A method for preparing a TA18 titanium alloy ultrafine wire

Abstract

The application relates to a preparation method of TA18 titanium alloy superfine wire, which comprises the following steps: obtaining a target TA18 titanium alloy wire blank, winding the target TA18 titanium alloy wire blank, and then performing temperature-controlled vacuum annealing; performing at least one cold drawing on the target TA18 titanium alloy wire blank, and then performing online temperature-controlled atmosphere annealing after each cold drawing; obtaining a final annealed wire blank with a diameter less than or equal to a target diameter after the last online temperature-controlled atmosphere annealing, wherein the target diameter is less than or equal to 1 mm; and finally performing online pickling treatment on the final annealed wire blank to obtain the TA18 titanium alloy superfine wire. The TA18 titanium alloy superfine wire prepared by the method has low impurity content, high surface quality, high size tolerance and high straightness.

Description

Technical Field

[0001] This invention relates to the field of titanium alloy wire processing technology, and in particular to a method for preparing TA18 titanium alloy ultrafine wire. Background Technology

[0002] TA18 titanium alloy is a near-α type titanium alloy with a nominal composition of Ti-3Al-2.5V. It has good cold formability, corrosion resistance and biocompatibility. At room temperature, its strength is 20% to 50% higher than that of industrial pure titanium, and its comprehensive performance is excellent.

[0003] TA18 titanium alloy ultrafine wires can be used to process products such as sutures in the medical field. The processing of sutures and similar products requires high-quality TA18 ultrafine wires with excellent chemical and mechanical properties. However, currently, when using TA18 titanium alloy to prepare ultrafine wires smaller than 1 mm, the processing involves multiple drawing operations, resulting in severe work hardening. This necessitates repeated annealing cycles before further drawing, which easily leads to oxygen and hydrogen accumulation in the TA18 ultrafine wires during annealing, causing excessive levels of impurities. These impurities significantly impact the mechanical properties of the TA18 ultrafine wires. Furthermore, due to the excellent plasticity of TA18, mechanical polishing after processing into ultrafine wires smaller than 1 mm easily causes wire bending and dimensional inconsistencies, which is detrimental to the subsequent processing of sutures and similar products. Summary of the Invention

[0004] Therefore, it is necessary to provide a method for preparing TA18 titanium alloy ultrafine wire to address the above-mentioned technical problems. The prepared TA18 titanium alloy ultrafine wire has low impurity content and excellent surface quality and dimensional tolerance.

[0005] This invention provides a method for preparing TA18 titanium alloy ultrafine wire, comprising:

[0006] Obtain the target TA18 titanium alloy wire blank. The surface of the target TA18 titanium alloy wire blank is bright, and the diameter is 1.2mm to 1.0mm.

[0007] The target TA18 titanium alloy wire blank is coiled and then subjected to temperature-controlled vacuum annealing.

[0008] The target TA18 titanium alloy wire blank is subjected to at least one cold drawing. After each cold drawing, an online temperature-controlled atmosphere annealing treatment is performed. After the last online temperature-controlled atmosphere annealing treatment, a final annealed wire blank with a diameter less than or equal to the target diameter is obtained. The target diameter is less than or equal to 1 mm.

[0009] In this process, a wire drawing die group consisting of multiple wire drawing dies with different die hole diameters is used for each cold drawing. The wire drawing dies in the wire drawing die group are connected in series. The die hole diameter of the wire drawing die in the wire drawing die group decreases by 7% to 9% from the wire inlet end to the wire outlet end. The total deformation of the wire drawing die group is 25% to 45%. When there are multiple cold drawing cycles, the die hole diameter of the wire drawing die at the wire inlet end of the wire drawing die group used in the later cold drawing is smaller than the die hole diameter of the wire outlet end of the wire drawing die group used in the previous cold drawing, or the number of wire drawing dies in the wire drawing die group in the later cold drawing is greater than the number of wire drawing dies in the wire drawing die group in the previous cold drawing.

[0010] The final annealed wire blank was subjected to online pickling treatment to obtain TA18 titanium alloy ultrafine wire.

[0011] In one embodiment, the target TA18 titanium alloy wire blank is cold-drawn N times. After the first N-1 cold drawing, an intermediate drawn wire blank is obtained. The intermediate drawn wire blank is subjected to intermediate online temperature-controlled atmosphere annealing treatment to obtain an intermediate annealed wire blank. After the last cold drawing, a final drawn wire blank is obtained. The final drawn wire blank is subjected to final online temperature-controlled atmosphere annealing treatment to obtain a final annealed wire blank. N is greater than or equal to 2.

[0012] In one embodiment, the online pickling process for the final annealed yarn blank involves sequentially placing the final annealed yarn blank into a pickling tank, a water tank, and a drying chamber.

[0013] In one embodiment, the coiled target TA18 titanium alloy wire blank is subjected to temperature-controlled vacuum annealing in a vacuum annealing furnace. The annealing temperature during temperature-controlled vacuum annealing is 700℃~850℃, the holding time is 1h~3h, and the vacuum degree is less than 2.0×10⁻⁶. -3 Pa.

