CN115255825A - Preparation process of magnesium alloy wire with high axial-diameter ratio and fine-grain structure - Google Patents
Preparation process of magnesium alloy wire with high axial-diameter ratio and fine-grain structure Download PDFInfo
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Abstract
The invention discloses a preparation process of a magnesium alloy wire with a high axial-diameter ratio and a fine grain structure, and belongs to the technical field of metal material processing. It comprises the following steps: s1, preparing a magnesium alloy ingot; s2, hot rolling the magnesium alloy ingot to obtain a magnesium alloy plate; and S3, selecting a strip-shaped area with the width matched with the thickness on the magnesium alloy plate, carrying out static recrystallization annealing, cutting the strip-shaped area after plastic deformation treatment to obtain strip-shaped magnesium alloy, and drawing and processing the strip-shaped magnesium alloy into a magnesium alloy wire rod along the axial direction. The invention aims to make metal single crystals in magnesium alloy undergo hot rolling to achieve quasi-bidimensionalization, then carry out thermal deformation shearing to obtain strip-shaped magnesium alloy, draw the magnesium alloy into a wire rod, and fibrillate the metal single crystals in the wire rod direction, thereby greatly improving the axial-to-radial ratio of the metal single crystals in the metallographic phase and improving the mechanical properties of the magnesium alloy wire rod.
Description
Technical Field
The invention relates to processing of magnesium alloy wires, in particular to a preparation process of a magnesium alloy wire with a high axial-diameter ratio and a fine-grain structure.
Background
The magnesium alloy has the characteristics of low density, high specific strength, high specific rigidity, good damping and shock absorption properties, good electromagnetic shielding effect, easiness in recovery, good biological safety and the like, and has wide application prospects in the fields of automobile lightweight, biomedical fields and the like in recent years. However, conventional wrought magnesium alloys, although having relatively good deformability, have insufficient absolute strength, poor corrosion resistance, low high temperature strength and creep resistance, and the like, which limit their wide use. The new generation of magnesium alloy material mainly made of magnesium alloy wire gradually becomes the mainstream application product in the alloy field. The structural mechanical strength, plasticity and corrosion rate of the magnesium alloy wire are the key points for realizing the application.
Like conventional wire processing techniques, magnesium wire is generally obtained by a simple drawing process, and the microstructure, mechanical properties and corrosion resistance of the magnesium alloy are not improved in the whole wire processing process. The improvement of the mechanical property of the magnesium alloy wire only depends on the layout design of the alloy wire, but not from the improvement of indexes such as the structural strength of the magnesium alloy wire. In addition, in the process of preparing the magnesium alloy wire by the conventional hot drawing technology, recovery and recrystallization are easy to occur, so that the grains of the wire continue to grow, the comprehensive mechanical property is reduced, continuous drawing is not facilitated, in addition, the work hardening effect of the wire is weakened due to high temperature, the strength is reduced, and wire breakage frequently occurs in the wire drawing at a die outlet.
The prior art also adopts a room temperature multi-pass cold drawing process, the single-pass deformation is 7-12%, the accumulated deformation is 50-60%, the annealing temperature is 400-420 ℃, the annealing time is 1-3 min, and the room temperature cold drawing and the recrystallization annealing are matched to smoothly process the fine grain magnesium alloy wire rod with the diameter of 2-3 mm to the diameter of 0.22mm. The process method is a mature conventional method for producing the deformed magnesium alloy wire, but the drawing process requires that the raw material grain size is fine, and the grain size is required to be less than 20 mu m when the hot extrusion wire is selected as the raw material, so that the variety of the magnesium alloy is greatly limited, and only a few kinds of magnesium alloys with small crystal phase structures can be processed by the process.
Therefore, the processing method capable of effectively improving the mechanical parameters of the magnesium alloy wire and the component proportion of the magnesium alloy are problems which need to be solved in the field of processing of the magnesium alloy wire at present.
