CN114318187B - Biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire and preparation method thereof - Google Patents
Biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of biomedical materials, and discloses a biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire and a preparation method thereof, wherein the method comprises the following steps: carrying out hot extrusion treatment on the high-purity Mg-Zn-Mn magnesium alloy ingot to obtain an extruded bar; carrying out recrystallization annealing treatment on the extrusion bar to obtain a recrystallization annealing bar; and sequentially carrying out primary rotary swaging deformation treatment and secondary rotary swaging deformation treatment on the recrystallized annealed bar to obtain the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire. The biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire material is obtained by utilizing the advantage of excellent low degradation rate of the high-purity magnesium alloy through multi-step continuous plastic deformation processing, and the dual requirements of biodegradable implant devices on mechanics and degradation are met.
Description
Technical Field
The invention belongs to the field of biomedical materials, and particularly relates to a biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire and a preparation method thereof.
Background
At present, biodegradable and absorbable materials in organisms are becoming a research hotspot of biomaterials, and the research on a new generation of degradable medical metal materials mainly represented by biodegradable magnesium and alloys is receiving special attention of people. Mg and Mg alloys have many better properties as biomedical materials than the existing biomedical metal materials. Numerous studies have shown that magnesium and magnesium are considered to be suitable both in terms of mechanical properties and biocompatibilityThe alloy is an excellent biological implant material. However, the degradation rate of magnesium and magnesium alloy is too fast, so that the mechanical property attenuation rate in the body of the degradable magnesium alloy implant device is too fast, and the degradable magnesium alloy implant device fails before the tissues are completely healed, thereby affecting the treatment effect. Therefore, the control of the degradation rate of magnesium and magnesium alloys in physiological electrolyte environments (especially uniform corrosion of materials) remains a major bottleneck problem in the application of biological magnesium alloys. The reason why magnesium alloys are prone to corrosion is that, in addition to their natural characteristics (the surface of magnesium alloys cannot spontaneously form a protective surface film), the key reason is that stable second phases in magnesium alloys form galvanic corrosion with the matrix. And impurity elements such as Fe, Ni and Cu gathered in grain boundary and impurity element phase distributed in matrix (such as Al) 3 Fe, etc.) has active cathode properties, promoting the formation of microcells on the surface of magnesium alloys.
The existing research shows that compared with the internationally adopted modified WE43 and MgCaZn alloy, the high-purity magnesium (the purity is more than 99.99 percent) and the high-purity magnesium alloy (AZ91E) avoid the problem of accelerated degradation of galvanic corrosion of impurity elements such as Fe, Ni, Cu and the like in the alloy, have excellent corrosion resistance and can effectively solve the problem of premature failure of mechanical properties caused by over-quick degradation of a magnesium implant device. However, high-purity magnesium (purity more than 99.99%) and high-purity magnesium alloy (AZ91E) have low mechanical properties, for example, the tensile strength of extruded ultra-high-purity magnesium is not ultra-high 150MPa, and AZ91E can only reach 250MPa, and cannot meet the requirements of load-bearing biodegradable implant devices.
Therefore, in order to solve the problems, a biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire and a preparation method thereof are urgently needed to be provided.
Disclosure of Invention
The invention aims to solve the problems of low mechanical property and high magnesium alloy degradation rate of the existing high-purity magnesium, and provides a biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire material and a preparation method thereof. The biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire material is obtained by utilizing the advantage of excellent low degradation rate of the high-purity magnesium alloy through multi-step continuous plastic deformation processing, and the dual requirements of biodegradable implant devices on mechanics and degradation are met.
In order to achieve the above object, the present invention provides a method for preparing biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire, which comprises the following steps:
s1: carrying out hot extrusion treatment on the high-purity Mg-Zn-Mn magnesium alloy ingot to obtain an extruded bar;
s2: carrying out recrystallization annealing treatment on the extruded bar to obtain a recrystallization annealing bar;
s3: and sequentially carrying out primary rotary swaging deformation treatment and secondary rotary swaging deformation treatment on the recrystallized annealed bar to obtain the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire.
