CN101503764A - Preparation of nontoxic magnesium alloy material for biological implantation - Google Patents
Preparation of nontoxic magnesium alloy material for biological implantation Download PDFInfo
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- CN101503764A CN101503764A CNA2009100107351A CN200910010735A CN101503764A CN 101503764 A CN101503764 A CN 101503764A CN A2009100107351 A CNA2009100107351 A CN A2009100107351A CN 200910010735 A CN200910010735 A CN 200910010735A CN 101503764 A CN101503764 A CN 101503764A
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Abstract
The invention relates to a method for preparing a magnesium alloy material suitable for biological implantation, which comprises the following steps: preparing raw materials by the following chemical compositions in percentage by weight: 2.0 to 6.0 percent of Zn, 0.5 to 1.9 percent of Mn, 0.6 to 5.0 percent of Ca, less than or equal to 0.1 percent of total impurities, and the balance of Mg; or preparing the raw materials by the following chemical compositions in percentage by weight: 2.0 to 6.0 percent of Zn, 0.3 to 0.9 percent of Zr, 0.5 to 5.0 percent of Ca, less than or equal to 0.1 percent of total impurities, and the balance of Mg; preheating smelting equipment and adding the Mg into the raw materials; heating the mixture under the protection of argon gas with the flow rate of between 5 and 6 L/min and the pressure of 14 MPa; adding a fire retardant into the molten liquid when the temperature of the molten liquid reaches between 650 and 660 DEG C, raising the temperature of the molten liquid to between 700 and 720 DEG C, adding other alloy elements into the molten liquid respectively, and performing melting reaction; and stirring the mixture until the mixture is uniformly mixed after alloy is completely molten, keeping the mixture stand for 30 to 40 minutes, pressing a deslagging agent into the solution for deslagging, casting the alloy solution into a cast die after keeping the alloy solution for 10 to 20 minutes at the temperature of between 690 and 710 DEG C, and preparing a Mg-Mn series or Mg-Zr series biomedical magnesium alloy material ingot.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium alloy materials, particularly relating to Mg-Mn system and Mg-Zr is the biological medical magnesium alloy preparation methods.
Technical background
In recent years, magnesium and magnesium alloy are also at the early-stage abroad as the research of hard tissue implanting material, China magnesium source is abundant, the state key research project has been listed in the development of magnesium industry goods in, people's primary design such as the Yang Ke of metal institute of the Chinese Academy of Sciences Mg-Mn system be alloy with Mg-Mn-Zn, the magnesium alloy implantation big white mouse body of finding design is interior respond well, has obtained the important research progress.People such as Lee Longchuan of University Of Chongqing have studied corrosion behavior and the alkali heat treatment technics of magnesium in bionical body fluid, find through the corrosion resisting property of magnesium metal in bionical body fluid after the alkali thermal treatment good.In the 1750th page of " Northeastern University's journal " natural science edition 2008 the 12nd phase, in " towards the magnesium alloy composition and the solidified structure research of bio-medical " that people such as Guan Renguo deliver the Mg-Mn-Ca magnesium alloy materials is studied as biological implantation material.Its processing method is as follows:
Table 1 alloy smelting process
Fully show according to existing result of study, magnesium alloy has important research and using value as biomaterial aspect sclerous tissues's implantation, perishable, the degradable characteristics of magnesium alloy by improving its solidity to corrosion, can be used as degradable embedded material and use.
Though above-mentioned research has obtained certain progress, but because the composition of magnesium alloy is more single, cause magnesium alloy ingot to organize even inadequately, rounding, stress distribution is even inadequately, and also there are certain defective in the plasticity of foundry goods, hardness, mechanical property and resistance to corrosion.
Summary of the invention
The objective of the invention is problem at the prior art existence, a kind of novel preparation method who contains nontoxic alloying constituent and can be used as the magnesium alloy materials of bio-medical implantation is provided, by optimizing alloying constituent, improve the comprehensive mechanical property of magnesium alloy plate, determined the optimum composition range of Mg-Mn system and Mg-Zr series magnesium alloy.And reach the magnesium alloy materials homogeneous microstructure, and rounding, stress distribution is even, the effect that foundry goods plasticity, hardness, mechanical property and resistance to corrosion are improved.
