CN104451303A - Biomedical magnesium alloy and preparation method and application of biomedical magnesium alloy wire - Google Patents
Biomedical magnesium alloy and preparation method and application of biomedical magnesium alloy wire Download PDFInfo
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- CN104451303A CN104451303A CN201410725691.1A CN201410725691A CN104451303A CN 104451303 A CN104451303 A CN 104451303A CN 201410725691 A CN201410725691 A CN 201410725691A CN 104451303 A CN104451303 A CN 104451303A
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Abstract
The invention discloses a biomedical magnesium alloy. The biomedical magnesium alloy comprises the following components in percentage by mass: 1-10% of Gd, 0.1-5% of Sr, 0.1-2.5% Si, 0.1-3% of M and the balance of Mg and inevitable impurities, wherein M is Ca, Mn and/or Zn. The invention further discloses a preparation method of a biomedical magnesium alloy wire. The preparation method of the biomedical magnesium alloy wire comprises the following steps of smelting, heat treatment, extruding, drawing and surface treatment. The obtained biomedical magnesium alloy wire has excellent properties such as good mechanical properties and biocompatibility, is nontoxic, can be independently used for human body sutures and staples and can also be compounded with a polymer material to serve as a bone fixation material such as a bone plate and a bone screw.
Description
Technical field
The present invention relates to medical metal material technical field, be specifically related to the preparation method and application of a kind of biological medical magnesium alloy and silk material thereof.
Background technology
The orthopaedics implantation instrument of current Clinical practice is mainly titanium alloy, stainless steel, cobalt base alloy etc., has stable fixed effect and superior biocompatibility, but also have that Young's modulus is high, density is large, can not the shortcoming such as degraded and absorbed.
In recent years, the application prospect of degradable magnesium alloy in Absorbable rod orthopaedics implantation instrument receives the extensive concern of whole world investigator.Magnesium alloy has excellent mechanical property and degradability; Good mechanical compatibility, its Young's modulus is about 41 ~ 45GPa, and density is at 1.7 ~ 1.9g/cm
3left and right, and skeleton is close; Its specific tenacity, specific rigidity are higher, and have good biocompatibility.But magnesium alloy erosion rate in human body is too fast, later strength is not enough, hinders the application of magnesium alloy as biological implantation material.Therefore, the medical magnesium alloy of exploitation controllable degradation rate, excellent mechanical performances is the key of magnesium alloy as medical material.
Along with deepening continuously of biological medical magnesium alloy research and development, magnesium alloy filament material is fixed at bone the potential using value strengthening multiple medical fields such as polymer composite, gastrointestinal anastomosis anastomosis staple/suture line, braiding shop intracavity stent with magnesium silk and is excavated gradually.For filament material, industry maturation is also best production method is at present adopt drawing processing.But the hexagonal crystallographic texture characteristic of magnesium alloy makes its deformation at room temperature working ability be very limited.Therefore, the exploitation of high plastic magnesium alloy silk material is one of medical magnesium alloy research field important directions.
Summary of the invention
The object of the invention is to provide the preparation method and application of a kind of biological medical magnesium alloy and silk material thereof, to solve the deficiencies in the prior art.
The present invention is by the following technical solutions:
A kind of biological medical magnesium alloy, by mass percentage, comprising: 1 ~ 10%Gd, 0.1 ~ 5%Sr, 0.1 ~ 2.5%Si, 0.1 ~ 3%M, surplus is Mg and inevitable impurity, and wherein, described M is one or more in Ca, Mn, Zn.
Further, described biological medical magnesium alloy, by mass percentage, comprising: 1 ~ 5%Gd, 2 ~ 5%Sr, 0.1 ~ 1.5%Si, 0.1 ~ 1.5%M, and surplus is Mg and inevitable impurity, and wherein, described M is one or more in Ca, Mn, Zn.
Further, described biological medical magnesium alloy, by mass percentage, comprising: 6 ~ 10%Gd, 0.1 ~ 1.8%Sr, 1.2 ~ 2.5%Si, 1.5 ~ 3%M, and surplus is Mg and inevitable impurity, and wherein, described M is one or more in Ca, Mn, Zn.
Inevitable impurity described in above-mentioned biological medical magnesium alloy by mass percentage, Fe≤0.05%, Ni≤0.02%.
