CN114480919B - Manufacturing method of high-strength nickel-based high-temperature alloy cold-drawn material - Google Patents
Manufacturing method of high-strength nickel-based high-temperature alloy cold-drawn material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract
The invention discloses a manufacturing method of a high-strength nickel-based high-temperature alloy cold-drawn material, which achieves the technical index required by a high-strength fastener through the optimization control of a full-flow process. The method mainly comprises the steps of carrying out high-temperature homogenization diffusion annealing treatment on a consumable ingot and a forged intermediate blank twice, eliminating component segregation, carrying out temperature reduction forging on the forging by fire, ensuring the uniform structure of the blank, carrying out 20-25% cold drawing and large deformation on the hot-rolled and cogging bar, improving the structural uniformity from the center to the edge of the 1500MPa high-strength GH4169 alloy cold-drawn bar, and realizing the optimal matching of the strength and the plasticity of the cold-drawn bar. The invention has the following effects: (1) the grain size grade is improved from 6 grade to 8 grade of common cold-drawn materials, and the grain structure from the center to the edge of the material is finer and more uniform; (2) the tensile strength at room temperature is improved by 300MPa compared with the common cold-drawn material; (3) the cold drawing has large deformation amount, thereby not only ensuring the full and uniform deformation from the center to the edge of the bar, but also ensuring the best strong plasticity matching of the room temperature performance of the bar.
Description
Technical Field
The invention belongs to the field of nickel-based high-temperature alloy manufacturing, and particularly relates to a manufacturing method of a high-strength nickel-based high-temperature alloy cold-drawn material, which is a manufacturing method of a 1500 MPa-grade nickel-based high-temperature alloy GH4169 fastener material.
Technical Field
The GH4169 deformation high-temperature alloy for the fastener has higher tensile strength, yield strength, durability and creep strength, high notch sensitivity resistance and better ductility and toughness at the temperature of between 253 ℃ below zero and 650 ℃, has excellent comprehensive performances such as corrosion resistance, irradiation resistance, welding performance and the like, and is a high-strength bearing bolt, nut and other fasteners processed by the GH4169 alloy for various aviation and aerospace equipment. The strength of the GH4169 alloy cold-drawn material stably produced in batches at early stage is not less than 1300MPa, and can actually reach 1350 MPa-1450 MPa, and with the rapid development of high-end industries such as domestic aviation and aerospace, GH4169 alloy fasteners with the strength of 1515 MPa-1725 MPa are urgently needed. In the past, due to factors such as drawing capability of a cold drawing machine, improper surface lubrication, low strength of a drawing die and the like, the strength of a bar needs to be improved by a method of multiple solid solution softening and multiple drawing for increasing cold drawing deformation, so that the cold-drawn bar is poor in structural uniformity, low in working efficiency and poor in batch stability.
Disclosure of Invention
The invention discloses a manufacturing method of a high-strength nickel-based high-temperature alloy cold-drawn material, which can achieve the technical index required by a high-strength fastener by replacing multiple drawing with 20-25% cold-drawing large deformation at one time in the final cold-drawing production through the optimization control of a full-flow process.
The following technical route is adopted:
the method mainly comprises the steps of carrying out twice high-temperature homogenization diffusion annealing treatment on a consumable ingot and a forged intermediate blank, eliminating component segregation, carrying out gradual heating and cooling forging on the forging to ensure uniform blank tissues, carrying out 20-25% cold drawing and large deformation on a hot-rolled and cogging bar, improving the tissue uniformity from the center to the edge of the 1500MPa high-strength GH4169 alloy cold-drawn bar, and realizing the optimal matching of the strength and the plasticity of the cold-drawn bar.
Specific technical scheme
1. The production process is adopted: vacuum Induction (VIM) + vacuum consumable remelting (VAR) smelting → consumable ingot high-temperature homogenization diffusion annealing → combined cogging of a rapid forging machine and a radial forging machine → billet secondary high-temperature homogenization diffusion annealing → cogging of a 500 model reversible rolling mill → cogging of a 200 model reversible rolling mill → material drawing of a cold drawing machine → standardized heat treatment.