[0014] In one embodiment, the annealing temperature during online temperature-controlled annealing is 600℃~800℃, the holding time is 20s~60s, the atmosphere is an inert gas, the atmosphere flow rate is 5L / min~10L / min, and the leakage rate is less than 2L / min.

[0015] In one embodiment, the pickling solution composition of the pickling tank, by volume, is HF:HNO3:H2O = 2~3:3~4:5~3;

[0016] The final annealed filament is placed in the pickling tank for 10 to 50 seconds, and the temperature of the drying chamber is 50 to 100 degrees Celsius.

[0017] In one embodiment, a lubricant is sprayed onto the wire drawing die assembly during cold drawing. The lubricant is titanium alloy wire drawing oil, and the wire drawing die is a diamond wire drawing die.

[0018] In one embodiment, the intermediate online temperature-controlled annealing parameters for intermediate drawn wire blanks of different diameters are different, specifically:

[0019] When the diameter of the intermediate drawn wire blank is 1.0mm to 0.8mm, the intermediate online temperature-controlled atmosphere annealing temperature is 800℃ and the holding time is 60s;

[0020] When the diameter of the intermediate drawn wire blank is 0.6mm to 0.8mm, the intermediate online temperature-controlled atmosphere annealing temperature is 750℃ and the holding time is 50s;

[0021] When the diameter of the intermediate drawn wire blank is 0.4mm to 0.6mm, the intermediate online temperature-controlled annealing temperature is 700℃ and the holding time is 40s;

[0022] When the diameter of the intermediate drawn wire blank is 0.2mm to 0.4mm, the intermediate online temperature-controlled atmosphere annealing temperature is 650℃ and the holding time is 30s;

[0023] When the diameter of the intermediate drawn wire blank is 0mm to 0.2mm, the intermediate online temperature-controlled annealing temperature is 600℃ and the holding time is 20s.

[0024] In one embodiment, the final online temperature-controlled annealing parameters differ for wire blanks of different diameters in the final drawn state. Specifically:

[0025] When the diameter of the final drawn wire blank is 1.0 mm to 0.8 mm, the online temperature-controlled annealing temperature is 750℃ and the holding time is 40 s;

[0026] When the diameter of the final drawn wire blank is 0.6mm to 0.8mm, the online temperature-controlled annealing temperature is 740℃ and the holding time is 40s;

[0027] When the diameter of the final drawn wire blank is 0.4mm to 0.6mm, the online temperature-controlled annealing temperature is 730℃ and the holding time is 30s;

[0028] When the diameter of the final drawn wire blank is 0.2mm to 0.4mm, the online temperature-controlled annealing temperature is 720℃ and the holding time is 30s;

[0029] When the diameter of the final drawn wire blank is 0mm to 0.2mm, the online temperature-controlled annealing temperature is 700℃ and the holding time is 20s.

[0030] In one embodiment, the final annealed yarn blanks of different diameters are placed in the pickling bath for different times, specifically:

[0031] When the diameter of the final annealed wire blank is 1.0 mm to 0.8 mm, the pickling time is 50 s.

[0032] When the diameter of the final annealed wire blank is 0.6mm to 0.8mm, the pickling time is 40s.

[0033] When the diameter of the final annealed wire blank is 0.4mm to 0.6mm, the pickling time is 30s.

[0034] When the diameter of the final annealed wire blank is 0.2mm to 0.4mm, the pickling time is 20s.

[0035] When the diameter of the final annealed wire blank is 0mm to 0.2mm, the pickling time is 10s.

[0036] The beneficial effects of this invention are:

[0037] (1) In the cold drawing process, the present invention uses an online temperature-controlled atmosphere annealing method to anneal the drawn wire blank. Different annealing temperatures and holding times are selected according to the different diameters of the intermediate drawn wire blank and the final drawn wire blank. The atmosphere is used to protect the wire blank, which can effectively reduce the entry of impurity elements such as oxygen and hydrogen during the preparation of TA18 titanium alloy ultrafine wire and reduce the impurity content of TA18 titanium alloy ultrafine wire.

[0038] (2) In this invention, the target TA18 titanium alloy wire blank is coiled and then subjected to temperature-controlled vacuum annealing. Temperature-controlled vacuum annealing effectively reduces the impurity content of TA18 titanium alloy ultrafine wire.

[0039] (3) In this invention, the diameter of the die hole of the wire drawing die group from the wire inlet end to the wire outlet end decreases by 7% to 9% according to the deformation amount. The total deformation amount of the wire drawing die group is 25% to 45%. Using the wire drawing die group with precise control of deformation amount to cold draw the wire blank is beneficial to continuous cold drawing and uniform deformation of the wire blank, forming TA18 titanium alloy ultrafine wire with excellent surface quality and dimensional tolerance.

