CN104711473A - Nonmagnetic biomedical implant material and preparation method thereof - Google Patents
Nonmagnetic biomedical implant material and preparation method thereof Download PDFInfo
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- CN104711473A CN104711473A CN201510043123.8A CN201510043123A CN104711473A CN 104711473 A CN104711473 A CN 104711473A CN 201510043123 A CN201510043123 A CN 201510043123A CN 104711473 A CN104711473 A CN 104711473A
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- single phase
- implant material
- phase austenite
- liquid nitrogen
- nonmagnetic
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- 239000007943 implant Substances 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 38
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 34
- 239000010959 steel Substances 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 23
- 238000005097 cold rolling Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 62
- 229910052742 iron Inorganic materials 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 150000001722 carbon compounds Chemical class 0.000 description 4
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000012620 biological material 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
- 239000012141 concentrate Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004151 rapid thermal annealing Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
Abstract
A nonmagnetic biomedical implant material is single phase austenite, and comprises 0.6-1.5wt% of C, 13-35wt% of Mn, 0.5-0.6wt% of Si, 0.5-2wt% of Ca, 0.5-2wt% of Zn, 0.5-2wt% of Ag, 0.016-0.020wt% of S, 0.022-0.025wt% of P, and the balance of Fe. A preparation method of the nonmagnetic biomedical implant material comprises the following steps: carrying out three-pass liquid nitrogen cold rolling on the above single phase austenite steel with the press amounts of 10-20%, 8-15% and 2-5% respectively; and carrying out two-stage annealing treatment: heating at a rate of 5-40DEG C/min to 200-300DEG C, carrying out heat insulation for 60-180min, cooling in a furnace, heating at a rate of 30-40DEG C/min to 600-800DEG C, carrying out heat insulation for 20-40min, and cooling in the furnace to prepare the nonmagnetic biomedical implant material. The nonmagnetic biomedical implant material has the advantages of short production period, low cost, and obviously improved integral degradation rate.
Description
Technical field
The present invention relates to a kind of degradable metal material, particularly a kind of medical embedded material and preparation method thereof.
Background technology
At present, study hotter degradable metal material and mainly concentrate on pure magnesium, magnesium-base metal alloy and pure iron, ferrous metals alloy two general orientation.Compared with Magnuminium, pure iron and alloy thereof have excellent mechanical property, and in degradation process, do not have evolving hydrogen reaction to occur.In addition, Fe is also extremely important trace element in human body, and Related Experimental Study shows, pure iron or iron alloy have certain biological safety as implant.Good biocompatibility is also a large advantage of pure iron and alloy thereof, according to some current achievements in research, comprises the extracorporeal blood experiment of pure iron and iron alloy, cytotoxicity experiment and animal experiment in vivo etc., all shows that it has good biocompatibility.
The corrosion degradation process of iron is subject to various factors, mainly comprises its chemical composition, processing mode, residing environment etc.In the corrosion resistance improving iron and alloy thereof, have a lot of scholar carry out a large amount of research work, but about reducing the corrosion resistance of iron and alloy thereof, improving the rare report of work of its degradation rate.The slower degradation rate of iron is its topmost restriction bottleneck as degradable biomaterial.
Summary of the invention:
The object of the present invention is to provide a kind of with short production cycle, cost is low, degradation rate is high non-magnetic iron-based biological and medicinal implant material and preparation method thereof.The present invention mainly utilizes that three liquid nitrogen are cold rolling adds second annealing process to prepare the biological steel of high degradation rate.
Non-magnetic iron-based biological and medicinal implant material of the present invention is single phase austenite, its chemical composition mass percent is: C:0.6 ~ 1.5%, Mn:13 ~ 35%, Si:0.5 ~ 0.6%, Ca:0.5 ~ 2%, Zn:0.5 ~ 2%, Ag:0.5 ~ 2%, S:0.016 ~ 0.020%, P:0.022 ~ 0.025%, and all the other are Fe.
The preparation method of above-mentioned non-magnetic iron-based biological and medicinal implant material:
(1) three passage liquid nitrogen carry out to the single phase austenite steel of mentioned component cold rolling: is put into by single phase austenite steel in liquid nitrogen before every time rolling and be incubated 10 ~ 20min, liquid nitrogen and single phase austenite steel volume ratio are: 10 ~ 50:1, and three passes volumes under pressure are respectively 10 ~ 20%, 8 ~ 15%, 2 ~ 5%.
(2) second annealing process: with the ramp of 5 ~ 40 DEG C/min to 200 ~ 300 DEG C, insulation 60 ~ 180min, furnace cooling, after single phase austenite steel is returned to room temperature, with the ramp of 30 ~ 40 DEG C/min to 600 ~ 800 DEG C, insulation 20 ~ 40min, furnace cooling, prepares non-magnetic iron-based biological and medicinal implant material.