In the invention, the design idea of the invention is as follows:
firstly, in order to improve the corrosion resistance of the alloy material, firstly, high-purity raw materials and vacuum induction melting are adopted, and the content of impurity elements such as Fe, Ni, Cu and the like (the total amount is less than or equal to 10ppm) is strictly controlled; secondly, adopting low-alloying alloy design (the total content of alloying elements is less than or equal to 3 percent), and controlling the size and the quantity of a second phase; thirdly, obtaining uniform and fine tissues and breaking large second phases through multi-step continuous plastic processing. By combining the effects of the three aspects, the galvanic corrosion caused by harmful impurity elements such as Fe, Ni, Cu and the like and a coarse second phase can be obviously reduced, so that the corrosion failure mode of the alloy is changed from point corrosion to uniform corrosion, and the corrosion resistance of the alloy material is improved.
On the basis, the mechanical property of the high-purity magnesium alloy is greatly improved by a multi-step continuous plastic deformation processing method. In the multi-step continuous plastic processing process, a coarse as-cast structure is refined through the action of hot extrusion, and subsequent recrystallization annealing provides a refined grain structure and an alloy material with excellent plasticity for subsequent swaging deformation treatment, so that cracking in the swaging process is prevented. The swaging deformation process of the present invention includes a first swaging deformation process (a large deformation amount swaging process) and a second swaging deformation process (a small deformation amount swaging process): the large-deformation rotary swaging processing is utilized to refine the sizes of alloy grains and a second phase, the dislocation density of the alloy material is improved, and the small-deformation rotary swaging processing can reduce the processing stress and improve the surface quality of the wire, so that the high-quality and high-strength biological magnesium alloy material is finally obtained.
In addition, the high-strength biological magnesium alloy material obtained by multi-step continuous plastic processing has uniform and fine tissue, the corrosion failure mode of the material is changed from pitting corrosion to uniform corrosion, and the corrosion resistance of the material is further improved, so that the high-purity magnesium alloy wire which has good biocompatibility, good corrosion resistance and enough strength is obtained.
According to the invention, preferably, based on the total mass of the high-purity Mg-Zn-Mn magnesium alloy ingot, the Zn content in the high-purity Mg-Zn-Mn magnesium alloy ingot is 0.5-2.5%, the Mn content is 0.01-1.0%, the total content of impurity elements such as Fe, Ni and Cu is less than or equal to 10ppm, and the balance is Mg.
According to the invention, the high-purity Mg-Zn-Mn magnesium alloy ingot is prepared by a vacuum induction melting method.
According to the present invention, preferably, the steps of the vacuum induction melting method include:
(1) baking high-purity magnesium, high-purity zinc and high-purity manganese raw materials;
(2) putting the baked high-purity magnesium, high-purity zinc and high-purity manganese raw materials into a crucible of a vacuum induction smelting furnace, closing the furnace, vacuumizing until the vacuum degree in the furnace is less than 1Pa, filling high-purity argon into the furnace to 0.3-0.5 atmospheric pressure, vacuumizing again until the vacuum degree in the furnace is less than 1Pa, and filling high-purity argon into the furnace to 0.3-0.5 atmospheric pressure;
(3) opening a heating power supply of the vacuum induction smelting furnace, and carrying out induction smelting until the high-purity magnesium, high-purity zinc and high-purity manganese raw materials are completely clear;
(4) heating to a refining temperature, and carrying out refining treatment; and after the refining treatment is finished, pouring to obtain the high-purity Mg-Zn-Mn magnesium alloy ingot.
According to the invention, preferably, the high-purity magnesium has a magnesium content of > 99.99%; the zinc content of the high-purity zinc is more than 99.99 percent; the manganese content of the high-purity manganese is more than 99.99 percent.
