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CN108913923A - A kind of medical degradable Mg-Nd-Ag ternary-alloy material and preparation method thereof - Google Patents

A kind of medical degradable Mg-Nd-Ag ternary-alloy material and preparation method thereof Download PDF

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CN108913923A
CN108913923A CN201810695170.4A CN201810695170A CN108913923A CN 108913923 A CN108913923 A CN 108913923A CN 201810695170 A CN201810695170 A CN 201810695170A CN 108913923 A CN108913923 A CN 108913923A
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CN108913923B (en
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杨磊
申留杰
张二林
麻连功
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C23/00—Alloys based on magnesium
    • C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/04—Metals or alloys
    • A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

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Abstract

本发明公开一种医用可降解Mg‑Nd‑Ag三元合金材料及其制备方法，按质量百分比分为：Nd0‑2％、Ag1‑2％，其余为Mg以及不可避免的杂质，不可避免的杂质含量≤0.01％。本发明通过合理的原材料配比，采用真空铸造的方式，制备出一种具有质轻、耐腐蚀以及抗菌的新型可降解镁合金。Nd的引入有效提高镁合金的力学性能和耐腐蚀性能，Ag的引入使合金表现出极强的广谱抗菌性，持久性和不会产生耐药性等优点。最后通过固溶处理和时效处理来延缓合金的腐蚀速率。本发明的可降解抗菌镁合金组分设计合理、质量轻、强度高、降解速度符合临床要求，具有抗菌作用且对人体无毒害作用。同时，还提出了一种操作简单、工艺合理、制备的镁合金强度高、降解速度符合临床要求的镁合金制备方法。

The invention discloses a medical degradable Mg-Nd-Ag ternary alloy material and a preparation method thereof, which are divided into: Nd0-2%, Ag1-2% by mass percentage, and the rest are Mg and unavoidable impurities, unavoidable Impurity content ≤0.01%. The invention prepares a new type of degradable magnesium alloy with light weight, corrosion resistance and antibacterial properties through a reasonable ratio of raw materials and vacuum casting. The introduction of Nd effectively improves the mechanical properties and corrosion resistance of magnesium alloys, and the introduction of Ag makes the alloy exhibit strong broad-spectrum antibacterial properties, durability and no drug resistance. Finally, the corrosion rate of the alloy is delayed by solution treatment and aging treatment. The degradable antibacterial magnesium alloy of the invention has reasonable component design, light weight, high strength, and degradation speed meeting clinical requirements, has antibacterial effect and has no toxic effect on human body. At the same time, a preparation method of magnesium alloy with simple operation, reasonable process, high strength of the prepared magnesium alloy and degradation speed meeting clinical requirements is also proposed.

