CN116987917A - Preparation method of nickel-based high-temperature alloy foil for aviation - Google Patents
Preparation method of nickel-based high-temperature alloy foil for aviation Download PDFInfo
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- CN116987917A CN116987917A CN202311264089.8A CN202311264089A CN116987917A CN 116987917 A CN116987917 A CN 116987917A CN 202311264089 A CN202311264089 A CN 202311264089A CN 116987917 A CN116987917 A CN 116987917A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 62
- 239000000956 alloy Substances 0.000 title claims abstract description 62
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 35
- 239000011888 foil Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005097 cold rolling Methods 0.000 claims abstract description 51
- 239000011265 semifinished product Substances 0.000 claims abstract description 48
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 238000005242 forging Methods 0.000 claims abstract description 40
- 239000000047 product Substances 0.000 claims abstract description 23
- 238000003723 Smelting Methods 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000005098 hot rolling Methods 0.000 claims abstract description 9
- 238000009792 diffusion process Methods 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 23
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 239000010936 titanium Substances 0.000 claims description 13
- 239000002893 slag Substances 0.000 claims description 12
- 239000010955 niobium Substances 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 8
- 238000010583 slow cooling Methods 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 238000010309 melting process Methods 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005238 degreasing Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000010079 rubber tapping Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- 238000009966 trimming Methods 0.000 claims description 4
- 239000012856 weighed raw material Substances 0.000 claims description 4
- 238000005422 blasting Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 4
- 239000006104 solid solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910000601 superalloy Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- -1 low S Chemical compound 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
-
- 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%
-
- C—CHEMISTRY; METALLURGY
- 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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- 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
Abstract
The invention relates to a preparation method of a nickel-based high-temperature alloy foil for aviation, which comprises the following process flows: vacuum smelting, electroslag smelting, diffusion annealing, forging cogging, hot rolling of a semi-finished product delta 5.0-5.5 mm, solution heat treatment, four-roller cold rolling of a semi-finished product delta 1.5-1.6 mm, and twenty-roller cold rolling of a finished product delta 0.018-0.03mm; wherein, forge cogging specification: δ (60-70) (300-430) Lmm; hot rolling cogging specification: delta 5.0-5.5 (315-445) Lmm; the uniformity of the temperature of the solid solution furnace is less than or equal to 5 ℃. The invention can produce high-quality nickel-based high-temperature alloy foil finished products by optimizing the process, the performance of the finished products is stable, and the performance index of the strip finished products is (mechanical property) that the tensile strength (MPa) is more than or equal to 1300; yield strength (MPa) is more than or equal to 1200; the elongation percentage (%) is more than or equal to 1; the elastic modulus (GPa) is more than or equal to 200.
Description
Technical Field
The invention belongs to the technical field of special material smelting, and particularly relates to a preparation method of an aviation nickel-based high-temperature alloy foil.
Background
The nickel-base superalloy foil can be supplied in the forms of plates, strips, bars, forgings, annular parts, wires and pipes.
In recent years, with the development of aerospace industry in China, nickel-based high-temperature alloy foil is mainly used for manufacturing relaxation-resistant plane springs and coil springs of an aeroengine, which work below 800 ℃ and are required to have higher strength; the method can also be used for manufacturing parts such as turbine blades of gas turbines, and the like, so the demand of the parts is gradually increased, and the higher requirements on the performance of materials are put forth.
