CN104846371B - A kind of method for preparing molecular sieve coating in medical magnesium alloy surface - Google Patents
A kind of method for preparing molecular sieve coating in medical magnesium alloy surface Download PDFInfo
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Abstract
A kind of method for preparing molecular sieve coating in medical magnesium alloy surface, belong to the preparing technical field of biological and medicinal implant material Mg alloy surface molecular sieve coating, more particularly to a kind of method for preparing the molecular sieve coating with ion-exchange capacity and resistance to corrosion in medical magnesium alloy surface using in situ synthesis, so that magnesium alloy has good biocompatibility, corrosion resistance and ion exchangeable, application of such composite in biomedicine etc. is realized.First passage in situ synthesis of the present invention prepares the corrosion resistance molecular sieve coating with ion-exchange capacity in Mg alloy surface, it has preparation condition gentle, uniform coating can be prepared in the magnesium alloy substrate surface of complexity, and molecular sieve coating has good resistance to corrosion, the advantage of the corrosion rate of magnesium alloy can effectively be slowed down, it is possible to increase application of the composite in biomedicine etc..
Description
Technical field
The invention belongs to the preparing technical field of biological and medicinal implant material Mg alloy surface molecular sieve coating, and in particular to
It is a kind of that the molecular sieve painting with ion-exchange capacity and resistance to corrosion is prepared in medical magnesium alloy surface using in situ synthesis
The method of layer, so that magnesium alloy has good biocompatibility, corrosion resistance and ion exchangeable, realizes such composite wood
Expect the application in biomedicine etc..
Background technology
Compared with traditional medical metal implanted material titanium alloy, stainless steel etc., magnesium alloy has unrivaled advantage：
The modulus of elasticity of magnesium alloy is about 41~45GPa, very close with the modulus of elasticity (3~20GPa) of people's bone, can effectively be reduced
Or " stress shielding " effect existing for other metal implant materials is avoided, improve the combination between implantation material and skeleton
Power；Magnesium is the main component for forming bone, important adjustment effect is played in the mineral metabolism of bone, and can promote cell, tooth
And the formation of bone.Medical research shows：The content of magnesium is about 20~30g in adult body, and almost all of metabolic processes are all
There is the participation of magnesium.Cytotoxicity shows that magnesium alloy has good biocompatibility.It is a complexity yet with human body environment
Physiological Medium, corrosion phenomenon easily occurs in this context for magnesium alloy, especially in the corrosive medium of chloride ion-containing, corrosion plus
Play, a large amount of magnesium ions of precipitation have had a strong impact on the growth of surrounding tissue.In addition, the hydrogen that magnesium generates in corrosion process is to machine
Body tissue produces harmful effect, and therefore, it is necessary approach that the method being modified using surface, which slows down its corrosion,.
It is common improve corrosion resistance of magnesium alloy surface treatment method have chemical conversion, anodic oxidation, collosol and gel, etc. from
Son spraying etc., surface coating type includes：Bioactivity glass, hydroxyapatite, metal oxide, high molecular polymer etc..
Chinese patent (CN103495202) is prepared using sol-gal process in Mg alloy surface has good biological activity and degradability
Mesoporous bioglass coating, realize the degraded of controllable adjustment magnesium alloy.Chinese patent (CN104189963) will by spin-coating method
Polymer-coated, to suppress the too fast degraded of substrate, improves the biocompatibility of composite in Mg alloy surface.Chinese patent
(CN102220551) Ca-P biological coatings are prepared in Mg alloy surface using plasma spraying method, the coating can effectively be alleviated
The degradation speed of magnesium alloy, improve its corrosion resistance in physiological environment.Although these achievements in research are medical magnesium alloy
It is surface-treated and has established certain basis, but the diversity of the complexity and implantation piece shape due to human body environment, it is existing
Processing method can not prepare uniform coating in complex-shaped Mg alloy surface, therefore develop a kind of simple to operate, anti-corrosion effect
The good bioactivity coatings of fruit are extremely urgent.
Molecular sieve is a kind of inorganic crystal material with regular, homogeneous pore passage structure, not only with good biofacies
Capacitive and film forming, and there is excellent anticorrosion and antibacterial ability, its unique pore structure can be loaded with specific
Functional ionic, so as to assign composite more excellent performance.Chinese patent (CN 101791433) is by hydro-thermal method in titanium
Alloy substrates surface is prepared for the aluminosilicate molecular sieves coating with antibacterial ability, presents good biologic applications prospect.
