Control method of GH4169 nickel-based superalloy banded structure

Through triple smelting, multiple upsetting and homogenization treatment combined with hot rolling/modification technology, the problems of element segregation and stress corrosion of GH4169 nickel-based high-temperature alloy during processing are solved, and the stable control of GH4169 nickel-based high-temperature alloy is realized and Performance uniformity meets the application needs of the nuclear power field.

CN119082634APending Publication Date: 2024-12-06BAIMTEC MATERIAL CO LTD
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Patent Information

Application Number
CN202411239178.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-05
Publication Date
2024-12-06

AI Technical Summary

Technical Problem

GH4169 nickel-based high-temperature alloy has elemental segregation problems during processing, resulting in stress corrosion and cannot meet the strict requirements in the field of nuclear power. The existing technology is difficult to effectively control strip-like structure, affecting the stability and performance of the material.

Method used

The integrated processing and forming technology of triple smelting + homogenization + four upsetting + secondary uniformization + draw length + hot rolling/modification is adopted to reduce element segregation and control the generation of strip-like tissue through multiple deformation and heat treatment. Achieve stable control of small-size GH4169 nickel-based high-temperature alloy bar/plate structure.

Benefits of technology

It effectively reduces the generation of stress corrosion, ensures uniform performance of the alloy, meets the requirements of the stable control of the strip-like structure of GH4169 nickel-based high-temperature alloy in the nuclear power field, and the carbide and δ phases are distributed uniformly, avoiding stress concentration.

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Abstract

The invention discloses a control method for a strip-shaped structure of a GH4169 nickel-based superalloy. The control method comprises the following steps that a GH4169 nickel-based superalloy cast ingot is prepared, and first homogenization treatment is conducted on the GH4169 nickel-based superalloy cast ingot; the GH4169 nickel-based superalloy cast ingot is transferred to a press machine to be subjected to first upsetting and drawing to obtain a bar blank, and first annealing treatment is carried out; the bar billet is transferred to the press machine to be subjected to second upsetting and drawing to further obtain the bar billet, and second annealing treatment is carried out; the bar billet is transferred to the press machine to be subjected to third upsetting and drawing to further obtain the bar billet, and third annealing treatment is carried out; the bar billet is transferred to the press machine to be subjected to fourth upsetting and drawing to further obtain the bar billet, and second homogenization treatment is carried out; the bar billet is transferred to a press machine to be drawn out, and the drawn-out bar billet is subjected to fourth-time annealing treatment; and forging or hot rolling is carried out according to requirements, and the strip-shaped structure controllable plate or bar is obtained. According to the method, segregation can be reduced to the maximum extent, and generation of banded structures is controlled.
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Description

Technical Field

[0001] The invention belongs to the technical field of nickel-based high-temperature alloy material processing, and in particular relates to a method for controlling a strip-shaped structure of a GH4169 nickel-based high-temperature alloy. Background Art

[0002] As we all know, GH4169 nickel-based high-temperature alloy has high tensile strength and durability, good corrosion resistance, high-temperature oxidation resistance, hot workability and welding performance, and has been widely used in important structural materials in aerospace and other fields. In the field of nuclear power, higher requirements are put forward for the technical parameters of nuclear power equipment. The types of products using GH4169 nickel-based high-temperature alloy in different parts of the nuclear island are different. For example, the nuclear reactor fuel positioning grid uses strips with a thickness of about 0.3mm, nuclear equipment welding materials or drive rod spring wires use wires and round rods with a diameter of 0.3-10mm, and the compression springs in the fuel rods of the fuel assembly and the springs of related components use wires. The materials used above have high production process requirements for each processing procedure.

[0003] The banded structure in the GH4169 nickel-based high-temperature alloy will have an adverse effect on the stress corrosion of the material, which will cause equipment damage due to stress corrosion of the material during the operation phase of the nuclear power plant. Therefore, it is of great practical significance to prepare the GH4169 nickel-based high-temperature alloy with qualified banded structure.

[0004] With the enhancement of material processing equipment capabilities, nickel-based superalloys are developing in the direction of large-scale production. However, the increase in specifications will inevitably lead to an increase in the degree of segregation. Even if cooling is increased during the preparation process, due to the limited heat dissipation of the nickel-based superalloy itself, excessive size will also lead to corresponding segregation. The elements in the GH4169 nickel-based superalloy are severely segregated, and the current preparation method cannot meet the requirements of harsh environments such as nuclear power. Therefore, it is urgent to develop a control method for the banded structure of the GH4169 nickel-based superalloy to minimize segregation while enabling large-scale industrial production.

[0005] The invention patent with application publication number CN114799000A discloses a method for preparing a small-size diameter forged bar of GH4169 alloy, which includes the following steps: obtaining a GH4169 alloy ingot by a triple smelting process of VIM+ESR+VAR; subjecting the obtained GH4169 alloy ingot to high-temperature homogenization treatment; processing the ingot by an 80MN fast forging machine to obtain the required fast forging blank bar; and performing diameter forging by a 1800t large precision forging machine to obtain a GH4169 alloy bar with a size of Φ100-150mm. This technical solution does not control the specifications of the ingot, nor does it take measures to reduce segregation. Summary of the invention

[0006] In order to solve the problems existing in the prior art, the present invention provides a method for controlling the strip-shaped structure of GH4169 nickel-based high-temperature alloy, and the control method comprises the following steps in chronological order:

[0007] Step 1: Prepare a cylindrical GH4169 nickel-based high-temperature alloy ingot according to design requirements;

[0008] Step 2: placing the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace for the first homogenization treatment;

[0009] Step 3: After the first homogenization treatment is completed, the cylindrical GH4169 nickel-based high-temperature alloy ingot is transferred to a press for the first upsetting and drawing to obtain a bar blank, and the bar blank obtained by the first upsetting is placed in a heat treatment furnace for the first annealing treatment;