However, the interior of the existing nickel-based high-temperature alloy foil can generate complex precipitated phases, so that the tissue nonuniformity and the mechanical property are reduced; and a compound film with certain thickness, dark color and hard texture is generated on the surface of the semi-finished product during preparation, so that the production and processing difficulties are extremely high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an aviation nickel-based high-temperature alloy foil, and the preparation method can be used for producing a high-quality nickel-based high-temperature alloy foil finished product by optimizing a process, has stable performance of the finished product and lower production and processing difficulty, and can realize industrial production.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
1. the preparation method of the nickel-based high-temperature alloy foil for aviation comprises the following operations:
1) Vacuum melting
The raw materials are mixed according to the smelting requirement of the alloy in percentage by mass: less than or equal to 0.020% of C, less than or equal to 0.100% of Si, less than or equal to 0.200% of Mn, less than or equal to 0.015% of P, less than or equal to 0.01% of S, 0.6-1.0% of Al, 15.5-16.5% of Cr, 2.25-2.75% of Ti, 7.5-8.5% of Fe, 0.8-1.2% of Nb, less than or equal to 0.100% of Mo, less than or equal to 0.10% of Cu, less than or equal to 71% of Ni and less than or equal to 0.1% of impurity elements. Sequentially loading the weighed raw materials into an intermediate frequency vacuum induction furnace from the lower part of the crucible to the upper part in sequence of nickel, chromium, niobium, manganese, iron, titanium and aluminum for smelting; vacuumizing after closing the furnace, adjusting the power of the electric cabinet to 300Kw after the vacuum degree is 9Pa, and adjusting the power of the electric cabinet to 500Kw after the electric power is transmitted to preheat the crucible to reden; the splashing occurs in the material melting process, so that the power is timely reduced; material melting time: 3-6 hours; adding carbon for deoxidization every 5-8 minutes after the refining temperature is reached, and entering a refining period after the carbon reaction is finished; refining temperature: 1520-1550 ℃ and refining time: 60 minutes; the tapping temperature is 1450-1480 ℃; pouring the alloy ingot into an electrode under vacuum, performing small flow feeding after pouring the alloy ingot into a cap line, rapidly breaking the vacuum after pouring, adding a heating agent, and performing good feeding on the alloy ingot to obtain an alloy ingot;
2) Electroslag smelting
Finishing the alloy ingot and then smelting the alloy ingot by electroslag; the electroslag material selected by electroslag remelting is CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 Five-membered slag system is baked for more than or equal to 24 hours at 600-800 ℃ before the slag is used; the arc starting current of electroslag remelting is 4000A-4500A, the current in a stable melting stage is 800A-8500A, and the current in feeding is gradually reduced by 7900A-7300A; the melting rate in the melting process is 3.5 kg/min-4.5 kg/min; cooling the electroslag ingot in a crystallizer for 1-1.5 h, and lifting the alloy ingot into a slow cooling box for slow cooling within 10-15 min after demoulding, wherein the sand cooling time is 13-15 h; obtaining an electroslag ingot;
3) Diffusion annealing
Charging the electroslag ingot into a furnace at room temperature, heating to 1160 ℃ along with the furnace, preserving heat for 15-20 h, and then heating to 1200 ℃ along with the furnace, preserving heat for 25-30 h; cooling to 1000 ℃ along with the furnace, discharging from the furnace, and air cooling to room temperature;
4) Forging cogging
Heating an electroslag ingot by adopting a resistance furnace, raising the temperature to 1160-1180 ℃, and preserving heat for 2-3 hours; then cogging and forging the electroslag ingot according to the specification of delta 60-70 mm and the forging ratio of 6-8; the forging terminal temperature is lower than 950 ℃ and needs to be returned to the furnace to raise the temperature for re-forging; cooling after forging; air cooling to obtain forging stock;
5) Hot-rolled semifinished product
Charging the forging stock, heating to 1160-1180 ℃, and starting rolling in a hot rolling mill after the heat preservation time is 1.5-2.5 hours; the initial rolling temperature is more than or equal to 1100 ℃, the final rolling temperature is more than or equal to 950 ℃, and the specification of the hot rolled semi-finished product is as follows: delta 5.0-5.5 mm, and shot blasting is carried out on the hot-rolled semi-finished product;
6) Solution heat treatment
Placing the shot-blasted hot-rolled semi-finished product into a heat treatment furnace for heat treatment; heating to 1100-1200 ℃, preserving heat for 1.5-2.5 h, and quenching; surface treatment is carried out after quenching is finished;
7) Four-roller cold-rolled semi-finished product
Cold rolling the hot-rolled semi-finished product after the step 6) to a semi-finished product material, wherein the semi-finished product material has the following specification: delta 1.5-1.6 mm; the total deformation of a single rolling process is 35% -45%, and the deformation of each pass is less than or equal to 15%;
8) Twenty-roller cold-rolled semi-finished product
Cold rolling the semi-finished product material in the step 7) to a semi-finished product, wherein the semi-finished product has the following specification: delta 0.3 + -0.007 mm; the total deformation of a single rolling process is 35% -50%, and the deformation of each pass is less than or equal to 15%;
9) Twenty-roller secondary cold-rolled finished product
Cold rolling the semi-finished product in the step 8) to a finished product, wherein the specification of the finished product is as follows: delta 0.018+ -0.005 mm; trimming and degreasing after cold rolling; the total deformation of a single rolling process is 35% -50%, and the deformation of each pass is less than or equal to 15%.
