A method for preparing a metallurgical defect of a high-temperature alloy ingot

Abstract

The present application relates to the alloy technical field, especially to a kind of preparation method of high-temperature alloy ingot metallurgical defect.The preparation method of high-temperature alloy ingot metallurgical defect of the present application includes the preparation method of high-temperature alloy ingot black spot defect and the preparation method of high-temperature alloy ingot white spot defect;By adjusting the smelting process parameters in the high-temperature alloy smelting process, black spot defect and white spot defect can be effectively pre-set in high-temperature alloy ingot;By pre-setting black spot defect and white spot defect in high-temperature alloy ingot, alloy microstructure can be changed, thereby affecting the final performance of the material, and this special alloy composition and structure can meet some special application requirements, and provide an important basis for studying the constitutive parameters of defects and optimizing the detection means.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of alloy, in particular to a preparation method of metallurgical defects of high-temperature alloy ingot. BACKGROUND

[0002] High-temperature alloys are a class of high-performance alloy materials that can work in high-temperature environments for a long time, widely used in aerospace, nuclear industry, petroleum and chemical industry, etc. These alloy materials are usually composed of nickel, chromium, titanium, aluminum, molybdenum and other elements, with good oxidation resistance, corrosion resistance and high-temperature mechanical properties. Due to its important industrial application value, the preparation technology of high-temperature alloy material has been widely concerned. In the preparation process of high-temperature alloy material, ingot metallurgy is a key link. By controlling the process parameters in the ingot metallurgy process, the microstructure of the alloy can be adjusted, thereby affecting the final performance of the material. However, due to the complex composition and special organizational structure of high-temperature alloy materials, various metallurgical defects such as segregation, grain boundary embrittlement and hot cracks may occur during the ingot metallurgy process, which will affect the mechanical properties and service life of the material.

[0003] The existing high-temperature alloy ingot preparation technology mainly includes vacuum induction melting, vacuum arc remelting, vacuum consumable electrode melting and other methods. These methods can reduce impurities and gas content in the alloy through vacuum environment and high-temperature melting, improve the purity and performance of the material. In terms of controlling the process parameters in the ingot metallurgy process, the existing technology mainly adjusts the melting temperature, holding time, cooling speed and other parameters to adjust the alloy composition and organizational structure. For example, by reducing the melting temperature and prolonging the holding time, the diffusion and homogenization of alloy elements can be promoted, thereby reducing the segregation phenomenon. Through rapid cooling, the grain boundary coarsening can be inhibited, and the toughness of the material can be improved.

[0004] However, based on the research direction of materials science, the preparation of high-temperature alloy samples containing certain defects can effectively help researchers understand the formation mechanism of defects and form effective detection and testing techniques, providing guidance for subsequent production of high-quality alloy ingots and improving the qualification rate of finished products.

[0005] Therefore, the present application is proposed. SUMMARY

[0006] The purpose of the present application is to provide a preparation method of metallurgical defects of high-temperature alloy ingot, which realizes the pre-setting of black spot defects and white spot defects in high-temperature alloy ingot by adjusting the smelting process parameters in the smelting process.

[0007] In order to achieve the above-mentioned purpose of the present application, the following technical scheme is adopted:

[0008] The application provides a preparation method of metallurgical defects of high-temperature alloy ingot, including a preparation method of black spot defects of high-temperature alloy ingot and a preparation method of white spot defects of high-temperature alloy ingot.

[0009] The preparation method of black spot defects of high-temperature alloy ingot comprises the following steps:

[0010] The high-temperature alloy raw material is subjected to vacuum induction smelting to obtain a vacuum induction smelting ingot; the vacuum induction smelting ingot is subjected to protective atmosphere electroslag remelting to obtain an electrode rod; and the electrode rod is subjected to vacuum consumable remelting to obtain a high-temperature alloy ingot containing black spot defects.

[0011] In the process of the protective atmosphere electroslag remelting, the slag resistance swing and the voltage swing are each independently 0.2-1 mOhm; and the melting rate is 2.5-8 kg / min.

[0012] In the smelting stage of the vacuum consumable remelting, the melting rate in the process from the start of smelting to 1 / 3 length of the smelting electrode rod is 3.5-7 kg / min, the melting rate in the process from 1 / 3 length of the smelting electrode rod to 2 / 3 length of the smelting electrode rod is 3-6.5 kg / min, and the melting rate in the process from 2 / 3 length of the smelting electrode rod to the end of smelting is 2.5-6 kg / min; the droplet size in the smelting stage is 1-12 mm; and helium is introduced in the smelting stage, and the pressure of the helium is 300-1000 Pa.

[0013] The preparation method of white spot defects of high-temperature alloy ingot comprises the following steps:

[0014] The high-temperature alloy raw material is subjected to vacuum induction smelting to obtain a vacuum induction smelting ingot; and the vacuum induction smelting ingot is subjected to vacuum consumable remelting to obtain a high-temperature alloy ingot containing white spot defects.

[0015] The vacuum consumable remelting comprises an arc starting stage and a smelting stage; the melting rate in the arc starting stage is 2.2-5 kg / min; in the smelting stage, the melting rate in the process from the start of smelting to 1 / 3 length of the smelting electrode rod is 1.5-3.5 kg / min, the melting rate in the process from 1 / 3 length of the smelting electrode rod to 2 / 3 length of the smelting electrode rod is 2-5.5 kg / min, and the melting rate in the process from 2 / 3 length of the smelting electrode rod to the end of smelting is 3-6 kg / min; and the droplet size in the smelting stage is 2-9 mm.

[0016] Further, the high-temperature alloy comprises GH4169 alloy.

[0017] Further, the preparation method of black spot defects of high-temperature alloy ingot comprises at least one of the following features (1) to (3):

[0018] (1) the protective atmosphere for the electroslag remelting comprises argon;

[0019] (2) the flow rate of the argon is 20-120 L / min;

[0020] (3) the amount of slag for the electroslag remelting is 20-70 Kg.

[0021] Further, the preparation method of the high-temperature alloy ingot black spot defect comprises at least one of the following features (1) to (3);

[0022] (1) the filling time for the electroslag remelting is 10-70 min;

[0023] (2) the in-furnace cooling time for the electroslag remelting is 20-80 min;

[0024] (3) the diameter of the electrode rod is 350-450 mm.

[0025] Further, the preparation method of the high-temperature alloy ingot black spot defect comprises at least one of the following features (1) to (3);

[0026] (1) in the arc starting stage of the vacuum consumable remelting, the arc starting weight is 120-220 Kg, and the arc starting melting rate is 2.2-8 Kg / min;

[0027] (2) during the vacuum consumable remelting, after the melting, the in-furnace cooling is sequentially performed for 1-4 h, the vacuum is broken, the mold is removed, and the air cooling is performed;

[0028] (3) the diameter of the high-temperature alloy ingot containing the black spot defect is 400-550 mm.