Above-mentioned biological medical magnesium alloy carries out method prepared by a material, comprises the steps:
1) SF is adopted
6+ CO
2mixed gas as shielding gas, SF
6and CO
2throughput ratio is 1:100, is melted completely by magnesium ingot, adds Si, M afterwards, stirs; When melt rises to 730 DEG C ~ 780 DEG C, add Gd, Sr, stir and remove slag, insulation 10 ~ 30min, intermediate agitation 3 ~ 5 times, after alloy all dissolves, stop heating;
2) when melt is down to 700 ~ 710 DEG C, melt being poured into cross-sectional diameter is in the mold of 50 ~ 100mm, obtains magnesium alloy ingot blank; At 450 DEG C ~ 530 DEG C, annealing 10 ~ 30h is carried out to magnesium alloy ingot blank;
3) extrude after magnesium alloy ingot blank being incubated 2 ~ 2.5h at 400 DEG C ~ 500 DEG C, extrusion temperature is 450 DEG C, and obtaining diameter is the magnesium alloy silk material of 2 ~ 5mm;
4) by step 3) magnesium alloy silk material that obtains carries out drawing in cold drawing bench, and single pass heavy deformation is 10 ~ 50%; When drawing is frequently ruptured, adopt intermediate annealing process: 300 DEG C ~ 460 DEG C, time 10min ~ 60min.
Further, step 4) described drawing carries out drawing at 25 DEG C ~ 200 DEG C.
Further, the surface of the magnesium alloy silk material after drawing also applies degradable ceramic coating, and the method for employing comprises anodic oxidation, differential arc oxidation, plasma spraying or galvanic deposit.
Further, crystal pulling method or even glue method is adopted to obtain degradable macromolecule coating on the surface of the magnesium alloy silk material of coating degradable ceramic coating.
The magnesium alloy silk material of above-mentioned preparation is complex magnesium alloy material, has good biocompatibility and mechanical property, and cytotoxicity is rated 0 grade, and tensile strength is 210MPa ~ 350MPa, and unit elongation is 10% ~ 25%.Can separately for human body, such as suture line, anastomosis staple etc., also can with high score subclass Material cladding, such as, as bone internal fixation material, hone lamella, nail etc.
Medical magnesium alloy Composition Design of the present invention is according to being: Gd adds the solidity to corrosion can improving magnesium alloy, and stress-free corrosion tendency; The castability of magnesium alloy can also be improved simultaneously, improve alloy strength and ductility.Sr is one of trace element of needed by human, 99% is present in bone and tooth, and wherein in bone, Sr content is approximately 100 ~ 120mg/kg, and Sr salt has the osteoblastic growth of promotion on the one hand, and suppress the growth of osteoclast, prevent molten bone phenomenon and promote the effects such as vascularization; Appropriate Sr can improve intensity and the corrosion resistance nature of magnesium alloy on the other hand.Alloy element Si is the element of needed by human equally, can promote that skeleton development grows.
Beneficial effect of the present invention:
1) biological medical magnesium alloy of the present invention is by the control of the conditions such as alloy component proportions, machined parameters and silk material top coat, realize degradation rate, the mechanical property of regulation and control medical embedded material, thus obtain the magnesium alloy implant material of optimum human body application.
2) the invention provides a kind of preparation method of medical magnesium alloy silk material, this material has good biocompatibility, and cytotoxicity is rated 0 grade, and tensile strength is 210MPa ~ 350MPa, and unit elongation is 10% ~ 25%.Can separately for human body, such as suture line, anastomosis staple etc., also can with high score subclass Material cladding, such as, as bone internal fixation material, hone lamella, nail etc.
Accompanying drawing explanation
Fig. 1 is preparation
magnesium alloy silk material.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example only for illustration of the present invention, but is not used for limiting practical range of the present invention.
Embodiment 1
The biological medical magnesium alloy of the present embodiment is grouped into by the one-tenth of following mass percent: 10%Gd, 0.1%Sr, 2.5%Si, 1%Ca, 1%Mn, 1%Zn, and surplus is Mg and inevitable impurity.
The preparation method of the biological medical magnesium alloy silk material of the present embodiment is as follows:
1) SF is adopted
6+ CO
2mixed gas as shielding gas, SF
6and CO
2throughput ratio is 1:100, is melted completely by magnesium ingot, adds Si, Zn afterwards, stirs; When melt rises to 730 DEG C, add Gd, Sr, stir and remove slag, insulation 15min, intermediate agitation 3 ~ 5 times, after alloy all dissolves, stop heating.
2) when melt is down to 710 DEG C, melt being poured into cross-sectional diameter is in the mold of 50mm, obtains magnesium alloy ingot blank; At 450 DEG C to magnesium alloy ingot blank annealing 30h.
