Nickel alloy strip and preparation method thereof
By adding Mn, Ti, and Mg to pure nickel and processing it with specific processes, the nickel alloy strip is prepared, and the problem of insufficient strength of pure nickel materials is solved, and the combination of high strength and high conductivity is achieved, which improves the service life of electronic devices.
Patent Information
- Application Number
- CN202510546251.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-28
- Publication Date
- 2025-08-01
AI Technical Summary
Existing pure nickel materials cannot obtain high strength through processing and heat treatment strengthening, resulting in a short service life of electronic devices.
By adding Mn, Ti, Mg to pure nickel, combined with vacuum smelting, forging, hot rolling, solid solution treatment and cold rolling processes, a nickel alloy strip is prepared to form a Ni3 (Ti, Mg) reinforced phase to improve the strength and conductivity of the material.
On the basis of maintaining good conductivity and corrosion resistance, the tensile strength and yield strength of nickel alloy strips are significantly improved, shortening the manufacturing cycle and saving energy consumption.
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Abstract
Description
Technical Field
[0001] The present invention relates to a nickel alloy strip, and more particularly to a nickel alloy strip and a preparation method thereof. Background Art
[0002] Pure nickel is widely used in the fields of aerospace, energy, chemical industry, instrumentation, electronic appliances, etc. due to its excellent electrical conductivity, ductility and corrosion resistance. The normal temperature resistivity of industrially commonly used pure nickel is 7.8 - 8.2 uΩcm, and the tensile strength is about 580 MPa, which can basically meet the applicable requirements of common electronic devices. However, due to the characteristics of its material, its strength is not high, and pure nickel materials cannot be strengthened by processing and heat treatment, which makes the service life of electronic devices prepared with pure nickel relatively short. With the development of the electronics industry and new energy, higher requirements are put forward for the service life of electronic device products, which not only need to have certain electrical conductivity, but also need to have corrosion resistance and high strength characteristics.
[0003] Therefore, there is an urgent need to provide a nickel alloy strip and a preparation method thereof. Summary of the Invention
[0004] The purpose of the present invention is to solve the technical problem that existing pure nickel materials cannot be strengthened by processing and heat treatment to obtain high strength characteristics, and to provide a nickel alloy strip and a preparation method thereof.
[0005] To solve the above technical problems, the technical solution provided by the present invention is as follows:
[0006] A nickel alloy strip, in terms of mass percentage, the chemical composition includes: Mn: 0.20% - 0.35%, Ti: 0.20% - 0.50%, Mg: 0.20% - 0.40%, and the balance is Ni and unavoidable impurities.
[0007] Further, in terms of mass percentage, the chemical composition includes: Mn: 0.20%, Ti: 0.30%, Mg: 0.30%, and the balance is Ni and unavoidable impurities.
[0008] Further, in terms of mass percentage, the chemical composition includes: Mn: 0.35%, Ti: 0.20%, Mg: 0.40%, and the balance is Ni and unavoidable impurities.
[0009] Further, in terms of mass percentage, the chemical composition includes: Mn: 0.30%, Ti: 0.50%, Mg: 0.20%, and the balance is Ni and unavoidable impurities.
[0010] A preparation method of a nickel alloy strip, comprising the following steps:
[0011] 1) Weigh the corresponding masses of metallic manganese, metallic titanium, metallic nickel, and nickel-magnesium alloy according to the chemical composition of the nickel alloy strip.
[0012] 2) Place the metallic nickel into the crucible of the intermediate-frequency vacuum induction melting furnace.
[0013] After evacuating to 5 Pa, heat the crucible at a power of 250 kW for 30 min, then evacuate to 1 Pa; heat to melt all the raw materials at a power of 400 kW, reach 1480 °C and enter the refining stage, and maintain refining for 40 min.
[0014] Add metallic manganese and stir for 2 min at a power of 400 kW, then add metallic titanium and nickel-magnesium alloy and stir for 5 min at a power of 400 kW, then pour out the molten metal to cast an alloy ingot, air-cool for 10 h and then demold to obtain the alloy ingot.
[0015] 3) Place the alloy ingot in a high-temperature resistance furnace, heat from room temperature to 750 °C and hold for 60 min.
[0016] Then heat up to 1100 °C with the furnace and hold for 120 min, and take out and forge into a flat billet of 50×200×L mm; where L is the length of the flat billet.