Scape dawn swallow et al. (Corrosion Science, 2011,53,1732~1737) is assembled using cladding process in Mg-Li alloy surfaces
NaY/ epoxy resin composite membrane layers, the uniform membrane structure that such material is formed effectively have obstructed invading for erosion carbon dioxide
Enter, protective action is served to alloy.But still prepare molecular sieve in Mg alloy surface not in situ synthesis at present and apply
The report of layer.
The content of the invention
It is the invention provides a kind of method for preparing anticorrosive property molecular sieve coating in Mg alloy surface, i.e., raw by original position
Regular way prepares the molecular sieve coating with ion-exchange capacity, corrosion resistance in Mg alloy surface.Pass through skill of the present invention
Art scheme, uniform coating can be prepared in the magnesium alloy substrate surface of complexity.Because molecular sieve has good corrosion resistance
And film forming, by the way that resistance to corrosion of the magnesium alloy in simulated body fluid can be significantly improved after growing molecular sieve, meet
The demand of Medical implant etc..
A kind of method for preparing molecular sieve coating in medical magnesium alloy surface of the present invention, its step are as follows：
(1) surface preparation of medical magnesium alloy：Under alcoholic environment, medical magnesium alloy surface is polished, is subsequently placed in
It is cleaned by ultrasonic 10~30min in ethanol；
(2) preparation of medical magnesium alloy surface transition zone：The magnesium alloy of surface preparation is impregnated into 0 in transition zone solution
~20s, drying at room temperature after taking-up；
(3) preparation of medical magnesium alloy surface molecular sieve coating：Magnesium alloy with surface depletion layer is impregnated into molecule
Sieve in Synthesis liquid, 5~30h of in-situ crystallization under the conditions of 70~110 DEG C；Then magnesium alloy is taken out, respectively with deionized water, second
Alcohol is cleaned by ultrasonic the residue on surface, drying at room temperature, so as to which molecular sieve coating be prepared in medical magnesium alloy surface.
The instrument used when being polished in above-mentioned steps is polishing cloth, one kind in sand paper (1000~3000 mesh)；
Transition zone solution is the ethanol solution of the aminopropyl triethoxysilane of volume fraction 10~30%；Or it is quality point
The aqueous solution of the chitosan of number 1~3%, wherein adding the acetic acid that mass fraction is 1~2%；Or it is mass fraction 10~20%
Aq. polyethyleneimine；
The element of the magnesium alloy used is formed as Mg-Gd-Nd-Zn-Zr (its preparation method referenced patents
CN104328319A, the percentage by weight of composition are：Gd 2~7%, Nd 0~2%, Zn 0.1~1%, Zr0.1~0.5%,
Surplus is Mg.In experiment, magnesium alloy is processed into a diameter of 8~15mm, thickness is 1~3mm disk；
Molecular sieve is prepared under lower temperature conditions and had in NaA, NaX of ion-exchange capacity, NaY molecular sieve
It is a kind of.The active ingredient mol ratio of NaA Synthesis liquids is Na2O:SiO2:Al2O3:H2O=43:4.4:1:840；NaX Synthesis liquids have
Effect component molar ratio is Na2O:SiO2:Al2O3:H2O=3~7:2~10:1:130~200；The active ingredient of NaY Synthesis liquids is rubbed
Your ratio is Na2O:SiO2:Al2O3:H2O=14:10:1:750~900.
As the optimization experiment scope of the present invention, crystallization time described in step (3) is 20~24h, crystallization temperature 80
~90 DEG C.
First passage in situ synthesis of the present invention prepares the corrosion resistance point with ion-exchange capacity in Mg alloy surface
Son sieve coating, it has following advantage：
Molecular sieve coating preparation condition is gentle, can prepare uniform coating in the magnesium alloy substrate surface of complexity, and divide
Son sieve coating has good resistance to corrosion, can effectively slow down the corrosion rate of magnesium alloy, improves composite in biology
The application of medical science etc..
Brief description of the drawings
Fig. 1：For the SEM pictures of the magnesium alloy of the embodiment of the present invention 1.
Fig. 2：The SEM pictures of magnesium alloy after being polished for the sand paper of the embodiment of the present invention 1.
Fig. 3：The XRD piece of magnesium alloy after being polished for the sand paper of the embodiment of the present invention 1.
