CN106957999A - A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof - Google Patents

A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof Download PDF

Info

Publication number
CN106957999A
CN106957999A CN201710123451.8A CN201710123451A CN106957999A CN 106957999 A CN106957999 A CN 106957999A CN 201710123451 A CN201710123451 A CN 201710123451A CN 106957999 A CN106957999 A CN 106957999A
Authority
CN
China
Prior art keywords
magnesium
yttrium
zinc
alloy material
alloy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710123451.8A
Other languages
Chinese (zh)
Inventor
何美凤
任帅
刘芳
潘登
周锟广
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Shanghai for Science and Technology
Original Assignee
University of Shanghai for Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Shanghai for Science and Technology filed Critical University of Shanghai for Science and Technology
Priority to CN201710123451.8A priority Critical patent/CN106957999A/en
Publication of CN106957999A publication Critical patent/CN106957999A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/11Making amorphous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/005Amorphous alloys with Mg as the major constituent

Abstract

A kind of magnesium zinc yttrium amorphous alloy material, is prepared from by magnesium, zinc and yttrium, in magnesium zinc yttrium amorphous alloy material, and the mass percent concentration of zinc is 2at % ~ 20at%, and the mass percent concentration of yttrium is 2at % ~ 20at%, and surplus is magnesium.The preparation method of above-mentioned alloy material is additionally provided, is put into together in reaction vessel after magnesium, zinc and yttrium are mixed, reaction vessel is put into vaccum sensitive stove, argon gas is filled with;Vaccum sensitive stove is heated to 400 600 DEG C, uniform temperature is reduced until completely melted and is stirred, furnace temperature is then risen into 400 600 DEG C of 5 30min of insulation, 350 580 DEG C is cooled to, then cools down;Alloy is cut into small pieces, using vacuum list roller melt supercooled equipment, amorphous sample is prepared, obtains magnesium zinc yttrium amorphous alloy material.The magnesium zinc yttrium amorphous alloy material of the present invention has higher corrosion resistance, reduces the degradation speed of magnesium alloy.