[0017] 4) Mill the surface of the flat billet until there is no scale, chamfer and grind the edges, then place it in a high-temperature resistance furnace and heat from room temperature to 750 °C and hold for 60 min; then heat up to 1050 °C with the furnace and hold for 40 min, and take out and roll into a strip billet with a thickness of 5.5 mm.
[0018] 5) Put the strip billet into the furnace and heat to 1080 °C, hold for 30 min and then carry out solution treatment.
[0019] 6) Immerse the strip billet after solution treatment in the pickling bath for 30 min, then take it out and rinse with high-pressure water to remove the surface scale.
[0020] 7) Roll the pickled strip billet into a strip with a thickness of 0.40 - 0.45 mm to obtain the nickel alloy strip and complete the preparation of the nickel alloy strip.
[0021] Furthermore, in step 3), the starting forging temperature is 1050 °C, and the final forging temperature ≥ 800 °C; during forging:
[0022] First, upset and blunt the edges at both ends of the alloy ingot.
[0023] Second, upset the height of the alloy ingot after upsetting and blunting to 1 / 2 of the original height.
[0024] Finally, draw out the alloy ingot upset in the height direction into a flat billet of 50×200×L mm.
[0025] Further, in step 4), the starting rolling temperature of the hot rolling is 1000 °C, and the finishing rolling temperature ≥ 750 °C.
[0026] Further, step 5) is specifically as follows:
[0027] Place the strip blank in a resistance furnace, heat the strip blank to 1080 °C through the resistance furnace, and keep it warm for 30 min;
[0028] After the heat preservation is completed, put the strip blank into water for rapid cooling and keep it for 30 min;
[0029] After taking out the strip blank from the water, the solution treatment is completed.
[0030] Further, in step 6), by weight percentage, the pickling solution in the pickling bath includes: 10% nitric acid, 5% hydrofluoric acid and the balance water.
[0031] Further, in step 7), the cold rolling should be completed within one rolling pass. The cold rolling is carried out in multiple passes, and the reduction per pass is 0.3 - 0.5 mm.
[0032] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0033] The nickel alloy strip and its preparation method provided by the present invention, by adding Mn, Ti, and Mg to pure nickel, while maintaining the good electrical conductivity and corrosion resistance of pure nickel, improve the strength of the material. The addition of Mn can enhance the hot working plasticity of the material, and the addition of Ti and Mg can cause the material to precipitate Ni3(Ti, Mg) strengthening phases to improve the strength of the material; by adopting solution rapid cooling treatment, the material maintains the austenite phase at high temperature, preparing for subsequent precipitation strengthening; by means of large deformation in one rolling pass of cold rolling, the strengthening precipitation degree of the material is improved, and the strength of the material is increased; by directly carrying out solution treatment after hot rolling for the processing technology, the process operation is simple, the manufacturing cycle can be shortened, and energy consumption can be saved. Description of the Drawings
[0034] Figure 1 It is the grain distribution diagram of the nickel alloy strip under an electron microscope in Example 1 of the present invention;
[0035] Figure 2 It is the grain distribution diagram of the nickel alloy strip under an electron microscope in Comparative Example 1 of the present invention. Detailed Embodiments
[0036] Next, the technical solutions in the present invention will be clearly and completely described in conjunction with the drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present invention.
[0037] A nickel alloy strip, whose chemical composition is: Mn: 0.20% - 0.35%, Ti: 0.20% - 0.50%, Mg: 0.20% - 0.40%, and the balance is Ni and unavoidable impurities.
[0038] Among them, the purity of Ni ≥ 99.99%; the purity of Mn ≥ 99.9%; the purity of Ti ≥ 99.6%; Mg uses a nickel-magnesium master alloy with a magnesium content of 20%; the thickness of the made nickel alloy strip is 0.40 - 0.45 mm, the tensile strength ≥ 1000 MPa, the hardness HV ≥ 300, and the resistivity ≤ 14 uΩ·cm.
[0039] The preparation method of the above nickel alloy strip is specifically as follows:
[0040] 1) Alloy batching
[0041] Prepare raw materials according to the chemical composition of the alloy; the raw materials are Mn, Ti, Mg, and Ni.
