Preparation method of GH4141 high-temperature alloy

Through the triple smelting process of vacuum induction, electroslag remelting and vacuum self-consumption, the process parameters and raw material addition sequence are optimized, and the problems of impurities and inclusions in GH4141 high-temperature alloy are solved, and the preparation of high-purity alloy is realized.

CN120536765APending Publication Date: 2025-08-26PANGANG GROUP JIANGYOU CHANGCHENG SPECIAL STEEL COMPANY LIMITED +1
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202510816189.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-18
Publication Date
2025-08-26

AI Technical Summary

Technical Problem

The prior art is difficult to effectively control the content of impurities and harmful elements in GH4141 high-temperature alloys, and the number of inclusions is large, which affects the purity and mechanical properties of the alloy.

Method used

The triple smelting process of vacuum induction + electroslag remelting + vacuum self-consumption is adopted. By optimizing the process parameters of vacuum induction, electroslag remelting and vacuum self-consumption, the order of adding microalloy raw materials is controlled, and vacuum carbon deoxygenation and reasonable slag system ratio is used to reduce carbide segregation and inclusions.

Benefits of technology

A high-purity GH4141 high-temperature alloy with low content of impurity and harmful elements and low inclusions was prepared, which significantly improved the purity and mechanical properties of the alloy.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure HDA0005455298360000011
    Figure HDA0005455298360000011
  • Figure HDA0005455298360000012
    Figure HDA0005455298360000012
  • Figure HDA0005455298360000021
    Figure HDA0005455298360000021
Patent Text Reader

Abstract

The invention provides a preparation method of a GH4141 high-temperature alloy, which comprises the following steps: S1) proportioning according to the composition proportion of the GH4141 high-temperature alloy, melting a nickel raw material, a chromium raw material, a molybdenum raw material, a carbon raw material, an aluminum raw material, a titanium raw material, a boron raw material, a zirconium raw material and a nickel-magnesium alloy in batches, refining, tapping and pouring to obtain a cast ingot; the cast ingot is annealed, and the electrode for electroslag remelting is obtained; s2) carrying out electroslag remelting on the electrode for electroslag remelting to obtain a vacuum self-consuming electrode; and S3) the vacuum self-consuming electrode is subjected to vacuum self-consuming remelting, and the GH4141 high-temperature alloy is obtained. According to the preparation method of the GH4141 difficult-to-deform high-temperature alloy, the triple smelting means of vacuum induction smelting, electroslag remelting and vacuum consumable remelting is utilized, and the process of each stage is controlled, so that the content of impurity elements and harmful elements is low, the number of inclusions is small, and the high-purity GH4141 high-temperature alloy is obtained.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of high-temperature alloy preparation, and in particular to a preparation method of GH4141 high-temperature alloy. Background Art

[0002] GH4141 superalloy is a precipitation-hardening nickel-based wrought alloy with γ′ phase and M6C carbides as its primary strengthening phases. It is widely used in aerospace components requiring high strength below 870°C and oxidation resistance below 980°C. GH4141 superalloy has a high alloying element content and contains three carbide phases: MC, M6C, and M23C6. MC and M6C carbides are prone to precipitation during solidification. The primary carbides in the as-cast structure of GH4141 superalloy are large, making them difficult to dissolve or eliminate through conventional homogenization heat treatment and forging deformation. This results in a clustered or banded distribution of carbides within the alloy, reducing the alloy's mechanical properties. Furthermore, carbide precipitation is closely related to inclusions, with a large number of carbides nucleating and growing around inclusions. Therefore, improving the alloy's purity and reducing the number of inclusions are effective approaches to improving the microstructure homogeneity of GH4141 alloy.

[0003] Based on the above, researchers have conducted many studies. For example, Chinese patent publication number CN115233013A discloses a method for preparing an ingot of a difficult-to-deform high-temperature alloy GH4141. This method reduces the gas O and N content in the alloy by adjusting the process of vacuum induction melting to a reasonable order of feeding, melting temperature and time, refining temperature and time, and electromagnetic stirring time, without paying attention to the content of impurity element S and other harmful elements. Chinese patent publication number CN115821117A discloses a GH4141 high-temperature alloy and its preparation method. This method uses a dual smelting process of vacuum induction + electroslag remelting to improve the solidification structure of the ingot, and uses homogenization and forging to eliminate element segregation. This method mainly solves the problem of hot working plasticity of the alloy and improves the yield rate.

[0004] The above-mentioned technology still needs to improve the control of impurity elements, harmful elements and inclusions in GH4141 difficult-to-deform high-temperature alloy. Therefore, it is of great significance to provide a high-purity GH4141 difficult-to-deform high-temperature alloy and a preparation method thereof to reduce the content of impurity elements and harmful elements and the number of inclusions in the alloy. Summary of the Invention

[0005] The technical problem solved by the present invention is to provide a method for preparing a GH4141 high-temperature alloy. The GH4141 high-temperature alloy prepared in the present application has low contents of impurity elements and harmful elements and a small number of inclusions.

[0006] In view of this, the present application provides a method for preparing GH4141 high-temperature alloy, comprising the following steps:

[0007] S1) According to the composition ratio of GH4141 high-temperature alloy, nickel raw material, chromium raw material, molybdenum raw material and 2 / 3 carbon are added as a first batch of raw materials into a vacuum induction furnace for melting, the remaining carbon is added after the first batch of raw materials are melted, and then aluminum raw material and titanium raw material are added as a second batch of raw materials after a film is formed on the surface of the molten steel, and then a third batch of raw materials, boron raw material and zirconium raw material, are added, and nickel-magnesium alloy is added after argon filling. After tapping, the ingot is cast to obtain an ingot; the ingot is annealed to obtain an electrode for electroslag remelting;

[0008] S2) electroslag remelting the electrode for electroslag remelting, wherein in a steady-state smelting stage, the melting rate is 3.5 to 5.5 kg / min and the slag resistance swing is 0.35 to 0.55 mΩ to obtain a vacuum consumable electrode;

[0009] S3) remelting the vacuum consumable electrode to obtain GH4141 high-temperature alloy.

[0010] In some specific embodiments, in step S1), the nickel raw material is selected from electrolytic nickel plate, the chromium raw material is selected from metallic chromium, the molybdenum raw material is selected from molybdenum bar, the aluminum raw material is selected from aluminum bar, the titanium raw material is selected from metallic titanium, the boron raw material is selected from ferroboron, and the zirconium raw material is selected from sponge zirconium.

