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KR-102963242-B1 - Biodegradable magnesium alloy

KR102963242B1KR 102963242 B1KR102963242 B1KR 102963242B1KR-102963242-B1

Abstract

The present invention relates to a biodegradable alloy of formula (I): Mg-Zn-X, wherein X represents -Ca-Mn or -Dy-Sr, wherein Zn is about 0.1 wt% to about 3.0 wt%, Dy is about 0.1 wt% to about 0.7 wt%, Sr is about 0.1 wt% to about 0.9 wt%, Ca is about 0.1 wt% to about 1.5 wt%, Mn is about 0.1 wt% to about 0.9 wt%, and Mg constitutes the remainder together with impurities. The present invention further relates to a method for manufacturing an alloy, wherein the method comprises: (a) placing alloy components in a crucible, wherein the alloy components are placed in the crucible in a multilayer arrangement; (b) melting the alloy components at about 700 °C to about 850 °C; (c) a step of stirring the molten material of step (b) at about 400 rpm to about 500 rpm; (d) a step of spraying the molten material of step (c) into millimeter-sized droplets using an inert gas jet; and (e) a step of cooling and depositing the sprayed alloy molten material to obtain an ingot.

Inventors

  • 굽타 마노이
  • 파란드 구루라이
  • 마나카리 비야사라이 바다리나스
  • 웡 청 웬 레이몬드
  • 프라사드 소마순다람

Assignees

  • 내셔널 유니버시티 오브 싱가포르

Dates

Publication Date
20260508
Application Date
20201202
Priority Date
20191202

Claims (20)

  1. A method for manufacturing an alloy comprising the following steps: (a) a step of positioning alloy components in a crucible, wherein the alloy components are positioned in the crucible in a multilayer arrangement; (b) a step of melting the alloy components at 700 ℃ to 850 ℃; (c) a step of stirring the melt of step (b) at 400 rpm to 500 rpm; (d) a step of spraying the molten material of step (c) into millimeter-sized droplets using an inert gas jet; (e) A step of cooling and depositing the sprayed alloy melt to obtain an ingot.
  2. A method for manufacturing an alloy of formula (I) comprising the following steps: (a) a step of positioning alloy components in a crucible, wherein the alloy components are positioned in the crucible in a multilayer arrangement; (b) a step of melting the alloy components at 700 ℃ to 850 ℃; (c) a step of stirring the melt of step (b) at 400 rpm to 500 rpm; (d) a step of spraying the molten material of step (c) into millimeter-sized droplets using an inert gas jet; (e) Step of cooling and depositing the sprayed alloy molten material to obtain an ingot: Mg-Zn-X chemical formula (I) In the above formula X represents -Ca-Mn or -Dy-Sr; Mg is magnesium, Zn is zinc, Dy is dysprosium, Sr is strontium, Ca is calcium, Mn is manganese; Herein, the alloy comprises the following based on total weight: 0.1 wt% to 3.0 wt% of Zn; 0.1 wt% to 0.7 wt% of Dy; 0.1 wt% to 0.9 wt% of Sr; 0.1 wt% to 1.5 wt% of Ca; 0.1 wt% to 0.9 wt% of Mn; and Remaining amount of Mg and impurities.
  3. In paragraph 2, A method comprising the step (a) of controlling the volume of the alloy component to 70% to 75% of the crucible volume.
  4. In paragraph 2, A method in which the multilayer array of step (a) comprises an ABA array, wherein A is composed of a first alloy component and B is composed of a second alloy component, wherein the first and second alloy components may each be composed of a single alloy material or a blended alloy mixture of two or more alloy materials.
  5. In paragraph 2, A method in which the multilayer array of step (a) comprises an ABABA array, wherein A is composed of a first alloy component and B is composed of a second alloy component, wherein the first and second alloy components may each be composed of a single alloy material or a blended alloy mixture of two or more alloy materials.
  6. In paragraph 4 or 5, A method in which A is composed of magnesium and B is composed of a blended alloy mixture of zinc and X.
  7. In paragraph 2, A method in which each layer of a multilayer array has substantially the same volume.
  8. In paragraph 2, A method comprising step (d) using 2 to 4 jets of inert gas.
  9. In paragraph 2, Method in which the inert gas of step (d) is argon.
  10. In paragraph 2, A method in which the diameter of each jet in step (d) is 1 mm to 2 mm.
  11. In paragraph 2, A method in which the gas flow rate in step (d) is 20 to 30 liters per minute.
  12. In paragraph 2, A method further comprising the step (f) of applying the ingot to hot extrusion at 250 ℃ to 400 ℃.
  13. In Paragraph 12, A method in which the extrusion rate range is 25:1 to 12:1.
  14. In paragraph 2, the method comprises the following based on the total weight of the alloy: 0.8 wt% to 1.6 wt% of Zn; 0.3 wt% to 0.9 wt% Ca; 0.1 wt% to 0.5 wt% of Mn; and Remaining amount of Mg and impurities.
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Description