[0042] 2) Vacuum melting
[0043] First, load the raw material Ni into the crucible of the intermediate frequency vacuum induction melting furnace; after pumping to 5 Pa, heat the crucible at a power of 250 kW, after heating for 30 min, pump to 1 Pa; heat to all the raw materials are melted at a power of 400 kW, reach 1480 °C and enter the refining period, keep refining for 40 min; add Mn, stir for 2 min at a power of 400 kW, then add Ti and Mg and stir for 5 min at a power of 400 kW and then pour out the molten metal to cast the alloy ingot, air-cool for 10 h and then demold to obtain the alloy ingot;
[0044] In specific implementation, when loading the raw materials into the furnace, first load all Ni into the crucible, and load Mn, Ti, and Mg into the small hoppers in sequence.
[0045] 3) Forging
[0046] Place the alloy ingot in a high-temperature resistance furnace at room temperature and heat it to 750 °C, keep it warm for 60 min, then heat it up to 1100 °C with the furnace and keep it warm for 120 min, take it out of the furnace and forge it into a flat blank of 50×200×L; where L is the length;
[0047] In specific implementation, when taking it out of the furnace for forging, the starting forging temperature of the forging is 1050 °C, the final forging temperature ≥ 800 °C, air-cool after forging, first upset and blunt the edges of both ends of the blank during forging, then upset the height of the blank to 1 / 2 of the original height, and then draw out the blank.
[0048] 4) Hot rolling
[0049] The surface of the slab is milled smooth until there is no scale, and after the edges are chamfered and ground, it is placed in a high-temperature resistance furnace at room temperature and heated to 750 °C, held for 60 min, then heated to 1050 °C with the furnace and held for 40 min, and then taken out of the furnace and rolled into a strip blank with a thickness of 5.5 mm;
[0050] Specifically, when hot rolling is carried out after taking out of the furnace, the starting rolling temperature of the hot rolling is 1000 °C, and the final rolling temperature ≥ 750 °C.
[0051] 5) Solution annealing
[0052] The strip blank is directly put into the furnace and heated to 1080 °C, held for 30 min, and then taken out of the furnace and rapidly cooled to room temperature;
[0053] Specifically, the solution treatment is carried out in a resistance furnace with an air atmosphere. After the holding is completed, the material is immediately put into normal-temperature water for rapid cooling, taken out after staying in the water for 30 min and placed on a dry ground.
[0054] 6) Pickling
[0055] The strip blank that has completed step 5) is put into a pickling tank and soaked for 30 min, and then taken out and rinsed with high-pressure water to remove the surface scale;
[0056] Specifically, the pickling solution in the pickling tank is an aqueous solution prepared by mixing nitric acid and hydrofluoric acid to form a pickling solution; among them, the weight content of nitric acid is 10%, the weight content of hydrofluoric acid is 5%, and the rest is water.
[0057] 7) Cold rolling
[0058] The strip blank that has completed step 6) is rolled into a strip with a thickness of 0.40 - 0.45 mm to obtain a nickel alloy strip.
[0059] Specifically, the cold rolling should be completed within one rolling pass. The cold rolling is carried out in multiple passes, and the reduction per pass is 0.3 - 0.5 mm.
[0060] The following gives specific examples.
[0061] Example 1:
[0062] Alloy batching: The raw materials are charged according to the mass percentage of the alloy components. The components of the alloy are: Mn: 0.20%, Ti: 0.30%, Mg: 0.30%, and the balance is Ni and unavoidable impurities;
[0063] Vacuum Melting: First, load all the raw material Ni into the crucible of the intermediate frequency vacuum induction melting furnace, and load Mn, Ti, and Mg into the small hopper in sequence; after evacuating to 5 Pa, heat the crucible at a power of 250 kW. After heating for 30 min, evacuate to 1 Pa; heat at a power of 400 kW until all the raw materials are melted. When it reaches 1480 °C, enter the refining stage and keep refining for 40 min; add Mn and stir at a power of 400 kW for 2 min, then add Ti and Mg and stir at a power of 400 kW for 5 min, and then pour out the molten metal to cast the alloy ingot. After air cooling for 10 h, demold to obtain the alloy ingot;
[0064] Forging: Place the alloy ingot in a high-temperature resistance furnace at room temperature and heat it to 750 °C, hold for 60 min, then heat it to 1100 °C with the furnace and hold for 120 min. Take it out of the furnace for forging. The starting forging temperature is 1050 °C, and the final forging temperature ≥ 800 °C. When forging, first upset and blunt the edges at both ends of the blank, then upset the height of the blank to 1 / 2 of the original height, and then stretch the blank into a flat blank with dimensions of 50×200×L; where L is the length.