The chemical composition of the GH4169 alloy is as follows: carbon: 0.25%, sulfur not more than 0.002%, phosphorus not more than 0.015%, manganese not more than 0.35%, silicon not more than 0.35%, chromium: 18.0%, molybdenum: 3.0%, niobium: 5.25%, aluminum: 0.5%, titanium: 1.0%, nickel: 53.5 percent, boron not more than 0.006 percent and the balance of iron.
3. Primary high-temperature homogenizing diffusion annealing: smelting and casting an electrode rod with phi 340mm by adopting a vacuum induction furnace (VIM), remelting the electrode rod into a steel ingot with phi 406mm through vacuum consumable electrode (VAR), and ensuring that the oxygen content of the steel ingot gas is less than 50 multiplied by 10 -6 Nitrogen content of less than 100X 10 -6 The main element components and harmful elements meet the requirements of smelting standards; the steel ingot is subjected to high-temperature homogenization diffusion annealing treatment of heat preservation for 40 hours at 1180-1200 ℃ (preferably 1190 ℃) in a chamber furnace of natural gas, so as to eliminate cast component segregation.
4. Cogging of a fast forging machine and a radial forging machine: after the diffusion-treated steel ingot is subjected to heat preservation for 2 hours at 1110 ℃ in a natural gas chamber furnace, a 3150-ton quick forging machine is adopted to perform cogging for 3 times to a blank with the diameter of 240mm, and the temperature is preserved for 2 hours at 1050 ℃ before the last forging; and (3) after the blank with the diameter of 240mm is subjected to heat preservation for 2 hours at 1050 ℃ in a natural gas chamber furnace, forging the blank into the blank with the diameter of 120mm by adopting an 1800-ton diameter forging machine.
5. Secondary high-temperature homogenizing diffusion annealing: the intermediate blank with the diameter of 120mm is subjected to heat preservation for no less than 30 hours at 1180-1200 ℃ (preferably 1190 ℃).
6. Hot rolling and cogging: keeping the temperature of the intermediate blank with the diameter of 120mm for 2 hours at 1100 ℃ in a natural gas chamber furnace, and then rolling the intermediate blank into square billets with the diameter of 40mm to 50mm by 4 times of fire by using a 500 model reversible rolling mill; and (3) after the square billet is subjected to heat preservation for 0.5h at 1120 ℃ by a chamber furnace of natural gas, rolling the square billet into round steel blanks with phi 10 mm-phi 30mm by adopting a 200 model rolling mill for one fire.
7. The high-strength cold-drawing process comprises the following steps: the round steel blank is subjected to solution softening treatment of heat preservation at 960 ℃ for 1h by water cooling, the blank is polished to remove surface defects, the surface roughness of the blank is not more than 3.2 mu m, one end of the blank is twisted to be sharp, and the surface is treated by grassing and saponification surfaces to be adhered with lubricant; the blank is drawn by a 65 ton chain cold drawing machine at one time, the cold drawing deformation is 20-25%, and the blank is finely ground into a finished product.
8. The technical indexes are as follows:
making method of cooling water in cooling water
The aging temperature is 720 +/-10 ℃, the temperature is kept for 8h after soaking, then the mixture is cooled to 620 +/-10 ℃ at the speed of (50 +/-10) DEG C/h, the temperature is kept for 8h after soaking, and then the mixture is cooled in air.
Good mechanical properties
After the cold-drawn bar is treated by a standard heat treatment system, the room-temperature mechanical properties of the cold-drawn bar are in accordance with Table 1.