[0040] (4) In this invention, the final annealed wire blank is subjected to online pickling treatment to obtain TA18 titanium alloy ultrafine wire that is non-bending, has good straightness, and has uniform and stable dimensions. Attached Figure Description

[0041] Figure 1 This is one of the flowcharts illustrating the preparation method of TA18 titanium alloy ultrafine wire provided in this embodiment of the invention;

[0042] Figure 2 This is a schematic diagram of the microstructure of TA18 titanium alloy ultrafine wire provided in one embodiment of the present invention. Detailed Implementation

[0043] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0044] In one embodiment, such as Figure 1 As shown, Figure 1 This is one of the flowcharts illustrating the preparation method of TA18 titanium alloy ultrafine wire provided in this embodiment of the invention. The preparation method of TA18 titanium alloy ultrafine wire includes:

[0045] S101. Obtain the target TA18 titanium alloy wire blank. The surface of the target TA18 titanium alloy wire blank is bright and the diameter is 1.2mm to 1.0mm.

[0046] Specifically, the chemical composition of the target TA18 titanium alloy wire blank meets the requirements of GB / T 3620.1.

[0047] S102. After coiling the target TA18 titanium alloy wire blank, perform temperature-controlled vacuum annealing. The vacuum environment avoids the participation of oxygen and hydrogen, and at the same time, performs vacuum dehydrogenation, thereby reducing the impurity content in the wire blank.

[0048] S103. Perform at least one cold drawing on the target TA18 titanium alloy wire blank, and perform online temperature-controlled atmosphere annealing after each cold drawing. After the last online temperature-controlled atmosphere annealing, obtain the final annealed wire blank with a diameter less than or equal to the target diameter, and the target diameter is less than or equal to 1 mm.

[0049] It should be noted that if a final annealed wire blank with a diameter less than or equal to the target diameter can be obtained by performing a single cold drawing and online temperature-controlled atmosphere annealing on the target TA18 titanium alloy wire blank, then the last cold drawing in this embodiment refers to the same thing as the first cold drawing.

[0050] Specifically, each cold drawing operation uses a drawing die group consisting of multiple drawing dies with different die hole diameters. The drawing dies are connected in series, and the die hole diameter of the drawing dies decreases by 7% to 9% from the wire inlet end to the wire outlet end, with the total deformation of the drawing die group being 25% to 45%. The decreasing die hole diameter of the drawing dies in the drawing die group ensures uniform deformation during drawing, increases and stabilizes work hardening, and results in superior overall performance of the drawn wire blank.

[0051] When the number of cold drawing operations is multiple, the diameter of the die hole of the wire drawing die at the wire feeding end in the wire drawing die group used in the later cold drawing is smaller than the diameter of the die hole of the wire drawing die at the wire exit end in the wire drawing die group used in the previous cold drawing, or the number of wire drawing dies in the wire drawing die group in the later cold drawing is greater than the number of wire drawing dies in the wire drawing die group in the previous cold drawing.

[0052] During cold drawing, the diameter of the drawn wire is the same as that of the last drawing die in the drawing die group. In this embodiment, whether it is adopted that the diameter of the die hole of the wire drawing die at the wire inlet end of the drawing die group used in the later cold drawing is smaller than the diameter of the die hole of the wire drawing die at the wire outlet end of the drawing die group used in the previous cold drawing, or that the number of drawing dies in the drawing die group in the later cold drawing is greater than the number of drawing dies in the drawing die group in the previous cold drawing, the essence is to control the wire blank obtained in the next cold drawing to be thinner than the wire blank obtained in the previous cold drawing. In the first method, the diameter of the die hole of the wire drawing die at the wire inlet end of the drawing die group in the next drawing is controlled to be smaller than the diameter of the die hole of the wire outlet end of the previous drawing. Since the diameter of the die hole of the wire drawing die from the wire inlet end to the wire outlet end in the drawing die group decreases by 7% to 9% according to the deformation amount, when the number of drawing dies in the drawing die group is the same, the diameter of the wire exiting in the later drawing is smaller than the diameter of the wire exiting in the previous drawing. In the second method, increasing the number of wire drawing dies in the wire drawing die group increases the total deformation of the wire drawing die group, resulting in a smaller final wire diameter.

[0053] It should be noted that the cold-drawn wire blank undergoes significant work hardening, resulting in high strength, high hardness, and high brittleness. Therefore, it is necessary to perform online temperature-controlled atmosphere annealing to soften the wire blank and facilitate cold drawing again.

[0054] It should also be noted that in this embodiment, the wire drawing die set is only used to cold draw one target TA18 titanium alloy wire blank. In actual use, multiple wire drawing die sets can be used to cold draw multiple target TA18 titanium alloy wire blanks.

[0055] S104. The final annealed wire blank is subjected to online pickling treatment to obtain TA18 titanium alloy ultrafine wire.

[0056] In one embodiment, the target TA18 titanium alloy wire blank is cold-drawn N times. After the first N-1 cold drawing, an intermediate drawn wire blank is obtained. The intermediate drawn wire blank is subjected to intermediate online temperature-controlled atmosphere annealing treatment to obtain an intermediate annealed wire blank. After the last cold drawing, a final drawn wire blank is obtained. The final drawn wire blank is subjected to final online temperature-controlled atmosphere annealing treatment to obtain a final annealed wire blank. N is greater than or equal to 2.