According to the invention, the temperature of the baking treatment is preferably 120-160 ℃, and the time is preferably 1.5-2.5 h.
According to the present invention, preferably, the crucible of the vacuum induction melting furnace is selected from a graphite crucible, a metal crucible, or a calcium oxide crucible.
According to the invention, the temperature of the refining treatment is preferably 720-760 ℃, and the time is 8-12 min.
According to the invention, the melt casting is preferably carried out at 690 to 710 ℃.
According to the invention, the cross section diameter of the high-purity Mg-Zn-Mn magnesium alloy ingot is preferably 90-110 mm.
According to the present invention, preferably, the step S1 further includes: the high-purity Mg-Zn-Mn magnesium alloy ingot is subjected to heat preservation treatment for 1.5-2.5 hours at the temperature of 340-380 ℃ before hot extrusion treatment.
According to the invention, the extrusion forming temperature of the hot extrusion treatment is preferably 250-400 ℃, and the extrusion ratio is preferably 20-90.
According to the invention, the treatment temperature of the recrystallization annealing treatment is preferably 100-280 ℃, and the treatment time of the recrystallization annealing treatment is preferably 0.25-3 h.
According to the invention, the temperature of the first rotary swaging deformation treatment is preferably 20-180 ℃;
the diameter of the cross section of the wire obtained through the first rotary swaging deformation treatment is reduced by 2-15 mm compared with that of the cross section of the extruded bar, wherein the diameter of each pass of the first rotary swaging deformation treatment is reduced by 0.5-2 mm;
the feeding speed of the first rotary swaging deformation treatment is less than or equal to 10 m/min.
According to the invention, the temperature of the second rotary swaging deformation treatment is preferably 20-120 ℃;
the diameter of the cross section of the wire obtained through the second rotary swaging deformation treatment is reduced by 0.2-2 mm compared with that of the wire obtained through the first rotary swaging deformation treatment, wherein the diameter of each pass of the second rotary swaging deformation treatment is reduced by 0.1-0.5 mm;
the feeding speed of the second rotary swaging deformation treatment is less than or equal to 5 m/min;
the cross section diameter of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire is 2-30 mm, and the axial length of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire is 2000-10000 mm.
On the other hand, the invention provides the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire prepared by the preparation method of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire.
The technical scheme of the invention has the following beneficial effects:
(1) the invention adopts high-purity raw materials and vacuum induction melting, strictly controls the content of impurity elements such as Fe, Ni, Cu and the like (the total amount is less than or equal to 10ppm), and solves the problem of accelerated degradation of galvanic corrosion caused by harmful impurity elements such as Fe, Ni, Cu and the like; the low-alloying alloy design (the total content of alloying elements is less than or equal to 3 percent) is adopted, so that the size of the second phase is small, the quantity of the second phase is small, and the rate of galvanic corrosion caused by the second phase is obviously reduced; meanwhile, the magnesium alloy wire prepared by multi-step continuous plastic processing has uniform and refined tissue, the corrosion failure mode of the alloy is finally changed from pitting corrosion to uniform corrosion, and the corrosion resistance is obviously improved, so that the problem of premature failure of mechanical properties caused by too fast degradation of a magnesium implant device is solved, and the simulated body fluid degradation rate is less than or equal to 0.5 mm/year.
(2) The invention provides an alloy material with refined grain structure and excellent plasticity for the rotary swaging deformation treatment by a multi-step continuous plastic deformation processing method and utilizing hot extrusion and subsequent recrystallization annealing, thereby preventing cracking in the rotary swaging process. The invention utilizes the rotary swaging processing with large deformation amount to refine the sizes of alloy crystal grains and a second phase, improves the dislocation density of the alloy material, and then utilizes the rotary swaging processing with small deformation amount to reduce the processing stress, thereby improving the strength of the material, ensuring that the room-temperature tensile strength of the high-purity magnesium alloy wire is more than or equal to 330MPa, and the elongation is more than or equal to 12 percent, and meeting the requirements of force-bearing biodegradable implant devices.