[0029] Further, in the preparation method of the high-temperature alloy ingot white spot defect, in the arc starting stage of the vacuum consumable remelting, the arc starting weight is 120-220 Kg, and the arc starting melting rate is 2.2-5 Kg / min.

[0030] Further, the preparation method of the high-temperature alloy ingot white spot defect comprises at least one of the following features (1) to (3);

[0031] (1) during the vacuum consumable remelting, the helium is introduced in the melting stage, and the pressure of the helium is 300-1000 Pa;

[0032] (2) during the vacuum consumable remelting, after the melting, the in-furnace cooling is sequentially performed for 1-4 h, the vacuum is broken, the mold is removed, and the air cooling is performed;

[0033] (3) the diameter of the high-temperature alloy ingot containing the white spot defect is 400-550 mm.

[0034] Further, the preparation method of the high-temperature alloy ingot black spot defect comprises at least one of the following features (1) to (3);

[0035] (1) the vacuum induction melting comprises sequentially performing melting, pouring, furnace cooling, breaking vacuum, mold slow cooling and demolding;

[0036] (2) the power of the vacuum induction melting is 700-1000 KW;

[0037] (3) the refining temperature of the melting is 1450-1700 DEG C.

[0038] Further, the preparation method of the high-temperature alloy ingot black spot defect comprises at least one of the following features (1) to (4);

[0039] (1) the pouring pouring nozzle diameter is 20-35 mm

[0040] (2) the time of the furnace cooling is 60-120 min;

[0041] (3) the time of the mold slow cooling is 16-36 h;

[0042] (4) the diameter of the vacuum induction melting ingot is 300-400 mm.

[0043] Further, the preparation method of the high-temperature alloy ingot white spot defect comprises at least one of the following features (1) to (7);

[0044] (1) the vacuum induction melting comprises sequentially performing melting, pouring, furnace cooling, breaking vacuum, furnace cooling, mold slow cooling and demolding;

[0045] (2) the power of the vacuum induction melting is 700-1000 KW;

[0046] (3) the refining temperature of the melting is 1450-1700 DEG C.

[0047] (4) the pouring pouring nozzle diameter is 20-35 mm;

[0048] (5) after pouring, sequentially performing furnace cooling for 15-60 min, breaking vacuum, furnace cooling for 60-120 min;

[0049] (6) the time of the mold slow cooling is 1-4 h;

[0050] (7) the diameter of the vacuum induction melting ingot is 350-500 mm.

[0051] Compared with the prior art, the present application has the following beneficial effects:

[0052] The present application can effectively preset black spot defects and white spot defects in high-temperature alloy ingots by adjusting smelting process parameters in the smelting process of high-temperature alloys such as GH4169 alloy; by presetting black spot defects and white spot defects in high-temperature alloy ingots, the microstructure of the alloy can be changed, thereby affecting the final performance of the material. This special alloy composition and structure can meet some special application requirements, and provide an important basis for studying the constitutive parameters of defects and optimizing the detection means. BRIEF DESCRIPTION OF DRAWINGS

[0053] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can also be obtained without creative labor.

[0054] Figure 1 A macrograph of the high-temperature alloy ingot containing black spot defects of the present application embodiment 1.

[0055] Figure 2 An SEM image of the black spot defects in the high-temperature alloy ingot containing black spot defects of the present application embodiment 1.

[0056] Figure 3 An SEM image of the matrix in the high-temperature alloy ingot containing black spot defects of the present application embodiment 1.

[0057] Figure 4 An EDS image of the black spot defects in the high-temperature alloy ingot containing black spot defects of the present application embodiment 1.

[0058] Figure 5 An EDS image of the matrix in the high-temperature alloy ingot containing black spot defects of the present application embodiment 1.

[0059] Figure 6 A macrograph of the high-temperature alloy ingot of the high-temperature alloy ingot containing white spot defects of the present application embodiment 4.

[0060] Figure 7 An SEM image of the white spot defects in the high-temperature alloy ingot containing white spot defects of the present application embodiment 4.

[0061] Figure 8 An SEM image of the matrix in the high-temperature alloy ingot containing white spot defects of the present application embodiment 4.

[0062] Figure 9 An EDS image of the white spot defects in the high-temperature alloy ingot containing white spot defects of the present application embodiment 4.

[0063] Figure 10 EDS map of the matrix of the high-temperature alloy ingot with white spot defects of Example 4 of the present application. DETAILED DESCRIPTION

[0064] The technical solutions of the present application will be described clearly and completely in combination with the drawings and specific embodiments, but those skilled in the art will understand that the following described embodiments are part of the embodiments of the present application, not all the embodiments, and are only used to illustrate the present application, and should not be regarded as limiting the scope of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application. The specific conditions are not specified in the embodiments, and are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not specified by the manufacturer, and are conventional products that can be purchased on the market.

[0065] The preparation method of the high-temperature alloy ingot metallurgical defects of the present application will be described in detail below.

[0066] In some embodiments of the present application, a preparation method of high-temperature alloy ingot metallurgical defects is provided, including a preparation method of high-temperature alloy ingot black spot defects and a preparation method of high-temperature alloy ingot white spot defects;

[0067] The preparation method of high-temperature alloy ingot black spot defects comprises the following steps:

[0068] The high-temperature alloy raw material is vacuum induction melted to obtain a vacuum induction melting ingot; the vacuum induction melting ingot is subjected to protective atmosphere electroslag remelting to obtain an electrode rod; the electrode rod is subjected to vacuum consumable remelting to obtain a high-temperature alloy ingot containing black spot defects;

[0069] In the process of protective atmosphere electroslag remelting, the slag resistance swing and the voltage swing are each independently 0.2-1 mOhm; the melting rate is 2.5-8 kg / min;

[0070] In the melting stage of vacuum consumable remelting, the melting rate in the process from the start of melting to 1 / 3 length of the melting electrode rod is 3.5-7 kg / min, the melting rate in the process from 1 / 3 length of the melting electrode rod to 2 / 3 length of the melting electrode rod is 3-6.5 kg / min, and the melting rate in the process from 2 / 3 length of the melting electrode rod to the end of melting is 2.5-6 kg / min; the droplet size in the melting stage is 1-12 mm; helium is introduced in the melting stage, and the pressure of the helium is 300-1000 Pa;

[0071] The preparation method of high-temperature alloy ingot white spot defects comprises the following steps:

[0072] High-temperature alloy raw materials are subjected to vacuum induction melting to obtain vacuum induction melting ingots; vacuum induction melting ingots are subjected to vacuum arc remelting to obtain high-temperature alloy ingots containing white spot defects.

[0073] Vacuum consumable remelting includes an arc initiation stage and a melting stage. The melting rate during the arc initiation stage is 2.2–5 kg / min. During the melting stage, the melting rate is 1.5–3.5 kg / min from the start of melting to 1 / 3 of the length of the melting electrode rod, 2–5.5 kg / min from 1 / 3 to 2 / 3 of the length of the melting electrode rod, and 3–6 kg / min from 2 / 3 of the length of the melting electrode rod to the end of melting. The droplet size during the melting stage is 2–9 mm.