[0057] Specifically, the cold drawing process and the online temperature-controlled atmosphere annealing treatment can be carried out separately or simultaneously. When carried out simultaneously, the cold-drawn wire blank can be guided by guide wheels to an atmosphere tube furnace for online temperature-controlled atmosphere annealing. It should be noted that when carried out separately, the wire is taken up by a speed-adjustable take-up machine after cold drawing, and the take-up speed can be relatively fast. When carried out simultaneously, in order to ensure that the drawn wire blank stays in the atmosphere tube furnace cavity for a sufficient period of time during annealing to allow the material to soften completely and facilitate subsequent processing, the take-up speed should be slower.

[0058] In one embodiment, the online pickling process for the final annealed yarn blank involves sequentially placing the final annealed yarn blank into a pickling tank, a water tank, and a drying chamber.

[0059] In one embodiment, the coiled target TA18 titanium alloy wire blank is subjected to temperature-controlled vacuum annealing in a vacuum annealing furnace. The annealing temperature during temperature-controlled vacuum annealing is 700℃~850℃, the holding time is 1h~3h, and the vacuum degree is less than 2.0×10⁻⁶. -3 Pa.

[0060] In one embodiment, the annealing temperature during online temperature-controlled annealing is 600℃~800℃, the holding time is 20s~60s, the atmosphere is an inert gas, the atmosphere flow rate is 5L / min~10L / min, and the leakage rate is less than 2L / min.

[0061] During online temperature-controlled annealing, if the annealing temperature is too low or the annealing time is too short, the high work-hardening drawn wire blank will not stay in the furnace cavity for long enough to de-harden sufficiently. After annealing, the wire blank will still be relatively hard and will easily break when drawn again. If the annealing temperature is too high or the annealing time is too long, the drawn wire blank will stay in the furnace cavity for too long, causing the material grains to coarsen continuously and even overheating, ultimately leading to a decrease in the overall performance of the wire blank. Therefore, the temperature of the temperature-controlled annealing process needs to be controlled at 600℃~800℃ and the time at 20s~60s. The temperature and time of the temperature-controlled annealing will also change with the wire diameter.

[0062] Preferably, the online temperature-controlled annealing parameters for intermediate drawn wire blanks of different diameters are different, specifically:

[0063] When the diameter of the intermediate drawn wire blank is 1.0mm to 0.8mm, the intermediate online temperature-controlled atmosphere annealing temperature is 800℃ and the holding time is 60s;

[0064] When the diameter of the intermediate drawn wire blank is 0.6mm to 0.8mm, the intermediate online temperature-controlled atmosphere annealing temperature is 750℃ and the holding time is 50s;

[0065] When the diameter of the intermediate drawn wire blank is 0.4mm to 0.6mm, the intermediate online temperature-controlled annealing temperature is 700℃ and the holding time is 40s;

[0066] When the diameter of the intermediate drawn wire blank is 0.2mm to 0.4mm, the intermediate online temperature-controlled atmosphere annealing temperature is 650℃ and the holding time is 30s;

[0067] When the diameter of the intermediate drawn wire blank is 0mm to 0.2mm, the intermediate online temperature-controlled annealing temperature is 600℃ and the holding time is 20s.

[0068] The final online temperature-controlled annealing parameters differ for wire blanks of different diameters in the final drawn state. Specifically:

[0069] When the diameter of the final drawn wire blank is 1.0 mm to 0.8 mm, the online temperature-controlled annealing temperature is 750℃ and the holding time is 40 s;

[0070] When the diameter of the final drawn wire blank is 0.6mm to 0.8mm, the online temperature-controlled annealing temperature is 740℃ and the holding time is 40s;

[0071] When the diameter of the final drawn wire blank is 0.4mm to 0.6mm, the online temperature-controlled annealing temperature is 730℃ and the holding time is 30s;

[0072] When the diameter of the final drawn wire blank is 0.2mm to 0.4mm, the online temperature-controlled annealing temperature is 720℃ and the holding time is 30s;

[0073] When the diameter of the final drawn wire blank is 0mm to 0.2mm, the online temperature-controlled annealing temperature is 700℃ and the holding time is 20s.

[0074] In one embodiment, the pickling solution in the pickling tank, by volume, has a composition of HF:HNO3:H2O = 2-3:3-4:5-3. The final annealed wire blank is placed in the pickling tank for 10-50 seconds, and the temperature of the drying chamber is 50-100°C. During pickling, the surface of the wire blank is cleaned online with a strong acid solution prepared from hydrofluoric acid, nitric acid, and water to remove oil and micro-oxidation layers, making the surface of the wire blank bright. The remaining acid is then removed by washing the surface of the wire blank in a water tank, and finally the wire blank is dried in the drying chamber to obtain a bright and clean TA18 titanium alloy ultrafine wire. The dried TA18 titanium alloy ultrafine wire is then wound up by a speed-adjustable take-up machine.

