Preparation method of iron-nickel-based high-temperature alloy ultra-thin material

Abstract

This invention relates to a method for preparing ultrathin iron-nickel-based superalloy materials, belonging to the field of superalloy processing technology. It solves one of the problems of existing preparation processes that easily cause edge cracking and breakage of ultrathin materials, as well as poor dimensional accuracy, plasticity, plate shape, and surface quality of the finished ultrathin materials. This invention discloses a method for preparing ultrathin iron-nickel-based superalloy materials, using solution-treated iron-nickel-based superalloy sheet coils as billets; undergoing multi-pass rolling, including roughing and finishing sections; performing intermediate bright annealing between rolling passes; performing bright annealing of the semi-finished product after the roughing section; and performing bright annealing of the finished product after the finishing section to obtain the finished ultrathin material. The ultrathin iron-nickel-based superalloy GH3536 prepared by the above method has high dimensional accuracy, excellent plasticity, good plate shape, and excellent surface quality, and can be widely used in the manufacture of honeycomb structural components in aerospace and other fields.

Description

Technical Field

[0001] This invention relates to the field of high-temperature alloy processing technology, and in particular to a method for preparing ultrathin iron-nickel-based high-temperature alloy materials. Background Technology

[0002] High-temperature alloys are irreplaceable materials in aero-engines, rocket engines, and gas turbines. Honeycomb structures are a critical component of the hot-section of aerospace engines, formed by stamping hexagonal honeycomb strips from high-temperature alloy strips (0.05–0.2 mm thick) and then welding them together. Therefore, high-temperature alloy strips are the most important manufacturing material for honeycomb structures. Furthermore, to meet the need for engine weight reduction, honeycomb structures are increasingly being manufactured using thinner strips.

[0003] High-temperature alloy strips and foils with a thickness of less than 0.1 mm fall into the category of ultra-thin materials. When using traditional cold rolling and annealing processes, problems such as strip breakage, edge cracking, poor plate shape (warping, side bending), poor surface quality (large roughness, surface oxidation) and poor plasticity often occur during the preparation process. Summary of the Invention

[0004] Based on the above analysis, the present invention aims to provide a method for preparing iron-nickel-based high-temperature alloy ultrathin materials, in order to solve one of the problems of existing preparation processes that easily cause edge cracking and breakage of ultrathin materials, as well as poor dimensional accuracy, plasticity, plate shape and surface quality of finished ultrathin materials.

[0005] This invention discloses a method for preparing an ultrathin iron-nickel-based superalloy material, the method comprising:

[0006] Solid solution-treated iron-nickel-based high-temperature alloy plates and coils are used as raw materials;

[0007] Multi-pass rolling, wherein the multi-pass rolling includes a roughing section and a finishing section;

[0008] Bright annealing is performed as an intermediate process between the passes of multi-pass rolling.

[0009] The semi-finished product is bright annealed after the rough rolling section; the finished product is bright annealed after the finish rolling section.

[0010] Specifically, the roughing section is rolled using a four-roll cold rolling mill, and the finishing section is rolled using a twenty-roll cold rolling mill.

[0011] Specifically, the roughing section includes multiple rolling passes, with the left and right tensions of the mill decreasing with each pass; the finishing section includes multiple rolling passes, with the left and right tensions of the mill decreasing with each pass.

[0012] Specifically, the roughing section includes two cold rolling passes; the left and right tension of the first cold rolling pass in the roughing section is 15-20 kN; the left and right tension of the second cold rolling pass in the roughing section is 10-15 kN.

[0013] Specifically, the finishing rolling section includes three cold rolling passes; the left and right tension of the first cold rolling pass of the finishing rolling section is 10-15 kN; the left and right tension of the second cold rolling pass of the finishing rolling section is 8-10 kN; and the left and right tension of the third cold rolling pass of the finishing rolling section is 5-10 kN.

[0014] Specifically, the bright annealing temperature is 1065-1105℃, and the strip needs to be rapidly cooled by hydrogen injection before exiting the furnace.

[0015] The specific steps of the above preparation method include:

[0016] The roughing section includes:

[0017] S1: Use 0.80-1.50mm solid solution iron-nickel-based high-temperature alloy plate coils as billets, cold roll the billets to 0.45-0.80mm, and then perform bright annealing in a hydrogen-protected continuous annealing furnace;

[0018] S2: The cold-rolled material obtained in S1 is cold-rolled to 0.25-0.40mm, and then bright annealed in a hydrogen-protected continuous annealing furnace to obtain a semi-finished thin strip.

[0019] The finishing rolling section includes:

[0020] S3: The semi-finished thin strip obtained in S2 is cold rolled to 0.15-0.20 mm and then bright annealed in a hydrogen-protected continuous annealing furnace;

[0021] S4: The strip obtained in S3 is cold rolled to 0.08-0.10 mm and then bright annealed in a hydrogen-protected continuous annealing furnace;

[0022] S5: The strip obtained in S4 is cold rolled to 0.05±0.004mm and then bright annealed in a hydrogen-protected continuous annealing furnace to obtain the finished ultra-thin material.