3) extrude after magnesium alloy ingot blank being incubated about 2h at 400 DEG C, extrusion temperature is 450 DEG C, and obtaining diameter is the magnesium alloy silk material of 2mm.
4) above-mentioned magnesium alloy silk material is carried out drawing under room temperature, single pass average deformation amount is 11.3%, after continuous drawing 10 passages, silk material is incubated 60min at 300 DEG C.
The magnesium alloy silk material tensile strength that the present embodiment obtains is 347MPa, unit elongation 23.6%.
Embodiment 2
The composition of biological medical magnesium alloy and the preparation method of silk material thereof are with embodiment 1, differential arc oxidation process is carried out on the magnesium alloy silk material surface that drawing obtains, adopt the electrolyte system of 10g/L water glass, 8g/L hydroxyapatite and 3g/L sodium hydroxide composition, electric current: 10mA/cm
2, process cleaning-drying after 20min under normal temperature, obtain the magnesium alloy silk material of rich surface containing the degradable ceramic coating of one deck Magnesium Silicate q-agent, magnesium oxide, hydroxyapatite, clean up, prepare stand-by.
37 DEG C, carry out Degrading experiment in the neutral phosphate buffer liquid of pH=7.4, along with the prolongation of time, degradable ceramic coating and magnesium alloy silk material dissolve gradually, and degradation half life is about 5 months.
Embodiment 3
The biological medical magnesium alloy of the present embodiment is grouped into by the one-tenth of following mass percent: 1%Gd, 5%Sr, 0.1%Si, 0.1%Zn, and surplus is Mg and inevitable impurity.
The preparation method of the biological medical magnesium alloy silk material of the present embodiment is as follows:
1) SF is adopted
6+ CO
2mixed gas as shielding gas, SF
6and CO
2throughput ratio is 1:100, is melted completely by magnesium ingot, adds Si, Ca, Mn, Zn afterwards, stirs; When melt rises to 780 DEG C, add Gd, Sr, stir and remove slag, insulation 20min, intermediate agitation 3 ~ 5 times, after alloy all dissolves, stop heating.
2) when melt is down to 700 DEG C, melt being poured into cross-sectional diameter is in the mold of 100mm, obtains magnesium alloy ingot blank; At 530 DEG C, annealing 10h is carried out to magnesium alloy ingot blank.
3) extrude after magnesium alloy ingot blank being incubated about 2h at 500 DEG C, extrusion temperature is 450 DEG C, and obtaining diameter is the magnesium alloy silk material of 5mm.
4) above-mentioned magnesium alloy silk material is carried out drawing at 50 DEG C, single pass average deformation amount is 50%, after continuous drawing 5 passages, silk material is incubated 10min at 460 DEG C.
5) by the magnesium alloy silk material in step 4 at HNO
3carry out pickling 5min with in HF mixing solutions, be then immersed in by magnesium alloy silk material and be dissolved with in the trichloromethane organic solvent of poly(lactic acid), centrifugal treating is carried out in rear pull-out.
This surface-treated magnesium alloy silk material tensile strength obtained is 257MPa, unit elongation 11.1%.
Embodiment 4
The biological medical magnesium alloy of the present embodiment is grouped into by the one-tenth of following mass percent: 5%Gd, 2%Sr, 1.5%Si, 1.5%Ca, and surplus is Mg and inevitable impurity.
The preparation method of the biological medical magnesium alloy silk material of the present embodiment is as follows:
1) SF is adopted
6+ CO
2mixed gas as shielding gas, SF
6and CO
2the throughput ratio of flow is 1:100, is melted completely by magnesium ingot, adds Si, Ca afterwards, stir; When melt rises to 750 DEG C, add Gd, Sr, stir and remove slag, insulation 30min, intermediate agitation 3 ~ 5 times, after alloy all dissolves, stop heating.
2) when melt is down to 710 DEG C, melt being poured into cross-sectional diameter is in the mold of 60mm, obtains magnesium alloy ingot blank; At 490 DEG C, annealing 18h is carried out to magnesium alloy ingot blank.
3) extrude after magnesium alloy ingot blank being incubated about 2h at 450 DEG C, extrusion temperature is 450 DEG C, obtains the magnesium alloy extrusion silk material that diameter is 3mm.
4) above-mentioned magnesium alloy extrusion silk material is carried out drawing at 100 DEG C, single pass average deformation amount is 30%, continuous drawing 11 passages, obtains magnesium alloy silk material.