[0075] Preferably, the final annealed yarn blanks of different diameters are placed in the pickling bath for different times, specifically:

[0076] When the diameter of the final annealed wire blank is 1.0 mm to 0.8 mm, the pickling time is 50 s.

[0077] When the diameter of the final annealed wire blank is 0.6mm to 0.8mm, the pickling time is 40s.

[0078] When the diameter of the final annealed wire blank is 0.4mm to 0.6mm, the pickling time is 30s.

[0079] When the diameter of the final annealed wire blank is 0.2mm to 0.4mm, the pickling time is 20s.

[0080] When the diameter of the final annealed wire blank is 0mm to 0.2mm, the pickling time is 10s.

[0081] To facilitate obtaining the relationship between the diameter of TA18 titanium alloy ultrafine wire and the online temperature-controlled atmosphere annealing and pickling processes, as shown in Table 1, this embodiment provides a table showing the relationship between the diameter of TA18 titanium alloy ultrafine wire and the online temperature-controlled atmosphere annealing and pickling processes.

[0082] Table 1 shows the relationship between the diameter of TA18 titanium alloy ultrafine wire and the online temperature-controlled atmosphere annealing and pickling processes.

[0083]

[0084] Because TA18 titanium alloy ultrafine wire, especially medical-grade TA18 titanium alloy ultrafine wire, has high requirements for alloy composition, mechanical properties, surface quality, dimensional tolerances, and straightness, and its processing technology is complex and difficult, the market currently mainly relies on imports for TA18 titanium alloy ultrafine wire, which is expensive. By using the relationship table between the diameter of TA18 titanium alloy ultrafine wire and the online temperature-controlled atmosphere annealing process and pickling process in this embodiment, combined with the preparation method of TA18 titanium alloy ultrafine wire, it is possible to prepare TA18 titanium alloy ultrafine wire that meets the requirements of GB / T 3620.1, eliminating the need to rely on imports and reducing the cost of obtaining TA18 titanium alloy ultrafine wire.

[0085] In one embodiment, a lubricant is sprayed onto the wire drawing die assembly during cold drawing. The lubricant is titanium alloy wire drawing oil, and the wire drawing die is a diamond wire drawing die.

[0086] In practical use, a nozzle can be installed above the drawing die to spray titanium alloy drawing oil, so as to reduce frictional heat during the drawing process and promote drawing stability.

[0087] In a specific embodiment 1, this embodiment involves a diameter of 0.52 ±0.005A method for preparing TA18 titanium alloy ultrafine wire with a diameter of 0.52 mm involves multiple cold drawing processes on the target TA18 titanium alloy wire blank. ±0.005 The preparation methods of TA18 titanium alloy ultrafine wires with a diameter of mm include:

[0088] Step 1: Select a TA18 titanium alloy wire blank that meets the requirements of GB / T 3620.1, has a wire diameter of 1.2 mm, and a bright surface as the target TA18 titanium alloy wire blank;

[0089] Step 2: Vacuum anneal the target TA18 titanium alloy wire blank from Step 1. The temperature is set to 800℃, the holding time is 2 hours, and the vacuum degree is 1.5×10⁻⁶. -3 Pa, after the heat preservation is completed, cool with the furnace, and remove from the furnace when the furnace temperature drops below 100℃;

[0090] Step 3: Perform multiple cold drawing operations on the wire blank obtained in Step 2. During the first cold drawing, the deformation of a single diamond die is controlled at approximately 9%. Four diamond dies are used as a group of drawing dies, and the deformation of the group is controlled at approximately 35%. Titanium alloy drawing oil is sprayed on the wire blank for cold drawing, thereby obtaining the intermediate drawn wire blank.

[0091] Step 4: After cold drawing one set of wire blanks, perform online temperature-controlled atmosphere annealing in an atmosphere tube furnace. The annealing temperature is set to 700℃~800℃. By adjusting the speed of the take-up machine, the wire is kept at the temperature in the furnace cavity for 40s~60s. The specific annealing temperature and holding time are as described in the above embodiment. During the annealing process, nitrogen is introduced into the furnace cavity at a flow rate of 10L / min. After annealing, an intermediate annealed wire blank is obtained.

[0092] Step 5: Add or remove one drawing die at the wire exit end of the drawing die set to cold draw the previously obtained intermediate annealed wire blank and return to step 4, until the drawn diameter is 0.52 mm. +0.005 The final drawn wire blank (mm) proceeds to step 6.

[0093] Step 6: Referring to the above examples of different final online temperature-controlled annealing parameters for drawn wire blanks of different diameters, the 0.52... +0.005 The final drawn wire blank is annealed in an online temperature-controlled atmosphere at 730℃ for 30 seconds to obtain the final annealed wire blank.

