A method for preparing GH4169 alloy foil

Abstract

This invention provides a method for preparing GH4169 alloy foil, comprising the following steps: solution treatment of GH4169 alloy sheet; first-stage rolling and intermediate annealing of GH4169 alloy sheet; second-stage rolling and intermediate vacuum annealing of GH4169 alloy sheet; and annealing of the finished GH4169 alloy foil. This method for preparing GH4169 alloy foil fully utilizes the control effect of large deformation rolling and annealing on precipitated phases, as well as the influence of precipitated phases on grain size, to obtain alloy foil with uniform microstructure. Furthermore, the process is simple, low-cost, and economically efficient.

Description

Technical Field

[0001] This invention relates to the field of foil preparation technology, and in particular to a method for preparing GH4169 alloy foil based on a multi-stage rolling and annealing process. Background Technology

[0002] High-precision, ultra-thin strips are widely used in aerospace, electronics and communications, and chemical industries, serving as a crucial foundation for the development of cutting-edge science and technologies. GH4169 high-temperature alloy possesses excellent machinability and is widely used in harsh environments such as high temperature, high pressure, and overload cycling, making it one of the most important industrial materials.

[0003] During the rolling process, GH4169 high-temperature alloy undergoes severe work hardening, which increases the difficulty of the forming process. Furthermore, the influence of specimen geometry and material microstructure on plastic deformation behavior remains unclear. Therefore, the rolling and heat treatment process parameters in the preparation of high-temperature alloy foils require further exploration. Thus, research on the preparation process of high-temperature alloy foils has certain application value.

[0004] The distribution, morphology, and volume fraction of precipitated phases in GH4169 high-temperature alloy affect the mechanical properties of the foil. Selecting appropriate rolling and annealing processes to control the microstructure is an effective method to improve product performance. Currently, there is an urgent need for a simple, low-cost process for preparing GH4169 alloy foil that produces a uniform microstructure, providing a reference for the industrial production of GH4169 alloy foil. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for preparing GH4169 alloy foil with a simple process, low cost and uniform microstructure based on multi-stage rolling and annealing process.

[0006] To solve the above-mentioned technical problems, the present invention provides a method for preparing GH4169 alloy foil, comprising the following steps:

[0007] Solution treatment of GH4169 alloy plates is performed at a temperature of 1040-1050℃, followed by air cooling after holding at that temperature for 0.5-1 hour.

[0008] The first stage of rolling and intermediate annealing: GH4169 alloy sheet is rolled into 0.09-0.12mm sheet in multiple rolling processes, with a rolling deformation of ≥ 95%, and intermediate annealing is performed after each rolling process;

[0009] The second stage of rolling: the 0.12-0.09 mm plate is rolled into 0.05-0.08 mm GH4169 alloy foil and then subjected to intermediate vacuum annealing.

[0010] The finished GH4169 alloy foil is annealed at 900℃-960℃ for 10-300 min and then furnace cooled.

[0011] Furthermore, the initial thickness of the GH4169 alloy sheet is no greater than 3 mm.

[0012] Furthermore, for GH4169 alloy plates with a thickness greater than 2 mm, intermediate annealing is performed when the GH4169 alloy plates are rolled to a thickness of 0.45-0.55 mm, 0.35-0.4 mm, 0.28-0.32 mm and 0.12-0.09 mm respectively.

[0013] Furthermore, for GH4169 alloy plates with a thickness of no more than 2 mm, intermediate annealing is performed when the GH4169 alloy plates are rolled to a thickness of 0.35-0.4 mm, 0.28-0.32 mm and 0.12-0.09 mm respectively.

[0014] Furthermore, when the GH4169 alloy sheet is rolled to 0.32-0.28mm, it needs to be pickled and trimmed.

[0015] Furthermore, when the GH4169 alloy sheet is rolled to a thickness of not less than 0.32-0.28 mm, the intermediate annealing temperature is 920℃-980℃, held for 10-30 min, and then air-cooled.

[0016] Furthermore, when the GH4169 alloy sheet is rolled to a thickness of less than 0.32-0.28 mm, the intermediate annealing treatment adopts vacuum annealing treatment, the annealing temperature is 920℃-980℃, and the heat is held for 10-30 min before furnace cooling.

