Preparation method of modified high-strength magnesium-aluminum alloy wire

Abstract

The application discloses a preparation method of modified high-strength magnesium-aluminum alloy wire, which comprises the following steps: weighing the following raw materials with the following weight percentages: Mg 3-5%, Cr 0.1-0.2%, Si 0.1-0.2%, Mn 0.1-0.15%, Y 0.02-0.05%, Gd 0.02-0.04%, and the rest is Al. The high-strength magnesium-aluminum alloy wire is made of Mg, Cr, Si, Mn, Y, Gd and Al raw materials as the matrix raw material of the wire, the raw materials are mutually matched and mutually enhanced, the overall performance of the matrix is improved, and then the oscillation modification treatment and the heat cycle improvement treatment are carried out, the strength performance and the elongation performance of the product are improved through the mutual coordination of the two, and the high-temperature stability performance of the product is obviously improved.

Description

Technical Field

[0001] This invention relates to the field of magnesium-aluminum alloy wire technology, and specifically to a method for preparing modified high-strength magnesium-aluminum alloy wire. Background Technology

[0002] Aluminum-magnesium alloy wire is now widely used in coaxial cable for cable television, high-frequency signal transmission, and in the military and aerospace industries. It is a major supporting product for broadband transmission networks and communication network cables.

[0003] Existing magnesium-aluminum alloy wires have poor tensile strength. In order to improve tensile strength, the elongation performance of the product deteriorates, making the product prone to breakage. It is difficult to achieve a coordinated improvement in tensile strength and elongation performance. In addition, the product has poor stability under high temperature and saline-alkali conditions, which further limits the product's efficiency. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the purpose of this invention is to provide a method for preparing modified high-strength magnesium-aluminum alloy wire, so as to solve the problems mentioned in the background art.

[0005] The present invention solves the technical problem by adopting the following technical solution:

[0006] This invention provides a method for preparing modified high-strength magnesium-aluminum alloy wire, comprising the following steps:

[0007] Step 1: Preparation of the magnesium-aluminum alloy rod:

[0008] Weigh the following raw materials by weight percentage: Mg 3-5%, Cr 0.1-0.2%, Si 0.1-0.2%, Mn 0.1-0.15%, Y 0.02-0.05%, Gd 0.02-0.04%, with the balance being Al;

[0009] The above raw materials are then added to a smelting furnace for smelting. After complete smelting, the raw materials are cast into ingots.

[0010] The billet is then rolled into shape to obtain an 8-10mm magnesium-aluminum alloy rod;

[0011] Step 2: Adjust and oscillate the magnesium-aluminum alloy rod from Step 1 to modify it. After the process is completed, the modified magnesium-aluminum alloy rod is obtained.

[0012] Step 3: The modified magnesium-aluminum alloy rod is then subjected to a thermal cycling improvement treatment to obtain a cyclically thermally modified magnesium-aluminum alloy rod;

[0013] Step 4: The cyclically heat-modified magnesium-aluminum alloy rod is then further improved by continuous hot drawing.

[0014] The specific steps are as follows: the cyclically heat-modified magnesium-aluminum alloy rod is first drawn into a primary alloy wire using a wire drawing machine at a drawing speed of 2-3 m / s;

[0015] Then it is heat-treated, cooled to room temperature, and then drawn into a secondary alloy wire by a wire drawing machine. Finally, it is continuously drawn into a final alloy wire by a wire drawing machine.

[0016] Once the processing is complete, the modified high-strength magnesium-aluminum alloy wire of this invention will be obtained.

[0017] Preferably, the casting temperature for casting into ingots is 680-700℃; the rolling temperature is 480℃; and the heat treatment temperature in the continuous hot drawing improvement process is 550-750℃ for 3-5 minutes.

[0018] Preferably, the diameter of the primary alloy wire is 3.0 mm; the diameter of the secondary alloy wire is 0.70 mm; and the diameter of the final alloy wire is 0.08 mm.

[0019] Preferably, the specific steps for adjusting the oscillation modification treatment are as follows:

[0020] S01: Prepare a solution by mixing a 5-10% sodium dodecyl sulfate solution and a 3-5% chitosan solution at a weight ratio of 3:5. Then add a 5-7% phosphate buffer solution to the sodium dodecyl sulfate solution and stir thoroughly to obtain a sodium dodecyl sulfate solution.

[0021] S02: Preheat hydroxyapatite at 110-130℃ for 5-10 minutes, then air cool to room temperature;

[0022] Add 2-5% silica sol (total weight of preheated hydroxyapatite), 1-3% yttrium nitrate solution (total weight of preheated hydroxyapatite), and 5-10% sodium citrate solution (total weight of preheated hydroxyapatite) to preheated hydroxyapatite. Ball mill at 1000-1500 r / min for 1-2 h. After ball milling, wash with water and dry to obtain hydroxyapatite doped agent.

[0023] S03: Add 3-5 parts of sodium carboxymethyl cellulose and 4-7 parts of hydroxyapatite dopant to 8-12 parts of sodium dodecyl sulfate solution, stir at 750-850 r / min for 15-25 min, and after stirring, obtain the conditioning and modification solution.

[0024] S04: Place the magnesium-aluminum alloy rod in the conditioning and modifying liquid for ultrasonic oscillation modification treatment. After the treatment is completed, wash with water and dry.

[0025] Preferably, the pH value of the phosphate buffer solution is 5.5; the mass fraction of the yttrium nitrate solution is 2-5%; and the mass fraction of the sodium citrate solution is 10-15%.