(3) The preparation technology of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire material can be used for large-scale production to prepare the high-purity high-strength corrosion-resistant magnesium alloy wire material with the diameter of 2-30 mm and the length of 2000-10000 mm, and solves the problem that the processes such as equal channel extrusion can only prepare laboratory-level samples.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
FIG. 1 shows a microscopic view of the surface morphology of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire prepared in example 1 of the present invention after being subjected to salt spray corrosion at 5% NaCl/35 ℃/48 h.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
The embodiment provides a preparation method of a biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire, which comprises the following steps:
s1: baking high-purity magnesium (more than 99.99%), high-purity zinc (more than 99.99%) and high-purity manganese (more than 99.99%) at 150 ℃ for 2 h;
s2: putting the baked high-purity magnesium, high-purity zinc and high-purity manganese raw materials into a crucible of a vacuum induction smelting furnace, then putting the crucible of the vacuum induction smelting furnace into the vacuum induction smelting furnace, closing the furnace, vacuumizing until the vacuum degree in the furnace is less than 1Pa, filling high-purity argon into the furnace to 0.4 atmospheric pressure, vacuumizing again until the vacuum degree in the furnace is 1Pa, and filling the high-purity argon into the furnace to 0.4 atmospheric pressure;
s3: opening a heating power supply of the vacuum induction smelting furnace, and carrying out induction smelting until the high-purity magnesium, high-purity zinc and high-purity manganese raw materials are completely purified;
s4: heating to 740 ℃ for refining for 10 min; after the refining treatment is finished, pouring the alloy into a metal die with the diameter of 100mm at 700 ℃ to prepare a high-purity Mg-1.5% Zn-0.5% Mn magnesium alloy ingot, wherein the total content of impurity elements of Fe, Ni and Cu is 5 ppm.
S5: putting a high-purity Mg-1.5% Zn-0.5% Mn magnesium alloy ingot into a heat preservation furnace, preserving heat at 350 ℃ for 2 hours, and then carrying out hot extrusion on a 3000-ton extruder at the extrusion temperature of 300 ℃ at the extrusion ratio of 40 to obtain an extruded bar with the cross section diameter of 16 mm;
s6: carrying out recrystallization annealing treatment on the extruded bar to obtain a recrystallization annealing bar; the crystallization annealing temperature is 240 ℃, and the crystallization annealing time is 0.5 h.
S7: performing primary rotary swaging deformation treatment on the recrystallized annealed bar, wherein the temperature of the primary rotary swaging deformation treatment is 20-180 ℃, the diameter of the cross section of the wire obtained by the primary rotary swaging deformation treatment is reduced by 4mm compared with that of the cross section of the extruded bar, the diameter of each pass is reduced by 0.8mm, and the feeding speed is 6 m/min;
performing secondary rotary swaging deformation treatment on the wire material obtained by the primary rotary swaging deformation treatment, wherein the temperature of the secondary rotary swaging deformation treatment is 20-120 ℃, the diameter of the cross section of the wire material obtained by the secondary rotary swaging deformation treatment is reduced by 0.6mm compared with that of the wire material obtained by the primary rotary swaging deformation treatment, the diameter of each pass is reduced by 0.2mm, and the feeding speed is less than or equal to 5 m/min;
the biomedical high-purity high-strength corrosion-resistant Mg-1.5% Zn-0.5% Mn magnesium alloy wire is obtained, the cross section diameter is 11.4mm, and the axial length is 3000 mm.
Example 2
The embodiment provides a preparation method of biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire, which uses a high-purity Mg-1.8% Zn-0.6% Mn magnesium alloy ingot, wherein the total content of impurity elements of Fe, Ni and Cu is 6 ppm;
the steps for preparing the high-purity Mg-1.8% Zn-0.6% Mn magnesium alloy ingot are different from the steps S1 to S4 of example 1 only in that: refining at 750 deg.C for 10 min; after the completion of the refining treatment, the molten steel was poured into a metal crucible having a diameter of 100mm at 710 ℃.