[0010] Step 4: After the first annealing treatment is completed, the rod blank is transferred to a press for a second upsetting and further obtained as a rod blank, and the rod blank obtained by the second upsetting is placed in a heat treatment furnace for a second annealing treatment;

[0011] Step 5: After the second annealing treatment is completed, the rod blank is transferred to a press for a third upsetting and further obtained as a rod blank, and the rod blank obtained by the third upsetting is placed in a heat treatment furnace for a third annealing treatment;

[0012] Step 6: After the third annealing treatment is completed, the rod blank is transferred to a press for a fourth upsetting and further obtained as a rod blank, and the rod blank obtained by the fourth upsetting is placed in a heat treatment furnace for a second homogenization treatment;

[0013] Step 7: After the second homogenization treatment is completed, the rod blank is transferred to a press for drawing. After the drawing is completed, a deformed GH4169 nickel-based high-temperature alloy rod blank can be obtained. The drawn rod blank is placed in a heat treatment furnace for the fourth annealing treatment;

[0014] Step 8: After the fourth annealing treatment is completed, small-sized billets are cut according to demand and transferred to an electro-hydraulic hammer or a hot rolling mill for reforging or hot rolling. After the reforging or hot rolling is completed, a GH4169 nickel-based high-temperature alloy plate or GH4169 nickel-based high-temperature alloy bar with controllable strip-shaped structure can be obtained.

[0015] Preferably, in step 1, the chemical composition of the cylindrical GH4169 nickel-based high-temperature alloy ingot includes Ni 50.0-55.0%, Cr 17.0-21.0%, Nb+Ta 4.75-5.5%, Mo 2.8-3.3%, Ti0.65-1.15%, Al 0.2-0.8%, Co≤0.04%, C 0.02-0.08%, the balance is Fe; the cylindrical GH4169 nickel-based high-temperature alloy ingot is prepared by triple smelting, namely, vacuum induction melting process, protective atmosphere electroslag remelting process and vacuum consumable remelting process; the key parameters of the vacuum induction melting process are that the vacuum pressure of chemical cleaning does not exceed 30Pa, the vacuum pressure of the refining stage does not exceed 10Pa, and the pouring temperature is 1500-1550℃; the key parameters of the protective atmosphere electroslag remelting process are that the melting speed is not higher than 4.5kg / min, the argon flow rate is not lower than 5L / min, and the shrinkage feeding weight is not less than 85kg; the key parameters of the vacuum consumable remelting process are that the melting speed is not higher than 4.5kg / min, the helium pressure does not exceed 600Pa, the shrinkage feeding weight is not less than 85kg, and the diameter of the consumable ingot does not exceed 410mm.

[0016] In any of the above schemes, preferably, in step 2, the process system of the first homogenization treatment is to place the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace, heat it from room temperature to 800°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 800°C to 1000°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 1000°C to 1000°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; ℃ to 1130℃, keep warm for 5-7h; continue to increase the temperature from 1130℃ to 1160℃ at a rate of 5-10℃ / min, and keep warm for 25-30h; continue to increase the temperature from 1160℃ to 1200℃ at a rate of 5-10℃ / min, and keep warm for 72-80h; continue to decrease the temperature from 1200℃ to 1150℃ at a rate of 5-10℃ / min, and keep warm for 4-6h; no protective atmosphere is required during the first homogenization treatment.

[0017] In any of the above schemes, it is preferred that in step 3, after the first homogenization treatment is completed, the cylindrical GH4169 nickel-based high-temperature alloy ingot is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the first upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy billet vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the billet, and the deformation amount is 20-40%, and then the upset GH4169 nickel-based high-temperature alloy billet is placed horizontally on the platform of the press, and the pressure head of the press starts from one end of the billet. The first drawing is performed from one end to the other end. After the first drawing is completed, the rod blank is axially rotated 60°, and the ram of the press continues to draw the rod blank from one end to the other end for the second drawing. After the second drawing is completed, the rod blank is axially rotated 60°, and the ram of the press continues to draw the rod blank from one end to the other end for the third drawing, and so on, until the rod blank is drawn to the length before the first upsetting and drawing begins, that is, the first upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent drawing passes is 1-4%. After the last drawing pass, the temperature of the rod blank is not lower than 900℃.

[0018] The process system of the first annealing treatment is as follows: annealing temperature is 1100-1150° C., annealing time is 2-4 hours, and no protective atmosphere is required during the first annealing treatment.

[0019] In any of the above schemes, it is preferred that in step 4, after the first annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the second upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30-50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press is pressed from one end of the bar blank to the bottom of the bar blank. The first drawing is carried out at the other end. After the first drawing is completed, the rod blank is axially rotated 60°, and the ram of the press continues to draw the rod blank from one end to the other end for the second drawing. After the second drawing is completed, the rod blank is axially rotated 60°, and the ram of the press continues to draw the rod blank from one end to the other end for the third drawing, and so on, until the rod blank is drawn to the length before the second upsetting and drawing begins, that is, the second upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent drawing passes is 1-4%. After the last drawing pass, the temperature of the rod blank is not less than 900℃.

[0020] The process system of the second annealing treatment is as follows: annealing temperature is 1100-1150° C., annealing time is 2-4 hours, and no protective atmosphere is required during the second annealing treatment.

[0021] In any of the above schemes, it is preferred that in step 5, after the second annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the third upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30-50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press is pressed from one end of the bar blank to the bottom of the bar blank. The first drawing is carried out at the other end. After the first drawing is completed, the rod blank is axially rotated 60°, and the ram of the press continues to draw the rod blank from one end to the other end for the second drawing. After the second drawing is completed, the rod blank is axially rotated 60°, and the ram of the press continues to draw the rod blank from one end to the other end for the third drawing, and so on, until the rod blank is drawn to the length before the third upsetting and drawing begins, that is, the third upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent drawing passes is 1-4%. After the last drawing pass, the temperature of the rod blank is not less than 900℃.