[0026] Preferably, the ultrasonic oscillation modification has an oscillation power of 400-500W and an oscillation time of 1-2h.

[0027] Preferably, the specific steps of the thermal cycling improvement treatment are as follows:

[0028] S101: First, heat the modified magnesium-aluminum alloy rod to 310-320℃ at a rate of 1-3℃ / min, and hold for 5-7 minutes;

[0029] S102: Then heat to 450-470℃ at a rate of 4-6℃ / min, hold for 1-3 minutes, then cool to 55℃ at a rate of 2-5℃ / min and hold for heat treatment.

[0030] S103: The magnesium-aluminum alloy rod that has undergone S102 heat preservation treatment is immersed in a layered nano-mica modifier for improvement treatment. After the immersion improvement treatment is completed, it is washed with water and dried. Finally, it is hot-pressed at 105-115℃ and 10MPa for 4-7 minutes. After the treatment is completed, it is air-cooled to room temperature.

[0031] Preferably, the immersion pressure of the immersion improvement treatment is 5-10 MPa, and the immersion time is 20-30 min.

[0032] Preferably, the preparation method of the layered nano-mica modifier is as follows:

[0033] The layered nano-mica powder was first stirred and dispersed evenly in a 2% hydrochloric acid solution, then washed with water and dried, and then heat-treated at 210-230℃ for 10-15 min. After that, it was cooled to 48-50℃ at a rate of 1-3℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 450-550W and the ultrasonic time was 20-30 min. After the treatment was completed, the layered nano-mica modifier was obtained.

[0034] Preferably, the modified liquid comprises the following raw materials in parts by weight:

[0035] 6-10 parts of 5-7% lanthanum chloride solution, 1-3 parts of sodium lignosulfonate, 2-5 parts of diethanolamine and 0.25-0.35 parts of silane coupling agent KH560.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] 1. The high-strength magnesium-aluminum alloy wire of this invention uses Mg, Cr, Si, Mn, Y, Gd and Al raw materials to make the base material of the wire. Through the mutual combination and reinforcement of the raw materials, the overall performance of the base material is improved. The alloy rod is obtained by melting, casting into ingots, and rolling into shape. Then, it undergoes adjustment and vibration modification treatment and thermal cycling improvement treatment. Through the synergistic effect of the two, the strength and elongation properties of the product are coordinated and improved, and the high temperature resistance and salt and alkali stability of the product are significantly improved. Finally, it undergoes continuous hot drawing improvement treatment, with first-level, second-level and final drawing improvement treatments. The performance of the magnesium-aluminum alloy wire obtained is significantly improved compared with the prior art, the performance coordination of the product is improved, and the heat resistance and salt and alkali resistance are enhanced.

[0038] 2. In the oscillation modification process, sodium dodecyl sulfate solution, chitosan solution, and phosphate buffer solution are first prepared into a sodium dodecyl sulfate solution. Hydroxyapatite is then preheated at 110-130℃ for 5-10 minutes to optimize its activity. Further improvements are achieved through ball milling with silica sol, yttrium nitrate solution, and sodium citrate solution. The ball-milled hydroxyapatite then exhibits better miscibility with the sodium dodecyl sulfate solution. Simultaneously, sodium carboxymethyl cellulose is added. By adjusting the synergistic effects of the raw materials in the modification solution, the surface performance of the magnesium-aluminum alloy rod is enhanced, and the microstructure activity is improved. This better complements the thermal cycling modification treatment, enhancing the system's strength and elongation properties, and improving the overall performance of both processes. It also improves the product's heat resistance and salt and alkali resistance.

[0039] 3. Thermal cycling improvement treatment: First, the temperature is raised to 310-320℃ at a rate of 1-3℃ / min and held for 5-7min; then, the temperature is raised to 450-470℃ at a rate of 4-6℃ / min and held for 1-3min. Then, the temperature is cooled to 55℃ at a rate of 2-5℃ / min. Through this cycle of heating, holding, and constant-temperature cooling, the microstructure is optimized, and the grain structure is refined and thoroughly wetted. At the same time, a layered nano-mica modifier is added for further improvement treatment. Finally, the product is hot-pressed at 105-115℃ and 10MPa for 4-7min. The resulting product shows significant improvements in strength and elongation properties, as well as significantly enhanced heat resistance, salt and alkali resistance, and stability.

[0040] 4. The layered nano-mica modifier is made by dispersing layered nano-mica in hydrochloric acid solution to activate its activity. Simultaneously, it undergoes heat treatment at 210-230℃ for 10-15 minutes, followed by cooling to 48-50℃ at a rate of 1-3℃ / min to improve the interlayer spacing. This better synergistic effect of the layered nano-mica modifier on the alloy wire is achieved through a modifying liquid composed of lanthanum chloride solution, sodium lignosulfonate, diethanolamine, and silane coupling agent KH560. The synergistic effect of the raw materials in the modifying liquid further enhances the alloy microstructure during thermal cycling, improving the density of the microstructure. This results in a coordinated improvement in the product's strength and elongation properties, as well as a significant improvement in its high-temperature resistance and salt and alkali resistance. Detailed Implementation

[0041] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific examples. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0042] This embodiment describes a method for preparing modified high-strength magnesium-aluminum alloy wire, comprising the following steps:

[0043] Step 1: Preparation of the magnesium-aluminum alloy rod:

[0044] Weigh the following raw materials by weight percentage: Mg 3-5%, Cr 0.1-0.2%, Si 0.1-0.2%, Mn 0.1-0.15%, Y 0.02-0.05%, Gd 0.02-0.04%, with the balance being Al;

[0045] The above raw materials are then added to a smelting furnace for smelting. After complete smelting, the raw materials are cast into ingots.

