Disclosure of Invention
The invention aims to provide a high-strength TC4 titanium alloy wire and a preparation method thereof, which are used for solving the technical problems that the strength of the traditional drawing process of TC4 titanium alloy in the prior art is difficult to meet the requirement of high-strength performance and the processing efficiency is low.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides a preparation method of a high-strength TC4 titanium alloy wire, which comprises the following steps:
carrying out multi-pass roller die drawing on the TC4 titanium alloy hot-rolled wire blank in a high-temperature two-phase region, and then carrying out annealing treatment to obtain a wire;
carrying out multi-pass roller die drawing on the annealed wire again, and gradually reducing the temperature in the drawing process;
And carrying out multi-pass fixed die drawing on the wire rod subjected to roller die drawing in a low-temperature two-phase region, keeping the temperature unchanged in the drawing process, and finally carrying out secondary annealing treatment to obtain the high-strength TC4 titanium alloy wire rod.
Further, in the step of carrying out multi-pass roller die drawing on the TC4 titanium alloy hot-rolled wire blank in a high-temperature two-phase region and then carrying out annealing treatment to obtain a wire, before carrying out multi-pass roller die drawing, carrying out stress relief annealing treatment on the TC4 titanium alloy hot-rolled wire blank, wherein the temperature of the stress relief annealing treatment is 700-850 ℃ and the heat preservation time is 30-90 min.
Further, in the step of carrying out multi-pass roller die drawing on the TC4 titanium alloy hot-rolled wire blank in a high-temperature two-phase region and then carrying out annealing treatment to obtain the wire, the total drawing deformation of the multi-pass roller die drawing is 30% -50%, the deformation of each pass is not less than 5% -10%, and the pass drawing temperature is 700 ℃ -850 ℃.
Further, in the step of carrying out multi-pass roller die drawing on the TC4 titanium alloy hot-rolled wire blank in a high-temperature two-phase region and then carrying out annealing treatment to obtain the wire, the diameter of the TC4 titanium alloy hot-rolled wire blank is 8 mm-14 mm, and the drawing speed of multi-pass roller die drawing is 2.0 m/min-8.0 m/min.
Further, in the step of carrying out multi-pass roller die drawing on the TC4 titanium alloy hot-rolled wire blank in a high-temperature two-phase region and then carrying out annealing treatment to obtain the wire, the annealing treatment temperature is 700-850 ℃, and the heat preservation time is 30-90 min.
Further, the annealed wire is subjected to multi-pass roller die drawing again, and in the step of gradually reducing the temperature in the drawing process, the total drawing deformation of the multi-pass roller die drawing is 20% -50%, the deformation of each pass is not less than 8% -15%, the pass drawing temperature is 700 ℃ -850 ℃, and the drawing speed is 2.0 m/min-8.0 m/min.
Further, in the step of carrying out multi-pass fixed die drawing on the wire rod subjected to roller die drawing in a low-temperature two-phase region, wherein the temperature is unchanged in the drawing process, and finally carrying out secondary annealing treatment to obtain the high-strength TC4 titanium alloy wire rod, the total deformation of the multi-pass fixed die drawing is 20% -50%, the fixed die drawing temperature is 600 ℃ -700 ℃, the deformation of each pass is not less than 10% -15%, and the drawing speed is 2.0 m/min-8.0 m/min.
Further, the wire rod after the roller die drawing is subjected to multi-pass fixed die drawing in a low-temperature two-phase region, the temperature is unchanged in the drawing process, and finally, in the step of obtaining the high-strength TC4 titanium alloy wire rod through secondary annealing treatment, the temperature of the secondary annealing treatment is 650-800 ℃, and the heat preservation time is 30-90 min.
And further, finally, carrying out secondary annealing treatment to obtain the high-strength TC4 titanium alloy wire with the diameter of 2 mm-5 mm.
In a second aspect, the invention provides a high-strength TC4 titanium alloy wire, which is prepared by the preparation method of the high-strength TC4 titanium alloy wire.
Compared with the prior art, the invention has the following beneficial effects:
The invention discloses a high-strength TC4 titanium alloy wire and a preparation method thereof, wherein the TC4 high-strength titanium alloy wire prepared by a roller die and fixed die drawing method has tensile strength of more than 1180Mpa, yield strength of more than 1000Mpa, elongation after fracture of more than 5 percent and reduction of area of more than 40 percent in a room-temperature drawing state, the tensile strength of more than 1100MPa at room temperature, yield strength of more than 980MPa, elongation after fracture of more than 15 percent and reduction of area of more than 40 percent after fracture of the drawn wire after annealing heat treatment, and the strength of the drawn wire is more excellent than that of the TC4 alloy wire prepared by drawing only the fixed die in the prior art. In addition, the TC4 alloy wire prepared by the roller die and fixed die drawing method has good surface quality, uniform and fine microstructure and room temperature tensile property far exceeding the performance requirements of related standards such as GB/T13810-2017 on medical appliance materials.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of," and "consisting essentially of," such as "a includes a" encompassing "a and other" and "a includes only a".