[0011] In some specific embodiments, in step S1), after adding the vacuum induction furnace, the vacuum is evacuated to a vacuum degree of ≤1Pa; and / or, after adding the remaining carbon, the temperature is adjusted to 1500-1600°C and stirred for 30-60min; and / or, after adding the second batch of raw materials, stirring is performed for 10-30min; and / or, argon is filled to 5000-6500Pa; and / or, the temperature of the steel tapping is 1450-1500°C.

[0012] In some specific embodiments, in step S1), the heating rate of the annealing is 1-1.5 min / mm, the annealing temperature is 1050-1150° C., and the holding time of the annealing is 10-15 h.

[0013] In some specific embodiments, in step S2), pre-melted slag is introduced during the electroslag remelting process. The pre-melted slag includes, by mass percentage, 10-30% CaO, 13.5-16.5% Al2O3, 4-70% CaF2, and 2.5-3.5% TiO2. The amount of pre-melted slag added is 50-55 kg / furnace.

[0014] In some specific embodiments, in step S2), before the electroslag remelting, the process further includes: introducing argon gas into the crystallizer for 15 to 20 minutes; and maintaining the introduction of argon gas during the electroslag remelting process.

[0015] In some specific embodiments, in step S2), during the steady-state smelting stage, the slag resistance swing fluctuation is ≤±0.25mΩ; and / or, the steel ingot after electroslag remelting is furnace cooled for ≥1h before being taken out of the furnace.

[0016] In some specific embodiments, in step S3), before the vacuum consumable remelting, the step further includes: adjusting the vacuum degree of the vacuum consumable furnace to ≤0.1 Pa.

[0017] In some specific embodiments, in step S3), during the vacuum consumable remelting process, in the arc starting stage of melting, the arc starting current is 3000-5000A, and the arc starting voltage is 20.0-25.0V; and / or, in the steady-state melting stage, helium is filled, the helium pressure is 300-500Pa, and the melting rate is 2.5-5kg / min; and / or, in the hot capping stage, the melting rate is 1.2-3.5kg / min; and / or, after the vacuum consumable remelting is completed, the steel is taken out of the furnace after vacuum cooling for ≥2h.

[0018] In some specific embodiments, the composition of the GH4141 high-temperature alloy, in percentage by mass, includes: C: 0.06-0.12%, Cr: 18.0-20.0%, Co: 10.0-12.0%, Mo: 9.50-10.50%, Al: 1.4-1.8%, Ti: 3.0-3.5%, B: 0.003-0.010%, Si≤0.5%, Mn≤0.5%, Cu≤0.5%, P≤0.015%, S≤0.015%, Fe≤5.0%, Zr≤0.07%, and the balance is Ni.

[0019] The present application provides a preparation method of GH4141 high-temperature alloy, which firstly prepares the ingredients according to the composition ratio of GH4141 high-temperature alloy, and adds the raw materials in four batches for smelting, refining and pouring respectively to obtain an electrode for electroslag remelting, and then electroslag remelting the electrode for electroslag remelting, and then vacuum consumable remelting the obtained electrode for electroslag consumable to obtain GH4141 high-temperature alloy; in the preparation process of GH4141 high-temperature alloy, a triple smelting process of vacuum induction + electroslag remelting + vacuum consumable is adopted, wherein, in the melting period of vacuum induction melting, a special carbon addition method is adopted to fully utilize vacuum carbon deoxidation, and in the later refining, the order of adding micro-alloy raw materials is reasonably controlled, and further The first step ensures the removal of impurity elements. During the electroslag remelting process, the control of melting rate and slag resistance swing can reduce carbide segregation and effectively remove inclusions. The final vacuum consumable remelting can remove gas elements and harmful impurity elements in the alloy again, thereby obtaining a high-purity GH4141 alloy with low content of alloy impurity elements and harmful elements and a small number of inclusions. Experimental results show that the GH4141 alloy prepared by the present application has O≤8ppm, N≤20ppm, S≤5ppm, harmful elements As≤2ppm, Sb≤0.5ppm, Bi≤0.01ppm, Sn≤1ppm, Pb≤0.1ppm, and inclusion number density≤25 pieces / mm 2 . BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a bar chart of the inclusion scanning results of the GH4141 high-temperature alloy prepared in Example 1 of the present invention;

[0021] Figure 2 This is a bar chart of the inclusion scanning results of the GH4141 high-temperature alloy prepared in Example 2 of the present invention;

[0022] Figure 3 This is a bar chart of the inclusion scanning results of the GH4141 high-temperature alloy prepared in Example 3 of the present invention;

[0023] Figure 4 This is a bar chart of the inclusion scanning results of the GH4141 high-temperature alloy prepared in Example 4 of the present invention;

[0024] Figure 5 This is a bar chart showing the inclusion scanning results of the GH4141 high-temperature alloy prepared in Comparative Example 1 of the present invention;

[0025] Figure 6 This is a bar chart of the inclusion scanning results of the GH4141 high-temperature alloy prepared in Comparative Example 2 of the present invention;

[0026] Figure 7 This is a bar chart of the inclusion scanning results of the GH4141 high-temperature alloy prepared in Comparative Example 3 of the present invention. DETAILED DESCRIPTION

[0027] In order to further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples. However, it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, rather than limiting the claims of the present invention.

[0028] In response to the problems of high content of impurity elements and harmful elements and large number of inclusions in GH4141 high-temperature alloy prepared by existing preparation methods, the present application provides a preparation method of GH4141 high-temperature alloy, which adopts a triple smelting process of vacuum induction + electroslag remelting + vacuum consumable smelting, optimizes the process parameters of vacuum induction, electroslag remelting and vacuum consumable smelting, optimizes the carbon addition method during the melting period of vacuum induction melting, fully utilizes vacuum carbon deoxidation, and reasonably regulates the order of adding micro-alloying raw materials during the refining period to further ensure the removal of impurity elements; during the electroslag remelting process, it is preferred to control the burnout of Al and Ti in the alloy through a reasonable slag system ratio, and remove S and inclusions; during the vacuum consumable remelting process, the gas elements and harmful impurity elements in the alloy are removed again, thereby obtaining a high-purity GH4141 alloy with low content of alloy impurity elements and harmful elements and a small number of inclusions. Specifically, the embodiment of the present invention discloses a preparation method of GH4141 high-temperature alloy, comprising the following steps:

[0029] S1) According to the composition ratio of GH4141 high-temperature alloy, nickel raw material, chromium raw material, molybdenum raw material and 2 / 3 carbon are added as a first batch of raw materials into a vacuum induction furnace for melting, the remaining carbon is added after the first batch of raw materials are melted, and then aluminum raw material and titanium raw material are added as a second batch of raw materials after a film is formed on the surface of the molten steel, and then a third batch of raw materials, boron raw material and zirconium raw material, are added, and nickel-magnesium alloy is added after argon filling. After tapping, the ingot is cast to obtain an ingot; the ingot is annealed to obtain an electrode for electroslag remelting;

[0030] S2) electroslag remelting the electrode for electroslag remelting, wherein in a steady-state smelting stage, the melting rate is 3.5 to 5.5 kg / min and the slag resistance swing is 0.35 to 0.55 mΩ to obtain a vacuum consumable electrode;

[0031] S3) remelting the vacuum consumable electrode to obtain GH4141 high-temperature alloy.