[0046] The billet is then rolled into shape to obtain an 8-10mm magnesium-aluminum alloy rod;

[0047] Step 2: Adjust and oscillate the magnesium-aluminum alloy rod from Step 1 to modify it. After the process is completed, the modified magnesium-aluminum alloy rod is obtained.

[0048] Step 3: The modified magnesium-aluminum alloy rod is then subjected to a thermal cycling improvement treatment to obtain a cyclically thermally modified magnesium-aluminum alloy rod;

[0049] Step 4: The cyclically heat-modified magnesium-aluminum alloy rod is then further improved by continuous hot drawing.

[0050] The specific steps are as follows: the cyclically heat-modified magnesium-aluminum alloy rod is first drawn into a primary alloy wire using a wire drawing machine at a drawing speed of 2-3 m / s;

[0051] Then it is heat-treated, cooled to room temperature, and then drawn into a secondary alloy wire by a wire drawing machine. Finally, it is continuously drawn into a final alloy wire by a wire drawing machine.

[0052] Once the processing is complete, the modified high-strength magnesium-aluminum alloy wire of this invention will be obtained.

[0053] In this embodiment, the casting temperature for casting into ingots is 680-700℃; the rolling temperature is 480℃; and the heat treatment temperature in the continuous hot drawing improvement process is 550-750℃ for 3-5 minutes.

[0054] In this embodiment, the diameter of the primary alloy wire is 3.0 mm; the diameter of the secondary alloy wire is 0.70 mm; and the diameter of the final alloy wire is 0.08 mm.

[0055] The specific steps of the oscillation modification process in this embodiment are as follows:

[0056] S01: Prepare a solution by mixing a 5-10% sodium dodecyl sulfate solution and a 3-5% chitosan solution at a weight ratio of 3:5. Then add a 5-7% phosphate buffer solution to the sodium dodecyl sulfate solution and stir thoroughly to obtain a sodium dodecyl sulfate solution.

[0057] S02: Preheat hydroxyapatite at 110-130℃ for 5-10 minutes, then air cool to room temperature;

[0058] Add 2-5% silica sol (total weight of preheated hydroxyapatite), 1-3% yttrium nitrate solution (total weight of preheated hydroxyapatite), and 5-10% sodium citrate solution (total weight of preheated hydroxyapatite) to preheated hydroxyapatite. Ball mill at 1000-1500 r / min for 1-2 h. After ball milling, wash with water and dry to obtain hydroxyapatite doped agent.

[0059] S03: Add 3-5 parts of sodium carboxymethyl cellulose and 4-7 parts of hydroxyapatite dopant to 8-12 parts of sodium dodecyl sulfate solution, stir at 750-850 r / min for 15-25 min, and after stirring, obtain the conditioning and modification solution.

[0060] S04: Place the magnesium-aluminum alloy rod in the conditioning and modifying liquid for ultrasonic oscillation modification treatment. After the treatment is completed, wash with water and dry.

[0061] The phosphate buffer solution in this embodiment has a pH of 5.5; the yttrium nitrate solution has a mass fraction of 2-5%; and the sodium citrate solution has a mass fraction of 10-15%.

[0062] In this embodiment, the ultrasonic oscillation modification has an oscillation power of 400-500W and an oscillation time of 1-2h.

[0063] The specific steps of the thermal cycling improvement process in this embodiment are as follows:

[0064] S101: First, heat the modified magnesium-aluminum alloy rod to 310-320℃ at a rate of 1-3℃ / min, and hold for 5-7 minutes;

[0065] S102: Then heat to 450-470℃ at a rate of 4-6℃ / min, hold for 1-3 minutes, then cool to 55℃ at a rate of 2-5℃ / min and hold for heat treatment.

[0066] S103: The magnesium-aluminum alloy rod that has undergone S102 heat preservation treatment is immersed in a layered nano-mica modifier for improvement treatment. After the immersion improvement treatment is completed, it is washed with water and dried. Finally, it is hot-pressed at 105-115℃ and 10MPa for 4-7 minutes. After the treatment is completed, it is air-cooled to room temperature.

[0067] In this embodiment, the immersion pressure for the improved immersion treatment is 5-10 MPa, and the immersion time is 20-30 min.

[0068] The preparation method of the layered nano-mica modifier in this embodiment is as follows:

[0069] The layered nano-mica powder was first stirred and dispersed evenly in a 2% hydrochloric acid solution, then washed with water and dried, and then heat-treated at 210-230℃ for 10-15 min. After that, it was cooled to 48-50℃ at a rate of 1-3℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 450-550W and the ultrasonic time was 20-30 min. After the treatment was completed, the layered nano-mica modifier was obtained.

[0070] The modified liquid in this embodiment comprises the following raw materials in parts by weight:

[0071] 6-10 parts of 5-7% lanthanum chloride solution, 1-3 parts of sodium lignosulfonate, 2-5 parts of diethanolamine and 0.25-0.35 parts of silane coupling agent KH560.

[0072] Example 1.

[0073] This embodiment describes a method for preparing modified high-strength magnesium-aluminum alloy wire, comprising the following steps:

[0074] Step 1: Preparation of the magnesium-aluminum alloy rod:

[0075] Weigh the following raw materials by weight percentage: Mg 3%, Cr 0.1%, Si 0.1%, Mn 0.1%, Y 0.02%, Gd 0.02%, with the balance being Al;

[0076] The above raw materials are then added to a smelting furnace for smelting. After complete smelting, the raw materials are cast into ingots.

