CN104694848B - A kind of biodegradable quaternary ferrous alloy material and preparation method thereof - Google Patents
A kind of biodegradable quaternary ferrous alloy material and preparation method thereof Download PDFInfo
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- CN104694848B CN104694848B CN201510042513.3A CN201510042513A CN104694848B CN 104694848 B CN104694848 B CN 104694848B CN 201510042513 A CN201510042513 A CN 201510042513A CN 104694848 B CN104694848 B CN 104694848B
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- 239000000956 alloy Substances 0.000 title claims abstract description 38
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical group [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 238000005275 alloying Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 6
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 9
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 61
- 229910052742 iron Inorganic materials 0.000 description 23
- 238000005260 corrosion Methods 0.000 description 20
- 230000007797 corrosion Effects 0.000 description 20
- 239000011572 manganese Substances 0.000 description 12
- 229910052748 manganese Inorganic materials 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 9
- 229960000074 biopharmaceutical Drugs 0.000 description 9
- 238000002156 mixing Methods 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 6
- 229910001566 austenite Inorganic materials 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910000754 Wrought iron Inorganic materials 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910015136 FeMn Inorganic materials 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 210000002808 connective tissue Anatomy 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
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Abstract
The invention discloses a kind of biodegradable quaternary ferrous alloy material, its chemical composition is：Fe 30Mn nX kY, n, k are mass percent (wt.%), wherein 1%≤n≤3%, 0.5%≤k≤3%；X is the one kind in metallic alloying element, including Mg, Zn, Ag；Y is the one kind in non-metallic alloying elements, including C, Si, S.The preparation method of above-mentioned biodegradable quaternary ferrous alloy material is to mix the metal of mentioned component and non-metal powder, by 20～25:1 ratio of grinding media to material carries out ball milling in adding liquid nitrogen type ball mill, rotating speed is 400～450r/min, often 30min is stalled after operating 120min, 16～24 h of ball milling, by the powder pre-molding for obtaining, then in 4～6GPa, 30～60min of heat-insulation pressure keeping at 1200～1600 DEG C, the degradable quaternary ferrous alloy material of synthesising biological.Preparation process is simple of the present invention, low cost, safety non-toxic, degradation rate can be significantly improved.
Description
Technical field
The present invention relates to a kind of degradable alloy material and preparation method thereof.
Background technology
At present, study hotter degradable metal material and be concentrated mainly on pure magnesium, magnesium-base metal alloy and pure iron, iron-based gold
Category two general orientation of alloy.Compared with magnesium base alloy, pure iron and its alloy have excellent mechanical performance, and do not have in degradation process
There is evolving hydrogen reaction.Additionally, Fe is also extremely important trace element in human body, Related Experimental Study shows, pure iron or iron
Alloy has certain biological safety as implant.Preferably biocompatibility is also the big excellent of pure iron and its alloy
Point, according to some current achievements in research, including the extracorporeal blood experiment of pure iron and ferroalloy, cytotoxicity experiment and animal body
Interior experiment etc., shows which has preferable biocompatibility.
The corrosion degradation process of iron-based biomaterial is influenced by factors, mainly including its chemical composition, process side
Formula, residing environment etc..In terms of the corrosion resistance of iron and its alloy is improved, existing many scholars have carried out substantial amounts of research
Work, and achievement is significantly, but with regard to reduce iron and its alloy corrosion resistance, improve its degradation rate work it is rare
Report.The slower degradation rate of iron is its topmost restriction bottleneck as biodegradable metals material.
In order to improve the degradation rate of pure iron, researchers have carried out substantial amounts of exploration and have attempted, the normal electrode of Mn
Potential is lower than Fe, and many researchers are locked in sight on the degradation rate that can Mn improve Fe as alloying element.Such as
The powder metallurgic method such as Hermawan H is prepared for Fe- (25%～35%) Mn alloys, have studied alloying first to iron-based material
The impact of material, it is found that its degradation rate is compared with pure iron and be increased slightly, but the requirement from Clinical practice also has with a distance from larger,
The raising of iron-based biomaterial degradation rate also has much room.