[0023] Specifically, the holding time for bright annealing in steps S1 and S2 is 3 to 5 minutes, and / or the holding time for bright annealing in steps S3 and S4 is 2 to 4 minutes, and / or the holding time for bright annealing in step S5 is 2 to 3 minutes.

[0024] Specifically, the solid solution-treated iron-nickel-based high-temperature alloy sheet / coil is a GH3536 alloy sheet / coil.

[0025] The present invention also discloses an ultrathin iron-nickel-based high-temperature alloy material, which is prepared by the above-described preparation method.

[0026] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects:

[0027] 1. Less prone to edge cracking and breakage of ultra-thin materials. By rationally allocating the deformation amount of each cold rolling pass, the impact of work hardening on the rolling process is effectively reduced. At the same time, considering the different original thickness and deformation amount of the billet in different rolling passes, the tension is rationally controlled under the condition of a certain rolling rate, thereby accurately controlling the effective deformation degree of the billet in the rolling process and avoiding the problems of edge cracking and strip breakage of the billet.

[0028] 2. High dimensional accuracy of finished ultra-thin sheets. A 20-roll precision cold rolling mill is used to precisely control the final cold rolling deformation parameters under specific cold rolling rates. Combined with online reduction detection and real-time fine-tuning, and the application of small stress tension control, high dimensional accuracy of the finished ultra-thin sheets is ensured.

[0029] 3. The obtained ultra-thin material exhibits good plasticity. Cold-rolled hard ultra-thin materials are annealed in a continuous bright annealing furnace under high-purity hydrogen protection. To improve the plasticity of the ultra-thin material, the lower limit heating temperature specified in the GH3536 alloy standard can be used. The holding time can be appropriately shortened compared to the aforementioned semi-finished product bright annealing or intermediate bright annealing to avoid excessive recrystallization, especially grain growth, which could lead to coarse grains. Furthermore, using a large volume of hydrogen injection to increase the cooling rate after annealing can effectively suppress the excessive precipitation of strengthening phases during slow cooling, thereby significantly reducing the hardness of the finished ultra-thin material. Through the above process measures, such as... Figure 3 and Figure 5 As shown, this results in uniform grain size and no mixed crystal phenomenon in the finished ultrathin material, fewer precipitated strengthening phases, smaller size and more dispersed distribution, and significantly reduced material hardness, thereby greatly improving the plasticity of the finished ultrathin material.

[0030] 4. The obtained ultra-thin material exhibits excellent sheet shape and surface quality. Appropriate low-stress tension control not only ensures high dimensional accuracy of the finished ultra-thin material but also improves its sheet shape, avoiding breakage and warping caused by excessive stress and tension, and lateral bending and surface wrinkling caused by insufficient stress and tension. Furthermore, the finished ultra-thin material undergoes continuous bright annealing under high-purity hydrogen protection, effectively avoiding surface oxidation and ablation during high-temperature annealing, thereby significantly improving the surface quality of the finished ultra-thin material.

[0031] In this invention, the above-described technical solutions can be combined with each other to achieve more preferred combinations. Other features and advantages of this invention will be set forth in the following description, and some advantages may become apparent from the description or be learned by practicing the invention. The objects and other advantages of this invention can be realized and obtained from what is particularly pointed out in the description and drawings. Attached Figure Description

[0032] The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Throughout the drawings, the same reference numerals denote the same parts.

[0033] Figure 1 This is a schematic diagram of the ultrathin material preparation process;

[0034] Figure 2 This is a photo of an actual ultra-thin material.

[0035] Figure 3 The image shows the grain microstructure of Example 1;

[0036] Figure 4 The image shows the grain microstructure of Comparative Example 3;

[0037] Figure 5 This is a photograph of the microstructure of the precipitated phase in Example 1. Detailed Implementation

[0038] Preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form part of this application and are used together with the embodiments of the present invention to illustrate the principles of the present invention, but are not intended to limit the scope of the present invention.

[0039] This invention discloses a method for preparing an ultrathin iron-nickel-based superalloy material, the method comprising:

[0040] Solid solution-treated iron-nickel-based high-temperature alloy plates and coils are used as raw materials;

[0041] Multi-pass rolling, wherein the multi-pass rolling includes a roughing section and a finishing section;

[0042] Bright annealing is performed as an intermediate process between the passes of multi-pass rolling.

[0043] The semi-finished product is bright annealed after the rough rolling section; the finished product is bright annealed after the finish rolling section to obtain an ultra-thin iron-nickel-based high-temperature alloy material.

[0044] Using solution-treated steel coils as billets, such as GH3536 iron-nickel-based high-temperature alloy solution-treated steel coils, provides suitable raw materials for the implementation of continuous cold rolling and continuous bright annealing processes in subsequent four-roll and twenty-roll cold rolling mills. Moreover, the billets are in a solution-soft state after solution treatment, with low hardness, low deformation resistance, and good plasticity, which facilitates the optimization and control of deformation parameters during cold rolling.