Disclosure of Invention
The invention provides a preparation process of a magnesium alloy wire with a high-axial-diameter-ratio crystal phase structure, and aims to enable metal single crystals in magnesium alloy to be subjected to hot rolling quasi-bidimensionalization, then to be subjected to thermal deformation shearing to obtain strip-shaped magnesium alloy, to be drawn into a wire, and to fibrillate the metal single crystals in the wire direction, so that the axial-diameter ratio of the metal single crystals in a metallographic phase is greatly improved, the mechanical property of the magnesium alloy wire is improved, and the problems that the conventional magnesium alloy wire processing method has more limited factors, low processing efficiency and the strength of the wire is reduced due to the change of the crystal phase of the processed magnesium alloy wire are solved.
The invention is realized by adopting the following technical scheme:
a preparation process of a magnesium alloy wire rod with a high axial-to-radial ratio and a fine crystal structure comprises the following steps:
s1, preparing a magnesium alloy ingot;
s2, hot rolling the magnesium alloy ingot to obtain a magnesium alloy plate, and hot rolling to ensure that the thickness of the magnesium alloy plate is 2-5mm;
and S3, selecting a strip-shaped area with the width matched with the thickness on the magnesium alloy plate for static recrystallization annealing, cutting the strip-shaped area after plastic deformation treatment to obtain strip-shaped magnesium alloy, and drawing and processing the strip-shaped magnesium alloy into a magnesium alloy wire rod along the axial direction.
Preferably, in S1, the magnesium alloy ingot is prepared from magnesium alloy raw materials according to a mixture ratio, wherein the magnesium alloy raw materials comprise, by mass, 0.2% -2.5% of Zn, 0.1% -4.1% of Y and the balance of Mg;
after the magnesium alloy ingot is prepared, surface treatment is carried out, preferably, the surface treatment comprises mechanical polishing, oil removal by alkali solution, activation by acid solution, water washing and drying.
Preferably, before S2, homogenizing heat treatment is carried out, wherein the temperature of homogenizing heat treatment is 500-600 ℃, the temperature is increased to the heat treatment temperature at 0.9-1.1 ℃/min, the heat is preserved for 10-13 h, and then the cooling is carried out in water at 50-70 ℃.
Preferably, in S2, after the magnesium alloy ingot is hot-rolled to form a magnesium alloy sheet, the magnesium alloy sheet is hot-rolled for multiple times until the thickness of the magnesium alloy sheet is 2 to 5mm, and the thickness is 20 to 25% of the original thickness each time.
Preferably, the S2 includes the steps of:
s2.1, processing a magnesium alloy ingot into a magnesium alloy plate with the thickness of 50-70mm, wherein the tapping temperature of the metal is 400-450 ℃ during hot rolling, and the heating time is 3-4h;
s2.2, processing the magnesium alloy plate into a magnesium alloy plate with the thickness of 10-20mm, wherein the tapping temperature of the metal is 350-400 ℃ during hot rolling, and the heating time is 3-4h;
s2.3, processing the magnesium alloy plate into a magnesium alloy plate with the thickness of 2-5mm, wherein the tapping temperature of the metal is 250-300 ℃ during hot rolling, and the heating time is 2-3h.
Preferably, in S3, the annealing temperature is 200-250 ℃ and the time is 10min when the strip-shaped region with the width matched with the thickness is subjected to static crystallization reprocessing; further, the annealing temperature when the static crystallization reprocessing is carried out is 250 ℃;
the plastic deformation treatment is a thermoplastic deformation treatment processed by a static annealing process with the annealing temperature of 245-255 ℃ for 5-10 min;
the ratio of the width to the thickness of the strip-shaped area of the strip-shaped magnesium alloy plate is 0.9-1.1, and further the width and the thickness of the strip-shaped magnesium alloy plate are equal to each other;
in the process of drawing and processing the magnesium alloy wire rod along the axial direction, the single-pass deformation is 20-25%, and the crystallization annealing heat treatment with the crystallization annealing temperature of 400-450 ℃ and the time of 5-10min is adopted; furthermore, the crystallization annealing temperature in the drawing process is 400 ℃, the time is 10min, the single-pass deformation is 20%, and the drawing speed is 0.05m/s;
the diameter of the magnesium alloy wire rod is 0.3-1mm.
