A manufacturing method of a high-strength and low-wetting reinforced platinum nozzle

Abstract

The present invention discloses a method for manufacturing a strengthened platinum nozzle with high strength and low wettability, belonging to the technical field of metal materials. Through vacuum melting, adding a strengthening agent, casting and homogenization, hot forging into bars, rolling and straightening the bars, and turning and drilling, a strengthened platinum nozzle with high strength and low wettability is finally obtained. Its advantages are as follows: compared with the traditional pure platinum nozzle, the strength of the strengthened platinum nozzle of the present invention is doubled, and the contact angle measured at 1300 °C with E glass is increased by 20 °.

Description

Technical Field

[0001] The present invention relates to a method for manufacturing a strengthened platinum nozzle with high strength and low wettability, belonging to the technical field of metal materials. Background Art

[0002] Flow control during the glass fiber drawing process is crucial and is mainly affected by factors such as drawing speed, glass liquid temperature, liquid level height, nozzle aperture and length, and the wettability between the nozzle and the glass liquid. When most factors are set, the wettability between the nozzle and the glass liquid becomes particularly important.

[0003] The wettability between the nozzle and the glass liquid depends on the nozzle material, glass liquid type, and operating temperature. In the past, the material with the largest usage was the Pt-Rh material, with the Rh content usually being 5-20%. Its contact angle with E glass liquid at a working temperature of 1300°C is between 36-80°, which can better meet the flow requirements of glass fiber drawing. However, in recent years, with the soaring price of Rh, pure Pt nozzle plates have gradually replaced Pt-Rh nozzle plates. However, the contact angle between pure Pt nozzles and E glass liquid at a working temperature of 1300°C is less than 20°. At the same time, pure Pt nozzles are relatively soft and are prone to deformation at high temperatures, seriously affecting the flow rate of the nozzle plate.

[0004] Therefore, it is very necessary to reduce the wettability between the pure Pt nozzle and the glass liquid. Research has shown that adding 1-5% of Au to pure Pt can significantly increase the contact angle between the Pt-Au material and the glass liquid, but this method will increase the losses and costs of precious metal recovery, separation, and purification. Summary of the Invention

[0005] The present invention provides a method for manufacturing a strengthened platinum nozzle with high strength and low wettability. Compared with traditional pure Pt nozzles, the strength can be increased by up to 1 time at most, and the contact angle measured at 1300°C with E glass is increased by up to 20° at most.

[0006] A method for manufacturing a strengthened platinum nozzle with high strength and low wettability comprises the following steps:

[0007] S1. Vacuum melting: Weigh 5-20 kg of pure platinum and place it in a zirconia crucible in a vacuum furnace. Close the vacuum furnace lid, open the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop below 10 Pa and maintain it, turn on the induction power supply, and slowly heat up to 1800-1900°C to melt it;

[0008] S2. Adding strengthening agents: After all the furnace charge is melted, it is cooled at a rate of 50 - 100 °C / min to 1300 - 1400 °C for solidification, kept for 2 - 3 min, and then heated at a rate of 50 - 100 °C / min to 1800 - 1900 °C for melting. This is repeated 3 times in total. Strengthening agent one is added through the feeding bin during the second solidification holding, and strengthening agent two is added through the feeding bin during the third solidification holding. Adding strengthening agents during solidification holding can reduce the intensity of the reaction and increase the reaction time.

[0009] S3. Casting and homogenization: The alloy melt finally obtained in S2 is cast into a water-cooled copper mold at a rate of 500 - 1000 g / s. After the ingot is completely solidified, it is immediately taken out and put into an annealing furnace for homogenization annealing. The annealing temperature is 1100 - 1300 °C, and the annealing time is 2 - 4 h.

[0010] S4. Hot forging into bars: The ingot obtained in S3 is hot forged with an air hammer. The initial forging temperature is 1100 - 1300 °C, the final forging temperature is greater than 950 °C, and it is forged 2 - 4 times in total into a square bar with a cross-sectional side length of 12 - 14 mm. The square bar is put into the annealing furnace again for homogenization annealing. The annealing temperature is 1100 - 1300 °C, and the annealing time is 1 - 2 h.

[0011] S5. Rolling and straightening the bars: The square bar obtained in S4 is rolled into a round bar with a diameter of φ3 - 5 mm through a bar rolling machine, and the round bar is then cold drawn to φ2 - 4 mm, straightened by a straightening machine, and cut into a nozzle fine bar stock.

