CN105648272A - Degradable zinc alloy material, and preparation method and application thereof - Google Patents
Degradable zinc alloy material, and preparation method and application thereof Download PDFInfo
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- CN105648272A CN105648272A CN201610070048.9A CN201610070048A CN105648272A CN 105648272 A CN105648272 A CN 105648272A CN 201610070048 A CN201610070048 A CN 201610070048A CN 105648272 A CN105648272 A CN 105648272A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
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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
- A61L31/148—Materials at least partially resorbable by the body
-
- 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
- C22F1/16—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
The invention relates to a degradable zinc alloy material which comprises the following components in percent by mass: 0.5-3 percent of magnesium, 0.1-1 percent of calcium, and the balance of zinc. The invention further relates to a preparation method of the degradable zinc alloy material. The preparation method comprises the following steps: mixing and smelting the raw materials of magnesium, calcium and zinc for 5-15 min at the temperature of 550-700 DEG C to prepare an ingot; extruding the ingot to obtain a bar, and conducting the thermal treatment on the bar for 1-3 h at the temperature of 300-400 DEG C; and placing the bar in air for cooling, and conducting the cold-drawing to obtain a wire. The degradable zinc alloy material is applied to medical implantable instruments, especially nose bridge brackets. The zinc alloy material is high in mechanical property, machining property and biocompatibility and appropriate in biodegradation rate.
Description
Technical field
The present invention relates to degradable Material Field, be specifically related to a kind of degradable zinc alloy material and its preparation method and application.
Background technology
Nasal cavity problem is one of frequently-occurring disease in daily life, and especially present nasal cavity class disease not only kind is many but also sickness rate is high repeatedly, and sick crowd's rejuvenation trend is obvious. The nasal cavity timbering material having been enter into clinical stage at present is mainly rustless steel, Nitinol. The main deficiency that rustless steel nasal cavity support exists in clinical practice is that its effective percentage is low, and main cause is stainless poor biocompatibility, causes tissue neointimal hyperplasia, and when taking out, human body is caused secondary injury.
For the problems referred to above, the concept of " Biodegradable material " is suggested. The Biodegradable material of current clinical practice mainly includes machine macromolecular material and biological active ceramic material, but this kind of degradation material yet suffers from obvious defect: bioabsorbable polymer material mechanical property is too low, the sour environment that degraded produces can cause inflammation; The plasticity of bioceramic material and elasticity are all poor. A new generation has the appearance of the medical metal material of biodegradable characteristics and then compensate for the defect of traditional biological degradation material.
Present Domestic degradable metal research focuses primarily upon biodegradable magnesium alloy and ferrous alloy. As Chinese invention patent (publication number CN104755644A) discloses a kind of alloy and has the implant of the three dimensional structure based on this type of alloy. Described alloy includes single-phase MgZn alloy, and described single-phase MgZn alloy comprises the Zn of Zn to the 6 weight % of 2.0 weight %, has one or more other elements less than 0.001 weight %, and wherein remainder is Mg. Chinese invention patent (CN105143483A) discloses a kind of alloy and a kind of implant with the three dimensional structure based on this type of alloy. This alloy includes MgZnCa alloy, this MgZnCa alloy comprises the nanoprecipitation thing that inertia is less than the inertia of Mg matrix alloy, and there is the Zn content in the scope of the Zn of Zn to the 2 weight % of 0.1 weight % and the calcium content in the scope of 0.2 weight % to 0.5 weight %, and there is one or more other elements, wherein remainder is magnesium.
But magnesium alloy degradation speed is too fast, affects its biocompatibility and mechanical property in use, and ferrous alloy degradation speed is excessively slow, can cause a series of untoward reaction similar with bio-inert material. Current degradable magnesium alloy angiocarpy bracket, nail all have been enter into clinical experimental stage, but its degradation speed is fast, catabolite is difficult to the unfavorable factors such as absorption and limits its application prospect.
Summary of the invention
The technical problem to be solved, it is provided that a kind of Biodegradable zinc alloy material, this material possesses good mechanical property, machining property, biocompatibility and suitable biodegradation rate.
