CN101550510A - High intensity degradable biological medical magnesium alloy and preparation method thereof - Google Patents
High intensity degradable biological medical magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high intensity degradable biological medical magnesium alloy, whose component and weight percentage is that:2.5-6 .5% of Y; 1.2-3.5% of Nd; 0.4-0.8% of Zr; not more than 0.05% of the total amount of impurity elements Fe, Al, Cu, Si, and Ni; margin of magnesium. The preparation method includes: completely melting the pure magnesium ingot at protective atmosphere and then elevating the temperature to 1053-1073K, slowly adding Mg-Y, Mg-Nd, Mg-Zr intermediate alloy in sequence, uninterruptedly mixing until completely melting; modulating the alloy flux to 1023-1033K, scattering the refining agent for refining 5-8 minutes, and then elevating the temperature of the flux to 1053-1073K, standing for 10-20 minutes; skimming the surface floating slag when the flux temperature is dropped to 973-993K, casting in the copper mold and then rapidly cooling immediately. The magnesium alloy has fine grain size, high strength at room temperature, good plasticity, degradability, non-toxic and the like characteristics, but also can control the degrading rate of the alloy by changing the total rare earth content of alloy, can be used as base materials of vascular stents, bone screws, bone plates and the like, and is a new biomedical material.
Description
Technical field
The present invention relates to a kind of new bio medical metal material, specifically refer to a kind of high intensity degradable biological medical magnesium alloy, also relate to the preparation method of this magnesium alloy simultaneously.
Technical background
Compare with bioabsorbable polymer material with biological ceramics, the bio-medical metallic substance has high strength, good toughness and anti-fatigue performance, easy excellent properties such as machine-shaping, becomes present clinical application material the most widely.Traditional medical metal material has stainless steel, cobalt-base alloy, titanium or titanium alloy, tantalum niobium zirconium alloy and precious metal etc., permanent reservation in vivo behind their implant into body, existing discover under the physiology corrosive environment life-time service not only their physical strengths own descend may cause implanting and lost efficacy, and the metal ion of stripping (as V, Cu, Ni, Co, Al, Zn etc.) can make cell Inflammatory response or necrosis occur, therefore presses for the bio-medical metallic substance of a kind of novel non-toxic degradable of exploitation.
Magnesium and magnesium alloy have incomparable advantage as this new bio metallic substance.At first, magnesium is the interior positive ion of cell that human body is only second to potassium, and its participates in a series of metabolic processes in body, becomes human body interior every day of required amount of magnesium above 350mg, and the magnesium alloy materials that implants can not produce toxic side effect; Secondly, magnesium and magnesium alloy can be by the complete degraded and absorbed of human body after a few weeks or months after the implantation, and this has just in time met the design original intention of materials such as intravascular stent, hone lamella " urgent need, interim ".Therefore, magnesium and magnesium alloy have huge development potentiality as bio-medical material, have caused increasing people's attention and research.But traditional magnesium and magnesium alloy exist, and intensity is low, plasticity is poor, (Al, Zn etc.) etc. are not enough to contain poisonous element, has limited their application in the bio-medical field.
Summary of the invention
Be applied in the deficiency that the bio-medical field exists at existing magnesium alloy technology, the purpose of this invention is to provide that a kind of intensity height, plasticity are good, degradable, nontoxic new bio medical magnesium alloy.
Another object of the present invention provides the preparation method of described magnesium alloy.
For achieving the above object, the technical solution used in the present invention is: a kind of high intensity degradable biological medical magnesium alloy, and each component of this magnesium alloy and weight percent thereof are: the Y of 2.5-6.5%; The Nd of 1.2-3.5%; The Zr of 0.4-0.8%; Surplus is a magnesium.
Further, wherein the weight percent of Nd and Y total content is 4.5-8.5%; The total amount of impurity element Fe, Al, Cu, Si and Ni is not more than 0.05% in the magnesium alloy simultaneously.