The technical scheme that realizes the object of the invention is: utilize melting equipment heating melting pure magnesium ingot, add alloying element and refining agent by the titanium alloy bell jar in metal melt, the preparation method carries out as follows:
1) with the chemical component weight mark be: Mg-Mn system: the chemical component weight mark is Zn 2.0～6.0%, and Mn 0.5～1.9%, and Ca 0.6～5.0%, impurity summation≤0.1%, and surplus is Mg; Or Mg-Zr system: the chemical component weight mark is Zn 2.0～6.0%, and Zr 0.3～0.9%, and Ca 0.5～5.0%, impurity summation≤0.1%, and surplus is that Mg carries out preparation of raw material;
2) melting equipment is preheating to 550 ℃～580 ℃;
3) being that the pure magnesium ingot of 99.99wt% joins in the melting equipment with purity, is 5～6L/min at flow, and pressure is to carry out heating and melting under the argon shield of 14MPa;
When configuration proportion 4) when melt temperature reaches 660～650 ℃, set by step 1) adds metal Ca and is warmed up to 700～720 ℃, add other component Zn again, Mn or Zn, Zr melts reaction;
5) when alloy all after the fusing, stir it mixed, leave standstill 30～40min after, deslagging agent is pressed in the solution removes the gred, after leaving standstill 10～20min under 690～710 ℃ of temperature, pour into a mould;
6) the step 5) melt cast is prepared Mg-Mn system or Mg-Zr series magnesium alloy bio-medical material ingot blank in mold.
The deslagging agent of above-mentioned adding is a hexachloroethane, and chemical formula is C2Cl6, and add-on is 0.2～0.5wt% of alloy gross weight.
The present invention compared with the prior art, the beneficial effect of generation is to have broken through the traditional material system, has prepared the novel magnesium alloy of heterogeneity, and is nontoxic, can be used as biological implantation material and uses.Magnesium alloy by above-mentioned processing method preparation, as shown in drawings ingot structure evenly, rounding, crystal grain is tiny, stress distribution is more even, the plasticity and the hardness of foundry goods are improved simultaneously, satisfy the requirement of bio-medical material on mechanical property and resistance to corrosion substantially.Wherein the trace element that is added plays a part very big.The Ca element is an alloying element important in the magnesium alloy, plays the effect of fire retardant again.It can obviously improve the burning-point of magnesium alloy, forms the MgO+CaO composite protection film, and magnesium alloy fused mass is had provide protection, prevents alloy liquid oxidation burning, improves the alloy melt quality, improves the magnesium alloy ingot quality; The Zn element is effective alloy element of magnesium alloy, and its solid solubility is bigger, and reduces and significantly reduce with temperature, can make alloy produce solution strengthening and ageing strengthening.Zn can increase the flowability of melt, improves casting quality.Table 2 is different positions alloying element content values in the Mg-Mn system shown in the accompanying drawing 3, find by table 2, accompanying drawing 1 and 3, Ca, the content of Zn two elements in crystal boundary and intracrystalline point-like tissue are higher, wherein the solid solubility of Zn in matrix is 3.622%, and be highly beneficial for the solution strengthening and the ageing strengthening of alloy.Table 3 is different positions alloying element content values in the Mg-Zr system shown in the accompanying drawing 4, find by table 3, accompanying drawing 2 and 4, under normal temperature condition, the solid solubility of Zr element in the Mg matrix is less, do not form compound with magnesium, Zr can also form stable compound and purify melt with impurity F e, Si in the alloy and even H, O element, has improved the purity of alloy, has improved the corrosion resistance nature of magnesium alloy bio-medical material.
Table 2 Mg-Mn is a different positions alloying element content in the alloy structure
Table 3 Mg-Zr is a different positions alloying element content in the alloy structure
Description of drawings
Fig. 1 is that 700 ℃ of temperature, cooling water flow are that Mg-Mn under the 5L/min condition is the as-cast structure figure of alloy;
Fig. 2 is that 700 ℃ of temperature, cooling water flow are that Mg-Zr under the 5L/min condition is the as-cast structure figure of alloy;
Fig. 3 is that Mg-Mn is the SEM image and the EDS energy spectrum analysis figure of alloy;
Fig. 4 is that Mg-Zr is the SEM image and the EDS energy spectrum analysis figure of alloy;
A figure among Fig. 3 and Fig. 4 is the SEM image of alloy, and b, c, d figure are respectively the EDS energy spectrum analysis figure of A, B, C among a figure at 3.