[0032] During the preparation of the GH4141 superalloy, vacuum induction melting is first performed. The raw materials are prepared according to the composition ratio of the GH4141 superalloy. The raw materials are well known to those skilled in the art and are not particularly limited in this application. For example, the nickel raw material is selected from electrolytic nickel plate, the chromium raw material is selected from metallic chromium, the molybdenum raw material is selected from molybdenum bar, the aluminum raw material is selected from aluminum bar, the titanium raw material is selected from metallic titanium, the boron raw material is selected from ferroboron, and the zirconium raw material is selected from sponge zirconium. During the preparation process, the nickel raw material, chromium raw material, molybdenum raw material, and carbon can be used as the first batch of raw materials, the aluminum raw material and titanium raw material can be used as the second batch of raw materials, the boron raw material and zirconium raw material can be used as the third batch of raw materials, and the nickel-magnesium alloy can be used as the fourth batch of raw materials. After batching, the raw materials are then vacuum-induction melted in a vacuum induction furnace. First, nickel, chromium, molybdenum, and two-thirds of the carbon are added as the first batch of raw materials to the vacuum induction furnace for melting. The furnace is then evacuated to a vacuum of ≤1 Pa. Once all the raw materials are melted, the remaining carbon is added. The temperature is adjusted to 1500-1600°C and stirred for 30-60 minutes, more specifically 1540-1560°C, and stirred for 40-50 minutes, more specifically 1545-1550°C. Once the molten steel forms a film, the second batch of aluminum and titanium raw materials are added and stirred for 10-30 minutes, more specifically 10-20 minutes. Samples are then preferably taken for composition testing. If the composition does not meet the requirements for the GH4141 superalloy, the molten steel composition is fine-tuned. Simultaneously, the third batch of boron and zirconium raw materials are added. Finally, argon is filled to 5000-6500 Pa, and nickel-magnesium alloy is added to perform precipitation deoxidation and improve the distribution of inclusions. Specifically, the argon filling is to 5300-6200 Pa. After the above smelting, the temperature is adjusted to 1450-1500°C for tapping and pouring to obtain an ingot. Specifically, the temperature is adjusted to 1460-1490°C.

[0033] In the above vacuum induction melting process, due to the overall high carbon content of GH4141 alloy, 2 / 3 of carbon is added first, so as to make full use of the deoxidation ability of carbon under vacuum conditions and remove the O element in the alloy to the greatest extent. In addition, carbon combines with oxygen to generate CO gas, which precipitates from the molten steel, promotes the volatilization of gas elements such as N and H and harmful elements such as Pb, Sb, and Bi in the molten steel, and removes inclusions by floating up. Aluminum bars and metallic titanium are added after refining because Al and Ti elements are easily oxidized. Under the premise that they have been fully deoxidized and denitrified during the melting period, , added after refining to avoid combining with O and N to form more inclusions (Al2O3, nitrides, etc.); ferroboron and sponge zirconium are added after refining, because B and Zr are micro-alloying elements with low content, but they are very easy to oxidize. Therefore, in order to improve the element yield, they are added after the smelting temperature is lowered after refining; Mg element is very easy to oxidize and volatilize, so the nickel-magnesium alloy is added after argon filling to effectively ensure the yield of Mg element; on the other hand, adding raw materials in batches can effectively prevent bridging during the alloy smelting process and ensure the stability of the smelting process. The types of inclusions in GH4141 high-temperature alloy generally include oxides, carbides, nitrides, and sulfides such as Al2O3, Ti(CN), MgO, SiO2, and MgS; this application uses a reasonable smelting process to minimize the content of harmful elements such as O, N, and S in the alloy and ensure that the inclusions float up and are removed to achieve the purpose of reducing inclusions.

[0034] During the solidification process of the alloy steel liquid, the structural stress and solidification shrinkage stress will be generated due to the rapid solidification speed. In addition, the temperature at the head and tail of the ingot mold is low, and the temperature in the middle is high, which also forms a large tensile stress. Cracks are easily generated in the middle, affecting the stability of the subsequent remelting process. Therefore, the present application anneals the ingot to obtain an electrode for electroslag remelting. The annealing is to eliminate the residual stress inside the ingot and reduce the hardness of the ingot. The annealing heating rate is 1 to 1.5 min / mm, the annealing temperature is 1050 to 1150 ° C, and the annealing holding time is 10 to 15 hours; specifically, the annealing heating rate is 1.2 to 1.4 min / mm, the annealing temperature is 1080 to 1100 ° C, and the annealing holding time is 12 to 14 hours.

[0035] The present application then performs electroslag remelting on the electrodes for electroslag remelting, wherein the electroslag remelting remelts the metal electrodes by means of slag resistance heat and solidifies layer by layer in a water-cooled crystallizer to improve the structure and properties of the material; the electroslag remelting generally includes a preparation stage, an arc starting stage, a steady-state melting and a feeding stage. The pre-melted slag used in the electroslag remelting process of the present application includes CaO, Al2O3, CaF2, and TiO2, and includes, by mass percentage, 10-30% CaO, 13.5-16.5% Al2O3, 54-70% CaF2, and 2.5-3.5% TiO2. The amount of the pre-melted slag added is 50-55 kg per furnace. Specifically, 16-26% CaO, 14-16% Al2O3, 60-67% CaF2, and 2.8-3.2% TiO2. The amount of the pre-melted slag added is 52-53 kg per furnace. More specifically, 20-24% CaO, 14.5-15.5% Al2O3, 64-66% CaF2, and 2.9-3.0% TiO2. Argon is introduced into the crystallizer for 15-20 minutes before the electroslag remelting begins, and the argon gas is maintained throughout the electroslag remelting process. During the steady-state smelting stage, the present application controls the melting rate and slag resistance swing. The melting rate is 3.5-5.5 kg / min, and the slag resistance swing is 0.35-0.55 mΩ. Specifically, the melting rate is 3.8-5.0 kg / min, and the slag resistance swing is 0.38-0.50 mΩ. More specifically, the melting rate is 4.0-4.5 kg / min, and the slag resistance swing is 0.40-0.46 mΩ. The melting rate controls the depth of the alloy molten pool and reduces carbide segregation. The slag resistance swing controls the depth of the electrode rod inserted into the slag pool, improves the smelting conditions to effectively remove inclusions and avoid slag wrapping. Furthermore, the slag resistance swing fluctuates ≤±0.25 mΩ. Specifically, the slag resistance swing fluctuates at ±0.25 mΩ and ±0.20 mΩ. During the shrinkage feeding stage, the melting rate gradually decreases to 1 kg / min and remains constant for 1.5 hours before the smelting is terminated. After the electroslag remelting is completed, the obtained steel ingot is furnace cooled for ≥1h before being taken out of the furnace.

