CN111228577A - Medical magnesium alloy capable of being degraded in short term and preparation method thereof - Google Patents
Medical magnesium alloy capable of being degraded in short term and preparation method thereof Download PDFInfo
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- CN111228577A CN111228577A CN202010041263.2A CN202010041263A CN111228577A CN 111228577 A CN111228577 A CN 111228577A CN 202010041263 A CN202010041263 A CN 202010041263A CN 111228577 A CN111228577 A CN 111228577A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
The invention discloses a medical magnesium alloy capable of being degraded in a short term and a preparation method thereof, wherein the mass percent of each element in the alloy is as follows: 2 to 6 percent of Zn, 0.5 to 4 percent of Ca, 0.01 to 0.09 percent of Fe, 0.1 to 0.7 percent of Zr, 0.1 to 0.7 percent of Nd, and the balance of Mg and other impurity elements. The elements added in the invention have good biocompatibility, and the degraded product can not cause harm to human body. The magnesium alloy material which can be degraded in a short period in a human body is obtained by controlling the mechanical property and the degradation rate of the alloy by regulating the content of each element.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy materials, and particularly relates to a medical magnesium alloy capable of being degraded in a short term and a preparation method thereof.
Background
In recent years, intrauterine stents are placed in the uterus after the intrauterine adhesion decomposition to prevent re-adhesion, so that the intrauterine stent has a better effect. At present, the main materials clinically applied to the intrauterine stent are metal copper and the like, but the copper cannot be degraded, and needs to be taken out after a secondary operation after the function of human tissues is recovered for a period of time and the like in the uterine cavity, and the copper exists in the body for a long time and is easy to cause seroma, foreign body reaction and the like. The secondary operation not only increases medical costs but also causes great physical pain and mental stress to patients. In view of the above, a uterine cavity stent material which has biocompatibility and can automatically diminish inflammation, resist bacteria, degrade, absorb or fall off in a short-term contraception (3 months to one year) under a human body environment is developed, so that side effects caused by placing other contraceptive rings, harm to a body caused by long-term taking of contraceptives and the like are reduced.
Magnesium alloy has recently received wide attention from the medical materials community as a novel degradable medical metal material. Compared with the traditional medical metal materials (stainless steel, titanium alloy and cobalt-chromium alloy), the magnesium alloy as the medical metal material has the following advantages: 1. good biocompatibility, no toxicity, degradability in human body, and no harm to the degradation product. 2. Has higher specific strength and specific rigidity and good processing performance, and can meet the requirements of medical implant materials. 3. Rich resources and low price.
Disclosure of Invention
The invention aims to provide a medical magnesium alloy capable of being degraded in a short term and a preparation method thereof, and aims to overcome the defects that the strength and toughness are not high and the degradation rate is uncontrollable in the conventional medical magnesium alloy.
The invention is realized by the following technical scheme: the short-term degradable medical magnesium alloy comprises the following chemical components in percentage by weight: 2 to 6 percent of Zn, 0.5 to 4 percent of Ca, 0.01 to 0.09 percent of Fe, 0.1 to 0.7 percent of Zr, 0.1 to 0.7 percent of Nd, and the balance of Mg and other impurity elements.
Wherein, the impurity element is inevitable impurity element brought in during the smelting and forming process of the alloy, and preferably, the content of the impurity element is less than 0.05 percent.