Description

A kind of medical degradable Mg-Nd-Ag ternary-alloy material and preparation method thereof
Technical field
The present invention relates to the antibacterial magnesium alloys for the biomedical materials field that one kind can degrade in vivo completely, specifically It says, is a kind of medical degradable Mg-Nd-Ag ternary-alloy material and preparation method thereof.
Background technique
The density of magnesium and magnesium alloy is about 1.74g/cm3, the density of human body compact bone is about 1.75g/cm3, it two quite. Elasticity modulus is also more nearly with people's bone, can effectively avoid stress-shielding effect, has good mechanical compatibility.Separately Outside, magnesium or the important component of human body, the minimum intake about 420mg of the daily magnesium of adult, and excessive magnesium may be used also To be discharged by urine, therefore, suitable magnesium metabolism not only will not generate harm to human body, also help the life for promoting osteocyte It is long.
In bio-medical field, magnesium alloy can be used to prepare the organizational projects branch such as Bone Defect Repari implant and angiocarpy bracket Frame.For biological medical magnesium alloy compared with other medical metal materials, sharpest edges are its energy corrosion degradation in Service Environment, And catabolite can be absorbed by the body or be discharged, and not need second operation as human body implantation piece.
Summary of the invention
In view of the deficiencies of the prior art, the invention proposes a kind of designs of component rationally, light weight, intensity are high, degradation speed Rate meets clinical requirement, and the degradable antibacterial magnesium alloy to human body without any toxic action.Magnesium alloy degradation rate it is effective Regulation is the key that it really realizes clinical application, therefore improving the corrosion resistance of magnesium alloy in human body is always biological magnesium The hot spot of alloy research.Another object of the present invention is to prepare a kind of novel degradable antibacterial magnesium alloy to improve bio-medical The degradation property of magnesium alloy.
A kind of medical degradable Mg-Nd-Ag ternary-alloy material is ingredient in terms of 100% by the total weight of the magnesium alloy Composition includes：Nd 2~2.3%, Ag 1~2%, remaining be Mg and inevitable impurity element.
Mass percentage total amount shared by inevitable impurity element is not more than 0.01% in above-mentioned magnesium alloy, can not keep away The impurity element exempted from includes Mn and Zr.
Mg, Ag raw material metal are selected from the component pure metal that purity is more than or equal to 99.99% in each component.Nd Mg-Nd intermediate alloy selected from 30wt%.
The above-mentioned method for preparing degradable Mg-Nd-Ag ternary-alloy material, includes the following steps：
(1) raw material preparation：Raw material are respectively that pure magnesium (99.99wt%), fine silver (99.99wt%), Nd content are The Mg-Nd intermediate alloy of 30wt%；Raw material are cut, the polishing cleaning of sand for surface wheel removes oxide on surface, to subtract The generation of few melting impurity, and be successively cleaned by ultrasonic with ultrapure water and alcohol, it is carried out after drying process according to alloying component It weighs.
(2) smelting equipment prepares：The inner wall of vacuum induction melting furnace is cleaned, crucible remove oxidizing slag, mold into Row cleans and coating.
(3) alloy melting and casting, sampling：The pure MAG block for weighing up weight is put into togerther with the intermediate alloy block to be added In graphite crucible, smelting furnace outer cover is closed, mechanical pump is opened and is evacuated to 7.5~8Pa；Then to being passed through argon gas in crucible extremely 0.4~0.6 atmospheric pressure opens induction furnace heating device, and 260~265V of voltage is arranged, and 18~19A of electric current is heated to magnesium It is completely melt, is sufficiently stirred with each intermediate alloy, stood after the completion of stirring and stop heating；By the magnesium alloy liquid pressure casting in crucible Into in preheated mold already, last completely cooling taking-up ingot casting.
(4) it is heat-treated, ingot casting obtained by above-mentioned steps is cut into several fritters, sample is sealed up for safekeeping in graphite powder, is set In chamber type electric resistance furnace, heating rate is 10~12 DEG C/min, is warming up to 530~540 DEG C and keeps the temperature 15~16h, heat preservation terminates It is quenched in ice water afterwards.Ageing treatment is carried out, heating rate is 10~12 DEG C/min, is warming up to 180~200 DEG C and keeps the temperature 8~9h takes out air-cooled after heat preservation.