[0074] This invention can effectively pre-introduce black spot and white spot defects in high-temperature alloy ingots by adjusting the smelting process parameters during the high-temperature alloy smelting process.

[0075] By pre-incorporating black and white spot defects into high-temperature alloy ingots, the microstructure of the alloy can be altered, thereby affecting the final properties of the material. This special alloy composition and microstructure can meet some special application requirements and provide an important foundation for studying the constitutive parameters of defects and optimizing inspection and testing methods.

[0076] In some embodiments of the present invention, the high-temperature alloy includes GH4169 alloy.

[0077] In some embodiments of the present invention, the GH4169 alloy comprises, by weight percentage, the following components:

[0078] C≤0.08%, Cr 17.00%~21.00%, Ni 50.00%~55.00%, Co≤1.00%, Mo 2.80%~3.30%, Al 0.20%~0.80%, Ti 0.65%~1.15%, Nb 4.75%~5.50%, B≤0.006%, Mg≤0.010%, Mn≤0.35%, Si≤0.35%, P≤0.015%, S≤0.015%, Cu≤0.300%, with the balance being Fe.

[0079] The preparation technology of high-temperature alloy ingot mainly adjusts the process parameters to adjust the microstructure of the alloy when preparing the high-temperature alloy ingot, but this method is limited by the alloy composition and structure to a certain extent, and it is difficult to meet some special application requirements. The present application adjusts the smelting process parameters in the smelting process of GH4169 alloy, and prepositions the black spot and white spot defects in the GH4169 alloy ingot, which provides a method and idea for the special application requirements of studying the metallurgical defects of high-temperature alloy materials.

[0080] The preparation technology of high-temperature alloy ingot mainly adjusts the process parameters to adjust the microstructure of the alloy when preparing the high-temperature alloy ingot, but this method is limited by the alloy composition and structure to a certain extent, and it is difficult to meet some special application requirements. The present application adjusts the smelting process parameters in the smelting process of GH4169 alloy, and prepositions the black spot and white spot defects in the GH4169 alloy ingot, which provides a method and idea for the special application requirements of studying the metallurgical defects of high-temperature alloy materials.

[0081] The preparation method of the high-temperature alloy ingot black spot defect of the present application adopts a triple smelting process, which includes vacuum induction melting, protective atmosphere electroslag remelting and vacuum consumable remelting in sequence.

[0082] In some embodiments of the present application, the parameters of the protective atmosphere electroslag remelting in the preparation method of the high-temperature alloy ingot black spot defect are as follows:

[0083] The protective atmosphere electroslag remelting includes: peeling or roll grinding the surface of the vacuum induction melting ingot, seeing the metal as it is, the surface is clean, no oil stains and paint, and then cutting off more than 50-300mm at the shrinkage end, and then loading into the electroslag remelting furnace for smelting, and protective gas is introduced throughout the smelting process, and after smelting, the furnace is cooled down;

[0084] The protective gas includes argon;

[0085] The flow rate of argon is 20-120L / min; typically but not limited to, for example, the flow rate of argon can be 20L / min, 40L / min, 60L / min, 80L / min, 100L / min, 120L / min or a range value formed by any two of them; preferably 20-100L / min;

[0086] The amount of slag is 20-70Kg; typically but not limited to, for example, the amount of slag can be 20Kg, 30Kg, 40Kg, 50Kg, 60Kg, 70Kg or a range value formed by any two of them; preferably 30-60Kg;

[0087] The slag resistance swing and the voltage swing are each independently 0.2-1 mOhm; typically but not limitedly, for example, the slag resistance swing and the voltage swing can each independently be 0.2 mOhm, 0.3 mOhm, 0.4 mOhm, 0.5 mOhm, 0.6 mOhm, 0.7 mOhm, 0.8 mOhm, 0.9 mOhm, 1 mOhm, or a range value formed by any two of them; preferably 0.4-0.9 mOhm;

[0088] The melting rate is 2.5-8 kg / min; typically but not limitedly, for example, the melting rate can be 2.5 kg / min, 3 kg / min, 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min, 5.5 kg / min, 6 kg / min, 6.5 kg / min, 7 kg / min, 7.5 kg / min, 8 kg / min, or a range value formed by any two of them; preferably 3-7 kg / min;

[0089] The filling time is 10-70 min; typically but not limitedly, for example, the filling time can be 10 min, 20 min, 30 min, 40 min, 50 min, 60 min, 70 min, or a range value formed by any two of them; preferably 20-60 min; the filling time refers to the time required for the consumable electrode to continuously melt and fill into the molten pool until a steel ingot of a predetermined size and shape is formed in the electroslag remelting process;

[0090] The time for in-furnace cooling is 20-80 min; typically but not limitedly, for example, the time for in-furnace cooling can be 20 min, 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, or a range value formed by any two of them; preferably 25-65 min;

[0091] The diameter of the electrode rod is 350-450 mm; typically but not limitedly, for example, the diameter of the electrode rod can be 350 mm, 360 mm, 370 mm, 380 mm, 390 mm, 400 mm, 410 mm, 420 mm, 430 mm, 440 mm, 450 mm, or a range value formed by any two of them.

[0092] In some embodiments of the present application, the parameters of the vacuum consumable remelting in the preparation method of the high-temperature alloy ingot black spot defect are as follows:

[0093] The vacuum consumable remelting includes full peeling treatment of the electrode rod using a polishing method to ensure that the surface is free of black skin, and then cutting the head of the electrode rod flat using an electric spark cutting, and then performing vacuum consumable remelting; the vacuum consumable remelting includes an arc starting stage and a melting stage in sequence;

[0094] The arc starting weight in the arc starting stage is 120-220 Kg; typically but not limitedly, for example, the arc starting weight can be 120 Kg, 130 Kg, 140 Kg, 150 Kg, 160 Kg, 170 Kg, 180 Kg, 190 Kg, 200 Kg, 210 Kg, 220 Kg or a range value formed by any two of them; preferably 140-200 Kg;

[0095] The arc starting melting speed in the arc starting stage is 2.2-8 kg / min; typically but not limitedly, for example, the arc starting melting speed can be 2.2 kg / min, 3 kg / min, 4 kg / min, 5 kg / min, 6 kg / min, 7 kg / min, 8 kg / min or a range value formed by any two of them; preferably 2.5-6.5 kg / min; the arc starting melting speed is controlled by the current plus voltage;