[0094] Step 7: The final annealed titanium alloy ultrafine wire is sequentially passed through an pickling tank, a water tank, and a drying chamber. The pickling solution composition is HF:HNO3:H2O = 2:3:5. The drying chamber temperature is 70℃. By adjusting the winding machine speed, the wire is pickled for 30 seconds, ultimately obtaining wires with low impurity content, excellent mechanical properties, and surface quality and dimensions meeting requirements, with a diameter of 0.52 mm. ±0.005mm of bright, clean TA18 titanium alloy ultrafine filament.

[0095] In a specific embodiment 2, this embodiment involves a diameter of 0.24 ±0.005 A method for preparing TA18 titanium alloy ultrafine wire with a diameter of 0.24 mm involves multiple cold drawing processes on the target TA18 titanium alloy wire blank. ±0.005 The preparation methods of TA18 titanium alloy ultrafine wires with a diameter of mm include:

[0096] Step 1: Select a TA18 titanium alloy wire blank that meets the requirements of GB / T 3620.1, has a wire diameter of 1.0 mm, and a bright surface as the target TA18 titanium alloy wire blank;

[0097] Step 2: Vacuum anneal the target TA18 titanium alloy wire blank from Step 1 at a temperature of 750℃ for 3 hours, with a vacuum degree of 1.2×10⁻⁶. -3 Pa, after the heat preservation is completed, cool with the furnace, and remove from the furnace when the furnace temperature drops below 100℃;

[0098] Step 3: Perform multiple cold drawing operations on the wire blank obtained in Step 2. During the first cold drawing, the deformation of a single diamond die is controlled at approximately 8%. Five diamond dies are used as a group of drawing dies, and the deformation of the group is controlled at approximately 40%. Titanium alloy drawing oil is sprayed on the wire blank for cold drawing, thereby obtaining the intermediate drawn wire blank.

[0099] Step 4: After cold drawing one set of wire blanks, perform online temperature-controlled atmosphere annealing in an atmosphere tube furnace. The annealing temperature is set to 650℃~800℃. By adjusting the speed of the take-up machine, the wire is kept at the temperature in the furnace cavity for 30s~60s. The specific annealing temperature and holding time are as described in the above embodiment. Nitrogen gas is introduced into the furnace cavity during the annealing process at a flow rate of 8L / min. After annealing, an intermediate annealed wire blank is obtained.

[0100] Step 5: Add or remove one drawing die at the wire exit end of the drawing die set to cold draw the previously obtained intermediate annealed wire blank and return to step 4, until the diameter is drawn to 0.24 mm. +0.005 The final drawn wire blank (mm) proceeds to step 6.

[0101] Step 6: Referring to the above examples of different final online temperature-controlled annealing parameters for drawn wire blanks of different diameters, the 0.24... +0.005 The final drawn wire blank is then subjected to online temperature-controlled annealing at 720℃ for 30 seconds to obtain the final annealed wire blank.

[0102] Step 7: The final annealed titanium alloy ultrafine wire is sequentially passed through an acid pickling tank, a water tank, and a drying chamber. The acid pickling solution composition is HF:HNO3:H2O = 3:3:4. The drying chamber temperature is 50℃. By adjusting the winding machine speed, the wire is acid-washed for 20 seconds, ultimately obtaining wires with low impurity content, excellent mechanical properties, and surface quality and dimensions meeting requirements, with a diameter of 0.24 mm. ±0.005 mm of bright, clean TA18 titanium alloy ultrafine filament.

[0103] like Figure 2 As shown, Figure 2 This is a schematic diagram of the microstructure of TA18 titanium alloy ultrafine wire in an embodiment of the present invention. The diameter in this embodiment is 0.24 mm. ±0.005 The microstructure of the bright, clean TA18 titanium alloy ultrafine filament (mm) is an equiaxed single-phase structure with uniform and fine grains, and an average grain size of 8.5. Therefore, the diameter of the filament prepared using the method in this embodiment is 0.24 mm. ±0.005 The bright, clean TA18 titanium alloy ultrafine wire has high strength, good toughness, and good plasticity.

[0104] In a specific embodiment 3, this embodiment involves a diameter of 0.11 ±0.005 A method for preparing TA18 titanium alloy ultrafine wire with a diameter of 0.11 mm involves multiple cold drawing processes on the target TA18 titanium alloy wire blank. ±0.005 The preparation methods of TA18 titanium alloy ultrafine wires with a diameter of mm include:

[0105] Step 1: Select a TA18 titanium alloy wire blank that meets the requirements of GB / T 3620.1, has a wire diameter of 1.0 mm, and a bright surface as the target TA18 titanium alloy wire blank;

[0106] Step 2: Vacuum anneal the target TA18 titanium alloy wire blank from Step 1. The temperature is set to 700℃, the holding time is 3 hours, and the vacuum degree is 1.0×10⁻⁶. -3 Pa, after the heat preservation is completed, cool with the furnace, and remove from the furnace when the furnace temperature drops below 100℃;

[0107] Step 3: Perform multiple cold drawing operations on the wire blank obtained in Step 2. During the first cold drawing, the deformation of a single diamond die is controlled at approximately 7%. Five diamond dies are used as a group of drawing dies, and the deformation of the group is controlled at approximately 30%. Titanium alloy drawing oil is sprayed on the wire blank for cold drawing, thereby obtaining the intermediate drawn wire blank.