Description

A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof
Technical field:
The invention belongs to field of metallurgy, it is related to a kind of biological and medicinal implant material, specifically a kind of magnesium zinc yttrium non-crystaline amorphous metal Material and preparation method thereof.
Background technology:
Being applied to clinical biomedical metal material at present mainly has stainless steel, cochrome and titanium alloy etc., although their corrosion resistants Erosion is functional, in vivo can for a long time holding structure it is stable, but such material in vivo easily because of friction generation abrasive dust or because Slight erosion produces poisonous ion, reduces its biocompatibility.For example:After 316L stainless steels implantation human body, in physiological system ring In border, the problems such as crevice corrosion, fretting corrosion and fatigue corrosion rupture is produced sometimes, and can be because of reasons such as fretting wears Discharge Ni2+、Cr3+And Cr5+, so as to cause prosthetic loosening, ultimately result in implant failure;Again for example:Whether it is initial Ti6Al4V, or subsequent Ti5Al2.5Fe and Ti6Al7Nb alloys, such alloy contains Al elements, and Al elements can cause organ Damage, cause the symptoms such as osteomalacia, anaemia and neurological disorders;Further, the elastic modelling quantity of stainless steel is about 200 GPa, and titanium is closed Gold is about 100 GPa, and the elastic modelling quantity of people's bone only has 10~30 GPa, can so produce stress-shielding effect, causes healing It is slow, or even graft failure.In addition, for the non-degradable material in human body, be temporarily implanted material, this kind of materials application in Stress-shielding effect, and non-degradable easily are produced during Bone Defect Repari, such as material is temporarily implanted, need to be taken by second operation Go out, the pain and medical expense burden of increase patient.Magnesium alloy is applied to clinic as medical embedded material with existing Metal material is compared, with following advantage:(1) magnesium has good biocompatibility with human body.Magnesium ion almost participates in human body Interior all metabolic processes, harmful effect will not be produced under appropriate metabolic conditions to human body;(2) magnesium can be in human body Degraded.Magnesium has very low standard electrode potential, and magnesium ion is degraded into human body fluid, can be by surrounding body tissues Absorb;(3) magnesium is the indispensable element of bone uptake.Magnesium ion can promote the deposition of calcium, promote the formation of osteocyte, accelerate being cured for bone Close etc..There are some researches show growth unrestraint of the magnesium to osteocyte is acted on, also acellular dissolving.(4) magnesium alloy has suitable machine Tool performance, can avoid stress-shielding effect.The density of magnesium alloy is coincide with people's bone, is preferable bone plate.(5) it is magnesium alloy molded Good, the aboundresources of property, price is low.It can obtain what is needed by various ways such as hot investment casting, extruding, punching press, machinings Variously-shaped magnesium-alloy material.Therefore, magnesium alloy can be used as effective medical embedded material.
In a word, magnesium and magnesium alloy are as medical material compared with traditional material, and two the most prominent features are good Biocompatibility and degradability.Although magnesium and its alloy have had the research history in nearly twoth century as implantation material, It is to realize commercialization implantation material so as to be widely used, magnesium and magnesium alloy can not also reach requirement all the time.But magnesium and Good biocompatibility and degradability that magnesium alloy has by it, are still favored by many researchers, in biology Field of medical materials has very big application potential.The clinical practice problem encountered of current magnesium and magnesium alloy is also mainly body Now in terms of the two, one is that medical science aspect does not have systematic evaluation criterion and body to the clinical practice performance of magnesium and magnesium alloy System, in terms of two are materialogy, magnesium and magnesium alloy face and are occurring the problem of degraded is too fast after implanting, so as to cause material Premature failure.
Solving medical magnesium alloy Problems has following method:The biological capacitive that system is set up in terms of medical science evaluates body System;Improve in terms of materialogy decay resistance (1) the exploitation high purity magnesium alloy (2) of medical magnesium alloy improve magnesium alloy into Divide and microstructure (3) Mg alloy surface processing (4) flash set technology(5)Heat treatment technics(6)Magnesium-based composite material.
The content of the invention:
For above-mentioned technical problem of the prior art, the invention provides a kind of magnesium zinc yttrium amorphous alloy material and its preparation side Method, described this magnesium zinc yttrium amorphous alloy material and preparation method thereof will solve magnesium of the prior art and magnesium alloy in implantation Degraded is too fast after in vivo, so as to cause the technical problem of alloy material premature failure.