The content of the invention：
It is an object of the invention to provide a kind of preparation process is simple, with short production cycle, safety non-toxic, drop can be significantly improved
Biodegradable quaternary ferrous alloy material of solution speed and preparation method thereof.The present invention is mainly by adding in Fe, Mn powder
Plus a kind of metallic element and a kind of nonmetalloid, compressing tablet after ball milling, high-pressure synthesis iron-based biology alloy.
The biodegradable quaternary ferrous alloy material of the present invention, its chemical composition is：Fe-30Mn-nX-kY, n, k are matter
Amount percentage (wt.%), wherein 1%≤n≤3%, 0.5%≤k≤3%；During X is metallic alloying element, including Mg, Zn, Ag
One kind；Y is the one kind in non-metallic alloying elements, including C, Si, S.Mentioned component is purity metal >=99.9%
Or non-metal powder.
The preparation method of above-mentioned biodegradable quaternary ferrous alloy material：
The metal of mentioned component and non-metal powder are mixed, by 20～25:During 1 ratio of grinding media to material adds liquid nitrogen type ball mill
Ball milling is carried out, rotating speed is 400～450r/min, stalls 30min, 16～24h of ball milling, by the powder for obtaining after the 120min that often operates
Pre-molding, then using cubic hinge press in 4～6GPa, 30～60min of heat-insulation pressure keeping, synthesising biological at 1200～1600 DEG C
Degradable quaternary ferrous alloy material.
Active metal element M g, Zn of present invention addition, is allowed to solid solution by way of ball milling and is entered in Fe, reduce Fe's
Standard electrode potential, accelerates the corrosion of Fe；Inert metal elements A g of addition, is allowed to produce little and homodisperse negative electrode
The intermetallic compound of effect and improve galvanic corrosion；Nonmetalloid C, Si, S of addition, is human essential elementses, wherein
The presence of C element may participate in the phase in version of Fe, and Si can promote the formation of connective tissue and bone, and S is also constant necessary to body
One of element.
The present invention is had the advantage that compared with prior art：
1st, preparation process is simple, it is with short production cycle, cubic hinge press HTHP is adopted after pressed powder obtained in ball milling
Under the conditions of one-shot forming.
2nd, safety non-toxic, the alloying element of addition are human essential elementses, can improve degradation rate, can promote bone again
Bone grows, and supplements body indispensable element.
3rd, compared with FeMn bianry alloys and FeMn-x ternary alloy three-partalloys, its degradation rate improves two orders of magnitude, and machine
Tool is functional.
Description of the drawings
Fig. 1 is the XRD of Fe30Mn3Mg0.5C prepared by the embodiment of the present invention 1.
Fig. 2 is the corrosion electric current density figure of Fe30Mn3Zn0.5Si prepared by the embodiment of the present invention 2.
Fig. 3 is the corrosion electric current density figure of Fe30Mn3Ag 0.5S prepared by the embodiment of the present invention 3.
Fig. 4 is the corrosion electric current density figure of Fe30Mn1Zn3Si prepared by the embodiment of the present invention 4.
Fig. 5 is the corrosion electric current density figure of Fe30Mn1Ag3C prepared by the embodiment of the present invention 5.
Fig. 6 is the optical electron microscope figure of Fe30Mn1Mg3S prepared by the embodiment of the present invention 6.
Fig. 7 is the corrosion electric current density figure of Fe30Mn2Mg 1.5Si prepared by the embodiment of the present invention 7.
Fig. 8 is the corrosion electric current density figure of Fe30Mn1.5Zn 2C prepared by the embodiment of the present invention 8.
Fig. 9 is the corrosion electric current density figure of Fe30Mn2Ag 2.5S prepared by the embodiment of the present invention 9.
Specific embodiment：
Embodiment 1
Powder purity is >=99.9%, the Fe that mass percent is 66.5%, 30% Mn, 3% Mg and 0.5%
C mixing, by ratio of grinding media to material 20:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, rotating speed 400r/min, per ball milling 120min,
Stop 30min, continue ball milling 20h, collect the pre-molding under 6MPa of the alloyed powder after ball milling, be then placed in cubic hinge press and exist
4GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 30min synthesising biologicals at 1200 DEG C.