S5: putting a high-purity Mg-1.8% Zn-0.6% Mn magnesium alloy ingot into a heat preservation furnace, preserving heat at 360 ℃ for 2 hours, and then carrying out hot extrusion on a 3000-ton extruder at the extrusion temperature of 320 ℃ at the extrusion ratio of 60 to obtain an extruded bar with the cross section diameter of 12 mm;
s6: carrying out recrystallization annealing treatment on the extruded bar to obtain a recrystallization annealing bar; the crystallization annealing temperature is 220 ℃, and the crystallization annealing time is 0.5 h.
S7: performing primary rotary swaging deformation treatment on the recrystallized annealed bar at the temperature of 20-180 ℃, wherein the diameter of the cross section of the wire obtained by the primary rotary swaging deformation treatment is reduced by 3mm compared with that of the cross section of the extruded bar, the diameter of each pass is reduced by 0.5mm, and the feeding speed is 6 m/min;
performing secondary rotary swaging deformation treatment on the wire material obtained by the primary rotary swaging deformation treatment, wherein the temperature of the secondary rotary swaging deformation treatment is 20-120 ℃, the diameter of the cross section of the wire material obtained by the secondary rotary swaging deformation treatment is reduced by 0.6mm compared with that of the wire material obtained by the primary rotary swaging deformation treatment, the diameter of each pass is reduced by 0.15mm, and the feeding speed is less than or equal to 4 m/min;
the biomedical high-purity high-strength corrosion-resistant Mg-1.8% Zn-0.6% Mn magnesium alloy wire is obtained, the cross section diameter is 8.4mm, and the axial length is 3000 mm.
Example 3
The embodiment provides a preparation method of biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire, which uses a high-purity Mg-1.2% Zn-0.4% Mn magnesium alloy ingot, wherein the total content of impurity elements of Fe, Ni and Cu is 5 ppm;
the procedure for preparing the high purity Mg-1.2% Zn-0.4% Mn magnesium alloy ingot was exactly the same as that of steps S1-S7 of example 1.
Example 4
This example differs from example 1 only in that: and S7, carrying out rotary swaging deformation treatment for the first time, wherein the diameter of the cross section of the alloy bar is reduced by 2mm, the diameter of each pass is reduced by 0.8mm, and the feeding speed is 6 m/min.
Example 5
This example differs from example 1 only in that: the extrusion forming temperature of the S5 hot extrusion is 300 ℃, and the extrusion ratio is 20.
Comparative example 1
This comparative example differs from example 1 in that: and after the first rotary swaging deformation treatment, the second rotary swaging deformation treatment is not carried out.
Comparative example 2
This comparative example differs from example 1 in that: and the alloy ingot is smelted under the protection of normal pressure gas instead of vacuum induction smelting for subsequent processing. The total content of Fe, Ni and Cu impurity elements in the alloy is 40 ppm.
Test example
This test example performed room temperature tensile property tests on the high purity magnesium alloy wires of examples 1 to 5 and comparative examples 1 to 2, and the results of tensile strength, elongation, and simulated body fluid degradation rate of the high purity magnesium alloy wires of examples 1 to 5 and comparative examples 1 to 2 are shown in Table 1.
Wherein, the room-temperature tensile property of the high-purity magnesium wire material is determined according to GB/T228.1-2010 metallic material tensile experiment part 1: room temperature test method, INSTRON 55822 electronic Universal testing machine was used for the tests.
