag remelting step is selected, the consumable ingot with the specification size of phi 660mm can be stably prepared, the cracking problem of the large-size consumable ingot is solved, the dendritic crystal segregation degree of the obtained consumable ingot is low, the content of sulfur and impurities is greatly reduced, and the purity of metallurgy is improved.
Preferably, in the triple smelting step, the vacuum consumable remelting comprises the following steps: s3-1, performing polishing or grinding treatment on the surface of the annealed P-ESR electrode bar obtained by electroslag remelting in a protective atmosphere, processing the surface until two end faces are parallel, and then performing electrode welding;
s3-2, controlling the initial vacuum degree below 1.0Pa and the air leakage rate below 0.5 Pa/min;
s3-3, filling helium gas for cooling during smelting, and respectively performing the technical processes of an arc starting stage, a stabilizing stage, a feeding stage, cooling, breaking the air and demolding, wherein the control parameters of the technical process are set as follows: the control range of the melting speed is 2.8-5.0kg/min, the control range of the helium pressure is 1000Pa, the vacuum degree in the stable melting stage is less than or equal to 1.5Pa, and the control range of the cooling water temperature is 18-38 ℃, so that VAR consumable ingots are obtained;
s3-3 and VAR consumable ingots are transferred into an annealing furnace for stress relief annealing within 1 hour, the annealing temperature is 900-1200 ℃, and the temperature is kept for more than 12 hours.
By adopting the technical scheme, the consumable ingot with the specification of phi 660mm is successfully prepared by optimizing and screening the technological parameters of vacuum consumable remelting and smelting, and the dendritic crystal segregation degree of the consumable ingot is lower.
Preferably, the large-size nickel-based high-temperature alloy ingot difficult to deform is a GH4742 alloy ingot, and the high-temperature alloy raw material in the triple smelting step is a GH4742 alloy raw material.
By adopting the technical scheme, after the GH4742 alloy is subjected to triple smelting steps and homogenization treatment by adopting the parameters and the steps, a refractory high-temperature alloy ingot with the specification of phi 660mm can be stably obtained, the obtained ingot has low dendrite segregation and uniform structure, the plasticity is improved, the problem that the ingot with a large size is easy to crack when a traditional two-connection process is adopted in the prior art is solved, the batch production of the refractory high-temperature alloy is realized by the method, and a foundation is laid for preparing large-size GH4742 alloy bars and disc forgings.
Preferably, in the raw materials of the GH4742 alloy, the sum of the weight percentages (wt.%) of Al, Ti and Nb is between 7.20 and 8.40%.
Preferably, in the GH4742 alloy raw material, the sum of the weight percentages (wt.%) of Mo, Co and Cr is between 26.5 and 31.5%.
In a second aspect, the application provides a large-size nickel-based superalloy ingot difficult to deform, which adopts the following technical scheme:
a large-size Nees-sister high-temperature alloy cast ingot is prepared by the preparation method.
By adopting the technical scheme, on the basis of the original two-connection smelting process, the electroslag remelting smelting step in the protective atmosphere is added, the consumable ingot with the large specification of phi 660mm is prepared through the three-connection smelting process, dendritic crystal segregation of the obtained consumable ingot is reduced, and the consumable ingot is matched with a multi-stage homogenization system of a specific system, so that the consumable ingot can be pretreated at a low temperature, a low-melting-point phase appears at a dissolved crystal boundary, and then high-temperature diffusion is carried out, dendritic crystal segregation is further eliminated, the thermoplasticity of the ingot is improved, the cracking tendency in later-stage cogging forging is reduced, stable mass production can be realized, a good foundation is laid for preparing large-specification bars and disc forgings, and the problems that the consumable ingot obtained through the two-connection process in the prior art is small in specification, the large-specification consumable ingot is easy to crack, and mass production cannot be realized are solved.
In summary, the present application has the following beneficial effects:
according to the method, on the basis of the original two-connection smelting process, the electroslag remelting smelting step in the protective atmosphere is added, the consumable ingot with the large specification of phi 660mm is prepared through the three-connection smelting process, dendritic crystal segregation of the obtained consumable ingot is reduced, and the consumable ingot is matched with a multi-section homogenization system of a specific system, so that the consumable ingot can be pretreated at a low temperature, a low-melting-point phase appears at a dissolved crystal boundary, high-temperature diffusion is carried out, dendritic crystal segregation is further eliminated, the thermoplasticity of the ingot is improved, the cracking tendency in later cogging forging is reduced, stable mass production can be realized, a good foundation is laid for preparing large-specification bar and disc forgings, and the problems that the consumable ingot obtained through the two-connection process in the prior art is small in specification, and the large-specification consumable ingot is easy to crack are solved.
Drawings
FIG. 1 is a structural diagram of the as-cast structure of a consumable ingot obtained by triple smelting in example 2 of the present application;
FIG. 2 is a microstructure of a consumable ingot obtained by triple smelting in example 2 of the present application, wherein (a) is an interdendritic morphology, and (b) is a dendrite trunk morphology;
FIG. 3 is a metallographic graph showing a microstructure of an alloy ingot obtained by homogenization treatment in example 2 of the present application;
FIG. 4 is a gamma' -phase distribution diagram of an alloy ingot obtained after homogenization treatment in example 2 of the present application;
FIG. 5 is a carbide morphology distribution diagram of an alloy ingot obtained after homogenization treatment in example 2 of the present application;
FIG. 6 is a microstructure diagram of an alloy ingot obtained in comparative example 3 of the present application;
FIG. 7 is a microstructure diagram of an alloy ingot obtained in comparative example 4 of the present application;
FIG. 8 is a microstructure diagram of an alloy ingot obtained in comparative example 5 of the present application;
FIG. 9 is a microstructure diagram of an alloy ingot obtained in comparative example 6 of the present application.