The invention provides a kind of magnesium zinc yttrium amorphous alloy material, it is prepared from by magnesium, zinc and yttrium, in described magnesium zinc yttrium In amorphous alloy material, the mass percent concentration of zinc is 2at % ~ 20at%, the mass percent concentration of yttrium for 2at % ~ 20at%, surplus is magnesium, and the purity of described magnesium, zinc and yttrium is 99.9 more than wt%.
Present invention also offers a kind of preparation method of above-mentioned magnesium zinc yttrium amorphous alloy material, comprise the following steps:
1)Magnesium, zinc and yttrium are weighed according to mass percent, and the purity of described magnesium, zinc and yttrium is 99.9 more than wt%;
2)Using vacuum induction melting furnace, it is put into together in reaction vessel after magnesium, zinc and yttrium are mixed, the small magnesium of density is placed on Reaction vessel, is then put into vaccum sensitive stove by bottom;
3)Mechanical pump is opened, until when air pressure reaches below 5MPa in vaccum sensitive stove, diffusion pump is then driven, until vacuum sense Air pressure in stove is answered to reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is less than 1 atmospheric pressure, turns off argon inlet Mouthful;
4)Vaccum sensitive stove is heated to 400-600 DEG C, until completely melted, keeps furnace temperature constant, turn on agitator stirring 5- 30min, 400-600 DEG C of insulation 5-30min is risen to after stirring by furnace temperature;
5)When being cooled to 350-580 DEG C, alloy liquid in reaction vessel is poured into copper-made mould, then furnace cooling;
6)By step 5)Alloy be cut into small pieces, using vacuum list roller melt supercooled equipment, prepare thread and banding amorphous Sample, obtains magnesium zinc yttrium amorphous alloy material.
The present invention is, by improving the composition and microstructure of magnesium alloy, traditional magnesium alloy to be added into zinc and yttrium, Magnesium-base Amorphous Materials are prepared by high melt and RAPID SOLIDIFICATION TECHNIQUE, to improve the corrosion resistance of magnesium alloy.In recent years, it is golden Category glass causes the substantial amounts of concern of scientific circles, is the application of the 26S Proteasome Structure and Function of promising material.Many successful amorphous System, including Zr, Fe, Mg, Ni, Cu based alloy, have been developed in the past few decades.In these non-crystaline amorphous metals, magnesium-based Glassy metal(MMGS)Display application implantating biological material is afforded food for thought due to its unordered atomic structure current potential, low elasticity mould Amount, good biocompatibility and biodegradability.However, magnesium alloy has certain limitation, such as their intensity can be by Gradually deteriorate, in corrosion/degradation process, be currently available that the speed of corrosion/degradation rate of magnesium alloy than knitting rate.Therefore, It is that a kind of degradation rate of exploration is low and the uniform magnesium alloy of corrosion is extremely important.There is research, zinc member is added in the magnesium alloy Element is used for controlling its degradation process and preparing novel magnesium alloy to replace high molecular polymer.In addition, Ca, Mn, and zinc, magnesium is few Amount rare earth element can slow down the magnesium alloy of degradation rate, and zinc is the essential trace elements of the human body, is mainly distributed on all organs It is that Chengdu formation collagen synthesis is very important with the blood in body.Zn contents account for the 2.5g of human body, and about 15mg is every Day demand, Zn is human energy metabolism, and the effect with anti-inflammation, is absorbed in right amount nontoxic.In addition, containing in magnesium alloy Zn-ef ficiency can produce passivation, improve the pitting potential of alloy;Zinc can reduce the corrosion rate of pure magnesium, carry high purity magnesium Corrosion resistance;Zinc can improve corrosion potential of the magnesium in SBF solution, reduce alloy corrosion degradation rate.
Another Yt of the present invention(Y)It is that known can improve metallicity.Y reduces corrosion rate and thin simultaneously Change the microscopic structure of magnesium alloy, illustrate that Y can improve magnesium alloy mechanical performance and corrosion-resistant.Add Y, rare earth compound life The corrosion resistance of alloy can be improved into low activity.Other reports of rare earth element can purify the corrosion resistant that magnesium alloy improves alloy Corrosion liquid;A stabilization, fine and close surface protection film can also be formed, protection includes alloy.Cytotoxicity and hemolytic test table Bright Mg-Zn-Y amorphous does not cause significant toxicity, and inducing osteoblast is less than 5% haemolysis, illustrates that alloy element Y is closed to magnesium Application of the gold in biomedicine has a positive effect.
The a kind of of the present invention than traditional magnesium alloy there is novel magnesium alloy-pearl powder compared with highly corrosion resistant ability to be combined Material, reduces the degradation speed of magnesium alloy compared with traditional magnesium alloy, realizes homogeneous corrosion effect at a slow speed, is easy to evaluate biological The degradation cycle of material is implanted into, value of the magnesium alloy in medical embedded material field is improved.
The density and modulus of the non-crystalline material of the present invention are using natural skeleton as target, but zinc, and the determination of yttrium content is comprehensive Close the requirement in terms of consideration composite density, intensity, corrosion resistance and bone formation performance.