[0022] The process system of the third annealing treatment is as follows: annealing temperature is 1100-1150° C., annealing time is 2-4 hours, and no protective atmosphere is required during the third annealing treatment.

[0023] In any of the above schemes, it is preferred that in step 6, after the third annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the fourth upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30-50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press is pressed from one end of the bar blank to the bottom of the bar blank. The first drawing is carried out at the other end. After the first drawing is completed, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to draw the rod blank from one end to the other end for the second drawing. After the second drawing is completed, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to draw the rod blank from one end to the other end for the third drawing, and so on, until the rod blank is drawn to the length before the fourth upsetting and drawing begins, that is, the fourth upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent drawing passes is 1-4%. After the last drawing pass, the temperature of the rod blank is not less than 900℃.

[0024] In any of the above schemes, preferably, in step six, the process system of the second homogenization treatment is to place the GH4169 nickel-based high-temperature alloy billet into a heat treatment furnace, heat it from room temperature to 800°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 800°C to 1000°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 1000°C to 1000°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; ℃ to 1130℃, keep warm for 5-7h; continue to increase the temperature from 1130℃ to 1160℃ at a rate of 5-10℃ / min, keep warm for 5-7h; continue to increase the temperature from 1160℃ to 1200℃ at a rate of 5-10℃ / min, keep warm for 40-50h; continue to decrease the temperature from 1200℃ to 1150℃ at a rate of 5-10℃ / min, keep warm for 4-6h; no protective atmosphere is required during the second homogenization treatment.

[0025] In any of the above schemes, preferably, in step seven, after the second homogenization treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the drawing is that the GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first drawing from one end of the bar blank to the other end. After the first drawing is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to draw the bar blank from one end to the other end for a second time. After the second drawing is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to draw the bar blank from one end to the other end for a third time, and so on, until the specified size is reached, that is, the drawing is completed and the bar blank is obtained, the deformation of the adjacent two drawing passes is 1-4%, and after the last drawing pass, the temperature of the bar blank is not less than 900°C.

[0026] The process system of the fourth annealing treatment is as follows: annealing temperature is 1120-1170° C., annealing time is 2-4 hours, and no protective atmosphere is required during the fourth annealing treatment.

[0027] In any of the above schemes, it is preferred that in step eight, after the fourth annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to an electro-hydraulic hammer or a hot rolling mill within 3 minutes; it is prepared into a plate by a forging method, with a width of 50-200 mm, a thickness of 40-60 mm, and a deformation of 20-60%; it is prepared into a rod by a hot rolling method, with a diameter of 12-55 mm and a deformation of 30-95%.

[0028] In step one, the triple smelting method is used to prepare the GH4169 nickel-based high-temperature alloy ingot, which can reduce the element segregation to the greatest extent during the ingot preparation process. In step two, the GH4169 nickel-based high-temperature alloy ingot is homogenized, which can dissolve the precipitated phase, reduce segregation, and facilitate the ingot opening. In steps three to six, the GH4169 nickel-based high-temperature alloy ingot is continuously upset and drawn four times, and the structure is made more uniform through multiple deformations. In step six, the GH4169 nickel-based high-temperature alloy bar billet is homogenized to further diffuse the elements, further reduce segregation, and facilitate uniform distribution of elements. In step seven, the GH4169 nickel-based high-temperature alloy bar billet is stretched, and a fine grain structure is obtained through large deformation deformation.

[0029] The method for controlling the banded structure of the GH4169 nickel-based high-temperature alloy of the present invention adopts the integrated processing and forming technology of triple melting + homogenization + four upsetting and four drawing + secondary homogenization + drawing + hot rolling / forging to reduce segregation to the greatest extent, thereby controlling the generation of banded structure, and realizing stable control of the structure of small-sized GH4169 nickel-based high-temperature alloy bars / plates. The formed alloy can meet the stringent requirements of the nuclear power field for stable control of the banded structure in the alloy.

[0030] The carbide morphology in the rod / plate prepared by the method of the present invention meets the requirements of level 1 of the Class B purity rating diagram in GB / T 14999.5-1994, the carbides are small and evenly distributed, and no stress concentration is generated. The δ phase is detected according to the GB / T 14999.4-2012 detection method, and the δ phase morphology is evenly distributed, which is conducive to the uniform control of the grain size in the subsequent deformation, thereby ensuring the uniform performance of the alloy, reducing the generation of stress concentration, and meeting the requirements of the nuclear power field for the stable control of the banded structure of the GH4169 nickel-based high-temperature alloy. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a flow chart of a preferred embodiment of the method for controlling the strip-shaped structure of GH4169 nickel-based high-temperature alloy according to the present invention;

[0032] Figure 2 for Figure 1 A macroscopic photograph of a GH4169 nickel-based high-temperature alloy rod prepared in the embodiment shown;

[0033] Figure 3 for Figure 1 The carbide microstructure photograph of the GH4169 nickel-based high-temperature alloy rod prepared in the embodiment shown;

[0034] Figure 4 for Figure 1 The δ phase microstructure photograph of the GH4169 nickel-based high-temperature alloy rod prepared in the embodiment shown;

[0035] Figure 5 A photo of the carbide microstructure of a GH4169 nickel-based high-temperature alloy rod prepared according to another preferred embodiment of the method for controlling the strip-shaped structure of the GH4169 nickel-based high-temperature alloy of the present invention;

[0036] Figure 6 for Figure 5 The δ phase microstructure photograph of the GH4169 nickel-based high-temperature alloy rod prepared in the embodiment shown;

[0037] Figure 7 A photo of the carbide microstructure of a GH4169 nickel-based high-temperature alloy plate prepared according to another preferred embodiment of the method for controlling the strip-shaped structure of the GH4169 nickel-based high-temperature alloy of the present invention;

[0038] Figure 8 for Figure 7 The δ phase microstructure photograph of the GH4169 nickel-based high-temperature alloy plate prepared in the embodiment shown. DETAILED DESCRIPTION

[0039] In order to further understand the content of the present invention, the present invention will be described in detail below in conjunction with specific embodiments.