[0036] The present application then subjects the steel ingot obtained above to vacuum consumable remelting, a secondary refining process that uses arc heating to melt metal electrodes in a high vacuum environment and directionally solidify them in a crystallizer. This process includes a preparation phase, an arc-starting phase, a steady-state melting phase, and a feeding phase. In this application, the vacuum consumable furnace is evacuated to a vacuum of ≤0.1 Pa before power is supplied to the melting arc-starting phase. The arc starting current in the arc starting stage is 3000-5000A, and the arc starting voltage is 20.0-25.0V. Specifically, the arc starting current is 3200-4500A, and the arc starting voltage is 20.8-24.2V. More specifically, the arc starting current is 3500-4200A, and the arc starting voltage is 21.3-23.0V. More specifically, the arc starting current is 3800-4000A, and the arc starting voltage is 22.0-22.6V. The above-mentioned arc starting current and voltage are controlled to quickly form a molten pool, ensure the stability of the subsequent smelting process, reduce the depth of the non-steady-state molten pool, and improve the yield rate. In the steady-state smelting stage, helium is filled, and the helium pressure is 300-500Pa, and the melting rate is 2.5-5kg / min. Specifically, the helium pressure is 320-460Pa, and the melting rate is 2.7-4.8kg / min. More specifically, the helium pressure is 350-430Pa, and the melting rate is 3.2-4.5kg / min. More specifically, the helium pressure is 380-400Pa, and the melting rate is 3.8-4.3kg / min. The above-mentioned suitable helium pressure and melting rate are to ensure the depth and shape of the molten pool and reduce the solidification segregation of the consumable ingot. During the hot capping stage, the melting rate is 1.2 to 3.5 kg / min, specifically 1.8 to 3.2 kg / min, more specifically 2.3 to 3.0 kg / min, and even more specifically 2.5 to 2.8 kg / min. In this application, the melting rate during the hot capping stage is lower than the melting rate during the steady-state melting stage to reduce heat input at the ingot head, effectively reducing head segregation and shrinkage cavities, and promoting the floating and removal of inclusions. After the vacuum consumable remelting is completed, the ingot is continued to cool in vacuum for ≥ 2 hours before being discharged from the furnace.

[0037] The preparation method provided in the present application is applicable to the GH4141 high-temperature alloy, the composition of which, in terms of mass percentage, includes: C: 0.06-0.12%, Cr: 18.0-20.0%, Co: 10.0-12.0%, Mo: 9.50-10.50%, Al: 1.4-1.8%, Ti: 3.0-3.5%, B: 0.003-0.010%, Si≤0.5%, Mn≤0.5%, Cu≤0.5%, P≤0.015%, S≤0.015%, Fe≤5.0%, Zr≤0.07%, and the balance is Ni. In a specific embodiment, the composition of the GH4141 high-temperature alloy includes: C 0.07%, Cr 19%, Co 11%, Mo 9.8%, Al 1.6%, Ti 3.2%, B 0.006%, Zr 0.02%, and the balance is Ni; or, C 0.08%, Cr 19.5%, Co 11%, Mo 10%, Al 1.6%, Ti 3.2%, B 0.006%, Zr 0.03%, and the balance is Ni.

[0038] The present invention provides a method for preparing a GH4141 high-temperature alloy that is difficult to deform. This method utilizes a triple melting process consisting of vacuum induction melting, electroslag remelting, and vacuum consumable remelting, and by controlling the process parameters at each stage, the prepared alloy has low impurity and harmful element contents and a low number of inclusions, resulting in a high-purity GH4141 high-temperature alloy. Experimental results show that the GH4141 alloy prepared in this application has O ≤ 8ppm, N ≤ 20ppm, S ≤ 5ppm, harmful elements As ≤ 2ppm, Sb ≤ 0.5ppm, Bi ≤ 0.01ppm, Sn ≤ 1ppm, Pb ≤ 0.1ppm, and an inclusion density of ≤ 25 per mm. 2 .

[0039] In order to further understand the present invention, the preparation method of the GH4141 high-temperature alloy provided by the present invention is described in detail below with reference to the examples. The protection scope of the present invention is not limited by the following examples.

[0040] Example 1

[0041] This embodiment provides a method for preparing a high-purity GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a size of Φ508 mm. The steps are as follows:

[0042] A. Vacuum induction melting: The raw materials are prepared according to the chemical composition of GH4141 alloy. In terms of mass percentage, the chemical composition includes: C 0.07%, Cr 19%, Co 11%, Mo 9.8%, Al 1.6%, Ti 3.2%, B 0.006%, Zr0.02%, and the balance is Ni; electrolytic nickel plate, metallic chromium, metallic cobalt, molybdenum bar and 2 / 3 carbon as raw materials ① are added into a vacuum induction furnace, evacuated to a vacuum degree of ≤1Pa in the furnace, and power is supplied to melt the material. After all the raw materials ① are melted, the remaining 1 / 3 of the carbon is added, and the temperature is adjusted to 1540°C, and the steel is stirred at an industrial frequency for 40 minutes. Aluminum bar and metallic titanium are then added as raw materials ② after a film is formed on the surface of the molten steel, and stirred at an industrial frequency for 20 minutes. After that, samples are taken for component detection, and the composition of the molten steel is fine-tuned. At the same time, raw materials ③ ferroboron and sponge zirconium are added, and then argon is filled to 6500Pa. Raw material ④ nickel-magnesium alloy is added, and the temperature is adjusted to 1450°C for tapping and casting into a Φ360mm ingot;

[0043] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1 min / mm, an annealing temperature of 1100°C, and a holding time of 10 hours. The induction ingot is peeled by polishing and the head and tail are cut to obtain the electrode rod required for vacuum consumables.