Due to the content of magnesium, zinc and yttrium, and operating air pressure can be controlled in the preparation of the whole sample of the present invention Heating-up temperature, melt institute's pressure difference and copper roller rotating speed with device frequency and melt etc. obtain different samples.
The present invention uses vacuum induction melting, and vacuum list roller fast melt-quenching technology, the amorphous magnesium for having prepared high-purity is closed Gold.The magnesium zinc yttrium amorphous alloy material of the present invention has good bio-compatibility.The present invention it is carried out materialogy characterize and The test of performance in human simulation body fluid, can reach the effect of homogeneous corrosion, be easy to evaluate the degraded of biological implantation material Cycle.
The present invention is compared with prior art, and its technological progress is significant.
(1)Material system magnesium selected by the present invention, zinc, yttrium powder be it is existing be applied to industrial material, it Mature preparation process, performance is stable, is adapted to large-scale industrial production.
(2)The density of magnesium zinc yttrium amorphous alloy material of the present invention, intensity, elastic modelling quantity(Determine mechanics adaptability)And it is raw Thing activity can be controlled by zinc, the design of yttrium content, make its density and mechanics adaptability near in people's bone photo;
(3)Material system magnesium zinc yttrium selected by the present invention is respectively provided with good bio-compatibility, and is all beneficial, magnesium to human body One of the essential trace elements of the human body, it is that animal in-vivo content is only second to calcium, sodium, potassium, the intracellular sun for being only second to potassium from Son.Magnesium almost metabolic processes all in participant's body, include the formation of osteocyte, accelerate knitting ability.Magnesium also with Nerve, muscle and cardiac function are in close relations.
(4)Magnesium zinc yttrium amorphous alloy material prepared by the present invention improves the corrosion resistance of traditional magnesium alloy, can The degradation speed of magnesium alloy is effectively reduced, homogeneous corrosion effect at a slow speed is realized, is easy to evaluate the degraded week of biological implantation material Phase, improve value of the magnesium alloy in medical embedded material field.
Brief description of the drawings
Fig. 1 is Mg70-xZn30Yx(x=4,6,8at.%) polarization curve in simulated body fluid.
Relation curve between polarization curve galvanic current or polarized current density, the curve that the anode and negative electrode of electrode are obtained It is referred to as anodic polarization curves (anodic polarization curve) or cathodic polarization curve (cathodic polarization curve).Polarization curve can be by active dissolution area, transition passivation region, stable passivation region, trans-passive region etc. Four region compositions.By testing polarization curve, the decay resistance of metal can be studied, this is research metalwork corrosion mechanism Basic skills.Corresponding abscissa in polarization curve is current density, and corresponding ordinate is potential.Polarization curve In the corrosion potential that measures it is bigger, current density is smaller, and measured corrosive nature is better, and decay resistance is higher.By in figure It is observed that in the corrosion starting stage, with the increase of anode potential, corrosion electric current density is slowly increased.For Mg66Zn30Y4, when current potential increases to about 50 mV, corrosion potential, corrosion electric current density increase sharply.This shows, Mg66Zn30Y4Surface Creation protective oxide film, greatly slow down the corrosion of substrate material surface.When anode potential reaches film After disruptive potential, surface film oxide fracture, alloy substrate continues to corrode.For Mg64Zn30Y6, when current potential increases to about 180 mV, During 380mv, corrosion current density increase.As a result show, protection oxide-film production twice is had when current potential increases.For Mg62Zn30Y8, there is three protective oxide film generations in 130mV, 220mV and 380mV.This means in Mg62Zn30Y8 Alloy surface, the protective effect of oxide-film is maximally effective.
Fig. 2 is Mg70-xZn30Yx(x=4,6,8at.%) the OCP figure in simulated body fluid.
OCP:Refer to the current potential of system residing for sample when electrical current is 0, also known as corrosion potential.In open circuit Under current potential, sample is in self-corrosion state.Current potential(OCP)Refer to without extrinsic current by when system current potential.Mg66Zn30Y4(Y- 4), Mg64Zn30Y6(Y-6)And Mg62Zn30Y8(Y-8)Open circuit point position be -0.25 V/ SCE, -0.38 V/ SCE respectively and -0.37 V/ SCE。
Fig. 3 is Gegenbaur's cell in different amorphous leaching liquid cultures cytotoxicity flow cytometer detection (a) Mg two days later66Zn30Y4, (b) Mg64Zn30Y6, (c) Mg62Zn30Y8(d) control group;Apoptosis is used in experiment --- Annexin V- FITC/PI double-staining apoptosis kits.
1) it is the part of the third quadrant in Fig. 3, i.e. bottom left section in figure when feminine gender is presented in PI and FITC(LL)For Cell is no apoptosis, and cell is normal living cells.
2) when positive and FITC, which is presented, in PI is presented negative, when being the second quadrant in Fig. 3, i.e. upper left in figure (UL)Cell is in damage, necrosis or dead state.