Wherein Zn is essential trace element, and has zinc and more than seventy enzymes activated by zinc, and can promote skin and skeleton development, and maintain digestion and metabolism. In addition, the existence of Zn can also play a role in refining grains of the magnesium alloy, thereby improving the strength and toughness of the alloy. The existence of Zn element can also accelerate the formation of passive film on the surface of the alloy, and has great effect on improving the corrosion resistance of the alloy. The main function of Ca element is to strengthen the alloy by solid solution, the maximum solubility of Ca in Mg is 1.34wt%, and in magnesium alloy, the strength and elongation of the alloy are increased along with the increase of Ca content. The main existing form of Ca in magnesium alloy is Mg2Ca phase, Mg2The presence of the Ca phase induces galvanic corrosion and increases the degradation rate of the magnesium alloy. Meanwhile, Ca is also one of elements that are beneficial to the human body, and is one of elements essential to the human skeleton. The Fe element and the Zr element have low solubility in magnesium, cannot form an intermediate phase with the magnesium, mainly exist in the magnesium alloy in the form of mass points, and play a role in precipitation strengthening of the alloy. Fe is one of elements necessary for human body, and the addition of Fe element in magnesium alloy has great effect on improving the degradation rate of magnesium alloy. Nd element is a common rare earth element with low toxicity, and Nd salt is commonly used as an anticancer drug in medicine. The Nd element can play an alloying role on the magnesium alloy, refine the crystal grains of the alloy and play an important role in improving the strength and the elongation of the alloy. The degradation rate of the magnesium alloy in practical application is controlled mainly by regulating the contents of Zn element, Ca element and Fe element; the mechanical property requirement of the alloy in application can be met by regulating the content of each element.
Preferably, the Zr element and the Nd element in the invention are added in the form of an intermediate alloy, and the intermediate alloy refers to Mg-30% Zr intermediate alloy and Mg-30% Nd intermediate alloy.
The invention provides a medical magnesium alloy capable of being degraded in a short term, which comprises the following specific preparation steps:
(1) adding the pretreated pure Mg, pure Zn and Fe into a ceramic crucible, preheating to 100-180 ℃, and introducing SF into the ceramic crucible6Heating the crucible to 640-680 ℃ with mixed protective gas of Ar, and preserving heat for 30-45 minutes until the alloy is melted;
(2) heating to 760 ℃ of 720-;
(3) the magnesium alloy ingot obtained is subjected to solution treatment for 5 hours at 480 ℃ and then is quenched.
Compared with the prior art, the invention has the following advantages:
the Mg, Zn, Ca, Fe, Zr and Nd used in the invention have good biocompatibility, and the degraded products do not harm human bodies; the invention can well control the degradation rate of the alloy by regulating and controlling the content of each element, thereby better meeting the requirements in practical application. In addition, only trace rare earth elements are added, so that the cost of the alloy is reduced.
Detailed Description
The present invention will be described in detail with reference to embodiments, which are only used to further explain the present invention, but the scope of the present invention is not limited thereto.
The invention provides a medical magnesium alloy capable of being degraded in a short term, which comprises 2-6% of Zn, 0.5-4% of Ca, 0.01-0.09% of Fe, 0.1-0.7% of Zr, 0.1-0.7% of Nd, and the balance of Mg and other impurity elements. The tensile strength of the alloy obtained by regulating the content of each element in the alloy is more than 280MPa, and the corrosion rate in Hank's simulated body fluid at 37 ℃ is 0.25 mg-cm-2·day-1Left and right.
TABLE 1 Hank's chemical composition of simulated body fluids (g/L)
Embodiment 1
A medical magnesium alloy capable of being degraded in a short time comprises 2% of Zn, 0.5% of Ca, 0.01% of Fe, 0.7% of Zr, 0.7% of Nd, and the balance of Mg and other impurity elements.
The preparation method of the alloy comprises the following steps: firstly, adding pretreated pure Mg, pure Zn and Fe into a ceramic crucible, preheating to 100-180 ℃, and introducing SF into the ceramic crucible6Heating the crucible to 640-680 ℃ with mixed protective gas of Ar, and preserving heat for 30-45 minutes until the alloy is melted; heating to 720-760 ℃ at the heating rate of 10 ℃/min, adding Mg-20 percent of Ca, Mg-30 percent of Zr and Mg-30 percent of Nd intermediate alloy into a crucible, preserving heat for 25-40 min, casting into a preheated mold, and naturally cooling to room temperature; and machining the obtained magnesium alloy ingot to obtain the bracket.
Example II
A medical magnesium alloy capable of being degraded in a short time comprises 4% of Zn, 2% of Ca, 0.05% of Fe, 0.4% of Zr, 0.4% of Nd, and the balance of Mg and other impurity elements.