As seen from Figure 1, biodegradable quaternary iron-based of the material composition that high pressure is prepared for Fe30Mn3Mg0.5C
Alloy material, its phase composition are the oxide of austenite structure and manganese, for the Fe30Mn of single phase austenite tissue, raw
Into the second phase, the corrosion rate of iron-based body is accelerated.
Embodiment 2
Powder purity is >=99.9%, the Fe that mass percent is 66.5%, 30% Mn, 3% Zn and 0.5
Si mixes, by ratio of grinding media to material 25:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, rotating speed 450r/min, per ball milling 120min,
Stop 30min, continue ball milling 24h, collect the pre-molding under 6MPa of the alloyed powder after ball milling, be then placed in cubic hinge press and exist
6GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 60min synthesising biologicals at 1600 DEG C.
As seen from Figure 2, biodegradable four rod iron of the material composition that high pressure is prepared for Fe30Mn3Zn0.5Si
Base alloy material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.032mAcm-2。
Embodiment 3
Powder purity is >=99.9%, the Fe that mass percent is 66.5%, 30% Mn, 3% Ag and 0.5
S mixes, by ratio of grinding media to material 20:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, and rotating speed 400r/min, per ball milling 120min, stops
30min, continues ball milling 24h, collects the pre-molding under 6MPa of the alloyed powder after ball milling, is then placed in cubic hinge press and exists
5GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 60min synthesising biologicals at 1400 DEG C.
Biodegradable quaternary iron-based of the material composition that high pressure is prepared as seen from Figure 3 for Fe30Mn3Ag0.5S
Alloy material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.035mAcm-2。
Embodiment 4
Powder purity is >=99.9%, the Fe that mass percent is 66%, 30% Mn, the Si of 1% Zn and 3%
Mixing, by ratio of grinding media to material 25:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, and rotating speed 450r/min, per ball milling 120min, stops
30min, continues ball milling 16h, collects the pre-molding under 6MPa of the alloyed powder after ball milling, is then placed in cubic hinge press and exists
4GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 60min synthesising biologicals at 1200 DEG C.
As seen from Figure 4, biodegradable quaternary iron-based of the material composition that high pressure is prepared for Fe30Mn1Zn3Si
Alloy material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.031mAcm-2。
Embodiment 5
Powder purity is >=99.9%, the Fe that mass percent is 66%, 30% Mn, the C of 1% Ag and 3%
Mixing, by ratio of grinding media to material 20:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, and rotating speed 450r/min, per ball milling 120min, stops
30min, continues ball milling 20h, collects the pre-molding under 6MPa of the alloyed powder after ball milling, is then placed in cubic hinge press and exists
6GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 30min synthesising biologicals at 1600 DEG C.
As seen from Figure 5, the material composition that high pressure is prepared is closed for the biodegradable quaternary iron-based of Fe30Mn1Ag3C
Golden material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.037mAcm-2。
Embodiment 6
Powder purity is >=99.9%, the Fe that mass percent is 66%, 30% Mn, the S of 1% Mg and 3%
Mixing, by ratio of grinding media to material 25:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, and rotating speed 450r/min, per ball milling 120min, stops
30min, continues ball milling 16h, collects the pre-molding under 6MPa of the alloyed powder after ball milling, is then placed in cubic hinge press and exists
4GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 30min synthesising biologicals at 1600 DEG C.
As seen from Figure 6, biodegradable quaternary ferrous alloy of the material composition that high pressure is prepared for Fe30Mn1Mg3S
Material, optical texture is by austenite and the second phase composition.
Embodiment 7
Powder purity is >=99.9%, the Fe that mass percent is 66.5%, 30% Mn, 2% Mg and 1.5%
Si mixing, by ratio of grinding media to material 23:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, rotating speed 430r/min, per ball milling
120min, stops 30min, continues ball milling 20h, collects the pre-molding under 6MPa of the alloyed powder after ball milling, is then placed in cubic apparatus
Press in 5GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 40min synthesising biologicals at 1500 DEG C.
