CN112355586B - Preparation method of degradable double-layer biological magnesium alloy - Google Patents
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Abstract
本发明公开一种可降解双层生物镁合金的制备方法。包括：(1)熔炼：称取金属镁、锌、钙和锂，将原料熔炼，得Mg‑Zn‑Ca和Mg‑Li两种生物镁合金铸锭；(2)均匀化：将Mg‑Zn‑Ca和Mg‑Li均匀化处理，冷却；(3)挤压：均匀化处理后，将Mg‑Zn‑Ca挤压成管材、Mg‑Li挤压成棒材；(4)搅拌摩擦焊：将Mg‑Li棒材穿插于Mg‑Zn‑Ca管材中，用搅拌摩擦焊的方式实现Mg‑Li棒材和Mg‑Zn‑Ca管材双层镁合金间的连接，得双层生物镁合金棒；(5)拉拔：将双层生物镁合金棒拉拔至直径为5‑10毫米。本发明的制备方法简单，采用的两种生物镁合金的相组成均为完全的固溶体结构，在生物体内可完全降解，降解过程不产生难以溶解的第二相颗粒，保证了生物安全性；本发明制得的可降解双层生物镁合金，连接效果好，结合强度高。
The invention discloses a preparation method of a degradable double-layer biological magnesium alloy. Including: (1) smelting: take by weighing metal magnesium, zinc, calcium and lithium, and smelting raw materials to obtain two kinds of biological magnesium alloy ingots of Mg-Zn-Ca and Mg-Li; (2) homogenization: Mg-Zn is ‑Ca and Mg‑Li are homogenized and cooled; (3) Extrusion: After homogenization, Mg‑Zn‑Ca is extruded into pipes and Mg‑Li into bars; (4) friction stir welding: The Mg-Li rod is inserted into the Mg-Zn-Ca pipe, and the connection between the Mg-Li rod and the double-layer magnesium alloy of the Mg-Zn-Ca pipe is realized by friction stir welding, so as to obtain a double-layer biological magnesium alloy rod (5) Drawing: Drawing the double-layer biological magnesium alloy rod to a diameter of 5-10 mm. The preparation method of the invention is simple, and the phase compositions of the two bio-magnesium alloys used are complete solid solution structures, which can be completely degraded in the living body, and the second phase particles that are difficult to dissolve are not generated during the degradation process, thereby ensuring the biological safety; The degradable double-layer biological magnesium alloy prepared by the invention has good connection effect and high bonding strength.
Description
Technical Field
The invention belongs to the technical field of metal materials, relates to a preparation method of a biological magnesium alloy, and particularly relates to a preparation method of a degradable double-layer biological magnesium alloy.
Background
A great deal of bone injury caused by traffic accidents, sports and the like brings huge market space and prospect for the biological implant material, and greatly promotes the development of the biological implant material. Magnesium alloys have a series of unique advantages in the field of bioimplantation: (1) the magnesium alloy has good biocompatibility, Mg is a major metal element next to Ca, Na and K in a human body, can activate various enzymes and participate in a series of metabolic processes in the human body, excess Mg in the human body can be discharged out of the human body through urine, and has a good biological safety foundation, and in addition, Mg is also an essential element for bone growth, can promote the deposition of Ca and induce the generation of new bones; (2) the magnesium alloy has good mechanical compatibility, has higher specific strength and specific stiffness, can meet the mechanical property requirement of biological implantation materials, has the elastic modulus of about 41-45GPa, is far lower than materials such as stainless steel, titanium alloy and the like, is closer to the elastic modulus of human bones, can effectively relieve the stress shielding effect, and promotes the growth and healing of bones; (3) the standard electrode potential of pure Mg is only-2.37V, the electrode is extremely easy to corrode in a corrosive medium, and the electrode can be degraded in a human body after the bone repair or fixation function is completed, so that secondary operation is avoided, and the risk and burden of a patient are greatly reduced.
However, the existing biological magnesium alloy still has some obvious problems to be solved. For example, most of the existing biological magnesium alloys have second phases which belong to intermetallic compounds, are stable in chemical properties, are not easy to decompose in vivo and have potential biological safety hazards. Secondly, the biological magnesium alloy has higher requirements on the mechanical property and the corrosion resistance in the early implantation process, when bones develop and heal gradually, the biological magnesium alloy is expected to be degraded as soon as possible and discharged from organisms, but most of the existing biological magnesium alloys have uniform texture, and the mechanical property and the corrosion resistance of the biological magnesium alloy can not be changed obviously in the whole implantation process.
