CN117564234B - Degradable biomedical magnesium alloy wire and preparation method thereof - Google Patents
Degradable biomedical magnesium alloy wire and preparation method thereof Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000001125 extrusion Methods 0.000 claims abstract description 46
- 238000010438 heat treatment Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 33
- 230000032683 aging Effects 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 238000003723 Smelting Methods 0.000 claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 23
- 238000005266 casting Methods 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 238000000265 homogenisation Methods 0.000 claims abstract description 8
- 238000003754 machining Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 15
- 239000011777 magnesium Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 7
- 239000007769 metal material Substances 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 18
- 239000000956 alloy Substances 0.000 description 18
- 230000003247 decreasing effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 239000007943 implant Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 229910000882 Ca alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/005—Continuous casting of metals, i.e. casting in indefinite lengths of wire
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/06—At least partially resorbable materials
-
- 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
- A61L31/148—Materials at least partially resorbable by the body
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
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- 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
-
- 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
- C22F1/06—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
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Abstract
The invention discloses a degradable biomedical magnesium alloy wire and a preparation method thereof, belonging to the technical field of metal materials. The preparation method of the degradable biomedical magnesium alloy wire comprises the following steps: preparing raw materials, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of argon gas for smelting, and forming into cast ingots under a matched casting machine; homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, and placing the ingot into a homogenizing heat treatment furnace; extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment in an extruder for extrusion processing; primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace; and (5) spinning and forming: and (3) melting and spinning the magnesium alloy bar sample obtained by extrusion molding. According to the invention, the diameter refinement of the magnesium alloy wire is realized by utilizing the extrusion and wire throwing processes, the mechanical property of the magnesium alloy wire is improved, the repeated processing in the drawing process is eliminated, and the processing process flow is shortened.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a degradable biomedical magnesium alloy wire and a preparation method thereof.
Background
At present, clinically common implants are mostly made of stainless steel, titanium alloy and the like, and the implants have the defects of large elastic modulus, nondegradability and the like. The degradable magnesium alloy has the advantages of excellent mechanical property, good biocompatibility and degradable absorption, and can be used as a medical implant. In recent years, research shows that the degradable magnesium alloy has potential application value in the fields of biomedical absorbable sutures and the like.
However, in the prior art, most of magnesium alloy filaments for medical application are obtained by adopting a process of combining extrusion and drawing, for example, the application number is 201410725691.1-a biomedical magnesium alloy and a preparation method and application of the biomedical magnesium alloy filaments, and the biomedical magnesium alloy prepared by the scheme contains 1-10% of rare earth elements Gd, so that the risk of toxicity hazard exists in the filaments, and the recovery of patients is not facilitated; the scheme uses a process of extrusion and drawing, wherein the drawing process has the problems that the wire is broken, the diameter of the wire cannot meet the micrometer level, and the performance of different positions on the magnesium alloy thin wire is different, and the drawing process also leads to long wire preparation period.
For this reason, there is a need to provide a degradable biomedical magnesium alloy wire and a preparation method thereof to solve the above problems.
Disclosure of Invention
The invention aims to provide a degradable biomedical magnesium alloy wire and a preparation method thereof, which ensure the use safety of the magnesium alloy wire, and the alloy diameter can be further reduced to be unequal from micrometers to millimeters through the optimization of a wire throwing process technology, so that the magnesium alloy wire with degradability and excellent strength and plasticity is obtained, and the magnesium alloy wire is deeply used in medical application in the fields of degradable magnesium alloy suture lines or stents and the like, and the preparation period is shortened.
In order to achieve the above object, the following technical scheme is provided:
The preparation method of the degradable biomedical magnesium alloy wire comprises the following steps:
S1, smelting and casting: preparing raw materials, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of argon gas for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, and placing the ingot into a homogenizing heat treatment furnace;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment in an extruder for extrusion processing;
s4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace;
s5, spinning and forming: and (3) melting and spinning the magnesium alloy bar sample obtained by extrusion molding.