Detailed Description
The present application will now be described in further detail with reference to the following figures and examples, in which: the following examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer, and the starting materials used in the following examples are available from ordinary commercial sources unless otherwise specified.
Along with the development of a high thrust/power-weight ratio engine, the nickel-based wrought superalloy for a turbine disc is required to have higher and higher alloying degree and higher gamma 'phase content, the diameter of the turbine disc is also increased, large-sized bars and large-sized steel ingots are required, particularly, the specification and size requirements of ships on the turbine disc are higher and higher, for example, GH4742 alloy is a typical hard-to-deform nickel-based superalloy, the sum of main aging strengthening elements Al, Ti and Nb is close to 8.0 wt.%, the gamma' phase mass fraction exceeds 40% (exceeds the level of certain cast superalloys), and meanwhile, the nickel-based wrought superalloy also contains solid solution strengthening elements such as Cr, Co and Mo, the total amount of which is close to 30 wt.%. Due to such high alloying degree, dendrite segregation is severe and cracking tendency is large in the alloy smelting process, particularly dendrite segregation is severe and cracking risk is large for large ingot shapes, so that in the related technologies at home and abroad at present, the GH4742 ingot shape obtained by the two-link smelting process is only phi 508mm, and the requirements of ships on the size and the performance of the turbine disk cannot be met.
Aiming at the situation, the inventor researches a great deal of theoretical research and a great deal of test and exploration, develops a triple smelting process aiming at GH4742 alloy on the basis of the existing triple smelting, controls the process and process parameters, GH4742 alloy ingot shapes with the specification of phi 660mm can be prepared, aiming at the novel consumable ingot obtained by the triple smelting process, the homogenization system is improved and matched, through the multi-section homogenization treatment process and the control of process parameters such as heating rate, heating temperature and the like, the further treatment of the consumable ingot obtained by triple smelting can further reduce the dendrite segregation, so that the alloy components are distributed more uniformly, the obtained structure is more uniform, the alloy thermoplasticity is improved, the cracking tendency in the later cogging forging process is reduced, therefore, large-size cast ingots can be stably prepared, and a good foundation is laid for preparing large-size bar and disc forgings.
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform comprises the following steps:
triple smelting: smelting a high-temperature alloy raw material by a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting to obtain a consumable ingot, wherein the high-temperature alloy raw material can be selected from electrolytic nickel, metal chromium, a cobalt plate, a molybdenum strip, an electrolytic aluminum block, sponge titanium, high-purity carbon, nickel magnesium, nickel niobium and the like;
homogenizing: adopting multi-stage homogenization treatment, heating the consumable ingot (2-4) h to 830-970 ℃, and preserving the heat at 830-970 ℃ for (2-4) h; then heating to (1115) -1125 ℃ at the heating rate of (45-60) DEG C/h, and preserving the heat for 10-14 h; heating to 1130-; heating to 1190 ℃ at the temperature rise rate of 3-6 ℃ per hour, preserving the temperature for 62-66 hours, and cooling to obtain the large-specification nickel-based high-temperature alloy ingot difficult to deform.
More preferably, the temperature control in the multistage homogenization treatment system is: preserving the heat of the consumable ingot at 900 ℃; then heating to 1120 deg.C, and keeping the temperature for 10-14h, such as 10h, 12h or 14 h; heating to 1135 deg.C, and maintaining for 22-26h, such as 22h, 24h or 26 h; and heating to 1180 ℃, preserving the heat for 62-66 hours such as 62 hours, 64 hours or 66 hours, and then cooling to obtain the large-size nickel-based high-temperature alloy ingot difficult to deform.
In the case of the above-described temperature gradient selection, it is preferable to control the temperature rise rate as follows: the heating rate of heating to (1115) -1125 ℃ is (50-55) ° c/h, and specifically can be 50 ℃, 52 ℃ or 55 ℃; the temperature rise rate of the temperature rise to (1130-; the temperature rise rate when the temperature rises to (1170-.
The following is described in detail with reference to specific examples, and the triple smelting process in the following examples is described by taking a typical ingot shape of phi 660mm as an example, but an ingot with a specification size smaller than the phi 660mm can also be obtained by the method in the application. The percentages referred to in the following examples are percentages by weight.
Example 1
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform comprises the following steps:
triple smelting: raw materials of the GH4742 high-temperature deformation-resistant nickel-based superalloy sequentially pass through S1: vacuum induction melting, S2: protective atmosphere electroslag remelting and S3: carrying out vacuum consumable remelting triple smelting to obtain a consumable ingot, wherein the diameter of an alloy ingot subjected to vacuum induction smelting (VIM) is 410mm, the diameter of an alloy ingot subjected to protective atmosphere electroslag remelting (P-ESR) is 580mm, and the diameter of an alloy ingot subjected to vacuum consumable remelting (VAR) is 660 mm; wherein, S1: the Vacuum Induction Melting (VIM) operation specifically comprises the steps of:
s1-1, weighing the raw materials according to the component requirements of the GH4742 alloy, wherein the raw materials comprise the following components in percentage by weight: c: 0.04; co: 10.0; cr: 13.0; mo: 4.5; ti: 2.50; al: 2.5; nb: 2.7; adding the raw materials into a vacuum induction furnace, wherein the vacuum induction furnace comprises a full melting period, a refining period and a tapping period, the full melting temperature of the full melting period is 1480 ℃, and the vacuum degree of the full melting is 10 Pa; the refining temperature in the refining period is 1500 ℃, the refining vacuum degree is 8Pa, and the tapping temperature in the tapping period is controlled to 1410 ℃;
s1-2, after the tapping period, pouring in vacuum, pouring molten steel into an ingot mold which is heated to 200 ℃ in advance, and adding a heat preservation measure at a riser to obtain a VIM electrode rod;
s1-3, transferring the obtained VIM electrode rod into an annealing furnace within 2 hours for stress relief annealing, wherein the annealing temperature is 800-1200 ℃, the temperature is kept for 10 hours, and then the electrode rod is obtained through machining.