As seen from Figure 7, biodegradable four rod iron of the material composition that high pressure is prepared for Fe30Mn2Mg1.5Si
Base alloy material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.035mAcm-2。
Embodiment 8
Powder purity is >=99.9%, the Fe that mass percent is 66.5%, 30% Mn, 1.5% Zn and 2%
C mixing, by ratio of grinding media to material 25:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, rotating speed 425r/min, per ball milling 120min,
Stop 30min, continue ball milling 20h, collect the pre-molding under 6MPa of the alloyed powder after ball milling, be then placed in cubic hinge press and exist
5GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 50min synthesising biologicals at 1500 DEG C.
As seen from Figure 8, biodegradable quaternary iron-based of the material composition that high pressure is prepared for Fe30Mn1.5Zn2C
Alloy material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.036mAcm-2。
Embodiment 9
Powder purity is >=99.9%, the S of Fe, 30%Mn, 2%Ag that mass percent is 65.5% and 2.5%
Mixing, by ratio of grinding media to material 22:1 ratio adds liquid nitrogen type ball crusher to carry out ball milling, and rotating speed 450r/min, per ball milling 120min, stops
30min, continues ball milling 22h, collects the pre-molding under 6MPa of the alloyed powder after ball milling, is then placed in cubic hinge press and exists
5.5GPa, the degradable quaternary ferrous alloy material of heat-insulation pressure keeping 45min synthesising biologicals at 1450 DEG C.
As seen from Figure 9, biodegradable quaternary iron-based of the material composition that high pressure is prepared for Fe30Mn2Ag2.5S
Alloy material, corrosion electric current density relative to Fe30Mn 3.6 × 10-4mA·cm-2, brought up to 0.035mAcm-2。
Claims (1)
1. a kind of preparation method of biodegradable quaternary ferrous alloy material, the biodegradable quaternary ferrous alloy material
Chemical composition be：Fe-30Mn-nX-kY, 30, n, k be mass percent (wt.%), wherein 1≤n≤3,0.5≤k≤3；X
For the one kind in metallic alloying element, including Mg, Zn, Ag；Y is the one kind in non-metallic alloying elements, including C, Si, S, described
Composition is equal >=99.9% metal of purity or non-metal powder, it is characterised in that：By the metal of mentioned component and nonmetallic
Powder mixes, by 20～25:1 ratio of grinding media to material carries out ball milling in adding liquid nitrogen type ball mill, rotating speed is 400～450r/min, often
30min, 16～24h of ball milling are stalled after operating 120min, by the powder pre-molding for obtaining, then in 4～6GPa, 1200～
30～60min of heat-insulation pressure keeping at 1600 DEG C, the degradable quaternary ferrous alloy material of synthesising biological.
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| CN107648676A (en) * | 2017-11-08 | 2018-02-02 | 谭思暄 | A kind of degradable iron-based angiocarpy bracket material and preparation method thereof |
| US10512495B2 (en) | 2017-12-28 | 2019-12-24 | Industrial Technology Research Institute | Method for fabricating medical device and applications thereof |
| CN108677099B (en) * | 2018-04-17 | 2020-06-05 | 西南大学 | Medical degradable Fe-Mn-Ag alloy material and preparation and application thereof |
| CN110952038A (en) * | 2019-11-27 | 2020-04-03 | 苏州森锋医疗器械有限公司 | Biodegradable iron alloy, preparation method and device |
| IT202000003611A1 (en) | 2020-02-21 | 2021-08-21 | Getters Spa | Bioabsorbable pseudoelastic Fe-Mn-X-Y alloys for medical implants |
| CN113755738A (en) * | 2021-09-10 | 2021-12-07 | 广东粤海华金科技股份有限公司 | Degradable iron-based alloy material and preparation method and application thereof |
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| EP2399620B1 (en) * | 2010-06-28 | 2016-08-10 | Biotronik AG | Implant and method for producing the same |
| CN102776435B (en) * | 2011-05-13 | 2014-12-10 | 中国科学院金属研究所 | Degradable Fe-Mn-C ternary iron alloy material and its application |
| US20130243699A1 (en) * | 2011-12-07 | 2013-09-19 | Regents Of The University Of Minnesota | Biodegradable Magnetic Nanoparticles and Related Methods |
| US20150182674A1 (en) * | 2012-07-10 | 2015-07-02 | Fort Wayne Metals Research Products Corporation | Biodegradable composite wire for medical devices |
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