The preparation method of the alloy comprises the following steps: firstly, adding pretreated pure Mg, pure Zn and Fe into a ceramic crucible, preheating to 100-180 ℃, and introducing SF into the ceramic crucible6Heating the crucible to 640-680 ℃ with mixed protective gas of Ar, and preserving heat for 30-45 minutes until the alloy is melted; heating to 720-760 ℃ at the heating rate of 10 ℃/min, adding Mg-20 percent of Ca, Mg-30 percent of Zr and Mg-30 percent of Nd intermediate alloy into a crucible, preserving heat for 25-40 min, casting into a preheated mold, and naturally cooling to room temperature; carrying out solid solution treatment on the obtained magnesium alloy ingot for 5 hours at 480 ℃, and carrying out water quenching; and then, carrying out mechanical processing on the obtained magnesium alloy ingot to obtain the bracket.
Example three
A medical magnesium alloy capable of being degraded in a short time comprises 4% of Zn, 3% of Ca, 0.09% of Fe, 0.3% of Zr, 0.3% of Nd and the balance of Mg and other impurity elements.
The preparation method of the alloy comprises the following steps: firstly, adding pretreated pure Mg, pure Zn and Fe into a ceramic crucible, preheating to 100-180 DEG CSF is introduced into the ceramic crucible6Heating the crucible to 640-680 ℃ with mixed protective gas of Ar, and preserving heat for 30-45 minutes until the alloy is melted; heating to 720-760 ℃ at the heating rate of 10 ℃/min, adding Mg-20 percent of Ca, Mg-30 percent of Zr and Mg-30 percent of Nd intermediate alloy into a crucible, preserving heat for 25-40 min, casting into a preheated mold, and naturally cooling to room temperature; carrying out solid solution treatment on the obtained magnesium alloy ingot for 5 hours at 480 ℃, and carrying out water quenching; and then, carrying out mechanical processing on the obtained magnesium alloy ingot to obtain the bracket.
Example four
A medical magnesium alloy capable of being degraded in a short time comprises 6% of Zn, 4% of Ca, 0.09% of Fe, 0.1% of Zr, 0.1% of Nd, and the balance of Mg and other impurity elements.
The preparation method of the alloy comprises the following steps: firstly, adding pretreated pure Mg, pure Zn and Fe into a ceramic crucible, preheating to 100-180 ℃, and introducing SF into the ceramic crucible6Heating the crucible to 640-680 ℃ with mixed protective gas of Ar, and preserving heat for 30-45 minutes until the alloy is melted; heating to 720-760 ℃ at the heating rate of 10 ℃/min, adding Mg-20 percent of Ca, Mg-30 percent of Zr and Mg-30 percent of Nd intermediate alloy into a crucible, preserving heat for 25-40 min, casting into a preheated mold, and naturally cooling to room temperature; carrying out solid solution treatment on the obtained magnesium alloy ingot for 5 hours at 480 ℃, and carrying out water quenching; and then, carrying out mechanical processing on the obtained magnesium alloy ingot to obtain the bracket.
Table 2 shows the performance of each embodiment.
Table 2 tensile strength, yield strength, elongation and corrosion rate of the examples
Claims (2)
1. A medical magnesium alloy capable of being degraded in a short time is characterized in that: the alloy comprises the following elements in percentage by mass: 2 to 6 percent of Zn, 0.5 to 4 percent of Ca, 0.01 to 0.09 percent of Fe, 0.1 to 0.7 percent of Zr, 0.1 to 0.7 percent of Nd, and the balance of Mg and other impurity elements.
2. A medical magnesium alloy capable of being degraded in a short term is prepared by the following steps:
(1) adding the pretreated pure Mg, pure Zn and Fe into a ceramic crucible, preheating to 100-180 ℃, and introducing SF into the ceramic crucible6Heating the crucible to 640-680 ℃ with mixed protective gas of Ar, and preserving heat for 30-45 minutes until the alloy is melted;
(2) heating to 760 ℃ of 720-;
(3) the magnesium alloy ingot obtained is subjected to solution treatment for 5 hours at 480 ℃ and then is quenched.
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Application publication date: 20200605 |