[0045] The purpose of intermediate bright annealing, semi-finished bright annealing, and finished bright annealing is to provide soft strip for the next cold rolling process. After the previous cold rolling, the strip's hardness increases dramatically, its plasticity deteriorates, and its deformation resistance becomes extremely high. Continuing to cold roll would cause edge cracks and strip breakage. Therefore, after bright annealing, the deformed structure undergoes recovery recrystallization and grain growth, resulting in uniform grain size, dissolution of precipitates, and a significant reduction in the strip's hardness and deformation resistance, while improving its plasticity and deformation coordination. During intermediate bright annealing, the heating temperature can be set to the upper limit, and the holding time can be appropriately extended to improve the softening effect. Finished bright annealing aims to obtain a soft, ultra-thin finished product and improve the uniformity of the microstructure, resulting in fine, dispersed precipitates and good plasticity, which is beneficial for subsequent cold stamping and welding of honeycomb structures. When performing bright annealing on the finished product, the heating temperature can be set to the lower limit, the holding time does not need to be extended, and a large volume of hydrogen is injected for rapid cooling, thereby improving the overall performance of the ultra-thin material, further enhancing its plasticity and reducing surface oxidation.

[0046] The final result is a high-quality iron-nickel-based high-temperature alloy ultrathin material.

[0047] Specifically, the roughing section is rolled using a four-roll cold rolling mill, and the finishing section is rolled using a twenty-roll cold rolling mill. Commonly used cold rolling equipment for high-temperature alloy cold-rolled strip and foil includes four-roll and twenty-roll cold rolling mills. The former can generally achieve cold rolling with a thickness of 0.1mm, but the processing accuracy cannot be guaranteed for thinner thicknesses. The latter can complete precision cold rolling processing with a thickness below 0.1mm, achieving not only high dimensional accuracy but also good sheet shape and surface quality. Therefore, to complete the cold rolling processing of GH3536 iron-nickel-based high-temperature alloy ultra-thin material (thickness 0.05mm), both types of cold rolling mills can be used in combination: a four-roll cold rolling mill for roughing and a twenty-roll cold rolling mill for finishing. This improves production efficiency while ensuring the quality of the finished product.

[0048] Specifically, the roughing section includes multiple rolling passes, with the left and right tensions of the mill decreasing with each pass; the finishing section also includes multiple rolling passes, with the left and right tensions of the mill decreasing with each pass. The purpose of applying tension during cold rolling is to precisely control the effective deformation of the billet (i.e., the actual reduction, where actual reduction = pre-roll thickness - post-roll thickness) by rationally controlling the tension at a constant rolling rate, considering the different original thicknesses and deformation amounts of the billet in different rolling passes. Furthermore, appropriate low-stress tension control not only contributes to high dimensional accuracy control of the finished ultra-thin sheet but also improves the sheet shape.

[0049] Specifically, the roughing section includes two cold rolling passes; the left and right tension of the first cold rolling pass in the roughing section is 15-20 kN; the left and right tension of the second cold rolling pass in the roughing section is 10-15 kN.

[0050] Specifically, the finishing rolling section includes three cold rolling passes; the left and right tension of the first cold rolling pass of the finishing rolling section is 10-15 kN; the left and right tension of the second cold rolling pass of the finishing rolling section is 8-10 kN; and the left and right tension of the third cold rolling pass of the finishing rolling section is 5-10 kN.

[0051] The principle of optimizing tension control is as follows: During rough rolling, the billet is thicker and the weight per unit volume is larger, so a large stress tension should be applied to ensure that the preferred rolling speed is reached and the degree of deformation can be precisely controlled to avoid side bending and surface wrinkles caused by excessive stress tension; During finish rolling, the billet is thinner and the weight per unit volume is smaller, so a small stress tension should be applied to effectively control the plate shape, surface finish and dimensional accuracy while ensuring the rolling speed, and to avoid breakage and warping caused by excessive stress tension.

[0052] Specifically, the bright annealing temperature is 1065–1105℃, and the strip needs to be rapidly cooled by hydrogen injection before exiting the furnace. The purpose of high-flow-rate hydrogen injection is to ensure that the strip temperature after annealing and holding can be reduced to below 50℃ within 2–3 minutes; therefore, the hydrogen gas flow rate must reach >20 m³ / s. 3 / h. The purpose of rapid cooling after annealing is twofold: first, to suppress the excessive precipitation of strengthening phases in the alloy during the slow cooling process after annealing, which would lead to a surge in strip hardness and a decrease in plasticity; and second, to effectively prevent surface oxidation caused by the strip exiting the furnace at a high temperature, thus affecting surface quality.

[0053] The roughing section includes:

[0054] S1: Use 0.80-1.50mm solid solution iron-nickel-based high-temperature alloy plate coils as billets, cold roll the billets to 0.45-0.80mm, and then perform bright annealing in a hydrogen-protected continuous annealing furnace;

[0055] S2: The cold-rolled material obtained in S1 is cold-rolled to 0.25-0.40mm, and then bright annealed in a hydrogen-protected continuous annealing furnace to obtain a semi-finished thin strip.