[0096] In the melting stage, the melting speed in the process from the start of melting to the 1 / 3 length of the melting electrode rod is 3.5-7 kg / min (for example, it can be 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min, 5.5 kg / min, 6 kg / min, 6.5 kg / min, 7 kg / min, etc.), the melting speed in the process from the 1 / 3 length to the 2 / 3 length of the melting electrode rod is 3-6.5 kg / min (for example, it can be 3 kg / min, 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min, 5.5 kg / min, 6 kg / min, 6.5 kg / min, etc.), and the melting speed in the process from the 2 / 3 length to the end of melting is 2.5-6 kg / min (for example, it can be 2.5 kg / min, 3 kg / min, 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min, 5.5 kg / min, 6 kg / min, etc.); in the melting stage, the 1 / 3 length of the electrode rod at the start of melting is controlled at a melting speed of 3.5-7 kg / min, the middle 1 / 3 length is controlled at a melting speed of 3-6.5 kg / min, and the remaining 1 / 3 length is controlled at a melting speed of 2.5-6 kg / min; preferably, the 1 / 3 length of the electrode rod at the start of melting is controlled at a melting speed of 4-6.5 kg / min, the middle 1 / 3 length is controlled at a melting speed of 3-6 kg / min, and the remaining 1 / 3 length is controlled at a melting speed of 2.5-5.5 kg / min;

[0097] The droplet size in the melting stage (the whole process) is 1-12 mm; typically but not limitedly, for example, the droplet size can be 1 mm, 2 mm, 4 mm, 6 mm, 8 mm, 10 mm, 12 mm or a range value formed by any two of them; preferably 1.5-11 mm;

[0098] Helium is introduced during the melting stage, and the pressure of the helium is 300-1000 Pa; typically but not limitatively, for example, the pressure of the helium can be 300 Pa, 400 Pa, 500 Pa, 600 Pa, 700 Pa, 800 Pa, 900 Pa, 1000 Pa, or a range value formed by any two of them; preferably 300-700 Pa; helium is introduced during the whole melting process for cooling; the introduction of helium during the melting stage means that after the melting process reaches a stable state and various parameters such as current, voltage, melting rate, etc. are kept relatively stable, helium is introduced, and the role of the introduction of helium is to adjust the temperature of the consumable electrode to prevent overheating of the electrode; an overheated electrode can cause problems such as a decrease in material performance and excessive consumption of the electrode, while the introduction of helium can effectively take away part of the heat to maintain the electrode within a suitable temperature range, prolong the service life of the electrode, and at the same time help improve the melting efficiency;

[0099] After melting, the furnace cooling is performed for 1-4 h, the vacuum is broken, the mold is removed, and the air cooling is performed; typically but not limitatively, for example, the time of the furnace cooling can be 1 h, 2 h, 3 h, 4 h, or a range value formed by any two of them; preferably 1.5-3.5 h;

[0100] The diameter of the high-temperature alloy ingot containing black spot defects is 400-550 mm; typically but not limitatively, for example, the diameter of the high-temperature alloy ingot containing black spot defects can be 400 mm, 420 mm, 440 mm, 460 mm, 480 mm, 500 mm, 520 mm, 540 mm, 550 mm, or a range value formed by any two of them.

[0101] The main factors affecting the generation of black spot defects include the melting speed and the cooling rate of the formed ingot during the electroslag remelting process and the vacuum consumable remelting process. The present application controls the generation of black spot defects by controlling the melting speed of the vacuum consumable remelting, the cooling rate of the ingot, and other parameter settings; wherein a high melting speed means a high production rate, also means a deeper mushy zone and a stronger fluid flow between dendrites, which can lead to the formation of black spots; when the cooling rate of the ingot decreases, the local solidification time increases, the depth of the mushy zone of the ingot will become deeper, and the dendrite density inversion phenomenon will be enhanced, resulting in more black spot defects.

[0102] In some embodiments of the present application, the parameters of the vacuum induction melting in the preparation method of the high-temperature alloy ingot black spot defect are as follows:

[0103] The vacuum induction melting includes: sequentially performing melting, pouring, furnace cooling, vacuum breaking, mold slow cooling, and mold removal; preferably, the pouring is performed in a vacuum environment;

[0104] The power of the vacuum induction melting is 700-1000KW; typically but not exclusively, for example, the power of the vacuum induction melting can be 700KW, 750KW, 800KW, 850KW, 900KW, 950KW, 1000KW or a range value formed by any two of them; preferably 800-950KW;

[0105] The refining temperature of the melting is 1450-1700℃; typically but not exclusively, for example, the refining temperature of the melting can be 1450℃, 1500℃, 1550℃, 1600℃, 1650℃, 1700℃ or a range value formed by any two of them; preferably 1450-1600℃;

[0106] The pouring pouring nozzle diameter is 20-35mm; typically but not exclusively, for example, the pouring pouring nozzle diameter can be 20mm, 22mm, 24mm, 26mm, 28mm, 30mm, 32mm, 35mm or a range value formed by any two of them; preferably 23-33mm;

[0107] The time of the in-furnace cooling is 60-120min; typically but not exclusively, for example, the time of the in-furnace cooling can be 60min, 70min, 80min, 90min, 100min, 110min, 120min or a range value formed by any two of them; preferably 75-110min;

[0108] The time of the mold slow cooling is 16-36h; typically but not exclusively, for example, the time of the mold slow cooling can be 16h, 18h, 20h, 22h, 24h, 26h, 28h, 30h, 32h, 34h, 36h or a range value formed by any two of them; preferably 18-30h;

[0109] The diameter of the vacuum induction melting ingot is 300-400mm; typically but not exclusively, for example, the diameter of the vacuum induction melting ingot can be 300mm, 320mm, 340mm, 360mm, 380mm, 400mm or a range value formed by any two of them.

[0110] The preparation method of the white spot defect of the high-temperature alloy ingot of the application adopts a double-melting process, and sequentially includes vacuum induction melting and vacuum consumable remelting.

[0111] In some embodiments of the application, the parameters of the vacuum consumable remelting in the preparation method of the white spot defect of the high-temperature alloy ingot are as follows:

[0112] The vacuum self-consumption remelting includes: using polishing method to perform full skinning treatment on the vacuum induction melting ingot, ensuring that the surface is free of black skin, cutting off 50-300 mm from the riser end of the vacuum induction melting ingot by using a sawing machine or a wire cutting machine, and then performing vacuum self-consumption remelting;

[0113] The starting arc weight in the starting arc stage is 120-220 Kg, and typically but not limitatively, for example, the starting arc weight can be 120 Kg, 130 Kg, 140 Kg, 150 Kg, 160 Kg, 170 Kg, 180 Kg, 190 Kg, 200 Kg, 210 Kg, 220 Kg or a range value formed by any two of them; preferably 130-200 Kg;

[0114] The starting arc melting speed in the starting arc stage is 2.5-5 kg / min; typically but not limitatively, for example, the starting arc melting speed can be 2.5 kg / min, 3 kg / min, 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min or a range value formed by any two of them; preferably 2.5-4.5 kg / min; the starting arc melting speed is controlled by using current plus voltage;

