A titanium alloy foil strip and its preparation method

Through the high-precision reversible rolling mill and reasonable annealing process, the rolling method of titanium alloy foil is solved, and the existing cumbersome process and low efficiency are achieved, and the titanium alloy foil that meets the performance requirements of hydrogen fuel cell plates is achieved.

CN115301734BActive Publication Date: 2025-07-22PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP +1
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Patent Information

Application Number
CN202210945642.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-08-08
Publication Date
2025-07-22
Estimated Expiration
2042-08-08

AI Technical Summary

Technical Problem

The existing titanium alloy foil has cumbersome preparation technology, low production efficiency, and difficult product consistency control, making it difficult to meet the comprehensive performance needs of hydrogen fuel cell plates.

Method used

The titanium alloy cold-rolled coil is used as raw material, and a high-precision reversible rolling mill is used to design the coiled rolling of titanium alloy foil through reasonable cold-rolling deformation and annealing process, including multi-pass reversible rolling, online argon protection annealing and vacuum annealing treatment.

Benefits of technology

The production of high material yield and large single heavy foil reels has been achieved. The thickness accuracy and plate shape of the material under extremely thin specifications are good, which meets the comprehensive performance indicators of hydrogen fuel cell plates and the microchannel forming processing requirements, and improves production efficiency and moldability.

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Abstract

The present invention relates to a method for preparing a titanium alloy foil strip coil, and the steps are as follows: Select pickled and annealed cold-rolled strip coil as the raw material; perform the first rolling pass on the raw material to obtain the first cold-rolled strip coil; perform on-line annealing treatment on the first cold-rolled strip coil to obtain the first cold-rolled strip coil after intermediate annealing treatment; perform the second rolling pass on the first cold-rolled strip coil after intermediate annealing treatment to obtain the second cold-rolled strip coil; perform vacuum annealing treatment on the second cold-rolled strip coil to obtain the second cold-rolled strip coil after intermediate annealing treatment; perform the third rolling pass on the second cold-rolled strip coil after intermediate annealing treatment to obtain the rolled foil strip coil; perform vacuum annealing treatment on the rolled foil strip coil for the finished product to prepare the finished titanium alloy foil strip coil. The present invention uses a titanium alloy cold-rolled strip coil as the raw material, utilizes a high-precision reversible rolling mill, and through reasonable cold-rolling deformation process and annealing process design, conducts coiling rolling production of titanium alloy foil, and obtains high-yield and large-single-weight foil strip coil products.
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Description

Technical Field

[0001] The present invention belongs to the technical field of titanium alloy foil preparation, and specifically relates to a method for preparing a titanium alloy foil for a hydrogen fuel cell bipolar plate by coiling and rolling, and more specifically, to a method for preparing a titanium alloy foil coil and a titanium alloy foil coil prepared by the preparation method. Background Art

[0002] Hydrogen fuel cells have the advantages of zero pollution and high efficiency, and are an important development direction for the next generation of clean energy. At present, my country's fuel cells have a low life span and high cost, which restricts the development of industrialization. Bipolar plates are the main components that determine the life span and cost of fuel cells, and must meet comprehensive performance requirements such as corrosion resistance and conductivity, long life, ultra-thinness and high strength, and easy processing. The existing stainless steel substrates are in conflict with corrosion resistance and conductivity, and rely on coatings. The composite graphite substrates have strength and conductivity conflicts and cannot be taken into account. They are difficult to meet the application requirements of fuel cells. It is urgent to develop special substrates and mass preparation processes to fundamentally solve the performance and cost bottlenecks of the plates.

[0003] Due to the physical properties of titanium alloys such as low elastic modulus, high deformation resistance, and poor formability, there have always been many technical problems in the preparation of titanium alloy foil. The patent application number is CN202110715396.8, and the invention name is "A method for preparing fine-grained TA15 titanium alloy foil". The patent document involves a method for preparing TA15 titanium alloy foil, which specifically involves forging and hot-rolling the TA15 ingot to obtain a 4mm thick slab, shearing and welding the slab, and then coating the surface with a steel plate to make a coated rolling package. After multiple rolling passes, a 0.1-0.2mm rolled foil is obtained; the patent application number is 202110715398.7, and the invention name is The patent document "A method for preparing high-strength ultrafine-grained TC4 titanium alloy foil" involves a method for preparing TC4 titanium alloy foil, which specifically involves forging a TC4 titanium alloy ingot to obtain a blank, then hot-rolling the blank into a slab, welding the resulting slab to obtain a coated stacked rolling package, then hot-rolling, disassembling the stacked rolling package, welding the blank for a second time to obtain a coated stacked rolling package, rolling perpendicular to the last rolling direction, shearing the plate after rolling, and cold-rolling 3-7 times to obtain a rolled foil with a thickness of 0.08-0.2mm. The key point of the above two invention patent documents is the design of the coated stacked rolling package, which can use a hot rolling mill to roll the intermediate slab thinner, and then cold-roll to obtain a 0.1-0.2mm titanium alloy foil, but these process methods have problems such as cumbersome procedures, low production efficiency, and difficulty in controlling product consistency.