[0040] Embodiment 1:

[0041] like Figure 1 As shown, according to a preferred embodiment of the method for controlling the strip-shaped structure of GH4169 nickel-based high-temperature alloy of the present invention, the control method comprises the following steps in chronological order:

[0042] Step 1: Prepare a cylindrical GH4169 nickel-based high-temperature alloy ingot according to design requirements;

[0043] Step 2: placing the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace for the first homogenization treatment;

[0044] Step 3: After the first homogenization treatment is completed, the cylindrical GH4169 nickel-based high-temperature alloy ingot is transferred to a press for the first upsetting and drawing to obtain a bar blank, and the bar blank obtained by the first upsetting is placed in a heat treatment furnace for the first annealing treatment;

[0045] Step 4: After the first annealing treatment is completed, the rod blank is transferred to a press for a second upsetting and further obtained as a rod blank, and the rod blank obtained by the second upsetting is placed in a heat treatment furnace for a second annealing treatment;

[0046] Step 5: After the second annealing treatment is completed, the rod blank is transferred to a press for a third upsetting and further obtained as a rod blank, and the rod blank obtained by the third upsetting is placed in a heat treatment furnace for a third annealing treatment;

[0047] Step 6: After the third annealing treatment is completed, the rod blank is transferred to a press for a fourth upsetting and further obtained as a rod blank, and the rod blank obtained by the fourth upsetting is placed in a heat treatment furnace for a second homogenization treatment;

[0048] Step 7: After the second homogenization treatment is completed, the rod blank is transferred to a press for drawing. After the drawing is completed, a deformed GH4169 nickel-based high-temperature alloy rod blank can be obtained. The drawn rod blank is placed in a heat treatment furnace for the fourth annealing treatment;

[0049] Step 8: After the fourth annealing treatment is completed, small-sized billets are cut according to demand and transferred to an electro-hydraulic hammer or a hot rolling mill for reforging or hot rolling. After the reforging or hot rolling is completed, a GH4169 nickel-based high-temperature alloy plate or GH4169 nickel-based high-temperature alloy bar with controllable strip-shaped structure can be obtained.

[0050] In step 1, the chemical composition of the cylindrical GH4169 nickel-based high-temperature alloy ingot includes Ni 52.0%, Cr 19.0%, Nb+Ta 5.1%, Mo 3.1%, Ti 0.9%, Al 0.5%, Co 0.04%, C 0.05%, the balance is Fe; the cylindrical GH4169 nickel-based high-temperature alloy ingot is prepared by triple smelting, namely vacuum induction melting process, protective atmosphere electroslag remelting process and vacuum consumable remelting process; the key parameters of the vacuum induction melting process are that the vacuum pressure of chemical cleaning is 30Pa, the vacuum pressure of the refining stage is 10Pa, and the pouring temperature is 1525℃; the key parameters of the protective atmosphere electroslag remelting process are that the melting speed is 4.5kg / min, the argon flow rate is 5L / min, and the shrinkage feeding weight is 85kg; the key parameters of the vacuum consumable remelting process are that the melting speed is 4.5kg / min, the helium pressure is 600Pa, the shrinkage feeding weight is 85kg, and the diameter of the consumable ingot is 410mm.

[0051] In step 2, the process system for the first homogenization treatment is to place the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace, and heat it from room temperature to 800°C at a heating rate of 8°C / min, and keep it warm for 3 hours; continue to heat it from 800°C to 1000°C at a heating rate of 8°C / min, and keep it warm for 3 hours; continue to heat it from 1000°C to 1130°C at a heating rate of 8°C / min, and keep it warm for 6 hours; continue to heat it from 1130°C to 1160°C at a heating rate of 8°C / min, and keep it warm for 28 hours; continue to heat it from 1160°C to 1200°C at a heating rate of 8°C / min, and keep it warm for 76 hours; continue to cool it from 1200°C to 1150°C at a cooling rate of 8°C / min, and keep it warm for 5 hours; no protective atmosphere is required during the first homogenization treatment.

[0052] In step 3, after the first homogenization treatment is completed, the cylindrical GH4169 nickel-based high-temperature alloy ingot is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the first upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first upsetting from one end of the bar blank to the other end. After the first stretching, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the first upsetting and drawing, that is, the first upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching is 2.5%. After the last stretching, the temperature of the rod blank is not less than 900℃.

[0053] The process system of the first annealing treatment is as follows: annealing temperature is 1125° C., annealing time is 3 hours, and no protective atmosphere is required during the first annealing treatment.

[0054] In step 4, after the first annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the second upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 40%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first pass from one end of the bar blank to the other end. After the first stretching is completed, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching is completed, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the second upsetting and drawing begins, that is, the second upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching times is 2.5%. After the last stretching is completed, the temperature of the rod blank is not less than 900℃.

[0055] The process system of the second annealing treatment is as follows: annealing temperature is 1125° C., annealing time is 3 hours, and no protective atmosphere is required during the second annealing treatment.

[0056] In step 5, after the second annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the third upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 40%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first pass from one end of the bar blank to the other end. After the first stretching is completed, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching is completed, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the third upsetting and drawing begins, that is, the third upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching times is 2.5%. After the last stretching is completed, the temperature of the rod blank is not less than 900℃.

[0057] The process system of the third annealing treatment is as follows: annealing temperature is 1125° C., annealing time is 3 hours, and no protective atmosphere is required during the third annealing treatment.

[0058] In step 6, after the third annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the fourth upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 40%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first pass from one end of the bar blank to the other end. After the first stretching is completed, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching is completed, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the fourth upsetting and drawing begins, that is, the fourth upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching times is 2.5%. After the last stretching is completed, the temperature of the rod blank is not less than 900℃.