3) when the positive is presented in PI and FITC, during the first quartile part for being Fig. 3, i.e., the first quartile part in figure (UR), cell is considered to be in late apoptic state.
4) when feminine gender is presented in PI and FITC is to be presented positive, the lower right-most portion in the fourth quadrant part for being Fig. 3, i.e. figure (LR), cell is in early apoptosis state.
Cell under each sample leaching liquor culture ratio substantially phase shared under each state as can be seen from Figure 3 Together, the cell number in the Apoptosis phase(It is the upper right portion+lower right-most portion i.e. UR+LR of figure)And also essentially the same be. Sample Y-4, Y-6, Y-8 apoptotic cell ratio, respectively 4.9%, 5.26%, 2.05%, control group apoptotic cell ratio is 2.44%. Sample Y-4, Y-6, Y-8 viable apoptotic cell ratio, respectively 8.29%, 6.74%, 1.34%, and control group viable apoptotic cell Ratio is 3.46%.From laboratory sample it could be assumed that, with the increase of Y contents, cytotoxicity is reduced, sample Y-8 is to cell Activity has little to no effect, and shows good biocompatibility.
Specific embodiment:
Embodiment 1:
A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof, comprises the following steps:
(1)The raw material prepared are put into ultrasonic cleaner and clean a few minutes.Raw material after having cleaned and required Intermediate alloy be put into platinum crucible (the small Mg of density be placed on bottom) together, wherein 30 at of at %, Zn of Mg 66 Material, is then put into vaccum sensitive stove by the at % of %, Y 4.And by smelting furnace good seal.
(2)Mechanical pump is opened, until when air pressure reaches below 5MPa in stove, diffusion pump is then driven, until air pressure in stove Reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is about less than 1 atmospheric pressure, turns off argon inlet mouthful.
(3)Metal molten state is watched when smelting furnace is always heated into 600 DEG C, until completely melted turn on agitator 6min is sufficiently stirred at 570 DEG C, furnace temperature is risen into 600 DEG C of insulation 20min after stirring.
(4)When being cooled to about 570 DEG C, alloy liquid in crucible is poured into copper-made mould, then furnace cooling.
(5)Foundry alloy is cut into small pieces, takes 5g or so to be put into advance with the good quartz ampoule of alcohol washes, using vacuum Single roller melt supercooled equipment, roller degree of hastening is set as 45m/s.
(6) materialogy sign is carried out to it and corrosion and the test of bio-compatible performance in human simulation body fluid.(It is real Test result 1 sample Y-4, the sample Y-4 of accompanying drawing 2, accompanying drawing 3 referring to the drawings(a))
Prepared magnesium zinc yttrium amorphous alloy material improves the corrosion resistance of traditional magnesium alloy, can effectively reduce magnesium alloy Degradation speed, realize homogeneous corrosion effect at a slow speed, be easy to evaluate the degradation cycle of biological implantation material, improve magnesium alloy and exist The value in medical embedded material field.
Embodiment 2:
A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof, comprises the following steps:
(1)The raw material prepared are put into ultrasonic cleaner and clean a few minutes.Raw material after having cleaned and required Intermediate alloy be put into platinum crucible (the small Mg of density be placed on bottom) together, wherein 30 at of at %, Zn of Mg 64 Material, is then put into vaccum sensitive stove by the at % of %, Y 6.And by smelting furnace good seal.
(2)Mechanical pump is opened, until when air pressure reaches below 5MPa in stove, diffusion pump is then driven, until air pressure in stove Reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is about less than 1 atmospheric pressure, turns off argon inlet mouthful.
(3)Metal molten state is watched when smelting furnace is always heated into 600 DEG C, until completely melted turn on agitator 6min is sufficiently stirred at 570 DEG C, furnace temperature is risen into 600 DEG C of insulation 20min after stirring.
(4)When being cooled to about 570 DEG C, alloy liquid in crucible is poured into copper-made mould, then furnace cooling.
(5)Foundry alloy is cut into small pieces, takes 5g or so to be put into advance with the good quartz ampoule of alcohol washes, using vacuum Single roller melt supercooled equipment, roller degree of hastening is set as 45m/s.
(6) materialogy sign is carried out to it and corrosion and the test of bio-compatible performance in human simulation body fluid.(It is real Test result 1 sample Y-6, the sample Y-6 of accompanying drawing 2, accompanying drawing 3 referring to the drawings(b))
Prepared magnesium zinc yttrium amorphous alloy material improves the corrosion resistance of traditional magnesium alloy, can effectively reduce magnesium alloy Degradation speed, realize homogeneous corrosion effect at a slow speed, be easy to evaluate the degradation cycle of biological implantation material, improve magnesium alloy and exist The value in medical embedded material field.
Embodiment 3:
A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof, comprises the following steps:
(1)The raw material prepared are put into ultrasonic cleaner and clean a few minutes.Raw material after having cleaned and required Intermediate alloy be put into platinum crucible (the small Mg of density be placed on bottom) together, wherein 30 at of at %, Zn of Mg 62 Material, is then put into vaccum sensitive stove by the at % of %, Y 8.And by smelting furnace good seal.