[0012] S6. Turning and drilling: The nozzle fine bar stock obtained in S5 is turned and drilled to obtain the final finished nozzle.

[0013] Furthermore, the zirconia crucible described in S1 is one of yttria or calcia stabilized zirconia crucibles. Zirconia undergoes volume changes due to phase transitions at different temperatures and will crack, while after stabilization, the phase transitions are eliminated.

[0014] Furthermore, strengthening agent one in S2 is one or several mixtures of Ca, Al, Zr, Hf, Y, and the addition amount is 0.1 - 2% of the weight of the furnace charge.

[0015] Furthermore, strengthening agent two in S2 is one or several mixtures of Ca, Al, Zr, Hf, Y, and the addition amount is 0.1 - 2% of the weight of the furnace charge.

[0016] Furthermore, the water-cooled copper mold in S3 is one of a flat mold or a vertical mold.

[0017] Furthermore, the pass reduction during the bar rolling process in S5 is 10 - 20%.

[0018] Furthermore, the length of the nozzle fine bar stock in S5 is 300 - 500 mm.

[0019] Advantages of the present invention: The manufacturing method of the present invention forms an alloy with pure Pt by using one or several of Ca, Al, Zr, Hf, and Y through vacuum melting and homogenization annealing, which not only improves the material strength but also enhances the surface tension of the material, achieving the purpose of reducing wettability. The strengthened platinum nozzle manufactured by the present invention can increase the strength by up to 1 time compared with the traditional pure Pt nozzle, and the contact angle measured with E glass at 1300 °C is increased by up to 20 °; in addition, compared with precious metals such as Pt, Rh, and Au, the addition of the strengthening agent in the present invention is not only low in price but also easy to separate and purify. Specific embodiments

[0020] The following describes the preferred embodiments of the present invention. It should be understood that the preferred embodiments described herein are only for explaining and illustrating the present invention and are not used to limit the present invention.

[0021] Example 1, A manufacturing method of a strengthened platinum nozzle with high strength and low wettability, comprising the following steps:

[0022] S1. Vacuum melting: Weigh 5 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace cover, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 0.3 Pa and maintain it, turn on the induction power supply, and slowly heat up to 1900 °C to melt it;

[0023] S2. Add the strengthening agent: After all the furnace charges are melted, cool down to 1300 °C at a speed of 50 °C / min to solidify it, keep it for 2 min, and then heat up to 1850 °C at a speed of 50 °C / min to melt it. Repeat this process 3 times in total, and add 50 g of pure Zr through the feeding bin during the second solidification and holding;

[0024] S3. Casting and homogenization: Pour the alloy melt finally obtained in S2 into a water-cooled copper mold at a speed of 600 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1200 °C and the annealing time is 2 h;

[0025] S4. Hot forging into bars: Hot forge the ingot obtained in S3 with an air hammer. The initial forging temperature is 1200 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm through 2 passes. The square bar is put into the annealing furnace again for homogenization annealing. The annealing temperature is 1100 °C and the annealing time is 1 h;

[0026] 5. Rolling and straightening of bars: Roll the square bar obtained in S4 into a round bar with a diameter of φ3.2 mm through a bar rolling machine, with a pass processing rate of 10%. The round bar is then cold drawn to φ2.1 mm and cut into a 300 mm long nozzle fine rod material after being straightened by a straightening machine;

[0027] S6. Turning and Drilling: The leak nozzle fine rod material obtained in S5 is turned and drilled to obtain the final finished leak nozzle.

[0028] Testing: Cut a part from the square bar obtained in S4, turn it into a standard tensile specimen for tensile testing. The measured tensile strength is 236 MPa and the elongation is 37%. Compared with pure Pt (136 MPa / 38%), the strength is increased by 73%, and at the same time, the plasticity does not decrease significantly. Cut a part from the square bar obtained in S4 and roll it into a 20×20×2 mm thin sheet. After surface treatment, put it into a high-temperature and high-vacuum wetting test system together with 2 g of E glass beads. The contact angle between them at 1300 °C is measured to be 27°, which is 7° higher than that of pure Pt (20°).

[0029] Example 2. A method for manufacturing a reinforced platinum leak nozzle with high strength and low wettability, comprising the following steps:

[0030] S1. Vacuum Melting: Weigh 5 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace lid, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 0.3 Pa and maintain it. Turn on the induction power supply and slowly heat up to 1900 °C to melt it.