In the present invention, it is cold rolling single phase austenite steel to be carried out three passage liquid nitrogen, makes it to produce slip band defect, has activated its crystal boundary energy; Low temperature long term annealing for the first time, eliminate the stress through the cold rolling generation of liquid nitrogen in steel, second time high temperature rapid thermal annealing, single phase austenite steel is made to change austenite and homodisperse iron carbon, ferrimanganic carbon compound three-phase into by single phase austenite, change the weave construction of steel, the iron-carbon compound that anneal obtains and ferrimanganic carbon compound, its electrode potential is higher than iron, forming numerous microbattery with iron-based body, is a kind of method effectively improving biological steel degradation rate easily.
The present invention compared with prior art tool has the following advantages:
1, with short production cycle, cost is low.
2, the non-magnetic iron-based biological and medicinal implant material principal phase prepared is still austenite structure, slip band through the cold rolling generation of three passage liquid nitrogen has activated crystal boundary energy, the iron-carbon compound that anneal obtains and ferrimanganic carbon compound, micro-cell corrosion is formed with iron-based body, make the degradation rate of non-magnetic iron-based biological and medicinal implant material relative to single phase austenite steel, improve an order of magnitude, reach 0.28mmy
-1.
3, applied widely, not by the constraint of piece volumes, be both applicable to bulky part, be also applicable to small volume components.
Accompanying drawing explanation
Fig. 1 is the optical electron microscope figure of non-magnetic iron-based biological and medicinal implant material prepared by the embodiment of the present invention 1.
Fig. 2 is the erosion rate figure of non-magnetic iron-based biological and medicinal implant material prepared by the embodiment of the present invention 2.
Fig. 3 is the corrosion electric current density figure of non-magnetic iron-based biological and medicinal implant material prepared by the embodiment of the present invention 3.
Embodiment:
Embodiment 1
Select single phase austenite steel, its chemical composition mass percentage is: C:0.6%, Mn:13%, Si:0.5%, Ca:0.5%, Zn:0.5%, Ag:0.5%, S:0.016%, P:0.022%, and all the other are Fe.Carry out three passage liquid nitrogen to the single phase austenite steel of mentioned component cold rolling, put in liquid nitrogen by single phase austenite steel before every time rolling and be incubated 10min, liquid nitrogen and single phase austenite steel volume ratio are: 10:1.Three passes volumes under pressure are respectively 10%, 8%, 2%, and total volume under pressure is 20%.Then second annealing process is carried out: with the ramp of 5 DEG C/min to 200 DEG C, insulation 60min, furnace cooling, after single phase austenite steel is returned to room temperature, with the ramp of 30 DEG C/min to 600 DEG C, insulation 20min, furnace cooling, prepares non-magnetic iron-based biological and medicinal implant material.
As seen from Figure 1, the single phase austenite steel after liquid nitrogen cold rolling 20% and second annealing process, by single austenite phase, generates the iron carbon of austenite and needle-like, ferrimanganic carbon compound three-phase.
Embodiment 2
Select single phase austenite steel, its chemical composition mass percentage is: C:1.5%, Mn:35%, Si:0.6%, Ca:2%, Zn:2%, Ag:2%, S:0.020%, P:0.025%, and all the other are Fe.Carry out three passage liquid nitrogen to the single phase austenite steel of mentioned component cold rolling, put in liquid nitrogen by single phase austenite steel before every time rolling and be incubated 20min, liquid nitrogen and single phase austenite steel volume ratio are: 50:1.Three passes volumes under pressure are respectively 20%, 15%, 5%, and total volume under pressure is 40%.Then second annealing process is carried out: with the ramp of 40 DEG C/min to 300 DEG C, insulation 180min, furnace cooling, after single phase austenite steel is returned to room temperature, with the ramp of 40 DEG C/min to 800 DEG C, insulation 40min, furnace cooling, prepares non-magnetic iron-based biological and medicinal implant material.
As seen from Figure 2, the single phase austenite steel after liquid nitrogen cold rolling 40% and second annealing process, its erosion rate is relative to the 0.060mmy of unprocessed former state
-1, improve an order of magnitude, reach 0.28mmy
-1.
Embodiment 3
Select single phase austenite steel, its chemical composition mass percentage is: C:1.0%, Mn:25%, Si:0.55%, Ca:1%, Zn:1%, Ag:1%, S:0.018%, P:0.023%, and all the other are Fe.Carry out three passage liquid nitrogen to the single phase austenite steel of mentioned component cold rolling, put in liquid nitrogen by single phase austenite steel before every time rolling and be incubated 15min, liquid nitrogen and single phase austenite steel volume ratio are: 30:1.Three passes volumes under pressure are respectively 15%, 10%, 4%, and total volume under pressure is 29%.Then second annealing process is carried out: with the ramp of 20 DEG C/min to 250 DEG C, insulation 100min, furnace cooling, after single phase austenite steel is returned to room temperature, with the ramp of 35 DEG C/min to 700 DEG C, insulation 25min, furnace cooling, prepares non-magnetic iron-based biological and medicinal implant material.
As seen from Figure 3, the single phase austenite steel after liquid nitrogen cold rolling 29% and second annealing process, its corrosion electric current density is relative to the 0.0048mAcm of unprocessed former state
-2, improve an order of magnitude, reach 0.024mAcm
-2.