TABLE 1 mechanical Properties at Room temperature
| Test temperature | Rm(MPa) | Rp 0.2 (MPa) | A(L O ＝5d0)(％) | Z(％) | Hardness (HRC) |
| At room temperature | 1515～1725 | 1380 | ≥8 | ≥5 | ≥42 |
Tissue of high magnification
After the cold-drawn bar is treated by a standard heat treatment system, the average grain size should be finer than grade 5, allowing the existence of individual grade 3 grains.
Description of the innovative points of the present invention: carrying out high-temperature homogenization diffusion treatment on the steel ingot and the forged intermediate blank twice to eliminate component segregation; the forging is carried out for several times, the temperature is reduced, the forging cogging is carried out, and the uniform structure of the forging stock is ensured; the cogging deformation of hot rolling is not less than 65%, and the full refinement of the crystal grains of the hot-rolled bar is ensured; the cold drawing is carried out for 20% -25% of large deformation to be drawn into a finished product, and the large uniform cold deformation can not only ensure that the texture deformation from the edge to the center of the large-size bar is uniform and consistent, but also ensure the optimal strong plasticity matching of the room temperature performance of the bar.
Compared with the prior art, the invention has the following advantages:
the method is realized by adopting twice high-temperature homogenization diffusion annealing treatment of a consumable ingot and a forged intermediate blank, eliminating component segregation, forging, gradually heating, cooling and forging to ensure uniform blank tissue, and performing 20-25% cold drawing on a hot-rolled and cogging bar for one time to realize large deformation: (1) the grain size grade is improved from 6 grades (shown in figure 1) to 8 grades (shown in figure 2) of the common cold-drawn material, and the grain structure from the center to the edge of the material is finer and more uniform; (2) the tensile strength at room temperature is improved by 300MPa compared with the common cold-drawn material (see figure 3); (3) the cold drawing has large deformation, thereby ensuring the full and uniform deformation from the center to the edge of the bar and ensuring the best strong plasticity matching of the room temperature performance of the bar.
Drawings
FIG. 1 is a grain size diagram of a conventional cold-drawn material;
FIG. 2 is a grain size picture of a high strength cold drawn material;
FIG. 3 is a graph of room temperature tensile strength versus trend.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Examples 1 to 3 were all produced using the same process:
1. vacuum Induction (VIM) + vacuum consumable remelting (VAR) smelting → consumable ingot high-temperature homogenization diffusion annealing → combined cogging of a fast forging machine and a radial forging machine → billet secondary high-temperature homogenization diffusion annealing → cogging of a reversible rolling mill of model 500 → cogging of a reversible rolling mill of model 200 → material drawing of a cold drawing machine → standardized heat treatment.
2. Smelting and casting an electrode rod with phi 340mm by adopting a vacuum induction furnace (VIM), remelting the electrode rod into a steel ingot with phi 406mm through vacuum consumable electrode (VAR), and ensuring that the oxygen content of the steel ingot gas is less than 50 multiplied by 10 -6 Nitrogen content of less than 100X 10 -6 (ii) a The vacuum consumable ingot phi is 406mm, and the chemical components are shown in Table 2.
TABLE 2 vacuum consumable chemical composition of steel ingot
3. Preserving the heat of the consumable ingot in a natural gas chamber furnace at 1190 +/-10 ℃ for 40 hours, and carrying out primary high-temperature homogenization diffusion annealing treatment to eliminate cast component segregation;
4. the steel ingot is combined and cogging through a rapid forging machine and a radial forging machine, the steel ingot after diffusion treatment is kept warm for 2 hours at 1110 ℃ in a natural gas chamber furnace, then cogging is carried out by 3 times of fire by adopting a 3150-ton rapid forging machine to obtain a blank with the diameter of 240mm, and the temperature is kept for 2 hours at 1050 ℃ after the steel ingot is returned to the furnace before the last time of fire forging; and (3) after the blank with the diameter of 240mm is subjected to heat preservation for 2 hours at 1050 ℃ in a natural gas chamber furnace, forging the blank into the blank with the diameter of 120mm by adopting an 1800-ton diameter forging machine.