In the preparation method of the nickel-based high-temperature alloy foil for aviation, in the step 1), the mass ratio of the heating agent is 70% of aluminum powder and 30% of sodium nitrate; the dosage of the molten steel is 0.2-0.6% of the weight of the molten steel, the molten steel is added for 2 times in addition, and the interval time of 2 times is 15-25 minutes.
One of the above aviationPreparation method of nickel-based high-temperature alloy foil, in step 2), the CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 The five-membered slag system can ensure the component range of the alloy titanium content.
In the above method for preparing nickel-based high temperature alloy foil for aviation, in step 7), parameters of the four-roller cold rolling mill set are as follows: the diameter phi of the roller is 180mm, the width of the roller surface is 450mm, and the rolling force is 300 tons.
In the above method for preparing nickel-based high temperature alloy foil for aviation, in step 8), parameters of the twenty-high roll cold rolling unit are as follows: the maximum width of the inlet is 500mm, the minimum width of the outlet is 220mm, the rolling force of the rolling mill is 450kg/mm, and the rolling force is required to be 50t.
In the above method for preparing nickel-based high temperature alloy foil for aviation, in step 9), parameters of the twenty-roller secondary cold rolling unit are as follows: the maximum width of the inlet is 500mm, the minimum width of the outlet is 300mm, the rolling force of the rolling mill is 400kg/mm, and the rolling force is required to be 40t.
According to the preparation method of the nickel-based high-temperature alloy foil for aviation, the specification from forging cogging to twenty-roller secondary cold rolling is controlled as follows in mm: forging stock specification: delta (60-70) × (300-430) × (L); hot rolling specification: delta 5.0-5.5 (315-445) L; four-roller cold rolling to: δ1.5 to 1.6 (435 to 455) L; twenty-high cold rolling to: delta 0.3 + -0.007 mm; twenty-high secondary cold rolling to: delta 0.018.+ -. 0.005mm.
The invention has the technical effects and advantages that:
according to the preparation method of the nickel-based high-temperature alloy foil for aviation, provided by the invention, the nickel-based high-temperature alloy which contains less than or equal to 0.020% of C, less than or equal to 0.100% of Si, less than or equal to 0.200% of Mn, less than or equal to 0.015% of P, less than or equal to 0.01% of S, 0.6-1.0% of Al, 15.5-16.5% of Cr, 2.25-2.75% of Ti, 7.5-8.5% of Fe, 0.8-1.2% of Nb, less than or equal to 0.100% of Mo, less than or equal to 0.10% of Cu and more than or equal to 71% of Ni is adopted, and the nickel-based high-temperature alloy which is subjected to ageing strengthening mainly by gamma' [ Ni3 (Al, ti and Nb) ] phase can have good corrosion resistance and oxidation resistance at the temperature of below 980 ℃, has good relaxation resistance at the temperature of below 800 ℃, and good forming property, welding property and mechanical property; the finished nickel-based superalloy foil is high in quality and excellent in quality, and meets the use requirements of high-performance aeroengines; the performance index is (mechanical property) that the tensile strength (MPa) is more than or equal to 1300; yield strength (MPa) is more than or equal to 1200; the elongation percentage (%) is more than or equal to 1; elastic modulus (GPa) is more than or equal to 200; and the surface roughness is 0.05-0.10 mu m; the thickness precision of the finished product reaches +/-0.005 mm; the material is softened by high-temperature (1160-1180 ℃) continuous annealing under the protection of high-purity hydrogen (more than 99.9% hydrogen) atmosphere, so that the aim of easy processing is fulfilled, the problem of high production and processing difficulty is solved, the processing is easy, and the processing efficiency is greatly improved.
Detailed Description
The present invention will be described in further detail with reference to examples.
