CN107739940A - A kind of Biological magnesium alloy with corrosion-resistant function and preparation method thereof - Google Patents
A kind of Biological magnesium alloy with corrosion-resistant function and preparation method thereof Download PDFInfo
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- CN107739940A CN107739940A CN201711011430.3A CN201711011430A CN107739940A CN 107739940 A CN107739940 A CN 107739940A CN 201711011430 A CN201711011430 A CN 201711011430A CN 107739940 A CN107739940 A CN 107739940A
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- magnesium alloy
- biological magnesium
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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
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- 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
Abstract
The invention discloses a kind of Biological magnesium alloy with corrosion-resistant function, the Biological magnesium alloy is made up of Biological magnesium alloy matrix and the graphene oxide being distributed on Biological magnesium alloy matrix crystal boundary；The graphene oxide wrapping biological magnesium alloy crystal grain forms nano-honeycomb the second phase of structure.Invention additionally discloses a kind of preparation method, comprise the following steps：(1) design proportion is pressed, GO powder and Biological magnesium alloy powder are respectively placed in into ultrasonic agitation in absolute ethyl alcohol obtains GO suspension and Biological magnesium alloy suspension；(2) GO suspension is slowly added in Biological magnesium alloy suspension, continues ultrasonic agitation and obtain mixing suspension, mixing suspension obtains dispersed mixed-powder after vacuum filter, drying process；(3) by mixed-powder obtained above under protective atmosphere, the Biological magnesium alloy with corrosion-resistant function is prepared by selective laser fusing.The present invention can be completely cut off contact of the Biological magnesium alloy with body fluid as " protection shield ", be avoided the galvanic effect of conventional second phase, improve decay resistance using the phase of nano-honeycomb structure second of GO structures.
Description
Technical field
The invention belongs to biologic medical technical field of material, more particularly to a kind of biological magnesium with corrosion-resistant function
Alloy and preparation method thereof.
Background technology
In recent years, Biological magnesium alloy because of excellent biocompatibility and with skeleton similar in density and springform
Amount, increasing concern is obtained in fields such as bone tissue engineering scaffold, orthopaedics fixtures.As metal material, biological magnesium
Alloy has the intensity higher than high polymer material, toughness more more preferable than ceramic material, and with traditional stainless steel, titanium alloy etc.
Medical metal is compared, the maximum advantage of Biological magnesium alloy in can in human body it is degradable；Magnesium ion is human body the 4th simultaneously
Abundant cation, it almost take part in all metabolic processes and osteanagenesis can be promoted.However, Biological magnesium alloy is in body fluid
In degradation rate reach 0.2~1.0mm/a, far above Bone Defect Repari requirement<0.1mm/a, it is likely that during service with regard to because
It is too fast degraded and lose structural intergrity；A large amount of hydrogen caused by fast erosion and pH value rise can also hinder wound healing simultaneously
Even result in necrosis.Therefore, how to improve the decay resistance of Biological magnesium alloy, be it as implantation material there is an urgent need to
The problem of solution.
Graphene is a kind of two-dimension nano materials being made up of single layer of carbon atom close-packed arrays.Have benefited from the sp2 rails of uniqueness
Road hydridization connection and two-dimensional structure, graphene have very excellent physical and mechanical properties, specific surface area, fracture strength and bullet
Property modulus respectively reaches 2630m2/ g, 130GPa and 1TPa.Importantly, graphene also possesses prominent permeability resistance and change
Inertia is learned, the isolated area of " labyrinth type " can be erected between matrix and corrosive medium, gas, liquid are hindered by shielding action
The scattering and permeating of the corrosive mediums such as body, ion, and then block the interfacial charge transfer of matrix-corrosive medium.And it is used as graphene
A kind of important derivatives, graphene oxide (GO) not only remains its special layer structure and excellent properties, and in carbon
The oxy radicals such as numerous carboxyls, carbonyl, hydroxyl are distributed with atomic plane, there is good hydrophily and antibiotic property, moreover it is possible to
Promote the deposition of osteoid apatite.It is huge that these characteristics make it that GO has been shown in terms of Biological magnesium alloy decay resistance is improved
Potentiality.