[0004] Therefore, it is desirable to design a method for preparing a titanium alloy foil coil that overcomes the above-mentioned defects. Summary of the invention

[0005] In view of the deficiencies of the prior art, in response to the demand for titanium alloy foils in hydrogen fuel cell plates, the present invention uses cold-rolled coils of titanium alloy as raw materials, and utilizes a high-precision reversible rolling mill. Through reasonable design of cold rolling deformation process and annealing process, the coiled rolling preparation of titanium alloy foils is carried out.

[0006] To solve the above technical problems, the present invention adopts the following technical solutions:

[0007] According to one aspect of the present invention, there is provided a method for preparing a coiled strip of titanium alloy foil, comprising the following steps:

[0008] 1) Select pickled and annealed cold-rolled coils made of titanium alloy materials as raw materials;

[0009] 2) Perform the first rolling pass on the raw materials to obtain the first cold-rolled coil;

[0010] 3) Perform on-line annealing treatment on the first cold-rolled coil in an argon-protected continuous annealing furnace to obtain the first intermediate annealed cold-rolled coil;

[0011] 4) Perform the second rolling pass on the first intermediate annealed cold-rolled coil to obtain the second cold-rolled coil;

[0012] 5) Perform vacuum annealing treatment on the second cold-rolled coil in a bell-type vacuum annealing furnace to obtain the second intermediate annealed cold-rolled coil;

[0013] 6) Perform the third rolling pass on the second intermediate annealed cold-rolled coil to obtain the rolled foil coil;

[0014] 7) Perform vacuum annealing treatment on the rolled foil coil as the finished product in a bell-type vacuum annealing furnace to prepare the finished product of the coiled strip of titanium alloy foil.

[0015] In an embodiment of the present invention, in step 1), the thickness of the raw material is 3.0 - 3.5 mm, the width is 300 - 500 mm, the length is 80 - 120 m, and the weight is 400 - 600 kg.

[0016] In an embodiment of the present invention, in step 2), when performing the first rolling pass, the rolling speed is 2 - 5 m / s, the pass reduction is 20 - 30%, and multi-pass reversible rolling is carried out by using coiling machines respectively equipped at the inlet end and the outlet end of the rolling mill. The reduction of the final pass is 20 - 25%, and the final rolling thickness is 1.0 - 1.5 mm.

[0017] In an embodiment of the present invention, in step 3), the furnace body length of the annealing furnace is 25 - 30 m, the annealing temperature is 700 - 750 °C, the coiling speed during annealing is 2 - 6 m / min, and the argon concentration in each section of the annealing furnace is greater than 95%.

[0018] In one embodiment of the present invention, in step 4), when the second rolling process is carried out, the rolling speed is 8-10m / s, the deformation amount of each pass is 10-20%, and the coilers respectively equipped at the inlet and outlet ends of the rolling mill are used to carry out multiple passes of reversible rolling, the deformation amount of the final rolling pass is 10-15%, and the final rolling thickness is 0.3-0.5mm.

[0019] In one embodiment of the present invention, during the vacuum annealing process in step 5), the entire second cold-rolled coil is placed in a hood-type vacuum annealing furnace and evacuated to a vacuum degree of ≤10 -3 After Pa, the temperature is raised for annealing heat treatment, the heating rate is 60-100℃ / h, the annealing temperature is 650-680℃, the holding time is 6-8h, and then it is cooled to room temperature in the hood-type vacuum annealing furnace and taken out of the furnace to obtain the second intermediate annealing cold-rolled coil.

[0020] In one embodiment of the present invention, in step 6), when the third rolling process is carried out, the rolling speed is 10-15m / s, the deformation amount of each pass is 5-20%, and the coilers respectively equipped at the inlet and outlet ends of the rolling mill are used to carry out multiple reversible rolling passes, the deformation amount of the final rolling pass is 5-10%, and the final rolling thickness is 0.1-0.15mm.