The simulated body fluid degradation rate of the high-purity magnesium wire material is carried out in Hank's simulated body fluid (the components are shown in a table 2) according to ASTM-G31-72 laboratory immersion corrosion test of metals, and the simulated body fluid degradation rate is carried out by a hydrogen evolution method and a weight loss method. Volume of solution (mL) in the experiment was set as total surface area of sample (cm) 2 ) 100 times of the total weight of the sample before the soaking experiment, the sample is weighed (0.01mg) by using a high-precision balance, and the hydrogen evolution volume of the sample during the soaking process is recorded. After soaking for 48 hours, taking out the sample, ultrasonically cleaning the sample for 2 minutes by using a chromic acid solution (200g/L CrO3+10g/L AgNO3), then washing the surface of the sample by using deionized water, drying the sample by cold air, and weighing the sample after the soaking test. At least 3 sets of soaking tests were repeated for each sample and the results averaged.
The corrosion rate of the sample can be calculated according to the hydrogen evolution result (CRHE, mm/year) and the weight loss result (CRWL, mm/year), and the calculation formula is as follows:
wherein Sm is the total surface area (cm) of the sample 2 )，T m Is the soaking time (h), ρ m Is the sample density (g/cm) 3 )，ΔV H2 Volume of evolved hydrogen (mL), Δ M, for the samples in the soak experiment m Is the weight loss (g) of the sample in the soaking experiment.
TABLE 1
TABLE 2
As can be seen from the comparison of the data of example 1 and example 3 in Table 1, the tensile strength and degradation rate of the alloy are slightly reduced by reducing the content of Zn and Mn elements in the material.
As can be seen from a comparison of the data in Table 1 between example 1 and examples 4 and 5, it is advantageous to increase the extrusion ratio and increase the amount of swaging deformation in order to provide the tensile strength of the magnesium alloy wire.
As can be seen from the comparison of the data of example 1 and comparative example 1 in Table 1, the adoption of the secondary swaging is beneficial to improving the surface quality of the magnesium alloy wire and is also helpful to improving the tensile strength of the magnesium alloy wire.
As can be seen from the comparison of the data of the example 1 and the comparative example 2 in the table 1, the total content of the three impurity elements of Fe, Ni and Cu in the alloy obviously affects the degradation rate of the magnesium alloy wire, and the reduction of the total content of the three impurity elements is beneficial to improving the degradation resistance of the magnesium alloy wire.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (7)
1. A preparation method of biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire is characterized by comprising the following steps:
s1: carrying out hot extrusion treatment on the high-purity Mg-Zn-Mn magnesium alloy ingot to obtain an extruded bar;
s2: carrying out recrystallization annealing treatment on the extruded bar to obtain a recrystallization annealing bar;
s3: sequentially carrying out primary rotary swaging deformation treatment and secondary rotary swaging deformation treatment on the recrystallized annealed bar to obtain the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire;
based on the total mass of the high-purity Mg-Zn-Mn magnesium alloy ingot, the high-purity Mg-Zn-Mn magnesium alloy ingot contains 0.5-2.5% of Zn, 0.01-1.0% of Mn, less than or equal to 10ppm of Fe, Ni and Cu impurity elements, and the balance of Mg;
the temperature of the first rotary swaging deformation treatment is 20-180 ℃;
the diameter of the cross section of the wire obtained through the first rotary swaging deformation treatment is reduced by 2-15 mm compared with that of the cross section of the extruded bar, wherein the diameter of each pass of the first rotary swaging deformation treatment is reduced by 0.5-2 mm;
the feeding speed of the first rotary swaging deformation treatment is less than or equal to 10 m/min;
the temperature of the second rotary swaging deformation treatment is 20-120 ℃;
the diameter of the cross section of the wire obtained through the second rotary swaging deformation treatment is reduced by 0.2-2 mm compared with that of the wire obtained through the first rotary swaging deformation treatment, wherein the diameter of each pass of the second rotary swaging deformation treatment is reduced by 0.1-0.5 mm;
the feeding speed of the second rotary swaging deformation treatment is less than or equal to 5 m/min;
the cross section diameter of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire is 2-30 mm, and the axial length of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire is 2000-10000 mm.
2. The method for preparing biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire according to claim 1, wherein the preparation of the high-purity Mg-Zn-Mn magnesium alloy ingot adopts a vacuum induction melting method.