[0115] In the melting stage, the melting speed in the process from the start of melting to 1 / 3 length of the melting electrode rod is 2.2-5 kg / min (for example, it can be 2.2 kg / min, 2.5 kg / min, 3 kg / min, 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min, etc.), the melting speed in the process from 1 / 3 length to 2 / 3 length of the melting electrode rod is 1.5-3.5 kg / min (for example, it can be 1.5 kg / min, 2 kg / min, 2.5 kg / min, 3 kg / min, etc.), and the melting speed in the process from 2 / 3 length to the end of melting is 3-6 kg / min (for example, it can be 3 kg / min, 3.5 kg / min, 4 kg / min, 4.5 kg / min, 5 kg / min, 5.5 kg / min, 6 kg / min, etc.); in the melting stage, the melting speed in the 1 / 3 length at the start of the electrode rod melting is controlled to be between 2.2-5 kg / min, the melting speed in the middle 1 / 3 length is controlled to be between 1.5-3.5 kg / min, and the melting speed in the remaining 1 / 3 length is controlled to be between 3-6 kg / min; preferably, the melting speed in the 1 / 3 length at the start of the electrode rod melting is controlled to be between 1.75-3.5 kg / min, the melting speed in the middle 1 / 3 length is controlled to be between 2.5-5 kg / min, and the melting speed in the remaining 1 / 3 length is controlled to be between 3.5-5.5 kg / min;

[0116] The size of the molten droplet in the melting stage (the whole process) is 2-9 mm; typically but not limitatively, for example, the size of the molten droplet can be 2 mm, 3 mm, 4 mm, 5 mm, 6 mm, 7 mm, 8 mm, 9 mm or a range value formed by any two of them;

[0117] Helium is introduced into the melting stage, and the pressure of the helium is 300-1000 Pa; typically but not limitatively, for example, the pressure of the helium can be 300 Pa, 400 Pa, 500 Pa, 600 Pa, 700 Pa, 800 Pa, 900 Pa, 1000 Pa or a range value formed by any two of them; preferably, 400-800 Pa; helium is introduced into the melting stage for cooling; the introduction of helium into the melting stage refers to that after the melting process reaches a stable state, various parameters such as current, voltage, melting rate and the like are kept relatively stable, and then the helium is introduced;

[0118] After melting, the following steps are performed in sequence: in-furnace cooling for 1-4 h, breaking of the vacuum, demolding and air cooling; typically but not limitatively, for example, the time of in-furnace cooling can be 1 h, 2 h, 3 h, 4 h or a range value formed by any two of them; preferably, 1.5-3.5 h;

[0119] The diameter of the high-temperature alloy ingot containing the white spot defect is 400-550 mm; typically but not limitatively, for example, the diameter of the high-temperature alloy ingot containing the white spot defect can be 400 mm, 420 mm, 440 mm, 460 mm, 480 mm, 500 mm, 520 mm, 540 mm, 550 mm or a range value formed by any two of them.

[0120] The main factors affecting the generation of the white spot defect include the quality of the electrode in the vacuum consumable remelting process, the unstable voltage caused by the melting condition to cause the fluctuation of the melting rate and the filling amount of the helium. When there is a shrinkage cavity in the electrode, the melting process will cause the arc to be unstable, the normal melting of the electrode is affected and the electrode shedding is prone to falling into the molten pool to form dendritic white spots. Therefore, the parameters of the vacuum induction melting process are regulated and controlled in order to regulate the quality of the electrode rod. When the melting rate fluctuates, the depth of the ingot molten pool is reduced, the exogenous substances are prone to falling into the molten pool and are not easy to melt, and the white spots are prone to be formed. Therefore, the arc starting melting rate in the vacuum consumable remelting process and the melting rate in the melting stage are regulated and controlled.

[0121] In some embodiments of the present application, the parameters of the vacuum induction melting in the preparation method of the high-temperature alloy ingot white spot defect are as follows:

[0122] The vacuum induction melting comprises the following steps performed in sequence: melting, pouring, in-furnace cooling, breaking of the vacuum, in-furnace cooling, mold slow cooling and demolding; preferably, the pouring is performed in a vacuum environment;

[0123] The power of the vacuum induction melting is 700-1000KW; typically but not exclusively, for example, the power of the vacuum induction melting can be 700KW, 750KW, 800KW, 850KW, 900KW, 950KW, 1000KW or a range value formed by any two of them; preferably 800-950KW;

[0124] The refining temperature of the melting is 1450-1700℃; typically but not exclusively, for example, the refining temperature of the melting can be 1450℃, 1500℃, 1550℃, 1600℃, 1650℃, 1700℃ or a range value formed by any two of them; preferably 1450-1600℃;

[0125] The pouring pouring nozzle diameter is 20-35mm; typically but not exclusively, for example, the pouring pouring nozzle diameter can be 20mm, 22mm, 24mm, 26mm, 28mm, 30mm, 32mm, 35mm or a range value formed by any two of them; preferably 23-33mm;

[0126] Breaking the vacuum refers to breaking the vacuum environment and reducing the vacuum degree;

[0127] The time of the furnace cooling before breaking the vacuum is 15-60min; typically but not exclusively, for example, the time of the furnace cooling before breaking the vacuum can be 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min or a range value formed by any two of them; preferably 20-50min;

[0128] The time of the furnace cooling after breaking the vacuum is 60-120min; typically but not exclusively, for example, the time of the furnace cooling after breaking the vacuum can be 60min, 70min, 80min, 90min, 100min, 110min, 120min or a range value formed by any two of them; preferably 80-100min;

[0129] The time of the mold slow cooling is 1-4h; typically but not exclusively, for example, the time of the mold slow cooling can be 1h, 2h, 3h, 4h or a range value formed by any two of them; preferably 1.5-3.5h;

[0130] The diameter of the vacuum induction melting ingot is 350-500mm; typically but not exclusively, for example, the diameter of the vacuum induction melting ingot can be 350mm, 380mm, 400mm, 420mm, 440mm, 460mm, 480mm, 500mm or a range value formed by any two of them.

[0131] The present application can successfully preset black spot defects and white spot defects in GH4169 alloy ingots by adjusting the smelting process parameters in the smelting process of GH4169 alloy, and this purposeful metallurgical defect presetting can provide more data support and theoretical basis for subsequent research and application. For example, in the field of aerospace, by systematically studying the defects preset in the high-temperature alloy ingot, the failure mechanism of the high-temperature alloy material can be deeply understood, thereby providing guidance for the development and application of the high-temperature alloy material.