5) magnesium alloy silk material in step 4 is carried out plasma spraying, coat is tetracalcium phosphate, and its spraying conditions is as follows,
Ar:60scfh, H
2: 10scfh, spray voltage: 50V, spraying current: 500A, spray distance 300mm.Thus obtain the magnesium alloy silk material of degradable ceramic coating, clean up, prepare stand-by.
This surface-treated magnesium alloy silk material tensile strength obtained is 213MPa, and unit elongation is 16.4%.
Embodiment 5
The composition of biological medical magnesium alloy and the preparation method of silk material thereof are with embodiment 4, the Mg alloy wire of surface coverage one deck degradable pottery is aligned in mold cavity, appropriate poly(lactic acid) macromolecular material is dissolved in trichloroethane, then solution is injected mould to mix with magnesium alloy silk material, vacuum-drying at 80 DEG C, then compression molding at 195 DEG C, obtains magnesium alloy silk material-poly(lactic acid) polymer composite, can be processed into the bone such as nail, hone lamella internal fixation material.
37 DEG C, carry out Degrading experiment in the neutral phosphate buffer liquid of pH=7.4, along with the prolongation of time, poly(lactic acid) and magnesium silk dissolve gradually, and the degradative phase transformation period is about 6 months.
Embodiment 6
The biological medical magnesium alloy of the present embodiment is grouped into by the one-tenth of following mass percent: 6%Gd, 1.8%Sr, 1.2%Si, 1%Mn and 0.5%Zn, and surplus is Mg and inevitable impurity.
The preparation method of the biological medical magnesium alloy of the present embodiment is as follows:
1) SF is adopted
6+ CO
2mixed gas as shielding gas, SF
6and CO
2throughput ratio be 1:100, magnesium ingot is melted completely, adds Si, Mn, Zn afterwards, stir; When melt rises to 765 DEG C, add Gd, Sr, stir and remove slag, insulation 30min, intermediate agitation 3 ~ 5 times, after alloy all dissolves, stop heating.
2) when melt is down to 700 DEG C, melt is poured into the mold that cross-sectional diameter is 80mm, obtain magnesium alloy ingot blank; At 470 DEG C, annealing 24h is carried out to magnesium alloy ingot blank.
3) extrude after magnesium alloy ingot blank being incubated about 2h at 470 DEG C, extrusion temperature is 450 DEG C, and obtaining diameter is the magnesium alloy silk material of 3.5mm.
4) above-mentioned magnesium alloy silk material is carried out drawing at 150 DEG C, single pass average deformation amount is 13.7%, after continuous drawing 16 passages, silk material is incubated 40min at 420 DEG C, then carry out anneal (410 DEG C × 20min) after continuing drawing 12 passages, obtain
magnesium alloy silk material, as shown in Figure 1.
Claims (9)
1. a biological medical magnesium alloy, is characterized in that, by mass percentage, comprising: 1 ~ 10%Gd, 0.1 ~ 5%Sr, 0.1 ~ 2.5%Si, 0.1 ~ 3%M, surplus is Mg and inevitable impurity, and wherein, described M is one or more in Ca, Mn, Zn.
2. biological medical magnesium alloy according to claim 1, is characterized in that, by mass percentage, comprising: 1 ~ 5%Gd, 2 ~ 5%Sr, 0.1 ~ 1.5%Si, 0.1 ~ 1.5%M, surplus is Mg and inevitable impurity, and wherein, described M is one or more in Ca, Mn, Zn.
3. biological medical magnesium alloy according to claim 1, is characterized in that, by mass percentage, comprising: 6 ~ 10%Gd, 0.1 ~ 1.8%Sr, 1.2 ~ 2.5%Si, 1.5 ~ 3%M, surplus is Mg and inevitable impurity, and wherein, described M is one or more in Ca, Mn, Zn.
4. the biological medical magnesium alloy according to the arbitrary claim of claims 1 to 3, is characterized in that, described inevitable impurity by mass percentage, Fe≤0.05%, Ni≤0.02%.