The preparation method of magnesium alloy of the present invention comprises the steps:
(1) the preparation raw material is selected pure magnesium, Mg-Y, Mg-Nd and Mg-Zr master alloy for use, remove pure magnesium, Mg-Y, Mg-Nd and Mg-Zr master alloy surface scale earlier, put into acetone soln then and carry out ultrasonic cleaning, according to the weight percentage of Y, Nd and Zr in three kinds of master alloys with need in the magnesium alloy of preparation the weight percent of Y, Nd and Zr to get the raw materials ready, and with raw material preheating to 473-573K;
(2) under protective atmosphere, the pure magnesium intensification of preheating is made its whole fusings, control magnesium liquid temp is 1053-1073K, slowly add Mg-Y, Mg-Nd, Mg-Zr master alloy successively, a kind of under just beginning to add after having only current a kind of master alloy to melt fully, the continuous stirring makes it even in the adition process;
(3) (2) the alloy melt temperature that obtains of step is adjusted to 1023-1033K, strengthen power of agitator, be sprinkled into refining agent refining 5-8 minute of furnace charge gross weight 1-2%, then alloy melt is warming up to 1053-1073K, stop to stir, left standstill 10-20 minute;
(4) the alloy melt temperature is reduced to 973-993K; skim surface scum; under protective atmosphere, adopt the cast of copper mould; adopt quick copper mold cooling after the cast immediately; heat-eliminating medium is liquid nitrogen, saturated salt solution or mixture of ice and water, and the content of icing in the mixture of ice and water can guarantee to have all the time in the process of cooling ice to exist.
Described protective atmosphere is for by volumn concentration being the mixed gas that the SF6 of the argon gas of 99.2-99.5% and 0.5-0.8% forms; Described refining agent is the RJ-5 flux of 90-95% and the anhydrous Na of 5-10% by weight percentage
2B
4O
7Powder mixes forms.
Magnesium-rare earth has the potentiality that become the new bio medical material.Because the configuration of extra-nuclear electron of rare earth element uniqueness plays effects such as purifying melt, crystal grain thinning, raising castability in castingprocesses, have significant solid solution and ageing strengthening effect in magnesium alloy, can improve the over-all properties of magnesium alloy effectively.When adding two or more rare earth elements,, can also produce additional strengthening effect because the interaction between the rare earth element can be reduced in the solid solubility in the magnesium each other.Rare earth also is the intravital trace element of people, and the low dosage rare earth element is not only harmless, also can promote organism growing development, helps the enhance immunity function, has anti-oxidant and anti-mutagenic activity.
Specifically, the invention has the beneficial effects as follows:
(1) in pure magnesium, adds proper amount of rare-earth Y and Nd simultaneously, can improve the mechanical property and the processing characteristics of alloy, do not introduce harmful element again, can satisfy the requirement of bio-medical metallic substance fully.
(2) Mg-Y-Nd-Zr magnesium alloy crystal grain of the present invention is tiny, and size has only 20-40 μ m, and composition is even, reduced in segregation.Under the room temperature without the cast alloy tensile strength of heat treatment reinforcement and work strengthening more than 220Mpa, unit elongation is more than 5%.
(3) Mg-Y-Nd-Zr magnesium alloy of the present invention can be at simulated body fluid (simulated body fluid, SBF) corrosion degraded in, and the magnesium alloy of different Nd, Y content is corrosion weight loss speed difference in SBF, experimental result shows when content that the content as Nd in the alloy is about 2.0wt.%, Y is 3.0-5.0wt.%, the corrosion weight loss speed minimum of alloy.This explanation can be controlled the degradation rate of alloy by the content of adjusting Nd and Y, to satisfy the requirement of different implants.
(4) the present invention has the advantage that preparation technology is simple, equipment requirements is low, production cost is low.
Description of drawings
Fig. 1 (a), Fig. 1 (b) are high intensity degradable biological medical magnesium alloy (embodiment 1, embodiment 2) microcosmic metallographic structure photo;
Fig. 2 is a mechanical curves under high intensity degradable biological medical magnesium alloy (embodiment 1, the embodiment 2) normal temperature;
Fig. 3 is high intensity degradable biological medical magnesium alloy (embodiment 1, embodiment 2) corrosion weight loss rate curve in SBF;
Fig. 4 is that high intensity degradable biological medical magnesium alloy (embodiment 1) corrodes degraded back settling XRD diffracting spectrum fully in SBF.
Embodiment
Below by specific embodiment technical solution of the present invention is elaborated.