[0132] Embodiment 1

[0133] The preparation method of the black spot defect of the GH4169 alloy ingot provided in the embodiment comprises the following steps:

[0134] S1, vacuum induction melting of GH4169 alloy raw materials is carried out to obtain a vacuum induction melting ingot; the vacuum induction melting comprises: after adding the GH4169 alloy raw materials, starting to melt by power supply, the power is 1000KW, and the refining temperature is 1550℃; then pouring is carried out in a vacuum environment, the pouring nozzle diameter Φ is 27mm, after pouring, furnace cooling is carried out for 25min, then vacuum breaking is carried out, after vacuum breaking, mold slow cooling is carried out for 3.5h, then demolding is carried out, and a vacuum induction melting ingot with a diameter Φ of 360mm is obtained;

[0135] S2, the vacuum induction melting ingot is subjected to protective atmosphere electroslag remelting to obtain an electrode rod; the protective atmosphere electroslag remelting comprises: the surface of the vacuum induction melting ingot is scaled or rolled and polished to see the metal color, the surface is clean without oil stains and paint, and the shrinkage end is cut off by more than 70-200mm, then the vacuum induction melting ingot is loaded into an electroslag remelting furnace for melting, argon is filled throughout the melting process, the argon flow is 60L / min, the slag amount is 45Kg, the slag resistance swing and the voltage swing are both 0.6mOhm, the melting speed is 3kg / min, the filling time is 20-60min, after melting, furnace cooling is carried out for 45min, and an electrode rod with a diameter Φ of 430mm is obtained;

[0136] S3, vacuum consumable remelting the electrode rod to obtain a high-temperature alloy ingot containing black spot defects; the vacuum consumable remelting comprises: performing full skinning treatment on the electrode rod in a polishing manner to ensure that the surface is free of black skin, and then cutting the head of the electrode rod flat using an electric spark cutting, and then performing vacuum consumable remelting; the vacuum consumable remelting comprises an arc striking stage and a melting stage in sequence; in the arc striking stage, the arc striking weight is 170 Kg, and the arc striking speed is controlled to be 6.5 Kg / min using a current plus voltage mode; in the melting stage, the electrode rod is melted for the first 1 / 3 length, the melting speed is 5.75 Kg / min, the melting speed for the middle 1 / 3 length is 5.25 Kg / min, and the melting speed for the remaining 1 / 3 length is 4.75 Kg / min, the whole process molten droplet size is 7 mm, and when the melting process reaches a stable state, helium gas is introduced for cooling, and the pressure of the helium gas is 600 Pa; after melting, the furnace is cooled for 2 h, and then broken, demolded and cooled in air in sequence to obtain a high-temperature alloy ingot containing black spot defects with a diameter Φ of 508 mm.

[0137] A macrograph of the high-temperature alloy ingot containing black spot defects is shown in Figure 1 , Figure 1 wherein a is a macrograph of the high-temperature alloy ingot containing black spot defects, Figure 1 wherein b is another macrograph of the high-temperature alloy ingot containing black spot defects; it can be seen from Figure 1 that the heart and the outer edge of the ingot both appear in the form of black spot defects in patches of different sizes. Microstructure characterization of a certain black spot defect and the matrix in the high-temperature alloy ingot containing black spot defects is shown in Figure 2 , Figure 3 and Figure 4 , Figure 5 it can be seen from Figure 2 , Figure 3 , Figure 4 and Figure 5 that the Nb content in the black spot defect of the GH4169 alloy is 8.1wt%, which is higher than the Nb content in the matrix of the GH4169 alloy (5wt%), and because of the increase in the Nb content, a large number of strengthening phases appear at the grain boundaries, and because of the grain boundary pinning effect of the strengthening phases, the grain size at the black spot position is significantly smaller than the grain size at the matrix position.

[0138] Example 2

[0139] The preparation method of the black spot defect of the GH4169 alloy ingot provided in this embodiment comprises the following steps:

[0140] S1, the GH4169 alloy raw material is vacuum induction melted to obtain a vacuum induction melted ingot; the vacuum induction melting includes: after the GH4169 alloy raw material is added, power is turned on to melt, the power is 700KW, and the refining temperature is 1450 DEG C; then pouring is carried out in a vacuum environment, the pouring nozzle diameter Φ is 23mm, after pouring, the furnace is cooled for 75min, then broken, the mold is slowly cooled for 18h after breaking, and then demoulding is carried out, to obtain a vacuum induction melted ingot with a diameter Φ of 300mm;

[0141] S2, the vacuum induction melted ingot is protected atmosphere electroslag remelted to obtain an electrode rod; the protected atmosphere electroslag remelting includes: the surface of the vacuum induction melted ingot is scaled or roll-milled, the metal is exposed, the surface is clean, there is no oil stain and paint, and then more than 70-200mm of the shrinkage hole end is cut off, then the electroslag remelting furnace is loaded to melt, argon is filled throughout the melting process, the argon flow is 20L / min, the slag amount is 30Kg, the slag resistance swing and the voltage swing are both 0.4mOhm, the melting speed is 3kg / min, the filling time is 20-60min, the furnace is cooled for 25min after melting, and the electrode rod with a diameter Φ of 400mm is obtained;

[0142] S3, the electrode rod is vacuum consumable remelted to obtain a high-temperature alloy ingot containing black spot defects; the vacuum consumable remelting includes: the electrode rod is fully scaled by using polishing, so that the surface is free of black skin, and then the electrode rod head is cut flat by using electric spark cutting, and then vacuum consumable remelting is carried out; the vacuum consumable remelting includes an arc starting stage and a melting stage in sequence; in the arc starting stage, the arc starting weight is 120Kg, the arc starting melting speed is 2.2kg / min by using the current plus voltage control mode; in the melting stage, the electrode rod is melted for the first 1 / 3 length, the melting speed is 3.5kg / min, the melting speed of the middle 1 / 3 length is 3 / min, and the melting speed of the remaining 1 / 3 length is 2.5kg / min, the whole process is 1mm, and when the melting process reaches a stable state, helium is introduced for cooling, and the pressure of the helium is 300Pa; after melting, the furnace is cooled for 1h, then broken, demoulded, and cooled in air in sequence, to obtain a high-temperature alloy ingot containing black spot defects with a diameter Φ of 400mm.

[0143] Example 3

[0144] The GH4169 alloy ingot black spot defect preparation method provided in the embodiment includes the following steps:

[0145] S1, the GH4169 alloy raw material is vacuum induction melted, and a vacuum induction melted ingot is obtained; the vacuum induction melting includes: after the GH4169 alloy raw material is added, power is turned on to melt, the power is 1000KW, and the refining temperature is 1700 DEG C; then pouring is carried out in a vacuum environment, the pouring nozzle diameter Φ is 35mm, after pouring, the furnace is cooled for 120min, then the vacuum is broken, after the vacuum is broken, the mold is slowly cooled for 36h, then the mold is demoulded, and a vacuum induction melted ingot with a diameter Φ of 400mm is obtained;

[0146] S2, the vacuum induction melted ingot is protected atmosphere electroslag remelted, and an electrode rod is obtained; the protected atmosphere electroslag remelting includes: the surface of the vacuum induction melted ingot is scaled or rolled and polished, the metal is exposed, the surface is clean, there is no oil stain and paint, and then more than 70-200mm of the shrinkage end is cut off, then the electroslag remelting furnace is loaded for melting, argon is filled throughout the melting process, the argon flow is 120L / min, the slag amount is 70Kg, the slag resistance swing and the voltage swing are both 1mOhm, the melting speed is 3kg / min, the filling time is 20-60min, the furnace is cooled for 80min after melting, and an electrode rod with a diameter Φ of 550mm is obtained;