[0017] Furthermore, the vacuum annealing process is carried out in an annealing furnace protected by an inert gas.

[0018] Furthermore, the first stage of rolling is carried out using a four-roll cold rolling mill, and the second stage of rolling is carried out using a twenty-roll cold rolling mill.

[0019] Furthermore, the GH4169 alloy foil has a grain size of 1.7-3.4 μm, a tensile strength of 1020-1400 MPa, and an elongation of 6-16%.

[0020] This invention provides a method for preparing GH4169 alloy foil, based on a multi-stage rolling and multiple annealing process. The method involves solution treatment of GH4169 alloy sheet, multi-stage large deformation cold rolling, intermediate annealing, and final annealing, along with optimized control of process parameters at each stage. This yields GH4169 alloy foil with a thickness of 0.05-0.08 mm and high microstructure homogeneity. Under room temperature tensile testing, the obtained GH4169 alloy foil exhibits a tensile strength of 1020-1400 MPa and an elongation of 6-16%.

[0021] Furthermore, the preparation method of GH4169 alloy foil provided by the present invention utilizes a process of alternating large deformation rolling and intermediate annealing, which can fully promote the uniform precipitation of δ phase. Finally, the finished product annealing process is adopted, which utilizes the pinning effect of δ phase on grain boundaries to finally obtain GH4169 alloy foil with a uniform fine-grained structure with a grain size of 1.7-3.4 μm.

[0022] Meanwhile, the preparation method of GH4169 alloy foil provided by the present invention has strong process continuity, simple process, high production efficiency, and can save energy and reduce production costs. Attached Figure Description

[0023] Figure 1 A flowchart illustrating the preparation method of GH4169 alloy foil provided in this embodiment of the invention;

[0024] Figure 2 Temperature variation diagrams of each step in the preparation method of GH4169 alloy foil provided in various embodiments of the present invention;

[0025] Figure 3 Micrograph of the alloy sheet obtained by the GH4169 alloy foil preparation method provided in Example 1 of this invention;

[0026] Figure 4 Micrograph of the alloy sheet prepared by the GH4169 alloy foil preparation method provided in Example 2 of the present invention;

[0027] Figure 5 Micrograph of the alloy sheet obtained by the GH4169 alloy foil preparation method provided in Example 3 of the present invention;

[0028] Figure 6 The room temperature tensile curve of the alloy sheet prepared by the GH4169 alloy foil preparation method provided in Example 1 of this invention;

[0029] Figure 7 The room temperature tensile curve of the alloy sheet prepared by the GH4169 alloy foil preparation method provided in Example 2 of the present invention;

[0030] Figure 8 The room temperature tensile curve of the alloy sheet prepared by the GH4169 alloy foil preparation method provided in Example 3 of the present invention. Detailed Implementation

[0031] See Figure 1 The present invention provides a method for preparing GH4169 alloy foil, comprising the following steps:

[0032] Step 1) Solution treatment of GH4169 alloy sheet. Because the GH4169 alloy in the receiving state has high microhardness and large deformation resistance, the GH4169 alloy sheet is first solution treated to soften the material, facilitating subsequent multi-stage large deformation cold rolling. During solution treatment, the temperature is controlled at 1040-1050℃, and the solution treatment time is controlled at 0.5-1 hour. After solution treatment, the GH4169 alloy sheet is air-cooled to room temperature. The initial thickness of the GH4169 alloy sheet is no greater than 3 mm.

[0033] Step 2) First stage rolling: The GH4169 alloy sheet is rolled into 0.09-0.12mm sheet in multiple stages using a four-roll cold rolling mill, and intermediate annealing is performed during each rolling process.

[0034] For GH4169 alloy plates with a thickness greater than 2 mm, intermediate annealing is performed when the GH4169 alloy plates are rolled to thicknesses of 0.45-0.55 mm, 0.35-0.4 mm, 0.28-0.32 mm, and 0.12-0.09 mm, respectively. For GH4169 alloy plates with a thickness of no more than 2 mm, intermediate annealing is performed when the GH4169 alloy plates are rolled to thicknesses of 0.35-0.4 mm, 0.28-0.32 mm, and 0.12-0.09 mm, respectively.