Embodiment
1.Mg-Mn be bio-medical material
Embodiment 1: melting equipment is that the homemade power in laboratory is the hot resistance stove of 2kw.Structure mainly is by built-in Stainless Steel Crucible, the resistance wire of crucible surrounded, and insulating brick and outsourcing iron sheet formation.
Utilize melting equipment to heat molten alloy, in the time of experiment, use thermocouple measuring temperature, when reaching the teeming temperature of setting, emit the fused liquid magnesium alloy at the converter nose place and pour into a mould experiment.
Adopting this device to carry out Mg-Mn is the bio-medical material preparation, carries out as follows:
(1) be respectively with the chemical component weight mark: Zn2%, Mn0.5%, Ca5.0%, impurity summation≤0.1%, surplus is that Mg carries out preparation of raw material;
(2) melting equipment is preheating to 550 ℃;
(3) be full of argon gas in the melting equipment after preheating, the pure magnesium that will prepare purity then and be 99.99wt% joins in the melting equipment, and is 5L/min at flow, and pressure is to carry out heating and melting under the protection of 14MPa argon gas;
(4) with JWK-702 precision temperature housing control melt temperature, when treating that the magnesium liquid temp reaches 650 ℃, the fire-retardant calcium metal of the 0.6wt% of alloy gross weight is added and be warmed up to 700 ℃, again alloying element is added wherein, melt reaction;
(5) when alloy all after the fusing, stir it mixed, leave standstill 30min after, with the deslagging agent C of the 0.2wt% of alloy gross weight
2Cl
6Be pressed in the solution and remove the gred, after leaving standstill 10min under 700 ℃ of temperature, pour into a mould;
Embodiment 2: the device of this example is identical with embodiment 1, carries out as follows:
(1) be respectively with the chemical component weight mark: Zn4%, Mn0.8%, Ca2.5%, impurity summation≤0.1%, surplus is that Mg carries out preparation of raw material;
(2) melting equipment is preheating to 560 ℃;
(3) be full of argon gas in the melting equipment after preheating, the pure magnesium that will prepare purity then and be 99.99wt% joins in the melting equipment, and is 6L/min at flow, and pressure is to carry out heating and melting under the protection of 14MPa argon gas;
(4) with JWK-702 precision temperature housing control melt temperature, when treating that the magnesium liquid temp reaches 650 ℃, the fire-retardant calcium metal of the 2.0wt% of alloy gross weight is added and be warmed up to 710 ℃, again alloying element is added wherein, melt reaction;
(5) when alloy all after the fusing, stir it mixed, leave standstill 40min after, with the deslagging agent C of the 0.3wt% of alloy gross weight
2Cl
6Be pressed in the solution and remove the gred, after leaving standstill 10min under 690 ℃ of temperature, pour into a mould cooling water flow 5L/min;
Embodiment 3: the device of this example is identical with embodiment 1, carries out as follows:
(1) be respectively with the chemical component weight mark: Zn 6.0%, and Mn 1.9%, and Ca 0.6%, impurity summation≤0.1%, and surplus is that Mg carries out preparation of raw material;
(2) melting equipment is preheating to 580 ℃;
(3) be full of argon gas in the melting equipment after preheating, the pure magnesium that will prepare purity then and be 99.99wt% joins in the melting equipment, and is 5L/min at flow, and pressure is to carry out heating and melting under the protection of 14MPa argon gas;
(4) with JWK-702 precision temperature housing control melt temperature, when treating that the magnesium liquid temp reaches 660 ℃, the fire-retardant calcium metal of the 5.0wt% of alloy gross weight is added and be warmed up to 720 ℃, again alloying element is added wherein, melt reaction;
(5) when alloy all after the fusing, stir it mixed, leave standstill 40min after, with the deslagging agent C of the 0.5wt% of alloy gross weight
2Cl
6Be pressed in the solution and remove the gred, after leaving standstill 20min under 710 ℃ of temperature, pour into a mould cooling water flow 5L/min;
2.Mg-Zr be bio-medical material
Among the present invention, the material that Zr adopted in the Mg-Zr series magnesium alloy is magnesium zirconium master alloy (market purchase).