3. The method for preparing biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire according to claim 2, wherein the vacuum induction melting method comprises the following steps:
(1) baking high-purity magnesium, high-purity zinc and high-purity manganese raw materials;
(2) putting the baked high-purity magnesium, high-purity zinc and high-purity manganese raw materials into a crucible of a vacuum induction smelting furnace, closing the furnace, vacuumizing until the vacuum degree in the furnace is less than 1Pa, filling high-purity argon into the furnace to 0.3-0.5 atmospheric pressure, vacuumizing again until the vacuum degree in the furnace is less than 1Pa, and filling high-purity argon into the furnace to 0.3-0.5 atmospheric pressure;
(3) opening a heating power supply of the vacuum induction smelting furnace, and carrying out induction smelting until the high-purity magnesium, high-purity zinc and high-purity manganese raw materials are completely purified;
(4) heating to a refining temperature, and carrying out refining treatment; and after the refining treatment is finished, pouring to obtain the high-purity Mg-Zn-Mn magnesium alloy ingot.
4. The method for preparing biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire according to claim 3,
the high-purity magnesium has a magnesium content of more than 99.99 percent; the zinc content of the high-purity zinc is more than 99.99 percent; the manganese content of the high-purity manganese is more than 99.99 percent;
the baking treatment temperature is 120-160 ℃, and the baking treatment time is 1.5-2.5 h;
the crucible of the vacuum induction smelting furnace is a graphite crucible, a metal crucible or a calcium oxide crucible;
the refining treatment temperature is 720-760 ℃, and the refining treatment time is 8-12 min;
melt casting is carried out at 690-710 ℃;
the cross section diameter of the high-purity Mg-Zn-Mn magnesium alloy ingot is 90-110 mm.
5. The method for preparing biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire according to claim 1,
the step S1 further includes: the high-purity Mg-Zn-Mn magnesium alloy ingot is subjected to heat preservation treatment at 340-380 ℃ for 1.5-2.5 h before hot extrusion treatment;
the extrusion forming temperature of the hot extrusion treatment is 250-400 ℃, and the extrusion ratio is 20-90.
6. The method for preparing biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire according to claim 1, wherein the treatment temperature of the recrystallization annealing treatment is 100-280 ℃, and the treatment time of the recrystallization annealing treatment is 0.25-3 h.
7. The biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire prepared by the preparation method of the biomedical high-purity high-strength corrosion-resistant Mg-Zn-Mn magnesium alloy wire according to any one of claims 1 to 6.
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| CN101745592A (en) * | 2010-01-15 | 2010-06-23 | 北京工业大学 | Rotary swaging preparation method for high-strength magnesium alloy wire |
| CN105120907A (en) * | 2013-03-15 | 2015-12-02 | 西克索马特公司 | High strength and bio-absorbable magnesium alloys |
| CN108754270A (en) * | 2018-07-07 | 2018-11-06 | 中南大学 | A kind of superelevation low rare earth nano isomery magnesium alloy preparation method by force |
| CN110512129A (en) * | 2019-08-30 | 2019-11-29 | 中南大学 | A kind of forging torsion integrated technique preparing superelevation severe deformation magnesium alloy rod |
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|---|---|---|---|---|
| CN101745592A (en) * | 2010-01-15 | 2010-06-23 | 北京工业大学 | Rotary swaging preparation method for high-strength magnesium alloy wire |
| CN105120907A (en) * | 2013-03-15 | 2015-12-02 | 西克索马特公司 | High strength and bio-absorbable magnesium alloys |
| CN108754270A (en) * | 2018-07-07 | 2018-11-06 | 中南大学 | A kind of superelevation low rare earth nano isomery magnesium alloy preparation method by force |
| CN110512129A (en) * | 2019-08-30 | 2019-11-29 | 中南大学 | A kind of forging torsion integrated technique preparing superelevation severe deformation magnesium alloy rod |
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