[0077] The billet is then rolled into shape to obtain an 8mm magnesium-aluminum alloy rod;

[0078] Step 2: Adjust and oscillate the magnesium-aluminum alloy rod from Step 1 to modify it. After the process is completed, the modified magnesium-aluminum alloy rod is obtained.

[0079] Step 3: The modified magnesium-aluminum alloy rod is then subjected to a thermal cycling improvement treatment to obtain a cyclically thermally modified magnesium-aluminum alloy rod;

[0080] Step 4: The cyclically heat-modified magnesium-aluminum alloy rod is then further improved by continuous hot drawing.

[0081] The specific steps are as follows: the cyclically heat-modified magnesium-aluminum alloy rod is first drawn into a primary alloy wire using a wire drawing machine at a drawing speed of 2m / s;

[0082] Then it is heat-treated, cooled to room temperature, and then drawn into a secondary alloy wire by a wire drawing machine. Finally, it is continuously drawn into a final alloy wire by a wire drawing machine.

[0083] Once the processing is complete, the modified high-strength magnesium-aluminum alloy wire of this invention will be obtained.

[0084] In this embodiment, the casting temperature for casting into ingots is 680°C; the rolling temperature is 480°C; and the heat treatment temperature in the continuous hot drawing improvement process is 550°C for 3 minutes.

[0085] In this embodiment, the diameter of the primary alloy wire is 3.0 mm; the diameter of the secondary alloy wire is 0.70 mm; and the diameter of the final alloy wire is 0.08 mm.

[0086] The specific steps of the oscillation modification process in this embodiment are as follows:

[0087] S01: Prepare a solution by mixing 5% sodium dodecyl sulfate solution and 3% chitosan solution at a weight ratio of 3:5. Then add 5% of the total sodium dodecyl sulfate solution as phosphate buffer solution and stir thoroughly to obtain sodium dodecyl sulfate solution.

[0088] S02: Preheat hydroxyapatite at 110℃ for 5 minutes, then air cool to room temperature;

[0089] Add 2% silica sol (total weight of preheated hydroxyapatite), 1% yttrium nitrate solution (total weight of preheated hydroxyapatite), and 5% sodium citrate solution (total weight of preheated hydroxyapatite) to preheated hydroxyapatite. Ball mill at 1000 r / min for 1 h. After ball milling, wash with water and dry to obtain hydroxyapatite doped agent.

[0090] S03: Add 3 parts sodium carboxymethyl cellulose and 4 parts doped hydroxyapatite to 8 parts sodium dodecyl sulfate solution, stir at 750 r / min for 15 min, and after stirring, the modified solution is obtained.

[0091] S04: Place the magnesium-aluminum alloy rod in the conditioning and modifying liquid for ultrasonic oscillation modification treatment. After the treatment is completed, wash with water and dry.

[0092] The phosphate buffer solution in this embodiment has a pH of 5.5; the yttrium nitrate solution has a mass fraction of 2%; and the sodium citrate solution has a mass fraction of 10%.

[0093] In this embodiment, the ultrasonic oscillation modification has an oscillation power of 400W and an oscillation time of 1h.

[0094] The specific steps of the thermal cycling improvement process in this embodiment are as follows:

[0095] S101: The modified magnesium-aluminum alloy rod is first heated to 310℃ at a rate of 1℃ / min and held for 5min;

[0096] S102: Then heat to 450℃ at a rate of 4℃ / min, hold for 1 min, then cool to 55℃ at a rate of 2℃ / min and hold for 1 min.

[0097] S103: The magnesium-aluminum alloy rod that has undergone S102 heat preservation treatment is immersed in a layered nano-mica modifier for improvement treatment. After the immersion improvement treatment is completed, it is washed with water and dried. Finally, it is hot-pressed at 105℃ and 10MPa for 4 minutes. After the treatment is completed, it is air-cooled to room temperature.

[0098] In this embodiment, the immersion pressure for the improved immersion treatment is 5 MPa, and the immersion time is 20 min.

[0099] The preparation method of the layered nano-mica modifier in this embodiment is as follows:

[0100] The layered nano-mica powder was first stirred and dispersed evenly in a 2% hydrochloric acid solution, then washed with water and dried, and then heat-treated at 210℃ for 10 min. After that, it was cooled to 48℃ at a rate of 1℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 450W and the ultrasonic time was 20 min. After the treatment was completed, the layered nano-mica modifier was obtained.

[0101] The modified liquid in this embodiment comprises the following raw materials in parts by weight:

[0102] Six parts of a 5% (w / w) lanthanum chloride solution, one part of sodium lignosulfonate, two parts of diethanolamine, and 0.25 parts of silane coupling agent KH560.

[0103] Example 2.

[0104] This embodiment describes a method for preparing modified high-strength magnesium-aluminum alloy wire, comprising the following steps:

[0105] Step 1: Preparation of the magnesium-aluminum alloy rod:

[0106] Weigh the following raw materials by weight percentage: Mg 5%, Cr 0.2%, Si 0.2%, Mn 0.15%, Y 0.05%, Gd 0.04%, with the balance being Al;

[0107] The above raw materials are then added to a smelting furnace for smelting. After complete smelting, the raw materials are cast into ingots.

