CN113444919A - Zinc alloy material for degradable cardiovascular stent and preparation method thereof - Google Patents
Zinc alloy material for degradable cardiovascular stent and preparation method thereof Download PDFInfo
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/165—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon of zinc or cadmium or alloys based thereon
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Abstract
A zinc alloy material for a degradable cardiovascular stent and a preparation method thereof belong to the technical field of materials, and the alloy comprises, by weight, 0.03-0.07% of Mg, 0.03-0.07% of Mn, less than or equal to 10ppm of unavoidable impurities, and the balance of Zn. The preparation method comprises the following steps: (1) heating pure zinc to 600 +/-5 ℃, melting, sequentially adding metal magnesium, metal manganese and phosphorus, and uniformly stirring; cooling to 550 +/-5 ℃, pressing hexachloroethane, and standing for 10-20 min under heat preservation; cooling the molten metal to 500 +/-10 ℃, and casting; (2) carrying out secondary magnetic suspension smelting to ensure that the deviation of the component uniformity is less than +/-0.02 wt%; (3) keeping the temperature at 350 ℃ for 5 hours, then heating to 370 ℃ and keeping the temperature for 5 hours, and then cooling to room temperature in water; (4) preserving heat at 300-400 ℃ for 60-80 min, and then performing hot forging deformation at 300-400 ℃; (5) keeping the temperature at 150 ℃ for 30min, and then carrying out reverse hot extrusion deformation at 150 ℃. The Zn-Mg-Mn alloy disclosed by the invention is excellent in mechanical property and uniform in tissue components, and can be used for preparing biodegradable cardiovascular stents.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a zinc alloy material for a degradable cardiovascular stent and a preparation method thereof.
Background
The zinc alloy has a suitable degradation rate and good biocompatibility, and is the leading and research hot spot of the current biodegradable stent material. One important limitation of zinc alloy as a stent material is that it has low strength and plasticity, which is not sufficient to meet the requirements of use. One of the most effective methods for improving the mechanical properties of metals is to add alloying elements to the metal matrix. By means of solid solution strengthening and second phase strengthening, the chemical components and microstructure of zinc base alloy are changed to raise its mechanical performance, so that zinc base alloy meeting the use requirement is developed.
However, with the addition of alloying elements, problems with homogeneity of the alloy structure also follow. Galvanic corrosion will occur due to the presence of the second phase, thereby affecting the degradation uniformity thereof. The above problems are also present in the current studies on Zn-Mn-Li alloys (CN201810517961.8), Zn-Mg-Sr alloys and Zn-Mg-Zr alloys (CN 201911133161.7).
The present invention addresses the above problems by, on the one hand, using high purity metals as raw materials to reduce uneven degradation due to impurities. On the other hand, the component uniformity of the alloy material is ensured by microalloying and then a secondary magnetic suspension smelting technology and a homogenization treatment method, and the uniformity of alloy degradation is ensured from the perspective of alloy design. Then, the mechanical property of the material is improved by combining the free forging process and the reverse hot extrusion process. Finally, the Zn-Mg-Mn alloy material with uniform tissue and components and mechanical properties meeting the use requirements of the stent material is prepared, and the obtained alloy can be used for preparing the biodegradable cardiovascular stent.
Disclosure of Invention
The invention aims to provide a preparation process of a zinc-magnesium-manganese alloy, which aims to solve the problems that the structure and the components of the conventional zinc alloy are not uniform, and the mechanical property cannot meet the use requirement of medical metal.
The zinc-magnesium-manganese alloy comprises, by weight, 0.03-0.07% of Mg, 0.03-0.07% of Mn, less than or equal to 10ppm of unavoidable impurities, and the balance of Zn. The used raw material metals are composed of zinc blocks with the purity of 99.995 percent, magnesium blocks with the purity of 99.995 percent, Mn blocks with the purity of 99.995 percent,
the tensile strength of the zinc-magnesium-manganese alloy is 340-400 MPa, the tensile yield strength is 280-330 MPa, and the elongation is 20-40%.