As an alternative to the preparation method of the degradable biomedical magnesium alloy wire, the preparation method of the degradable biomedical magnesium alloy wire further comprises the following steps: step S6, secondary aging treatment: and (5) putting the wire material formed by throwing the wire into a heat treatment furnace.
As an alternative to the preparation method of the degradable biomedical magnesium alloy wire, in the step S6, aging is performed for 24 hours at 150 ℃, and then cooling to room temperature with a furnace.
As an alternative scheme of the preparation method of the degradable biomedical magnesium alloy wire, in the step S1, mg-Zn-Mn is taken as a matrix, and 0.1-0.5% of Ca element is added for preparing raw materials.
As an alternative scheme of the preparation method of the degradable biomedical magnesium alloy wire, the preparation raw materials are prepared according to the content ratio of Zn6%, mn1%, ca0.1% -0.5% and the balance Mg.
As an alternative scheme of the preparation method of the degradable biomedical magnesium alloy wire, in the step S2, a proper amount of protective material is put into a homogenizing heat treatment furnace, and is subjected to homogenizing heat treatment for 24 hours at 300 ℃, and then air cooling is carried out until the room temperature is reached.
As an alternative scheme of the preparation method of the degradable biomedical magnesium alloy wire, in the step S3, the extrusion temperature is 300-400 ℃, the extrusion speed is 1-5 mm/S, and the deformation is 80%.
As an alternative to the preparation method of the degradable biomedical magnesium alloy wire, in the step S4, aging is performed for 24 hours at 150 ℃, and then cooling to room temperature with a furnace.
As an alternative scheme of the preparation method of the degradable biomedical magnesium alloy wire, in the step S5, the wire rotation speed of the wire throwing device is set to be 5m/S-15m/S, and the wire with the diameter smaller than 1mm is obtained through quenching.
The degradable biomedical magnesium alloy wire is prepared by the preparation method according to any one of the above.
Compared with the prior art, the invention has the beneficial effects that:
According to the preparation method of the degradable biomedical magnesium alloy wire, the magnesium alloy bar sample obtained by extrusion molding is subjected to melting wire throwing in a wire throwing molding mode. The centrifugal acting force is used for leading the element distribution inside the magnesium alloy bar sample to be more uniform in the process of throwing wires, thereby being beneficial to reducing the performance difference of different positions on the magnesium alloy wire.
The invention prepares the Mg-Zn-Mn-Ca alloy wire with micron-sized diameter by adopting the process technology of extrusion and wire throwing. Each element in the adopted alloy has good biocompatibility, and compared with the alloy type added with rare earth elements, the harm of material toxicity is better avoided; the excellent mechanical property of the wire is closely related to the wire throwing process parameters, the wire is finer as the wire throwing speed is higher, and the strength is higher, so that the strengthening effect is achieved due to the fact that the grain refinement is realized in the wire throwing process. Note that the spin rate parameter should not be too high, which instead causes coarsening and non-uniformity of the grains, and the mechanical properties of the performance are poor.
By changing the components and the preparation process of the magnesium alloy, the mechanical property and the corrosion resistance of the magnesium alloy are effectively regulated and controlled. The degradable biomedical Mg-Zn-Mn-Ca alloy is prepared by adopting Mg-Zn-Mn as a matrix and adding Ca element, and the alloy has excellent mechanical properties and good biocompatibility by adjusting the content of Ca element, so that the alloy can be better applied to the medical field. The content of Ca is 0.1-0.5%, and Ca element exists in the form of a second phase in the alloy, so that the mechanical property of the alloy is improved. By regulating and controlling the content of Ca element, the elongation at break of the alloy can reach 20% under optimal solution, and the alloy has good biocompatibility.