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The invention is described in further detail below with reference to the attached drawing figures:
referring to fig. 3, the embodiment of the invention discloses a preparation method of a high-strength TC4 titanium alloy wire, which comprises the following steps:
Step 1, carrying out multi-pass roller die drawing on a TC4 titanium alloy hot-rolled wire blank in a high-temperature two-phase region, and then carrying out annealing treatment to obtain a wire;
In the step, the diameter of a hot rolled wire blank is d 8-d 14mm, the wire is subjected to stress relief annealing treatment at 700-850 ℃ for 30-90 min before drawing, the total drawing deformation of multi-pass roller die drawing is 30-50%, and the pass drawing temperature is 700-850 ℃;
And after the drawing, annealing treatment is needed, wherein the specific annealing treatment process is the same as stress relief annealing treatment, the temperature is 700-850 ℃, and the heat preservation time is 30-90 min.
Step 2, carrying out multi-pass roller die drawing on the annealed wire again, wherein the temperature is gradually reduced in the drawing process;
In the step, the total deformation of multi-pass roller die drawing is 20% -50%, and the pass drawing temperature is 700 ℃ -850 ℃.
And 3, carrying out multi-pass fixed die drawing on the wire drawn by the roller die in a low-temperature two-phase region, keeping the temperature unchanged in the drawing process, and finally carrying out secondary annealing treatment to obtain the high-strength TC4 titanium alloy wire.
In the step, the total deformation of the multi-pass fixed die drawing is 20% -50%, and the fixed die drawing temperature is 600 ℃ -700 ℃. The secondary annealing process is specifically carried out at 650-800 ℃ and the temperature is kept for 30-90 min. Finally obtaining the high-strength TC4 titanium alloy wire with the diameter of d2 mm-d 5 mm.
In one possible implementation mode of the invention, the deformation of each pass in the step 1 is not less than 5% -10%, the deformation of each pass in the step 2 is not less than 8% -15%, the deformation of each pass in the step 3 is not less than 10% -15%, and the drawing and wire drawing speeds of the multi-pass roller die and the fixed die in the steps 1,2 and 3 are all 2.0 m/min-8.0 m/min.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1:
The embodiment adopts a preparation method of high-strength TC4 titanium alloy wire roller die and fixed die, and uses hot rolled strips with the specification of phi 11mm as blanks to prepare the phi 5mm high-strength TC4 titanium alloy wire.
Step 1, carrying out stress relief annealing on a hot rolled blank with the diameter phi 11mm at 750 ℃ for 60min, and then carrying out roller die drawing at a heating temperature of 850 ℃, wherein the blank with the diameter phi 11mm is subjected to 4-pass drawing and reducing to phi 8.3mm, the deformation of each pass is not less than 7%, the drawing speed is 3.0m/min, and the total deformation is 43%, and then carrying out annealing treatment on a wire at 750 ℃ for 60 min;
Step 2, carrying out roller die drawing and reducing on the silk material with the diameter of phi 8.3mm after the heat treatment in the step 1 to the diameter of phi 6.3mm, wherein the drawing temperature is reduced from 700 ℃ to 650 ℃ in a die-by-die mode, the drawing speed is 3.0m/min, the deformation of each pass is not less than 10%, and the total deformation is 42%;
and 3, drawing the wire with the diameter phi of 6.3mm after the drawing of the roller die in the step 2 to phi of 5.0mm through a fixed die, wherein the drawing temperature is 650 ℃, the drawing speed is 2m/min, the deformation of each pass is not less than 13%, the total deformation is 37%, and finally, carrying out annealing heat treatment at 650 ℃ for 1 hour to obtain the high-strength TC4 titanium alloy wire.
The properties of the phi 5.0mm high-strength titanium alloy wire prepared by the above steps are shown in the following table 1:
TABLE 1
As shown in Table 1, the two-phase high-strength TC4 titanium alloy wires prepared by the method have good annealed state performance consistency, the data deviation of tensile strength and yield strength is not more than 10MPa, the difference of elongation and area shrinkage is not more than 0.5%, the detection data are far higher than the requirements of GB/T13810-2017 on the TC4 wire performance, the high strength is maintained, meanwhile, the high-strength TC4 titanium alloy wires have good toughness, and the comprehensive performance of the wires is better.
In addition, according to the graph shown in FIG. 1, the high-strength TC4 titanium alloy wire prepared by the method has uniform annealed structure, fully refined crystal grains and the grain size rating difference of different parts is less than or equal to 1. According to the high-strength TC4 titanium alloy wire prepared by the embodiment, the two-phase phi 5.0mm titanium alloy wire with super-standard performance and good consistent structure can be prepared by adopting the method.
Example 2:
The embodiment adopts a preparation method of high-strength TC4 titanium alloy wire roll die and fixed die, and uses hot rolled strips with the specification of phi 9.0mm as blanks to prepare the high-strength TC4 titanium alloy wire with the specification of phi 4.0 mm.