(2)Mechanical pump is opened, until when air pressure reaches below 5MPa in stove, diffusion pump is then driven, until air pressure in stove Reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is about less than 1 atmospheric pressure, turns off argon inlet mouthful.
(3)Metal molten state is watched when smelting furnace is always heated into 600 DEG C, until completely melted turn on agitator 6min is sufficiently stirred at 570 DEG C, furnace temperature is risen into 600 DEG C of insulation 20min after stirring.
(4)When being cooled to about 570 DEG C, alloy liquid in crucible is poured into copper-made mould, then furnace cooling.
(5)Foundry alloy is cut into small pieces, takes 5g or so to be put into advance with the good quartz ampoule of alcohol washes, using vacuum Single roller melt supercooled equipment, roller degree of hastening is set as 45m/s.
(6) materialogy sign is carried out to it and corrosion and the test of bio-compatible performance in human simulation body fluid.
(Experimental result is referring to the drawings 1 sample Y-8, the sample Y-8 of accompanying drawing 2, accompanying drawing 3(c))
Prepared magnesium zinc yttrium amorphous alloy material improves the corrosion resistance of traditional magnesium alloy, can effectively reduce magnesium alloy Degradation speed, realize homogeneous corrosion effect at a slow speed, be easy to evaluate the degradation cycle of biological implantation material, improve magnesium alloy and exist The value in medical embedded material field.
Embodiment 4:
A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof, comprises the following steps:
(1)The raw material prepared are put into ultrasonic cleaner and clean a few minutes.Raw material after having cleaned and required Intermediate alloy be put into platinum crucible (the small Mg of density be placed on bottom) together, wherein 30 at of at %, Zn of Mg 64 Material, is then put into vaccum sensitive stove by the at % of %, Y 6.And by smelting furnace good seal.
(2)Mechanical pump is opened, until when air pressure reaches below 5MPa in stove, diffusion pump is then driven, until air pressure in stove Reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is about less than 1 atmospheric pressure, turns off argon inlet mouthful.
(3)Metal molten state is watched when smelting furnace is always heated into 600 DEG C, until completely melted turn on agitator 6min is sufficiently stirred at 570 DEG C, furnace temperature is risen into 600 DEG C of insulation 20min after stirring.
(4)When being cooled to about 570 DEG C, alloy liquid in crucible is poured into copper-made mould, then furnace cooling.
(5)Foundry alloy is cut into small pieces, takes 5g or so to be put into advance with the good quartz ampoule of alcohol washes, using vacuum Single roller melt supercooled equipment, roller degree of hastening is set as 40m/s.
(6) materialogy sign is carried out to it and corrosion and the test of bio-compatible performance in human simulation body fluid.
(Experimental result is referring to the drawings 1 sample Y-6, the sample Y-6 of accompanying drawing 2, accompanying drawing 3(b))
Prepared magnesium zinc yttrium amorphous alloy material improves the corrosion resistance of traditional magnesium alloy, can effectively reduce magnesium alloy Degradation speed, realize homogeneous corrosion effect at a slow speed, be easy to evaluate the degradation cycle of biological implantation material, improve magnesium alloy and exist The value in medical embedded material field.
Embodiment 5:
A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof, comprises the following steps:
(1)The raw material prepared are put into ultrasonic cleaner and clean a few minutes.Raw material after having cleaned and required Intermediate alloy be put into platinum crucible (the small Mg of density be placed on bottom) together, wherein 30 at of at %, Zn of Mg 64 Material, is then put into vaccum sensitive stove by the at % of %, Y 6.And by smelting furnace good seal.
(2)Mechanical pump is opened, until when air pressure reaches below 5MPa in stove, diffusion pump is then driven, until air pressure in stove Reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is about less than 1 atmospheric pressure, turns off argon inlet mouthful.
(3)Metal molten state is watched when smelting furnace is always heated into 600 DEG C, until completely melted turn on agitator 6min is sufficiently stirred at 570 DEG C, furnace temperature is risen into 600 DEG C of insulation 20min after stirring.
(4)When being cooled to about 570 DEG C, alloy liquid in crucible is poured into copper-made mould, then furnace cooling.
(5)Foundry alloy is cut into small pieces, takes 5g or so to be put into advance with the good quartz ampoule of alcohol washes, using vacuum Single roller melt supercooled equipment, roller degree of hastening is set as 35m/s.
(6) materialogy sign is carried out to it and corrosion and the test of bio-compatible performance in human simulation body fluid.
(Experimental result is referring to the drawings 1 sample Y-6, the sample Y-6 of accompanying drawing 2, accompanying drawing 3(b))
Prepared magnesium zinc yttrium amorphous alloy material improves the corrosion resistance of traditional magnesium alloy, can effectively reduce magnesium alloy Degradation speed, realize homogeneous corrosion effect at a slow speed, be easy to evaluate the degradation cycle of biological implantation material, improve magnesium alloy and exist The value in medical embedded material field.