In addition, compared with the combination of the extrusion and the wire throwing process, the wire throwing process can widen the processed preparation range of the diameter of the magnesium alloy wire, can realize the preparation of the wire with good uniformity and has a diameter of micrometers to millimeters, and the practical application range of the magnesium alloy wire is enlarged. In the actual preparation process, the preparation period of the magnesium alloy wire can be shortened by adjusting the wire throwing speed according to the requirement, the phenomenon that the magnesium alloy wire is pulled apart in the drawing process is avoided, the process flow is simplified, and the mass production of the magnesium alloy wire is facilitated.
The degradable biomedical magnesium alloy wire provided by the invention realizes diameter refinement of the magnesium alloy wire by utilizing the extrusion and plastic deformation process of wire throwing, wherein the wire throwing speed range is 5m/s-15m/s, the mechanical property of the magnesium alloy wire is improved, the degradable biomedical magnesium alloy wire has a certain proper degradation speed, the multipass processing in the drawing process is eliminated, and the processing process flow is shortened. The strength of the alloy is improved and the plasticity is reduced due to the increase of the wire throwing speed, and a proper wire throwing process is selected according to the application field.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following description will briefly explain the drawings needed in the description of the embodiments of the present invention, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the contents of the embodiments of the present invention and these drawings without inventive effort for those skilled in the art.
FIG. 1 is a flow chart of a method for preparing a degradable biomedical magnesium alloy wire in an embodiment of the invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific direction, be configured and operated in a specific direction, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present invention, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed", "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected or integrally connected; either mechanically or electrically. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
In order to further reduce the alloy diameter to be different from micron to millimeter through optimizing the process technology of wire throwing, so as to obtain the magnesium alloy wire with degradability and excellent strength and plasticity, the embodiment is deeply applied to medical fields such as degradable magnesium alloy suture lines or stents, and the like, and the specific content of the embodiment is described in detail below with reference to fig. 1.
Embodiment one:
The embodiment provides a preparation method of a degradable biomedical magnesium alloy wire, which comprises the following steps:
s1, smelting and casting: preparing raw materials according to the content ratio of Zn6%, mn1%, ca0.1% and the balance Mg, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of Ar gas for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, placing the ingot into a homogenizing heat treatment furnace, placing a proper amount of protective material into the furnace, homogenizing and heat treating for 24 hours at 300 ℃, and then air cooling to room temperature;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment into an extruder for extrusion processing, wherein the extrusion temperature is 300-400 ℃, the extrusion speed is 1-5 mm/s, and the deformation is 80%;
S4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace, aging for 24 hours at 150 ℃, and then cooling to room temperature along with the furnace;
S5, spinning and forming: melting and spinning the magnesium alloy bar sample obtained by extrusion molding, setting the wire rotation speed of a wire spinning device to be 5m/s, and obtaining a wire with the diameter of 70+/-4 mu m through quenching;
S6, secondary aging treatment: and (3) putting the wire material formed by the wire throwing into a heat treatment furnace, aging for 24 hours at 150 ℃, and cooling to room temperature along with the furnace.
Embodiment two:
The embodiment provides a preparation method of a degradable biomedical magnesium alloy wire, which comprises the following steps:
s1, smelting and casting: preparing raw materials according to the content ratio of Zn6%, mn1%, ca0.3% and the balance Mg, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of Ar gas for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, placing the ingot into a homogenizing heat treatment furnace, placing a proper amount of protective material into the furnace, homogenizing and heat treating for 24 hours at 300 ℃, and then air cooling to room temperature;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment into an extruder for extrusion processing, wherein the extrusion temperature is 300-400 ℃, the extrusion speed is 1-5 mm/s, and the deformation is 80%;
S4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace, aging for 24 hours at 150 ℃, and then cooling to room temperature along with the furnace;
S5, spinning and forming: melting and spinning the magnesium alloy bar sample obtained by extrusion molding, setting the wire rotation speed of a wire spinning device to be 5m/s, and obtaining a wire with the diameter of 70+/-4 mu m through quenching;
S6, secondary aging treatment: and (3) putting the wire material formed by the wire throwing into a heat treatment furnace, aging for 24 hours at 150 ℃, and cooling to room temperature along with the furnace.