The present invention adopts first component of Y (yttrium) as alloy, because the solid solubility of Y in magnesium is about 2wt.% under the normal temperature, for guaranteeing that alloy can obtain enough timeliness precipitation strength and solid solution strengthening effect, the add-on of Y is not less than 2.5wt.%, simultaneously for fear of alloy embrittlement, and bring too much Y behind the implant into body into, the add-on of Y is no more than 6.5wt.%; Adopt second component of Nd (neodymium) as alloy, the solid solubility of Nd in magnesium is about 0.8wt.% under the normal temperature, and in order to guarantee strengthening effect, the add-on of Nd is not less than 1.2wt.%, because the maximum solid solution degree of Nd in magnesium is 3.6%, the add-on of Nd is not higher than 3.5wt.%; Consider influencing each other of Y in the magnesium, Nd solid solubility, should guarantee that alloy is fully strengthened, distortion brings difficulty to following process can not cause the undue embrittlement of alloy again, and Nd and Y total content are limited to 4.5-8.5wt.% in the alloy; Adopt Zr (zirconium) as grain-refining agent, generally the content of Zr is 0.4-0.8wt.% in the magnesium alloy.
Therefore, each component of a kind of high intensity degradable biological medical magnesium alloy provided by the invention and weight percent thereof are: 2.5-6.5%Y, and 1.2-3.5%Nd, 0.4-0.8%Zr, surplus is a magnesium, wherein the weight percent of Nd and Y total content is 4.5-8.5%.The gross weight of impurity element Fe, Al, Cu, Si and Ni≤0.05% in the magnesium alloy.
The preparation method of magnesium alloy of the present invention comprises the steps:
(1) the preparation raw material is selected pure magnesium, Mg-Y, Mg-Nd and Mg-Zr master alloy for use, remove pure magnesium, Mg-Y, Mg-Nd and Mg-Zr master alloy surface scale earlier, put into acetone soln then and carry out ultrasonic cleaning, according to the weight percentage of Y, Nd and Zr in three kinds of master alloys (needing to consider the recovery rate of Y, Nd and Zr in three kinds of master alloys simultaneously) with need in the magnesium alloy of preparation the weight percent of Y, Nd and Zr to get the raw materials ready, and with raw material preheating to 473-573K.
(2) under protective atmosphere, the pure magnesium intensification of preheating is made its whole fusings, control magnesium liquid temp is 1053-1073K, slowly add Mg-Y, Mg-Nd, Mg-Zr master alloy successively, a kind of under just beginning to add after having only current a kind of master alloy to melt fully, the continuous stirring makes it even in the adition process;
(3) (2) the alloy melt temperature that obtains of step is adjusted to 1023-1033K, strengthen power of agitator, be sprinkled into refining agent refining 5-8 minute of furnace charge gross weight 1-2%, then alloy melt is warming up to 1053-1073K, stop to stir, left standstill 10-20 minute;
(4) the alloy melt temperature is reduced to 973-993K, skim surface scum, under protective atmosphere, adopt the cast of copper mould, cooling fast immediately after the cast.
This preparation method is mingled with for fear of the slag that uses flux protection to bring, and adopts argon gas and 0.5%-0.8% volume SF
6Mixed gas as protective atmosphere; Adopt the special-purpose RJ-5 flux of magnesium-rare earth as main refining agent,, in RJ-5 flux, add the 8wt.% anhydrous Na for more effective deironing
2B
4O
7
This preparation method for evenly composition, crystal grain thinning, improve microstructure, further improve the obdurability of magnesium alloy, adopt flash set technology casting bulk alloy.Cooling fast immediately after alloy melt is poured into a mould in the thin-walled copper mold, in order to improve speed of cooling, heat-eliminating medium adopts liquid nitrogen, or saturated salt solution, or mixture of ice and water.
Below by two embodiment the present invention is described in detail.
The component of magnesium alloy and weight percent thereof are: 4%Y, and 2%Nd, 0.4%Zr, the total amount of impurity element Fe, Al, Cu, Si and Ni is not more than 0.05%, and surplus is a magnesium.
The detailed process of preparation 2Kg Mg-4Y-2Nd-0.4Zr magnesium alloy is as follows:
(1) removes pure magnesium (magnesium ingot) and three kinds of master alloy surface scales with the mechanical grinding method, to expect that then piece puts into acetone soln and carry out ultrasonic cleaning, according to the weight percentage of Y, Nd and Zr in three kinds of master alloys with need in the magnesium alloy of preparation the weight percent of Y, Nd and Zr to get the raw materials ready: 254gMg-31.5%Y master alloy (be that the weight percent of Y in the Mg-Y master alloy is 31.5%, down with), 125.8gMg-31.8%Nd master alloy, 25.6gMg-31.3%Zr master alloy and the pure magnesium of 1594.6g.To expect that piece and refining agent put into baking oven and be preheated to 473K, and melting be put into box-type furnace with instrument be preheated to 573K.