The invention has the beneficial effects that:
1. hot rolling the magnesium alloy ingot for multiple times to obtain a magnesium alloy plate with the thickness of 2-5mm, so that metal single crystals in the magnesium alloy extend towards two dimensions on a hot rolling plane, and the length of the metal single crystals in the Z-axis direction vertical to the hot rolling plane is reduced;
2. and selecting a strip-shaped area in the plane direction of the magnesium alloy plate for plastic deformation treatment, cutting and taking down the strip-shaped area subjected to plastic deformation treatment to obtain strip-shaped magnesium alloy, and drawing and processing the strip-shaped magnesium alloy into a magnesium alloy wire rod along the axial direction. The method comprises the following steps of cutting a metal single crystal which is hot rolled into a quasi-two-dimensional plane, recrystallizing the single crystal through plastic deformation treatment to obtain a metal single crystal with a smaller volume, further reducing the size of the metal single crystal in the strip-shaped magnesium alloy, wherein the plastic deformation area is a static recrystallization strip area with refined grains. Then adopting a method of drawing along the axial direction to further elongate the metal single crystal with small volume along the axial direction of the strip-shaped magnesium alloy to obtain a magnesium alloy wire with a high axial-to-radial ratio crystal phase structure;
3. according to the gold phase diagram, the crystal phase diagram shows that all crystal grains are arranged in a crossed manner in the magnesium alloy wire rod after being stretched, the crystal grain diameter is greatly reduced, the original spherical crystal grains are almost invisible, and the crystal grains exist in a strip-shaped mixed winding state single crystal form with a large axial ratio. Finally, the tensile property of the magnesium alloy wire is greatly improved, the tensile strength can reach 420MPa, and the elongation rate reaches more than 16%.
Drawings
FIG. 1 is a graph showing a distribution of a grain size of a magnesium alloy sheet material according to example 1;
FIG. 2 is a graph showing a distribution of grain sizes of a magnesium alloy sheet according to example 2;
FIG. 3 is a diagram of a gold phase of an undrawn magnesium alloy wire according to the present invention;
fig. 4 is a gold phase diagram of a drawn magnesium alloy wire rod according to the present invention.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purpose and the efficacy of the invention easily understood, the invention is further described with reference to the following embodiments.
Example 1
In the embodiment, the Mg-2Zn-0.2Y alloy comprises the following components in percentage by weight: 2% Zn,0.2% Y, the balance Mg.
The preparation process of the magnesium alloy wire rod with the high axial-diameter ratio and the fine crystal structure comprises the following steps:
s1, preheating a pre-smelted Mg-Zn alloy ingot to 300 ℃ according to weight percentage, putting the pre-smelted Mg-Zn alloy ingot into a crucible resistance furnace, heating to 700 ℃, keeping the temperature for 10min to completely melt, quickly adding weighed Mg-Y intermediate alloy, keeping the temperature for 15min, stirring for 1min, pouring the mixture into a metal mold, casting the mixture into an ingot, removing surface defects and impurities, and smelting the alloy in CO2And SF6Carrying out surface treatment in the protective atmosphere of mixed gas, sequentially carrying out mechanical polishing, alkali solution oil removal, acid solution activation, washing and drying in a drying box at low temperature to obtain magnesium alloy ingots; heating the magnesium alloy ingot to 500 ℃ at a speed of 0.9-1.1 ℃/min for homogenization heat treatment for 12h; then cooling in water at 50-70 ℃.
S2, hot rolling to form a magnesium alloy plate:
s2.1, hot rolling at the tapping temperature of 400 ℃ for 3.5 hours to form a magnesium alloy plate with the thickness of 50mm, the width of 400mm and the length of 250mm;
s2.2, then hot rolling at the tapping temperature of 350 ℃ for 3 hours to form a magnesium alloy plate with the thickness of 10mm, the width of 400mm and the length of 250mm;
s2.3, then hot rolling at the tapping temperature of 250 ℃ for 3h, and processing into a magnesium alloy plate with the thickness of 3mm, the width of 400mm and the length of 250 mm.