But the research at present on GO/ Biological magnesium alloy decay resistances is seldom, this is due to that Biological magnesium alloy is usual
Prepared using common process such as melting-casting, powder metallurgy, in forming process temperature more than 600 DEG C, for up to a few hours,
So prolonged high temperature action not only easily causes GO structure to be destroyed, and loses its original structure and performance；It can also make simultaneously
Interfacial reaction generation carbide occurs into GO and matrix, reduces the mechanical property of Biological magnesium alloy.Therefore, using GO as the second phase
It is a huge challenge to be effectively combined in Biological magnesium alloy.Existing study limitation is in using GO as face coat or coating
For additive application in Biological magnesium alloy, face coat can only protect Biological magnesium alloy not to be corroded initial stage degraded in implantation, of short duration
The time of contact of magnesium alloy and body fluid is delayed, and after coating breaks down comes off, magnesium alloy substrate loses protection or can occurred
Fast degradation.Therefore, new approach is explored so as to realize the lasting controlled degradation of Biological magnesium alloy, is turned into and is realized its tissue repair
The task of top priority of application.
The content of the invention
A kind of biological magnesium with corrosion-resistant function is provided it is an object of the invention to overcome the deficiencies in the prior art to close
Gold and preparation method thereof, GO, which can pass through, in this method forming process reduces contact and to promote forming core to refine Biological magnesium alloy brilliant
Grain, at the same be distributed in the GO on crystal boundary can wrap up magnesium alloy crystal grain formed nano-honeycomb the second phase of structure.
In order to solve the above technical problems, the Biological magnesium alloy provided by the invention with corrosion-resistant function, the biological magnesium closes
Gold is made up of Biological magnesium alloy matrix and the graphene oxide being uniformly distributed on Biological magnesium alloy matrix crystal boundary；The oxidation stone
Black alkene wrapping biological magnesium alloy crystal grain forms nano-honeycomb the second phase of structure；Wherein, the weight/mass percentage composition of graphene oxide is
0.8-1.2%.
Further, the weight/mass percentage composition of graphene oxide is 0.8-1.0%.
Further, the weight/mass percentage composition of graphene oxide is 1.0%.
A kind of method for preparing preceding claim and having the Biological magnesium alloy of corrosion-resistant function, comprises the following steps：
(1) design proportion is pressed, GO powder and Biological magnesium alloy powder are respectively placed in absolute ethyl alcohol ultrasonic agitation obtain GO and hang
Supernatant liquid and Biological magnesium alloy suspension；
(2) GO suspension is slowly added in Biological magnesium alloy suspension, continues ultrasonic agitation and obtain mixing suspension, mixed
Close suspension and dispersed mixed-powder is obtained after vacuum filter, drying process；
(3) by mixed-powder obtained above under protective atmosphere, it is prepared by selective laser fusing with corrosion resistant
Lose the Biological magnesium alloy of function；In preparation process, to control laser power be 70-90W, sweep speed 100-300mm/min, light
Spot diameter is 50-150 μm, the pressure of protective gas is 4-5.5MPa.
Preferably, laser power 78-85W；Sweep speed is 150-250mm/min；Spot diameter is 80-120 μm；Protect
Protect the pressure 4.8-5.2MPa of gas.
It is further preferable, laser power 80W；Sweep speed is 200mm/min；Spot diameter is 100 μm；Protection
The pressure 5MPa of gas.
Further, described Biological magnesium alloy powder is Mg-3Al-1Zn alloyed powders.
Further, described protective atmosphere is the high-purity argon gas atmosphere that purity is more than or equal to 99.999%.
Further, the thickness of GO powder be 0.8-1.2nm, piece footpath size be 8-15 microns.
Further, in step (2) drying time be 12-24h, drying temperature be 80-90 DEG C.
Further, in step (1) and step (2) ultrasonic agitation rotating speed be 150-300rad/min, time 3-5h.
Principle and advantage
The present invention has attempted that GO is added in Biological magnesium alloy using SLM technologies first, and acquisition has highly corrosion resistant
The Biological magnesium alloy integral material of energy.In the present invention, GO is present on magnesium alloy substrate crystal boundary as the second phase, and wraps up magnesium and close
Jin Jing's particle shape can continue efficiently to send out into the second phase with nano-honeycomb structure with the continuous degraded of Biological magnesium alloy
Wave corrosion-resistant effect.
The present invention is realized by the control to raw material particle size, cooperation ultrasonic agitation and specific sintering process parameter
The refinement of Biological magnesium alloy crystal grain and build to form the phase of nano-honeycomb structure second using GO parcel magnesium alloy crystal grain, utilize
Second phase avoids the galvanic effect of conventional second phase, carried as contact of " protection shield " isolation Biological magnesium alloy with body fluid
Its high decay resistance.The present invention is under the synergy of feedstock Particle size, ultrasonic agitation and specific SLM techniques, GO
Magnesium alloy crystal grain can be wrapped up and form nano-honeycomb the second phase of structure, so as to as " protection shield " isolation Biological magnesium alloy and body fluid
Contact, while pass through reduce contact and promote forming core refine Biological magnesium alloy crystal grain, there is provided the mechanical property of Biological magnesium alloy,
In addition, by adjusting GO contents and size, the speed of Biological magnesium alloy degraded can also be adjusted, this is the material designed by the present invention
Material is used as implant, has more favorable advantage.