[0044] C. Electroslag remelting: Pre-melted slag was used for smelting. The composition of the pre-melted slag was as follows: CaO: 20%, Al2O3: 13.5%, CaF2: 64%, and TiO2: 2.5% by weight. The slag volume was 50 kg / furnace. Argon was introduced into the crystallizer for 15 minutes before remelting and maintained during the remelting process. The melting rate and slag resistance swing were controlled during the steady-state melting stage. The melting rate was 4.5 kg / min, the slag resistance swing was set to 0.5 mΩ, and the slag resistance swing fluctuation was ±0.25 mΩ. The melting rate was gradually reduced to 1 kg / min during the feeding stage and maintained constant for 1.5 hours before the remelting was completed. After the remelting was completed, the steel ingot was cooled in the furnace for 1 hour and then removed from the furnace. The Φ430 mm electroslag ingot obtained by demoulding was polished and the head and tail were cut to produce the electrode rod required for vacuum consumables.

[0045] D. Vacuum consumable remelting: Place the electrode rod prepared in step C into a vacuum consumable furnace. When the vacuum degree is ≤0.1Pa, start power supply and enter the arc starting stage of melting. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 500Pa. The melting rate is controlled at 3.8kg / min. In the hot capping stage, the melting rate is 1.2-3.5kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0046] The GH4141 alloy prepared in this embodiment has high purity, and the detection results of impurity elements and harmful elements are shown in Table 1;

[0047] Table 1 Impurity and harmful element test results of GH4141 alloy prepared in Example 1 (ppm)

[0048] element O N S As Sb Bi Sn Pb Example 1 7 18 4 1.6 0.3 0.004 0.6 0.05

[0049] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. The results are as follows: Figure 1 As shown by Figure 1 It can be seen that the inclusions in the GH4141 high-temperature alloy prepared in this embodiment are mainly Al2O3 and Ti(CN), and the total number density of inclusions is 24 / mm 2 .

[0050] Example 2

[0051] This embodiment provides a method for preparing a high-purity GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a size of Φ508 mm. The steps are as follows:

[0052] A. Vacuum induction melting: Prepare the smelting raw materials according to the chemical composition of GH4141 alloy. In terms of mass percentage, its chemical composition includes: C0.08%, Cr19.5%, Co11%, Mo10%, Al1.6%, Ti3.2%, B0.006%, Zr0.03%, and the balance is Ni. Electrolytic nickel plate, metal chromium, metal cobalt, molybdenum bar and 2 / 3 carbon are used as raw materials. ① Add them into the vacuum induction furnace, evacuate the furnace until the vacuum degree is ≤1Pa, start to supply power to melt the materials, and when melting, The power can be adjusted according to the situation in the furnace. After raw material ① is completely melted, add the remaining 1 / 3 of carbon and adjust the temperature to 1560℃. Stir at industrial frequency for 30 minutes. Then, add aluminum bars and titanium metal as raw materials ②. After the surface of the molten steel forms a film, add them and stir at industrial frequency for 10 minutes. After that, take samples for component testing and fine-tune the composition of the molten steel. At the same time, add raw materials ③ such as ferroboron and sponge zirconium. Then, fill the furnace with argon to 5000Pa, add raw material ④ such as nickel-magnesium alloy, adjust the temperature to 1490℃, tap the steel, and cast it into a Φ360mm ingot.

[0053] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1.5 min / mm, an annealing temperature of 1080°C, and a holding time of 15 hours. The induction ingot is polished and peeled, and the head and tail are cut to obtain the electrode rod required for vacuum consumables;

[0054] C. Electroslag remelting: Pre-melted slag is used for smelting. The composition of the pre-melted slag is as follows by weight: CaO: 10%, Al2O3: 16.5%, CaF2: 70%, TiO2: 3.5%. The slag volume is 50 kg. Argon gas is introduced into the crystallizer for 15 minutes before remelting begins, and the argon flow is maintained during the remelting process. The steady-state melting stage is controlled by melting rate and slag resistance swing. The melting rate is 3.8 kg / min, the slag resistance swing is set to 0.35 mΩ, and the slag resistance swing fluctuation is ±0.2 mΩ. During the feeding stage, the melting rate is gradually reduced to 1 kg / min and maintained constant for 1.5 hours before remelting is completed. After remelting, the steel ingot is cooled for 1 hour and then removed from the furnace. The Φ430 mm electroslag ingot obtained by demolding is polished and the head and tail are cut to produce the electrode rod required for vacuum consumables.

[0055] D. Vacuum consumable remelting: Place the electrode rod prepared in step C into a vacuum consumable furnace. When the vacuum degree is ≤0.1Pa, start power supply to enter the arc starting stage of melting. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 400Pa. The melting rate is controlled at 3.2kg / min. In the hot capping stage, the melting rate is 1.2-3.5kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0056] The results of impurity and harmful element detection of the high-purity GH4141 alloy prepared in this embodiment are shown in Table 2.

[0057] Table 2 Impurity and harmful element test results of GH4141 alloy prepared in Example 2 (ppm)

[0058] element O N S As Sb Bi Sn Pb Example 2 8 13 5 1.4 0.5 0.006 0.7 0.03

[0059] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. The results are as follows: Figure 2 As shown by Figure 2 It can be seen that the inclusions of the GH4141 high-temperature alloy prepared in this embodiment are mainly Al2O3 and Ti(CN), and the total inclusion density is 20 / mm 2 .

[0060] Example 3

[0061] This embodiment provides a method for preparing a high-purity GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a size of Φ508 mm. The steps are as follows:

[0062] A. Vacuum induction melting: The raw materials are prepared according to the chemical composition of GH4141 alloy. In terms of mass percentage, its chemical composition includes: C0.07%, Cr19%, Co11%, Mo9.8%, Al 1.6%, Ti 3.2%, B 0.006%, Zr 0.02%, the remainder is Ni; after adding electrolytic nickel plate, metallic chromium, metallic cobalt, molybdenum bar and 2 / 3 carbon as raw materials ① into a vacuum induction furnace, evacuate the furnace to a vacuum degree of ≤1Pa, start power supply for material melting, and adjust the power according to the situation in the furnace during melting. After all the raw materials ① are melted, add the remaining 1 / 3 of carbon, adjust the temperature to 1540°C, stir at an industrial frequency for 60min, then add aluminum bar and metallic titanium as raw materials ②, add them after the surface of the molten steel forms a film, stir at an industrial frequency for 20min, then take samples for component detection, and fine-tune the composition of the molten steel, add raw materials ③ ferroboron and sponge zirconium, then fill argon to 6500Pa, add raw material ④ nickel-magnesium alloy, adjust the temperature to 1470°C for tapping and pouring into a Φ360mm ingot;

[0063] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1 min / mm, an annealing temperature of 1100°C, and a holding time of 10 hours. The induction ingot is polished and peeled, and the head and tail are cut to obtain the electrode rod required for vacuum consumables;

[0064] C. Electroslag remelting: Pre-melted slag was used for smelting. The composition of the pre-melted slag was as follows by weight: CaO: 16%, Al2O3: 15.5%, CaF2: 66%, TiO2: 2.5%, and the slag volume was 55 kg. Argon was introduced into the crystallizer for 15 minutes before remelting and maintained during the remelting process. Melting rate and slag resistance swing were used to control the steady-state melting stage. The melting rate was 5.5 kg / min, the slag resistance swing was set to 0.45 mΩ, and the slag resistance swing fluctuation was ±0.25 mΩ. At the beginning of the feeding stage, the melting rate was gradually reduced to 1 kg / min and maintained constant for 1.5 hours before the remelting was completed. After the remelting was completed, the steel ingot was cooled in the furnace for 1 hour and then removed from the furnace. The Φ430 mm electroslag ingot obtained by demoulding was polished and the head and tail were cut to produce the electrode rod required for vacuum consumables.