The preparation method of the nickel-based high-temperature alloy foil for aviation comprises the following operations:
1) Vacuum melting
The raw materials are mixed according to the smelting requirement of the alloy in percentage by mass: less than or equal to 0.020% of C, less than or equal to 0.100% of Si, less than or equal to 0.200% of Mn, less than or equal to 0.015% of P, less than or equal to 0.01% of S, 0.6-1.0% of Al, 15.5-16.5% of Cr, 2.25-2.75% of Ti, 7.5-8.5% of Fe, 0.8-1.2% of Nb, less than or equal to 0.100% of Mo, less than or equal to 0.10% of Cu, less than or equal to 71% of Ni and less than or equal to 0.1% of impurity elements. Sequentially loading the weighed raw materials into an intermediate frequency vacuum induction furnace from the lower part of the crucible to the upper part in sequence of nickel, chromium, niobium, manganese, iron, titanium and aluminum for smelting; vacuumizing after closing the furnace, adjusting the power of the electric cabinet to 300Kw after the vacuum degree is 9Pa, and adjusting the power of the electric cabinet to 500Kw after the electric power is transmitted to preheat the crucible to reden; the splashing occurs in the material melting process, so that the power is timely reduced; material melting time: 3-6 hours; adding carbon for deoxidization every 5-8 minutes after the refining temperature is reached, and entering a refining period after the carbon reaction is finished; refining temperature: 1520-1550 ℃ and refining time: 60 minutes; the tapping temperature is 1450-1480 ℃; and (3) pouring the alloy ingot into an electrode under vacuum, performing small-flow feeding after pouring the alloy ingot into a cap line, rapidly breaking the vacuum after pouring, and adding a heating agent, so that the alloy ingot is fed well, and the alloy ingot is obtained.
Wherein the mass ratio of the heat generating agent is 70% of aluminum powder and 30% of sodium nitrate; the dosage of the molten steel is 0.2-0.6% of the weight of the molten steel, the molten steel is added for 2 times in addition, and the interval time of 2 times is 15-25 minutes.
2) Electroslag smelting
Finishing the alloy ingot and then smelting the alloy ingot by electroslag; the electroslag material selected by electroslag remelting is CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 Five-membered slag system is baked for more than or equal to 24 hours at 600-800 ℃ before the slag is used; the arc starting current of electroslag remelting is 4000A-4500A, the current in a stable melting stage is 800A-8500A, and the current in feeding is gradually reduced by 7900A-7300A; the melting rate in the melting process is 3.5 kg/min-4.5 kg/min; cooling the electroslag ingot in a crystallizer for 1-1.5 h, and lifting the alloy ingot into a slow cooling box for slow cooling within 10-15 min after demoulding, wherein the sand cooling time is 13-15 h; and obtaining electroslag ingots.
Specifically, the CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 The five-membered slag system can ensure the component range of the alloy titanium content.
3) Diffusion annealing
Charging the electroslag ingot into a furnace at room temperature, heating to 1160 ℃ along with the furnace, preserving heat for 15-20 h, and then heating to 1200 ℃ along with the furnace, preserving heat for 25-30 h; cooling to 1000 ℃ along with the furnace, discharging from the furnace, and air cooling to room temperature;
4) Forging cogging
Heating an electroslag ingot by adopting a resistance furnace, raising the temperature to 1160-1180 ℃, and preserving heat for 2-3 hours; then cogging and forging the electroslag ingot according to the specification of delta 60-70 mm and the forging ratio of 6-8; the forging terminal temperature is lower than 950 ℃ and needs to be returned to the furnace to raise the temperature for re-forging; cooling after forging: air cooling to obtain forging stock;
5) Hot-rolled semifinished product
Charging the forging stock, heating to 1160-1180 ℃, and starting rolling in a hot rolling mill after the heat preservation time is 1.5-2.5 hours; the initial rolling temperature is more than or equal to 1100 ℃, the final rolling temperature is more than or equal to 950 ℃, and the specification of the hot rolled semi-finished product is as follows: delta 5.0-5.5 mm, and shot blasting is carried out on the hot-rolled semi-finished product;
6) Solution heat treatment
Placing the shot-blasted hot-rolled semi-finished product into a heat treatment furnace for heat treatment; heating to 1100-1200 ℃, preserving heat for 1.5-2.5 h, and quenching; surface treatment is carried out after quenching is finished;
7) Four-roller cold-rolled semi-finished product
Cold rolling the hot-rolled semi-finished product after the step 6) to a semi-finished product material, wherein the semi-finished product material has the following specification: delta 1.5-1.6 mm; the total deformation of a single rolling process is 35% -45%, and the deformation of each pass is less than or equal to 15%; parameters of the four-roller cold rolling unit: the diameter phi of the roller is 180mm, the width of the roller surface is 450mm, and the rolling force is 300 tons.