Fig. 4：The SEM pictures of NaA type molecular sieve coatings are grown for the Mg alloy surface of the embodiment of the present invention 1.
Fig. 5：The XRD piece of NaA type molecular sieve coatings is grown for the Mg alloy surface of the embodiment of the present invention 1.
Fig. 6：For the magnesium alloy of the embodiment of the present invention 1, in simulated body fluid, (active ingredient is mol ratio：(Na+：K+：Ca2+：Mg2+：
Cl-：HCO3-：HPO4 2-：SO4 2-=142.0：5.0：2.5：1.5：147.8：4.2：1.0：0.5) (pH=7.4)) in dipping it is 12 small
When after SEM pictures.
Fig. 7：For the Mg alloy surface of the embodiment of the present invention 1 grow NaA type molecular sieve coatings after in simulated body fluid (active ingredient
For mol ratio：(Na+：K+：Ca2+：Mg2+：Cl-：HCO3-：HPO4 2-：SO4 2-=142.0：5.0：2.5：1.5：147.8：4.2：
1.0：0.5) (pH=7.4)) in dipping 12 hours after SEM pictures.
It is the result obtained in embodiment 1 corresponding to each figure above, the characterizing method of other each embodiments and experiment are tied
Fruit is same as Example 1 or identical, and Mg alloy surface can grow uniform molecular sieve coating.
As shown in Fig. 1,2,4, after sand paper is polished, rough surface is presented in magnesium alloy.Handled through in situ synthesis
Afterwards, the molecular sieve crystal covering that Mg alloy surface is uniformly interlocked completely, forms continuous, fine and close film, and have necessarily
Roughness.
As shown in Fig. 3,5, after in situ synthesis processing, composite is in addition to the diffraction maximum intrinsic with magnesium alloy, separately
A set of typical NaA molecular sieve diffraction maximum be present, the molecular sieve type for showing Mg alloy surface growth is NaA molecular sieve.
As shown in Figure 6,7, larger crack is presented in magnesium alloy after being impregnated in simulated body fluid 12 hours, and growing has NaA
The Mg alloy surface of molecular sieve does not have significant change, is still the surface that bulk crystals are staggeredly accumulated, shows through in situ synthesis
Magnesium alloy after processing has preferable resistance to corrosion.
Embodiment
Below by embodiment, the present invention will be further described, but the implementation of the present invention is not limited to this, it is impossible to
It is interpreted as limiting the scope of the invention.
Embodiment 1
A small amount of ethanol is sprayed in the coated abrasive surface of 1000 mesh, then by a diameter of 10mm, thickness is 1mm medical magnesium alloy
Disk is put into ethanol and polished, and after the oxide for removing surface, is placed in ethanol and is cleaned by ultrasonic 30min.Magnesium alloy Ingredient Wt
Percentage is：Gd 3%, Nd 1%, Zn 0.5%, Zr 0.3%, Mg 95.2%.
By NaAlO2、Na2SiO3·9H2O, NaOH and water are according to mol ratio Na2O:SiO2:Al2O3:H2O=43:4.4:1:
840 ratio, stirs at ambient temperature, obtains NaA molecular sieve Synthesis liquid；Magnesium alloy is disposed vertically and is in volume
In 15mL reactor, 9mL Zeolite synthesis liquid is then added, reacts 18h in 85 DEG C of baking oven.Magnesium alloy is taken out, point
The residue on surface is not cleaned with deionized water, EtOH Sonicate, the magnesium that growth is obtained after drying at room temperature NaA molecular sieve coating closes
Metal/composite material, coating layer thickness are about 8 μm.
Embodiment 2
A small amount of ethanol is sprayed in the coated abrasive surface of 3000 mesh, then by a diameter of 8mm, the medical magnesium that thickness is 1.5mm closes
Golden disk, which is put into ethanol, polishes, and after the oxide for removing surface, is placed in ethanol and is cleaned by ultrasonic 30min.Magnesium alloy composition weight
Measuring percentage is：Gd 2%, Nd 2%, Zn 0.1%, Zr 0.5%, Mg 95.4%.
0.1g acetic acid is added drop-wise in 4.8g water, then adds 0.1g chitosans thereto, ultrasound degassing after stirring and dissolving.Will
Magnesium alloy takes out after impregnating 5s in the solution, and is uprightly positioned on filter paper and removes redundant solution, and drying at room temperature is standby.