[0056] The finishing rolling section includes:

[0057] S3: The semi-finished thin strip obtained in S2 is cold rolled to 0.15-0.20 mm and then bright annealed in a hydrogen-protected continuous annealing furnace;

[0058] S4: The strip obtained in S3 is cold rolled to 0.08-0.10 mm and then bright annealed in a hydrogen-protected continuous annealing furnace;

[0059] S5: The strip obtained in S4 is cold rolled to 0.05±0.004mm and then bright annealed in a hydrogen-protected continuous annealing furnace to obtain the finished ultra-thin material.

[0060] Optimizing the reduction amount and controlling the mill tension during cold rolling helps avoid problems such as edge cracks and strip breakage caused by excessive deformation, as well as poor sheet shape (warping, side bending) due to lack of tension control. Furthermore, appropriate low-stress tension control can improve the surface roughness of ultra-thin strips during cold rolling and prevent wrinkles and side bending. Solution-treated iron-nickel-based high-temperature alloy cold-rolled coils with a thickness between 0.80 and 1.50 mm are commonly used specifications of cold-rolled coils obtained by continuous cold rolling of hot-rolled coils (thickness 2.0–3.0 mm). After annealing, acid and alkali washing, and surface grinding of the above raw materials, solution-treated soft coils are obtained. Because the single-pass cold deformation of GH3536 alloy can reach about 60%, and if the deformation is too small (≤10%), there is a critical deformation leading to mixed crystals. To reduce the number of cold rolling passes and improve production efficiency, the single-pass cold rolling deformation of a four-high cold rolling mill is appropriately controlled at about 50%, which can roll to a thickness of 0.45–0.80 mm. As the strip thickness gradually decreases, the cold rolling process performance of the strip deteriorates, the size effect becomes more prominent, and the ability to coordinate deformation decreases. In other words, it is more sensitive to changes in the deformation amount of each pass. Therefore, the deformation amount of subsequent passes (i.e., the difference between the thickness before and after rolling) gradually decreases.

[0061] A continuous bright annealing furnace under high-purity hydrogen protection can effectively anneal cold-rolled hard strips. It is a specialized piece of equipment for the production of stainless steel, heat-resistant steel, and high-temperature alloy strips and foils. After bright annealing, the cold-rolled hard deformed microstructure undergoes recovery recrystallization and grain growth, resulting in uniform grain size, dissolution of precipitated phases, and a significant reduction in hardness and deformation resistance, while improving plasticity and deformation coordination. Furthermore, considering the microstructure and performance characteristics of ultra-thin high-temperature alloy materials, a high-flow-rate hydrogen injection (hydrogen gas flow rate > 20 m³ / s) is required. 3The rapid cooling process of annealing ( / h) improves the uniformity of the microstructure, further enhances plasticity, and reduces surface oxidation.

[0062] Specifically, the rolling speed in steps S1 to S5 is 0.5–1.0 m / s. Excessive rolling speed increases the strain rate of the metal strip during rolling, leading to overwork and even cracking or breakage. Insufficient rolling speed results in low processing efficiency and negatively impacts the surface quality and dimensional accuracy of the metal strip. Experiments have determined that a rolling speed of 0.5–1.0 m / s is optimal.

[0063] Specifically, the bright annealing temperature in steps S1 to S5 is 1065–1105°C, and the strip needs to be rapidly cooled by hydrogen injection before exiting the furnace (hydrogen gas flow rate > 20 m³ / h). 3 Using a continuous bright annealing furnace under high-purity hydrogen protection, bright annealing at 1065–1105℃ causes the deformed microstructure of the cold-rolled hard strip matrix to undergo recovery recrystallization and grain growth, with precipitated phases dissolving back. This significantly reduces the strip's hardness and deformation resistance, while improving its plasticity. Furthermore, the rapid cooling during the annealing process using large-volume hydrogen injection further enhances plasticity and reduces surface oxidation.

[0064] Specifically, the holding time for bright annealing in steps S1 and S2 is 3 to 5 minutes, and / or the holding time for bright annealing in steps S3 and S4 is 2 to 4 minutes, and / or the holding time for bright annealing in step S5 is 2 to 3 minutes.

[0065] The purpose of intermediate bright annealing is to provide soft strip for the next cold rolling pass, which is beneficial to the completion of subsequent cold rolling processing. Since the intermediate billet is thicker and the weight per unit volume is larger, in order to fully carry out the annealing process and achieve the purpose of softening the strip, the holding time should be extended under the condition of a fixed heating temperature. Therefore, holding the roughing section for 3 to 5 minutes is appropriate.

[0066] As the billet is gradually thinned by cold rolling, the thickness decreases and the weight per unit volume decreases. At this time, the holding time can be shortened to improve processing efficiency and reduce the degree of oxidation on the billet surface. Therefore, the holding time for steps S3 and S4 in the finishing rolling section can be preferably 2 to 4 minutes.