[0031] S2. Adding Reinforcing Agents: After all the furnace charges are melted, cool down to 1300 °C at a rate of 50 °C / min to solidify it, keep it for 2 min, and then heat up to 1850 °C at a rate of 50 °C / min to melt it again. Repeat this process 3 times in total. Add 50 g of pure Zr through the feeding bin during the second solidification and holding, and add 10 g of pure Ca through the feeding bin during the third solidification and holding.

[0032] S3. Casting and Homogenization: Pour the alloy melt finally obtained in S2 into a water-cooled copper mold at a speed of 600 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1200 °C and the annealing time is 2 h.

[0033] S4. Hot Forging into Bars: Hot forge the ingot obtained in S3 with an air hammer. The initial forging temperature is 1200 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm through 2 passes. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1100 °C and the annealing time is 1 h.

[0034] S5. Rolling and Straightening the Bars: Roll the square bar obtained in S4 through a bar rolling machine to a round bar with a diameter of φ3.2 mm. The pass processing rate is 10%. Cold draw the round bar to φ2.1 mm, and cut it into a 300 mm long leak nozzle fine rod material after straightening by a straightening machine.

[0035] S6. Turning and Drilling: The leak nozzle fine rod material obtained in S5 is turned and drilled to obtain the final finished leak nozzle.

[0036] Detection: Cut a part from the square bar obtained in S4, turn it into a standard tensile specimen by turning for a tensile test. The measured tensile strength is 264 MPa and the elongation is 36%. Compared with pure Pt (136 MPa / 38%), the strength is increased by 94%, and at the same time, the plasticity does not decrease significantly. Cut a part from the square bar obtained in S4 and roll it into a 20×20×2 mm thin sheet. After surface treatment, put it into a high-temperature and high-vacuum wetting test system together with 2 g of E glass balls. The contact angle between the two is measured to be 25° at 1300 °C, which is 5° higher than that of pure Pt (20°).

[0037] Example 3. A method for manufacturing a reinforced platinum nozzle with high strength and low wettability includes the following steps:

[0038] S1. Vacuum melting: Weigh 10 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace lid, turn on the rotary vane vacuum pump and the vacuum valve, evacuate the air until the air pressure drops to 0.5 Pa and maintain it. Turn on the induction power supply and slowly heat up to 1900 °C to melt it;

[0039] S2. Adding strengthening agents: After all the furnace charges are melted, cool it down to 1300 °C at a rate of 60 °C / min to solidify it. After maintaining for 2 min, then heat it up to 1850 °C at a rate of 60 °C / min to melt it. Repeat this process 3 times in total. Add 120 g of pure Zr through the feeding bin during the second solidification and holding, and add 40 g of pure Y through the feeding bin during the third solidification and holding;

[0040] S3. Casting and homogenization: Pour the alloy melt obtained in step 2 into a water-cooled copper mold at a speed of 720 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1300 °C and the annealing time is 3 h;

[0041] S4. Hot forging into a bar: Hot forge the ingot obtained in step 3 with an air hammer. The initial forging temperature is 1300 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm through 3 passes. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1150 °C and the annealing time is 2 h;

[0042] S5. Rolling and straightening the bar: Roll the square bar obtained in S4 into a round bar with a diameter of φ4.2 mm through a bar rolling mill. The pass processing rate is 12%. Cold draw the round bar to φ3.0 mm, and cut it into a 400 mm long nozzle fine bar stock after straightening by a straightening machine;

[0043] S6. Turning and drilling: Turn and drill the nozzle fine bar stock obtained in S5 to get the final finished nozzle.

[0044] Detection: Cut a part from the square bar obtained in S4, turn it into a standard tensile specimen by turning for a tensile test. The measured tensile strength is 288 MPa and the elongation is 33%. Compared with pure Pt (136 MPa / 38%), the strength is increased by 112%, and at the same time, the plasticity does not decrease significantly. Cut a part from the square bar obtained in step 4 into a 20×20×2 mm thin sheet, after surface treatment, put it into a high-temperature and high-vacuum wetting test system together with 2 g of E glass beads. The contact angle between the two is measured to be 40° at 1300 °C, which is 20° higher than that of pure Pt (20°).