Claims (2)
1. a non-magnetic iron-based biological and medicinal implant material, it is characterized in that: it is single phase austenite, its chemical composition mass percent is: C:0.6 ~ 1.5%, Mn:13 ~ 35%, Si:0.5 ~ 0.6%, Ca:0.5 ~ 2%, Zn:0.5 ~ 2%, Ag:0.5 ~ 2%, S:0.016 ~ 0.020%, P:0.022 ~ 0.025%, and all the other are Fe.
2. the preparation method of non-magnetic iron-based biological and medicinal implant material according to claim 1, is characterized in that:
(1) three passage liquid nitrogen carry out to the single phase austenite steel of mentioned component cold rolling: is put into by single phase austenite steel in liquid nitrogen before every time rolling and be incubated 10 ~ 20min, liquid nitrogen and single phase austenite steel volume ratio are: 10 ~ 50:1, and three passes volumes under pressure are respectively 10 ~ 20%, 8 ~ 15%, 2 ~ 5%;
(2) second annealing process: with the ramp of 5 ~ 40 DEG C/min to 200 ~ 300 DEG C, insulation 60 ~ 180min, furnace cooling, after single phase austenite steel is returned to room temperature, with the ramp of 30 ~ 40 DEG C/min to 600 ~ 800 DEG C, insulation 20 ~ 40min, furnace cooling, prepares non-magnetic iron-based biological and medicinal implant material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510043123.8A CN104711473B (en) | 2015-01-28 | 2015-01-28 | Nonmagnetic biomedical implant material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510043123.8A CN104711473B (en) | 2015-01-28 | 2015-01-28 | Nonmagnetic biomedical implant material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN104711473A true CN104711473A (en) | 2015-06-17 |
| CN104711473B CN104711473B (en) | 2017-04-26 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435131A (en) * | 2016-08-31 | 2017-02-22 | 东北大学 | Method for preparing nanocrystalline austenitic stainless steel plate through deep cooling rolling-rapid annealing |
| CN108677099A (en) * | 2018-04-17 | 2018-10-19 | 西南大学 | Medical degradable Fe-Mn-Ag alloy materials and preparation and application |
| JP2020510748A (en) * | 2016-11-23 | 2020-04-09 | オウトクンプ オサケイティオ ユルキネンＯｕｔｏｋｕｍｐｕ Ｏｙｊ | Manufacturing method of complex shape molded member |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090198320A1 (en) * | 2008-02-05 | 2009-08-06 | Biotronik Vi Patent Ag | Implant with a base body of a biocorrodible iron alloy |
| CN101636187A (en) * | 2007-01-30 | 2010-01-27 | 汉莫堤克股份有限公司 | Biodegradable vascular support |
| JP2012518474A (en) * | 2009-02-20 | 2012-08-16 | ボストン サイエンティフィック サイムド，インコーポレイテッド | Biodegradable prosthesis |
| CN102776435A (en) * | 2011-05-13 | 2012-11-14 | 中国科学院金属研究所 | Degradable Fe-Mn-C ternary iron alloy material and its application |
| CN103028148A (en) * | 2012-12-28 | 2013-04-10 | 上海交通大学 | Medical degradable Fe-Mg-X alloy material and preparation method thereof |
-
2015
- 2015-01-28 CN CN201510043123.8A patent/CN104711473B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101636187A (en) * | 2007-01-30 | 2010-01-27 | 汉莫堤克股份有限公司 | Biodegradable vascular support |
| US20090198320A1 (en) * | 2008-02-05 | 2009-08-06 | Biotronik Vi Patent Ag | Implant with a base body of a biocorrodible iron alloy |
| JP2012518474A (en) * | 2009-02-20 | 2012-08-16 | ボストン サイエンティフィック サイムド，インコーポレイテッド | Biodegradable prosthesis |
| CN102776435A (en) * | 2011-05-13 | 2012-11-14 | 中国科学院金属研究所 | Degradable Fe-Mn-C ternary iron alloy material and its application |
| CN103028148A (en) * | 2012-12-28 | 2013-04-10 | 上海交通大学 | Medical degradable Fe-Mg-X alloy material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435131A (en) * | 2016-08-31 | 2017-02-22 | 东北大学 | Method for preparing nanocrystalline austenitic stainless steel plate through deep cooling rolling-rapid annealing |
| CN106435131B (en) * | 2016-08-31 | 2019-07-23 | 东北大学 | The method that deep cooling rolling-short annealing prepares nanocrystalline austenite stainless steel plate |
| JP2020510748A (en) * | 2016-11-23 | 2020-04-09 | オウトクンプ オサケイティオ ユルキネンＯｕｔｏｋｕｍｐｕ Ｏｙｊ | Manufacturing method of complex shape molded member |
| CN108677099A (en) * | 2018-04-17 | 2018-10-19 | 西南大学 | Medical degradable Fe-Mn-Ag alloy materials and preparation and application |
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| CN104711473B (en) | 2017-04-26 |
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