S2: the specific operation of the protective atmosphere electroslag remelting (P-ESR) comprises the following steps:
s2-1, carrying out vacuum induction melting to obtain an annealed VIM electrode bar, carrying out surface polishing treatment, cutting off a cap, carrying out electrode welding, and carrying out preparation work of protective atmosphere electroslag remelting;
s2-2, selecting a slag system: the selected slag system comprises the following components in percentage by weight: CaF2：38％；Al2O3: 16 percent; CaO: 12 percent; MgO: 1 percent; the balance being TiO2；
S2-3: selecting a crystallizer, introducing argon for protection, wherein the filling ratio of the VIM electrode bar to the crystallizer is 0.7, the argon flow is 30-90L/min in the whole process, and then carrying out slagging, arcing, remelting, feeding, cooling and demolding treatment to obtain a P-ESR electrode bar;
s2-3, performing stress relief annealing on the obtained P-ESR electrode rod within 2 hours, keeping the annealing temperature at 850-1150 ℃ for 18 hours, and then machining to obtain the annealed P-ESR electrode rod.
S3: the specific operation of vacuum consumable remelting (VAR) comprises the following steps:
s3-1, performing polishing on the surface of the annealed P-ESR electrode bar obtained by electroslag remelting in a protective atmosphere, then cutting off a dead head, processing until two end faces are parallel, and then performing electrode welding;
s3-2, controlling the initial vacuum degree to be 0.9Pa, and controlling the air leakage rate to be 0.43 Pa/min;
s3-3, charging 400Pa helium gas for cooling during smelting, and respectively performing the processes of an arc starting stage, a stabilization stage, a feeding stage, cooling, breaking and demoulding, wherein the arc starting stage is controlled by current and molten drops, the current is 3.5kA, the voltage is 23.4V, and the time of the arc starting stage is 50 min; the melting speed in the stable stage is 2.9kg/min, and the vacuum degree in the stable melting stage is 1 Pa; in the feeding stage, the current is 1kA/s, the cooling water temperature is 20 ℃, the cooling time is 5 hours, and then the blank breaking and demoulding are carried out to obtain a VAR consumable ingot;
s3-3, transferring the obtained VAR consumable ingot into an annealing furnace for stress relief annealing within 1 hour, wherein the annealing temperature is 960-1170 ℃, and the temperature is maintained for 14 hours to obtain a GH4742 alloy consumable ingot with the diameter of 660 mm;
homogenizing: the homogenization treatment adopts multi-stage homogenization treatment, and the concrete operations are as follows: heating up GH4742 alloy consumable ingot phi of 660mm obtained by triple smelting to 900 ℃ within 2h, preserving heat for 4h, then heating up to 1120 ℃ at a heating rate of 52 ℃/h, and preserving heat for 12 h; heating to 1135 ℃ at the heating rate of 8 ℃/h, and keeping the temperature for 24 h; heating to 1180 ℃ at the heating rate of 5 ℃/h, preserving heat for 64h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Example 2
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform comprises the following steps:
triple smelting: sequentially passing raw materials of GH4742 high-temperature deformation-resistant nickel-based superalloy through S1: vacuum induction melting, S2: protective atmosphere electroslag remelting and S3: carrying out vacuum consumable remelting triple smelting to obtain a consumable ingot, wherein the diameter of an alloy ingot subjected to vacuum induction smelting (VIM) is 390mm, the diameter of an alloy ingot subjected to protective atmosphere electroslag remelting (P-ESR) is 600mm, and the diameter of an alloy ingot subjected to vacuum consumable remelting (VAR) is 660 mm; wherein, S1: the Vacuum Induction Melting (VIM) operation specifically comprises the steps of:
s1-1, weighing the raw materials according to the component requirements of the GH4742 alloy, wherein the raw materials comprise the following components in percentage by weight: c: 0.05; co: 10.5; cr: 13.5; mo: 5.5; ti: 2.60 of; al: 2.55; nb: 2.7; adding the balance of Ni into a vacuum induction furnace, wherein the vacuum induction furnace smelting comprises a full melting period, a refining period and a tapping period, the full melting temperature of the full melting period is 1500 ℃, and the vacuum degree of full melting is 15 Pa; the refining temperature in the refining period is 1520 ℃, the refining vacuum degree is 6Pa, and the tapping temperature in the tapping period is controlled to be 1430 ℃;
s1-2, after the tapping period, pouring in vacuum, pouring molten steel into an ingot mold which is heated to 300 ℃ in advance, and adding a heat preservation measure at a riser to obtain a VIM electrode rod;
s1-3, transferring the obtained VIM electrode rod into an annealing furnace within 2 hours for stress relief annealing, keeping the temperature at 850-1180 ℃ for 12 hours, and then machining to obtain the electrode rod.
S2: the specific operation of the protective atmosphere electroslag remelting (P-ESR) comprises the following steps: s2-1, carrying out vacuum induction melting to obtain an annealed VIM electrode bar, carrying out surface polishing treatment, cutting off a cap, carrying out electrode welding, and carrying out preparation work of protective atmosphere electroslag remelting;
s2-2, selecting a slag system: the selected slag system comprises the following weight percentageThe components of the ratio: CaF2：40％；Al2O3: 18 percent; CaO: 13 percent; MgO: 2 percent; the balance being TiO2；
S2-3: selecting a crystallizer, introducing argon for protection, wherein the filling ratio of the VIM electrode bar to the crystallizer is 0.65, the argon flow is 30-90L/min in the whole process, and then carrying out slagging, arcing, remelting, feeding, cooling and demolding treatment to obtain a P-ESR electrode bar;
s2-3, performing stress relief annealing on the obtained P-ESR electrode rod within 2 hours, keeping the annealing temperature at 850-1170 ℃, and then performing machining to obtain the annealed P-ESR electrode rod.