Claims (2)

1. a kind of magnesium zinc yttrium amorphous alloy material, it is characterised in that:It is prepared from by magnesium, zinc and yttrium, it is non-in described magnesium zinc yttrium In peritectic alloy material, the mass percent concentration of zinc is 2at % ~ 20at%, and the mass percent concentration of yttrium is 2at % ~ 20at% , surplus is magnesium, and the purity of described magnesium, zinc and yttrium is more than 99.9wt%.
2. the preparation method of a kind of magnesium zinc yttrium amorphous alloy material described in claim 1, it is characterised in that comprise the following steps:
1)Magnesium, zinc and yttrium are weighed according to mass percent, and the purity of described magnesium, zinc and yttrium is 99.9 more than wt%;
2)Using vacuum induction melting furnace, it is put into together in reaction vessel after magnesium, zinc and yttrium are mixed, the small magnesium of density is placed on most Below, then reaction vessel is put into vaccum sensitive stove;
3)Mechanical pump is opened, until when air pressure reaches below 5MPa in vaccum sensitive stove, diffusion pump is then driven, until vacuum sense Air pressure in stove is answered to reach 10-2During MPa, argon gas is filled with, when argon gas aeration quantity is less than 1 atmospheric pressure, turns off argon inlet Mouthful;
4)Vaccum sensitive stove is heated to 400-600 DEG C, until completely melted, keeps furnace temperature constant, turn on agitator stirring 5- 30min, 400-600 DEG C of insulation 5-30min is risen to after stirring by furnace temperature;
5)When being cooled to 350-580 DEG C, alloy liquid in reaction vessel is poured into copper-made mould, then furnace cooling;
6)By step 5)Alloy be cut into small pieces, using vacuum list roller melt supercooled equipment, prepare thread and banding amorphous Sample, obtains magnesium zinc yttrium amorphous alloy material.
CN201710123451.8A 2017-03-03 2017-03-03 A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof Pending CN106957999A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710123451.8A CN106957999A (en) 2017-03-03 2017-03-03 A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710123451.8A CN106957999A (en) 2017-03-03 2017-03-03 A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN106957999A true CN106957999A (en) 2017-07-18