[0108] Step 4: After cold drawing one set of wire blanks, perform online temperature-controlled atmosphere annealing in an atmosphere tube furnace. The annealing temperature is set to 600℃~800℃. By adjusting the speed of the take-up machine, the wire is kept at the temperature in the furnace cavity for 20s~60s. The specific annealing temperature and holding time are as described in the above embodiment. Nitrogen gas is introduced into the furnace cavity during the annealing process at a flow rate of 5L / min. After annealing, an intermediate annealed wire blank is obtained.

[0109] Step 5: Add or remove one drawing die at the wire exit end of the drawing die set to cold draw the previously obtained intermediate annealed wire blank and return to step 4, until the diameter is drawn to 0.11 mm. +0.005 The final drawn wire blank (mm) proceeds to step 6.

[0110] Step 6: Referring to the above examples of different final online temperature-controlled atmosphere annealing parameters for different diameter final drawn wire blanks, the 0.11... +0.005 The final drawn wire blank is subjected to online temperature-controlled annealing at 700℃ for 20 seconds to obtain the final annealed wire blank.

[0111] Step 7: The final annealed titanium alloy ultrafine wire is sequentially passed through an acid pickling tank, a water tank, and a drying chamber. The acid pickling solution composition is HF:HNO3:H2O = 3:3:4. The drying chamber temperature is 50℃. By adjusting the winding machine speed, the wire is acid-washed for 10 seconds, ultimately obtaining wires with low impurity content, excellent mechanical properties, and surface quality and dimensions meeting the requirements, with a diameter of 0.11 mm. ±0.005 mm of bright, clean TA18 titanium alloy ultrafine filament.

[0112] As shown in Table 2, the diameter obtained by applying specific embodiment 1 is 0.52. ± The chemical composition of the 0.005mm TA18 titanium alloy ultrafine wire meets the requirements of GB / T3620.1, especially the H and O content, which are far lower than the standard requirements and the impurity content of conventional wires. Its tensile strength Rm is 716MPa, yield strength Rp0.2 is 543MPa, and elongation after fracture A is 10.3%, significantly better than the mechanical properties of conventional wires, particularly its elongation, which is more than three times that of conventional wires. The diameter obtained in specific embodiment 2 is 0.24mm. ± The chemical composition of the 0.005mm TA18 titanium alloy ultrafine wire meets the requirements of GB / T3620.1. Its H and O content is significantly lower than the impurity content of conventional wires. The tensile strength Rm is 704MPa, the yield strength Rp0.2 is 520MPa, and the elongation after fracture A is 9.4%, significantly superior to the mechanical properties of conventional wires, especially the elongation, which is approximately three times that of conventional wires. The diameter obtained in specific embodiment 3 is 0.11mm. ±0.005The chemical composition of the TA18 titanium alloy ultrafine wire meets the requirements of GB / T3620.1. The H and O content is much lower than the impurity content of conventional wire. The tensile strength Rm is 715MPa, the yield strength Rp0.2 is 546MPa, and the elongation after fracture A is 10.5%, which is significantly better than the mechanical properties of conventional wire, especially the elongation is more than 3 times that of conventional wire.

[0113] Table 2 Comparison of Chemical Composition and Mechanical Properties of Specific Examples 1-3 and Conventional Titanium Alloy Wire

[0114]

[0115] As can be seen from the analysis in Table 2, the TA18 titanium alloy ultrafine wire prepared by the method of the present invention has the advantages of high strength, large elongation, and low impurity content.

[0116] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0117] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the appended claims.