The preparation method of the zinc-magnesium-manganese alloy comprises the following steps:
(1) preparing metal zinc, metal magnesium, metal manganese and phosphorus as raw materials according to the zinc alloy components, and smelting; firstly, heating metal zinc, adding metal magnesium, metal manganese and phosphorus in sequence after the metal zinc is melted, and stirring uniformly after the metal zinc is completely melted; cooling to 550 +/-5 ℃, introducing hexachloroethane into the molten metal by using a graphite bell jar to fully contact the molten metal, and standing for 15-20 min at the temperature of 550 +/-5 ℃; cooling the molten metal, casting into a water-cooling iron mold, and cooling to obtain a cast ingot;
(2) and (3) secondary magnetic suspension smelting: carrying out secondary magnetic suspension smelting on the cast ingot to ensure that the components and the structure of the cast ingot are uniform;
(3) homogenizing: keeping the temperature of the cast ingot at 350 +/-10 ℃ for 5 hours, then heating to 370 +/-10 ℃ and keeping the temperature for 5 hours, and then cooling to room temperature in water to obtain an ingot blank;
(4) hot forging deformation: keeping the temperature of the ingot blank at 300-400 ℃ for 60-80 min, and then performing hot forging deformation at 300-400 ℃;
(5) hot extrusion deformation: preserving the heat of the cylindrical ingot blank at 150 ℃ for 30min, and then carrying out reverse hot extrusion deformation at 150 ℃, wherein the extrusion speed is 0.5-3 mm/s, and the extrusion ratio is 4-25;
heating the zinc metal to 600 + -5 deg.C as described in step 1 above.
And (3) cooling the molten metal in the step 1 to 500 +/-10 ℃.
The uniformity deviation of the zinc alloy after magnetic suspension smelting in the step 2 is less than +/-0.02 wt%.
The thermal deformation alloy prepared by the method has the tensile strength of 340-400 MPa, the tensile yield strength of 280-330 MPa and the elongation of 20-40%.
The zinc alloy material of the degradable cardiovascular stent is measured to have a corrosion rate of 0.05-0.12 mm/year in SBF solution at 37 ℃ by adopting a weight loss method.
Has the advantages that:
(1) the invention ensures the component uniformity of the alloy material by the secondary magnetic suspension smelting technology and the homogenization treatment method, thereby effectively weakening the galvanic corrosion generated between the second phase and the magnesium matrix and improving the degradation uniformity of the material.
(2) The invention can further evenly refine the structure of the alloy material through the free forging process and the reverse hot extrusion process, and the grain refinement can simultaneously improve the strength, the plasticity and the corrosion resistance of the zinc alloy.
(3) The zinc alloy of the invention selects magnesium and manganese which are necessary for human metabolism, and improves the biocompatibility of the alloy. Meanwhile, the zinc alloy has good bactericidal effect, can reduce the risk of infection after operation, and reduces worry and pain of patients.
Drawings
FIG. 1 is a schematic view of a sampling site for compositional analysis of a cross-section of an ingot;
FIG. 2 is a stress-strain plot of three room temperature tensile tests of the zinc alloy of example 1;
FIG. 3 is a microstructure morphology and grain size distribution plot of the zinc alloy of example 1;
FIG. 4 is a graph of corrosion rate versus immersion time for the zinc alloy of example 1.
Detailed Description
Example 1
The zinc-magnesium-manganese alloy comprises 0.03 percent of Mg, 0.03 percent of Mn, less than or equal to 10ppm of unavoidable impurities and the balance of Zn according to weight percentage.
(1) Preparing metal zinc, metal magnesium, metal manganese and phosphorus as raw materials for smelting, heating the metal zinc to 600 +/-5 ℃, sequentially adding the metal magnesium, the metal manganese and the phosphorus (the boiling point is 350 ℃) after the metal zinc is molten, and uniformly stirring after the metal zinc, the metal manganese and the phosphorus are completely molten. Cooling to 550 +/-5 ℃, introducing hexachloroethane into the molten metal by using a graphite bell jar to fully contact the molten metal, and standing for 15-20 min at the temperature of 550 +/-5 ℃; cooling the molten metal to 500 +/-10 ℃, and casting the molten metal into a water-cooling iron mold for cooling to obtain a cast ingot;
(2) and (3) secondary magnetic suspension smelting: carrying out secondary magnetic suspension smelting on the cast ingot to ensure that the component uniformity deviation is less than +/-0.02 wt% and the structure is uniform;
(3) homogenizing: keeping the temperature of the cast ingot at 350 +/-10 ℃ for 5 hours, then heating to 370 +/-10 ℃ and keeping the temperature for 5 hours, and then cooling to room temperature in water to obtain an ingot blank;
(4) hot forging deformation: keeping the temperature of the ingot blank at 300-400 ℃ for 60-80 min, and then performing hot forging deformation at 300-400 ℃;
(5) hot extrusion deformation: preserving the heat of the cylindrical ingot blank at 150 ℃ for 30min, and then carrying out reverse hot extrusion deformation at 150 ℃, wherein the extrusion speed is 0.5-3 mm/s, and the extrusion ratio is 4-25;
finally obtaining the zinc-magnesium-manganese alloy with mechanical properties meeting the use requirements of medical metals. The yield strength of the obtained bar is 328MPa, the tensile strength is 398MPa, and the elongation is 22%; the crystal grains of the alloy are uniform and fine, and the average crystal grain size is only 1.26 mu m; the corrosion rate of the alloy is 0.05mm/year by adopting a weight loss method and measured in SBF solution at 37 ℃. Table 1 shows the results of the measurement of the components at different positions on the cross-section of the top, middle and bottom of the zinc alloy ingot.