Family

ID=59471704

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710123451.8A Pending CN106957999A (en) 2017-03-03 2017-03-03 A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106957999A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112210729A (en) * 2020-09-29 2021-01-12 上海理工大学 Ternary Mg-Zn-Ce amorphous alloy and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5348591A (en) * 1991-09-06 1994-09-20 Tsuyoshi Masumoto High-strength amorphous magnesium alloy
US5423969A (en) * 1991-03-07 1995-06-13 Ykk Corporation Sacrificial electrode material for corrosion prevention
JP2001207255A (en) * 2000-01-27 2001-07-31 Akihisa Inoue Magnesium alloy, and apparatus and method for manufacturing the same
US20050279427A1 (en) * 2004-06-14 2005-12-22 Park Eun S Magnesium based amorphous alloy having improved glass forming ability and ductility
CN101148711A (en) * 2007-10-18 2008-03-26 同济大学 Method for preparing Mg-base large-block amorphous alloy
CN104674093A (en) * 2013-12-03 2015-06-03 上海航天精密机械研究所 Medical high-toughness corrosion-resistant magnesium based composite material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5423969A (en) * 1991-03-07 1995-06-13 Ykk Corporation Sacrificial electrode material for corrosion prevention
US5348591A (en) * 1991-09-06 1994-09-20 Tsuyoshi Masumoto High-strength amorphous magnesium alloy
JP2001207255A (en) * 2000-01-27 2001-07-31 Akihisa Inoue Magnesium alloy, and apparatus and method for manufacturing the same
US20050279427A1 (en) * 2004-06-14 2005-12-22 Park Eun S Magnesium based amorphous alloy having improved glass forming ability and ductility
CN101148711A (en) * 2007-10-18 2008-03-26 同济大学 Method for preparing Mg-base large-block amorphous alloy
CN104674093A (en) * 2013-12-03 2015-06-03 上海航天精密机械研究所 Medical high-toughness corrosion-resistant magnesium based composite material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马毅龙等: "《现代化学功能材料及其应用研究》", 30 May 2015, 中国水利水电出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112210729A (en) * 2020-09-29 2021-01-12 上海理工大学 Ternary Mg-Zn-Ce amorphous alloy and preparation method thereof

Similar Documents

Publication Publication Date Title
CN109680195B (en) Mg-RE series magnesium alloy and preparation method and application thereof
CN102296220B (en) Biomedical corrosion-proof magnesium alloy and preparation method thereof
CN110423933A (en) A kind of bio-medical Ti-Zr-Hf-Nb-Ta system's high-entropy alloy and preparation method
CN108277386A (en) A kind of Zn-Li-Mg systems kirsite and the preparation method and application thereof
CN105154735B (en) Degradable biomedical Mg-Nd-Sr magnesium alloy as well as preparation method and application thereof
CN109097629A (en) A kind of biodegradable Zn-Mo system kirsite and preparation method thereof
CN104099501B (en) A kind of Margarita powder/magnesium alloy quasi natural bone composite and preparation method thereof
CN107190191B (en) A kind of biological medical magnesium alloy and preparation method thereof
CN105274393B (en) A kind of β types Zr Ti Nb Sn systems alloy and preparation method thereof
CN107456601A (en) A kind of Zn-Cu systems kirsite and preparation method and application
CN108203778B (en) Zr-based biomedical alloy and preparation method thereof
CN104674093B (en) Medical high-toughness corrosion-resistant magnesium based composite material and preparation method thereof
CN108754232A (en) High-strength high-plastic biodegradable Zn-Mn-Li systems kirsite of one kind and application thereof
CN107460372A (en) A kind of Zn Mn systems kirsite and preparation method and application
CN108315583A (en) A kind of Zn-Li-Mn systems kirsite and the preparation method and application thereof
CN102258806B (en) Degradable magnesium-base biomedical material for implantation in orthopaedics, and preparation method thereof
CN103184369A (en) Beta type Zr-Nb-Ti biomedical alloy and preparation method thereof
CN110016600B (en) High-intensitive highly corrosion resistant bio-medical Mg-Ga alloy and preparation method thereof
CN108165782B (en) Medical zinc-based alloy strip and preparation method thereof
CN103343273B (en) biomedical degradable corrosion-resistant Mg-Zn-Zr alloy and preparation method
CN108486450A (en) A kind of bio-medical high-entropy alloy and preparation method thereof
Luo et al. Novel function-structure-integrated Ti-Mo-Cu alloy combined with excellent antibacterial properties and mechanical compatibility as implant application
CN104846247B (en) Addition gadolinium, magnesium alloy biodegradation material of yttrium and preparation method thereof
CN109266909A (en) A kind of medical degradable zinc bismuth system alloy
CN106957999A (en) A kind of magnesium zinc yttrium amorphous alloy material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170718

RJ01 Rejection of invention patent application after publication