The present invention is achieved by the following technical solutions:
A kind of degradable zinc alloy material, wherein, described zinc alloy material includes following each component:
Magnesium 0.5��3wt%,
Calcium 0.1��1wt%,
Surplus is zinc.
Above-mentioned zinc alloy material is a kind of novel degradable metal base biomaterial. Compared with the iron-based biomaterial more with research at present and magnesio biomaterial, zinc-base biomaterial has suitable degradation rate in environment in nasal cavity, can ensure enough mechanical properties under arms in the phase, and after the phase terminates under arms, progressively degrade, it is not necessary to after recovering, take out support. Zinc is one of trace element of needed by human, can be absorbed by the body, will not health be damaged after the degraded of zinc-base biomaterial.
Adjustment by Mg content, zinc alloy material is made to form better simply duplex structure, so that zinc alloy material has higher tensile strength and elongation percentage, adjustment by Ca content, in conjunction with corresponding heat treatment and cold-drawing technology, zinc alloy material is made to form the hardening constituent of disperse in the course of processing, the tensile strength so that the corrosion resistance of zinc alloy material improves, after especially long-time immersion corrosion.
As preferably, described each component:
Magnesium 0.8��1.5wt%,
Calcium 0.12��0.2wt%,
Surplus is zinc.
When the mass percent of the Mg that zinc alloy material contains is when 0.8��1.5%, grain refinement and solution strengthening effect to zinc alloy material strengthen, Ca mass percent is when 0.12��0.2, the dispersion-strengthened action of zinc alloy material is increased, obtains the degradable zinc alloy material of high comprehensive performance.
It is preferred that, described each component:
Magnesium 1.0wt%,
Calcium 0.16wt%,
Surplus is zinc.
When the mass percent of the Mg that zinc alloy material contains is when 1%, grain refinement and solution strengthening effect to zinc alloy material are the strongest, Ca mass percent is when 0.16%, and the dispersion-strengthened action of zinc alloy material is maximum, obtains the degradable Zn alloy of high comprehensive performance.
As preferably, described degradable zinc alloy material is diameter is the silk material of 0.2��0.5mm. When silk material diameter is 0.2��0.5mm, the intensity of zinc alloy material now and elasticity are very suitable for preparing medical embedded apparatus. It is especially suitable for bridge of the nose support, there is higher tensile strength and certain elongation percentage.
The preparation method that the present invention also provides for a kind of degradable zinc alloy material, comprises the steps:
1) by the raw material containing magnesium, calcium and zinc, mixed smelting 5��15min at temperature 550��700 DEG C, prepares ingot;
2) ingot is obtained bar, heat treatment 1��3h at temperature 250��360 DEG C by extruding;
3) put in air and cool down, obtain a material then through cold-drawn.
The present invention, by preparing ingot-extruding-heat treatment-cold-drawn, obtains a material, by coordinating heat treatment and cold-drawing technology, makes Zn-Mg form relatively simple solid solution structure, makes the dispersion-strengtherning of Ca granule reach optimal effectiveness simultaneously.
By the optimizing components of Zn-Mg-Ca alloy and corresponding working process parameter optimization thereof, heavy alloyed tensile strength can be put forward, be maintained with certain plasticity. Comprehensively putting forward heavy alloyed corrosion resistance and mechanical property so that it is tensile strength reaches 240MPa, after within 30 days, soaking biological solution corrosion testing, tensile strength still can reach 150MPa.
As improvement, the diameter of described bar is 1��3mm. Ingot obtains bar, suitable diameter, it is simple to silk material, cold-drawn uniform force are prepared in next step heat treatment and cold-drawn, it is prevented that rupture in silk material Cold Drawing Process by extruding.
As improvement, the described method preparing ingot is: be cooled to ingot after stirring during fusing and standing again, it is also possible to by thermo forming or casting. After all raw material is completely melt, it is possible to by stirring the effect reaching non-uniform components and degasification, be cooled to ingot again after standing a period of time.