[0067] Specifically, the holding time for bright annealing in step S5 is 2–3 minutes. Bright annealing of the finished product is to obtain a soft, ultra-thin material, improve the uniformity of the microstructure, ensure fine and dispersed precipitates, and enhance plasticity, which is beneficial for subsequent cold stamping and welding of the honeycomb structure. The finished product thickness reaches 0.05 mm, falling within the ultra-thin material range; therefore, the bright annealing holding time should be reduced compared to the blank, thus minimizing oxidation on the finished product surface. Finished product inspection results show that holding for 2–3 minutes and implementing rapid cooling with a large volume of hydrogen spray is beneficial for improving the overall performance of the ultra-thin material.

[0068] Specifically, the solid solution-treated iron-nickel-based superalloy sheet / coil is a GH3536 alloy sheet / coil. The GH3536 ultrathin iron-nickel-based superalloy sheet / coil prepared using the above-mentioned raw materials and the preparation method disclosed in this invention has a thickness tolerance of ±0.004 mm and a dimensional accuracy of ±8%, which is better than the advanced accuracy requirement of ±10% in the national standard GJB3318A2016 (Specification for Cold-Rolled Strip of High-Temperature Alloys for Aerospace). It exhibits good plasticity, with an elongation of 30-50%; good sheet shape, with horizontal warpage ≤10 mm / m; excellent surface quality, with a smooth surface, a roughness Ra value ≤0.20 μm, and no defects such as cracks or oxidation.

[0069] To better illustrate the present invention, the following embodiments are further provided:

[0070] Example 1

[0071] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0072] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of δ1.0mm×200mm is used as billet.

[0073] (2) Cold rolling process, the steps are as follows:

[0074] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.45 mm. The mill tension is 17 kN and the rolling speed is 0.8 m / s.

[0075] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 4 minutes.

[0076] The annealed billet was cold-rolled to a thickness of 0.25 mm, with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0077] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 4 minutes.

[0078] The annealed billet is cold-rolled to a thickness of 0.15 mm using a 20-roll mill with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0079] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0080] Next, cold-roll to a thickness of 0.08 mm, with a mill tension of 9 kN and a rolling speed of 0.8 m / s;

[0081] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0082] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.050 mm, with a left and right tension of 7 kN and a rolling speed of 0.8 m / s.

[0083] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ and a holding time of 2.5min to obtain the finished ultra-thin material.

[0084] The prepared ultra-thin material has high dimensional accuracy; the thickness is 0.050 mm, the tolerance is within ±0.004 mm, and the dimensional accuracy reaches 8%, which is better than the high-precision requirement of ±10% of the national standard GJB3318A2016 (Specification for Cold-Rolled Strip of High-Temperature Alloy for Aerospace); the sheet shape is good: horizontal warpage is 8 mm / m; the surface quality is good: roughness Ra value is 0.18 μm; and the plasticity is good: elongation is 41%.

[0085] Example 2

[0086] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0087] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of δ1.0mm×200mm is used as billet.

[0088] (2) Cold rolling process, the steps are as follows:

[0089] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.65 mm. The mill tension is 17 kN and the rolling speed is 0.8 m / s.

[0090] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 4 minutes.

[0091] The annealed billet was cold-rolled to a thickness of 0.30 mm, with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0092] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 4 minutes.

[0093] The annealed billet is cold-rolled to a thickness of 0.18 mm using a 20-roll mill with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0094] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0095] Next, cold-roll to a thickness of 0.09 mm, with a left and right tension of 9 kN and a rolling speed of 0.8 m / s;

[0096] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0097] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.052 mm, with a left and right tension of 7 kN and a rolling speed of 0.8 m / s.

[0098] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ and a holding time of 2.5min to obtain the finished ultra-thin material.

[0099] The prepared ultrathin material has high dimensional accuracy; thickness 0.052mm, tolerance within ±0.004mm; good plate shape: horizontal warpage 8mm / m; good surface quality: roughness Ra value 0.19μm; good plasticity: elongation 38%.

[0100] Example 3

[0101] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0102] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of 1.5mm and a diameter of 200mm is used as billet.

[0103] (2) Cold rolling process, the steps are as follows:

[0104] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.80 mm. The mill tension is 17 kN and the rolling speed is 0.8 m / s.

[0105] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 4 minutes; the annealed billet was then cold-rolled to a thickness of 0.40 mm with a rolling mill tension of 12 kN and a rolling speed of 0.8 m / s.

[0106] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 4 minutes.

[0107] The annealed billet is cold-rolled to a thickness of 0.20 mm using a 20-roll mill with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0108] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0109] Next, cold-roll to a thickness of 0.10 mm, with a mill tension of 9 kN and a rolling speed of 0.8 m / s;

[0110] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0111] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.054 mm, with a left and right tension of 7 kN and a rolling speed of 0.8 m / s.

[0112] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ and a holding time of 2.5min to obtain the finished ultra-thin material.