[0065] D. Vacuum consumable remelting: Place the electrode rod prepared in step C into a vacuum consumable furnace. After the vacuum degree is ≤0.1Pa, start power supply to enter the arc starting stage of melting. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 500Pa. The melting rate is controlled at 3.8kg / min. In the hot capping stage, the melting rate is 1.2-3.5kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0066] The test results of impurity elements and harmful elements of the high-purity GH4141 alloy prepared in this embodiment are shown in Table 3;

[0067] Table 3 Impurity and harmful element test results of GH4141 alloy prepared in Example 3 (ppm)

[0068] element O N S As Sb Bi Sn Pb Example 3 6 17 5 1.8 0.5 0.009 0.8 0.1

[0069] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. The results are as follows: Figure 3 As shown by Figure 3 It can be seen that the inclusions of the GH4141 high-temperature alloy prepared in this embodiment are mainly Al2O3 and Ti(CN), and the total inclusion density is 23.2 / mm 2 .

[0070] Example 4

[0071] This embodiment provides a method for preparing a high-purity GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a size of Φ508 mm. The steps are as follows:

[0072] A. Vacuum induction melting: Prepare the smelting raw materials according to the chemical composition of GH4141 alloy. In terms of mass percentage, its chemical composition includes: C0.08%, Cr19.5%, Co11%, Mo10%, Al1.6%, Ti3.2%, B0.006%, Zr0.03%, and the balance is Ni. Electrolytic nickel plate, metal chromium, metal cobalt, molybdenum bar and 2 / 3 carbon are used as raw materials. ① Add them into the vacuum induction furnace, evacuate the furnace until the vacuum degree is ≤1Pa, start to supply power to melt the materials, and when melting, The power can be adjusted according to the situation in the furnace. After raw material ① is completely melted, add the remaining 1 / 3 of carbon and adjust the temperature to 1560℃. Stir at industrial frequency for 30 minutes. Then, add aluminum bars and titanium metal as raw materials ②. After the surface of the molten steel forms a film, add them and stir at industrial frequency for 10 minutes. After that, take samples for component testing and fine-tune the composition of the molten steel. At the same time, add raw materials ③ such as ferroboron and sponge zirconium. Then, fill the furnace with argon to 5000Pa, add raw material ④ such as nickel-magnesium alloy, adjust the temperature to 1490℃, tap the steel, and cast it into a Φ360mm ingot.

[0073] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1 min / mm, an annealing temperature of 1120°C, and a holding time of 10 hours. The induction ingot is polished and peeled, and the head and tail are cut to produce the electrode rod required for vacuum consumables;

[0074] C. Electroslag Remelting: Pre-melted slag is used for smelting. The weight percentage of the pre-melted slag is as follows: CaO: 16%, Al2O3: 14.0%, CaF2: 67%, and TiO2: 3%. The slag volume is 55 kg. Argon gas is introduced into the crystallizer for 15 minutes before remelting begins and maintained throughout the remelting process. Melting rate and slag resistance swing are used to control the steady-state melting stage. The melting rate is 3.5 kg / min, the slag resistance swing is set to 0.55 mΩ, and the slag resistance swing fluctuation is ±0.2 mΩ. During the feeding stage, the melting rate is gradually reduced to 1 kg / min and maintained constant for 1.5 hours before remelting is completed. After remelting, the steel ingot is cooled for 1 hour and then removed from the furnace. The Φ430 mm electroslag ingot obtained by demolding is polished and the head and tail are cut to produce the electrode rod required for vacuum consumables.

[0075] D. Vacuum consumable remelting: Place the electrode rod prepared in step C into a vacuum consumable furnace. After the vacuum degree is ≤0.1Pa, power is supplied to enter the melting arc starting stage. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 300Pa. The melting rate is controlled at 2.5kg / min. In the hot capping stage, the melting rate is 1.2-2.4kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0076] The results of impurity and harmful element detection of the high-purity GH4141 alloy prepared in this embodiment are shown in Table 4.

[0077] Table 4 Impurity and harmful element test results of GH4141 alloy prepared in Example 4 (ppm)

[0078] element O N S As Sb Bi Sn Pb Example 4 8 20 5 2 0.4 0.008 0.6 0.05

[0079] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. The results are as follows: Figure 4 As shown by Figure 4 It can be seen that the inclusions of the GH4141 high-temperature alloy prepared in this embodiment are mainly Al2O3 and Ti(CN), and the total inclusion density is 23.6 / mm 2 .

[0080] Comparative Example 1

[0081] This comparative example provides a preparation method for GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a specification of Φ508 mm. The steps are as follows:

[0082] A. Vacuum induction melting: Prepare the smelting raw materials according to the chemical composition of GH4141 alloy. The chemical composition by mass percentage includes: C0.08%, Cr19.5%, Co11%, Mo10%, Al1.6%, Ti3.2%, B0.006%, Zr0.03%, and the balance is Ni. Add electrolytic nickel plate, metal chromium, metal cobalt, molybdenum bar and carbon as raw materials① into the vacuum induction furnace, evacuate the furnace to a vacuum degree of ≤1Pa, and start to supply power for melting. During melting, the power can be adjusted according to the situation in the furnace. After all the raw materials ① are melted, the temperature is adjusted to 1580℃, and the raw materials are stirred at the power frequency for 30 minutes. Then, aluminum bars and titanium metal are added as raw materials ② after the surface of the molten steel forms a film. The raw materials are stirred at the power frequency for 10 minutes. After that, samples are taken for component detection and the composition of the molten steel is fine-tuned. At the same time, raw materials ③ ferroboron and sponge zirconium are added. Then, argon is filled to 5000Pa, and raw material ④ nickel-magnesium alloy is added. The temperature is adjusted to 1480℃ and the steel is tapped and cast into a Φ440mm ingot.