TABLE 1
Example 2
The zinc-magnesium-manganese alloy comprises, by weight, 0.05% of Mg, 0.05% of Mn, less than or equal to 10ppm of unavoidable impurities, and the balance of Zn.
(1) Preparing metal zinc, metal magnesium, metal manganese and phosphorus as raw materials for smelting, heating the metal zinc to 600 +/-5 ℃, sequentially adding the metal magnesium, the metal manganese and the phosphorus (the boiling point is 350 ℃) after the metal zinc is molten, and uniformly stirring after the metal zinc, the metal manganese and the phosphorus are completely molten. Cooling to 550 +/-5 ℃, introducing hexachloroethane into the molten metal by using a graphite bell jar to fully contact the molten metal, and standing for 15-20 min at the temperature of 550 +/-5 ℃; cooling the molten metal to 500 +/-10 ℃, and casting the molten metal into a water-cooling iron mold for cooling to obtain a cast ingot;
(2) and (3) secondary magnetic suspension smelting: carrying out secondary magnetic suspension smelting on the cast ingot to ensure that the component uniformity deviation is less than +/-0.02 wt% and the structure is uniform;
(3) homogenizing: keeping the temperature of the cast ingot at 350 +/-10 ℃ for 5 hours, then heating to 370 +/-10 ℃ and keeping the temperature for 5 hours, and then cooling to room temperature in water to obtain an ingot blank;
(4) hot forging deformation: keeping the temperature of the ingot blank at 300-400 ℃ for 60-80 min, and then performing hot forging deformation at 300-400 ℃;
(5) hot extrusion deformation: preserving the heat of the cylindrical ingot blank at 150 ℃ for 30min, and then carrying out reverse hot extrusion deformation at 150 ℃, wherein the extrusion speed is 0.5-3 mm/s, and the extrusion ratio is 4-25;
finally obtaining the zinc-magnesium-manganese alloy with mechanical properties meeting the use requirements of medical metals. The yield strength of the obtained bar is 309MPa, the tensile strength is 361MPa, and the elongation is 34%; the corrosion rate of the alloy is 0.08mm/year by adopting a weight loss method and being measured in SBF solution at 37 ℃.
Example 3
The zinc-magnesium-manganese alloy comprises 0.07 percent of Mg, 0.07 percent of Mn, less than or equal to 10ppm of unavoidable impurities and the balance of Zn according to weight percentage.
(1) Preparing metal zinc, metal magnesium, metal manganese and phosphorus as raw materials for smelting, heating the metal zinc to 600 +/-5 ℃, sequentially adding the metal magnesium, the metal manganese and the phosphorus (the boiling point is 350 ℃) after the metal zinc is molten, and uniformly stirring after the metal zinc, the metal manganese and the phosphorus are completely molten. Cooling to 550 +/-5 ℃, introducing hexachloroethane into the molten metal by using a graphite bell jar to fully contact the molten metal, and standing for 15-20 min at the temperature of 550 +/-5 ℃; cooling the molten metal to 500 +/-10 ℃, and casting the molten metal into a water-cooling iron mold for cooling to obtain a cast ingot;
(2) and (3) secondary magnetic suspension smelting: carrying out secondary magnetic suspension smelting on the cast ingot to ensure that the component uniformity deviation is less than +/-0.02 wt% and the structure is uniform;
(3) homogenizing: keeping the temperature of the cast ingot at 350 +/-10 ℃ for 5 hours, then heating to 370 +/-10 ℃ and keeping the temperature for 5 hours, and then cooling to room temperature in water to obtain an ingot blank;
(4) hot forging deformation: keeping the temperature of the ingot blank at 300-400 ℃ for 60-80 min, and then performing hot forging deformation at 300-400 ℃;
(5) hot extrusion deformation: preserving the heat of the cylindrical ingot blank at 150 ℃ for 30min, and then carrying out reverse hot extrusion deformation at 150 ℃, wherein the extrusion speed is 0.5-3 mm/s, and the extrusion ratio is 4-25;
finally obtaining the zinc-magnesium-manganese alloy with mechanical properties meeting the use requirements of medical metals. The yield strength of the obtained bar is 282MPa, the tensile strength is 341MPa, and the elongation is 40%; the corrosion rate of the alloy is 0.12mm/year by adopting a weight loss method and measured in SBF solution at 37 ℃.