The present invention is after ultrasonic agitation, and using the SLM techniques of special parameter, the high cooldown rate of SLM techniques can make
Biological magnesium alloy quickly solidifies, so that GO structure is not destroyed, while obtains uniformly tiny microstructure.Due into
Divide and the inconsistent situation appearance of degradation rate is uniformly just not present.
GO powder and Biological magnesium alloy powder cleverly are separately stirred by ultrasonic to obtain after suspension to remix and stirred by the present invention
Mix：Successfully solve the problems, such as that by the directly mixing of the powder of two kinds of aggregated forms be difficult to obtain dispersed mixed-powder.
The present invention avoids conventional ball-milling process from destroying GO structure by wet-mixing.Work is stirred by ultrasonic by controlling
Skill realizes that GO and magnesium alloy powder uniformly mix, and GO surfaces are negatively charged, easily by electrostatic interaction absorption in magnesium alloy particles,
In forming process, GO is present on magnesium alloy substrate crystal boundary as the second phase, and the crystal grain formation of parcel magnesium alloy has nanometer honeybee
Second phase of nest structure, while the ultrafast heating of laser can avoid the structure of the phase of nano-honeycomb structure second from breaking with cooldown rate
It is bad.And when parameter is stirred by ultrasonic not in invention which is intended to be protected, it is difficult to form nano-honeycomb structure the second phase bag
Effect is wrapped up in, is also easy to produce reunion, aggravates galvanic corrosion, so as to accelerate degradation process, and reduces the mechanical property of matrix；And work as laser
When molding parameter is not in invention which is intended to be protected, the phase of nano-honeycomb structure second may produce structure destroy and
Chemical reaction generation carbide between magnesium alloy substrate, so as to cause GO to lose its original structure and performance, loses protection and makees
With, and damage the mechanical property of matrix.When the rotating speed of ultrasonic agitation and time is not in invention which is intended to be protected, nothing
Method realizes the dispersed of GO and magnesium alloy powder, and then is difficult to form nano-honeycomb structure the second phase package action, or even production
It is raw to reunite, aggravate galvanic corrosion, so as to accelerate degradation process, and reduce the mechanical property of matrix.When GO contents are less than the present invention
During the scope of selection, package action can not be played, can only be used as the distributed mutually of disperse second that it is rotten to form galvanic couple in magnesium alloy substrate
Erosion, accelerates the degraded of magnesium alloy；And when GO too high levels, it is difficult to it is dispersed, reunion is easily produced, can also form galvanic couple corruption
Erosion, accelerate degraded, and reduce mechanical property.
In summary, the feedstock Particle size in the present invention, the ultrasonic agitation technique such as technological parameter and SLM technological parameters
The selection of parameter is not random value, but tests, pays the crystallization of creative work many times by inventor, in each work
Under the synergy of skill parameter, the GO of addition can be present on magnesium alloy substrate crystal boundary as the second phase, and wrap up magnesium alloy
Crystal grain forms the second phase with nano-honeycomb structure, and then obtains the Biological magnesium alloy entirety material with high-corrosion resistance
Material.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
GO powder and Mg-3Al-1Zn alloy powders are used as raw material, by 1:It is (thick that 99 mass ratio weighs 0.1gGO powder
Spend for 0.8-1.2nm, piece footpath 8-15 microns) and 9.9gMg-3Al-1Zn alloy powders, it is respectively placed in two 1L beakers, slowly
250ml absolute ethyl alcohols are added, ultrasonic agitation obtains GO suspension and Mg- under conditions of rotating speed 250rad/min, time 4h
3Al-1Zn suspension, GO suspension is slowly added in Mg-3Al-1Zn suspension, continued in rotating speed 250rad/min, time
Ultrasonic agitation obtains GO/Mg-3Al-1Zn suspension under conditions of 4h, (the drying temperature 80- after vacuum filter, dry 24h
90 DEG C), obtain dispersed GO/Mg-3Al-1Zn mixed-powders.It is in the protection of 99.999% high-purity argon gas, atmosphere pressures
5MPa, 100 μm of spot diameter, laser power 80W, sweep speed 200mm/min process conditions under, utilize SLM techniques prepare
GO/Mg-3Al-1Zn alloys.