[0065] Hot Rolling: Mill the surface of the flat blank until there is no scale, chamfer and grind the edges, then place it in a high-temperature resistance furnace at room temperature and heat it to 750 °C, hold for 60 min, then heat it to 1050 °C with the furnace and hold for 40 min. Take it out of the furnace for rolling. The starting rolling temperature is 1000 °C, and the final rolling temperature ≥ 750 °C. Roll it into a strip blank with a thickness of 5.5 mm;
[0066] Solution Annealing: Directly put the hot-rolled strip blank into a resistance furnace with an air atmosphere, heat it to 1080 °C, hold for 30 min, open the furnace door, immediately put the material into normal-temperature water for rapid cooling, and take it out after holding in water for 30 min and place it on a dry ground.
[0067] Pickling: Immerse the solution-annealed strip blank in the pickling tank for 30 min, take it out and rinse it with high-pressure water to remove the surface scale;
[0068] Cold Rolling: Roll the pickled strip blank through multiple passes in one rolling process. The reduction per pass is 0.3 - 0.5 mm, and roll it into a strip with a thickness of 0.40 - 0.45 mm to obtain the nickel alloy strip.
[0069] Example 2
[0070] Compared with Example 1, the difference in Example 2 is that the composition of the alloy is: Mn: 0.35%, Ti: 0.20%, Mg: 0.40%, and the balance is Ni and unavoidable impurities.
[0071] Example 3
[0072] Example 3 is different from Example 1 in that the composition of the alloy is: Mn: 0.30%, Ti: 0.50%, Mg: 0.20%, and the balance is Ni and unavoidable impurities.
[0073] Example 4
[0074] Example 4 is different from Example 1 in that the composition of the alloy is: Mn: 0.25%, Ti: 0.40%, Mg: 0.35%, and the balance is Ni and unavoidable impurities.
[0075] Comparative Example 1
[0076] Comparative Example 1 is different from Example 1 in that Comparative Example 1 is pure nickel, and the Ni content of pure nickel is greater than or equal to 99.8%; Vacuum melting: All the raw material Ni is loaded into the crucible of the intermediate frequency vacuum induction melting furnace; After pumping to 5 Pa, the crucible is heated at a power of 250 kW. After heating for 30 min, it is pumped to 1 Pa; It is heated to full melting of the raw materials at a power of 400 kW, reaches 1480 °C and enters the refining period, and the refining is maintained for 40 min; After the refining is completed, it is taken out of the furnace for casting, and after air cooling for 10 h, it is demolded to obtain a nickel ingot;
[0077] Now, the mechanical properties, resistivity, and corrosion resistance of the nickel alloy strips prepared in Examples 1-4 and the nickel strip prepared in Comparative Example 1 are detected, and the detection results are shown in the following table:
[0078] Table 1: Detection results of mechanical properties, resistivity, and corrosion resistance of alloy strips
[0079]
[0080] As can be seen from Table 1, compared with Comparative Example 1, the nickel alloy strips prepared in Examples 1-4 of the present invention have the following advantages: The tensile strength and yield strength are both superior to those of the strips in Comparative Example 1. Compared with Comparative Example 1, the tensile strength of the alloy strips of the present invention is increased by at least 153.8%, and the yield strength is increased by at least 458.4%; The resistivity and the corrosion rate in 10% H2SO4 of the nickel alloy strips prepared in Examples 1-4 of the present invention are close to those of Comparative Example 1.
[0081] Grains are a microscopic structure characterization of metal materials. The grain size grades of the nickel alloy strips prepared in Example 1 and Comparative Example 1 are detected using an electron microscope. The grain size of the nickel alloy strip prepared in Example 1 is 10th grade, see Figure 1 ; The grain size of the nickel alloy strip prepared in Comparative Example 1 is 8th grade, see Figure 2Among them, the grain size is rated according to the size. From grade 1 to grade 10 and above, it means that the grain size ranges from coarse to fine. Fine grains can strengthen the material (fine grain strengthening) and improve the strength, plasticity, toughness, etc. of the material. It is not difficult to see that compared with Comparative Example 1, in Example 1, by increasing Mn, Ti and Mg and adopting the processes of vacuum melting, forging, hot rolling, solution treatment, pickling and cold rolling in this application, the grains in the nickel alloy strip can be refined. Through grain refinement, the nickel alloy strip has relatively high tensile strength and yield strength.
