CN105695787A - Preparation method of medical implantation magnesium alloy material - Google Patents
Preparation method of medical implantation magnesium alloy material Download PDFInfo
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- CN105695787A CN105695787A CN201610202083.1A CN201610202083A CN105695787A CN 105695787 A CN105695787 A CN 105695787A CN 201610202083 A CN201610202083 A CN 201610202083A CN 105695787 A CN105695787 A CN 105695787A
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- 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
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Abstract
The invention provides a preparation method of a medical implantation magnesium alloy material. Firstly, magnesium oxide, soybean lecithin and citric acid are added in KOH solution for heating, insulating and filtering; then, a solid is dried, and is uniformly mixed with glycerinum and water to obtain a first mixture; then, zinc powder and water are taken for mixing to obtain a second mixture; then, the first mixture and the second mixture are mixed and dried for ball milling to obtain prefabricated powder; and finally, the prefabricated powder, ethylidene distearamide, methyl methacrylate, sodium hydrogen sulfite, diisononyl adipate, calcium stearate and polyoxyethylene lauryl ether are mixed to put in a sintering furnace for sintering to obtain the medical implantation magnesium alloy material. The medical implantation magnesium alloy material. Has the tensile strength of above 301 MPa, the yield strength of 231 MPa, the ductility of 13%, the self-corrosion potential of -1.713 V and the corrosion current density of 1.01*10-5 A.cm-2, and is excellent in mechanical performance and corrosion resistance.
Description
Technical field
The invention belongs to biology medical material technical field, the preparation method being specifically related to a kind of medical embedded magnesium alloy materials。
Background technology
The exploitation of bio-medical material is the crossing research direction jointly greatly developed at material and biological two big basic research fields in recent years, from investigation of materials angle, bio-medical material includes the material medically can implanted organism or can combine with biological tissue, medical material is used for treating or replace original tissue and organ in living organism, revises and improves its function。At present, the bio-medical material being applied to clinic mainly includes metal class, organic polymer class and inorganic non-metallic class bio-medical material and bio-medical composition prepared by above-mentioned three kinds of materials。In the material of these types, biomedical metallic material is a most widely used class Srgery grafting material in clinic, this material has high intensity, good toughness, good fatigue resistance and good machine-shaping property, has other irreplaceable premium properties of type medical material。
Magnesium alloy is as medical embedded material, compared with the existing own medical metal material through entering Clinical practice, there is better biocompatibility, under suitable metabolic conditions, human body will not be produced harmful effect magnesium can obtain degraded in human body, multiple metabolic process in perfect aspect, it is possible to promote energy i (in vivo) transhipment, store and utilize。Magnesium is the indispensable element of osteogenesis, and magnesium ion can promote the deposition of calcium, promotes the formation of osteocyte, healing acceleration etc.。The density of magnesium alloy and people's bone coincide, and meet the requirement of desirable synthetism material, it is to avoid reducing and the magnesium alloy molded property of retardation problem that heals is good owing to embedded material does not mate the bone strength caused with people's flexible bone modulus, aboundresources, price is low。The multiple methods such as casting, extruding, punching press, machining can be passed through and obtain the variously-shaped product needed。Therefore, magnesium alloy can obtain as effective medical embedded material and use。On the basis of existing magnesium alloy, the new alloy system that the applicable biomaterial of research uses, and the assessment of performance is carried out for medical Special use environment, it is the important directions of development of new medical embedded material。
Summary of the invention
The preparation method that it is an object of the invention to overcome the deficiencies in the prior art and provide a kind of medical embedded magnesium alloy materials, resulting materials has good mechanical property and corrosion resistance。
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 5~10 parts, soybean lecithin 1~4 part, citric acid 2~6 parts to the KOH solution of 20wt%, heating, insulation, after filtration, solids is dried, mixs homogeneously with glycerol 10~15 parts, 5~15 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 6~12 parts, 3~6 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 2~5 parts, methyl methacrylate 1~4 part, sodium sulfite 3~6 parts, diisononyl adipate 2~5 parts, calcium stearate 1~5 part, polyoxyethylene lauryl ether 3~6 parts mixing, put in sintering furnace and sinter, to obtain final product。