Test finds that GO holding structure can stablize in SLM forming processes, and wrap up Mg-3Al-1Zn alloy grain shapes
Into the phase of nano-honeycomb structure second；Compared to Mg-3Al-1Zn alloys, GO/Mg-3Al-1Zn alloy surfaces form more phosphorus
Lime stone, it is often more important that, effectively completely cut off Mg-3Al-1Zn alloys and body fluid using the GO phases of nano-honeycomb structure second built
Contact, so as to greatly improved decay resistance, the degradation rates of GO/Mg-3Al-1Zn alloys is 0.15mm/year, the limit
Tensile strength is 315MPa.
Embodiment 2
It is raw material to use GO powder (thickness 0.8-1.2nm, piece footpath 8-15 microns) and Mg-3Al-1Zn alloy powders, is pressed
0.8:99.2 mass ratio weighs 0.08gGO powder and 9.92gMg-3Al-1Zn alloy powders, is respectively placed in two 1L beakers
In, 250ml absolute ethyl alcohols are slowly added to, ultrasonic agitation obtains GO suspension under conditions of rotating speed 250rad/min, time 4h
With Mg-3Al-1Zn suspension, GO suspension is slowly added in Mg-3Al-1Zn suspension, continue rotating speed 250rad/min,
Ultrasonic agitation obtains GO/Mg-3Al-1Zn suspension under conditions of time 4h, after vacuum filter, dry 24h, is uniformly divided
Scattered GO/Mg-3Al-1Zn mixed-powders.In the protection of 99.999% high-purity argon gas, atmosphere pressures 5MPa, the μ of spot diameter 100
M, under laser power 80W, sweep speed 200mm/min process conditions, GO/Mg-3Al-1Zn alloys are prepared using SLM techniques.
Test finds that GO can wrap up Mg-3Al-1Zn alloy grains and form nano-honeycomb the second phase of structure, GO/Mg-
The degradation rate of 3Al-1Zn alloys is 0.24mm/year, ultimate tensile strength 302MPa.
Embodiment 3
It is raw material to use GO powder (thickness 0.8-1.2nm, piece footpath 8-15 microns) and Mg-3Al-1Zn alloy powders, is pressed
1.2:98.8 mass ratio weighs 0.12g GO powder and 9.88gMg-3Al-1Zn alloy powders, is respectively placed in two 1L beakers
In, 250ml absolute ethyl alcohols are slowly added to, ultrasonic agitation obtains GO suspension under conditions of rotating speed 250rad/min, time 4h
With Mg-3Al-1Zn suspension, GO suspension is slowly added in Mg-3Al-1Zn suspension, continue rotating speed 250rad/min,
Ultrasonic agitation obtains GO/Mg-3Al-1Zn suspension under conditions of time 4h, after vacuum filter, dry 24h, is uniformly divided
Scattered GO/Mg-3Al-1Zn mixed-powders.In the protection of 99.999% high-purity argon gas, atmosphere pressures 5.1MPa, spot diameter 120
μm, under laser power 80W, sweep speed 250mm/min process conditions, utilize SLM techniques to prepare GO/Mg-3Al-1Zn and close
Gold.
Test finds that GO can wrap up Mg-3Al-1Zn alloy grains and form nano-honeycomb the second phase of structure；GO/Mg-
The degradation rate of 3Al-1Zn alloys is 0.2mm/year, ultimate tensile strength 307MPa.
In the technology of the present invention development process, following scheme (such as comparative example 1, comparative example 2, comparative example 3) is have also been attempted, but
The performance of products obtained therefrom is much worse than embodiment.
Comparative example 1
Other conditions are consistent with embodiment 1, and difference is, by 0.5:99.5 mass ratio weighs 0.05g GO powder
GO/Mg-3Al-1Zn alloys are arrived in end and 9.95g Mg-3Al-1Zn alloy powders, preparation, detect the performance hair of its products obtained therefrom
Existing, GO is distributed on Mg-3Al-1Zn alloy grains border in disperse phase；The degradation rate of GO/Mg-3Al-1Zn alloys is
1.5mm/year, ultimate tensile strength 292MPa.
Comparative example 2
Other conditions are consistent with embodiment 1, and difference is, ultrasonic agitation rotating speed is 100rad/min, the time is
2h, the performance for detecting its products obtained therefrom find that GO fails to be evenly distributed on Mg-3Al-1Zn alloy grains border, GO/Mg-
The degradation rate of 3Al-1Zn alloys is 2.4mm/year, ultimate tensile strength 264MPa.