S3: the specific operation of vacuum consumable remelting (VAR) comprises the following steps:
s3-1, performing polishing on the surface of the annealed P-ESR electrode bar obtained by electroslag remelting in a protective atmosphere, then cutting off a dead head, processing until two end faces are parallel, and then performing electrode welding;
s3-2, controlling the initial vacuum degree to be 0.8Pa and the air leakage rate to be 0.45 Pa/min;
s3-3, charging helium gas of 400Pa for cooling during smelting, and respectively performing the technical processes of an arc starting stage, a stabilization stage, a feeding stage, cooling, air breaking and demoulding, wherein the arc starting stage adopts current and molten drop control, the current is 3.6kA, the voltage is 23.2V, and the time of the arc starting stage is 55 min; the melting speed in the stable stage is 3.0kg/min, and the vacuum degree in the stable melting stage is 2 Pa; in the feeding stage, the current is 1.2kA/s, the cooling water temperature is 22 ℃, the cooling time is 4 hours, and then the blank breaking and demoulding are carried out to obtain a VAR consumable ingot;
s3-3, transferring the obtained VAR consumable ingot into an annealing furnace for stress relief annealing within 1 hour, wherein the annealing temperature is 960-1150 ℃, and the temperature is kept for 15 hours to obtain a GH4742 alloy consumable ingot with the diameter of 660 mm;
homogenizing: the homogenization treatment adopts multi-stage homogenization treatment, and the concrete operations are as follows: heating up GH4742 alloy consumable ingot phi of 660mm obtained by triple smelting to 900 ℃ within 2h, preserving heat for 4h, then heating up to 1120 ℃ at a heating rate of 52 ℃/h, and preserving heat for 12 h; heating to 1135 ℃ at the heating rate of 8 ℃/h, and keeping the temperature for 24 h; heating to 1180 ℃ at the heating rate of 5 ℃/h, preserving heat for 64h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Example 3
A preparation method of a large-size deformation-resistant nickel-based superalloy ingot comprises the following steps:
triple smelting: raw materials of the GH4742 high-temperature deformation-resistant nickel-based superalloy sequentially pass through S1: vacuum induction melting, S2: protective atmosphere electroslag remelting and S3: carrying out vacuum consumable remelting triple smelting to obtain a consumable ingot, wherein the diameter of an alloy ingot subjected to vacuum induction smelting (VIM) is 360mm, the diameter of an alloy ingot subjected to protective atmosphere electroslag remelting (P-ESR) is 440mm, and the diameter of an alloy ingot subjected to vacuum consumable remelting (VAR) is 660 mm; wherein, S1: the Vacuum Induction Melting (VIM) operation specifically comprises the steps of:
s1-1, weighing the raw materials according to the component requirements of the GH4742 alloy, wherein the raw materials comprise the following components in percentage by weight: c: 0.08; co: 10.5; cr: 13.5; mo: 5.0; ti: 2.55; al: 2.55; nb: 2.75; adding the balance of Ni into a vacuum induction furnace, wherein the vacuum induction furnace smelting comprises a full melting period, a refining period and a tapping period, the full melting temperature of the full melting period is 1520 ℃, and the vacuum degree of full melting is 5 Pa; the refining temperature in the refining period is 1530 ℃, the refining vacuum degree is 5Pa, and the tapping temperature in the tapping period is controlled to 1440 ℃;
s1-2, after the tapping period, pouring in vacuum, pouring molten steel into an ingot mold which is heated to 350 ℃ in advance, and adding a heat preservation measure at a riser to obtain a VIM electrode rod;
s1-3, transferring the obtained VIM electrode rod into an annealing furnace within 2 hours for stress relief annealing, keeping the temperature for 10 hours at 860 and 1130 ℃, and then machining to obtain the electrode rod.
S2: the specific operation of the protective atmosphere electroslag remelting (P-ESR) comprises the following steps: s2-1, carrying out vacuum induction melting to obtain an annealed VIM electrode bar, carrying out surface polishing treatment, cutting off a cap, carrying out electrode welding, and carrying out preparation work of protective atmosphere electroslag remelting;
s2-2, selecting a slag system: the selected slag system comprises the following components in percentage by weight: CaF2：39％；Al2O3: 20 percent; CaO: 14 percent; MgO: 3 percent; the balance beingTiO2；
S2-3: selecting a crystallizer, introducing argon for protection, wherein the filling ratio of the VIM electrode bar to the crystallizer is 0.8, the argon flow is 30-90L/min in the whole process, and then carrying out slagging, arcing, remelting, feeding, cooling and demolding treatment to obtain a P-ESR electrode bar;
s2-3, performing stress relief annealing on the obtained P-ESR electrode rod within 2 hours, keeping the annealing temperature at 880-1160 ℃, preserving the heat for 18 hours, and then machining to obtain the annealed P-ESR electrode rod.