And S3, selecting a strip-shaped area with the width of 3mm on the magnesium alloy plate, processing the magnesium alloy plate through a static recrystallization annealing process, wherein the annealing temperature is 200 ℃, the annealing time is 10min, and a temperature measuring device (comprising a thermocouple and the like) is used for ensuring the annealing temperature to be stable, so that a static recrystallization strip area with refined grains is processed. Fig. 1 is a distribution diagram of the grain size of the region, and the grains are equiaxed grains. Cutting the area, machining the area into a bar with the diameter phi of 2mm, drawing the bar, and finally forming the wire with the diameter of 0.3mm by matching annealing heat treatment in the drawing process, wherein the temperature is 400 ℃, the time is 10min, the single-pass deformation is 20%, and the drawing speed is 0.05 m/s. The metallographic images before and after stretching are shown in FIGS. 3 and 4, respectively.
Tensile Properties (GB/T228-2002): the tensile strength is 400MPa, and the elongation is 15%.
Example 2
This example is the same as example 1 with the following main differences:
adopting Mg-0.2Zn-4.1Y alloy, and the components by weight percentage are as follows: 0.2% Zn,4.1% Y, the balance Mg.
In S2, the homogenization treatment temperature of the ingot is 550 ℃;
in S2.1, the tapping temperature is 450 ℃, the heating time is 4h, and the specification of the magnesium alloy plate is 45mm in thickness, 400mm in width and 250mm in length;
in S2.2, the tapping temperature is 400 ℃, the heating time is 3h, and the specification of the magnesium alloy plate is 10mm in thickness, 400mm in width and 250mm in length;
in S2.3, the tapping temperature is 300 ℃, the heating time is 3h, and the specification of the magnesium alloy plate is 2mm in thickness, 400mm in width and 250mm in length;
in S3, the width of the strip region was 2mm, the annealing temperature was 250 ℃ and the annealing time was 10min, and a grain size distribution diagram of the grain refined static recrystallization strip region is shown in FIG. 2.
Tensile Properties (GB/T228-2002): the tensile strength is 420MPa, and the elongation is 16%.
In S2 of example 1-2, a magnesium alloy ingot was hot-rolled a plurality of times to obtain a magnesium alloy sheet having a thickness of 2 to 5mm, in order to two-dimensionally stretch a metal single crystal inside the magnesium alloy on a hot-rolled plane and reduce the length of the metal single crystal in the Z-axis direction perpendicular to the hot-rolled plane.
In S3 of example 1-2, a strip-shaped region 2 to 5mm wide is selected in the plane direction of the magnesium alloy sheet and subjected to plastic deformation, the strip-shaped region subjected to plastic deformation is cut and removed to obtain a strip-shaped magnesium alloy, and the magnesium alloy sheet is axially drawn and processed into a magnesium alloy wire rod, so that the step is to cut a metal single crystal hot-rolled into a quasi-two-dimensional plane and recrystallize the single crystal through plastic deformation to obtain a metal single crystal with a smaller volume, further reduce the size of the metal single crystal in the strip-shaped magnesium alloy, and the plastic deformation region is a static recrystallization strip region with refined grains, and then further elongate the metal single crystal with a small volume along the axial direction of the strip-shaped magnesium alloy by an axial drawing method to obtain a magnesium alloy wire rod with a high axial-diameter ratio crystal phase structure.