Disclosure of Invention
The invention aims to provide a preparation method of a degradable double-layer biological magnesium alloy, which realizes the preparation of the degradable double-layer biological magnesium alloy by adopting the steps of smelting, homogenizing, extruding, friction stir ring welding, drawing and the like.
The invention is realized by the following technical scheme:
a preparation method of a degradable double-layer biological magnesium alloy comprises the following steps:
(1) smelting: weighing metal magnesium, zinc, calcium and lithium as raw materials according to target components, and then respectively smelting the raw materials in an inert atmosphere to obtain two biological magnesium alloy ingots of Mg-Zn-Ca and Mg-Li; specifically, the raw materials are placed in a vacuum induction smelting furnace and smelted under the protection of argon;
(2) homogenizing: respectively homogenizing the Mg-Zn-Ca biological magnesium alloy ingot and the Mg-Li biological magnesium alloy ingot at high temperature in an inert atmosphere, and then cooling; the step is also to carry out homogenization heat treatment under the protection of argon;
(3) extruding: extruding the homogenized Mg-Zn-Ca and Mg-Li biological magnesium alloy ingots; extruding the Mg-Zn-Ca biological magnesium alloy ingot into a pipe; extruding the Mg-Li biological magnesium alloy ingot into a bar;
(4) friction stir welding: inserting the Mg-Li biological magnesium alloy rod prepared by extrusion into the Mg-Zn-Ca biological magnesium alloy pipe, and connecting the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe by adopting a friction stir welding mode to obtain a double-layer biological magnesium alloy rod;
(5) drawing: and drawing the double-layer biological magnesium alloy rod until the diameter of the double-layer biological magnesium alloy rod is 5-10 mm. And (4) after the last drawing is finished, annealing treatment is not carried out, and the degradable double-layer biological magnesium alloy is obtained.
Further, the purity of the raw materials of the magnesium metal, the zinc metal, the calcium metal and the lithium metal in the step (1) is not less than 99.9 percent.
Further, the Mg-Zn-Ca biological magnesium alloy ingot in the step (1) comprises 1.0-2.0 wt% of Zn, 0.2-0.4 wt% of Ca and the balance of magnesium; the content of Li in the Mg-Li biological magnesium alloy ingot is 2.0-4.0 wt%, and the balance is magnesium.
Further, homogenizing step (2): homogenizing the Mg-Zn-Ca biological magnesium alloy ingot at the temperature of 450-500 ℃ for 8-16 hours in an inert atmosphere; homogenizing the Mg-Li biological magnesium alloy ingot at the temperature of 300-400 ℃ for 8-16 hours, and cooling by water quenching after the homogenization treatment is finished.
Further, extruding the Mg-Zn-Ca biological magnesium alloy ingot into a pipe with the outer diameter of 50-60 mm in the step (3), wherein the thickness of the pipe is 8-12 mm; and extruding the Mg-Li biological magnesium alloy ingot into a bar with the diameter of 42-48 mm.
Further, inserting the extruded Mg-Li biological magnesium alloy rod into the Mg-Zn-Ca biological magnesium alloy pipe in the step (4), and connecting the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe in a double-layer magnesium alloy mode by adopting friction stir welding to obtain a double-layer biological magnesium alloy rod; in the friction stir welding process, the rotating speed of a stirring pin is 800-1200rpm, the position of the stirring pin is kept still, a clamp is used for fixing the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe, the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe rotate at a constant speed and move forwards, wherein the rotating speeds of the rod and the pipe and the forward moving speed are kept consistent, the rotating speed is 5-10rpm, and the forward moving speed is 10-20 cm/min. The invention adopts the friction stir welding technology to connect the Mg-Zn-Ca biological alloy pipe material on the outer layer with the Mg-Li biological alloy bar material on the inner layer, and has good connection effect and high bonding strength.
Further, in the step (5), drawing the double-layer biological magnesium alloy rod at room temperature, wherein the diameter of the double-layer biological magnesium alloy rod before drawing is 50-60 mm, the diameter of the alloy rod in each pass is reduced by 5-10 mm in the drawing process, and the alloy rod is placed into an atmosphere furnace in each pass to be annealed in an inert atmosphere; and the final diameter of the double-layer biological magnesium alloy rod after drawing is 5-10 mm. And (4) after the last drawing is finished, annealing treatment is not carried out, and the degradable double-layer biological magnesium alloy is obtained. The invention adopts the drawing process to form and process the double-layer biological magnesium alloy bar, not only can reduce the diameter of the bar, but also can further improve the strength of the prepared double-layer biological magnesium alloy.