Embodiment 4: the device of this example is identical with embodiment 1, carries out as follows:
(1) be respectively with the chemical component weight mark: Zn2%, Zr0.3%, Ca5.0%, impurity summation≤0.1%, surplus is that Mg carries out preparation of raw material;
(2) melting equipment is preheating to 550 ℃;
(3) be full of argon gas in the melting equipment after preheating, the pure magnesium that will prepare purity then and be 99.99wt% joins in the melting equipment, and is 5L/min at flow, and pressure is to carry out heating and melting under the protection of 14MPa argon gas;
(4) with JWK-702 precision temperature housing control melt temperature, when treating that the magnesium liquid temp reaches 650 ℃, the fire-retardant calcium metal of the 0.5wt% of alloy gross weight is added and be warmed up to 700 ℃, again alloying element is added wherein, melt reaction;
(5) when alloy all after the fusing, stir it mixed, leave standstill 30min after, with the deslagging agent C of the 0.2wt% of alloy gross weight
2Cl
6Be pressed in the solution and remove the gred, after leaving standstill 10min under 700 ℃ of temperature, pour into a mould cooling water flow 5L/min;
Embodiment 5: the device of this example is identical with embodiment 1, carries out as follows:
(1) be respectively with the chemical component weight mark: Zn4%, Zr0.5%, Ca0.5%,, impurity summation≤0.1%, surplus is that Mg carries out preparation of raw material;
(2) melting equipment is preheating to 560 ℃;
(3) be full of argon gas in the melting equipment after preheating, the pure magnesium that will prepare purity then and be 99.99wt% joins in the melting equipment, and is 5L/min at flow, and pressure is to carry out heating and melting under the protection of 14MPa argon gas;
(4) with JWK-702 precision temperature housing control melt temperature, when treating that the magnesium liquid temp reaches 655 ℃, the fire-retardant calcium metal of the 2.5wt% of alloy gross weight is added and be warmed up to 710 ℃, again alloying element is added wherein, melt reaction;
(5) when alloy all after the fusing, stir it mixed, leave standstill 35min after, with the deslagging agent C of the 0.3wt% of alloy gross weight
2Cl
6Be pressed in the solution and remove the gred, after leaving standstill 15min under 690 ℃ of temperature, pour into a mould cooling water flow 5L/min;
Embodiment 6: the device of this example is identical with embodiment 1, carries out as follows:
(1) be respectively with the chemical component weight mark: Zn 6%, and Zr 0.8%, and Ca 2.5%,, impurity summation≤0.1%, surplus is that Mg carries out preparation of raw material;
(2) melting equipment is preheating to 580 ℃;
(3) be full of argon gas in the melting equipment after preheating, the pure magnesium that will prepare purity then and be 99.99wt% joins in the melting equipment, and is 6L/min at flow, and pressure is to carry out heating and melting under the protection of 14MPa argon gas;
(4) with JWK-702 precision temperature housing control melt temperature, when treating that the magnesium liquid temp reaches 660 ℃, the fire-retardant calcium metal of the 5.0wt% of alloy gross weight is added and be warmed up to 720 ℃, again alloying element is added wherein, melt reaction;
(5) when alloy all after the fusing, stir it mixed, leave standstill 40min after, with the deslagging agent C of the 0.5wt% of alloy gross weight
2Cl
6Be pressed in the solution and remove the gred, after leaving standstill 20min under 710 ℃ of temperature, pour into a mould cooling water flow 5L/min.