[0021] In one embodiment of the present invention, during the vacuum annealing process in step 7), the entire rolled foil strip is placed in a hood-type vacuum annealing furnace and evacuated to a vacuum degree of ≤10 -3 Pa, the temperature is raised for annealing heat treatment, the heating rate is 50-80℃ / h, the annealing temperature is 780-850℃, the holding time is 8-10h, and then it is cooled to room temperature in the hood-type vacuum annealing furnace and taken out of the furnace to obtain a finished titanium alloy foil coil.

[0022] According to another aspect of the present invention, a titanium alloy foil coil is provided. The titanium alloy foil coil is prepared according to the method for preparing the titanium alloy foil coil described above.

[0023] In one embodiment of the present invention, the weight of the titanium alloy foil strip is greater than 400 kg, and the yield rate is greater than 95%.

[0024] By adopting the above technical solution, the present invention has the following advantages compared with the prior art:

[0025] (1) The present invention uses titanium alloy cold-rolled coil as raw material, utilizes a high-precision reversible rolling mill, and through reasonable cold rolling deformation process and annealing process design, carries out coil rolling production of titanium alloy foil, obtains a high yield rate and large unit weight foil coil product, and the performance meets the comprehensive performance indicators of hydrogen fuel cell plates and the requirements of microchannel forming processing;

[0026] (2) The present invention can effectively ensure the thickness accuracy and good plate shape of the material under extremely thin specifications;

[0027] (3) The present invention is conducive to the formation of base surface texture of material plastic extension deformation, thereby improving the formability of the product;

[0028] (4) The entire cold rolling process of the present invention is rolled in the form of coils, and no slitting is required. The product weight can be greater than 400 kg, the surface is not oxidized, and no pickling is required. It has the characteristics of high production efficiency and high yield rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 A schematic flow chart of a method for preparing a titanium alloy foil strip provided by the present invention is shown; DETAILED DESCRIPTION

[0030] It should be understood that the embodiments of the present invention shown in the exemplary embodiments are only illustrative. Although only a few embodiments are described in detail in the present invention, it is easy for those skilled in the art to appreciate that multiple modifications are feasible without actually departing from the teaching of the subject matter of the present invention. Accordingly, all such modifications should be included within the scope of the present invention. Without departing from the gist of the present invention, other replacements, modifications, changes and deletions may be made to the design, operating conditions and parameters of the following exemplary embodiments.

[0031] like Figure 1 As shown, a method for preparing a titanium alloy foil strip comprises the following steps:

[0032] Step S101: Selecting a pickled annealed cold rolled coil made of titanium alloy material as a raw material;

[0033] Step S102: rolling the raw material in a first rolling process to obtain a first cold-rolled coil;

[0034] Step S103: performing an online annealing treatment on the first cold-rolled coil in an argon-protected continuous annealing furnace to obtain a first intermediate annealed cold-rolled coil;

[0035] Step S104: performing a second rolling process on the cold-rolled coil subjected to the first intermediate annealing treatment to obtain a second cold-rolled coil;

[0036] Step S105: performing vacuum annealing treatment on the second cold-rolled coil in a hood-type vacuum annealing furnace to obtain a second intermediate annealed cold-rolled coil;

[0037] Step S106: performing a third rolling process on the cold-rolled coil subjected to the second intermediate annealing treatment to obtain a rolled foil coil;

[0038] Step S107: performing vacuum annealing treatment on the rolled foil strip in a hood-type vacuum annealing furnace to obtain a finished titanium alloy foil strip.

[0039] Through the above-mentioned technical scheme of the present invention, the present invention uses titanium alloy cold-rolled coil as raw material, utilizes a high-precision reversible rolling mill, and through reasonable cold rolling deformation process and annealing process design, carries out coil rolling production of titanium alloy foil, obtains high yield rate and large unit weight foil coil products, and the performance meets the comprehensive performance indicators of hydrogen fuel cell plates and the requirements of microchannel forming processing.

[0040] In the above technical solution, the raw material in step S101 has a thickness of 3.0-3.5 mm, a width of 300-500 mm, a length of 80-120 m, and a weight of 400-600 kg.

[0041] In the above technical scheme, in step S102, when the first rolling process is carried out, the rolling speed is 2-5m / s, the deformation amount of each pass is 20-30%, and the coilers respectively equipped at the inlet and outlet ends of the rolling mill are used to carry out multiple reversible rolling passes, the deformation amount of the final rolling pass is 20-25%, and the final rolling thickness is 1.0-1.5mm.

[0042] In the above technical solution, the length of the annealing furnace in step S103 is 25-30m; the annealing temperature is 700-750°C, the coiling speed during annealing is 2-6m / min, and the argon concentration in each section of the annealing furnace is greater than 95%.