Further, the annealing treatment is carried out in an inert atmosphere, the temperature of the annealing treatment is 200-300 ℃, and the time of the annealing treatment is 1-3 hours.
The invention has the beneficial effects that:
(1) the preparation method of the degradable double-layer biological magnesium alloy adopts two biological magnesium alloy phases with complete solid solution structure, can be completely degraded in a living body, does not generate second-phase particles which are difficult to dissolve in the degradation process, and ensures the biological safety.
(2) The preparation method of the degradable double-layer biological magnesium alloy is simple, the design idea of the double-layer biological magnesium alloy is adopted, the outer-layer Mg-Zn-Ca biological magnesium alloy has better mechanical property and corrosion resistance, good fixing and supporting effects can be achieved at the early stage of implanting the biological magnesium alloy into an organism, the inner-layer Mg-Li biological magnesium alloy has poorer mechanical property and corrosion resistance, and bones are gradually healed; after the outer layer Mg-Zn-Ca biological magnesium alloy is degraded, the outer layer Mg-Zn-Ca biological magnesium alloy can be rapidly degraded under the action of body fluid.
(3) According to the preparation method of the degradable double-layer biological magnesium alloy, the outer-layer Mg-Zn-Ca biological magnesium alloy pipe and the inner-layer Mg-Li biological magnesium alloy rod are connected by adopting a friction stir ring welding technology, so that the connection effect is good, and the bonding strength is high.
(4) The method adopts the drawing process to form the double-layer biological magnesium alloy bar, not only can reduce the diameter of the bar, but also can further improve the strength of the double-layer biological magnesium alloy.
Drawings
FIG. 1 is a schematic diagram of friction stir welding of a double-layer biological magnesium alloy.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a degradable double-layer biological magnesium alloy comprises the following steps:
(1) smelting: weighing metal magnesium (Mg), zinc (Zn), calcium (Ca) and lithium (Li) with the purity of 99.9 wt% as raw materials according to target components, then placing the raw materials in a vacuum induction smelting furnace, introducing argon as protective gas, and respectively smelting to obtain two biological magnesium alloy ingots of Mg-Zn-Ca and Mg-Li; wherein: the content of Zn in the Mg-Zn-Ca biological magnesium alloy ingot is 1.0 wt%, the content of Ca is 0.2 wt%, and the balance is Mg; the content of Li in the Mg-Li biological magnesium alloy ingot is 2.0wt percent, and the balance is Mg;
(2) homogenizing: homogenizing the Mg-Zn-Ca biological magnesium alloy ingot at 450 ℃ for 8 hours under argon atmosphere, homogenizing the Mg-Li biological magnesium alloy ingot at 300 ℃ for 8 hours, and quenching with water and cooling after homogenization;
(3) extruding: extruding the homogenized Mg-Zn-Ca and Mg-Li biological magnesium alloy ingots; extruding the Mg-Zn-Ca biological magnesium alloy ingot into a pipe with the outer diameter of 50 mm and the wall thickness of 8 mm; extruding the Mg-Li biological magnesium alloy ingot into a bar with the diameter of 42 mm;
(4) friction stir welding: inserting the extruded Mg-Li biological magnesium alloy rod into the Mg-Zn-Ca biological magnesium alloy pipe, and connecting the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe by adopting a friction stir welding mode to obtain a double-layer biological magnesium alloy rod; as shown in fig. 1: in the friction stir ring welding process, the rotating speed of a stirring pin is 800rpm, the position of the stirring pin is kept still, a clamp is used for fixing an Mg-Li biological magnesium alloy rod and an Mg-Zn-Ca biological magnesium alloy pipe, the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe rotate at a constant speed and move forwards, wherein: the rotating speed and the forward moving speed of the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe are kept consistent, wherein the rotating speed is 5 revolutions per minute, and the forward moving speed is 10 centimeters per minute;
(5) drawing: and (2) drawing the double-layer biological magnesium alloy rod at room temperature, wherein the diameter of the double-layer biological magnesium alloy rod before drawing is 50 mm (namely the diameter of the double-layer biological magnesium alloy rod is the outer diameter of the Mg-Zn-Ca biological magnesium alloy pipe), the diameter of the double-layer biological magnesium alloy rod in each pass is reduced by 5mm in the drawing process, the double-layer biological magnesium alloy rod is placed into a high-temperature atmosphere furnace in each pass for annealing treatment under the argon atmosphere, the annealing treatment temperature is 200 ℃, the annealing time is 1 hour, the final diameter of the double-layer biological magnesium alloy rod after drawing is 5mm, and the annealing treatment is not performed after the last pass of drawing is finished, so that the degradable double-layer biological magnesium alloy is obtained.