[0108] The billet is then rolled into shape to obtain a 10mm magnesium-aluminum alloy rod;

[0109] Step 2: Adjust and oscillate the magnesium-aluminum alloy rod from Step 1 to modify it. After the process is completed, the modified magnesium-aluminum alloy rod is obtained.

[0110] Step 3: The modified magnesium-aluminum alloy rod is then subjected to a thermal cycling improvement treatment to obtain a cyclically thermally modified magnesium-aluminum alloy rod;

[0111] Step 4: The cyclically heat-modified magnesium-aluminum alloy rod is then further improved by continuous hot drawing.

[0112] The specific steps are as follows: the cyclically heat-modified magnesium-aluminum alloy rod is first drawn into a primary alloy wire using a wire drawing machine at a drawing speed of 3m / s;

[0113] Then it is heat-treated, cooled to room temperature, and then drawn into a secondary alloy wire by a wire drawing machine. Finally, it is continuously drawn into a final alloy wire by a wire drawing machine.

[0114] Once the processing is complete, the modified high-strength magnesium-aluminum alloy wire of this invention will be obtained.

[0115] In this embodiment, the casting temperature for casting into ingots is 700℃; the rolling temperature is 480℃; and the heat treatment temperature in the continuous hot drawing improvement process is 750℃ for 5 minutes.

[0116] In this embodiment, the diameter of the primary alloy wire is 3.0 mm; the diameter of the secondary alloy wire is 0.70 mm; and the diameter of the final alloy wire is 0.08 mm.

[0117] The specific steps of the oscillation modification process in this embodiment are as follows:

[0118] S01: Prepare a solution by mixing 10% sodium dodecyl sulfate solution and 5% chitosan solution at a weight ratio of 3:5. Then add 7% of the total sodium dodecyl sulfate solution as phosphate buffer solution and stir thoroughly to obtain sodium dodecyl sulfate solution.

[0119] S02: Preheat hydroxyapatite at 130℃ for 10 minutes, then air cool to room temperature;

[0120] Add 5% silica sol (total weight of preheated hydroxyapatite), 3% yttrium nitrate solution (total weight of preheated hydroxyapatite), and 10% sodium citrate solution (total weight of preheated hydroxyapatite) to preheated hydroxyapatite. Ball mill at 1500 r / min for 2 h. After ball milling, wash with water and dry to obtain hydroxyapatite doped agent.

[0121] S03: Add 5 parts of sodium carboxymethyl cellulose and 7 parts of doped hydroxyapatite to 12 parts of sodium dodecyl sulfate solution, stir at 850 r / min for 25 min, and after stirring, obtain the conditioning and modification solution;

[0122] S04: Place the magnesium-aluminum alloy rod in the conditioning and modifying liquid for ultrasonic oscillation modification treatment. After the treatment is completed, wash with water and dry.

[0123] The phosphate buffer solution in this embodiment has a pH of 5.5; the yttrium nitrate solution has a mass fraction of 5%; and the sodium citrate solution has a mass fraction of 15%.

[0124] In this embodiment, the ultrasonic oscillation modification uses an oscillation power of 500W and an oscillation time of 2h.

[0125] The specific steps of the thermal cycling improvement process in this embodiment are as follows:

[0126] S101: The modified magnesium-aluminum alloy rod is first heated to 320℃ at a rate of 3℃ / min and held for 7min;

[0127] S102: Then heat to 470℃ at a rate of 6℃ / min, hold for 3 minutes, then cool to 55℃ at a rate of 5℃ / min and hold for 3 minutes.

[0128] S103: The magnesium-aluminum alloy rod that has undergone S102 heat insulation treatment is immersed in a layered nano-mica modifier for improvement treatment. After the immersion improvement treatment is completed, it is washed with water and dried. Finally, it is hot-pressed at 115℃ and 10MPa for 7 minutes. After the treatment is completed, it is air-cooled to room temperature.

[0129] In this embodiment, the immersion pressure for the improved immersion treatment is 10 MPa, and the immersion time is 30 min.

[0130] The preparation method of the layered nano-mica modifier in this embodiment is as follows:

[0131] The layered nano-mica powder was first stirred and dispersed evenly in a 2% hydrochloric acid solution, then washed with water and dried, and then heat-treated at 230℃ for 15 min. After that, it was cooled to 50℃ at a rate of 3℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 550W and the ultrasonic time was 30 min. After the treatment was completed, the layered nano-mica modifier was obtained.

[0132] The modified liquid in this embodiment comprises the following raw materials in parts by weight:

[0133] 10 parts of a 7% (w / w) lanthanum chloride solution, 3 parts of sodium lignosulfonate, 5 parts of diethanolamine, and 0.35 parts of silane coupling agent KH560.

[0134] Example 3.

[0135] This embodiment describes a method for preparing modified high-strength magnesium-aluminum alloy wire, comprising the following steps:

[0136] Step 1: Preparation of the magnesium-aluminum alloy rod:

[0137] Weigh the following raw materials by weight percentage: Mg 4%, Cr 0.15%, Si 0.15%, Mn 0.12%, Y 0.035%, Gd 0.03%, with the balance being Al;

[0138] The above raw materials are then added to a smelting furnace for smelting. After complete smelting, the raw materials are cast into ingots.

[0139] The billet is then rolled into shape to obtain a 9mm magnesium-aluminum alloy rod;

[0140] Step 2: Adjust and oscillate the magnesium-aluminum alloy rod from Step 1 to modify it. After the process is completed, the modified magnesium-aluminum alloy rod is obtained.