[0035] When the GH4169 alloy sheet is rolled to a thickness of 0.32-0.28mm or more, the temperature of each intermediate annealing treatment is controlled at 920℃-980℃, and after holding at that temperature for 10-30 minutes, it is air-cooled to room temperature.

[0036] When GH4169 alloy sheets are rolled to a thickness of 0.32-0.28 mm or less, vacuum annealing is used for each intermediate annealing process. That is, an inert gas such as argon is filled into a vacuum annealing furnace, allowing the GH4169 alloy sheet to undergo annealing under inert gas protection. Since the GH4169 alloy sheet is already very thin when rolled to 0.32-0.28 mm, annealing it under the protection of an inert gas such as argon can prevent oxidation caused by excessive thinness, which would affect the processing effect of the sheet. The annealing temperature is controlled at 920℃-980℃, and after holding at that temperature for 10-30 minutes, the GH4169 alloy sheet is cooled to room temperature in the annealing furnace.

[0037] Furthermore, the first stage of rolling employs a large deformation rolling process with a total rolling deformation of ≥95%. The crystal defects introduced by the large deformation rolling not only provide nucleation sites for the δ phase but also provide recrystallization driving force. Combined with intermediate annealing, this can alleviate the work hardening phenomenon that occurs during the rolling process of GH4169 alloy. Moreover, the increased grain boundary aggregated dislocations can also fully promote the precipitation of granular δ phase, promote static recrystallization of GH4169 alloy, and ultimately obtain a homogeneous microstructure.

[0038] Meanwhile, when GH4169 alloy sheets are cold-rolled to a thickness of 0.32-0.28mm, pickling and edge trimming are required. Pickling removes oxides from the surface of the GH4169 alloy sheets, ensuring a bright and smooth surface before finishing rolling. After pickling, edge trimming removes portions of the sheet that do not meet thickness requirements.

[0039] Step 3) Second stage rolling: Use a 20-roll cold rolling mill to finish roll 0.12-0.09 mm sheet into 0.05-0.08 mm GH4169 alloy foil. The intermediate annealing treatment is vacuum annealing at a temperature of 920℃-980℃, held for 10-30 min and then furnace cooled.

[0040] Step 4) Annealing treatment of the finished GH4169 alloy foil. After GH4169 alloy sheet is rolled into GH4169 alloy foil through large deformation rolling and short-time intermediate annealing, the δ phase in the GH4169 alloy foil precipitates uniformly and densely, retaining a large amount of stored energy. The uniformly distributed δ phase can pin grain boundaries to the same extent to hinder grain growth during subsequent annealing, resulting in a uniform microstructure. Therefore, after multi-stage large deformation cold rolling and intermediate annealing, the GH4169 alloy foil is subjected to finished annealing treatment. During finished annealing, the GH4169 alloy foil is placed in a vacuum box annealing furnace, the temperature inside the box annealing furnace is adjusted to 900℃-960℃, the holding time is 10-300 min, and then the furnace is cooled to room temperature.

[0041] This invention provides a method for preparing GH4169 alloy foil. The method involves solution treatment of GH4169 alloy sheets with a thickness not exceeding 3 mm, multi-stage large deformation cold rolling, intermediate annealing, and final annealing, along with optimized control of process parameters during each process. This yields GH4169 alloy foil with a thickness of 0.05-0.08 mm. Since defects generated during large deformation cold rolling and grain boundaries added during annealing provide nucleation sites for precipitates, this method effectively promotes the precipitation of the δ phase. Furthermore, the δ phase pins grain boundaries during final annealing, hindering growth and ultimately resulting in GH4169 alloy foil with a uniform microstructure and a smooth surface. Tensile properties of the GH4169 alloy foil at room temperature show a tensile strength of 1020-1400 MPa and an elongation of 6-16%.

[0042] The following examples illustrate a specific method for preparing GH4169 alloy foil provided by the present invention.

[0043] The original thickness of the GH4169 alloy sheet provided in each embodiment of the present invention is 2-3 mm. The chemical composition and content of each component of the GH4169 alloy sheet are shown in Table 1.