As improvement, described raw material is pure zinc, pure magnesium and pure calcium; Or, raw material is zinc magnesium alloy, zinc calcium alloy and magnesium calcium alloy. Above-mentioned raw material, it is possible to according to calculating each chemical element mass percent and considering scaling loss amount, takes appropriate pure zinc, pure magnesium and pure calcium configuration raw material; According to calculating alloy mass percentage ratio and scaling loss amount can also be considered, configure raw material with the various intermediate alloys containing magnesium, calcium and zinc element.
As improvement, described step 2) in heat treated programming rate be 8��10 DEG C/min. Control programming rate so that bar heat treatment is heated evenly, it is simple to cold-drawn obtains a material.
The present invention also provides for the application in medical embedded apparatus of a kind of degradable zinc alloy material.
The present invention further provides the application in bridge of the nose support of a kind of degradable zinc alloy material.
Compared with the existing technology, beneficial effects of the present invention is embodied in:
(1) present invention is by the optimizing components of Zn-Mg-Ca alloy and working process parameter optimization accordingly thereof, can improve the tensile strength of zinc alloy material, is maintained with certain plasticity, forms 0.2��0.5mm silk material;
(2) the comprehensive corrosion resistance improving zinc alloy material and mechanical property so that it is tensile strength reaches 240MPa, after within 30 days, soaking biological solution corrosion testing, tensile strength still can reach 150MPa;
(3) degradable zinc alloy material prepared by the present invention is with a wide range of applications in fields such as bio-medical implantation instrument such as bridge of the nose support, suturing nails, also may extend to angiocarpy bracket application.
Accompanying drawing explanation
Fig. 1 is nasal cavity support compression view prepared by the degradable zinc alloy material of the present invention;
Fig. 2 is that nasal cavity support prepared by the degradable zinc alloy material of the present invention flicks view;
Fig. 3 is the metallograph of the degradable zinc alloy material of preparation in embodiment 1;
Fig. 4 is the SEM picture of the degradable zinc alloy material of preparation in embodiment 1;
Fig. 5 is the electrochemical impedance figure of the degradable zinc alloy material that the present invention prepares;
Fig. 6 is the activation polarization figure of the degradable zinc alloy material that the present invention prepares.
Detailed description of the invention
Prepare degradable zinc alloy material
Embodiment 1
Kirsite melting 10min, moulding by casting at 650 DEG C containing magnesium 1%, calcium 0.14%. The ingot casting that diameter is 30mm is squeezed into 2mm bar. The tensile strength of gained bar is 252MPa, and yield strength is 187MPa, and elongation percentage is 5.1%. The bar of gained is carried out metallographic and SEM characterizes, respectively as shown in Figures 3 and 4.Continue bar is carried out heat treatment, with 10 DEG C/min of programming rate, be warmed up to 330 DEG C and process 1h, put in air and cool down, obtain 0.5mm silk material then through cold-drawn.
Embodiment 2
Kirsite melting 10min, moulding by casting at 650 DEG C containing magnesium 1.2%, calcium 0.16%. The ingot casting that diameter is 30mm is squeezed into 1.6mm bar. The tensile strength of gained bar is 247MPa, and yield strength is 189MPa, and elongation percentage is 4.6%.
Embodiment 3
Kirsite melting 10min, moulding by casting at 650 DEG C containing magnesium 1.1%, calcium 0.15%. The ingot casting that diameter is 30mm is squeezed into 1.4mm bar. The tensile strength of gained bar is 258MPa, and yield strength is 193MPa, and elongation percentage is 4.9%.
Embodiment 4
Kirsite melting 6min, moulding by casting at 550 DEG C containing magnesium 0.5%, calcium 0.2%. The ingot casting that diameter is 30mm is squeezed into 1mm bar. Continue bar is carried out heat treatment, with 9 DEG C/min of programming rate, be warmed up to 300 DEG C and process 1h, put in air and cool down, obtain 0.2mm silk material then through cold-drawn.
Embodiment 5
Kirsite melting 15min, moulding by casting at 690 DEG C containing magnesium 1.4%, calcium 0.2%. The ingot casting that diameter is 30mm is squeezed into 3mm bar. Continue bar is carried out heat treatment, with 10 DEG C/min of programming rate, be warmed up to 320 DEG C and process 2.5h, put in air and cool down, obtain 0.5mm silk material then through cold-drawn.