5. the method utilizing the biological medical magnesium alloy described in the arbitrary claim of claim 1 ~ 3 to carry out a material to prepare, is characterized in that, comprise the steps:
1) SF is adopted
6+ CO
2mixed gas as shielding gas, SF
6and CO
2throughput ratio is 1:100, is melted completely by magnesium ingot, adds Si, M afterwards, stirs; When melt rises to 730 DEG C ~ 780 DEG C, add Gd, Sr, stir and remove slag, insulation 10 ~ 30min, intermediate agitation 3 ~ 5 times, after alloy all dissolves, stop heating;
2) when melt is down to 700 ~ 710 DEG C, melt being poured into cross-sectional diameter is in the mold of 50 ~ 100mm, obtains magnesium alloy ingot blank; At 450 DEG C ~ 530 DEG C, annealing 10 ~ 30h is carried out to magnesium alloy ingot blank;
3) extrude after magnesium alloy ingot blank being incubated 2 ~ 2.5h at 400 DEG C ~ 500 DEG C, extrusion temperature is 450 DEG C, and obtaining diameter is the magnesium alloy silk material of 2 ~ 5mm;
4) by step 3) magnesium alloy silk material that obtains carries out drawing in cold drawing bench, and single pass heavy deformation is 10 ~ 50%; When drawing is frequently ruptured, adopt intermediate annealing process: 300 DEG C ~ 460 DEG C, time 10min ~ 60min.
6. the preparation method of biological medical magnesium alloy silk material according to claim 5, is characterized in that, step 4) described drawing carries out drawing at 25 DEG C ~ 200 DEG C.
7. the preparation method of biological medical magnesium alloy silk material according to claim 5, it is characterized in that, the surface of the magnesium alloy silk material after drawing also applies degradable ceramic coating, and the method for employing comprises anodic oxidation, differential arc oxidation, plasma spraying or galvanic deposit.
8. the preparation method of biological medical magnesium alloy silk material according to claim 7, is characterized in that, adopts crystal pulling method or even glue method to obtain degradable macromolecule coating on the surface of the magnesium alloy silk material of coating degradable ceramic coating.
9. claim 5 prepare biological medical magnesium alloy silk material as human body suture line, anastomosis staple application or with the application of high score subclass Material cladding as bone internal fixation material.
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| CN105640601A (en) * | 2016-04-08 | 2016-06-08 | 苏州奥芮济医疗科技有限公司 | In-vivo absorbable metal surgical staple and preparation method thereof |
| CN106119644A (en) * | 2015-04-15 | 2016-11-16 | 丁永新 | Preferable medical magnesium base alloy material of biocompatibility and preparation method thereof |
| CN106606800A (en) * | 2015-10-21 | 2017-05-03 | 北京大学 | Zn-Fe system zinc alloy and preparation method and application thereof |
| CN106715737A (en) * | 2014-09-09 | 2017-05-24 | 国立大学法人神户大学 | Device for fixing biological soft tissue, and method for producing same |
| CN106917022A (en) * | 2017-03-17 | 2017-07-04 | 扬州大学 | A kind of preparation method of biological medical magnesium alloy silk |
| CN108149295A (en) * | 2017-12-26 | 2018-06-12 | 北京派尔特医疗科技股份有限公司 | Semi-automatic silk material differential arc oxidation system and its oxidation, cleaning equipment and method |
| CN108311853A (en) * | 2017-08-21 | 2018-07-24 | 广东省材料与加工研究所 | A kind of processing method of medical magnesium alloy angiocarpy bracket |
| CN108467981A (en) * | 2018-01-24 | 2018-08-31 | 烟台南山学院 | A kind of preparation method of magnesium alloy silk material |
| CN109316624A (en) * | 2017-07-31 | 2019-02-12 | 中国科学院金属研究所 | A kind of degradable cartilage connection suture of integrated strip needle |
| CN109536801A (en) * | 2018-11-30 | 2019-03-29 | 重庆医科大学附属永川医院 | A kind of bio-medical porous magnesium alloy and preparation method thereof |
| 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 |
| CN110042289A (en) * | 2019-04-18 | 2019-07-23 | 北京大学 | A kind of magnesium alloy containing Sr |
| CN111229855A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院金属研究所 | Preparation method of biomedical magnesium alloy wire |
| CN111424202A (en) * | 2019-01-30 | 2020-07-17 | 四川镁合医疗器械有限责任公司 | Degradable magnesium alloy in-situ composite anastomosis nail and preparation method thereof |
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| 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 |
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| CN106119644A (en) * | 2015-04-15 | 2016-11-16 | 丁永新 | Preferable medical magnesium base alloy material of biocompatibility and preparation method thereof |
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| CN108467981A (en) * | 2018-01-24 | 2018-08-31 | 烟台南山学院 | A kind of preparation method of magnesium alloy silk material |
| CN111229855A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院金属研究所 | Preparation method of biomedical magnesium alloy wire |
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Application publication date: 20150325 |