S3: the specific operation of vacuum consumable remelting smelting (VAR) comprises the following steps:
s3-1, performing polishing on the surface of an annealed P-ESR electrode bar obtained by electroslag remelting in a protective atmosphere, then cutting off a riser, processing until two end faces are parallel, and then performing electrode welding;
s3-2, controlling the initial vacuum degree to be 0.8Pa and the air leakage rate to be 0.45 Pa/min;
s3-3, charging helium gas of 400Pa for cooling during smelting, and respectively performing the technical processes of an arc starting stage, a stabilization stage, a feeding stage, cooling, air breaking and demoulding, wherein the arc starting stage adopts current and molten drop control, the current is 3.6kA, the voltage is 23.2V, and the time of the arc starting stage is 55 min; the melting speed in the stable stage is 3.0kg/min, and the vacuum degree in the stable melting stage is 2 Pa; in the feeding stage, the current is 1.2kA/s, the cooling water temperature is 22 ℃, the cooling time is 4 hours, and then the blank breaking and demoulding are carried out to obtain a VAR consumable ingot;
s3-3, transferring the obtained VAR consumable ingot into an annealing furnace for stress relief annealing within 1 hour, wherein the annealing temperature is 960-1150 ℃, and the temperature is kept for 15 hours to obtain a GH4742 alloy consumable ingot with the diameter of 660 mm;
homogenization treatment: the homogenization treatment adopts multi-stage homogenization treatment, and the concrete operations are as follows: heating up GH4742 alloy consumable ingots with the diameter of 660mm obtained by triple smelting to 900 ℃ within 2h, preserving heat for 4h, then heating up to 1120 ℃ at the heating rate of 52 ℃/h, and preserving heat for 12 h; heating to 1135 ℃ at the heating rate of 8 ℃/h, and keeping the temperature for 24 h; heating to 1180 ℃ at the heating rate of 5 ℃/h, preserving heat for 64h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Example 4
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that the homogenization treatment step comprises the following operations: heating up a GH4742 alloy consumable ingot with the diameter of 660mm obtained by triple smelting to 830 ℃, preserving heat for 2 hours, then heating up to 1115 ℃ at the heating rate of 55 ℃/h, and preserving heat for 12 hours; heating to 1130 ℃ at the heating rate of 8 ℃/h, and keeping the temperature for 24 h; raising the temperature to 1170 ℃ at the temperature raising rate of 5 ℃/h, preserving the temperature for 64h, and then cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Example 5
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that the homogenization treatment step comprises the following operations: heating up GH4742 alloy consumable ingots with the diameter of 660mm obtained by triple smelting to 970 ℃, preserving heat for 4 hours, then heating up to 1125 ℃ at the heating rate of 50 ℃/h, and preserving heat for 12 hours; heating to 1140 ℃ at the heating rate of 6 ℃/h, and keeping the temperature for 24 h; heating to 1190 ℃ at the heating rate of 4 ℃/h, preserving heat for 64h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Examples 6 to 8
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that in the homogenization treatment step, the heating rates of heating to 1120 ℃ are 45 ℃/h, 50 ℃/h and 60 ℃/h respectively.
Examples 8 to 11
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and the difference is that in the homogenization treatment step, the heating rates of heating to 1135 ℃ are 5 ℃, 8 ℃ and 10 ℃.
Examples 12 to 14
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and the difference is that in the homogenization treatment step, the heating rates of heating to 1180 ℃ are 3 ℃, 5 ℃ and 6 ℃.
Example 15
The preparation method of the large-size deformation-resistant nickel-based high-temperature alloy ingot is carried out according to the method in the embodiment 2, and the difference is that triple smelting adopts triple smelting process parameters in the embodiment 2 in a triple smelting process of the deformation-resistant nickel-based high-temperature alloy GH4151 with the application publication number of CN 111519068A.
Comparative example 1
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that a consumable ingot is obtained according to a duplex smelting process in CN105506390A to obtain a GH4742 alloy consumable ingot, and the homogenization treatment operation is as follows: heating the GH4742 alloy consumable ingot with the diameter of 660mm obtained by duplex smelting to 900 ℃, preserving heat for 4h, then heating to 1135 ℃ at the heating rate of 50 ℃/h, and preserving heat for 48 h.
Comparative example 2
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the example 2, and is characterized in that a consumable ingot is obtained according to a duplex smelting process in CN105506390A, and the homogenization treatment step is the same as that in the example 2.
Comparative example 3
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that the homogenization treatment step comprises the following operations: heating up GH4742 alloy consumable ingots with phi of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4 hours, then heating up to 1135 ℃ at the heating rate of 50 ℃/h, preserving heat for 48 hours, and cooling to obtain phi 660 nickel-based high-temperature alloy ingots difficult to deform.
Comparative example 4
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in a comparative example 3, and is characterized in that the homogenization treatment step is as follows: heating up GH4742 alloy consumable ingots with phi of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4h, then heating up to 1120 ℃ at the heating rate of 50 ℃/h, preserving heat for 48h, and cooling to obtain phi 660 nickel-based high-temperature alloy cast ingots difficult to deform.
Comparative example 5
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform is different from the method in a comparative example 3 in that the homogenization treatment step comprises the following steps of heating a GH4742 alloy consumable ingot with phi of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4 hours, then heating to 1150 ℃ at a heating rate of 50 ℃/h, preserving heat for 48 hours, and cooling to obtain the nickel-based high-temperature alloy ingot with phi of 660 difficult to deform.
Comparative example 6
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform is different from the method in a comparative example 3 in that the homogenization treatment step comprises the following steps of heating a GH4742 alloy consumable ingot with the diameter of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4 hours, then heating to 1180 ℃ at the heating rate of 50 ℃/h, preserving heat for 48 hours, and cooling to obtain the nickel-based high-temperature alloy ingot with the diameter of 660 mm.
Comparative example 7
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the comparative example 3, and is characterized in that the homogenization treatment step comprises the following operations: heating up GH4742 alloy consumable ingots with phi of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4h, then heating up to 1135 ℃ at the heating rate of 50 ℃/h, preserving heat for 72h, and cooling to obtain phi 660 nickel-based high-temperature alloy cast ingots difficult to deform.
Comparative example 8
A preparation method of a large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in a comparative example 3, and is characterized in that the homogenization treatment step is as follows: heating up GH4742 alloy consumable ingots with phi of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4 hours, then heating up to 1190 ℃ at the heating rate of 50 ℃/h, preserving heat for 100 hours, and cooling to obtain phi 660 nickel-based high-temperature alloy cast ingots difficult to deform.