[0141] Step 3: The modified magnesium-aluminum alloy rod is then subjected to a thermal cycling improvement treatment to obtain a cyclically thermally modified magnesium-aluminum alloy rod;

[0142] Step 4: The cyclically heat-modified magnesium-aluminum alloy rod is then further improved by continuous hot drawing.

[0143] The specific steps are as follows: the cyclically heat-modified magnesium-aluminum alloy rod is first drawn into a primary alloy wire using a wire drawing machine at a drawing speed of 2.5 m / s;

[0144] Then it is heat-treated, cooled to room temperature, and then drawn into a secondary alloy wire by a wire drawing machine. Finally, it is continuously drawn into a final alloy wire by a wire drawing machine.

[0145] Once the processing is complete, the modified high-strength magnesium-aluminum alloy wire of this invention will be obtained.

[0146] In this embodiment, the casting temperature for casting into ingots is 690°C; the rolling temperature is 480°C; and the heat treatment temperature in the continuous hot drawing improvement process is 600°C for 4 minutes.

[0147] In this embodiment, the diameter of the primary alloy wire is 3.0 mm; the diameter of the secondary alloy wire is 0.70 mm; and the diameter of the final alloy wire is 0.08 mm.

[0148] The specific steps of the oscillation modification process in this embodiment are as follows:

[0149] S01: Prepare a solution by mixing a 7.5% sodium dodecyl sulfate solution and a 4% chitosan solution at a weight ratio of 3:5. Then add 6% of the total sodium dodecyl sulfate solution as phosphate buffer solution and stir thoroughly to obtain a sodium dodecyl sulfate solution.

[0150] S02: Preheat hydroxyapatite at 120℃ for 7.5 min, then air cool to room temperature;

[0151] Add 3.5% silica sol (total weight of preheated hydroxyapatite), 2% yttrium nitrate solution (total weight of preheated hydroxyapatite), and 7.5% sodium citrate solution (total weight of preheated hydroxyapatite) to preheated hydroxyapatite. Ball mill at 1250 r / min for 1.5 h. After ball milling, wash with water and dry to obtain hydroxyapatite doped agent.

[0152] S03: Add 4 parts sodium carboxymethyl cellulose and 5.5 parts doped hydroxyapatite to 10 parts sodium dodecyl sulfate solution, stir at 800 r / min for 20 min, and after stirring, obtain the conditioning and modification solution;

[0153] S04: Place the magnesium-aluminum alloy rod in the conditioning and modifying liquid for ultrasonic oscillation modification treatment. After the treatment is completed, wash with water and dry.

[0154] The phosphate buffer solution in this embodiment has a pH of 5.5; the yttrium nitrate solution has a mass fraction of 3.5%; and the sodium citrate solution has a mass fraction of 12.5%.

[0155] In this embodiment, the ultrasonic oscillation modification has an oscillation power of 450W and an oscillation time of 1.5h.

[0156] The specific steps of the thermal cycling improvement process in this embodiment are as follows:

[0157] S101: The modified magnesium-aluminum alloy rod is first heated to 315℃ at a rate of 2℃ / min and held for 6min;

[0158] S102: Then heat to 460℃ at a rate of 5℃ / min, hold for 2min, then cool to 55℃ at a rate of 3.5℃ / min and hold for 2min.

[0159] S103: The magnesium-aluminum alloy rod that has undergone S102 heat preservation treatment is immersed in a layered nano-mica modifier for improvement treatment. After the immersion improvement treatment is completed, it is washed with water and dried. Finally, it is hot-pressed at 110℃ and 10MPa for 5.5 minutes. After the treatment is completed, it is air-cooled to room temperature.

[0160] In this embodiment, the immersion pressure for the improved immersion treatment is 7.5 MPa, and the immersion time is 25 min.

[0161] The preparation method of the layered nano-mica modifier in this embodiment is as follows:

[0162] The layered nano-mica powder was first stirred and dispersed evenly in a 2% hydrochloric acid solution, then washed with water and dried, and then heat-treated at 220℃ for 12.5 min. After that, it was cooled to 49℃ at a rate of 2℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 450-550W and the ultrasonic time was 25 min. After the treatment was completed, the layered nano-mica modifier was obtained.

[0163] The modified liquid in this embodiment comprises the following raw materials in parts by weight:

[0164] 8 parts of 6% lanthanum chloride solution, 2 parts of sodium lignosulfonate, 3.5 parts of diethanolamine and 0.30 parts of silane coupling agent KH560.

[0165] Comparative Example 1.

[0166] Unlike Example 3, the magnesium-aluminum alloy rod was not used to adjust the oscillation modification treatment.

[0167] Comparative Example 2.

[0168] Unlike Example 3, the sodium dodecyl sulfate solution in the magnesium-aluminum alloy rod oscillation modification treatment was replaced with a sodium dodecylbenzene sulfonate solution with a mass fraction of 7.5%.

[0169] Comparative Example 3.

[0170] Unlike Example 3, the oscillation modification treatment of the magnesium-aluminum alloy rod did not involve the addition of doped hydroxyapatite to the modification solution.

[0171] Comparative Example 4.

[0172] Unlike Example 3, the hydroxyapatite dopant is replaced with hydroxyapatite.

[0173] Comparative Example 5.

[0174] Unlike Example 3, the preparation of the doped hydroxyapatite agent did not involve treatment with silica sol or yttrium nitrate solution.

[0175] Comparative Example 6.

[0176] Unlike Example 3, no thermal cycling improvement treatment was used.

[0177] Comparative Example 7.