[0083] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1.5 min / mm, an annealing temperature of 1080°C, and a holding time of 15 hours. The induction ingot is polished and peeled, and the head and tail are cut to produce the electrode rod required for vacuum consumables.

[0084] C. Vacuum consumable remelting: Place the electrode rod prepared in step B into a vacuum consumable furnace. After the vacuum degree is ≤0.1Pa, start power supply to enter the melting arc starting stage. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 500Pa. The melting rate is controlled at 3.2kg / min. In the hot capping stage, the melting rate is 1.2-3.5kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0085] The test results of impurity elements and harmful elements of the GH4141 alloy prepared in this comparison are shown in Table 5;

[0086] Table 5 Impurity and harmful element test results of GH4141 alloy prepared in Comparative Example 1 (ppm)

[0087] element O N S As Sb Bi Sn Pb Comparative Example 1 9 13 10 2.1 0.6 0.01 1.2 0.1

[0088] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. The results are as follows: Figure 5 As shown by Figure 5 It can be seen that the inclusions of the GH4141 high-temperature alloy prepared in this comparative example are mainly Al2O3 and Ti(CN), and the total inclusion density is 51 / mm 2 .

[0089] Comparative Example 2

[0090] This comparative example provides a preparation method for GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a specification of Φ508 mm. The steps are as follows:

[0091] A. Vacuum Induction Melting: smelting raw materials are prepared according to the chemical composition of GH4141 alloy, and its chemical composition, by mass percentage, includes: C0.07%, Cr19%, Co11%, Mo9.8%, Al1.6%, Ti3.2%, B0.006%, Zr0.02%, and the balance is Ni; electrolytic nickel plate, metallic chromium, metallic cobalt, and molybdenum bar as raw materials ① are added to a vacuum induction furnace, and the furnace is evacuated to a vacuum degree of ≤1Pa. Power is then supplied to melt the materials. After the raw materials ① are completely melted, carbon is added, and the temperature is adjusted to 1540°C. The furnace is stirred at an industrial frequency for 40 minutes. Aluminum bar and metallic titanium are then added as raw materials ② after a film forms on the surface of the molten steel. The furnace is stirred at an industrial frequency for 20 minutes. Afterwards, samples are taken for composition testing, and the composition of the molten steel is finely adjusted. Simultaneously, raw materials ③, ferroboron, sponge zirconium, and nickel-magnesium alloy are added. The temperature is adjusted to 1450°C, and the steel is tapped and cast into a Φ360mm ingot;

[0092] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1 min / mm, an annealing temperature of 1100°C, and a holding time of 10 hours. The induction ingot is polished and peeled, and the head and tail are cut to obtain the electrode rod required for vacuum consumables;

[0093] C. Electroslag remelting: Pre-melted slag was used for smelting. The composition of the pre-melted slag was as follows by weight: CaO: 20%, Al2O3: 13.5%, CaF2: 64%, TiO2: 2.5%, and the slag volume was 50 kg. Argon was introduced into the crystallizer for 15 minutes before remelting and maintained during the remelting process. Melting rate and slag resistance swing were used to control the steady-state melting stage. The melting rate was 4.5 kg / min, the slag resistance swing was set to 0.5 mΩ, and the slag resistance swing fluctuation was ±0.25 mΩ. During the feeding stage, the melting rate was gradually reduced to 1 kg / min and maintained constant for 1.5 hours before the remelting was completed. After the remelting was completed, the steel ingot was cooled in the furnace for 1 hour and then removed from the furnace. The Φ430 mm electroslag ingot obtained by demoulding was peeled by polishing and the ends and tails were cut to produce the electrode rods required for vacuum consumables.

[0094] D. Vacuum consumable remelting: Place the electrode rod prepared in step C into a vacuum consumable furnace. After the vacuum degree is ≤0.1Pa, start power supply to enter the arc starting stage of melting. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 500Pa. The melting rate is controlled at 3.8kg / min. In the hot capping stage, the melting rate is 1.2-3.5kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0095] The test results of impurity elements and harmful elements of the GH4141 alloy prepared in this comparative example are shown in Table 6;

[0096] Table 6 Impurity and harmful element test results of GH4141 alloy prepared in Comparative Example 1 (ppm)

[0097] element O N S As Sb Bi Sn Pb Comparative Example 2 15 24 9 2.1 1.5 0.02 0.6 0.15

[0098] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. The results are as follows: Figure 6 As shown by Figure 6 It can be seen that the inclusions are mainly Al2O3, Ti(CN), silicates, and a small amount of sulfides. The total inclusion density is 61 / mm 2 .

[0099] Comparative Example 3

[0100] This comparative example provides a preparation method for GH4141 difficult-to-deform high-temperature alloy. The alloy consumable ingot has a specification of Φ508 mm. The steps are as follows:

[0101] A. Vacuum induction melting: The raw materials are prepared according to the chemical composition of GH4141 alloy. In terms of mass percentage, the chemical composition includes: C 0.08%, Cr 19.5%, Co 11%, Mo 10%, Al 1.6%, Ti 3.2%, B 0.006%, Zr0.03%, and the balance is Ni; after adding electrolytic nickel plate, metallic chromium, metallic cobalt, molybdenum bar and 2 / 3 carbon as raw materials ① into a vacuum induction furnace, evacuate the furnace to a vacuum degree of ≤1Pa, start power supply to melt the materials, and adjust the power according to the situation in the furnace during melting. After all the raw materials ① are melted, add the remaining 1 / 3 of the carbon, adjust the temperature to 1560°C, and stir at an industrial frequency for 30 minutes. Then, add aluminum bar and metallic titanium as raw materials ② after the surface of the molten steel forms a film, stir at an industrial frequency for 10 minutes, then take samples for component detection, and fine-tune the composition of the molten steel. At the same time, add raw materials ③ ferroboron and sponge zirconium, then fill the furnace with argon to 5000Pa, add raw material ④ nickel-magnesium alloy, adjust the temperature to 1490°C, tap and cast into a Φ360mm ingot;

[0102] B. Vacuum induction ingot annealing: After demoulding the vacuum induction ingot, annealing treatment is immediately carried out, with a heating rate of 1.5 min / mm, an annealing temperature of 1080°C, and a holding time of 15 hours. The induction ingot is polished and peeled, and the head and tail are cut to obtain the electrode rod required for vacuum consumables;

[0103] C. Electroslag remelting: Pre-melted slag was used for smelting. The composition of the pre-melted slag was as follows by weight: CaO: 10%, Al2O3: 16.5%, CaF2: 70%, TiO2: 3.5%, and the slag volume was 50 kg. Argon was introduced into the crystallizer for 15 minutes before remelting and maintained during the remelting process. Melting rate and slag resistance swing were used to control the steady-state melting stage. The melting rate was 3.2 kg / min, the slag resistance swing was set to 0.58 mΩ, and the slag resistance swing fluctuation was ±0.25 mΩ. During the feeding stage, the melting rate was gradually reduced to 1 kg / min and maintained constant for 1.5 hours before the remelting was completed. After the remelting was completed, the steel ingot was cooled in the furnace for 1 hour and then removed from the furnace. The Φ430 mm electroslag ingot obtained by demoulding was polished and the head and tail were cut to produce the electrode rod required for vacuum consumables.