[0147] S3, the electrode rod is vacuum consumable remelted, and a high-temperature alloy ingot containing black spot defects is obtained; the vacuum consumable remelting includes: the electrode rod is fully scaled by using polishing, so that the surface is free of black skin, and then the electrode rod head is cut flat by using electric spark cutting, and then vacuum consumable remelting is carried out; the vacuum consumable remelting includes an arc starting stage and a melting stage in sequence; in the arc starting stage, the arc starting weight is 220Kg, the arc starting melting speed is 8kg / min by using the current plus voltage control mode; in the melting stage, the electrode rod is melted for the first 1 / 3 length, the melting speed is 7kg / min, the melting speed of the middle 1 / 3 length is 6.5 / min, and the melting speed of the remaining 1 / 3 length is 6kg / min, the whole process is 12mm, and when the melting process reaches a stable state, helium is introduced for cooling, and the pressure of the helium is 1000Pa; after melting, the furnace is cooled for 4h, then the vacuum is broken, the mold is demoulded, and air cooling is carried out in sequence, and a high-temperature alloy ingot containing black spot defects with a diameter Φ of 550mm is obtained.

[0148] Example 4

[0149] The GH4169 alloy ingot white spot defect preparation method provided in the embodiment includes the following steps:

[0150] S1, vacuum induction melting of GH4169 alloy raw materials to obtain vacuum induction melting ingot; vacuum induction melting includes: after adding GH4169 alloy raw materials, start power melting, power is 1000KW, refining temperature is 1550℃; then pouring in vacuum environment, pouring nozzle diameter Φ is 27mm, after pouring, furnace cooling for 25min, then breaking vacuum, after breaking vacuum, furnace cooling for 1.5min, then slow cooling with mold for 2h, then demolding, obtaining vacuum induction melting ingot with diameter Φ of 360mm;

[0151] S2, vacuum consumable remelting of vacuum induction melting ingot to obtain high-temperature alloy ingot containing white spot defects; vacuum consumable remelting includes: using polishing method to fully skin treatment of vacuum induction melting ingot, ensuring that the surface is free of black skin, cutting off 100-250mm of the ingot end of the vacuum induction melting ingot by sawing or wire cutting, then vacuum consumable remelting; vacuum consumable remelting includes arc starting stage and melting stage in turn; in the arc starting stage, the arc starting weight is 170Kg, the arc starting melting speed is controlled to be 4.2kg / min by using current plus voltage; in the melting stage, the first 1 / 3 length of the electrode rod is melted, the melting speed is 3.25kg / min, the melting speed of the middle 1 / 3 length is 3.75 / min, and the melting speed of the remaining 1 / 3 length is 4.25kg / min, the whole process of melting droplet size is 4, helium gas is introduced for cooling when the melting process reaches a stable state, the pressure of helium gas is 600Pa; after melting, furnace cooling for 2h, then breaking vacuum, demolding, and cooling in air in turn, obtaining high-temperature alloy ingot containing white spot defects with diameter Φ of 440mm.

[0152] The macro photograph of the high-temperature alloy ingot containing white spot defects is shown in Figure 6 , Figure 5 wherein a is the macro photograph of the high-temperature alloy ingot containing white spot defects, Figure 5 wherein b is another macro photograph of the high-temperature alloy ingot containing white spot defects; it can be seen from Figure 5 that single sheet large size white spot defects and white spot defects of different sizes scattered on the macro photograph appear in the core and outer edge of the ingot. By microstructure characterization of a certain white spot defect and microstructure characterization of a certain black spot defect and matrix in the high-temperature alloy ingot containing white spot defects, the results are shown in Figure 7 , Figure 8 , Figure 9 and Figure 10 ; from Figure 7 , Figure 8 Figure 9 and Figure 10It can be seen that the Nb content in the white spot defect of the GH4169 alloy is 4.3wt%, which is lower than the Nb content in the GH4169 alloy matrix (5.5wt%). Because the white spot defect area contains a lower Nb content, the amount of strengthening phase precipitated at the grain boundary is less, the pinning effect is weak, and the grain size of the white spot defect area is obviously larger than that of the bulk area.

[0153] Example 5

[0154] The preparation method of the white spot defect of the GH4169 alloy ingot provided in the embodiment comprises the following steps:

[0155] S1, the GH4169 alloy raw material is vacuum induction melted to obtain a vacuum induction melted ingot; the vacuum induction melting comprises: after adding the GH4169 alloy raw material, starting to melt by power supply, the power is 700KW, and the refining temperature is 1550℃; then pouring in a vacuum environment, the pouring nozzle diameter Φ is 20mm, after pouring, furnace cooling for 15min, then breaking the vacuum, after breaking the vacuum, furnace cooling for 60min, then mold slow cooling for 1h, then demolding, to obtain a vacuum induction melted ingot with a diameter Φ of 350mm;

[0156] S2, the vacuum induction melted ingot is vacuum consumable remelted to obtain a high-temperature alloy ingot containing a white spot defect; the vacuum consumable remelting comprises: using the polishing method to fully skin the vacuum induction melted ingot to ensure that the surface is free of black skin, the riser end of the vacuum induction melted ingot is cut off by 100-250mm using a sawing machine or a wire cutting machine, and then vacuum consumable remelting; the vacuum consumable remelting comprises an arc striking stage and a melting stage in sequence; in the arc striking stage, the arc striking weight is 120Kg, the arc striking melting speed is controlled to be 2.2kg / min using the current plus voltage method; in the melting stage, the first 1 / 3 length of the electrode rod is melted, the melting speed is 1.5kg / min, the melting speed of the middle 1 / 3 length is 2 / min, and the melting speed of the remaining 1 / 3 length is 3kg / min, the whole process melting droplet size is 2, and when the melting process reaches a stable state, helium gas is introduced for cooling, and the pressure of the helium gas is 300Pa; after melting, the furnace is cooled for 1h, then broken, demolded and cooled in air in sequence, to obtain a high-temperature alloy ingot containing a white spot defect with a diameter Φ of 400mm.