[0045] Example 4, A method for manufacturing a reinforced platinum nozzle with high strength and low wetting, comprising the following steps:

[0046] S1. Vacuum melting: Weigh 15 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace cover, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 1.1 Pa and maintain it. Turn on the induction power supply and slowly heat up to 1950 °C to melt it;

[0047] S2. Adding strengthening agents: After all the furnace charges are melted, cool it down to 1400 °C at a rate of 80 °C / min to solidify it, keep it for 3 min, then heat it up to 1950 °C at a rate of 70 °C / min to melt it. Repeat this process 3 times in total. Add 250 g of pure Zr through the feeding bin during the second solidification holding, and add 80 g of pure Y through the feeding bin during the third solidification holding;

[0048] S3. Casting and homogenization: Pour the alloy melt finally obtained in S2 into a water-cooled copper mold at a speed of 900 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1300 °C and the annealing time is 4 h;

[0049] S4. Hot forging into bars: Hot forge the ingot obtained in S3 with an air hammer. The starting forging temperature is 1300 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm through 4 passes. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1150 °C and the annealing time is 3 h;

[0050] S5. Rolling and straightening the bars: Roll the square bar obtained in S4 into a round bar with a diameter of φ4.5 mm through a bar rolling mill. The pass processing rate is 12%. Cold draw the round bar to φ3.6 mm, and cut it into a 500 mm long nozzle blank after straightening by a straightening machine;

[0051] S6. Turning and drilling: Turn and drill the nozzle blank obtained in S5 to get the final finished nozzle.

[0052] Detection: Cut a part from the square bar obtained in S4, turn it into a standard tensile specimen by turning for a tensile test. The measured tensile strength is 271 MPa and the elongation is 30%. Compared with pure Pt (136 MPa / 38%), the strength is increased by 99% and the plasticity does not decrease significantly at the same time. Cut a part from the square bar obtained in S4 and roll it into a 20×20×2 mm thin sheet. After surface treatment, put it into a high-temperature and high-vacuum wetting test system together with 2 g E glass balls. The contact angle between the two is measured to be 28° at 1300 °C, which is 8° higher than that of pure Pt (20°).

[0053] Example 5. A method for manufacturing a reinforced platinum nozzle with high strength and low wettability includes the following steps:

[0054] S1. Vacuum melting: Weigh 16 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace lid, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 1.3 Pa and maintain it. Turn on the induction power supply and slowly heat up to 1950 °C to melt it;

[0055] S2. Adding strengtheners: After all the furnace charges are melted, cool it down to 1400 °C at a rate of 80 °C / min to solidify it, keep it for 3 min, then heat it up to 1950 °C at a rate of 80 °C / min to melt it again. Repeat this process 3 times in total. Add 120 g of pure Al through the feeding bin during the second solidification holding, and add 210 g of pure Zr through the feeding bin during the third solidification holding;

[0056] S3. Casting and homogenization: Pour the alloy melt finally obtained in S2 into a water-cooled copper mold at a speed of 960 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1300 °C and the annealing time is 4 h;

[0057] S4. Hot forging into bars: Hot forge the ingot obtained in S3 with an air hammer. The initial forging temperature is 1300 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm in 3 passes. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1150 °C and the annealing time is 3 h;

[0058] S5. Rolling and straightening the bars: Roll the square bar obtained in S4 into a φ4.2 mm round bar through a bar rolling machine. The pass processing rate is 13%. Cold draw the round bar to φ3.2 mm, and cut it into a 400 mm long nozzle fine bar stock after straightening by a straightening machine;

[0059] S6. Turning and drilling: Turn and drill the nozzle fine bar stock obtained in S5 to get the final finished nozzle.

[0060] Detection: Cut a part from the square bar obtained in S4, turn it into a standard tensile specimen by turning for tensile test. The measured tensile strength is 231 MPa and the elongation is 33%. Compared with pure Pt (136 MPa / 38%), the strength is increased by 69% and the plasticity does not decrease significantly at the same time. Cut a part from the square bar obtained in S4 and roll it into a 20×20×2 mm thin sheet. After surface treatment, put it into a high-temperature and high-vacuum wetting test system together with 2 g E glass balls. The contact angle between the two is measured to be 31° at 1300 °C, which is 11° higher than that of pure Pt (20°).