(2) under the protection of the mixed gas of argon gas and 0.5%-0.8% volume SF6, the pure magnesium ingot of preheating is added the plumbago crucible that capacity is 3kg, medium-frequency induction furnace heats up and makes its whole fusings.Control magnesium liquid temp slowly adds Mg-Y, Mg-Nd, Mg-Zr master alloy successively at 1053-1073K, just begins to add after having only current a kind of master alloy to melt fully a kind of down, constantly carries out induction stirring in the adition process and makes its homogenizing.
(3) the alloy melt temperature is adjusted to 1023-1033K, strengthen power of agitator, make the melt vigorous agitation but do not splash, constantly be sprinkled into the RJ-5+8wt.% anhydrous Na of quality of furnace charge total amount about 1% at the melt crest
2B
4O
7Refining agent, refining 6 minutes.Then melt is warming up to 1053-1073K, turns off stirring, left standstill 10 minutes.
(4) the alloy melt temperature is reduced to about 993K, skim surface scum, under gas shield, adopt the cast of cylindricality copper mould, immediately copper mold is put into saturated salt solution after the cast and cool off fast.
The head and the afterbody of excision ingot casting keep middle portion and railway carriage.Intercepting centre one fritter is made metallographic specimen, observes the alloy casting state tissue under the OLYMPUS metaloscope; According to Chinese national standard GB/T228-2002 alloy cast ingot is machined to the circular section standard test specimen, on CMT5105 type microcomputer control electronics universal testing machine, carries out the room-temperature mechanical property tension test.Intercepting fritter alloy is made 10 * 10 * 2mm sample through the 1400# sand papering, putting into simulated body fluid (SBF) in acetone behind the ultrasonic cleaning 10min soaks, measure its erosion rate with weight-loss method, SBF solution keeps constant temperature 37 ℃ ± 0.5 in the immersion process, measures sample with X-ray diffractometer (XRD) and corrodes the sedimental thing phase composite in back fully.
The present embodiment alloy structure is even, and crystal grain is tiny, and mean sizes is at 20-30 μ m, and Fig. 1 (a) is seen in its metallographic structure.This cast alloy has mechanical property preferably, and tensile strength is 242Mpa under the room temperature, and unit elongation is 7.5%, and corresponding stress strain curve is listed on the sequence number 1 of Fig. 2.This alloy has corrosion resistance preferably, and the rate of weight loss that soaks after 42 days in SBF is 6.4%, and its corrosion weight loss curve is listed in Fig. 3, and the settling that this alloy of XRD test shows corrodes after the degraded fully has only Mg (OH)
2, it the results are shown in accompanying drawing 4.
The component of magnesium alloy and weight percent thereof are: 5%Y, and 3%Nd, 0.6%Zr, the total amount of impurity element Fe, Al, Cu, Si and Ni is not more than 0.05%, and surplus is a magnesium.
The fusion process of preparation 1Kg Mg-5Y-3Nd-0.6Zr magnesium alloy is with reference to embodiment 1, difference be to be equipped with raw material be 158.7g Mg-31.5%Y master alloy, 94.3g Mg-31.8%Nd master alloy, 19.2gMg-31.3%Zr master alloy and the pure magnesium of 727.8g.
The microstructure of alloy, mechanical property tension test, corrosion weight loss are tested all with embodiment 1.Experiment shows that the present embodiment alloy grain is more tiny, the compound showed increased on the crystal boundary; This strength of alloy significantly improves, and reaches 270Mpa, but unit elongation has decline slightly, is 6.4%; The rate of weight loss that this alloy soaked in SBF after 42 days is 7.9%.Its metallographic structure, stress strain curve and corrosion weight loss curve result list in accompanying drawing 1 (b), accompanying drawing 2 and accompanying drawing 3 respectively.
Claims (6)
1. high intensity degradable biological medical magnesium alloy, it is characterized in that: each component of this magnesium alloy and weight percent thereof are: the Y of 2.5-6.5%; The Nd of 1.2-3.5%; The Zr of 0.4-0.8%; The total amount of impurity element Fe, Al, Cu, Si and Ni is not more than 0.05%, and surplus is a magnesium.
2. high intensity degradable biological medical magnesium alloy according to claim 1 is characterized in that: the weight percent of Nd and Y total content is 4.5-8.5% in this magnesium alloy.