Beneficial outcomes of the invention：The present invention is prepared by the way of vacuum pressing and casting by reasonable raw material ratio With the high degradable antibacterial magnesium alloy of light, intensity.The introducing of Nd effectively improves the mechanical property and corrosion resistant of magnesium alloy It the advantages that corrosion energy, the introducing of Ag makes alloy show extremely strong broad spectrum antibacterial, persistence and will not generate drug resistance, is curing It is widely applied on anti-biotic material.
Detailed description of the invention
Fig. 1 is that aging state Mg2Nd2Ag alloy is immersed in erosion profile and energy spectrum diagram in SBF solution after 48h.Wherein (a), (b), (c) be different up-sizings under aging state Mg2Nd2Ag erosion profile figure, (d), (e) be in figure white The corresponding energy spectrum diagram of grain.
Fig. 2 is the weightless average corrosion rate figure of the degradable antibacterial magnesium alloy under the different conditions that the present invention is implemented.
Fig. 3 is the liberation of hydrogen average corrosion rate figure of the degradable antibacterial magnesium alloy under the different conditions that the present invention is implemented.
Fig. 4 is antibacterial of Mg-2Nd-xAg (x=0,1,2) the alloy leaching liquor under different conditions to staphylococcus aureus Rate figure.
Fig. 5 is that the back scattering containing Argent grain in aging state Mg2Nd2Ag alloy leaching liquor scans shape appearance figure and arrow is signified The corresponding EDS gamma-spectrometric data of white particle.
Specific embodiment
The embodiment of the present invention is given below, and the present invention is further described, is not intended to limit the scope of the invention.
It is former for selecting the Mg-Nd intermediate alloy that pure magnesium (99.99wt%), fine silver (99.99wt%), Nd content are 30wt% Material is equipped with, and is then carried out melting with vacuum induction melting furnace, is obtained alloy cast ingot.Respectively to three kinds of different implementations after melting The magnesium base alloy material of example institute melting carries out solution treatment and ageing treatment.Mg, Nd, Ag ratio of three kinds of embodiments are different, tool Body mode of operation is as follows：
(1) raw material preparation：Raw material are respectively that pure magnesium (99.99wt%), fine silver (99.99wt%), Nd content are The Mg-Nd intermediate alloy of 30wt%.Raw material are cut, the polishing cleaning of sand for surface wheel removes oxide on surface, to subtract The generation of few melting impurity, and be successively cleaned by ultrasonic with ultrapure water and alcohol, it is carried out after drying process according to alloying component It weighs.
(2) smelting equipment prepares：The inner wall of vacuum induction melting furnace is cleaned, crucible remove oxidizing slag, mold into Row cleans and coating.
(3) alloy melting and casting, sampling：The pure MAG block for weighing up weight is put into togerther with the intermediate alloy block to be added In graphite crucible, smelting furnace outer cover is closed, mechanical pump is opened and is evacuated to 7.5~8Pa；Then to being passed through argon gas in crucible extremely 0.4~0.6 atmospheric pressure opens induction furnace heating device, and 260~265V of voltage is arranged, and 18~19A of electric current is heated to magnesium It is completely melt, is sufficiently stirred with each intermediate alloy, stood after the completion of stirring and stop heating；By the magnesium alloy liquid pressure casting in crucible Into in preheated mold already, last completely cooling taking-up ingot casting.
(4) it is heat-treated, ingot casting obtained by above-mentioned steps is cut into several cube fritters, sample is sealed up for safekeeping in graphite powder In, it being placed in chamber type electric resistance furnace, heating rate is 10~12 DEG C/min, it is warming up to 530~540 DEG C and keeps the temperature 15~16h, heat preservation After quenched in ice water, what is obtained herein is solution treatment sample.Then the sample after solution treatment is placed in heat In treatment furnace, ageing treatment is carried out, heating rate is 10~12 DEG C/min, it is warming up to 180~200 DEG C and keeps the temperature 8~9h, heat preservation After take out air-cooled, what is obtained herein is ageing treatment sample.
Table 1 is the pH that Mg-2Nd-xAg (x=0,1,2) alloy is not centrifuged leaching liquor, Ag ion concentration and antibiotic rate
Table 2 is the pH of leaching liquor after Mg-2Nd-xAg (x=0,1,2) alloy centrifugal, Ag ion concentration and antibiotic rate
Wherein, the Mg2Nd2Ag alloy after ageing treatment has relatively good corrosion resistance, it may have preferable antibacterial Property, and these anti-microbial properties contain Argent grain what degradation process generated from alloy, and these are mainly fine silver containing Argent grain Little particle, Nd-Ag phase particle and AgCl corrosion product, wherein what is played a major role is fine silver little particle.