8) Twenty-roller cold-rolled semi-finished product
Cold rolling the semi-finished product material in the step 7) to a semi-finished product, wherein the semi-finished product has the following specification: delta 0.3 + -0.007 mm; the total deformation of a single rolling process is 35% -50%, and the deformation of each pass is less than or equal to 15%; parameters of the twenty-roller cold rolling unit: the maximum width of the inlet is 500mm, the minimum width of the outlet is 220mm, the rolling force of the rolling mill is 450kg/mm, and the rolling force is required to be 50t.
9) Twenty-roller secondary cold-rolled finished product
Cold rolling the semi-finished product in the step 8) to a finished product, wherein the specification of the finished product is as follows: delta 0.018+ -0.005 mm; trimming and degreasing after cold rolling; the total deformation of a single rolling process is 35% -50%, and the deformation of each pass is less than or equal to 15%; parameters of the twenty-roller secondary cold rolling unit: the maximum width of the inlet is 500mm, the minimum width of the outlet is 300mm, the rolling force of the rolling mill is 400kg/mm, and the rolling force is required to be 40t.
Example 1
The preparation method of the nickel-based high-temperature alloy foil for aviation comprises the following steps:
1) Vacuum melting (VIM):
preparing materials according to smelting requirements, namely taking high-grade pure iron (mainly low S, P), electrolytic nickel, metallic chromium, metallic niobium, metallic manganese, aluminum powder and titanium sponge (grade 0) as main raw materials, and weighing the materials according to the requirements in percentage by mass: c0.01%, si:0.08 percent of raw materials, 0.2 percent of Mn, 0.85 percent of Al, 15.9 percent of Cr, 2.65 percent of Ti, 7.9 percent of Fe, 0.95 percent of Nb and the balance of Ni, and sequentially loading the weighed raw materials into an intermediate frequency vacuum induction furnace from the lower part of a crucible to be smelted according to the sequence of nickel, chromium, niobium, manganese, iron, titanium and aluminum;
vacuumizing after closing the furnace, adjusting the power of the electric cabinet to 300Kw after the vacuum degree is 9Pa, and adjusting the power of the electric cabinet to 500Kw after the electric power is transmitted to preheat the crucible to reden; the splashing occurs in the material melting process, so that the power is timely reduced; material melting time: 3-6 hours; adding carbon for deoxidization every 5-8 minutes after the refining temperature is reached, and entering a refining period after the carbon reaction is finished; refining temperature: 1520-1550 ℃ and refining time: 60 minutes; the tapping temperature is 1450-1480 ℃; and (3) pouring the alloy ingot into an electrode under vacuum, feeding the alloy ingot into small flow after pouring the alloy ingot into a cap line, and rapidly breaking the vacuum heating agent after pouring (the heating agent is added for 2 times at 15-25 minutes).
The exothermic agent comprises the following components: 70% of aluminum powder and 30% of sodium nitrate; the consumption of the heating agent is 0.2-0.6% of the weight of the molten steel; the alloy ingot is fed well.
2) Electroslag smelting: and (3) finishing the electrode rod in the step (1) and then carrying out electroslag smelting.
The electroslag material selected by electroslag remelting is CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 Five-membered slag system (the slag system can ensure the component range of the alloy titanium content), and the slag material is baked for more than or equal to 24 hours at 600-800 ℃ before being used;
the arc starting current of electroslag remelting is 4000-4500A, the current in a stable melting stage is 8000-8500A, and the current in feeding is gradually reduced by 7900A-7300 00A; the melting rate in the smelting process is 3.5-4.5 kg/min;
cooling the electroslag ingot in a crystallizer for 1-1.5 h, lifting the alloy ingot into a slow cooling box for slow cooling within 10-15 min after demoulding, and carrying out sand cooling for 13-15 h; thus, an electroslag ingot was obtained.
3) Diffusion annealing
Charging the furnace at room temperature, heating to 1160 ℃ along with the furnace, preserving heat for 15-20 h, and then heating to 1200 ℃ along with the furnace, preserving heat for 25-30 h; and cooling to 1000 ℃ along with the furnace, discharging, and air cooling to room temperature.