[0043] In the above technical scheme, in step S104, when the second rolling process is carried out, the rolling speed is 8-10m / s, the deformation amount of each pass is 10-20%, and the coilers respectively equipped at the inlet and outlet ends of the rolling mill are used to carry out multiple passes of reversible rolling, the deformation amount of the final rolling pass is 10-15%, and the final rolling thickness is 0.3-0.5mm.

[0044] In the above technical solution, in the vacuum annealing process in step S105, the entire second cold-rolled coil is placed in a hood-type vacuum annealing furnace and evacuated to a vacuum degree of ≤10 -3 After Pa, the temperature is raised for annealing heat treatment, the heating rate is 60-100℃ / h, the annealing temperature is 650-680℃, the holding time is 6-8h, and then it is cooled to room temperature in the hood-type vacuum annealing furnace and taken out of the furnace to obtain the second intermediate annealing cold-rolled coil.

[0045] In the above technical scheme, when the third rolling process is carried out in step S106, the rolling speed is 10-15m / s, the deformation amount of each pass is 5-20%, and the coilers respectively equipped at the inlet and outlet ends of the rolling mill are used to carry out multiple reversible rolling passes, the deformation amount of the final rolling pass is 5-10%, and the final rolling thickness is 0.1-0.15mm.

[0046] In the above technical solution, in the vacuum annealing process in step S107, the entire rolled foil strip is placed in a hood-type vacuum annealing furnace and evacuated to a vacuum degree of ≤10 -3 Pa, the temperature is raised for annealing heat treatment, the heating rate is 50-80℃ / h, the annealing temperature is 780-850℃, the holding time is 8-10h, and then it is cooled to room temperature in the hood-type vacuum annealing furnace and taken out of the furnace to obtain a finished titanium alloy foil coil.

[0047] The annealing treatment after rolling in the first rolling process, the second rolling process and the third rolling process of the present invention respectively adopts online argon protection annealing and vacuum furnace annealing. The online annealing has high efficiency and short process cycle. Moreover, although the micro-area may still be oxidized to form color difference and the vacuum annealing cycle is long, the temperature uniformity is good and color difference will not be formed due to oxidation. Moreover, the first rolling process adopts high-efficiency online annealing, and the color difference can be eliminated in the subsequent process without affecting the finished product. The subsequent rolling process adopts long-term vacuum annealing to ensure the temperature uniformity and surface consistency of the whole coil.

[0048] The deformation amount of the final rolling pass of the first rolling process of the present invention is 20-25%, the deformation amount of the final rolling pass of the second rolling process is 10-15%, and the deformation amount of the final rolling pass of the third rolling process is 5-10%. The thinner the material is rolled, the smaller the deformation amount of the final rolling pass of the rolling process is, which can effectively ensure the thickness accuracy and good plate shape of the material under extremely thin specifications.

[0049] The intermediate annealing temperature after the first rolling process of the present invention is 700-750°C, the intermediate annealing temperature after the second rolling process is 650-680°C, and the finished product annealing temperature after the third rolling process is 780-850°C. The purpose is to promote the formation of a base surface texture that is beneficial to the plastic extension deformation of the material and improve the formability of the product by regulating the annealing temperature of the material under different deformation states.

[0050] In addition, a titanium alloy foil strip is provided. The titanium alloy foil strip is prepared according to the steps S101 to S107 described above.

[0051] In the above technical solution, the weight of the titanium alloy foil coil is greater than 400 kg, and the yield rate is more than 95%.

[0052] The entire cold rolling process of the present invention is rolled in the form of coils, and does not require slitting. The product weight is greater than 400 kg, the surface is not oxidized, and pickling is not required. It has the characteristics of high production efficiency and high yield rate.

[0053] The above technical solution of the present invention is described in detail below through specific embodiments.

[0054] Embodiment 1

[0055] A method for preparing a titanium alloy foil strip, the specific steps are as follows:

[0056] 1) The pickled annealed cold rolled coil is used as the raw material, the grade is TA10, the thickness is 3.5mm, the width is 350mm, the coil length is 90m, and the weight is 500kg.