Claims (3)

1.一种医用可降解Mg-Nd-Ag三元合金材料，其特征在于，以该镁合金的总重量为100％计，其成分组成包括：Nd 2～2.3％、Ag 1～2％、其余为Mg和不可避免的杂质元素。1. A medical degradable Mg-Nd-Ag ternary alloy material is characterized in that, taking the total weight of the magnesium alloy as 100%, its composition comprises: Nd 2～2.3%, Ag 1～2%, The rest are Mg and unavoidable impurity elements. 2.根据权利要求1所述的可降解抗菌镁合金，其特征在于，镁合金中不可避免的杂质元素所占质量百分含量总量不大于0.01％，不可避免的杂质元素包括Mn和Zr。2. The degradable antibacterial magnesium alloy according to claim 1, characterized in that the total mass percentage of unavoidable impurity elements in the magnesium alloy is not more than 0.01%, and the unavoidable impurity elements include Mn and Zr. 3.制备权利要求1所述的可降解Mg-Nd-Ag三元合金材料的方法，其特征在于，包括以下步骤：3. prepare the method for degradable Mg-Nd-Ag ternary alloy material described in claim 1, it is characterized in that, comprise the following steps: (1)原料准备：原材料分别为纯镁(99.99wt％)、纯银(99.99wt％)、Nd含量为30wt％的Mg-Nd中间合金；将原材料进行切割，表面用砂轮打磨清理，清除表面氧化物，以减少熔炼杂质的产生，并先后用超纯水和酒精进行超声清洗，干燥处理后按照合金成分进行称量；(1) Raw material preparation: the raw materials are pure magnesium (99.99wt%), pure silver (99.99wt%), and Mg-Nd master alloy with a Nd content of 30wt%; the raw materials are cut, and the surface is polished and cleaned with a grinding wheel to remove the surface Oxide, in order to reduce the production of smelting impurities, and ultrasonically cleaned with ultrapure water and alcohol successively, and weighed according to the alloy composition after drying; (2)熔炼设备准备：将真空感应熔炼炉的内壁进行清扫，坩埚去除氧化渣，模具进行清扫和涂料；(2) Melting equipment preparation: clean the inner wall of the vacuum induction melting furnace, remove the oxide slag from the crucible, clean and paint the mold; (3)合金熔炼、浇铸和取样：将称好重量的纯镁块与所要加的中间合金块一起放入石墨坩埚内，关闭熔炼炉外盖，打开机械泵抽真空至7.5～8Pa；随后向坩埚内通入氩气至0.4～0.6个大气压，打开感应炉加热装置，并设置电压260～265V，电流18～19A，加热至镁和各中间合金完全熔化，充分搅拌，搅拌完成后静置停止加热；将坩埚里的镁合金液体浇铸进早已预热好模具中，最后完全冷却取出铸锭；(3) Alloy smelting, casting and sampling: Put the weighed pure magnesium block and the intermediate alloy block to be added into the graphite crucible, close the outer cover of the melting furnace, turn on the mechanical pump to evacuate to 7.5-8Pa; Introduce argon gas into the crucible to 0.4-0.6 atmospheres, turn on the induction furnace heating device, and set the voltage to 260-265V, the current to 18-19A, heat until the magnesium and each intermediate alloy are completely melted, stir fully, and stop after the stirring is completed. Heating; cast the magnesium alloy liquid in the crucible into the preheated mold, and finally cool down completely to take out the ingot; (4)热处理：将上述步骤所得铸锭切割成若干个小块，将试样封存在石墨粉里，置于箱式电阻炉中，升温速率为10～12℃/min，升温至530～540℃并保温15～16h，保温结束后于冰水中进行淬火；然后将固溶处理后的试样置于热处理炉中，进行时效处理，升温速率为10～12℃/min，升温至180～200℃并保温8～9h，保温结束后取出空冷，此处得到的是时效处理样品。(4) Heat treatment: Cut the ingot obtained in the above steps into several small pieces, seal the sample in graphite powder, place it in a box-type resistance furnace, and heat up at a rate of 10-12°C/min to 530-540°C. ℃ and keep it warm for 15-16 hours, and then quench it in ice water after the heat preservation is over; then put the solution-treated sample in a heat treatment furnace for aging treatment, the heating rate is 10-12°C/min, and the temperature rises to 180-200 ℃ and keep it warm for 8-9 hours, take it out and air-cool after the heat preservation is over, and the sample obtained here is the aging treatment sample.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112192919A (en) * 2020-10-16 2021-01-08 珠海中科先进技术研究院有限公司 Degradable composite material with antibacterial function and toughness and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101550510A (en) * 2009-05-08 2009-10-07 重庆大学 High intensity degradable biological medical magnesium alloy and preparation method thereof
CN102220529A (en) * 2011-02-23 2011-10-19 郑州大学 Mg-Zn-Y-Nd alloy for novel biodegradable vascular stents and preparation method thereof
WO2011160533A1 (en) * 2010-06-22 2011-12-29 上海交通大学 Magnesium alloy used for degradable implant material of bone in vivo and preparation method thereof
CN106467947A (en) * 2015-08-23 2017-03-01 孙仁 A kind of degradable medical magnesium alloy

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101550510A (en) * 2009-05-08 2009-10-07 重庆大学 High intensity degradable biological medical magnesium alloy and preparation method thereof
WO2011160533A1 (en) * 2010-06-22 2011-12-29 上海交通大学 Magnesium alloy used for degradable implant material of bone in vivo and preparation method thereof
CN102220529A (en) * 2011-02-23 2011-10-19 郑州大学 Mg-Zn-Y-Nd alloy for novel biodegradable vascular stents and preparation method thereof
CN106467947A (en) * 2015-08-23 2017-03-01 孙仁 A kind of degradable medical magnesium alloy

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112192919A (en) * 2020-10-16 2021-01-08 珠海中科先进技术研究院有限公司 Degradable composite material with antibacterial function and toughness and preparation method thereof

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