Embodiment III:
The embodiment provides a preparation method of a degradable biomedical magnesium alloy wire, which comprises the following steps:
S1, smelting and casting: preparing raw materials according to the content ratio of Zn6%, mn1%, ca0.5% and the balance Mg, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of Ar gas for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, placing the ingot into a homogenizing heat treatment furnace, placing a proper amount of protective material into the furnace, homogenizing and heat treating for 24 hours at 300 ℃, and then air cooling to room temperature;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment into an extruder for extrusion processing, wherein the extrusion temperature is 300-400 ℃, the extrusion speed is 1-5 mm/s, and the deformation is 80%;
S4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace, aging for 24 hours at 150 ℃, and then cooling to room temperature along with the furnace;
S5, spinning and forming: melting and spinning the magnesium alloy bar sample obtained by extrusion molding, setting the wire rotation speed of a wire spinning device to be 5m/s, and obtaining a wire with the diameter of 70+/-4 mu m through quenching;
S6, secondary aging treatment: and (3) putting the wire material formed by the wire throwing into a heat treatment furnace, aging for 24 hours at 150 ℃, and cooling to room temperature along with the furnace.
Example IV
The embodiment provides a preparation method of a degradable biomedical magnesium alloy wire, which comprises the following steps:
S1, smelting and casting: preparing raw materials according to the content ratio of Zn6%, mn1%, ca0.5% and the balance Mg, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of Ar gas for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, placing the ingot into a homogenizing heat treatment furnace, placing a proper amount of protective material into the furnace, homogenizing and heat treating for 24 hours at 300 ℃, and then air cooling to room temperature;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment into an extruder for extrusion processing, wherein the extrusion temperature is 300-400 ℃, the extrusion speed is 1-5 mm/s, and the deformation is 80%;
S4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace, aging for 24 hours at 150 ℃, and then cooling to room temperature along with the furnace;
S5, spinning and forming: melting and spinning the magnesium alloy bar sample obtained by extrusion molding, setting the wire rotation speed of a wire spinning device to be 10m/s, and obtaining a 65+/-5 mu m wire by quenching;
S6, secondary aging treatment: and (3) putting the wire material formed by the wire throwing into a heat treatment furnace, aging for 24 hours at 150 ℃, and cooling to room temperature along with the furnace.
Example five
The embodiment provides a preparation method of a degradable biomedical magnesium alloy wire, which comprises the following steps:
S1, smelting and casting: preparing raw materials according to the content ratio of Zn6%, mn1%, ca0.5% and the balance Mg, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of Ar gas for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, placing the ingot into a homogenizing heat treatment furnace, placing a proper amount of protective material into the furnace, homogenizing and heat treating for 24 hours at 300 ℃, and then air cooling to room temperature;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment into an extruder for extrusion processing, wherein the extrusion temperature is 300-400 ℃, the extrusion speed is 1-5 mm/s, and the deformation is 80%;
S4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace, aging for 24 hours at 150 ℃, and then cooling to room temperature along with the furnace;
s5, spinning and forming: melting and spinning the magnesium alloy bar sample obtained by extrusion molding, setting the wire rotation speed of a wire spinning device to be 15m/s, and obtaining a 61+/-3 mu m wire by quenching;
S6, secondary aging treatment: and (3) putting the wire material formed by the wire throwing into a heat treatment furnace, aging for 24 hours at 150 ℃, and cooling to room temperature along with the furnace.