Prepare nasal cavity support
The silk material that diameter is 0.3mm that will prepare, bending makes the molding such as support shown in Fig. 1��2, and the size of support can be adjusted according to disease.
Electrochemical property test
Sample is made �� 1.6 �� 10mm carefully excellent, inlay with epoxy resin, then polishing, finally ultrasonic cleaning 5min clock in ethanol after being polishing to 2000 with abrasive paper for metallograph. Before electro-chemical test, sample first soaks 20min in PBS (solution composition is with reference to rower: YY-T0695-2008), electrochemical impedance is tested from 100KHz to 10mHz, as shown in Figure 5, the electrochemical impedance result display kirsite big corrosion resistance of the resistance value in PBS is good, and its impedance results in PBS is RS=11.8 �� cm2, RP=15k �� cm2, CPE=238.4 �� F cm-2; Activation polarization is from-1.72VSCETo-0.46VSCE, it is platinum electrode to electrode, as shown in Figure 6, current potential polarization result shows that the corrosion potential of kirsite is close to pure zinc, and corrosion current is low, and has obvious passivating process, and its corrosion potential in PBS and corrosion current are Ecorr=-1.22VSCE, icorr=1.0196 �� 10-6��
Biological solution corrosion testing
The thread sample of �� 1.6 �� 80mm is made, again with ethanol ultrasonic cleaning 5min after abrasive paper for metallograph is polishing to 2000, by sample hot blast drying after being extruded by sample. First PBS solution is led to nitrogen 2 hours before immersion, then solution is placed in test tube. Being fixed on rubber closure by sample, put in the test tube filling PBS solution and soak, after within 30 days, soaking biological solution corrosion testing, tensile strength still can reach 150MPa.
Claims (10)
1. a degradable zinc alloy material, it is characterised in that described zinc alloy material includes following each component:
Magnesium 0.5��3wt%,
Calcium 0.1��1wt%,
Surplus is zinc.
2. degradable zinc alloy material according to claim 1, it is characterised in that described each component:
Magnesium 0.8��1.5wt%,
Calcium 0.12��0.2wt%,
Surplus is zinc.
3. degradable zinc alloy material according to claim 1 and 2, it is characterised in that described degradable zinc alloy material is diameter is the silk material of 0.2��0.5mm.
4. the preparation method of a degradable zinc alloy material as claimed in claim 3, it is characterised in that comprise the steps:
1) by the raw material containing magnesium, calcium and zinc, mixed smelting 5��15min at temperature 550��700 DEG C, prepares ingot;
2) ingot is obtained bar, heat treatment 1��3h at temperature 250��360 DEG C by extruding;
3) put in air and cool down, obtain a material then through cold-drawn.
5. the preparation method of degradable zinc alloy material according to claim 4, it is characterised in that the diameter of described bar is 1��3mm.
6. the preparation method of degradable zinc alloy material according to claim 4, it is characterised in that the described method preparing ingot is: be cooled to ingot after stirring during fusing and standing again, it is also possible to by thermo forming or casting.
7. the preparation method of degradable zinc alloy material according to claim 4, it is characterised in that described raw material is pure zinc, pure magnesium and pure calcium; Or, raw material is zinc magnesium alloy, zinc calcium alloy and magnesium calcium alloy.
8. the preparation method of degradable zinc alloy material according to claim 4, it is characterised in that described step 2) in heat treated programming rate be 8��10 DEG C/min.
9. one kind as arbitrary in claims 1 to 3 as described in the application in medical embedded apparatus of the degradable zinc alloy material.