4) Forging cogging
Heating by adopting a resistance furnace, heating to 750 ℃ at a speed of 15 ℃/min, preserving heat for 1-2 h, heating to 1020-1040 ℃ at a speed of 50 ℃/h, preserving heat for 1-2 h, heating to 1160-1180 ℃ at a speed of 50 ℃/h, and preserving heat for 2-3 h. Forging stock specification delta (60-70) × (300-430) × (Lmm), forging ratio 6-8.
The single-hammer rolling reduction is 40-60 mm in the state of alloy ingot, the maximum rolling reduction can be increased to 100mm when forging, and chamfering is carried out after forging into a plate blank; the forging terminal temperature is lower than 950 ℃ and needs to be returned to the furnace to raise the temperature for re-forging; cooling after forging: and (5) air cooling. The forging stock is transferred to hot rolling after flaw detection, grinding and sawing.
5) Hot-rolled semifinished product
The forging stock is heated according to a hot rolling system and then rolled, and the specification of a hot rolled semi-finished product is: delta 5.0-5.5 (315-445) Lmm; the charging temperature of the plate blank is less than or equal to 700 ℃; heating to 800 ℃ along with a furnace, and preserving heat for 1h; heating to 1180 ℃ at a speed of 50 ℃/h, and starting rolling after the heat preservation time is 1.5-2.5 h; the initial rolling temperature is more than or equal to 1100 ℃, the final rolling temperature is more than or equal to 950 ℃, the rolling is carried out for 5 times, and the deformation of each pass is more than or equal to 30 percent. The hot rolled strip is shot-blasted and then ready for heat treatment.
6) Solution heat treatment
Placing the shot-blasted hot-rolled strip blank into a special heat treatment furnace for heat treatment; the specific operation is as follows: charging at room temperature, firstly raising the furnace temperature to (850-900) DEG C at a speed of 5 ℃/min, and preserving heat for (0.5-1.5) h; then heating to (1100-1200) DEG C at 3 ℃/min, preserving heat for (1.5-2.5) h, and quenching; surface treatment is carried out after quenching is finished;
7) Four-roll cold rolling
Parameters of the four-roller cold rolling unit: the diameter phi of the roller is 180mm, the width of the roller surface is 450mm, and the rolling force is 300 tons. Cold rolling the semi-finished product material delta 5.0-5.5 (315-445) Lmm in the step 6 to obtain a semi-finished product delta 1.5-1.6 (435-455) Lmm; the pass deformation of delta 5.0-delta 5.5mm to delta 3.0-delta 3.5mm is controlled to be 10% -15%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 3.0-delta 3.5mm to delta 2.0-delta 2.5mm is controlled to be 8% -12%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 2.0-delta 2.5mm cold-rolled to delta 1.5-delta 1.6mm is controlled to be 8% -12%, and continuous bright annealing is carried out after cold rolling is finished; and then transferring into twenty-roller cold-rolled finished products.
8) Twenty-high cold-rolled product
(1) Parameters of the twenty-high cold rolling mill train: the maximum width of the inlet is 500mm, the minimum width of the outlet is 220mm, the rolling force of the rolling mill is 450kg/mm, and the rolling force is required to be 50t; cold rolling the semi-finished product material delta 1.5-delta 1.6mm in the step 7 to a finished product delta 0.3+/-0.007 mm; the pass deformation of delta 1.5-delta 1.6mm to delta 1.0 plus or minus 0.05mm is controlled to be 8-12%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 1.0 plus or minus 0.05mm cold rolling to delta 0.6 plus or minus 0.007mm is controlled to be 8% -12%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 0.6 plus or minus 0.07mm cold rolling to delta 0.3 plus or minus 0.007mm is controlled to be 8% -10%, and continuous bright annealing is carried out after the cold rolling is finished; and enters the next twenty rollers.
(2) Parameters of the twenty-high cold rolling mill train: parameters of the twenty-high cold rolling mill train: the maximum width of the inlet is 500mm, the minimum width of the outlet is 300mm, the rolling force of the rolling mill is 400kg/mm, and the rolling force is required to be 40t; cold rolling the semi-finished product delta 0.3 plus or minus 0.007mm in the step (1) to a finished product delta 0.018 plus or minus 0.005mm; the pass deformation of delta 0.3+/-0.007 mm to delta 0.15+/-0.005 mm is controlled to be 8% -10%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 0.15 plus or minus 0.005mm to delta 0.07 plus or minus 0.005mm is controlled to be 6-10%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 0.07 plus or minus 0.005mm to delta 0.035 plus or minus 0.005mm is controlled to be 5% -10%, and continuous bright annealing is carried out after the cold rolling is finished; the pass deformation of delta 0.035 plus or minus 0.005mm to delta 0.018 plus or minus 0.005mm is controlled to be 5% -10%; trimming and degreasing after cold rolling.