TABLE 1 results of mechanical Properties test of alloys with different Ca contents
| Tensile strength/MPa | Yield strength/MPa | Elongation/% | |
| Example 1 | 350 | 242 | 24.3 |
| Example two | 320 | 254 | 22.6 |
| Example III | 300 | 260 | 20.1 |
The above table 1 shows experimental control groups with different Ca element content ratios, and the experimental control groups can be obtained by comparing the first embodiment, the second embodiment and the third embodiment: the content ratio of Ca element in the first, second and third embodiments is sequentially increased, the tensile strength of the magnesium alloy wire is sequentially decreased, the yield strength is sequentially increased, and the elongation is sequentially decreased.
TABLE 2 results of mechanical properties test of alloys at different wire-throwing rates
| Tensile strength/MPa | Yield strength/MPa | Elongation/% | Wire diameter/μm | |
| Example III | 300 | 260 | 20.1 | 70±4 |
| Example IV | 350 | 280 | 13.2 | 65±5 |
| Example five | 380 | 296 | 10.4 | 61±3 |
The experimental control groups with different wire rotation rates of the wire throwing device are shown in the table 2, and can be obtained by comparing the third embodiment, the fourth embodiment and the fifth embodiment: the wire-rotating speed of the wire-throwing device in the third embodiment, the fourth embodiment and the fifth embodiment is sequentially increased, the tensile strength of the magnesium alloy wire is sequentially increased, the yield strength is sequentially decreased, the elongation is sequentially decreased, and the diameter of the wire is sequentially decreased. The wire throwing process parameters can be adjusted according to the existing actual requirements to obtain wires with proper diameters for application in different medical aspects.
The embodiment also provides a degradable biomedical magnesium alloy wire, which is prepared by the preparation method of the degradable biomedical magnesium alloy wire. The diameter refinement of the magnesium alloy wire is realized by utilizing the plastic deformation process of extrusion and wire throwing, the mechanical property of the magnesium alloy wire is improved, the magnesium alloy wire has a certain proper degradation rate, the multipass processing in the drawing process is eliminated, and the processing process flow is shortened. The strength of the alloy is improved and the plasticity is reduced due to the increase of the wire throwing speed, and a proper wire throwing process is selected according to the application field. The content of Ca is 0.1-0.5%, and Ca element exists in the form of a second phase in the alloy, so that the mechanical property of the alloy is improved. By regulating and controlling the content of Ca element, the elongation at break of the alloy can reach 20% under optimal solution, and the alloy has good biocompatibility.
Note that the above is only a preferred embodiment of the present invention and the technical principle applied. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, while the invention has been described in connection with the above embodiments, the invention is not limited to the embodiments, but may be embodied in many other equivalent forms without departing from the spirit or scope of the invention, which is set forth in the following claims.
Claims (8)
1. The preparation method of the degradable biomedical magnesium alloy wire is characterized by comprising the following steps:
s1, smelting and casting: taking Mg-Zn-Mn as a matrix, adding 0.1-0.5% of Ca element to prepare raw materials, mixing the raw materials, placing the raw materials in a vacuum smelting furnace under the protection of argon for smelting, and forming into cast ingots under a matched casting machine;
S2, homogenizing heat treatment: machining a magnesium alloy ingot into a required shape and size, and placing the ingot into a homogenizing heat treatment furnace;
S3, extrusion molding: placing the magnesium alloy cast ingot subjected to homogenization heat treatment in an extruder for extrusion processing;
s4, primary aging treatment: placing the extruded magnesium alloy bar into a heat treatment furnace;
s5, spinning and forming: and (3) melting and spinning the magnesium alloy bar sample obtained by extrusion molding, wherein the wire-spinning speed of a wire-spinning device is set to be 5-15 m/s, and the wire with the diameter smaller than 1mm is obtained by quenching.
2. The method for preparing the degradable biomedical magnesium alloy wire according to claim 1, further comprising:
step S6, secondary aging treatment: and (5) putting the wire material formed by throwing the wire into a heat treatment furnace.