Claims

1. A method for preparing TA18 titanium alloy ultrafine wire, characterized in that, include: Obtain a target TA18 titanium alloy wire blank, wherein the surface of the target TA18 titanium alloy wire blank is bright and the diameter is 1.2mm~1.0mm; The target TA18 titanium alloy wire blank is coiled and then subjected to temperature-controlled vacuum annealing. The target TA18 titanium alloy wire blank is subjected to at least one cold drawing, and after each cold drawing, it is subjected to online temperature-controlled atmosphere annealing. After the last online temperature-controlled atmosphere annealing, a final annealed wire blank with a diameter less than or equal to the target diameter is obtained, wherein the target diameter is less than or equal to 1 mm. In this process, a wire drawing die group consisting of multiple wire drawing dies with different die hole diameters is used for each cold drawing. The wire drawing dies in the wire drawing die group are connected in series. The die hole diameter of the wire drawing die in the wire drawing die group decreases by 7% to 9% from the wire inlet end to the wire outlet end. The total deformation of the wire drawing die group is 25% to 45%. When there are multiple cold drawing cycles, the die hole diameter of the wire drawing die at the wire inlet end of the wire drawing die group used in the later cold drawing is smaller than the die hole diameter of the wire outlet end of the wire drawing die group used in the previous cold drawing, or the number of wire drawing dies in the wire drawing die group in the later cold drawing is greater than the number of wire drawing dies in the wire drawing die group in the previous cold drawing. The final annealed wire blank is subjected to online pickling treatment to obtain TA18 titanium alloy ultrafine wire; The target TA18 titanium alloy wire blank is subjected to N cold drawing cycles. After the first N-1 cold drawing cycles, an intermediate drawn wire blank is obtained. The intermediate drawn wire blank is subjected to intermediate online temperature-controlled atmosphere annealing treatment to obtain an intermediate annealed wire blank. After the last cold drawing cycle, a final drawn wire blank is obtained. The final drawn wire blank is subjected to final online temperature-controlled atmosphere annealing treatment to obtain a final annealed wire blank. N is greater than or equal to 2. The annealing temperature during online temperature-controlled atmosphere annealing is 600℃~800℃, the holding time is 20s~60s, the atmosphere is an inert gas, the atmosphere flow rate is 5 L / min~10L / min, and the leakage rate is less than 2L / min. The online temperature-controlled annealing parameters for intermediate drawn wire blanks of different diameters are different, specifically: When the diameter of the intermediate drawn wire blank is 1.0mm~0.8mm, the intermediate online temperature-controlled annealing temperature is 800℃ and the holding time is 60s; When the diameter of the intermediate drawn wire blank is 0.6mm~0.8mm, the intermediate online temperature-controlled annealing temperature is 750℃ and the holding time is 50s; When the diameter of the intermediate drawn wire blank is 0.4mm~0.6mm, the intermediate online temperature-controlled atmosphere annealing temperature is 700℃ and the holding time is 40s; When the diameter of the intermediate drawn wire blank is 0.2mm~0.4mm, the intermediate online temperature-controlled annealing temperature is 650℃ and the holding time is 30s; When the diameter of the intermediate drawn wire blank is less than 0.2 mm, the intermediate online temperature-controlled annealing temperature is 600℃ and the holding time is 20 s.

2. The method for preparing TA18 titanium alloy ultrafine wire according to claim 1, characterized in that, The online pickling process for the final annealed yarn blank involves placing the final annealed yarn blank into a pickling tank, a water tank, and a drying chamber in sequence.

3. The method for preparing TA18 titanium alloy ultrafine wire according to claim 2, characterized in that, The coiled TA18 titanium alloy wire blank was subjected to temperature-controlled vacuum annealing in a vacuum annealing furnace. The annealing temperature was 700℃~850℃, the holding time was 1h~3h, and the vacuum degree was less than 2.0×10⁻⁶. -3 Pa.

4. The method for preparing TA18 titanium alloy ultrafine wire according to claim 2, characterized in that, The pickling solution composition of the pickling tank, by volume, is HF:HNO3:H2O = 2~3:3~4:5~3; The final annealed filament is placed in the pickling tank for 10 to 50 seconds, and the temperature of the drying chamber is 50°C to 100°C.

5. The method for preparing TA18 titanium alloy ultrafine wire according to claim 4, characterized in that, During cold drawing, a lubricant is sprayed onto the wire drawing die assembly. The lubricant is titanium alloy wire drawing oil, and the wire drawing die is a diamond wire drawing die.

6. The method for preparing TA18 titanium alloy ultrafine wire according to claim 1, characterized in that, The final online temperature-controlled annealing parameters differ for wire blanks of different diameters in the final drawn state. Specifically: When the diameter of the final drawn wire blank is 1.0mm~0.8mm, the online temperature-controlled atmosphere annealing temperature is 750℃ and the holding time is 40s; When the diameter of the final drawn wire blank is 0.6mm~0.8mm, the online temperature-controlled annealing temperature is 740℃ and the holding time is 40s; When the diameter of the final drawn wire blank is 0.4mm~0.6mm, the online temperature-controlled annealing temperature is 730℃ and the holding time is 30s; When the diameter of the final drawn wire blank is 0.2mm~0.4mm, the online temperature-controlled annealing temperature is 720℃ and the holding time is 30s; When the diameter of the final drawn wire blank is less than 0.2 mm, the online temperature-controlled annealing temperature is 700℃ and the holding time is 20 s.

7. The method for preparing TA18 titanium alloy ultrafine wire according to claim 4, characterized in that, The time for immersing the final annealed yarn blanks of different diameters in the pickling bath varies, specifically: When the diameter of the final annealed wire blank is 1.0 mm to 0.8 mm, the time for immersion in the pickling tank is 50 s; When the diameter of the final annealed wire blank is 0.6mm~0.8mm, the time for immersion in the pickling tank is 40s; When the diameter of the final annealed wire blank is 0.4mm~0.6mm, the time for immersion in the pickling tank is 30s; When the diameter of the final annealed wire blank is 0.2mm~0.4mm, the time for immersion in the pickling tank is 20s; When the diameter of the final annealed wire blank is less than 0.2 mm, the time for immersion in the pickling tank is 10 s.

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