The nickel-based superalloy cold rolled foil prepared by the embodiment has high quality and excellent quality, and meets the use requirement of a high-performance aeroengine; the performance of the finished product can be achieved: the tensile strength (MPa) is more than or equal to 1300; yield strength (MPa) is more than or equal to 1200; the elongation percentage (%) is more than or equal to 1; elastic modulus (GPa) is more than or equal to 200; the surface roughness is 0.05 mu m to 0.10 mu m; the thickness precision of the finished product reaches +/-0.005 mm; the composition index and the performance index of the strip prepared according to the present invention are given below.
Table 1 shows the composition index of the finished product of the strip
Table 2 shows the mechanical properties of the finished strip
Table 3 shows the mechanical properties of the samples drawn from the final product of the strip with a delta of 0.018mm
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and improvements could be made by those skilled in the art without departing from the inventive concept, which falls within the scope of the present invention.
Claims (7)
1. A preparation method of an aviation nickel-based high-temperature alloy foil is characterized by comprising the following steps of: comprising the following operations:
1) Vacuum melting
The raw materials are mixed according to the smelting requirement of the alloy in percentage by mass: less than or equal to 0.020% of C, less than or equal to 0.100% of Si, less than or equal to 0.200% of Mn, less than or equal to 0.015% of P, less than or equal to 0.01% of S, 0.6-1.0% of Al, 15.5-16.5% of Cr, 2.25-2.75% of Ti, 7.5-8.5% of Fe, 0.8-1.2% of Nb, less than or equal to 0.100% of Mo, less than or equal to 0.10% of Cu, less than or equal to 71% of Ni and less than or equal to 0.1% of impurity elements. Sequentially loading the weighed raw materials into an intermediate frequency vacuum induction furnace from the lower part of the crucible to the upper part in sequence of nickel, chromium, niobium, manganese, iron, titanium and aluminum for smelting; vacuumizing after closing the furnace, adjusting the power of the electric cabinet to 300Kw after the vacuum degree reaches 9Pa, and adjusting the power of the electric cabinet to 500Kw after the electric power of the electric cabinet is transmitted to preheat the crucible to reden; the splashing occurs in the material melting process, so that the power is timely reduced; material melting time: 3-6 hours; adding carbon for deoxidization every 5-8 minutes after the refining temperature is reached, and entering a refining period after the carbon reaction is finished; refining temperature: 1520-1550 ℃ and refining time: 60 minutes; the tapping temperature is 1450-1480 ℃; pouring the alloy ingot into an electrode under vacuum, performing small flow feeding after pouring the alloy ingot into a cap line, rapidly breaking the vacuum after pouring, adding a heating agent, and performing good feeding on the alloy ingot to obtain an alloy ingot;
2) Electroslag smelting
Finishing the alloy ingot and then smelting the alloy ingot by electroslag; the electroslag material selected by electroslag remelting is CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 Five-membered slag system is baked for more than or equal to 24 hours at 600-800 ℃ before the slag is used; the arc starting current of electroslag remelting is 4000A-4500A, the current in a stable melting stage is 800A-8500A, and the current in feeding is gradually reduced by 7900A-7300A; the melting rate in the melting process is 3.5 kg/min-4.5 kg/min; the electroslag ingot is cooled in a crystallizer for 1 to 1.5 hours,after demolding, hanging the alloy ingot into a slow cooling box for slow cooling within 10-15 min, wherein the sand cooling time is 13-15 h; obtaining an electroslag ingot;
3) Diffusion annealing
Charging the electroslag ingot into a furnace at room temperature, heating to 1160 ℃ along with the furnace, preserving heat for 15-20 h, and then heating to 1200 ℃ along with the furnace, preserving heat for 25-30 h; cooling to 1000 ℃ along with the furnace, discharging from the furnace, and air cooling to room temperature;
4) Forging cogging
Heating an electroslag ingot by adopting a resistance furnace, raising the temperature to 1160-1180 ℃, and preserving heat for 2-3 hours; then cogging and forging the electroslag ingot according to the specification of delta 60-70 mm and the forging ratio of 6-8; the forging terminal temperature is lower than 950 ℃ and needs to be returned to the furnace to raise the temperature for re-forging; cooling after forging; air cooling to obtain forging stock;