[0113] The prepared ultrathin material has high dimensional accuracy; thickness 0.054mm, tolerance within ±0.004mm; good plate shape: horizontal warpage 7mm / m; good surface quality: roughness Ra value 0.18μm; good plasticity: elongation 40%.

[0114] Example 4

[0115] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0116] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of δ1.0mm×200mm is used as billet.

[0117] (2) Cold rolling process, the steps are as follows:

[0118] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.55 mm. The mill tension is 15 kN and the rolling speed is 0.6 m / s.

[0119] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes; the annealed billet was then cold-rolled to a thickness of 0.25 mm with a rolling mill tension of 11 kN and a rolling speed of 0.6 m / s.

[0120] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 3 minutes.

[0121] The annealed billet is cold-rolled to a thickness of 0.17 mm using a 20-roll mill with a left and right tension of 10 kN and a rolling speed of 0.6 m / s.

[0122] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 2 minutes.

[0123] Next, cold-roll to a thickness of 0.09 mm, with a left and right tension of 10 kN and a rolling speed of 0.6 m / s;

[0124] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0125] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.051mm, with a left and right tension of 8kN and a rolling speed of 0.6m / s.

[0126] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ for 2 minutes to obtain the finished ultra-thin material.

[0127] The prepared ultrathin material has high dimensional accuracy; thickness 0.051mm, tolerance within ±0.004mm, good plate shape: horizontal warpage 8mm / m; good surface quality: roughness Ra value 0.19μm; good plasticity: elongation 43%.

[0128] Example 5

[0129] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0130] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of 1.5mm and a diameter of 200mm is used as billet.

[0131] (2) Cold rolling process, the steps are as follows:

[0132] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.70 mm. The mill tension is 20 kN and the rolling speed is 1.0 m / s.

[0133] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 5 minutes.

[0134] The annealed billet was cold-rolled to a thickness of 0.40 mm, with a left and right tension of 15 kN and a rolling speed of 1.0 m / s.

[0135] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 4 minutes.

[0136] The annealed billet is cold-rolled to a thickness of 0.25 mm using a 20-roll mill with a left and right tension of 14 kN and a rolling speed of 1.0 m / s.

[0137] Secondly, annealing is carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3.5 minutes; then, cold rolling is performed to a thickness of 0.10 mm with a rolling mill tension of 9 kN and a rolling speed of 1.0 m / s.

[0138] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3.5 minutes.

[0139] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.053 mm, with a left and right tension of 10 kN and a rolling speed of 1.0 m / s.

[0140] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ for 3 minutes to obtain the finished ultra-thin material.

[0141] The prepared ultrathin material has high dimensional accuracy; thickness 0.053mm, tolerance within ±0.004mm, good plate shape: horizontal warpage 7mm / m; good surface quality: roughness Ra value 0.20μm; good plasticity: elongation 40%.

[0142] Example 6

[0143] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0144] (1) Select billet: annealed soft GH3536 alloy plate coil with δ0.8mm×200mm is used as billet.

[0145] (2) Cold rolling process, the steps are as follows:

[0146] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.48 mm. The mill tension is 18 kN and the rolling speed is 0.5 m / s.

[0147] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1070℃ for 4 minutes.

[0148] The annealed billet was cold-rolled to a thickness of 0.28 mm, with a left and right tension of 13 kN and a rolling speed of 0.5 m / s.

[0149] Next, annealing was performed in a protective atmosphere furnace at a temperature of 1070℃ for 4 minutes.

[0150] The annealed billet is cold-rolled to a thickness of 0.18 mm using a 20-roll mill with a left and right tension of 13 kN and a rolling speed of 0.5 m / s.

[0151] Secondly, annealing is carried out in a protective atmosphere furnace at a temperature of 1070℃ for 3 minutes; then, cold rolling is performed to a thickness of 0.09mm, with a rolling mill tension of 9kN and a rolling speed of 0.5m / s.

[0152] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1070℃ for 3 minutes.

[0153] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.052 mm, with a left and right tension of 8 kN and a rolling speed of 0.5 m / s.

[0154] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1070℃ for 3 minutes to obtain the finished ultra-thin material.

[0155] The prepared ultrathin material has high dimensional accuracy; thickness 0.052mm, tolerance within ±0.004mm, good plate shape: horizontal warpage 9mm / m; good surface quality: roughness Ra value 0.17μm; good plasticity: elongation 45%.

[0156] Example 7

[0157] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0158] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of δ1.0mm×200mm is used as billet.

[0159] (2) Cold rolling process, the steps are as follows:

[0160] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.59 mm. The mill tension is 17 kN and the rolling speed is 0.7 m / s.

[0161] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1100℃ for 3.5 minutes.

[0162] The annealed billet was cold-rolled to a thickness of 0.40 mm, with a left and right tension of 13 kN and a rolling speed of 0.7 m / s.

[0163] Next, annealing was performed in a protective atmosphere furnace at 100°C for 3.5 minutes.

[0164] The annealed billet is cold-rolled to a thickness of 0.20 mm using a 20-roll mill with a left and right tension of 12 kN and a rolling speed of 0.7 m / s.