3. the preparation method of high intensity degradable biological medical magnesium alloy according to claim 1, it is characterized in that: it comprises the steps:
(1) the preparation raw material is selected pure magnesium, Mg-Y, Mg-Nd and Mg-Zr master alloy for use, remove pure magnesium, Mg-Y, Mg-Nd and Mg-Zr master alloy surface scale earlier, put into acetone soln then and carry out ultrasonic cleaning, again as required the preparation the magnesium alloy composition get the raw materials ready, and with raw material preheating to 473-573K;
(2) under protective atmosphere, the pure magnesium intensification of preheating is made its whole fusings, control magnesium liquid temp is 1053-1073K, slowly add Mg-Y, Mg-Nd, Mg-Zr master alloy successively, a kind of under just beginning to add after having only current a kind of master alloy to melt fully, the continuous stirring makes it even in the adition process;
(3) the alloy melt temperature that (2) step was obtained is adjusted to 1023-1033K, is sprinkled into refining agent refining 5-8 minute of furnace charge gross weight 1-2% and constantly stirring, then alloy melt is warming up to 1053-1073K, stops to stir, and leaves standstill 10-20 minute;
(4) the alloy melt temperature is reduced to 973-993K, skim surface scum, under protective atmosphere, adopt the cast of copper mould, cooling fast immediately after the cast.
4. the preparation method of high intensity degradable biological medical magnesium alloy according to claim 3 is characterized in that: described protective atmosphere is for being the argon gas of 99.2-99.5% and the SF of 0.5-0.8% by volumn concentration
6The mixed gas of forming.
5. according to the preparation method of claim 3 or 4 described high intensity degradable biological medical magnesium alloys, it is characterized in that: described refining agent is the RJ-5 flux of 90-95% and the anhydrous Na of 5-10% by weight percentage
2B
4O
7Powder mixes forms.
6. the preparation method of high intensity degradable biological medical magnesium alloy according to claim 5, it is characterized in that: adopt quick copper mold cooling after the cast immediately, heat-eliminating medium is liquid nitrogen, saturated salt solution or mixture of ice and water, and the content of icing in the mixture of ice and water can guarantee to have all the time in the process of cooling ice to exist.
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| CN102294054A (en) * | 2010-06-24 | 2011-12-28 | 乐普（北京）医疗器械股份有限公司 | Bioabsorbable compound stent and preparation method thereof |
| CN103103426A (en) * | 2012-11-13 | 2013-05-15 | 苏州谷力生物科技有限公司 | Preparation process of seamless pipe for magnesium alloy vascular stent |
| CN103826668A (en) * | 2011-09-06 | 2014-05-28 | 斯特里克斯股份公司 | Method for producing a medical implant from a magnesium alloy |
| CN104975214A (en) * | 2015-07-31 | 2015-10-14 | 重庆大学 | High-plasticity magnesium alloy and preparation method thereof |
| CN105126240A (en) * | 2014-06-03 | 2015-12-09 | 陈彦彪 | Degradable ultrafine needle piece |
| CN105177384A (en) * | 2015-08-28 | 2015-12-23 | 上海交通大学 | Mg-RE-Zr system multielement magnesium alloy and preparation method thereof |
| CN105950931A (en) * | 2016-07-20 | 2016-09-21 | 肖旅 | High-strength and high-hardness magnesium alloy in controllable reaction with water, and manufacturing method of component thereof |
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| CN107962170A (en) * | 2016-10-19 | 2018-04-27 | 中国科学院金属研究所 | A kind of anisotropy bio-medical directional solidification magnesium-zinc alloy material preparation method |
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| CN109266889A (en) * | 2018-12-05 | 2019-01-25 | 四川大学 | A kind of composite refining method of the magnesium alloy containing zirconium |
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- 2009-05-08 CN CN2009101038151A patent/CN101550510B/en not_active Expired - Fee Related
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| CN103103426A (en) * | 2012-11-13 | 2013-05-15 | 苏州谷力生物科技有限公司 | Preparation process of seamless pipe for magnesium alloy vascular stent |
| CN105126240A (en) * | 2014-06-03 | 2015-12-09 | 陈彦彪 | Degradable ultrafine needle piece |
| CN107427603A (en) * | 2015-03-11 | 2017-12-01 | 波士顿科学国际有限公司 | Bioerodible magnesium alloy micro-structural for interior prosthese |
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| CN107962170A (en) * | 2016-10-19 | 2018-04-27 | 中国科学院金属研究所 | A kind of anisotropy bio-medical directional solidification magnesium-zinc alloy material preparation method |
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