[0057] 2) The raw material in step 1) is subjected to first rolling at a rolling speed of 3 m / s, and three passes of reversible rolling are performed using coilers respectively provided at the inlet and outlet ends of the rolling mill, wherein the first pass is rolled from 3.5 mm to 2.5 mm, and the deformation amount of the pass is 28.6%; the second pass is rolled from 2.5 mm to 1.9 mm, and the deformation amount of the pass is 24%; the third pass is final rolling, and the thickness is rolled from 1.9 mm to 1.5 mm, and the deformation amount of the pass is 21%, thereby obtaining a first cold-rolled coil;

[0058] 3) performing an online annealing treatment on the first cold-rolled coil obtained in step 2), using an argon-protected continuous annealing furnace, with an annealing temperature of 750° C., a furnace length of 25 m, a coiling speed of 3 m / min, and a coil annealing time equivalent to 8.3 min. The argon concentration in each section of the furnace is maintained at 98%, thereby obtaining a first intermediate annealed cold-rolled coil;

[0059] 4) The first intermediate annealing cold-rolled coil completed in step 3) is subjected to a second rolling process at a rolling speed of 10 m / s, and 6 passes of reversible rolling are performed using coilers respectively provided at the inlet and outlet ends of the rolling mill. The first pass is rolled from 1.5 mm to 1.2 mm, and the pass deformation is 20%; the second pass is rolled from 1.2 mm to 1.0 mm, and the pass deformation is 16.7%; the third pass is rolled from 1.0 mm to 0.85 mm, and the pass deformation is 15%; the fourth pass is rolled from 0.85 mm to 0.7 mm, and the pass deformation is 17.6%; the fifth pass is rolled from 0.7 mm to 0.6 mm, and the pass deformation is 14.3%; the sixth pass is final rolling, and is rolled from 0.6 mm to 0.5 mm, and the pass deformation is 14.3% to obtain a second cold-rolled coil.

[0060] 5) The second cold-rolled coil obtained in step 4) is subjected to vacuum annealing treatment, using a hood-type vacuum annealing furnace, placing the entire second cold-rolled coil in the furnace, and evacuating the vacuum to a vacuum degree of ≤10 -3 After Pa, the temperature is increased for annealing heat treatment, the heating rate is 100℃ / h, the holding temperature is 650℃, the holding time is 8h, and the steel strip is taken out of the furnace after cooling to room temperature to obtain the second intermediate annealing cold-rolled coil.

[0061] 6) The second intermediate annealing cold-rolled coil completed in step 5) is subjected to a third rolling process, with a rolling speed of 12 m / s, and 10 passes of reversible rolling are performed using coilers respectively provided at the inlet and outlet ends of the rolling mill. The first pass is rolled from 0.5 mm to 0.4 mm, with a pass deformation of 20%, the second pass is rolled from 0.4 mm to 0.33 mm, with a pass deformation of 17.5%, the third pass is rolled from 0.33 mm to 0.28 mm, with a pass deformation of 15.2%, and the fourth pass is rolled from 0.28 mm to 0.24 mm. mm, with a deformation of 14.3% per pass; the fifth pass is rolled from 0.24 mm to 0.21 mm, with a deformation of 12.5% per pass; the sixth pass is rolled from 0.21 mm to 0.18 mm, with a deformation of 14.3% per pass; the seventh pass is rolled from 0.18 mm to 0.15 mm, with a deformation of 16.7% per pass; the eighth pass is rolled from 0.15 mm to 0.13 mm, with a deformation of 13.3% per pass; the ninth pass is rolled from 0.13 mm to 0.11 mm, with a deformation of 15.4% per pass; the tenth pass is final rolling, rolled from 0.11 mm to 0.10 mm, with a deformation of 9.1% per pass, and a rolled foil coil is obtained.

[0062] 7) The rolled foil strip obtained in step 6) is subjected to finished product annealing treatment in a hood-type vacuum annealing furnace, the entire rolled foil strip is placed in the furnace, and vacuum is evacuated to a vacuum degree of ≤10 -3 After Pa, the temperature was started to be raised for annealing heat treatment, the heating rate was 60℃ / h, the holding temperature was 800℃, the holding time was 8h, and the foil was taken out of the furnace after being cooled to room temperature to obtain a TA10 titanium alloy foil coil with a thickness of 0.10mm.

[0063] Through the above-mentioned Example 1, the weight of the titanium alloy foil coil product prepared by the present invention is 478 kg, and the yield rate is 95.6%.

[0064] Embodiment 2

[0065] A method for preparing a titanium alloy foil strip, the specific steps are as follows:

[0066] 1) Using pickled and annealed cold-rolled coil strip as raw material, with grade TA10, thickness specification of 3.0 mm, width of 400 mm, coil strip length of 110 m, and weight of 595 kg.