[0165] Secondly, annealing is carried out in a protective atmosphere furnace at a temperature of 1100℃ and a holding time of 3.5 min; then, cold rolling is performed to a thickness of 0.10 mm, with a rolling mill tension of 9 kN and a rolling speed of 0.7 m / s.

[0166] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1100℃ for 3.5 minutes.

[0167] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.054 mm, with a left and right tension of 6 kN and a rolling speed of 0.7 m / s.

[0168] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1100℃ and a holding time of 2.5min to obtain the finished ultra-thin material.

[0169] The prepared ultrathin material has high dimensional accuracy; thickness 0.054mm, tolerance within ±0.004mm, good plate shape: horizontal warpage 9mm / m; good surface quality: roughness Ra value 0.19μm; good plasticity: elongation 39.5%.

[0170] Comparative Example 1

[0171] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0172] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of 1.5mm and a diameter of 200mm is used as billet.

[0173] (2) Cold rolling process, the steps are as follows:

[0174] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.60 mm (60% deformation). The mill tension is 17 kN and the rolling speed is 0.8 m / s.

[0175] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 4 minutes.

[0176] The annealed billet was cold rolled to a thickness of 0.20 mm (67% deformation), with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0177] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 4 minutes.

[0178] The annealed billet is cold-rolled to an ultra-thin material of 0.054 mm (73% deformation) using a 20-roll precision rolling mill. The mill tension is 7 kN and the rolling speed is 0.8 m / s.

[0179] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ and a holding time of 2.5min to obtain the finished ultra-thin material.

[0180] Comparative Example 1 used a two-pass four-roll cold rolling mill for roughing and a one-pass twenty-roll cold rolling mill for finishing. During the cold rolling process, edge cracks and strip breakage frequently occurred. The reduction design of this process has greatly exceeded the optimal control range of cold deformation preferred in this invention, reaching as high as 73%. At this point, the deformation resistance of the strip surges, the plasticity deteriorates, and strip breakage and cracking become inevitable.

[0181] Comparative Example 2

[0182] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0183] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of δ1.0mm×200mm is used as billet.

[0184] (2) Cold rolling process, the steps are as follows:

[0185] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.80 mm. The mill tension is 17 kN and the rolling speed is 0.8 m / s.

[0186] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 4 minutes; the annealed billet was then cold-rolled to a thickness of 0.60 mm with a rolling mill tension of 17 kN and a rolling speed of 0.8 m / s.

[0187] Then, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 4 minutes.

[0188] The annealed billet was cold-rolled to a thickness of 0.40 mm, with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0189] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 4 minutes.

[0190] The annealed billet is cold-rolled to a thickness of 0.30 mm using a 20-roll mill with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0191] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes; the annealed billet was then cold-rolled to a thickness of 0.20 mm with a rolling mill tension of 12 kN and a rolling speed of 0.8 m / s.

[0192] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0193] Next, cold-roll to a thickness of 0.10 mm, with a mill tension of 9 kN and a rolling speed of 0.8 m / s;

[0194] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 3 minutes.

[0195] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.052 mm, with a left and right tension of 7 kN and a rolling speed of 0.8 m / s.

[0196] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ and a holding time of 2.5min to obtain the finished ultra-thin material.

[0197] Comparative Example 2 employed a 3-pass four-roll cold rolling mill for roughing and a 4-pass twenty-roll cold rolling mill for finishing. Compared to the 2-pass roughing and 3-pass finishing of this invention, the number of rolling passes for both roughing and finishing is increased. The finished ultra-thin material was inspected as follows:

[0198] The prepared ultrathin material has high dimensional accuracy; thickness 0.052mm, tolerance within ±0.004mm; good plate shape: horizontal warpage 8mm / m; good surface quality: roughness Ra value 0.19μm; good plasticity: elongation 43%.

[0199] As can be seen, compared with the embodiments of the present invention, the results of Comparative Example 2 show no significant changes in dimensional accuracy, plate shape, surface quality, and plasticity, and the quality of the finished ultra-thin material is basically the same. Therefore, increasing the number of rough rolling and finish rolling passes in the process has no adverse effects, but increasing the number of bright annealing processes also increases the process time, inevitably leading to a significant increase in production costs.

[0200] Comparative Example 3

[0201] The preparation method of ultrathin iron-nickel-based superalloy materials includes the following steps:

[0202] (1) Select billet: annealed soft GH3536 alloy plate coil with a diameter of δ1.0mm×200mm is used as billet.

[0203] (2) Cold rolling process, the steps are as follows:

[0204] First, a four-roll cold rolling mill is used for rough rolling to cold roll the billet to a thickness of 0.45 mm. The mill tension is 17 kN and the rolling speed is 0.8 m / s.

[0205] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 1.5 minutes.

[0206] The annealed billet was cold-rolled to a thickness of 0.25 mm, with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0207] Next, annealing was performed in a protective atmosphere furnace at 1080℃ for 1.5 minutes. The annealed billet was then cold-rolled to a thickness of 0.15 mm using a 20-roll mill with a left and right tension of 12 kN and a rolling speed of 0.8 m / s.