[0157] Example 6

[0158] The preparation method of the white spot defect of the GH4169 alloy ingot provided in the embodiment comprises the following steps:

[0159] S1, the GH4169 alloy raw material is vacuum induction melted to obtain a vacuum induction melted ingot; the vacuum induction melting comprises: after the GH4169 alloy raw material is added, power is turned on to melt, the power is 1000KW, and the refining temperature is 1700 DEG C; then pouring is carried out in a vacuum environment, the pouring nozzle diameter Φ is 35mm, after pouring, the furnace is cooled for 60min, then vacuum breaking is carried out, after vacuum breaking, the furnace is cooled for 120min, then the mold is slowly cooled for 4h, and then demolding is carried out, to obtain a vacuum induction melted ingot with a diameter Φ of 500mm;

[0160] S2, the vacuum induction melted ingot is vacuum self-consumption remelted to obtain a high-temperature alloy ingot containing white spot defects; the vacuum self-consumption remelting comprises: the vacuum induction melted ingot is fully skinned by using polishing, so that the surface is free of black skin, the ingot end of the vacuum induction melted ingot is cut off by 100-250mm by using a sawing machine or a wire cutting machine, and then vacuum self-consumption remelting is carried out; the vacuum self-consumption remelting comprises an arc striking stage and a melting stage in sequence; in the arc striking stage, the arc striking weight is 220Kg, the arc striking melting speed is controlled to be 3.5kg / min by using current and voltage; in the melting stage, the electrode rod is melted at the first 1 / 3 length, the melting speed is 3.5kg / min, the melting speed is 5.5 / min at the middle 1 / 3 length, and the melting speed is 6kg / min at the remaining 1 / 3 length, the whole process droplet size is 9mm, helium is introduced to cool in the stable state of the melting process, the pressure of the helium is 1000Pa; after melting, the furnace is cooled for 4h, then vacuum breaking, demolding and air cooling are carried out in sequence, to obtain a high-temperature alloy ingot containing white spot defects with a diameter Φ of 500mm.

[0161] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing metallurgical defects in high-temperature alloy ingots, characterized in that, This includes methods for preparing black spot defects and white spot defects in high-temperature alloy ingots; The method for preparing the black spot defect in the high-temperature alloy ingot includes the following steps: High-temperature alloy raw materials are subjected to vacuum induction melting to obtain vacuum induction melting ingots; the vacuum induction melting ingots are subjected to protective atmosphere electroslag remelting to obtain electrode rods; the electrode rods are subjected to vacuum arc remelting to obtain high-temperature alloy ingots containing black spot defects. During the protective atmosphere electroslag remelting process, the slag resistance sway and voltage sway are each independently 0.2~1 mOhm; the melting rate is 2.5~8 kg / min. In the vacuum self-consumable remelting process, the melting rate during the melting stage is 3.5~7 kg / min from the start of melting to 1 / 3 of the length of the melting electrode rod, 3~6.5 kg / min from 1 / 3 to 2 / 3 of the length of the melting electrode rod, and 2.5~6 kg / min from 2 / 3 of the length of the melting electrode rod to the end of melting; the droplet size during the melting stage is 1~12 mm; helium gas is introduced during the melting stage at a pressure of 300~1000 Pa; The method for preparing white spot defects in the high-temperature alloy ingot includes the following steps: High-temperature alloy raw materials are subjected to vacuum induction melting to obtain vacuum induction melting ingots; the vacuum induction melting ingots are subjected to vacuum consumable remelting to obtain high-temperature alloy ingots containing white spot defects. The vacuum consumable remelting includes an arc initiation stage and a melting stage; the melting rate during the arc initiation stage is 2.2~5 kg / min; during the melting stage, the melting rate is 1.5~3.5 kg / min from the start of melting to 1 / 3 of the length of the electrode rod, 2~5.5 kg / min from 1 / 3 to 2 / 3 of the length of the electrode rod, and 3~6 kg / min from 2 / 3 of the length of the electrode rod to the end of melting; the droplet size during the melting stage is 2~9 mm. The high-temperature alloy includes GH4169 alloy.

2. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 1, characterized in that, The method for preparing the black spot defect in the high-temperature alloy ingot includes at least one of the following features (1) to (3); (1) The protective gas for the protective atmosphere electroslag remelting includes argon; (2) The flow rate of the argon gas is 20~120 L / min; (3) The amount of slag in the protective atmosphere electroslag remelting is 20~70Kg.

3. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 2, characterized in that, The method for preparing the black spot defect in the high-temperature alloy ingot includes at least one of the following features (1) to (3); (1) The filling time for the protective atmosphere electroslag remelting is 10~70 min; (2) The furnace cooling time for the protective atmosphere electroslag remelting is 20~80 min; (3) The diameter of the electrode rod is 350~450mm.

4. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 1, characterized in that, The method for preparing the black spot defect in the high-temperature alloy ingot includes at least one of the following features (1) to (3); (1) In the arc-starting stage of the vacuum self-consumable remelting, the arc-starting weight is 120~220Kg and the arc-starting melting rate is 2.2~8kg / min; (2) In the vacuum consumable remelting process, after melting, the furnace is cooled for 1-4 hours, the vacuum is broken, the mold is removed and the air is cooled in sequence; (3) The diameter of the high-temperature alloy ingot containing black spot defects is 400~550mm.

5. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 1, characterized in that, In the method for preparing white spot defects in high-temperature alloy ingots, the arc-starting stage of the vacuum self-consuming remelting process has an arc-starting weight of 120~220Kg and an arc-starting melting rate of 2.2~5kg / min.

6. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 5, characterized in that, The method for preparing white spot defects in the high-temperature alloy ingot includes at least one of the following features (1) to (3); (1) During the vacuum self-consumable remelting process, helium gas is introduced during the smelting stage, and the pressure of the helium gas is 300~1000Pa; (2) In the vacuum consumable remelting process, after melting, the furnace is cooled for 1-4 hours, the vacuum is broken, the mold is removed and the air is cooled in sequence; (3) The diameter of the high-temperature alloy ingot containing white spot defects is 400~550mm.

7. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 1, characterized in that, The method for preparing the black spot defect in the high-temperature alloy ingot includes at least one of the following features (1) to (3); (1) The vacuum induction melting process includes: melting, casting, furnace cooling, void breaking, slow cooling with mold and demolding in sequence; (2) The power of the vacuum induction melting is 700~1000KW; (3) The refining temperature of the smelting is 1450~1700℃.

8. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 7, characterized in that, The method for preparing the black spot defect in the high-temperature alloy ingot includes at least one of the following features (1) to (4); (1) The diameter of the pouring nozzle is 20~35mm; (2) The furnace cooling time is 60~120 min; (3) The slow cooling time of the mold belt is 16~36h; (4) The diameter of the vacuum induction melting ingot is 300~400mm.

9. The method for preparing metallurgical defects in high-temperature alloy ingots according to claim 1, characterized in that, The method for preparing white spot defects in the high-temperature alloy ingot includes at least one of the following features (1) to (7); (1) The vacuum induction melting process includes: melting, casting, furnace cooling, void breaking, furnace cooling, slow cooling with mold and demolding in sequence; (2) The power of the vacuum induction melting is 700~1000KW; (3) The refining temperature of the smelting is 1450~1700℃; (4) The diameter of the pouring nozzle is 20~35mm; (5) After casting, the furnace is cooled for 15-60 minutes, the void is broken, and the furnace is cooled for 60-120 minutes in sequence; (6) The slow cooling time of the mold belt is 1~4h; (7) The diameter of the vacuum induction melting ingot is 350~500mm.

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