Comparative example 9
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that the homogenization treatment step comprises the following operations: heating up a GH4742 alloy consumable ingot with the diameter of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4h, then heating up to 1120 ℃ at the heating rate of 52 ℃/h, and preserving heat for 12 h; heating to 1135 ℃ at the heating rate of 8 ℃/h, preserving heat for 48h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Comparative example 10
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that the homogenization treatment step comprises the following operations: heating up a GH4742 alloy consumable ingot with the diameter of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4 hours, then heating up to 1135 ℃ at the heating rate of 50 ℃/h, and preserving heat for 24 hours; heating to 1180 ℃ at the heating rate of 8 ℃/h, preserving heat for 64h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Comparative example 11
The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is carried out according to the method in the embodiment 2, and is characterized in that the homogenization treatment step comprises the following operations: heating up a GH4742 alloy consumable ingot with the diameter of 660mm obtained by triple smelting to 900 ℃, preserving heat for 4 hours, then heating up to 1100 ℃ at the heating rate of 40 ℃/h, and preserving heat for 12 hours; heating to 1150 ℃ at the heating rate of 15 ℃/h, preserving heat for 24h, heating to 1180 ℃ at the heating rate of 5 ℃/h, preserving heat for 64h, and cooling to obtain the phi 660 nickel-based high-temperature alloy cast ingot difficult to deform.
Performance detection
1. Crack performance detection
The triple smelting in examples 1-3 and the duplex smelting in comparative example 1 are respectively smelted for 10 furnaces according to the process, the cracking conditions of the electrode/consumable ingot are compared, and the comparison result is shown in the following table 1, wherein the cracking percentage refers to the percentage of the number of cracked electrodes or consumable ingots to the total number of steel ingots put into the process.
Table 1:
in the table, the higher the cracking percentage is, the more serious the cracking is, and as can be seen from table 1 above, the triple smelting process in the present application can be used to produce a consumable ingot with a specification of phi 660, and more importantly, the cracking phenomenon of the produced phi 660 consumable ingot is obviously improved, and the performance is greatly improved.
2. Segregation Performance testing
The detection of the cast structure morphology of the consumable ingot obtained after triple smelting in example 2 is shown in fig. 1, and the detection of the microstructure between dendrite trunk and dendrite is also performed on the consumable ingot, as shown in fig. 2, it can be seen from fig. 2 that the consumable ingot obtained after triple smelting still has segregation. And observing the structure and crystal phase of the ingot obtained in the example 2 after the triple smelting and the homogenization treatment in sequence, as shown in fig. 3, and by combining fig. 4 and fig. 5, the gamma' phase distribution diagram and the morphology distribution of carbides can be seen, and it can be seen that the component segregation and the structure segregation of the large-size phi 660 ingot obtained after the multi-stage homogenization treatment are obviously improved, the carbides are granular, and no melting or holes appear at the grain boundary.
In addition, microscopic structure observation is respectively carried out on the ingot obtained after the homogenization system of 1120 ℃ and 48h is adopted in the comparative example 4, the ingot obtained after the homogenization system of 1135 ℃ and 48h is adopted in the comparative example 3, the ingot obtained after the homogenization system of 1150 ℃ and 48h is adopted in the comparative example 5 and the ingot obtained after the homogenization system of 1180 ℃ and 48h is adopted in the comparative example 6, as shown in fig. 6, the phenomena of grain boundary and grain boundary holes appear when the homogenization treatment is carried out at the temperature of more than 1150 ℃, element segregation is still serious when the homogenization treatment is carried out at the temperature of less than 1135 ℃, and a large gamma' phase cannot be completely dissolved into a matrix, so that the aim of homogenization cannot be achieved.
Typical element segregation coefficients were measured and compared between the consumable ingot core part obtained by the triple smelting process in examples 1 to 3 and the consumable ingot core part obtained by the two-up process in comparative example 1, and the results are shown in table 2 below, where the element segregation coefficient is interdendritic element content ÷ dendrite dry element content.
TABLE 2 elemental segregation test for consumable ingots after smelting in examples 1-3 and comparative example 1
In the above table, the segregation coefficients of both Nb and Ti elements are greater than 1, and the larger the segregation coefficient is, the more the dendrite segregation of the element is heavy. As can be seen from the above table 2, the element segregation coefficient of the consumable ingot with the specification of phi 660 obtained by the triple smelting of the present application is obviously reduced, and the performance of the alloy ingot is obviously improved.
In addition, segregation coefficients of Nb elements were measured for ingots obtained in the above examples and comparative examples after triple smelting and homogenization treatment in this order, and the measurement results are shown in table 3 below.
TABLE 3 detection of Nb element segregation in ingot casting after smelting and homogenization treatment in examples and comparative examples
By combining the detection results of the embodiments 1-3 in the above table 2 and the above table 3, it can be seen that the triple smelting process provided in the present application is adopted, the obtained consumable ingot has lower dendrite segregation, and the dendrite segregation of the obtained cast ingot with the phi 660 specification is further significantly improved after the consumable ingot obtained by the triple smelting process is subjected to multi-stage homogenization treatment, and referring to the detection results in the embodiments 6-8, it can be seen that in the homogenization treatment step, the segregation phenomenon becomes weaker finally as the temperature rise rate of the temperature rise to 1120 ℃ is reduced; referring to the test data of examples 8 to 11, the segregation phenomenon of the obtained ingot becomes weaker as the temperature increase rate to 1135 ℃ is decreased; referring to the test data of examples 12-14, the segregation of the ingot decreases as the temperature rise rate decreases to 1180 ℃.