[0059] In step six, the process system of the second homogenization treatment is to place the GH4169 nickel-based high-temperature alloy rod billet into a heat treatment furnace, and heat it from room temperature to 800°C at a heating rate of 8°C / min, and keep it warm for 3 hours; continue to heat it from 800°C to 1000°C at a heating rate of 8°C / min, and keep it warm for 3 hours; continue to heat it from 1000°C to 1130°C at a heating rate of 8°C / min, and keep it warm for 6 hours; continue to heat it from 1130°C to 1160°C at a heating rate of 8°C / min, and keep it warm for 6 hours; continue to heat it from 1160°C to 1200°C at a heating rate of 8°C / min, and keep it warm for 45 hours; continue to cool it from 1200°C to 1150°C at a cooling rate of 8°C / min, and keep it warm for 5 hours; no protective atmosphere is required during the second homogenization treatment.

[0060] In step seven, after the second homogenization treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the drawing is that the GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first drawing from one end of the bar blank to the other end. After the first drawing is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for a second time. After the second drawing is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for a third time, and so on, until the specified size is reached, that is, the drawing is completed and the bar blank is obtained, the deformation of the adjacent two drawing passes is 2.5%, and after the last drawing pass, the temperature of the bar blank is not less than 900°C.

[0061] The process system of the fourth annealing treatment is as follows: annealing temperature is 1145° C., annealing time is 3 hours, and no protective atmosphere is required during the fourth annealing treatment.

[0062] In step eight, after the fourth annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a hot rolling mill within 3 minutes, and is prepared into a bar with a diameter of 30 mm by hot rolling.

[0063] In step one, the triple smelting method is used to prepare the GH4169 nickel-based high-temperature alloy ingot, which can reduce the element segregation to the greatest extent during the ingot preparation process. In step two, the GH4169 nickel-based high-temperature alloy ingot is homogenized, which can dissolve the precipitated phase, reduce segregation, and facilitate the ingot opening. In steps three to six, the GH4169 nickel-based high-temperature alloy ingot is continuously upset and drawn four times, and the structure is made more uniform through multiple deformations. In step six, the GH4169 nickel-based high-temperature alloy bar billet is homogenized to further diffuse the elements, further reduce segregation, and facilitate uniform distribution of elements. In step seven, the GH4169 nickel-based high-temperature alloy bar billet is stretched, and a fine grain structure is obtained through large deformation deformation.

[0064] The rods prepared by the method of this embodiment are as follows Figure 2 As shown in the figure, the carbide morphology in the rod meets the requirements of Class 1 of the Class B purity rating chart in GB / T14999.5-1994. The carbides are small and evenly distributed, and no stress concentration will occur. The microstructure of the carbide is as follows Figure 3 As shown. According to the GB / T 14999.4-2012 test method, the δ phase is tested. The microstructure of the δ phase is as follows Figure 4 As shown in the figure, the δ phase is evenly distributed, which is beneficial to the uniform control of grain size in subsequent deformation, ensuring the uniform performance of the alloy, reducing stress concentration, and meeting the requirements of the nuclear power field for stable control of the banded structure of the GH4169 nickel-based high-temperature alloy.

[0065] The method for controlling the banded structure of the GH4169 nickel-based high-temperature alloy of the present embodiment adopts the integrated processing and forming technology of triple melting + homogenization + four upsetting and four drawing + secondary homogenization + drawing + hot rolling / reforging to minimize segregation and control the generation of banded structure, thereby achieving stable control of the structure of small-sized GH4169 nickel-based high-temperature alloy bars. The formed alloy can meet the stringent requirements of the nuclear power field for stable control of the banded structure in the alloy.

[0066] Embodiment 2:

[0067] According to another preferred embodiment of the method for controlling the strip-shaped structure of GH4169 nickel-based high-temperature alloy of the present invention, its process flow, technical principle, beneficial effects, etc. are basically the same as those of the first embodiment, except that:

[0068] In step 1, the chemical composition of the cylindrical GH4169 nickel-based high-temperature alloy ingot includes Ni50.0%, Cr 17.0%, Nb+Ta 4.75%, Mo 2.8%, Ti 0.65%, Al 0.2%, Co 0.04%, C0.02%, and the balance is Fe. The key parameters of the vacuum induction melting process are: the vacuum pressure of the chemical cleaning is 30Pa, the vacuum pressure of the refining stage is 10Pa, and the pouring temperature is 1500℃; the key parameters of the protective atmosphere electroslag remelting process are: the melting speed is 4.5kg / min, the argon flow rate is 5L / min, and the shrinkage weight is 85kg; the key parameters of the vacuum consumable remelting process are: the melting speed is 4.5kg / min, the helium pressure is 600Pa, the shrinkage weight is 85kg, and the diameter of the consumable ingot is 410mm.

[0069] In step 2, the process system for the first homogenization treatment is to place the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace, and heat it from room temperature to 800°C at a heating rate of 5°C / min, and keep it warm for 2h; continue to heat it from 800°C to 1000°C at a heating rate of 5°C / min, and keep it warm for 2h; continue to heat it from 1000°C to 1130°C at a heating rate of 5°C / min, and keep it warm for 5h; continue to heat it from 1130°C to 1160°C at a heating rate of 5°C / min, and keep it warm for 25h; continue to heat it from 1160°C to 1200°C at a heating rate of 5°C / min, and keep it warm for 72h; continue to cool it from 1200°C to 1150°C at a cooling rate of 5°C / min, and keep it warm for 4h; no protective atmosphere is required during the first homogenization treatment.

[0070] In step three, the process system of the first upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 20%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the first upsetting begins, that is, the first upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretching times is 1%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C. The process system of the first annealing treatment is as follows: annealing temperature is 1100° C., annealing time is 4 hours, and no protective atmosphere is required during the first annealing treatment.