Further, in step 1, heating-up temperature is 70~80 DEG C, and temperature retention time is 2~4h。
Further, in step 1, magnesian mean diameter is 100~500 μm。
Further, the mean diameter of the zinc powder of step 2 is 50~100 μm。
Further, in step 4, sintering temperature is 600~750 DEG C, and sintering time is 30~50min。
Further, after solids is dried by step 1, in addition it is also necessary to add polymine 1~2 part。
Further, step 2 also needs to add ammonium polymethacrylate 1~2 part。
The medical embedded magnesium alloy materials tensile strength of the present invention reaches 13% in more than 301MPa, yield strength at 231MPa, elongation percentage, corrosion potential is 1.01 × 10 at-1.713V, corrosion electric current density-5A·cm-2, there is good mechanical property and corrosion resistance。
Detailed description of the invention
Embodiment 1
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 5 parts, soybean lecithin 1 part, citric acid 2 parts to the KOH solution of 20wt%, heating, insulation, after filtration, is dried by solids, mix homogeneously with glycerol 10 parts, 5 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 6 parts, 3 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 2 parts, methyl methacrylate 1 part, sodium sulfite 3 parts, diisononyl adipate 2 parts, calcium stearate 1 part, polyoxyethylene lauryl ether 3 parts mixing, put in sintering furnace and sinter, to obtain final product。
Wherein, in step 1, heating-up temperature is 70 DEG C, and temperature retention time is 4h, and magnesian mean diameter is 100 μm;The mean diameter of the zinc powder of step 2 is 50 μm;In step 4, sintering temperature is 600 DEG C, and sintering time is 50min。
Embodiment 2
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 7 parts, soybean lecithin 2 parts, citric acid 5 parts to the KOH solution of 20wt%, heating, insulation, after filtration, is dried by solids, mix homogeneously with glycerol 11 parts, 8 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 8 parts, 5 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 4 parts, methyl methacrylate 2 parts, sodium sulfite 5 parts, diisononyl adipate 4 parts, calcium stearate 3 parts, polyoxyethylene lauryl ether 5 parts mixing, put in sintering furnace and sinter, to obtain final product。
Wherein, in step 1, heating-up temperature is 75 DEG C, and temperature retention time is 3h, and magnesian mean diameter is 200 μm;The mean diameter of the zinc powder of step 2 is 80 μm;In step 4, sintering temperature is 700 DEG C, and sintering time is 40min。
Embodiment 3
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 9 parts, soybean lecithin 2 parts, citric acid 5 parts to the KOH solution of 20wt%, heating, insulation, after filtration, is dried by solids, mix homogeneously with glycerol 13 parts, 12 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 9 parts, 5 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 4 parts, methyl methacrylate 3 parts, sodium sulfite 5 parts, diisononyl adipate 4 parts, calcium stearate 2 parts, polyoxyethylene lauryl ether 5 parts mixing, put in sintering furnace and sinter, to obtain final product。
Wherein, in step 1, heating-up temperature is 80 DEG C, and temperature retention time is 2h, and magnesian mean diameter is 500 μm;The mean diameter of the zinc powder of step 2 is 100 μm;In step 4, sintering temperature is 750 DEG C, and sintering time is 30min。
Embodiment 4
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 10 parts, soybean lecithin 4 parts, citric acid 6 parts to the KOH solution of 20wt%, heating, insulation, after filtration, is dried by solids, mix homogeneously with glycerol 15 parts, 15 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 12 parts, 6 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 5 parts, methyl methacrylate 4 parts, sodium sulfite 6 parts, diisononyl adipate 5 parts, calcium stearate 5 parts, polyoxyethylene lauryl ether 6 parts mixing, put in sintering furnace and sinter, to obtain final product。
Wherein, in step 1, heating-up temperature is 70 DEG C, and temperature retention time is 4h, and magnesian mean diameter is 100 μm;The mean diameter of the zinc powder of step 2 is 50 μm;In step 4, sintering temperature is 600 DEG C, and sintering time is 50min。
Embodiment 5
The present embodiment and embodiment 2 are distinctive in that: after being dried by solids in step 1, in addition it is also necessary to add polymine 1~2 part。
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 7 parts, soybean lecithin 2 parts, citric acid 5 parts to the KOH solution of 20wt%, heating, insulation, after filtration, solids is dried, mixs homogeneously with polymine 1 part, glycerol 11 parts, 8 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 8 parts, 5 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 4 parts, methyl methacrylate 2 parts, sodium sulfite 5 parts, diisononyl adipate 4 parts, calcium stearate 3 parts, polyoxyethylene lauryl ether 5 parts mixing, put in sintering furnace and sinter, to obtain final product。