[0067] 2) Conduct the first rolling process using the raw material in step 1), with a rolling speed of 3 m / s. Using the coiling machines respectively equipped at the inlet and outlet ends of the rolling mill, conduct 3-pass reversible rolling. In the first pass, roll from 3.0 mm to 2.2 mm, with a pass deformation of 26.7%. In the second pass, roll from 2.2 mm to 1.6 mm, with a pass deformation of 27.3%. In the third pass, final rolling, roll from 1.6 mm to 1.2 mm, with a pass deformation of 25%, to obtain the first cold-rolled coil strip;

[0068] 3) Conduct on-line annealing treatment on the first cold-rolled coil strip obtained in step 2). Use an argon-protected continuous annealing furnace, with an annealing temperature in the furnace of 750 °C, the furnace body length of the annealing furnace being 25 meters, the coiling speed during annealing being 4 m / min, the equivalent annealing time of the coil strip being 6.25 min, and the argon concentration in each section of the furnace being maintained at 98%, thereby obtaining the first intermediate annealed cold-rolled coil strip;

[0069] 4) Conduct the second rolling process on the first intermediate annealed cold-rolled coil strip completed in step 3), with a rolling speed of 8 m / s. Using the coiling machines respectively equipped at the inlet and outlet ends of the rolling mill, conduct 6-pass reversible rolling. In the first pass, roll from 1.2 mm to 1.0 mm, with a pass deformation of 16.7%. In the second pass, roll from 1.0 mm to 0.85 mm, with a pass deformation of 15%. In the third pass, roll from 0.85 mm to 0.7 mm, with a pass deformation of 17.6%. In the fourth pass, roll from 0.7 mm to 0.6 mm, with a pass deformation of 14.3%. In the fifth pass, roll from 0.6 mm to 0.5 mm, with a pass deformation of 16.7%. In the sixth pass, final rolling, roll from 0.5 mm to 0.45 mm, with a pass deformation of 10%, to obtain the second cold-rolled coil strip.

[0070] 5) Conduct vacuum annealing treatment on the second cold-rolled coil strip obtained in step 4). Use a bell-type vacuum annealing furnace, place the entire second cold-rolled coil strip in the furnace, evacuate to a vacuum degree ≤ 10 -3 Pa, then start heating for annealing treatment, with a heating rate of 100 °C / h, a holding temperature of 680 °C, a holding time of 7 h, and cool in the furnace to room temperature and then take out of the furnace to obtain the second intermediate annealed cold-rolled coil strip.

[0071] 6) The second intermediate annealing cold-rolled coil completed in step 5) is subjected to a third rolling process, with a rolling speed of 12 m / s, and 9 passes of reversible rolling are performed using coilers respectively provided at the inlet and outlet ends of the rolling mill. The first pass is rolled from 0.45 mm to 0.38 mm, with a pass deformation of 15.6%, the second pass is rolled from 0.38 mm to 0.32 mm, with a pass deformation of 15.8%, the third pass is rolled from 0.32 mm to 0.28 mm, with a pass deformation of 14.3%, and the fourth pass is rolled from 0.28 mm to 0.24 mm. mm, with a deformation of 14.3% per pass; the fifth pass is rolled from 0.24 mm to 0.21 mm, with a deformation of 12.5% per pass; the sixth pass is rolled from 0.21 mm to 0.18 mm, with a deformation of 14.3% per pass; the seventh pass is rolled from 0.18 mm to 0.15 mm, with a deformation of 16.7% per pass; the eighth pass is rolled from 0.15 mm to 0.13 mm, with a deformation of 13.3% per pass; the ninth pass is final rolling, rolled from 0.13 mm to 0.12 mm, with a deformation of 7.7% per pass, and a rolled foil coil is obtained.

[0072] 7) The rolled foil strip obtained in step 6) is subjected to finished product annealing treatment in a hood-type vacuum annealing furnace, the entire rolled foil strip is placed in the furnace, and vacuum is evacuated to a vacuum degree of ≤10 -3 After Pa, the temperature was started to be raised for annealing heat treatment, the heating rate was 60℃ / h, the holding temperature was 800℃, the holding time was 8h, and the foil was taken out of the furnace after cooling to room temperature to obtain a TA10 titanium alloy foil coil with a thickness of 0.12mm.

[0073] Through the above-mentioned Example 2, the weight of the titanium alloy foil coil product prepared by the present invention is 578 kg, and the yield rate is 97.1%.

[0074] Embodiment 3

[0075] A method for preparing a titanium alloy foil strip, the specific steps are as follows:

[0076] 1) The pickled annealed cold rolled coil is used as the raw material, the grade is TA10, the thickness is 3.0mm, the width is 500mm, the coil length is 80m, and the weight is 540kg.