Step 1, carrying out stress relief annealing on a hot rolled blank with the diameter phi 9.0mm at 800 ℃ for 50min, and then carrying out roller die drawing at a drawing speed of 3.5m/min at a heating temperature of 800 ℃, wherein the deformation of each pass is not less than 6% and the total deformation is 36% from the blank with the diameter phi 9.0mm to the diameter phi 7.2mm through roller die drawing, and then carrying out annealing treatment of 800 ℃ and heat preservation for 50min on a wire;
Step2, drawing the wire rod roller with the diameter of 7.2mm after the heat treatment in the step 1 to the diameter of 5.4mm, and cooling the drawing temperature from 800 ℃ to 740 ℃ in a mode-by-mode manner, wherein the drawing speed is 4m/min, the deformation of each pass is not less than 9%, and the total deformation is 43%;
And 3, carrying out fixed die drawing on the wire with the diameter phi 5.4mm after the die drawing of the roller in the step 2 at the heating temperature of 700 ℃ at a drawing speed of 3m/min, wherein the deformation of each pass is not less than 12%, the total deformation is 45%, and the wire with the diameter phi 5.7mm is drawn to the diameter phi 4.0mm through the fixed die. Finally, carrying out 680 ℃ and heat treatment of annealing for 60min to obtain the high-strength TC4 titanium alloy wire.
The properties of the phi 4.0mm high-strength titanium alloy wire prepared by the steps are shown in table 2:
TABLE 2
The high-strength titanium alloy wire prepared by the embodiment has high annealed performance strength and good toughness. Meanwhile, the consistency of mechanical properties is good. And observing microstructure of the high-strength titanium alloy wire with the diameter of 4.0mm, wherein the microstructure is uniform, crystal grains are refined, and the grain size grading difference of different parts is less than or equal to 1, as shown in figure 2.
Example 3:
the embodiment adopts a preparation method of high-strength TC4 titanium alloy wire roll die and fixed die, and uses hot rolled strips with the specification of phi 13.0mm as blanks to prepare the high-strength TC4 titanium alloy wire with the specification of phi 5.2 mm.
Step 1, carrying out stress relief annealing on a hot rolled blank with the diameter phi of 13.0mm at 850 ℃ for 80min, and then carrying out roller die drawing at a drawing speed of 7m/min at a heating temperature of 800 ℃, wherein the deformation of each pass is not less than 9% and the total deformation is 46% from the blank with the diameter phi of 13.0mm to the diameter phi of 9.5mm through roller die drawing, and then carrying out annealing treatment on a wire at 850 ℃ for 80 min;
Step 2, drawing the wire rod roller with the diameter of 9.5mm after the heat treatment in the step 1 to the diameter of 6.9mm, wherein the drawing temperature is gradually reduced to 750 ℃ from 850 ℃, the drawing speed is 7m/min, the deformation of each pass is not less than 13%, and the total deformation is 47%;
and 3, carrying out fixed die drawing on the wire with the diameter phi 6.9mm after the die drawing of the roller in the step 2 at the heating temperature of 600 ℃ at the drawing speed of 7m/min, wherein the deformation of each pass is not less than 10%, the total deformation is 43%, and the wire with the diameter phi 6.9mm is drawn to the diameter phi 5.2mm through the fixed die. Finally, carrying out annealing heat treatment at 750 ℃ for 50min to obtain the high-strength TC4 titanium alloy wire.
Example 4:
The embodiment adopts a preparation method of high-strength TC4 titanium alloy wire roll die and fixed die, and uses hot rolled strips with the specification of phi 10.0mm as blanks to prepare the phi 4.5mm high-strength TC4 titanium alloy wire.
Step 1, carrying out stress relief annealing on a hot rolled blank with the diameter phi of 10.0mm at the temperature of 700 ℃ for 40min, and then carrying out roller die drawing at the drawing speed of 6m/min at the heating temperature of 750 ℃, reducing the diameter from the blank with the diameter phi of 10.0mm to the diameter phi of 7.8mm through roller die drawing, wherein the deformation of each pass is not less than 8 percent and the total deformation is 39 percent, and carrying out annealing treatment on a wire at the temperature of 700 ℃ for 40 min;
step 2, drawing the wire rod roller with the diameter of 7.8mm after the heat treatment in the step 1 to the diameter of 6.2mm, and cooling the drawing temperature from 750 ℃ to 680 ℃ in a die-by-die mode, wherein the drawing speed is 5m/min, the deformation of each pass is not less than 12%, and the total deformation is 37%;
And 3, carrying out fixed die drawing on the wire material with the diameter phi 6.2mm after the die drawing of the roller in the step 2 at the heating temperature of 650 ℃ at the drawing speed of 6m/min, wherein the deformation of each pass is not less than 11%, the total deformation is 47%, and the wire material with the diameter phi 6.2mm is drawn to the diameter phi 4.5mm through the fixed die. Finally, carrying out annealing heat treatment at 700 ℃ for 80min to obtain the high-strength TC4 titanium alloy wire.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.