5) Hot-rolled semifinished product
Charging the forging stock, heating to 1160-1180 ℃, and starting rolling in a hot rolling mill after the heat preservation time is 1.5-2.5 hours; the initial rolling temperature is more than or equal to 1100 ℃, the final rolling temperature is more than or equal to 950 ℃, and the specification of the hot rolled semi-finished product is as follows: delta 5.0-5.5 mm, and shot blasting is carried out on the hot-rolled semi-finished product;
6) Solution heat treatment
Placing the shot-blasted hot-rolled semi-finished product into a heat treatment furnace for heat treatment; heating to 1100-1200 ℃, preserving heat for 1.5-2.5 h, and quenching; surface treatment is carried out after quenching is finished;
7) Four-roller cold-rolled semi-finished product
Cold rolling the hot-rolled semi-finished product after the step 6) to a semi-finished product material, wherein the semi-finished product material has the following specification: delta 1.5-1.6 mm; the total deformation of a single rolling process is 35% -45%, and the deformation of each pass is less than or equal to 15%;
8) Twenty-roller cold-rolled semi-finished product
Cold rolling the semi-finished product material in the step 7) to a semi-finished product, wherein the semi-finished product has the following specification: delta 0.3 + -0.007 mm; the total deformation of a single rolling process is 35% -50%, and the deformation of each pass is less than or equal to 15%;
9) Twenty-roller secondary cold-rolled finished product
Cold rolling the semi-finished product in the step 8) to a finished product, wherein the specification of the finished product is as follows: delta 0.018+ -0.005 mm; trimming and degreasing after cold rolling; the total deformation of a single rolling process is 35% -50%, and the deformation of each pass is less than or equal to 15%.
2. The method for preparing the nickel-based high-temperature alloy foil for aviation according to claim 1, which is characterized in that: in the step 1), the mass ratio of the heat generating agent is 70% of aluminum powder and 30% of sodium nitrate; the dosage of the molten steel is 0.2-0.6% of the weight of the molten steel, the molten steel is added for 2 times in addition, and the interval time of 2 times is 15-25 minutes.
3. The method for preparing the nickel-based high-temperature alloy foil for aviation according to claim 1, which is characterized in that: in step 2), the CaF 2 -Al 2 O 3 -CaO-MgO-TiO 2 The five-membered slag system can ensure the component range of the alloy titanium content.
4. The method for preparing the nickel-based high-temperature alloy foil for aviation according to claim 1, which is characterized in that: in step 7), parameters of the four-roll cold rolling unit are as follows: the diameter phi of the roller is 180mm, the width of the roller surface is 450mm, and the rolling force is 300 tons.
5. The method for preparing the nickel-based high-temperature alloy foil for aviation according to claim 1, which is characterized in that: in step 8), parameters of the twenty-high cold rolling mill train are as follows: the maximum width of the inlet is 500mm, the minimum width of the outlet is 220mm, the rolling force of the rolling mill is 450kg/mm, and the rolling force is required to be 50t.
6. The method for preparing the nickel-based high-temperature alloy foil for aviation according to claim 1, which is characterized in that: in the step 9), parameters of the twenty-high secondary cold rolling unit are as follows: the maximum width of the inlet is 500mm, the minimum width of the outlet is 300mm, the rolling force of the rolling mill is 400kg/mm, and the rolling force is required to be 40t.
7. The method for preparing the nickel-based high-temperature alloy foil for aviation according to claim 1, which is characterized in that: in mm, the specification of the secondary cold rolling from forging cogging to twenty rolls is controlled as follows: forging stock specification: delta (60-70) × (300-430) × (L); hot rolling specification: delta 5.0-5.5 (315-445) L; four-roller cold rolling to: δ1.5 to 1.6 (435 to 455) L; twenty-high cold rolling to: delta 0.3 + -0.007 mm; twenty-high secondary cold rolling to: delta 0.018.+ -. 0.005mm.
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