[0044] Table 1 Chemical composition and content of GH4169 high-temperature alloy sheet

[0045]

[0046] The temperature variations of each annealing process in each embodiment are as follows: Figure 2 As shown, the specific process of each embodiment is as follows.

[0047] Example 1

[0048] 1) Solution treatment: The treatment temperature is 1050℃, the holding time is 1 h, and then air cooling is performed.

[0049] 2) First stage rolling and intermediate annealing: The original thickness of the alloy plate is 2 mm. It is rough rolled to 0.1 mm by a four-roll cold rolling mill. Intermediate annealing is performed at 0.35 mm: temperature is 950℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.3 mm: temperature is 920℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.1 mm: temperature is 950℃, holding time is 10 min, and furnace cooling is performed.

[0050] 3) Second stage rolling: The 0.1 mm alloy plate is rolled to 0.05 mm by a 20-roll cold rolling mill. The intermediate annealing treatment is vacuum annealing at a temperature of 920℃-980℃. After holding at the temperature for 10-30 minutes, it is furnace cooled.

[0051] Throughout the rolling process, the total rolling deformation rate was controlled at 97.5%.

[0052] 4) Finished product annealing treatment: The treatment temperature is 950℃ and the holding time is 10 min.

[0053] This embodiment ultimately yields an alloy foil with a thickness of 0.05 mm, and its microstructure is as follows: Figure 3 As shown. From Figure 3 It can be seen that the alloy foil obtained in this embodiment has a high degree of microstructure homogeneity, with an average grain size of 1.78 μm, a tensile strength of 1024 MPa, and an elongation of 6.93%.

[0054] See Figure 6 A tensile test was conducted on the alloy foil obtained in Example 1 of the present invention at room temperature. It can be seen that the alloy foil obtained in Example 1 of the present invention exhibits good plasticity, with a tensile strength of 1024 MPa and an elongation of 6.93%.

[0055] Example 2

[0056] 1) Solution treatment: The treatment temperature is 1050℃, the holding time is 1 h, and then air cooling is performed.

[0057] 2) First stage rolling and intermediate annealing: The original thickness of the alloy plate is 2 mm. It is rough rolled to 0.1 mm by a four-roll cold rolling mill. Intermediate annealing is performed at 0.35 mm: temperature is 950℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.3 mm: temperature is 920℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.1 mm: temperature is 950℃, holding time is 10 min, and furnace cooling is performed.

[0058] 3) Second stage rolling: The 0.1 mm alloy plate is rolled to 0.05 mm by a 20-roll cold rolling mill. The intermediate annealing treatment is vacuum annealing at a temperature of 920℃-980℃. After holding at the temperature for 10-30 minutes, it is furnace cooled.

[0059] Throughout the rolling process, the total rolling deformation rate was controlled at 97.5%.

[0060] 4) Finished product annealing treatment: The treatment temperature is 900℃, the holding temperature is 240 min, and the furnace temperature is raised to 950℃ and the holding time is 60 min.

[0061] This embodiment ultimately yields an alloy foil with a thickness of 0.05 mm, and its microstructure is as follows: Figure 4 As shown. From Figure 4 It can be seen that the alloy foil obtained in this embodiment has a high degree of microstructure homogeneity, with an average grain size of 2.68 μm, a tensile strength of 1305 MPa, and an elongation of 12.8%.

[0062] See Figure 7 A tensile test was conducted on the alloy foil obtained in Example 2 of the present invention at room temperature. It can be seen that the alloy foil obtained in Example 2 of the present invention exhibits good plasticity, with a tensile strength of 1305 MPa and an elongation of 12.8%.

[0063] Example 3

[0064] 1) Solution treatment: The treatment temperature is 1050℃, the holding time is 1 h, and then air cooling is performed.

[0065] 2) First stage rolling and intermediate annealing: The original thickness of the alloy sheet is 3 mm. It is rough rolled to 0.1 mm by a four-roll cold rolling mill. Intermediate annealing is performed at 0.5 mm: temperature is 950℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.35 mm: temperature is 920℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.3 mm: temperature is 920℃, holding time is 10 min, and air cooling is performed. Intermediate annealing is performed at 0.1 mm: temperature is 950℃, holding time is 10 min, and furnace cooling is performed.