[0178] Unlike Example 3, in the thermal cycling improvement treatment, S101: the modified magnesium-aluminum alloy rod is directly heated to 460°C at a rate of 5°C / min and held at that temperature for 2min. The conditions for the remaining steps are the same.

[0179] Comparative Example 8.

[0180] Unlike Example 3, in the thermal cycling improvement treatment S101: the modified magnesium-aluminum alloy rod is first heated to 315°C at a rate of 2°C / min and held for 6min; then cooled to 55°C at a rate of 3.5°C / min and held for 6min. The remaining steps are the same.

[0181] Comparative Example 9.

[0182] Unlike Example 3, this method did not employ the immersion and improvement treatment with a layered nano-mica modifier.

[0183] The tensile strength and elongation properties of the products in Examples 1-3 and Comparative Examples 1-9 were tested. At the same time, the products were placed in a 2% sodium chloride salt spray for 5 hours and then placed at 210°C for 2 hours to test their salt and alkali resistance and temperature stability. The test results are as follows.

[0184]

[0185] As can be seen from Comparative Examples 1-9 and Examples 1-3;

[0186] The product in Example 3 has excellent tensile strength and elongation, and the two properties can be improved in a coordinated manner. At the same time, the product has excellent stability under salt and alkali resistance and temperature resistance conditions.

[0187] As can be seen from Comparative Examples 1-5 and Example 3, the performance of the product deteriorates significantly because the magnesium-aluminum alloy rod oscillation modification treatment was not used in this invention. In the magnesium-aluminum alloy rod oscillation modification treatment, sodium dodecyl sulfate solution was replaced with a 7.5% sodium dodecylbenzenesulfonate solution; no hydroxyapatite dopant was added to the modification solution; hydroxyapatite was used instead of the hydroxyapatite dopant; and silica sol and yttrium nitrate solution were not used in the preparation of the hydroxyapatite dopant. The performance of the product deteriorates in all these cases. The hydroxyapatite dopant prepared by the method of this invention, combined with the sodium dodecyl sulfate solution prepared by the specific process of this invention and the modification solution prepared by the method of this invention, results in the most significant performance improvement. Other methods are not as effective as those of this invention.

[0188] As can be seen from Comparative Examples 6-9, Comparative Example 1 and Example 3, the performance of the products showed a significant trend of deterioration when neither the magnesium-aluminum alloy rod regulation oscillation modification treatment nor the thermal cycling improvement treatment was used. The product performance was most significantly improved when both were used in combination for synergistic effect.

[0189] In the thermal cycling improvement treatment, the modified magnesium-aluminum alloy rod was directly heated to 460°C at a rate of 5°C / min and held for 2 minutes. The modified magnesium-aluminum alloy rod was then heated to 315°C at a rate of 2°C / min and held for 6 minutes; subsequently, it was cooled to 55°C at a rate of 3.5°C / min and held. Both methods, including those without the use of layered nano-mica modifier, resulted in a deterioration in product performance. The deterioration was more pronounced without the layered nano-mica modifier. The thermal cycling improvement treatment using the method of this invention yielded the most significant performance improvement.

[0190] This invention further explores the product performance through the preparation of a layered nano-mica modifier;

[0191] The preparation method of the layered nano-mica modifier is as follows:

[0192] The layered nano-mica powder was first stirred and dispersed evenly in a 2% hydrochloric acid solution, then washed with water and dried, and then heat-treated at 220℃ for 12.5 min. After that, it was cooled to 49℃ at a rate of 2℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 450-550W and the ultrasonic time was 25 min. After the treatment was completed, the layered nano-mica modifier was obtained.

[0193] The modified liquid comprises the following raw materials in parts by weight:

[0194] 8 parts of 6% lanthanum chloride solution, 2 parts of sodium lignosulfonate, 3.5 parts of diethanolamine and 0.30 parts of silane coupling agent KH560.

[0195] Experimental Example 1.

[0196] Similar to Example 3, except that the layered nano-mica modifier was not heat-treated at 220°C for 12.5 min and then cooled to 49°C at a rate of 2°C / min.

[0197] Experimental Example 2.

[0198] Same as Example 3, except that no modifying liquid was used in the preparation of the layered nano-mica modifier.

[0199] Experimental Example 3.

[0200] Same as Example 3, except that lanthanum chloride solution was not added in the preparation of the modified liquid.

[0201] Experimental Example 4.

[0202] Same as Example 3, except that diethanolamine was not added in the preparation of the modified liquid.

[0203] Experimental Example 5.

[0204] Same as Example 3, except that silane coupling agent KH560 was not added in the preparation of the modified liquid.

[0205] Experimental Example 6.

[0206] Same as Example 3, except that sodium lignosulfonate was not added in the preparation of the modified liquid.

[0207] The performance test results of Experiment 1-6 are as follows:

[0208]

[0209] As can be seen from Experiments 1-6, the performance of the product deteriorated significantly when no modifying liquid treatment was used in the preparation of the layered nano-mica modifier. The performance of the product also deteriorated to varying degrees when one of the following was not added to the modifying liquid: lanthanum chloride solution, sodium lignosulfonate, diethanolamine, or silane coupling agent KH560. The product showed the most significant performance improvement when the raw materials of the modifying liquid were mixed and combined. Furthermore, the performance of the product deteriorated when the layered nano-mica modifier was not prepared by heat treatment at 220°C for 12.5 min followed by cooling to 49°C at a rate of 2°C / min. Only the layered nano-mica modifier prepared using the method of this invention showed the most significant performance improvement.