Referring to the detection data of comparative example 1, it can be seen that the segregation phenomenon is serious in the ingot obtained by the two-couple smelting process in the prior art and the single-stage homogenization treatment system at 1135 ℃ for 48 hours in the prior art, and referring to the detection data of comparative example 2, it can be seen that the segregation phenomenon is serious in the ingot obtained by the two-couple process in the prior art and the multi-stage homogenization treatment system provided by the present application, compared with the segregation phenomenon in the ingot obtained by the triple smelting process and the multi-stage homogenization treatment system in example 2, and referring to the detection data of comparative example 3, it can be seen that the segregation phenomenon in the ingot obtained by the triple smelting process and the single-stage homogenization treatment system at 1135 ℃ for 48 hours in the present application is serious in the ingot obtained by the triple smelting and the multi-stage homogenization treatment system in example 2.
Referring to the detection data in the comparative example 4, when the homogenization system is changed, the element segregation phenomenon is still serious by adopting the homogenization system at 1135 ℃; referring to the detection results of comparative examples 5 and 6, it can be seen that the element segregation phenomenon of the obtained ingot is still serious at the homogenization treatment of 1150 ℃ and above, and referring to the detection result of comparative example 7, it can be seen that on the basis of adopting the triple smelting process provided by the application, the treatment temperature is unchanged at the homogenization treatment temperature of 1135 ℃ in the prior art, the homogenization time is increased, and the obtained alloy ingot still has serious segregation; in comparative example 9, the homogenization temperature was continuously increased, and a homogenization treatment system of 1190 ℃ for 100 hours was adopted, so that the obtained ingot suffered from a severe scale peeling phenomenon due to the influence of oxidation.
Referring to the test of comparative example 9 and comparative example 10, it can be seen that the ingot still has segregation phenomenon by adopting the two-pole homogenization system of 1120 ℃, 12h, 1135 ℃, 48h or 1135 ℃, 24h, 1180 ℃ and 64 h. Referring to the test results of comparative example 11, it can be seen that the ingot segregation phenomenon obtained using the 1120 ℃/12h +1135 ℃/24h +1180 ℃/64h homogenization scheme provided herein is lower than that obtained using the three-stage homogenization scheme using other parameters.
The ingots obtained in example 2, comparative example 3 and comparative example 6 after the triple smelting and homogenization treatment were also subjected to the detection of segregation of other elements, and the detection results are shown in table 4 below.
Table 4:
| segregation of elements | Segregation of Al | Segregation of Cr | Segregation of Mo | Segregation of Ti |
| Example 2 | 0.041 | 0.017 | 0.014 | 0.041 |
| Comparative example 3 | 0.76 | 0.037 | 0.46 | 0.77 |
| Comparative example 6 | 0.39 | 0.18 | 0.22 | 0.42 |
3. Purity of smelting process
The sulfur content and the inclusion volume fraction of the consumable ingots obtained by triple smelting and the consumable ingots obtained by double smelting in examples 1-3 and comparative example 1 were respectively detected, and the purity of the double and triple smelting processes of the GH4742 alloy was compared, and the results are shown in table 5 below, where the inclusion volume fraction is the total volume of the inclusions divided by the volume of the statistical sample multiplied by 100%.
Table 5:
in the above table, the smaller the volume fraction of inclusions, the higher the purity. The lower the sulfur content, the higher the purity. As can be seen from the above table 5, the sulfur content of the triple phi 660mm ingot mold is obviously reduced and the impurities in the alloy ingot are obviously reduced in the smelting process of the triple phi 660mm consumable ingot.
Thermoplastic detection
The consumable ingot obtained by triple smelting in example 2 and the ingot after homogenization treatment were subjected to the high-temperature tensile property test at 1150 ℃ according to the standard GB/T228.2-2015 part 2 of the tensile test for metallic materials, namely the high-temperature test method, and the test results are shown in the following table 6.
Table 6:
as can be seen from the above table 6, the thermoplasticity of the alloy is greatly improved after the homogenization treatment of the triple-smelted consumable ingot.
In the process of preparing the large-size deformation-resistant nickel-base superalloy GH4742 alloy, the inventor finds out through optimized experiments that when the sum of the weight percentages (wt.%) of Al, Ti and Nb in the raw materials of the GH4742 alloy is in an optimal range of 7.20-8.40%, the cracking tendency of an electrode rod and a consumable ingot can be further reduced while the strength of the alloy is ensured. Further, for the large-size deformation-resistant nickel-based high-temperature alloy GH4742, the inventor finds out through optimized experiments that the sum of the weight percentages (wt.%) of Mo, Co and Cr in the raw materials of the GH4742 alloy is between 26.5 and 31.5 percent, and the oxidation resistance of a consumable ingot in a high-temperature homogenization process is improved.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The preparation method of the large-size nickel-based high-temperature alloy ingot difficult to deform is characterized by comprising the following steps of:
triple smelting: smelting a high-temperature alloy raw material by a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting to obtain a consumable ingot;
homogenizing: carrying out multi-stage homogenization treatment, and preserving the temperature of the consumable ingot at 830 ℃ -; then heating to 1115-1125 ℃, and preserving heat; heating to 1130-1140 deg.c and maintaining; heating to 1170-1190 deg.c, maintaining and cooling to obtain large scale hard-to-deform Ni-base high temperature alloy ingot.
2. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: in the homogenization treatment step, the temperature of the consumable ingot is raised to 1120 +/-10 ℃ and then is kept for 10-14 h;
heating the consumable ingot to 1135 +/-10 ℃, and then preserving heat for 22-26 h;
and heating the consumable ingot to 1180 +/-20 ℃, and then preserving the temperature for 62-66 h.
3. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: in the homogenization treatment step, the temperature rise rate of the temperature rise to 1120 +/-10 ℃ is (45-60) DEG C/h;
the heating rate of heating to 1135 +/-10 ℃ is (4-10) DEG C/h;
the heating rate of heating to 1180 +/-20 ℃ is 3-6 ℃.