[0071] In step 4, the process system of the second upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 30%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the second upsetting begins, that is, the second upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretching times is 1%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C. The process system of the second annealing treatment is as follows: annealing temperature is 1100° C., annealing time is 4 hours, and no protective atmosphere is required during the second annealing treatment.

[0072] In step 5, the process system of the third upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 30%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the third upsetting begins, that is, the third upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretchings is 1%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C. The process system of the third annealing treatment is as follows: annealing temperature is 1100° C., annealing time is 4 hours, and no protective atmosphere is required during the third annealing treatment.

[0073] In step six, the process system of the fourth upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 30%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the fourth upsetting begins, that is, the fourth upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretching times is 1%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C.

[0074] The process system of the second homogenization treatment is as follows: placing the GH4169 nickel-based high-temperature alloy rod billet into a heat treatment furnace, heating the temperature from room temperature to 800°C at a heating rate of 5°C / min, and keeping it warm for 2 hours; continuing to heating the temperature from 800°C to 1000°C at a heating rate of 5°C / min, and keeping it warm for 2 hours; continuing to heating the temperature from 1000°C to 1130°C at a heating rate of 5°C / min, and keeping it warm for 5 hours; continuing to heating the temperature from 1130°C to 1160°C at a heating rate of 5°C / min, and keeping it warm for 5 hours; continuing to heating the temperature from 1160°C to 1200°C at a heating rate of 5°C / min, and keeping it warm for 40 hours; continuing to cooling the temperature from 1200°C to 1150°C at a cooling rate of 5°C / min, and keeping it warm for 4 hours; no protective atmosphere is required during the second homogenization treatment.

[0075] In step seven, the process of drawing is to place the GH4169 nickel-based high-temperature alloy bar blank horizontally on the platform of the press, and the pressure head of the press performs the first drawing from one end of the bar blank to the other end. After the first drawing is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for the second time. After the second drawing is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for the third time, and so on, until the specified size is reached, that is, the drawing is completed and the bar blank is obtained, and the deformation of the adjacent two drawing times is 1%. After the last drawing is completed, the temperature of the bar blank is not less than 900°C. The process of the fourth annealing treatment is that the annealing temperature is 1120°C, the annealing time is 4h, and no protective atmosphere is required during the fourth annealing treatment.

[0076] In step eight, after the fourth annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a hot rolling mill within 3 minutes to be prepared into a bar with a diameter of 40 mm by hot rolling.

[0077] The carbide microstructure of the rod prepared by the method of this embodiment is as follows: Figure 5 As shown in Figure 1, the carbides are small and evenly distributed, and no stress concentration will occur. The microstructure of the δ phase is shown in Figure 1. Figure 6 As shown, the δ phase has a uniform distribution in morphology, which is beneficial to the uniform control of grain size in subsequent deformation, ensuring uniform properties of the alloy and reducing stress concentration.

[0078] Embodiment three:

[0079] According to another preferred embodiment of the method for controlling the strip-shaped structure of GH4169 nickel-based high-temperature alloy of the present invention, its process flow, technical principle, beneficial effects, etc. are basically the same as those of the first embodiment, except that:

[0080] In step 1, the chemical composition of the cylindrical GH4169 nickel-based high-temperature alloy ingot includes Ni55.0%, Cr 21.0%, Nb+Ta 5.5%, Mo 3.3%, Ti 1.15%, Al 0.8%, Co 0.04%, C0.08%, and the balance is Fe. The key parameters of the vacuum induction melting process are: the vacuum pressure of the chemical cleaning is 30Pa, the vacuum pressure of the refining stage is 10Pa, and the pouring temperature is 1550℃; the key parameters of the protective atmosphere electroslag remelting process are: the melting speed is 4.5kg / min, the argon flow rate is 5L / min, and the shrinkage weight is 85kg; the key parameters of the vacuum consumable remelting process are: the melting speed is 4.5kg / min, the helium pressure is 600Pa, the shrinkage weight is 85kg, and the diameter of the consumable ingot is 410mm.

[0081] In step 2, the process system for the first homogenization treatment is to place the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace, and heat it from room temperature to 800°C at a heating rate of 10°C / min, and keep it warm for 4 hours; continue to heat it from 800°C to 1000°C at a heating rate of 10°C / min, and keep it warm for 4 hours; continue to heat it from 1000°C to 1130°C at a heating rate of 10°C / min, and keep it warm for 7 hours; continue to heat it from 1130°C to 1160°C at a heating rate of 10°C / min, and keep it warm for 30 hours; continue to heat it from 1160°C to 1200°C at a heating rate of 10°C / min, and keep it warm for 80 hours; continue to cool it from 1200°C to 1150°C at a cooling rate of 10°C / min, and keep it warm for 6 hours; no protective atmosphere is required during the first homogenization treatment.

[0082] In step three, the process system of the first upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 40%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the first upsetting begins, that is, the first upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretching times is 4%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C. The process system of the first annealing treatment is as follows: annealing temperature is 1150° C., annealing time is 2 hours, and no protective atmosphere is required during the first annealing treatment.

[0083] In step 4, the process system of the second upsetting and drawing is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass drawing from one end of the bar blank to the other end. After the first drawing is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for a second time. After the second drawing is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for a third time, and so on, until the bar blank is drawn to the length before the second upsetting and drawing begins, that is, the second upsetting and drawing is completed and the bar blank is obtained, and the deformation of the two adjacent drawing passes is 4%, and after the last drawing pass, the temperature of the bar blank is not less than 900°C. The process system of the second annealing treatment is as follows: annealing temperature is 1150° C., annealing time is 2 hours, and no protective atmosphere is required during the second annealing treatment.

[0084] In step 5, the process system of the third upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the third upsetting begins, that is, the third upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretchings is 4%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C. The process system of the third annealing treatment is as follows: annealing temperature is 1150° C., annealing time is 2 hours, and no protective atmosphere is required during the third annealing treatment.