By NaAlO2、Na2SiO3·9H2O, NaOH and water are according to mol ratio Na2O:SiO2:Al2O3:H2O=43:4.4:1:
840 ratio, stirs at ambient temperature, obtains NaA molecular sieve Synthesis liquid；By the magnesium alloy of pretreatment be disposed vertically in
Volume is the Zeolite synthesis liquid that 9mL is then added in 15mL reactor, reacts 6h in 110 DEG C of baking oven.Magnesium alloy is taken
Go out, clean the residue on surface with deionized water, EtOH Sonicate respectively, growth is obtained after drying at room temperature NaA molecular sieve coating
Composite material of magnesium alloy, the thickness of coating is about 4 μm.
Growth prepared by this example is had into the composite material of magnesium alloy of NaA molecular sieve coating, and in simulated body fluid, (active ingredient is
Mol ratio：(Na+：K+：Ca2+：Mg2+：Cl-：HCO3-：HPO4 2-：SO4 2-=142.0：5.0：2.5：1.5：147.8：4.2：1.0：
0.5) (pH=7.4)) in dipping after 12 hours, test result indicates that, Mg alloy surface does not have significant change, is still block brilliant
The surface that body is staggeredly accumulated, it is similar to the result of embodiment 1, it is preferably anti-to show that the magnesium alloy after in situ synthesis is handled has
Corrosive power.
Embodiment 3
A small amount of ethanol is sprayed on the polishing cloth surface of 2000 mesh, then by a diameter of 15mm, the medical magnesium that thickness is 1mm closes
Golden disk, which is put into ethanol, polishes, and after the oxide for removing surface, is placed in ethanol and is cleaned by ultrasonic 30min.Magnesium alloy composition weight
Measuring percentage is：Gd 5%, Nd 2%, Zn 0.1%, Zr 0.1%, Mg 92.8%.
The ethanol solution for the aminopropyl triethoxysilane that volume fraction is 10% is configured, magnesium alloy is soaked in the solution
Taken out after stain 10s, and be uprightly positioned on filter paper and remove redundant solution, drying at room temperature is standby.
By NaAlO2、Na2SiO3·9H2O, NaOH and water are according to mol ratio Na2O:SiO2:Al2O3:H2O=43:4.4:1:
840 ratio, stirs at ambient temperature, obtains NaA molecular sieve Synthesis liquid；By the magnesium alloy of pretreatment be disposed vertically in
Volume is the Zeolite synthesis liquid that 9mL is then added in 15mL reactor, reacts 24h in 70 DEG C of baking oven.Magnesium alloy is taken
Go out, clean the residue on surface with deionized water, EtOH Sonicate respectively, growth is obtained after drying at room temperature NaA molecular sieve coating
Composite material of magnesium alloy, the thickness of coating is about 6 μm.
Growth prepared by this example is had into the composite material of magnesium alloy of NaA molecular sieve coating, and in simulated body fluid, (active ingredient is
Mol ratio：(Na+：K+：Ca2+：Mg2+：Cl-：HCO3-：HPO4 2-：SO4 2-=142.0：5.0：2.5：1.5：147.8：4.2：1.0：
0.5) (pH=7.4)) in dipping after 12 hours, test result indicates that, Mg alloy surface does not have significant change, is still block brilliant
The surface that body is staggeredly accumulated, it is similar to the result of embodiment 1, it is preferably anti-to show that the magnesium alloy after in situ synthesis is handled has
Corrosive power.
Embodiment 4
A small amount of ethanol is sprayed in the coated abrasive surface of 2000 mesh, then by a diameter of 10mm, thickness is 1mm medical magnesium alloy
Disk is put into ethanol and polished, and after the oxide for removing surface, is placed in ethanol and is cleaned by ultrasonic 30min.Magnesium alloy Ingredient Wt
Percentage is：Gd 3%, Nd 1%, Zn 0.5%, Zr 0.3%, Mg 95.2%.
By Al2(SO4)3·18H2O, Ludox, NaOH and deionized water are according to mol ratio Na2O：SiO2：Al2O3：H2O=
14：10：1：800 ratio, stirs at ambient temperature, obtains NaY molecular sieve Synthesis liquid；The magnesium alloy of pretreatment is hung down
It is straight to be positioned in the reactor that volume is 15mL, 9mL Zeolite synthesis liquid is then added, reacts 24h in 90 DEG C of baking oven.Will
Magnesium alloy takes out, and cleans the residue on surface with deionized water, EtOH Sonicate respectively, and growth is obtained after drying at room temperature NaY points
The composite material of magnesium alloy of son sieve coating, the thickness of coating is about 8 μm.