Claims (8)
1. The zinc alloy material for the degradable cardiovascular stent is characterized by comprising 0.03-0.07% of Mg, 0.03-0.07% of Mn and the balance of Zn by weight percent.
2. The zinc alloy material for degradable cardiovascular stents according to claim 1, wherein the unavoidable impurities in the zinc alloy are less than or equal to 10 ppm.
3. The preparation method of the zinc alloy material for the degradable cardiovascular stent in claim 1 is characterized by comprising the following steps:
(1) preparing metal zinc, metal magnesium, metal manganese and phosphorus as raw materials according to the zinc alloy components, and smelting; firstly, heating metal zinc, adding metal magnesium, metal manganese and phosphorus in sequence after the metal zinc is melted, and stirring uniformly after the metal zinc is completely melted; cooling to 550 +/-5 ℃, introducing hexachloroethane into the molten metal by using a graphite bell jar to fully contact the molten metal, and standing for 15-20 min at the temperature of 550 +/-5 ℃; cooling the molten metal, casting into a water-cooling iron mold, and cooling to obtain a cast ingot;
(2) and (3) secondary magnetic suspension smelting: carrying out secondary magnetic suspension smelting on the cast ingot to ensure that the components and the structure of the cast ingot are uniform;
(3) homogenizing: keeping the temperature of the cast ingot at 350 +/-10 ℃ for 5 hours, then heating to 370 +/-10 ℃ and keeping the temperature for 5 hours, and then cooling to room temperature in water to obtain an ingot blank;
(4) hot forging deformation: keeping the temperature of the ingot blank at 300-400 ℃ for 60-80 min, and then performing hot forging deformation at 300-400 ℃;
(5) hot extrusion deformation: and (3) preserving the heat of the cylindrical ingot blank at 150 ℃ for 30min, and then carrying out reverse hot extrusion deformation at 150 ℃, wherein the extrusion speed is 0.5-3 mm/s, and the extrusion ratio is 4-25.
4. The method for preparing the zinc alloy material for the degradable cardiovascular stent according to claim 2, wherein the metal zinc is heated to 600 ± 5 ℃.
5. The method for preparing the zinc alloy material for the degradable cardiovascular stent according to claim 2, wherein the temperature of the molten metal is reduced to 500 ± 10 ℃.
6. The method for preparing the zinc alloy material for the degradable cardiovascular stent according to claim 2, wherein the uniformity deviation of the zinc alloy after magnetic suspension smelting is less than +/-0.02 wt.%.
7. The preparation method of the zinc alloy material for the degradable cardiovascular stent according to claim 2, wherein the thermal deformation alloy has a tensile strength of 340-400 MPa, a tensile yield strength of 280-330 MPa, and an elongation of 20-40%.
8. The preparation method of the zinc alloy material for the degradable cardiovascular stent according to claim 2, wherein the corrosion rate of the zinc alloy material for the degradable cardiovascular stent is 0.05-0.12 mm/year measured in SBF solution at 37 ℃ by a weight loss method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115029584A (en) * | 2022-04-28 | 2022-09-09 | 东北大学 | Biodegradable medical zinc alloy and preparation method and application thereof |
| CN115029583A (en) * | 2022-04-28 | 2022-09-09 | 东北大学 | Medical degradable zinc alloy and preparation method of thin-wall microtube thereof |
| CN118218613A (en) * | 2024-05-22 | 2024-06-21 | 北京科技大学 | Degradable high-strength high-tensile plastic Zn-Mn-Mg alloy, preparation method and application |
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