Biodegradable magnesium alloy The present invention generally relates to biodegradable alloys. The present invention also relates to a method and technique for manufacturing said biodegradable alloys. Biodegradable alloys may be useful for orthopedic applications. Along with the global aging population, age-related orthopedic conditions, such as osteoporosis and fractures, are increasing dramatically. This has ultimately led to a heightened demand for effective and affordable orthopedic implants and devices. Research and development are underway to explore ideal orthopedic implant materials. Various factors (e.g., orthopedic application/field, function, fit, and cost) and material properties, such as chemical and biological inertness, strength, stiffness, corrosion resistance, stability, biocompatibility, and tissue acceptance, must be considered. Currently, orthopedic implants and devices are fabricated using polymer, ceramic, or metallic materials. Each of these possesses unique strengths and limitations. Metallic materials, such as stainless steel, platinum, titanium, and alloys like titanium and chromium-cobalt, are commonly used due to their superior strength and mechanical properties. However, these metallic implants are prone to bone misalignment and can cause loosening, ultimately leading to implant failure. Consequently, these metallic implants may need to be removed after serving their healing purpose due to potential recovery complications (e.g., allergies, infections, and sensitization). In the case of polymers, polyethylene and polymethyl methacrylate are some common examples used for orthopedic implants. However, due to their low strength and potential deformation, they are not suitable for heavy-duty orthopedic applications (e.g., bone healing). Ceramics, such as aluminum oxide, silicon oxide, zirconium oxide, and calcium phosphate, possess good mechanical properties and are chemically and biocompatible. However, they are brittle. The attached drawings serve to illustrate the disclosed embodiments and explain the principles of the disclosed embodiments. However, it should be understood that the drawings are intended for illustrative purposes only and are not intended to define the limitations of the invention.Fig. 1 Figure 1 shows the particle size morphology of the magnesium alloy of the present invention studied under an optical microscope. Fig. 2 Figure 2 shows an optical microscope image analysis of a magnesium alloy. Fig. 3 Figure 3 shows the corrosion rate of the magnesium alloy. Figures 4A and 4B Figure 4A shows scanning electron microscope (SEM) analysis of magnesium alloys Mg-Zn-xSr, Mg-Zn-xDy-ySr, Mg-Zn-xDy-xSr, and Mg-Zn-xDy-zSr after corrosion at the end of day 14. Figure 4B shows scanning electron microscope (SEM) analysis of magnesium alloys Mg-Zn-aCa, Mg-Zn-aCa-cMn, and Mg-Zn-aCa-dMn after corrosion at the end of day 14. Figures 5A and 5B Figure 5A shows the compressive properties of magnesium alloys Mg-Zn-xSr, Mg-Zn-xDy-ySr, Mg-Zn-xDy-xSr, and Mg-Zn-xDy-zSr. Figure 5B shows the compressive properties of magnesium alloys Mg-Zn-aCa, Mg-Zn-aCa-cMn, and Mg-Zn-aCa-dMn. Figures 6A and 6B Figure 6A shows the cell viability of MC3T3-E1 osteoblast progenitor cells as a percentage of the viability of cells cultured in a negative control after incubation in magnesium alloys Mg-Zn-ySr, Mg-Zn-xDy-xSr, and Mg-Zn-xDy-zSr for 1, 3, and 5 days. Figure 6B shows the magnesium alloy for 1, 3, and 5 days This shows the cell viability of MC3T3-E1 osteoblast progenitor cells as the percentage of viability of cells cultured in a negative control after incubation with Mg-Zn-aCa, Mg-Zn-aCa-cMn, and Mg-Zn-aCa-dMn. Fig. 7 Figure 7 is a cross-sectional schematic of a crucible showing a multilayer arrangement of alloy components. Figures 8A and 8B Fig. 8A shows fracture samples after compression of magnesium alloys Mg-Zn-xSr, Mg-Zn-xDy-ySr, Mg-Zn-xDy-xSr, and Mg-Zn-xDy-zSr. Fig. 8B shows fracture samples after compression of magnesium alloys Mg-Zn-aCa, Mg-Zn-aCa-cMn, and Mg-Zn-aCa-dMn. Specific description of the drawing Referring to Figures 4A and 4B, Figures 4A and 4B show scanning electron microscope (SEM) analysis of the magnesium alloy after corrosion at the end of day 14. The magnesium alloy exhibits crack formation due to moisture loss. The alloy surface is covered with a needle-like structure. The formation of hydrotalc compounds is enhanced with increasing immersion time of the magnesium alloy in Hank's balanced salt solution (HBSS). The scale of compound formation was more uniformly distributed within the alloy sample. This behavior may contribute to the retention of strength and ductility of the material after in vitro corrosion. Referring to Figures 5A and 5B, Figures 5A and 5B show the compressive characteristics of a magnesium alloy. Figures 5A and 5B show stress graphs or compression tests against strain of the magnesium alloy and provide a deeper understanding of the mechanical integrity of