Growth prepared by this example is had into the composite material of magnesium alloy of NaY molecular sieve coating, and in simulated body fluid, (active ingredient is
Mol ratio：(Na+：K+：Ca2+：Mg2+：Cl-：HCO3-：HPO4 2-：SO4 2-=142.0：5.0：2.5：1.5：147.8：4.2：1.0：
0.5) (pH=7.4)) in dipping after 12 hours, test result indicates that, Mg alloy surface does not have significant change, is still block brilliant
The surface that body is staggeredly accumulated, it is similar to the result of embodiment 1, it is preferably anti-to show that the magnesium alloy after in situ synthesis is handled has
Corrosive power.
Claims (5)
1. a kind of method for preparing molecular sieve coating in medical magnesium alloy surface, its step are as follows：
(1) surface preparation of medical magnesium alloy：Under alcoholic environment, medical magnesium alloy surface is polished, is subsequently placed in ethanol
10~30min of middle ultrasonic cleaning；The element composition of medical magnesium alloy is Mg-Gd-Nd-Zn-Zr, and the percentage by weight of each composition is
Gd 2~7%, Nd 0~2%, Zn 0.1~1%, Zr 0.1~0.5%, surplus Mg；
(2) preparation of medical magnesium alloy surface transition zone：The magnesium alloy of surface preparation is impregnated into 0 in transition zone solution~
20s, drying at room temperature after taking-up；
Transition zone solution, it is the ethanol solution of the aminopropyl triethoxysilane of volume fraction 10~30%；Or it is mass fraction 1
The aqueous solution of~3% chitosan, wherein adding the acetic acid that mass fraction is 1~2%；Or it is the poly- of mass fraction 10~20%
The aziridine aqueous solution；
(3) preparation of medical magnesium alloy surface molecular sieve coating：Magnesium alloy with surface depletion layer is impregnated into molecular sieve to close
Into in liquid, 5~30h of in-situ crystallization under the conditions of 70~110 DEG C；Then magnesium alloy is taken out, respectively with deionized water and ethanol
It is cleaned by ultrasonic the residue of Mg alloy surface, drying at room temperature, so as to which molecular sieve coating be prepared in medical magnesium alloy surface.
A kind of 2. method for preparing molecular sieve coating in medical magnesium alloy surface as claimed in claim 1, it is characterised in that：Step
One kind in polishing cloth or sand paper is used when being polished suddenly in (1).
A kind of 3. method for preparing molecular sieve coating in medical magnesium alloy surface as claimed in claim 1, it is characterised in that：Step
Suddenly molecular sieve described in (3) is NaA, NaX or NaY molecular sieve that be being prepared under lower temperature conditions and having ion-exchange capacity
In one kind.
A kind of 4. method for preparing molecular sieve coating in medical magnesium alloy surface as claimed in claim 3, it is characterised in that：
The active ingredient mol ratio of NaA Synthesis liquids is Na2O:SiO2:Al2O3:H2O=43:4.4:1:840；NaX Synthesis liquids it is effective into
It is Na to divide mol ratio2O:SiO2:Al2O3:H2O=3~7:2~10:1:130~200；The active ingredient mol ratio of NaY Synthesis liquids
For Na2O:SiO2:Al2O3:H2O=14:10:1:750~900.
A kind of 5. method for preparing molecular sieve coating in medical magnesium alloy surface as claimed in claim 1, it is characterised in that：Step
Suddenly crystallization time described in (3) is 20~24h, and crystallization temperature is 80~90 DEG C.
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| CN109847092B (en) * | 2018-06-18 | 2020-03-31 | 浙江大学 | Hemostatic compound and preparation method thereof |
| CN108823439A (en) * | 2018-07-19 | 2018-11-16 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of high-strength biology zinc magnesium alloy composite material |
| CN111893375B (en) * | 2020-06-16 | 2021-09-28 | 宁波市华涛不锈钢管材有限公司 | Thin-wall stainless steel for three-way pipe fitting and preparation method thereof |
| CN112206349B (en) * | 2020-10-19 | 2021-08-20 | 吉林大学 | ZIF-8@ antibacterial ion coating prepared on surface of medical metal implant material and preparation method thereof |
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