5. Keeping the temperature of the intermediate blank with the diameter of 120mm at 1190 +/-10 ℃ for 30 hours, and carrying out high-temperature homogenization diffusion annealing treatment for the second time;
rolling square steel by a reversible continuous rolling mill of model 6.500, keeping the temperature of an intermediate blank with a diameter of 120mm in a chamber furnace of natural gas at 1100 ℃ for 2h, and rolling the intermediate blank into square steel billets by a reversible rolling mill of model 500 at 4 times, wherein the specifications of the embodiment 1-3 are as follows: case 1 (40 mm. Times.40 mm square), case 2 (45 mm. Times.45 mm square), and case 3 (50 mm. Times.50 mm square).
7. After the square billets are subjected to heat preservation for 0.5h at 1120 ℃ in a chamber furnace for natural gas, rolling round billets by using a 200 model reversible rolling mill; examples the specifications are as follows: example 1: Φ 19mm, example 2: Φ 21mm, example 3: phi 24mm.
8. Performing high-strength cold drawing, namely performing solution softening treatment on hot-rolled round steel blanks by keeping the temperature at 960 ℃ for 1h and cooling with water, wherein the surface roughness of the blanks is not more than 3.2 mu m, performing grass chemical treatment and saponification surface adhesion lubricant treatment on the surfaces, and drawing the blanks into materials by a 65t chain cold drawing machine for one time; examples the specifications are as follows: example 1: Φ 15mm, example 2: Φ 17mm, example 3: phi 20mm.
Height of
The high strength cold drawing deformation is as follows:
example 1
Specification of a finished product: phi 15mm
Blank with phi 19mm → solid solution furnace heating (960 ℃ multiplied by 1h, water cooling) solid solution treatment → blank with phi 19mm is polished to phi 17.5mm → one end of blank is twisted sharp, the surface of blank is grassed, saponification treatment → cold drawing to phi 15.3mm → fine grinding to phi 15mm.
Example 2
Specification of a finished product: phi 17mm
Blank of phi 21mm → solution treatment by heating in a solution furnace (960 ℃ C.. Times.1 h, water cooling) → blank of phi 21mm is polished to phi 19.6mm → treatment of one end of blank with twisted tip → grass on surface of blank, saponification treatment → cold drawing to phi 17.3mm → fine grinding to phi 17mm.
Example 3
Specification of a finished product: phi 20mm
Blank of phi 24mm → solution furnace heating (960 ℃ multiplied by 1h, water cooling) solution treatment → blank of phi 24mm is polished to phi 23.0mm → one end of blank is twisted sharp processing → surface of blank is grassed, saponification processing → cold drawing to phi 20.3mm → fine grinding to phi 20mm.
9. Standardized heat treatment (electric heating furnace)
Soaking the finished round steel at the temperature of 720 +/-10 ℃, preserving heat for 8 hours, cooling to the temperature of 620 +/-10 ℃ at the speed of (50 +/-10) DEG C/h, preserving heat for 8 hours after soaking, and then cooling in air.
10. Test results
The room temperature mechanical properties are shown in table 3 (see fig. 3).
TABLE 3 mechanical Properties at Room temperature
The particle size grades are shown in table 4 (see fig. 2).