[0061] Example 6, A method for manufacturing a reinforced platinum nozzle with high strength and low wettability, comprising the following steps:

[0062] S1. Vacuum melting: Weigh 10 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace lid, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 0.9 Pa and maintain it, turn on the induction power supply, and slowly heat up to 1900 °C to melt it;

[0063] S2. Adding strengthening agents: After all the furnace charges are melted, cool down to 1300 °C at a rate of 70 °C / min to solidify it, keep it for 2 min, then heat up to 1900 °C at a rate of 80 °C / min to melt it. Repeat this process 3 times in total. Add 130 g of pure Al through the feeding bin during the second solidification holding, and add 160 g of pure Y through the feeding bin during the third solidification holding;

[0064] S3. Casting and homogenization: Pour the alloy melt finally obtained in S2 into a water-cooled copper mold at a speed of 800 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1300 °C and the annealing time is 3 h;

[0065] S4. Hot forging into bars: Hot forge the ingot obtained in S3 with an air hammer. The initial forging temperature is 1300 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm through 2 passes. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1150 °C and the annealing time is 2 h;

[0066] S5. Rolling and straightening the bars: Roll the square bar obtained in S4 into a round bar with a diameter of φ3.9 mm through a bar rolling mill. The pass processing rate is 11%. Cold draw the round bar to φ2.6 mm, and cut it into a 400 mm long nozzle fine bar stock after straightening by a straightening machine;

[0067] S6. Turning and drilling: Turn and drill the nozzle fine bar stock obtained in S5 to obtain the final finished nozzle.

[0068] Detection: Take a part from the square bar obtained in S4, turn it into a standard tensile specimen by turning for tensile test. The measured tensile strength is 212 MPa and the elongation is 29%. Compared with pure Pt (136 Mpa / 38%), the strength is increased by 59% and the plasticity does not decrease significantly at the same time. Take a part from the square bar obtained in step 4 and roll it into a 20×20×2 mm thin sheet. After surface treatment, put it into a high-temperature and high-vacuum wetting test system together with 2 g E glass beads. The contact angle between the two is measured to be 29° at 1300 °C, which is 9° higher than that of pure Pt (20°).

[0069] Example 7. A method for manufacturing a reinforced platinum nozzle with high strength and low wettability includes the following steps:

[0070] S1. Vacuum melting: Weigh 7 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace cover, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 0.6 Pa and maintain it. Turn on the induction power supply and slowly heat up to 1900 °C to melt it;

[0071] S2. Adding strengthening agents: After all the furnace charges are melted, cool down to 1300 °C at a speed of 60 °C / min to solidify it, keep it for 2 min and then heat up to 1900 °C at a speed of 60 °C / min to melt it again. Repeat this process 3 times in total. Add 15 g of pure Y through the feeding bin during the second solidification and holding, and add 130 g of pure Zr through the feeding bin during the third solidification and holding;

[0072] S3. Casting and homogenization: Pour the alloy melt obtained in step 2 into a water-cooled copper mold at a speed of 600 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1200 °C and the annealing time is 2 h;

[0073] S4. Hot forging into a bar: Hot forge the ingot obtained in step 3 with an air hammer. The initial forging temperature is 1200 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm through 2 passes. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1100 °C and the annealing time is 1.5 h;

[0074] S5. Rolling and straightening the bar: Roll the square bar obtained in step 4 into a round bar with a diameter of φ3.5 mm by a bar rolling mill. The pass processing rate is 10%. Cold draw the round bar to φ2.3 mm and cut it into a 300 mm long nozzle fine rod material after straightening by a straightening machine;

[0075] S6. Turning and drilling: Carry out turning and drilling on the nozzle fine rod material obtained in S5 to obtain the final finished nozzle.

[0076] Detection: A part is cut from the square bar obtained in S4, turned into a standard tensile specimen for tensile testing. The measured tensile strength is 259 MPa and the elongation is 36%. Compared with pure Pt (136 Mpa / 38%), the strength is increased by 90%, and at the same time, the plasticity does not decrease significantly. A part is cut from the square bar obtained in step 4 and rolled into a 20×20×2 mm thin sheet. After surface treatment, it is put into a high-temperature and high-vacuum wetting test system together with 2 g of E glass beads. The contact angle between the two is measured to be 37° at 1300 °C, which is 17° higher than that of pure Pt (20°).