As shown in fig. 3, the crystal phase diagram shows that the boundaries of each phase are clear, and the crystal grain size is more in the size range of 20 microns;
as shown in fig. 4, in the magnesium alloy wire rod after stretching, a crystal phase diagram shows that the crystal grains are arranged in a crossed manner, the crystal grain size is greatly reduced, the original spherical crystal grains are almost invisible, and the crystal grains exist in a single crystal form with a strip winding state and a large axial ratio, so that the stretching performance of the magnesium alloy wire rod is greatly improved, the tensile strength can reach 420MPa, and the elongation rate reaches more than 16%.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation process of a magnesium alloy wire with a high axial-diameter ratio and a fine crystal structure is characterized by comprising the following steps of: the method comprises the following steps:
s1, preparing a magnesium alloy ingot;
s2, hot rolling the magnesium alloy ingot to obtain a magnesium alloy plate; hot rolling to make the thickness of the steel plate 2-5mm;
and S3, selecting a strip-shaped area with the width matched with the thickness on the magnesium alloy plate, carrying out static recrystallization annealing, cutting the strip-shaped area after plastic deformation treatment to obtain strip-shaped magnesium alloy, and drawing and processing the strip-shaped magnesium alloy into a magnesium alloy wire rod along the axial direction.
2. The preparation process of the magnesium alloy wire rod with the high axial-to-diameter ratio and the fine crystal structure according to claim 1, characterized in that: in S1, the magnesium alloy ingot is prepared from magnesium alloy raw materials according to a mixture ratio, wherein the magnesium alloy raw materials comprise, by mass, 0.2% -2.5% of Zn, 0.1% -4.1% of Y and the balance of Mg.
3. The process for preparing the magnesium alloy wire rod with the fine crystal structure and the high axial diameter ratio according to claim 1, wherein the process comprises the following steps: before S2, homogenizing heat treatment is carried out, the temperature of homogenizing heat treatment is 500-600 ℃, the temperature is raised to the heat treatment temperature at 0.9-1.1 ℃/min, heat preservation is carried out for 10-13 h, and then cooling is carried out in water at 50-70 ℃.
4. The process for preparing the magnesium alloy wire rod with the fine crystal structure and the high axial diameter ratio according to claim 1, wherein the process comprises the following steps: in S2, after the magnesium alloy ingot is hot-rolled to form a magnesium alloy plate, hot-rolling is carried out for multiple times until the thickness of the magnesium alloy plate is 2-5mm, and the thickness is 20% -25% of the original thickness each time.
5. The preparation process of the magnesium alloy wire rod with the high axial-to-diameter ratio and the fine crystal structure according to claim 4, wherein the preparation process comprises the following steps: the S2 comprises the following steps:
s2.1, processing a magnesium alloy ingot into a magnesium alloy plate with the thickness of 50-70mm, wherein the tapping temperature of the metal is 400-450 ℃ during hot rolling, and the heating time is 3-4h;
s2.2, processing the magnesium alloy plate into a magnesium alloy plate with the thickness of 10-20mm, wherein the tapping temperature of the metal is 350-400 ℃ during hot rolling, and the heating time is 3-4h;
s2.3, processing the magnesium alloy plate into a magnesium alloy plate with the thickness of 2-5mm, wherein the tapping temperature of the metal is 250-300 ℃ during hot rolling, and the heating time is 2-3h.
6. The preparation process of the magnesium alloy wire rod with the high axial-to-diameter ratio and the fine crystal structure according to claim 1, characterized in that: in S3, the annealing temperature is 250 ℃ and the time is 10min when the strip-shaped area with the width matched with the thickness is subjected to static crystallization reprocessing;
the plastic deformation treatment is a thermoplastic deformation treatment which is processed by a static annealing process with the annealing temperature of 245-255 ℃ and the time of 5-10 min;
the ratio of the width to the thickness of the strip-shaped area of the strip-shaped magnesium alloy plate is 0.9-1.1;
in the process of drawing and processing the magnesium alloy wire rod along the axial direction, the single-pass deformation is 20-25%, and the crystallization annealing heat treatment with the crystallization annealing temperature of 400-450 ℃, the time of 5-10min and the drawing speed of 0.05-0.1m/S is adopted;
the diameter of the magnesium alloy wire rod is 0.3-1mm.
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