Claims (2)
1, a kind of nontoxic, preparation method of being applicable to the biological magnesium alloy materials of implanting is characterized in that carrying out as follows:
1) choose Mg-Mn system: the chemical component weight mark is Zn 2.0～6.0%, and Mn 0.5～1.9%, and Ca 0.6～5.0%, impurity summation≤0.1%, and surplus is Mg; Or Mg-Zr system: the chemical component weight mark is Zn 2.0～6.0%, and Zr 0.3～0.9%, and Ca 0.5～5.0%, impurity summation≤0.1%, and surplus is that Mg carries out preparation of raw material;
2) melting equipment is preheating to 550 ℃～580 ℃;
3) magnesium ingot being joined in the melting equipment, is 5～6L/min at flow, and pressure is to carry out heating and melting under the argon shield of 14MPa;
When configuration proportion 4) when the magnesium melt temperature reaches 650～660 ℃, set by step 1) adds metal Ca and is warmed up to 700～720 ℃, add other component Zn again, Mn, or Zn, Zr melts reaction;
5) when alloy all after the fusing, stir it mixed, leave standstill 30～40min after, deslagging agent is pressed in the solution removes the gred, after leaving standstill 10～20min under 690～710 ℃ of temperature, pour into a mould;
6) the step 5) melt cast is prepared Mg-Mn system or Mg-Zr series magnesium alloy bio-medical material ingot blank in mold.
2, according to described a kind of nontoxic, the preparation method that is applicable to the biological magnesium alloy materials of implanting of claim 1, the deslagging agent that it is characterized in that described adding is a hexachloroethane, and chemical formula is C
2Cl
6, add-on is 0.2～0.5wt% of alloy gross weight.
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| CN103243251A (en) * | 2013-05-21 | 2013-08-14 | 上海交通大学医学院附属上海儿童医学中心 | Magnesium alloy and smelting and heat treatment processes thereof |
| CN103725942A (en) * | 2013-12-31 | 2014-04-16 | 重庆大学 | Mg-Zn-Sr-Ca system magnesium alloy and preparation method thereof |
| CN103757511A (en) * | 2013-12-27 | 2014-04-30 | 南通河海大学海洋与近海工程研究院 | Dispersion strengthened medical Mg-Zn-Ce-Ca-Mn alloy and preparation method thereof |
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| CN105603277A (en) * | 2015-12-28 | 2016-05-25 | 青岛博泰美联化工技术有限公司 | Easily-degraded medical magnesium-alloy material and preparation method thereof |
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| CN105779839A (en) * | 2016-05-09 | 2016-07-20 | 天津理工大学 | Self-protection degradable MgO/Mg-Zn-Ca biological composite material |
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| CN103757511A (en) * | 2013-12-27 | 2014-04-30 | 南通河海大学海洋与近海工程研究院 | Dispersion strengthened medical Mg-Zn-Ce-Ca-Mn alloy and preparation method thereof |
| CN103725942A (en) * | 2013-12-31 | 2014-04-16 | 重庆大学 | Mg-Zn-Sr-Ca system magnesium alloy and preparation method thereof |
| US20190001027A1 (en) * | 2015-12-21 | 2019-01-03 | The University Of Toledo | Process to produce high-strength and corrosion resistant alloy for patient-specific bioresorbable bone fixation implants and hardware |
| CN105624496A (en) * | 2015-12-28 | 2016-06-01 | 青岛博泰美联化工技术有限公司 | Bone nail and preparation method |
| CN105603277A (en) * | 2015-12-28 | 2016-05-25 | 青岛博泰美联化工技术有限公司 | Easily-degraded medical magnesium-alloy material and preparation method thereof |
| CN105435302A (en) * | 2015-12-28 | 2016-03-30 | 青岛博泰美联化工技术有限公司 | Bone filling material and preparation method thereof |
| CN105624495A (en) * | 2015-12-28 | 2016-06-01 | 青岛博泰美联化工技术有限公司 | Medical suture material and preparation method |
| CN105381508A (en) * | 2015-12-28 | 2016-03-09 | 青岛博泰美联化工技术有限公司 | Endovascular stent and preparation method |
| CN105779839A (en) * | 2016-05-09 | 2016-07-20 | 天津理工大学 | Self-protection degradable MgO/Mg-Zn-Ca biological composite material |
| CN106676357A (en) * | 2017-01-19 | 2017-05-17 | 重庆大学 | High-plasticity magnesium alloy and preparation method thereof |
| CN106676357B (en) * | 2017-01-19 | 2018-05-04 | 重庆大学 | A kind of high plastic magnesium alloy and preparation method thereof |
| CN109280828A (en) * | 2018-12-10 | 2019-01-29 | 南京工程学院 | A kind of high-strength degradable implantation instrument composite material and preparation method |
| CN109280828B (en) * | 2018-12-10 | 2021-03-02 | 南京工程学院 | High-strength degradable composite material for implanting instrument and preparation method thereof |
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