10. one kind as arbitrary in claims 1 to 3 as described in the application in bridge of the nose support of the degradable zinc alloy material.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105925848A (en) * | 2016-06-28 | 2016-09-07 | 东北大学 | Biomedical degradable zinc alloy inner implantation material and preparation method of sheet material of biomedical degradable zinc alloy inner implantation material |
| CN106399885A (en) * | 2016-09-30 | 2017-02-15 | 西安爱德万思医疗科技有限公司 | Zinc alloy, heat treatment method of zinc alloy and implant material |
| WO2017117922A1 (en) * | 2016-01-08 | 2017-07-13 | 先健科技(深圳)有限公司 | Implanted device |
| CN107773781A (en) * | 2016-08-29 | 2018-03-09 | 上海交通大学 | The preparation method of flexible degradable kirsite nerve trachea |
| CN108411158A (en) * | 2018-03-05 | 2018-08-17 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | A kind of biodegradable Zn-Mg-Zr alloy materials, preparation method and application |
| CN110512117A (en) * | 2019-09-27 | 2019-11-29 | 石家庄新日锌业有限公司 | Medical zinc alloy material and preparation method thereof |
| CN111012420A (en) * | 2018-10-09 | 2020-04-17 | 上海交通大学 | Preparation method and application of antibacterial and biodegradable zinc alloy anastomosis nail |
| CN112143923A (en) * | 2020-09-28 | 2020-12-29 | 中国矿业大学 | Preparation method of 3mm Zn-Cu-Ti alloy wire for spraying |
| CN112494189A (en) * | 2020-11-03 | 2021-03-16 | 北京科技大学 | Degradable metal uterine cavity stent and release system and use method |
| CN114086030A (en) * | 2021-11-22 | 2022-02-25 | 江苏时代铭阳生物新技术研究院有限公司 | Degradable high-compatibility biomedical material and preparation method thereof |
| CN115161513A (en) * | 2022-08-15 | 2022-10-11 | 西安交通大学 | Biomedical degradable alloy and preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10799612B2 (en) | 2016-01-08 | 2020-10-13 | Lifetech Scientific (Shenzhen) Co. Ltd. | Implanted device |
| WO2017117922A1 (en) * | 2016-01-08 | 2017-07-13 | 先健科技(深圳)有限公司 | Implanted device |
| CN105925848A (en) * | 2016-06-28 | 2016-09-07 | 东北大学 | Biomedical degradable zinc alloy inner implantation material and preparation method of sheet material of biomedical degradable zinc alloy inner implantation material |
| CN107773781A (en) * | 2016-08-29 | 2018-03-09 | 上海交通大学 | The preparation method of flexible degradable kirsite nerve trachea |
| CN106399885A (en) * | 2016-09-30 | 2017-02-15 | 西安爱德万思医疗科技有限公司 | Zinc alloy, heat treatment method of zinc alloy and implant material |
| CN108411158A (en) * | 2018-03-05 | 2018-08-17 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | A kind of biodegradable Zn-Mg-Zr alloy materials, preparation method and application |
| CN108411158B (en) * | 2018-03-05 | 2019-10-15 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | A kind of biodegradable Zn-Mg-Zr alloy material, preparation method and application |
| CN111012420A (en) * | 2018-10-09 | 2020-04-17 | 上海交通大学 | Preparation method and application of antibacterial and biodegradable zinc alloy anastomosis nail |
| CN110512117A (en) * | 2019-09-27 | 2019-11-29 | 石家庄新日锌业有限公司 | Medical zinc alloy material and preparation method thereof |
| CN110512117B (en) * | 2019-09-27 | 2022-05-13 | 石家庄新日锌业有限公司 | Medical zinc alloy material and preparation method thereof |
| CN112143923A (en) * | 2020-09-28 | 2020-12-29 | 中国矿业大学 | Preparation method of 3mm Zn-Cu-Ti alloy wire for spraying |
| CN112494189A (en) * | 2020-11-03 | 2021-03-16 | 北京科技大学 | Degradable metal uterine cavity stent and release system and use method |
| CN114086030A (en) * | 2021-11-22 | 2022-02-25 | 江苏时代铭阳生物新技术研究院有限公司 | Degradable high-compatibility biomedical material and preparation method thereof |
| CN115161513A (en) * | 2022-08-15 | 2022-10-11 | 西安交通大学 | Biomedical degradable alloy and preparation method and application thereof |
| CN115161513B (en) * | 2022-08-15 | 2023-08-25 | 西安交通大学 | Biomedical degradable alloy and preparation method and application thereof |
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Application publication date: 20160608 |