[0210] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

[0211] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for preparing modified high-strength magnesium-aluminum alloy wire, characterized in that, Includes the following steps: Step 1: Preparation of the magnesium-aluminum alloy rod: Weigh the following raw materials by weight percentage: Mg 3-5%, Cr 0.1-0.2%, Si 0.1-0.2%, Mn 0.1-0.15%, Y 0.02-0.05%, Gd 0.02-0.04%, with the balance being Al; The above raw materials are then added to a smelting furnace for smelting. After complete smelting, the raw materials are cast into ingots. Then it is rolled into shape to obtain a magnesium-aluminum alloy rod with a thickness of 8-10mm; Step 2: Adjust and oscillate the magnesium-aluminum alloy rod from Step 1 to modify it. After the process is completed, the modified magnesium-aluminum alloy rod is obtained. Step 3: The modified magnesium-aluminum alloy rod is then subjected to a thermal cycling improvement treatment to obtain a cyclically thermally modified magnesium-aluminum alloy rod; Step 4: The cyclically heat-modified magnesium-aluminum alloy rod is then further improved by continuous hot drawing. The specific steps are as follows: the cyclically heat-modified magnesium-aluminum alloy rod is first drawn into a primary alloy wire using a wire drawing machine at a drawing speed of 2-3 m / s; Then it is heat-treated, cooled to room temperature, and then drawn into a secondary alloy wire by a wire drawing machine. Finally, it is continuously drawn into a final alloy wire by a wire drawing machine. Once the process is complete, modified high-strength magnesium-aluminum alloy wire is obtained; The specific steps for adjusting the oscillation modification treatment are as follows: S01: Prepare a solution by mixing a 5-10% sodium dodecyl sulfate solution and a 3-5% chitosan solution at a weight ratio of 3:

5. Then add a 5-7% phosphate buffer solution to the sodium dodecyl sulfate solution and stir thoroughly to obtain a sodium dodecyl sulfate solution. S02: Preheat hydroxyapatite at 110-130℃ for 5-10 minutes, then air cool to room temperature; Add 2-5% silica sol (total weight of preheated hydroxyapatite), 1-3% yttrium nitrate solution (total weight of preheated hydroxyapatite), and 5-10% sodium citrate solution (total weight of preheated hydroxyapatite) to preheated hydroxyapatite. Ball mill at 1000-1500 r / min for 1-2 h. After ball milling, wash with water and dry to obtain hydroxyapatite doped agent. S03: Add 3-5 parts of sodium carboxymethyl cellulose and 4-7 parts of hydroxyapatite dopant to 8-12 parts of sodium dodecyl sulfate solution, stir at 750-850 r / min for 15-25 min, and after stirring, obtain the conditioning and modification solution. S04: Place the magnesium-aluminum alloy rod in the conditioning and modifying liquid for ultrasonic oscillation modification treatment. After the treatment is completed, wash with water and dry.

2. The method for preparing modified high-strength magnesium-aluminum alloy wire according to claim 1, characterized in that, The casting temperature for casting into ingots is 680-700℃; the rolling temperature is 480℃; and the heat treatment temperature in the continuous hot drawing improvement process is 550-750℃ for 3-5 minutes.

3. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 1, characterized in that, The diameter of the primary alloy wire is 3.0 mm; the diameter of the secondary alloy wire is 0.70 mm; and the diameter of the final alloy wire is 0.08 mm.

4. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 1, characterized in that, The pH value of the phosphate buffer solution is 5.5; the mass fraction of the yttrium nitrate solution is 2-5%; and the mass fraction of the sodium citrate solution is 10-15%.

5. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 1, characterized in that, The ultrasonic oscillation modification has an oscillation power of 400-500W and an oscillation time of 1-2h.

6. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 1, characterized in that, The specific steps of the thermal cycling improvement treatment are as follows: S101: First, heat the modified magnesium-aluminum alloy rod to 310-320℃ at a rate of 1-3℃ / min, and hold for 5-7 minutes; S102: Then heat to 450-470℃ at a rate of 4-6℃ / min, hold for 1-3 minutes, then cool to 55℃ at a rate of 2-5℃ / min and hold for heat treatment. S103: The magnesium-aluminum alloy rod that has undergone S102 heat preservation treatment is immersed in a layered nano-mica modifier for improvement treatment. After the immersion improvement treatment is completed, it is washed with water and dried. Finally, it is hot-pressed at 105-115℃ and 10MPa for 4-7 minutes. After the treatment is completed, it is air-cooled to room temperature.

7. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 6, characterized in that, The immersion pressure for the improved immersion treatment is 5-10 MPa, and the immersion time is 20-30 min.

8. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 6, characterized in that, The preparation method of the layered nano-mica modifier is as follows: The layered nano-mica powder was first dispersed evenly in a 2% hydrochloric acid solution by stirring, then washed with water and dried, and then heat-treated at 210-230℃ for 10-15 min. After that, it was cooled to 48-50℃ at a rate of 1-3℃ / min, and finally placed in a modifying liquid for ultrasonic modification treatment. The ultrasonic power was 450-550W and the ultrasonic time was 20-30 min. After the treatment was completed, the layered nano-mica modifier was obtained.

9. The method for preparing a modified high-strength magnesium-aluminum alloy wire according to claim 8, characterized in that, The modified liquid comprises the following raw materials in parts by weight: 6-10 parts of lanthanum chloride solution (5-7% by mass), 1-3 parts of sodium lignosulfonate, 2-5 parts of diethanolamine, and 0.25-0.35 parts of silane coupling agent KH560.

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