[0066] 3) Second stage rolling: The 0.1 mm alloy plate is rolled to 0.08 mm by a 20-roll cold rolling mill. The intermediate annealing treatment is vacuum annealing at a temperature of 920℃-980℃. After holding at the temperature for 10-30 minutes, it is furnace cooled.

[0067] Throughout the rolling process, the total rolling deformation rate was controlled at 97.5%.

[0068] 4) Finished product annealing treatment: The treatment temperature is 950℃ and the holding time is 10 min.

[0069] This embodiment ultimately yields an alloy foil with a thickness of 0.08 mm, and its microstructure is as follows: Figure 5 As shown. From Figure 5 It can be seen that the alloy foil obtained in this embodiment has a high degree of microstructure homogeneity, with an average grain size of 2.44 μm, a tensile strength of 1092 MPa, and an elongation of 13.28%.

[0070] See Figure 8Tensile tests were conducted on the alloy foil obtained in Example 3 of the present invention at room temperature. A comparison with the tensile curve of the cold-rolled state shows that the alloy foil obtained in Example 3 of the present invention exhibits good plasticity and an elongation of up to 13.28%.

[0071] Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to examples, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A method of producing a GH4169 alloy foil, characterized by, The method comprises the following steps: solid solution treatment of the GH4169 alloy plate at a temperature of 1040-1050℃ for 0.5-1h, and then air cooling; first stage rolling and intermediate annealing: the GH4169 alloy plate is rolled into a 0.09-0.12mm plate in multiple times, with a rolling deformation of ≥95%, and intermediate annealing is performed after each rolling; second stage rolling: the 0.12-0.09mm plate is rolled into a 0.05-0.08mm GH4169 alloy foil, and intermediate vacuum annealing is performed; final annealing of the GH4169 alloy foil at a temperature of 900℃-960℃ for 10-300min, and then furnace cooling.

2. The method of making a GH4169 alloy foil according to claim 1, wherein: The initial thickness of the GH4169 alloy plate is not more than 3mm.

3. The method of claim 2, wherein: For the GH4169 alloy plate with a thickness of more than 2mm, intermediate annealing is performed when the GH4169 alloy plate is rolled to a thickness of 0.45-0.55mm, 0.35-0.4mm, 0.28-0.32mm and 0.12-0.09mm.

4. The method of making a GH4169 alloy foil according to claim 2, wherein: For the GH4169 alloy plate with a thickness of not more than 2mm, intermediate annealing is performed when the GH4169 alloy plate is rolled to a thickness of 0.35-0.4mm, 0.28-0.32mm and 0.12-0.09mm.

5. The method of producing a GH4169 alloy foil according to claim 3 or 4, characterized in that: The GH4169 alloy plate needs to be pickled and edge cut when rolled to a thickness of 0.32-0.28mm.

6. The method of producing a GH4169 alloy foil according to claim 3 or 4, characterized in that: When the GH4169 alloy plate is rolled to a thickness of not less than 0.30mm, the intermediate annealing is performed at a temperature of 920℃-980℃ for 10-30min, and then air cooling is performed.

7. The method of making a GH4169 alloy foil according to claim 3 or 4, wherein: When the GH4169 alloy plate is rolled to a thickness of less than 0.30mm, the intermediate annealing is performed by vacuum annealing at a temperature of 920℃-980℃ for 10-30min, and then furnace cooling is performed.

8. The method of making a GH4169 alloy foil according to claim 7, wherein: The vacuum annealing is performed in an inert gas protected annealing furnace.

9. The method of making a GH4169 alloy foil of claim 1 wherein: The first stage rolling is performed by a four-roll cold rolling mill, and the second stage rolling is performed by a twenty-roll cold rolling mill.

10. The method of making a GH4169 alloy foil according to claim 9, wherein: The grain size of the GH4169 alloy foil is 1.7-3.4μm, the tensile strength is 1020-1400MPa, and the elongation is 6-16%.

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