TABLE 4 grain size grades
| Inspection item | Grain size/grade |
| Control of | ≥5 |
| Example 1 | 8～9 |
| Example 2 | 8～7 |
| Example 3 | 8～9 |
Claims (2)
1. The manufacturing method of the high-strength nickel-based high-temperature alloy cold-drawn material is characterized by comprising the following steps: vacuum Induction (VIM) + vacuum consumable remelting (VAR) smelting → consumable ingot high-temperature homogenization diffusion annealing → combined cogging of a rapid forging machine and a radial forging machine → blank secondary high-temperature homogenization diffusion annealing → cogging of a 500 model reversible rolling mill → cogging of a 200 model reversible rolling mill → material drawing of a cold drawing machine → standardized heat treatment;
the consumable ingot GH4169 alloy comprises the following chemical components: carbon: 0.25%, sulfur not more than 0.002%, phosphorus not more than 0.015%, manganese not more than 0.35%, silicon not more than 0.35%, chromium: 18.0%, molybdenum: 3.0%, niobium: 5.25%, aluminum: 0.5%, titanium: 1.0%, nickel: 53.5 percent, boron not more than 0.006 percent and the balance of iron;
the method comprises the following steps of: smelting and casting an electrode rod with phi 340mm by adopting a vacuum induction furnace (VIM), remelting the electrode rod into a steel ingot with phi 406mm through vacuum consumable electrode (VAR), and ensuring that the oxygen content of the steel ingot gas is less than 50 multiplied by 10 -6 Nitrogen content of less than 100X 10 -6 The main element components and harmful elements meet the requirements of smelting standards; the steel ingot is subjected to high-temperature homogenization diffusion annealing treatment of heat preservation for 40 hours at 1180-1200 ℃ in a natural gas chamber furnace to eliminate cast component segregation;
thirdly, the rapid forging machine and the radial forging machine are combined for cogging: after the diffusion-treated steel ingot is subjected to heat preservation for 2 hours at 1110 ℃ in a natural gas chamber furnace, a 3150-ton quick forging machine is adopted to perform cogging for 3 times to a blank with the diameter of 240mm, and the temperature is preserved for 2 hours at 1050 ℃ before the last forging; after the blank with the diameter of 240mm is subjected to heat preservation for 2 hours at 1050 ℃ in a natural gas chamber furnace, forging the blank into the blank with the diameter of 120mm by adopting an 1800-ton diameter forging machine;
fourth, performing secondary high-temperature homogenization diffusion annealing on the blank: the intermediate blank with the diameter of 120mm is subjected to heat preservation at 1180-1200 ℃ for no less than 30 hours;
fifthly, cogging of the reversible rolling mill: keeping the temperature of the intermediate blank with the diameter of 120mm for 2 hours at 1100 ℃ in a natural gas chamber furnace, and then rolling the intermediate blank into square billets with the diameter of 40mm to 50mm by 4 times of fire by using a 500 model reversible rolling mill; after the square billet is subjected to heat preservation for 0.5h at 1120 ℃ in a chamber furnace of natural gas, rolling the square billet into round steel blanks with phi 10 mm-phi 30mm by adopting a 200 model rolling mill for one fire;
sixthly, drawing the blank into a material by a cold drawing machine: the round steel blank is subjected to solution softening treatment of heat preservation at 960 ℃ for 1h by water cooling, the blank is polished to remove surface defects, the surface roughness of the blank is not more than 3.2 mu m, one end of the blank is twisted to be sharp, and the surface is treated by grassing and saponification surfaces to be adhered with lubricant; the blank is once drawn by a 65 ton chain cold drawing machine, the cold drawing deformation is 20-25%, and the blank is finely ground into a finished product.
2. The method for manufacturing the high-strength nickel-base superalloy cold-drawn material according to claim 1, wherein the cold-drawn material is subjected to aging at 720 ℃ ± 10 ℃, soaking, heat preservation for 8 hours, cooling to 620 ℃ ± 10 ℃ at a rate of (50 ± 10) ° c/h, soaking, heat preservation for 8 hours, and air cooling; performance index after heat treatment:
the method has the advantages of mechanical properties:
at room temperature, the tensile strength (MPa) is 1515 to 1725, the yield strength (MPa) is 1380, and the elongation after fracture (%): not less than 8, reduction of area (%): not less than 5, hardness (HRC): not less than 42.
The high-power tissue:
the average grain size should be finer than grade 5, allowing for the presence of individual grade 3 grains.
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| CN116804261B (en) * | 2023-08-21 | 2023-12-01 | 成都先进金属材料产业技术研究院股份有限公司 | GH738 alloy bar and preparation method thereof |
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