Comparative example 3
Other conditions are consistent with embodiment 1, and difference is, SLM controls laser power as 100W, scanning when sintering
Speed is 60mm/min, detects the performance of its products obtained therefrom, it is found that GO generates part-structure destruction, and alloy grain border
On generate carbide, the degradation rate of GO/Mg-3Al-1Zn alloys is 2.8mm/year, ultimate tensile strength 270MPa.
Claims (10)
- A kind of 1. Biological magnesium alloy with corrosion-resistant function, it is characterised in that：The Biological magnesium alloy is by Biological magnesium alloy matrix Formed with the graphene oxide being uniformly distributed on Biological magnesium alloy matrix crystal boundary；The graphene oxide wrapping biological magnesium alloy Crystal grain forms nano-honeycomb the second phase of structure；Wherein, the weight/mass percentage composition of graphene oxide is 0.8-1.2%.
- 2. the Biological magnesium alloy according to claim 1 with corrosion-resistant function, it is characterised in that：The matter of graphene oxide Amount percentage composition is 0.8-1.0%.
- 3. the Biological magnesium alloy according to claim 2 with corrosion-resistant function, it is characterised in that：The matter of graphene oxide It is 1.0% to measure percentage composition.
- 4. a kind of method for preparing the Biological magnesium alloy with corrosion-resistant function described in claim any one of 1-3, its feature It is：Comprise the following steps：(1) design proportion is pressed, GO powder and Biological magnesium alloy powder are respectively placed in into ultrasonic agitation in absolute ethyl alcohol obtains GO suspension With Biological magnesium alloy suspension；(2) GO suspension is slowly added in Biological magnesium alloy suspension, continues ultrasonic agitation and obtain mixing suspension, mixing is outstanding Supernatant liquid obtains dispersed mixed-powder after vacuum filter, drying process；(3) by mixed-powder obtained above under protective atmosphere, it is prepared by selective laser fusing with corrosion-resistant work( The Biological magnesium alloy of energy；In preparation process, to control laser power be 70-90W, sweep speed 100-300mm/min, hot spot are straight Footpath is 50-150 μm, the pressure of protective gas is 4-5.5MPa.
- 5. the method according to claim 4 for preparing the Biological magnesium alloy with corrosion-resistant function, it is characterised in that：Laser power is 78-85W；Sweep speed is 150-250mm/min；Spot diameter is 80-120 μm；The pressure 4.8-5.2MPa of protective gas.
- 6. the method according to claim 5 for preparing the Biological magnesium alloy with corrosion-resistant function, it is characterised in that：Laser power is 80W；Sweep speed is 200mm/min；Spot diameter is 100 μm；The pressure 5MPa of protective gas.
- 7. the method for Biological magnesium alloy of the preparation with corrosion-resistant function according to claim any one of 4-6, its feature It is：Described Biological magnesium alloy powder is Mg-3Al-1Zn alloyed powders.
- 8. the method for Biological magnesium alloy of the preparation with corrosion-resistant function according to claim any one of 4-6, its feature It is：Described protective atmosphere is the high-purity argon gas atmosphere that purity is more than or equal to 99.999%.
- 9. the method for Biological magnesium alloy of the preparation with corrosion-resistant function according to claim any one of 4-6, its feature It is：The thickness of GO powder is 0.8-1.2nm, piece footpath size is 8-15 microns.
- 10. the method for Biological magnesium alloy of the preparation with corrosion-resistant function according to claim any one of 4-6, its feature It is：In step (2) drying time be 12-24h, drying temperature be 80-90 DEG C；Ultrasonic agitation turns in step (1) and step (2) Speed is 150-300rad/min, time 3-5h.
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Cited By (4)
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| CN108950334A (en) * | 2018-08-10 | 2018-12-07 | 中南大学 | A kind of magnesium alloy and preparation method thereof with continuous eutectic structure |
| CN109014184A (en) * | 2018-08-10 | 2018-12-18 | 中南大学 | A kind of biological medical magnesium alloy and preparation method thereof with dual corrosion drag |
| CN111020327A (en) * | 2019-11-25 | 2020-04-17 | 温州广立生物医药科技有限公司 | Tissue-regenerating absorbable magnesium alloy and preparation method thereof |
| CN113454256A (en) * | 2018-12-18 | 2021-09-28 | Lkr轻金属能力中心兰斯霍芬有限责任公司 | Method for improving the corrosion resistance of a part formed with a magnesium-based alloy against galvanic corrosion and corrosion-resistant part obtainable by this method |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190430 Termination date: 20191026 |