[0085] In step six, the process system of the fourth upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, with a deformation of 50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs a first-pass stretching from one end of the bar blank to the other end. After the first stretching is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a second time. After the second stretching is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to stretch from one end of the bar blank to the other end for a third time, and so on, until the bar blank is stretched to the length before the fourth upsetting begins, that is, the fourth upsetting is completed and the bar blank is obtained, and the deformation of the two adjacent stretching times is 4%. After the last stretching is completed, the temperature of the bar blank is not less than 900°C.

[0086] The process system of the second homogenization treatment is as follows: placing the GH4169 nickel-based high-temperature alloy rod billet into a heat treatment furnace, heating the temperature from room temperature to 800°C at a heating rate of 10°C / min, and keeping it warm for 4 hours; continuing to heating the temperature from 800°C to 1000°C at a heating rate of 10°C / min, and keeping it warm for 4 hours; continuing to heating the temperature from 1000°C to 1130°C at a heating rate of 10°C / min, and keeping it warm for 7 hours; continuing to heating the temperature from 1130°C to 1160°C at a heating rate of 10°C / min, and keeping it warm for 7 hours; continuing to heating the temperature from 1160°C to 1200°C at a heating rate of 10°C / min, and keeping it warm for 50 hours; continuing to cooling the temperature from 1200°C to 1150°C at a cooling rate of 10°C / min, and keeping it warm for 6 hours; no protective atmosphere is required during the second homogenization treatment.

[0087] In step seven, the process of drawing is to place the GH4169 nickel-based high-temperature alloy bar blank horizontally on the platform of the press, and the pressure head of the press performs the first drawing from one end of the bar blank to the other end. After the first drawing is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for the second time. After the second drawing is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for the third time, and so on, until the specified size is reached, that is, the drawing is completed and the bar blank is obtained, and the deformation of the adjacent two drawing times is 4%. After the last drawing is completed, the temperature of the bar blank is not less than 900°C. The process of the fourth annealing treatment is annealing temperature 1170°C, annealing time 2h, and no protective atmosphere is required during the fourth annealing treatment.

[0088] In step eight, after the fourth annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to an electro-hydraulic hammer within 3 minutes, and is prepared into a plate with a width of 100 mm and a thickness of 50 mm by a reforming forging method.

[0089] The carbide microstructure of the plate prepared by the method of this embodiment is as follows: Figure 7 As shown in Figure 1, the carbides are small and evenly distributed, and no stress concentration will occur. The microstructure of the δ phase is shown in Figure 1. Figure 8 As shown, the δ phase has a uniform distribution in morphology, which is beneficial to the uniform control of grain size in subsequent deformation, ensuring uniform properties of the alloy and reducing stress concentration.

[0090] Special note: The technical solution of the present invention involves many parameters, and the synergistic effects between the various parameters need to be comprehensively considered to obtain the beneficial effects and significant progress of the present invention. Moreover, the value ranges of the various parameters in the technical solution are obtained after a large number of experiments. For each parameter and the combination of each parameter, the inventor has recorded a large amount of experimental data. Due to space limitations, the specific experimental data will not be disclosed here.

[0091] It is not difficult for those skilled in the art to understand that the control method of the strip-shaped structure of the GH4169 nickel-based high-temperature alloy of the present invention includes any combination of the invention content and the specific implementation method of the above-mentioned invention specification and the various parts shown in the drawings. Due to the limited space and to make the specification concise, the various schemes composed of these combinations are not described one by one. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for controlling the banded structure of GH4169 nickel-based high-temperature alloy, characterized in that: The control method comprises the following steps in order: Step 1: Prepare a cylindrical GH4169 nickel-based high-temperature alloy ingot according to design requirements; Step 2: placing the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace for the first homogenization treatment; Step 3: After the first homogenization treatment is completed, the cylindrical GH4169 nickel-based high-temperature alloy ingot is transferred to a press for the first upsetting and drawing to obtain a bar blank, and the bar blank obtained by the first upsetting is placed in a heat treatment furnace for the first annealing treatment; Step 4: After the first annealing treatment is completed, the rod blank is transferred to a press for a second upsetting and further obtained as a rod blank, and the rod blank obtained by the second upsetting is placed in a heat treatment furnace for a second annealing treatment; Step 5: After the second annealing treatment is completed, the rod blank is transferred to a press for a third upsetting and further obtained as a rod blank, and the rod blank obtained by the third upsetting is placed in a heat treatment furnace for a third annealing treatment; Step 6: After the third annealing treatment is completed, the rod blank is transferred to a press for a fourth upsetting and further obtained as a rod blank, and the rod blank obtained by the fourth upsetting is placed in a heat treatment furnace for a second homogenization treatment; Step 7: After the second homogenization treatment is completed, the rod blank is transferred to a press for drawing. After the drawing is completed, a deformed GH4169 nickel-based high-temperature alloy rod blank can be obtained. The drawn rod blank is placed in a heat treatment furnace for the fourth annealing treatment; Step 8: After the fourth annealing treatment is completed, small-sized billets are cut according to demand and transferred to an electro-hydraulic hammer or a hot rolling mill for reforging or hot rolling. After the reforging or hot rolling is completed, a GH4169 nickel-based high-temperature alloy plate or GH4169 nickel-based high-temperature alloy bar with controllable strip-shaped structure can be obtained.

2. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 1, characterized in that: In step 1, the chemical composition of the cylindrical GH4169 nickel-based high-temperature alloy ingot includes Ni 50.0-55.0%, Cr 17.0-21.0%, Nb+Ta 4.75-5.5%, Mo 2.8-3.3%, Ti 0.65-1.15%, Al 0.2-0.8%, Co≤0.04%, C0.02-0.08%, and the balance is Fe; the cylindrical GH4169 nickel-based high-temperature alloy ingot is prepared by triple smelting, namely, vacuum induction melting process, protective atmosphere electroslag remelting process and vacuum consumable remelting process; the key parameters of the vacuum induction melting process are that the vacuum pressure of chemical cleaning does not exceed 30Pa, the vacuum pressure in the refining stage does not exceed 10Pa, and the pouring temperature is 1500-1550℃; the key parameters of the protective atmosphere electroslag remelting process are that the melting speed is not higher than 4.5kg / min, the argon flow rate is not less than 5L / min, and the shrinkage feeding weight is not less than 85kg; the key parameters of the vacuum consumable remelting process are that the melting speed is not higher than 4.5kg / min, the helium pressure does not exceed 600Pa, the shrinkage feeding weight is not less than 85kg, and the diameter of the consumable ingot does not exceed 410mm.

3. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 2, characterized in that: In step 2, the process system for the first homogenization treatment is to place the cylindrical GH4169 nickel-based high-temperature alloy ingot into a heat treatment furnace, and heat it from room temperature to 800°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 800°C to 1000°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 1000°C to 1130°C at a heating rate of 5-10°C / min, and keep it warm for 5-7h; continue to heat it from 1130°C to 1160°C at a heating rate of 5-10°C / min, and keep it warm for 25-30h; continue to heat it from 1160°C to 1200°C at a heating rate of 5-10°C / min, and keep it warm for 72-80h; continue to cool it from 1200°C to 1150°C at a cooling rate of 5-10°C / min, and keep it warm for 4-6h; no protective atmosphere is required during the first homogenization treatment.

4. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 3, characterized in that: In step 3, after the first homogenization treatment is completed, the cylindrical GH4169 nickel-based high-temperature alloy ingot is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the first upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 20-40%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press moves from one end of the bar blank to the other end. After the first stretching, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the first upsetting and drawing, that is, the first upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching is 1-4%. After the last stretching, the temperature of the rod blank is not less than 900℃; The process system of the first annealing treatment is as follows: annealing temperature is 1100-1150° C., annealing time is 2-4 hours, and no protective atmosphere is required during the first annealing treatment.

5. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 4, characterized in that: In step 4, after the first annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the second upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30-50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first upsetting from one end of the bar blank to the other end. After the first stretching, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the second upsetting and drawing, that is, the second upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching is 1-4%. After the last stretching, the temperature of the rod blank is not less than 900℃; The process system of the second annealing treatment is as follows: annealing temperature is 1100-1150° C., annealing time is 2-4 hours, and no protective atmosphere is required during the second annealing treatment.

6. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 5, characterized in that: In step 5, after the second annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the third upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30-50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the third upsetting from one end of the bar blank to the other end. After the first stretching, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the third upsetting and drawing, that is, the third upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching is 1-4%. After the last stretching, the temperature of the rod blank is not less than 900℃; The process system of the third annealing treatment is as follows: annealing temperature is 1100-1150° C., annealing time is 2-4 hours, and no protective atmosphere is required during the third annealing treatment.

7. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 6, characterized in that: In step six, after the third annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to a press within 3 minutes; the process system of the fourth upsetting is to place the cylindrical GH4169 nickel-based high-temperature alloy bar blank vertically on the platform of the press, and the pressure head of the press starts to press down from the upper end surface of the bar blank, and the deformation amount is 30-50%, and then the upset GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first upsetting from one end of the bar blank to the other end. After the first stretching, the rod blank is rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the second stretching. After the second stretching, the rod blank is further rotated 60° along the axial direction, and the ram of the press continues to stretch the rod blank from one end to the other end for the third stretching, and so on, until the rod blank is stretched to the length before the fourth upsetting and drawing begins, that is, the fourth upsetting and drawing is completed and the rod blank is obtained. The deformation of the two adjacent stretching is 1-4%. After the last stretching, the temperature of the rod blank is not less than 900℃.

8. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 7, characterized in that: In step six, the process system of the second homogenization treatment is to place the GH4169 nickel-based high-temperature alloy billet into a heat treatment furnace, and heat it from room temperature to 800°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 800°C to 1000°C at a heating rate of 5-10°C / min, and keep it warm for 2-4h; continue to heat it from 1000°C to 1130°C at a heating rate of 5-10°C / min, and keep it warm for 5-7h; continue to heat it from 1130°C to 1160°C at a heating rate of 5-10°C / min, and keep it warm for 5-7h; continue to heat it from 1160°C to 1200°C at a heating rate of 5-10°C / min, and keep it warm for 40-50h; continue to cool it from 1200°C to 1150°C at a cooling rate of 5-10°C / min, and keep it warm for 4-6h; no protective atmosphere is required during the second homogenization treatment.

9. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 8, characterized in that: In step seven, after the second homogenization treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to the press within 3 minutes; the process system of the drawing is that the GH4169 nickel-based high-temperature alloy bar blank is placed horizontally on the platform of the press, and the pressure head of the press performs the first drawing from one end of the bar blank to the other end. After the first drawing is completed, the bar blank is rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for the second time. After the second drawing is completed, the bar blank is further rotated 60° axially, and the pressure head of the press continues to draw from one end of the bar blank to the other end for the third time, and so on, until the specified size is reached, that is, the drawing is completed and the bar blank is obtained, the deformation of the adjacent two drawing passes is 1-4%, and after the last drawing pass, the temperature of the bar blank is not less than 900°C; The process system of the fourth annealing treatment is as follows: annealing temperature is 1120-1170° C., annealing time is 2-4 hours, and no protective atmosphere is required during the fourth annealing treatment.

10. The method for controlling the banded structure of GH4169 nickel-based high-temperature alloy according to claim 9, characterized in that: In step eight, after the fourth annealing treatment is completed, the GH4169 nickel-based high-temperature alloy bar blank is taken out from the heat treatment furnace and transferred to an electro-hydraulic hammer or a hot rolling mill within 3 minutes; it is prepared into a plate by a forging method, with a width of 50-200 mm, a thickness of 40-60 mm, and a deformation of 20-60%; it is prepared into a rod by a hot rolling method, with a diameter of 12-55 mm and a deformation of 30-95%.

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