The tensile strength of the degradable double-layer biological magnesium alloy prepared in the example 1 is 232MPa according to GB/T228-2010 metal material tensile test. The Corrosion performance test was carried out according to ASTM G31-1972(2004) Standard Practice for Lab Immersion Testing of Metals, the Corrosion medium being a simulated body fluid, the temperature being maintained at 36.5. + -. 0.5 ℃ and the simulated body fluid being replaced every 24 hours. Test results show that the corrosion rates of the double-layer biological magnesium alloy are obviously different, the corrosion rate of the Mg-Zn-Ca biological magnesium alloy on the outer layer is 0.16mm/year, and the corrosion rate of the Mg-Li biological magnesium alloy on the inner layer is 0.45 mm/year.
Example 2
A preparation method of a degradable double-layer biological magnesium alloy comprises the following steps:
(1) smelting: weighing metal magnesium (Mg), zinc (Zn), calcium (Ca) and lithium (Li) with the purity of 99.9 wt% as raw materials according to target components, then placing the raw materials in a vacuum induction smelting furnace, introducing argon as protective gas, and respectively smelting to obtain two biological magnesium alloy ingots of Mg-Zn-Ca and Mg-Li; wherein: the content of Zn in the Mg-Zn-Ca biological magnesium alloy ingot is 1.5 wt%, the content of Ca is 0.3 wt%, and the balance is Mg; the content of Li in the Mg-Li biological magnesium alloy ingot is 3.0wt percent, and the balance is Mg;
(2) homogenizing: homogenizing the Mg-Zn-Ca biological magnesium alloy ingot at 475 ℃ for 12 hours under argon atmosphere, homogenizing the Mg-Li biological magnesium alloy ingot at 350 ℃ for 12 hours, and cooling by water quenching after homogenization is finished;
(3) extruding: extruding the homogenized Mg-Zn-Ca and Mg-Li biological magnesium alloy ingots; extruding the Mg-Zn-Ca biological magnesium alloy ingot into a pipe with the outer diameter of 55 mm and the wall thickness of 10 mm; extruding the Mg-Li biological magnesium alloy ingot into a bar with the diameter of 45 mm;
(4) friction stir welding: inserting the extruded Mg-Li biological magnesium alloy rod into the Mg-Zn-Ca biological magnesium alloy pipe, and connecting the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe by adopting a friction stir welding mode to obtain a double-layer biological magnesium alloy rod; as shown in fig. 1: in the friction stir ring welding process, the rotating speed of a stirring pin is 1000rpm, the position of the stirring pin is kept still, a clamp is used for fixing an Mg-Li biological magnesium alloy rod and an Mg-Zn-Ca biological magnesium alloy pipe, the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe rotate at a constant speed and move forwards, wherein: the rotating speed and the forward moving speed of the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe are kept consistent, wherein the rotating speed is 8 revolutions per minute, and the forward moving speed is 15 centimeters per minute;
(5) drawing: and (2) drawing the double-layer biological magnesium alloy rod at room temperature, wherein the diameter of the double-layer biological magnesium alloy rod before drawing is 55 mm (namely the diameter of the double-layer biological magnesium alloy rod is the outer diameter of the Mg-Zn-Ca biological magnesium alloy pipe), the diameter of the double-layer biological magnesium alloy rod in each pass is reduced by 5mm in the drawing process, the double-layer biological magnesium alloy rod is placed into a high-temperature atmosphere furnace in each pass for annealing treatment under the argon atmosphere, the annealing treatment temperature is 200 ℃, the annealing time is 1 hour, the final diameter of the double-layer biological magnesium alloy rod after drawing is 5mm, and the annealing treatment is not performed after the last pass of drawing is finished, so that the degradable double-layer biological magnesium alloy is obtained.