[0208] Secondly, annealing is carried out in a protective atmosphere furnace at a temperature of 1080℃ and a holding time of 1.5 min; then, cold rolling is performed to a thickness of 0.08 mm, with a rolling mill tension of 9 kN and a rolling speed of 0.8 m / s.

[0209] Secondly, annealing was carried out in a protective atmosphere furnace at a temperature of 1080℃ for 1.5 minutes.

[0210] Finally, it is cold-rolled to an ultra-thin material with a thickness of 0.050 mm, with a left and right tension of 7 kN and a rolling speed of 0.8 m / s.

[0211] (3) The cold-rolled ultra-thin material is subjected to continuous bright annealing under hydrogen protection at a temperature of 1080℃ and held for 1 minute to obtain the finished ultra-thin material.

[0212] As can be seen, compared with the embodiments of the present invention, the holding time for intermediate and finished bright annealing in Comparative Example 3 is significantly shortened. The intermediate annealing holding time is reduced from 3-4 min to 1.5 min, leading to the following problems during roughing and finishing cold rolling: due to insufficient holding time, the annealing softening effect is poor, the billet hardness remains high, resulting in increased deformation resistance, and low plasticity, leading to strip edge cracking and breakage. Furthermore, the finished annealing holding time is reduced from 2.5 min to 1 min, resulting in the following issues during quality inspection of the finished ultra-thin material: low plasticity (<30%), poor microstructure uniformity, residual deformed structures, poor sheet shape, and horizontal warpage >10 mm / m. Therefore, it can be concluded that improper control of intermediate and finished annealing holding time will greatly affect the precise control of the cold rolling process of ultra-thin material and cause unqualified finished product quality.

[0213] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing an ultra-thin iron-nickel based superalloy material, characterized in that: The preparation method includes: Solid solution-treated iron-nickel-based high-temperature alloy plates and coils are used as raw materials; Multi-pass rolling, wherein the multi-pass rolling includes a roughing section and a finishing section; Bright annealing is performed as an intermediate process between the passes of multi-pass rolling. The semi-finished product is bright annealed after the rough rolling section; the finished product is bright annealed after the finish rolling section. The roughing section includes multiple rolling passes, with the left and right tensions of the mill decreasing with each pass; the finishing section includes multiple rolling passes, with the left and right tensions of the mill decreasing with each pass. The bright annealing temperature is 1065–1105℃, and the strip needs to be rapidly cooled by hydrogen injection before exiting the furnace. The hydrogen gas flow rate should reach >20m³ / h. 3 / h; The roughing section includes: S1: Use 0.80-1.50mm solid solution iron-nickel-based high-temperature alloy plate coils as billets, cold roll the billets to 0.45-0.80mm, and then perform bright annealing in a hydrogen-protected continuous annealing furnace; S2: The cold-rolled material obtained in S1 is cold-rolled to 0.25-0.40mm, and then bright annealed in a hydrogen-protected continuous annealing furnace to obtain a semi-finished thin strip. The finishing rolling section includes: S3: The semi-finished thin strip obtained in S2 is cold rolled to 0.15-0.20 mm and then bright annealed in a hydrogen-protected continuous annealing furnace; S4: The strip obtained in S3 is cold rolled to 0.08-0.10 mm and then bright annealed in a hydrogen-protected continuous annealing furnace; S5: The strip obtained in S4 is cold rolled to 0.05±0.004mm and then bright annealed in a hydrogen-protected continuous annealing furnace to obtain the finished ultra-thin material; The rolling speed in steps S1 to S5 is 0.5 to 1.0 m / s.

2. The production method according to claim 1, characterized by, The roughing section is rolled using a four-roll cold rolling mill, and the finishing section is rolled using a twenty-roll cold rolling mill.

3. The preparation method according to claim 1, characterized in that, The left and right tension of the first cold rolling pass in the roughing section is 15-20 kN; the left and right tension of the second cold rolling pass in the roughing section is 10-15 kN.

4. The preparation method according to claim 1, characterized in that: The left and right tension of the first cold rolling pass in the finishing section is 10-15 kN; the left and right tension of the second cold rolling pass in the finishing section is 8-10 kN; and the left and right tension of the third cold rolling pass in the finishing section is 5-10 kN.

5. The preparation method according to claim 1, characterized in that: The bright annealing temperature is 1080–1105°C.

6. The preparation method according to claim 1, characterized in that: The holding time for bright annealing in steps S1 and S2 is 3 to 5 minutes, and / or the holding time for bright annealing in steps S3 and S4 is 2 to 4 minutes, and / or the holding time for bright annealing in step S5 is 2 to 3 minutes.

7. The preparation method according to any one of claims 1 to 6, characterized in that: The solid solution-treated iron-nickel-based high-temperature alloy sheet / coil is a GH3536 alloy sheet / coil.

8. A thin iron-nickel-based high-temperature alloy material, characterized in that: It is prepared by the preparation method according to any one of claims 1 to 7.

Images