[0077] 2) Use the raw materials in step 1) for the first rolling process. The rolling speed is 3 m / s. Using the coiling machines respectively equipped at the inlet end and the outlet end of the rolling mill, perform 4-pass reversible rolling. In the first pass, roll from 3.0 mm to 2.2 mm, with a pass reduction of 26.7%. In the second pass, roll from 2.2 mm to 1.7 mm, with a pass reduction of 22.7%. In the third pass, roll from 1.7 mm to 1.3 mm, with a pass reduction of 23.5%. In the fourth pass, finish rolling, roll from 1.3 mm to 1.0 mm, with a pass reduction of 23.1%, to obtain the first cold-rolled coil strip;

[0078] 3) Perform an on-line annealing treatment on the first cold-rolled coil strip obtained in step 2). Use a continuous annealing furnace with argon protection. The annealing temperature in the furnace is 700 °C. The length of the furnace body of the annealing furnace is 25 m. The coiling speed during annealing is 5 m / min. The annealing time of the coil strip is equivalent to 5 min. The argon concentration in each section of the furnace is maintained at 98%, thereby obtaining the first cold-rolled coil strip after intermediate annealing treatment;

[0079] 4) Perform the second rolling process on the first cold-rolled coil strip after intermediate annealing treatment completed in step 3). The rolling speed is 10 m / s. Using the coiling machines respectively equipped at the inlet end and the outlet end of the rolling mill, perform 6-pass reversible rolling. In the first pass, roll from 1.0 mm to 0.8 mm, with a pass reduction of 20%. In the second pass, roll from 0.8 mm to 0.65 mm, with a pass reduction of 18.8%. In the third pass, roll from 0.65 mm to 0.55 mm, with a pass reduction of 15.4%. In the fourth pass, roll from 0.55 mm to 0.45 mm, with a pass reduction of 18.2%. In the fifth pass, roll from 0.45 mm to 0.38 mm, with a pass reduction of 15.6%. In the sixth pass, finish rolling, roll from 0.38 mm to 0.33 mm, with a pass reduction of 13.2%, to obtain the second cold-rolled coil strip.

[0080] 5) Perform a vacuum annealing treatment on the second cold-rolled coil strip obtained in step 4). Use a bell-type vacuum annealing furnace. Place the entire second cold-rolled coil strip in the furnace. After evacuating to a vacuum degree ≤ 10 -3 Pa, start heating for annealing treatment. The heating rate is 100 °C / h. The holding temperature is 680 °C. The holding time is 6 h. And then cool in the furnace to room temperature and then take out of the furnace to obtain the second cold-rolled coil strip after intermediate annealing treatment.

[0081] 6) The second intermediate annealing cold-rolled coil completed in step 5) is subjected to a third rolling process, with a rolling speed of 12 m / s, and 8 passes of reversible rolling are performed using coilers respectively equipped at the inlet and outlet ends of the rolling mill. The first pass is rolled from 0.33 mm to 0.28 mm, with a pass deformation of 15.2%, the second pass is rolled from 0.28 mm to 0.24 mm, with a pass deformation of 14.3%, the third pass is rolled from 0.24 mm to 0.20 mm, with a pass deformation of 16.7%, and the fourth pass is rolled from 0.20 mm to 0.17 mm. mm, with a deformation of 15% per pass; the fifth pass is rolled from 0.17mm to 0.15mm, with a deformation of 11.8% per pass; the sixth pass is rolled from 0.15mm to 0.13mm, with a deformation of 13.3% per pass; the seventh pass is rolled from 0.13mm to 0.11mm, with a deformation of 15.4% per pass; the eighth pass is final rolling, from 0.11mm to 0.10mm, with a deformation of 9.1% per pass, to obtain a rolled foil coil.

[0082] 7) The rolled foil strip obtained in step 6) is subjected to finished product annealing treatment in a hood-type vacuum annealing furnace, the entire rolled foil strip is placed in the furnace, and vacuum is evacuated to a vacuum degree of ≤10 -3 After Pa, the temperature was started to rise for annealing heat treatment, the heating rate was 60℃ / h, the holding temperature was 750℃, the holding time was 8h, and the furnace was cooled to room temperature and then taken out of the furnace to obtain TA10 titanium alloy foil coil with a thickness of 0.10mm.

[0083] Through the above-mentioned Example 3, the weight of the titanium alloy foil coil product prepared by the present invention is 528 kg, and the yield rate is 97.8%.

[0084] It can be seen from the above embodiments 1-3 that the present invention uses titanium alloy cold-rolled coil as raw material, utilizes a high-precision reversible rolling mill, and through reasonable cold rolling deformation process and annealing process design, carries out coil rolling production of titanium alloy foil, and obtains a high yield rate of more than 95%, a large single weight foil coil product with a weight greater than 400kg, and the performance can meet the comprehensive performance indicators of hydrogen fuel cell plates and the requirements of microchannel forming processing.