The tensile strength of the degradable double-layer biological magnesium alloy prepared in the example 2 is 256MPa according to GB/T228-2010 metal material tensile test. The Corrosion performance test was carried out according to ASTM G31-1972(2004) Standard Practice for Lab Immersion Testing of Metals, the Corrosion medium being a simulated body fluid, the temperature being maintained at 36.5. + -. 0.5 ℃ and the simulated body fluid being replaced every 24 hours. Test results show that the corrosion rates of the double-layer biological magnesium alloy are obviously different, the corrosion rate of the Mg-Zn-Ca biological magnesium alloy on the outer layer is 0.23mm/year, and the corrosion rate of the Mg-Li biological magnesium alloy on the inner layer is 0.54 mm/year.
Example 3
A preparation method of a degradable double-layer biological magnesium alloy comprises the following steps:
(1) smelting: weighing metal magnesium (Mg), zinc (Zn), calcium (Ca) and lithium (Li) with the purity of 99.9 wt% as raw materials according to target components, then placing the raw materials in a vacuum induction smelting furnace, introducing argon as protective gas, and respectively smelting to obtain two biological magnesium alloy ingots of Mg-Zn-Ca and Mg-Li; wherein: the content of Zn in the Mg-Zn-Ca biological magnesium alloy ingot is 2.0 wt%, the content of Ca is 0.4 wt%, and the balance is Mg; the content of Li in the Mg-Li biological magnesium alloy ingot is 4.0wt percent, and the balance is Mg;
(2) homogenizing: homogenizing the Mg-Zn-Ca biological magnesium alloy ingot at 500 ℃ for 16 hours under argon atmosphere, homogenizing the Mg-Li biological magnesium alloy ingot at 400 ℃ for 16 hours, and quenching with water and cooling after homogenization;
(3) extruding: extruding the homogenized Mg-Zn-Ca and Mg-Li biological magnesium alloy ingots; extruding the Mg-Zn-Ca biological magnesium alloy ingot into a pipe with the outer diameter of 60 mm and the wall thickness of 12 mm; extruding the Mg-Li biological magnesium alloy ingot into a bar with the diameter of 48 mm;
(4) friction stir welding: inserting the extruded Mg-Li biological magnesium alloy rod into the Mg-Zn-Ca biological magnesium alloy pipe, and connecting the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe by adopting a friction stir welding mode to obtain a double-layer biological magnesium alloy rod; as shown in fig. 1: in the friction stir ring welding process, the rotating speed of a stirring pin is 1200rpm, the position of the stirring pin is kept still, a clamp is used for fixing an Mg-Li biological magnesium alloy rod and an Mg-Zn-Ca biological magnesium alloy pipe, the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe rotate at a constant speed and move forwards, wherein: the rotating speed and the forward moving speed of the Mg-Li biological magnesium alloy rod and the Mg-Zn-Ca biological magnesium alloy pipe are kept consistent, wherein the rotating speed is 10 revolutions per minute, and the forward moving speed is 20 centimeters per minute;
(5) drawing: and (2) drawing the double-layer biological magnesium alloy rod at room temperature, wherein the diameter of the double-layer biological magnesium alloy rod before drawing is 60 mm (namely the diameter of the double-layer biological magnesium alloy rod is the outer diameter of the Mg-Zn-Ca biological magnesium alloy pipe), the diameter of the double-layer biological magnesium alloy rod in each pass is reduced by 5mm in the drawing process, the double-layer biological magnesium alloy rod is placed into a high-temperature atmosphere furnace in each pass for annealing treatment under the argon atmosphere, the annealing treatment temperature is 200 ℃, the annealing time is 1 hour, the final diameter of the double-layer biological magnesium alloy rod after drawing is 5mm, and the annealing treatment is not performed after the last pass of drawing is finished, so that the degradable double-layer biological magnesium alloy is obtained.
The tensile strength of the degradable double-layer biological magnesium alloy prepared in the embodiment 3 is 278MPa according to GB/T228-2010 metal material tensile test. The Corrosion performance test was carried out according to ASTM G31-1972(2004) Standard Practice for Lab Immersion Testing of Metals, the Corrosion medium being a simulated body fluid, the temperature being maintained at 36.5. + -. 0.5 ℃ and the simulated body fluid being replaced every 24 hours. Test results show that the corrosion rates of the double-layer biological magnesium alloy are obviously different, the corrosion rate of the Mg-Zn-Ca biological magnesium alloy on the outer layer is 0.31mm/year, and the corrosion rate of the Mg-Li biological magnesium alloy on the inner layer is 0.65 mm/year.
The above-mentioned preferred embodiments of the present invention are provided for illustration only and not for the purpose of limiting the invention. Obvious variations or modifications of the present invention are within the scope of the present invention.
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