[0077] Comparative example, a method for manufacturing a reinforced platinum nozzle with high strength and low wetting, comprising the following steps:

[0078] S1. Vacuum melting: Weigh 7 kg of pure platinum and put it into a zirconia crucible in a vacuum furnace. Close the vacuum furnace lid, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop to 0.6 Pa and maintain it, turn on the induction power supply, and slowly heat up to 1900 °C to melt it;

[0079] S2. Adding a strengthening agent: After all the furnace charges are melted, cool it at a rate of 60 °C / min to 1300 °C to solidify it, keep it for 2 min, and then heat it up to 1900 °C at a rate of 60 °C / min to melt it. Repeat this process 2 times in total;

[0080] S3. Casting and homogenization: Pour the melt finally obtained in step 2 into a water-cooled copper mold at a speed of 600 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1200 °C and the annealing time is 2 h;

[0081] S4. Hot forging into a bar: Hot forge the ingot obtained in step 3 with an air hammer. The initial forging temperature is 1200 °C and the final forging temperature is 1000 °C. Forge it into a square bar with a cross-sectional side length of 12 mm in 2 passes. The square bar is put into an annealing furnace again for homogenization annealing. The annealing temperature is 1100 °C and the annealing time is 1.5 h;

[0082] S5. Rolling and straightening the bar: Roll the square bar obtained in S4 through a bar rolling machine into a round bar with a diameter of φ3.5 mm. The pass processing rate is 10%. The round bar is then cold drawn to φ2.3 mm and cut into a 300 mm long nozzle fine rod material after being straightened by a straightening machine;

[0083] S6. Turning and drilling: Turn and drill the nozzle fine rod material obtained in S5 to obtain the final finished nozzle.

[0084] Detection: A part is cut from the square bar obtained in S4, turned into a standard tensile specimen for tensile testing. The measured tensile strength is 136 MPa and the elongation is 38%.

[0085] Comparison between Example 1-7 and the comparative example

[0086]

[0087] Finally, it should be noted that the above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or perform equivalent replacements on some of the technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for manufacturing a high-strength and low-wetting reinforced platinum nozzle, characterized in that, It includes the following steps: S1. Vacuum melting: Weigh pure platinum and put it into a vacuum furnace to melt it; S2. Adding a strengthening agent: After the pure platinum melts, cool it at a rate of 50 - 100 °C / min to 1300 - 1400 °C to solidify it, keep it for 2 - 3 minutes, then heat it at a rate of 50 - 100 °C / min to 1800 - 1900 °C to melt it. Repeat this process 3 times in total, and add the strengthening agent through the feeding bin during the second and third solidification and holding; S3. Casting and homogenization S4. Hot forging into bars: S5. Rolling and straightening the bars S6. Turning and drilling; The strengthening agent added in S2 is any one or more of the metals Ca, Al, Zr, Hf, Y; the amount of each addition of the strengthening agent accounts for 0.1 - 2% of the weight of platinum.

2. The method for manufacturing a high-strength and low-wetting reinforced platinum nozzle according to claim 1, characterized in that, The method of vacuum melting in S1 is to put pure platinum into a zirconia crucible in the vacuum furnace, close the vacuum furnace cover, turn on the rotary vane vacuum pump and the vacuum valve, evacuate to make the air pressure drop below 10 Pa and keep it, turn on the induction power supply, and slowly heat it to 1800 - 1900 °C to melt it.

3. The method for manufacturing a high-strength and low-wetting reinforced platinum nozzle according to claim 1, characterized in that, The method of casting and homogenization in S3 is: Pour the alloy melt into a water-cooled copper mold at a speed of 500 - 1000 g / s. Immediately take out the ingot after it is completely solidified and put it into an annealing furnace for homogenization annealing. The annealing temperature is 1100 - 1300 °C, and the annealing time is 2 - 4 h.

4. The method for manufacturing a high-strength and low-wetting reinforced platinum nozzle according to claim 1, characterized in that, When hot forging into bars in S4, hot forge the ingot with an air hammer. The initial forging temperature is 1100 - 1300 °C, the final forging temperature is greater than 950 °C. Forge it 2 - 4 times in total to form a square bar with a cross-sectional side length of 12 - 14 mm. Put the square bar into the annealing furnace again for homogenization annealing. The annealing temperature is 1100 - 1300 °C, and the annealing time is 1 - 2 h.

5. The method for manufacturing a high-strength and low-wetting reinforced platinum nozzle according to claim 1, characterized in that, When rolling and straightening the bars in S5, roll the square bar through a bar rolling machine to a round bar with a diameter of φ3 - 5 mm, then cold draw the round bar to φ2 - 4 mm, and straighten and cut it into a nozzle thin bar stock by a straightening machine.

6. The method for manufacturing a high-strength and low-wetting reinforced platinum nozzle according to claim 5, characterized in that: the pass deformation amount in the bar rolling process described in S5 is 10-20%, and the length of the nozzle thin rod material is 300-500 mm.

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