[0082] Therefore, the present invention can improve the mechanical properties (tensile strength and yield strength) of the material on the basis of maintaining the good electrical conductivity and corrosion resistance of pure nickel.
[0083] The above is only the specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions within the technical scope disclosed in the present invention should be covered by the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims
1. A nickel alloy strip, characterized in that, By mass percentage, the chemical composition includes: Mn: 0.20% - 0.35%, Ti: 0.20% - 0.50%, Mg: 0.20% - 0.40%, and the balance is Ni and unavoidable impurities.
2. The nickel alloy strip according to claim 1, wherein By mass percentage, the chemical composition includes: Mn: 0.20%, Ti: 0.30%, Mg: 0.30%, and the balance is Ni and unavoidable impurities.
3. The nickel alloy strip according to claim 1, characterized in that, By mass percentage, the chemical composition includes: Mn: 0.35%, Ti: 0.20%, Mg: 0.40%, and the balance is Ni and unavoidable impurities.
4. The nickel alloy strip according to claim 1, characterized in that, By mass percentage, the chemical composition includes: Mn: 0.30%, Ti: 0.50%, Mg: 0.20%, and the balance is Ni and unavoidable impurities.
5. A preparation method of a nickel alloy strip, characterized in that, It includes the following steps: 1) Weigh corresponding masses of metallic manganese, metallic titanium, metallic nickel, and nickel-magnesium alloy according to the chemical composition of the nickel alloy strip. 2) Load the metallic nickel into the crucible of the intermediate frequency vacuum induction melting furnace. After evacuating to 5 Pa, heat the crucible at a power of 250 kW for 30 min, then evacuate to 1 Pa. Heat at a power of 400 kW until all the raw materials are melted. When reaching 1480 °C, enter the refining stage and maintain refining for 40 min. Add metallic manganese and stir at a power of 400 kW for 2 min, then add metallic titanium and nickel-magnesium alloy and stir at a power of 400 kW for 5 min, then pour out the molten metal to cast an alloy ingot. After air cooling for 10 h, demold to obtain the alloy ingot. 3) Place the alloy ingot in a high-temperature resistance furnace, heat from room temperature to 750 °C and hold for 60 min. Then heat up with the furnace to 1100 °C, hold for 120 min, and take out and forge into a flat blank of 50×200×L mm; where L is the length of the flat blank. 4) Mill the surface of the flat blank until there is no scale, chamfer and grind the edges, then place it in a high-temperature resistance furnace and heat from room temperature to 750 °C and hold for 60 min; then heat up with the furnace to 1050 °C, hold for 40 min, and take out and roll into a strip blank with a thickness of 5.5 mm. 5) Heat the strip blank in the furnace to 1080 °C, hold for 30 min and then carry out solution treatment. 6) Immerse the strip blank after solution treatment in the pickling bath for 30 min, then take it out and rinse with high-pressure water to remove the surface scale. 7) Roll the pickled strip blank into a strip with a thickness of 0.40 - 0.45 mm to obtain the nickel alloy strip and complete the preparation of the nickel alloy strip.
6. The preparation method of the nickel alloy strip according to claim 2, characterized in that: In step 3), the starting forging temperature is 1050 °C, and the final forging temperature ≥ 800 °C; during forging: First, upset and blunt the edges at both ends of the alloy ingot. Secondly, upset the height of the alloy ingot after upsetting and blunting to 1 / 2 of the original height. Finally, draw out the alloy ingot upset in the height direction into a flat blank of 50×200×L mm.
7. The method for preparing a nickel alloy strip according to claim 2, wherein: In step 4), the starting rolling temperature of hot rolling is 1000 °C, and the final rolling temperature ≥ 750 °C.
8. The method for preparing a nickel alloy strip according to claim 2, wherein Step 5) is specifically: Place the strip blank in the resistance furnace and heat the strip blank to 1080 °C through the resistance furnace and hold for 30 min. After the holding is completed, put the strip blank into water for rapid cooling and keep it for 30 min. After taking out the strip blank from the water, complete the solution treatment.
9. The preparation method of the nickel alloy strip according to claim 2, characterized in that: In step 6), the pickling solution in the pickling bath includes, by weight percentage: 10% nitric acid, 5% hydrofluoric acid, and the balance water.
10. The preparation method of the nickel alloy strip according to claim 2, wherein: In step 7), cold rolling should be completed within one rolling pass, and cold rolling is carried out in multiple passes, with the reduction per pass being 0.3 - 0.5 mm.