Wherein, in step 1, heating-up temperature is 75 DEG C, and temperature retention time is 3h, and magnesian mean diameter is 200 μm;The mean diameter of the zinc powder of step 2 is 80 μm;In step 4, sintering temperature is 700 DEG C, and sintering time is 40min。
Embodiment 6
The present embodiment and embodiment 5 are distinctive in that: also need in step 2 add ammonium polymethacrylate 1~2 part。
The preparation method of a kind of medical embedded magnesium alloy materials, comprises the following steps:
Step 1, with parts by weight, adds magnesium oxide 7 parts, soybean lecithin 2 parts, citric acid 5 parts to the KOH solution of 20wt%, heating, insulation, after filtration, solids is dried, mixs homogeneously with polymine 1 part, glycerol 11 parts, 8 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 8 parts, 5 parts of water, ammonium polymethacrylate 1 part, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 4 parts, methyl methacrylate 2 parts, sodium sulfite 5 parts, diisononyl adipate 4 parts, calcium stearate 3 parts, polyoxyethylene lauryl ether 5 parts mixing, put in sintering furnace and sinter, to obtain final product。
Wherein, in step 1, heating-up temperature is 75 DEG C, and temperature retention time is 3h, and magnesian mean diameter is 200 μm;The mean diameter of the zinc powder of step 2 is 80 μm;In step 4, sintering temperature is 700 DEG C, and sintering time is 40min。
Embodiment 1 to 6 gained magnesium alloy materials is carried out performance test, and result is as follows:
As seen from the above table, the magnesium alloy materials tensile strength of the present invention reaches 13% in more than 301MPa, yield strength at 231MPa, elongation percentage, corrosion potential is 1.01 × 10 at-1.713V, corrosion electric current density-5A·cm-2, there is good mechanical property and corrosion resistance。Due to the addition of polymine in embodiment 5, enhancing the decay resistance of material, this is possibly due to polymine and has promoted magnesium and zinc Dispersed precipitate in the base, reduces the potential difference of matrix, thus slowing down corrosion;Due to the addition of ammonium polymethacrylate in embodiment 6 so that the granularity of magnesium alloy obtains uniformly further, thus enhancing mechanical property。
Claims (7)
1. the preparation method of a medical embedded magnesium alloy materials, it is characterised in that: comprise the following steps:
Step 1, with parts by weight, adds magnesium oxide 5~10 parts, soybean lecithin 1~4 part, citric acid 2~6 parts to the KOH solution of 20wt%, heating, insulation, after filtration, solids is dried, mixs homogeneously with glycerol 10~15 parts, 5~15 parts of water, obtain the first mixture;
Step 2, with parts by weight, takes zinc powder 6~12 parts, 3~6 parts of water, mixing, obtains the second mixture;
Step 3, mixes the first mixture and the second mixture, dries, after ball milling, obtain pre-powder process;
Step 4, with parts by weight, by pre-powder process, ethylene bis stearamide 2~5 parts, methyl methacrylate 1~4 part, sodium sulfite 3~6 parts, diisononyl adipate 2~5 parts, calcium stearate 1~5 part, polyoxyethylene lauryl ether 3~6 parts mixing, put in sintering furnace and sinter, to obtain final product。
2. the preparation method of medical embedded magnesium alloy materials according to claim 1, it is characterised in that: in step 1, heating-up temperature is 70~80 DEG C, and temperature retention time is 2~4h。
3. the preparation method of medical embedded magnesium alloy materials according to claim 1, it is characterised in that: in step 1, magnesian mean diameter is 100~500 μm。
4. the preparation method of medical embedded magnesium alloy materials according to claim 1, it is characterised in that: the mean diameter of the zinc powder of step 2 is 50~100 μm。
5. the preparation method of medical embedded magnesium alloy materials according to claim 1, it is characterised in that: in step 4, sintering temperature is 600~750 DEG C, and sintering time is 30~50min。
6. the preparation method of medical embedded magnesium alloy materials according to claim 1, it is characterised in that: after solids is dried by step 1, in addition it is also necessary to add polymine 1~2 part。
7. the preparation method of medical embedded magnesium alloy materials according to claim 1, it is characterised in that: step 2 also needs to add ammonium polymethacrylate 1~2 part。
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CN111134746A (en) * | 2019-12-30 | 2020-05-12 | 山东省肿瘤防治研究院(山东省肿瘤医院) | Surgical suture for gastrointestinal surgery and manufacturing method thereof |
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CN103526091A (en) * | 2013-09-15 | 2014-01-22 | 郑州大学 | Biodegradable medical magnesium alloy as well as preparation method thereof |
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CN103526091A (en) * | 2013-09-15 | 2014-01-22 | 郑州大学 | Biodegradable medical magnesium alloy as well as preparation method thereof |
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CN111134746A (en) * | 2019-12-30 | 2020-05-12 | 山东省肿瘤防治研究院(山东省肿瘤医院) | Surgical suture for gastrointestinal surgery and manufacturing method thereof |
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