3. The method for preparing a degradable biomedical magnesium alloy wire according to claim 2, wherein in the step S6, the aging treatment is performed at 150 ℃ for 24 hours, and then the wire is cooled to room temperature in a furnace.
4. The method for preparing the degradable biomedical magnesium alloy wire according to claim 1, wherein the raw materials are prepared according to the content ratio of Zn6%, mn1%, ca0.1% -0.5% and the balance Mg.
5. The method for preparing a degradable biomedical magnesium alloy wire according to claim 1, wherein in the step S2, a proper amount of protective material is placed in a homogenizing heat treatment furnace, and the homogenizing heat treatment is performed for 24 hours at 300 ℃, and then the air cooling is performed until the room temperature.
6. The method for preparing a degradable biomedical magnesium alloy wire according to claim 1, wherein in the step S3, the extrusion temperature is 300 ℃ to 400 ℃, the extrusion speed is 1mm/S to 5mm/S, and the deformation amount is 80%.
7. The method for preparing a degradable biomedical magnesium alloy wire according to claim 1, wherein in the step S4, the aging treatment is performed at 150 ℃ for 24 hours, and then the wire is cooled to room temperature in a furnace.
8. A degradable biomedical magnesium alloy wire, which is characterized by being prepared by the preparation method of any one of claims 1-7.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5329231A (en) * | 1976-08-31 | 1978-03-18 | Hitachi Cable | Method and device for continuous casting extrusion |
| US4649983A (en) * | 1983-10-26 | 1987-03-17 | Allied Corporation | Chill roll casting of metal strip |
| CN103785801A (en) * | 2014-01-16 | 2014-05-14 | 燕山大学 | Device for producing magnesium alloy cellosilk |
| CN109972007A (en) * | 2019-03-20 | 2019-07-05 | 北京科技大学 | A kind of anastomosis staple material and preparation method thereof of biology degradable in vivo Mg-Zn-Ca-M |
| CN116005023A (en) * | 2022-11-11 | 2023-04-25 | 西安交通大学 | Biomedical magnesium alloy wire for 3D printing and preparation method thereof |
| CN116099031A (en) * | 2023-01-19 | 2023-05-12 | 北京科技大学 | Degradable and absorbable magnesium alloy suture line and preparation method and application thereof |
| CN116197370A (en) * | 2023-02-20 | 2023-06-02 | 哈尔滨工业大学 | Device and method for rapidly preparing magnesium and magnesium alloy micron-sized wire |
-
2024
- 2024-01-15 CN CN202410051981.6A patent/CN117564234B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5329231A (en) * | 1976-08-31 | 1978-03-18 | Hitachi Cable | Method and device for continuous casting extrusion |
| US4649983A (en) * | 1983-10-26 | 1987-03-17 | Allied Corporation | Chill roll casting of metal strip |
| CN103785801A (en) * | 2014-01-16 | 2014-05-14 | 燕山大学 | Device for producing magnesium alloy cellosilk |
| CN109972007A (en) * | 2019-03-20 | 2019-07-05 | 北京科技大学 | A kind of anastomosis staple material and preparation method thereof of biology degradable in vivo Mg-Zn-Ca-M |
| CN116005023A (en) * | 2022-11-11 | 2023-04-25 | 西安交通大学 | Biomedical magnesium alloy wire for 3D printing and preparation method thereof |
| CN116099031A (en) * | 2023-01-19 | 2023-05-12 | 北京科技大学 | Degradable and absorbable magnesium alloy suture line and preparation method and application thereof |
| CN116197370A (en) * | 2023-02-20 | 2023-06-02 | 哈尔滨工业大学 | Device and method for rapidly preparing magnesium and magnesium alloy micron-sized wire |
Non-Patent Citations (1)
| Title |
|---|
| 高性能镁合金丝的制备及其弯曲性能研究;郭学锋 等;中国稀土学报;20110615(第03期);第259-265页 * |
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