[0104] D. Vacuum consumable remelting: Place the electrode rod prepared in step C into a vacuum consumable furnace. When the vacuum degree is ≤0.1Pa, start power supply to enter the arc starting stage of melting. The arc starting current is 3000-5000A and the arc starting voltage is 20.0-25.0V. In the steady-state melting stage, helium is filled into the consumable furnace with a helium pressure of 400Pa. The melting rate is controlled at 3.2kg / min. In the hot capping stage, the melting rate is 1.2-3.5kg / min. After the melting is completed, continue vacuum cooling for ≥2h before taking out of the furnace to obtain a Φ508mm GH4141 alloy vacuum consumable ingot.

[0105] The test results of impurity elements and harmful elements of the GH4141 alloy prepared in this comparative example are shown in Table 7;

[0106] Table 7 Impurity and harmful element test results of GH4141 alloy prepared in Comparative Example 2 (ppm)

[0107] element O N S As Sb Bi Sn Pb Comparative Example 2 9 15 10 1.8 0.6 0.005 1.1 0.08

[0108] The inclusions in the alloy were scanned and analyzed using a scanning electron microscope. Figure 7 As shown by Figure 7 It can be seen that the inclusions of the GH4141 high-temperature alloy prepared in this comparative example are mainly Ti(CN), Al2O3, silicates, and a small amount of sulfides. The inclusion number density is 58 / mm 2 .

[0109] The above embodiments are only intended to help understand the method and core concept of the present invention. It should be noted that, without departing from the principles of the present invention, a number of improvements and modifications may be made to the present invention by those skilled in the art, and such improvements and modifications also fall within the scope of protection of the claims of the present invention.

[0110] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing GH4141 high-temperature alloy, comprising the following steps: S1) According to the composition ratio of GH4141 high-temperature alloy, nickel raw material, chromium raw material, molybdenum raw material and 2 / 3 carbon are added as a first batch of raw materials into a vacuum induction furnace for melting, the remaining carbon is added after the first batch of raw materials are melted, and then aluminum raw material and titanium raw material are added as a second batch of raw materials after a film is formed on the surface of the molten steel, and then a third batch of raw materials, boron raw material and zirconium raw material, are added, and nickel-magnesium alloy is added after argon filling. After tapping, the ingot is cast to obtain an ingot; the ingot is annealed to obtain an electrode for electroslag remelting; S2) electroslag remelting the electrode for electroslag remelting, wherein in a steady-state smelting stage, the melting rate is 3.5 to 5.5 kg / min and the slag resistance swing is 0.35 to 0.55 mΩ to obtain a vacuum consumable electrode; S3) remelting the vacuum consumable electrode to obtain GH4141 high-temperature alloy.

2. The preparation method according to claim 1, characterized in that In step S1), the nickel raw material is selected from electrolytic nickel plate, the chromium raw material is selected from metallic chromium, the molybdenum raw material is selected from molybdenum bar, the aluminum raw material is selected from aluminum bar, the titanium raw material is selected from metallic titanium, the boron raw material is selected from ferroboron, and the zirconium raw material is selected from sponge zirconium.

3. The preparation method according to claim 1 or 2, characterized in that In step S1), after adding the raw materials into the vacuum induction furnace, the vacuum is evacuated to a vacuum degree of ≤1Pa; and / or, after adding the remaining carbon, the temperature is adjusted to 1500-1600°C and stirred for 30-60 minutes; and / or, after adding the second batch of raw materials, the raw materials are stirred for 10-30 minutes; and / or, the argon is filled to 5000-6500Pa; and / or, the tapping temperature is 1450-1500°C.

4. The preparation method according to claim 1 or 2, characterized in that In step S1), the heating rate of the annealing is 1-1.5 min / mm, the annealing temperature is 1050-1150° C., and the annealing holding time is 10-15 h.

5. The preparation method according to claim 1 or 2, characterized in that In step S2), pre-melted slag is introduced during the electroslag remelting process. The pre-melted slag comprises, by mass percentage, 10-30% CaO, 13.5-16.5% Al2O3, 4-70% CaF2, and 2.5-3.5% TiO2. The amount of pre-melted slag added is 50-55 kg / furnace.

6. The preparation method according to claim 5, characterized in that In step S2), before the electroslag remelting, the process further includes: introducing argon gas into the crystallizer for 15 to 20 minutes; and maintaining the introduction of argon gas during the electroslag remelting process.

7. The preparation method according to claim 6, characterized in that In step S2), during the steady-state smelting stage, the slag resistance swing fluctuation is ≤±0.25mΩ; and / or, the steel ingot after electroslag remelting is furnace cooled for ≥1h before being taken out of the furnace.

8. The preparation method according to claim 7, characterized in that In step S3), before the vacuum consumable remelting, the process further includes: adjusting the vacuum degree of the vacuum consumable furnace to ≤0.1 Pa.

9. The preparation method according to claim 7, characterized in that In step S3), during the vacuum consumable remelting process, in the arc starting stage of melting, the arc starting current is 3000~5000A, and the arc starting voltage is 20.0~25.0V; and / or, in the steady-state melting stage, helium is filled, the helium pressure is 300~500Pa, and the melting rate is 2.5~5kg / min; and / or, in the hot capping stage, the melting rate is 1.2~3.5kg / min; and / or, after the vacuum consumable remelting is completed, the steel is taken out of the furnace after vacuum cooling for ≥2h.

10. The method according to any one of claims 1 to 9, characterized in that The composition of the GH4141 high-temperature alloy, calculated in percentage by mass, includes: C: 0.06-0.12%, Cr: 18.0-20.0%, Co: 10.0-12.0%, Mo: 9.50-10.50%, Al: 1.4-1.8%, Ti: 3.0-3.5%, B: 0.003-0.010%, Si≤0.5%, Mn≤0.5%, Cu≤0.5%, P≤0.015%, S≤0.015%, Fe≤5.0%, Zr≤0.07%, and the balance is Ni.

Citation Information

Patent Citations

  • Preparation method of difficult-to-deform high-temperature alloy GH4141 alloy ingot

    CN115233013A

  • GH4141 high-temperature alloy and preparation method thereof

    CN115821117A