4. The preparation method of the large-size difficult-deformation nickel-based superalloy ingot according to claim 1, wherein the preparation method comprises the following steps: the vacuum induction smelting in the triple smelting step comprises the following steps:
s1-1, smelting the high-temperature alloy raw material in a vacuum induction furnace, wherein the smelting in the vacuum induction furnace comprises full melting, refining and tapping, the full melting temperature is 1480-1580 ℃, and the vacuum degree of the full melting is 0-50 Pa; the refining temperature is 1500-;
s1-2, pouring in vacuum, pouring the molten steel into an ingot mold which is heated to 200 and 500 ℃ in advance to obtain a VIM electrode rod;
s1-3, transferring the obtained VIM electrode bar into an annealing furnace within 2 hours for stress relief annealing, wherein the annealing temperature is 800-1200 ℃, and the temperature is kept for more than 10 hours to obtain the annealed VIM electrode bar.
5. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: in the triple smelting step, the protective atmosphere electroslag remelting comprises the following steps:
s2-1, carrying out surface polishing treatment on the surface of the annealed VIM electrode bar obtained after vacuum induction melting operation, and then carrying out electrode welding to prepare for protective atmosphere electroslag remelting;
s2-2, selecting a slag system: the electroslag comprises the following components in percentage by weight: CaF2：36-60%；Al2O3: 13 to 30 percent; CaO: 12 to 35 percent; MgO: 1 to 15 percent; the balance being TiO2；
S2-3: selecting a crystallizer, introducing argon for protection, wherein the filling ratio of the VIM electrode bar to the crystallizer is 0.5-0.9, the whole argon flow is 30-120L/min, and performing the working procedures of slagging, arcing, remelting, feeding, cooling and demolding to obtain a P-ESR electrode bar;
s2-4, performing stress relief annealing on the obtained P-ESR electrode rod within 2 hours, wherein the annealing temperature is 800-1180 ℃, and preserving the heat for 18 hours to obtain the annealed P-ESR electrode rod.
6. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: in the triple smelting step, the vacuum consumable remelting comprises the following steps:
s3-1, performing polishing or grinding treatment on the surface of the annealed P-ESR electrode bar obtained by electroslag remelting in the protective atmosphere, processing until the two end faces are parallel, and then performing electrode welding;
s3-2, controlling the initial vacuum degree below 1.0Pa and the air leakage rate below 0.5 Pa/min;
s3-3, filling helium gas for cooling during smelting, and respectively performing the technical processes of an arc starting stage, a stabilizing stage, a feeding stage, cooling, breaking the air and demolding, wherein the control parameters of the technical process are set as follows: the control range of the melting speed is 2.8-5.0kg/min, the control range of the helium pressure is 1000Pa, the vacuum degree in the stable melting stage is less than or equal to 1.5Pa, and the control range of the cooling water temperature is 18-38 ℃, so that VAR consumable ingots are obtained;
s3-3, transferring the VAR consumable ingot to an annealing furnace for stress relief annealing within 1 hour, wherein the annealing temperature is 900-1200 ℃, and the temperature is kept for more than 12 hours.
7. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: the large-size nickel-based high-temperature alloy ingot difficult to deform is a GH4742 alloy ingot, and the high-temperature alloy raw material in the triple smelting step is a GH4742 alloy raw material.
8. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: in the raw materials of the GH4742 alloy, the sum of the weight percentages (wt.%) of Al, Ti and Nb is between 7.20 and 8.40 percent.
9. The preparation method of the large-size difficultly-deformed nickel-based superalloy ingot according to claim 1, wherein the method comprises the following steps: in the GH4742 alloy raw material, the sum of the weight percentages (wt.%) of Mo, Co and Cr is 26.5-31.5%.
10. A large-gauge hard-to-deform nickel-base superalloy ingot produced by the production method according to any one of claims 1 to 9.
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| CN115094360A (en) * | 2022-07-13 | 2022-09-23 | 北航（四川）西部国际创新港科技有限公司 | Heat treatment process of single crystal high temperature alloy with deformation and recrystallization resistant effects |
| CN115612949A (en) * | 2022-10-13 | 2023-01-17 | 大冶特殊钢有限公司 | Iron-nickel-based alloy large ingot blank with high titanium-aluminum content and smelting method thereof |
| CN115652235A (en) * | 2022-08-24 | 2023-01-31 | 北京钢研高纳科技股份有限公司 | GH4151 alloy fine-grain bar and preparation method and application thereof |
| CN115896506A (en) * | 2022-11-18 | 2023-04-04 | 陕西宝锐金属有限公司 | Preparation technology of low segregation GH3230 alloy high-quality slab |
| CN116855779A (en) * | 2023-07-28 | 2023-10-10 | 北京钢研高纳科技股份有限公司 | Preparation method of nickel-based alloy for high temperature and nickel-based alloy for high temperature |
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| CN115094360A (en) * | 2022-07-13 | 2022-09-23 | 北航（四川）西部国际创新港科技有限公司 | Heat treatment process of single crystal high temperature alloy with deformation and recrystallization resistant effects |
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| CN115652235A (en) * | 2022-08-24 | 2023-01-31 | 北京钢研高纳科技股份有限公司 | GH4151 alloy fine-grain bar and preparation method and application thereof |
| CN115652235B (en) * | 2022-08-24 | 2023-11-28 | 北京钢研高纳科技股份有限公司 | GH4151 alloy fine crystal bar and preparation method and application thereof |
| CN115612949A (en) * | 2022-10-13 | 2023-01-17 | 大冶特殊钢有限公司 | Iron-nickel-based alloy large ingot blank with high titanium-aluminum content and smelting method thereof |
| CN115612949B (en) * | 2022-10-13 | 2024-05-28 | 大冶特殊钢有限公司 | Large iron-nickel base alloy ingot blank with high titanium-aluminum content and smelting method thereof |
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