[0085] The above description is only a preferred embodiment of the present invention and is not intended to limit the scope of implementation of the present invention. If the present invention is modified or replaced by equivalents without departing from the spirit and scope of the present invention, it should be included in the protection scope of the claims of the present invention.

Claims

1. A preparation method of a titanium alloy foil strip, characterized in that, It includes the following steps: 1) Select pickled and annealed cold-rolled coil strips made of titanium alloy materials as raw materials; 2) Perform the first rolling process on the raw materials to obtain the first cold-rolled coil strips; 3) Perform on-line annealing treatment on the first cold-rolled coil strips in an argon-protected continuous annealing furnace to obtain the first intermediate annealing-treated cold-rolled coil strips; 4) Perform the second rolling process on the first intermediate annealing-treated cold-rolled coil strips to obtain the second cold-rolled coil strips; 5) Perform vacuum annealing treatment on the second cold-rolled coil strips in a bell-type vacuum annealing furnace to obtain the second intermediate annealing-treated cold-rolled coil strips; during the vacuum annealing treatment, the entire second cold-rolled coil strip is placed in the bell-type vacuum annealing furnace, evacuated to a vacuum degree of ≤10-3 Pa, then heated up for annealing treatment, the heating rate is 60-100 °C / h, the annealing temperature is 650-680 °C, the holding time is 6-8 h, and then it is cooled to room temperature with the bell-type vacuum annealing furnace and taken out of the furnace to obtain the second intermediate annealing-treated cold-rolled coil strips; 6) Perform the third rolling process on the second intermediate annealing-treated cold-rolled coil strips to obtain rolled foil coil strips; 7) Perform vacuum annealing treatment on the rolled foil coil strips in a bell-type vacuum annealing furnace to prepare finished titanium alloy foil coil strips; during the vacuum annealing treatment, the entire rolled foil coil strip is placed in the bell-type vacuum annealing furnace, evacuated to a vacuum degree of ≤10-3 Pa, then heated up for annealing treatment, the heating rate is 50-80 °C / h, the annealing temperature is 780-850 °C, the holding time is 8-10 h, and then it is cooled to room temperature with the bell-type vacuum annealing furnace and taken out of the furnace to obtain finished titanium alloy foil coil strips.

2. The preparation method of the titanium alloy foil strip according to claim 1, characterized in that, In step 1), the thickness of the raw materials is 3.0-3.5 mm, the width is 300-500 mm, the length is 80-120 m, and the weight is 400-600 kg.

3. The preparation method of the titanium alloy foil strip according to claim 1, characterized in that In step 2), when performing the first rolling process, the rolling speed is 2-5 m / s, the pass reduction is 20-30%, and the coiling machines respectively equipped at the inlet end and the outlet end of the rolling mill are used for multi-pass reversible rolling, the reduction of the final pass is 20-25%, and the final rolling thickness is 1.0-1.5 mm.

4. The preparation method of the titanium alloy foil strip according to claim 1, characterized in that, In step 3), the length of the furnace body of the annealing furnace is 25-30 m, the annealing temperature is 700-750 °C, the coiling speed during annealing is 2-6 m / min, and the argon concentration in each section of the annealing furnace is greater than 95%.

5. The preparation method of the titanium alloy foil strip according to claim 1, characterized in that, In step 4), when performing the second rolling process, the rolling speed is 8-10 m / s, the pass reduction is 10-20%, and the coiling machines respectively equipped at the inlet end and the outlet end of the rolling mill are used for multi-pass reversible rolling, the reduction of the final pass is 10-15%, and the final rolling thickness is 0.3-0.5 mm.

6. The preparation method of the titanium alloy foil strip according to claim 1, characterized in that, In step 6), when performing the third rolling process, the rolling speed is 10-15 m / s, the pass reduction is 5-20%, and the coiling machines respectively equipped at the inlet end and the outlet end of the rolling mill are used for multi-pass reversible rolling, the reduction of the final pass is 5-10%, and the final rolling thickness is 0.1-0.15 mm.

7. A titanium alloy foil strip, characterized in that, The titanium alloy foil coil is prepared by the preparation method of the titanium alloy foil coil according to any one of the foregoing claims 1-6.

8. The titanium alloy foil strip according to claim 7, characterized in that, The weight of the titanium alloy foil coil is greater than 400 kg, and the yield rate is more than 95%.

Citation Information

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