CN108914100A - A kind of method of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 - Google Patents
A kind of method of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 Download PDFInfo
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- CN108914100A CN108914100A CN201810859905.2A CN201810859905A CN108914100A CN 108914100 A CN108914100 A CN 108914100A CN 201810859905 A CN201810859905 A CN 201810859905A CN 108914100 A CN108914100 A CN 108914100A
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
- C23C22/22—Orthophosphates containing alkaline earth metal cations
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Abstract
The present invention provides a kind of method of modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550.AZ60 magnesium alloy after polishing is rinsed, magnesium alloy is placed in pre-prepared calcium phosphorus conversion solution and is impregnated, corresponding single layer calcium phosphorus conversion film is obtained, is again put into magnesium alloy in the KH550 alcoholic solution hydrolyzed later by the method.After taking-up is dried, will be silane coupler modified after calcium phosphorus conversion film be immersed in the dichloromethane solution of polylactic acid, polylactic acid is covered on its surface by dip-coating method, obtains the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite coating of KH550.Gained composite film surface topography uniform ground.Compared with unmodified composite film, there is better organic/inorganic phase interface bonding strength and the higher corrosion resistance in human body fluid.Preparation method of the present invention is simple and novel, convenient and efficient, low in cost, acts on human body and environment nonhazardous, has broad application prospects in biological bone field of tissue engineering technology.
Description
Technical field
The invention belongs to bio-medical fields, are related to a kind of Metal surface anti-corrosion processing technique, and in particular to a kind of magnesium conjunction
Gold surface biodegradable coating antiseptic technology.
Background technique
Magnesium alloy is widely regarded as the material for having wide potential applicability in clinical practice in bone tissue engineer field.Due to it
Excellent biocompatibility, good biological degradability and with mechanical property as human body bone photo, be used as studying for a long time
Use bone implant material.However, very big limitation of the clinical application of magnesium alloy by its too fast degradation rate in human body fluid.
The fast degradation of magnesium alloy can damage its mechanical integrity before bone tissue heals completely, to influence its clinical application.
It is attempted there are many aseptic technic to solve the problems, such as this, at acid etching, alkali process, anodic oxidation, fluoride
Reason, calcium series phosphatating object coating, biological organic coating etc..Wherein, calcium series phosphatating object coating is to realize magnesium alloy in orthopaedics implant
The most potential method of middle application, because it is with excellent biocompatibility and osteoinduction.However, in calcium series phosphatating
Generally existing a large amount of hole defects in object coating.These holes become the channel that corrosive medium corrodes magnesium alloy, seriously undermine painting
The corrosion resistance of layer.In order to improve the corrosion resistance of calcium series phosphatating object coating, need to utilize the less new coating of another defect and its
In conjunction with carrying out sealing pores to it.
Polylactic acid is a kind of ideal sealing pores material due to its splendid biocompatibility and uniform structure.Make
For a kind of degradable polymer, it is widely used as the matrix of orthopaedics implant, angiocarpy bracket and pharmaceutical carrier.Research shows that poly-
Lactic acid has humidification to corrosion stability of the magnesium-based bone implant in body fluid.But the bonding between calcium series phosphatating object and polylactic acid is strong
It spends very poor, significantly inhibits polylactic acid/antiseptic property of the calcium series phosphatating object composite coating in long service.So far, it improves
Polylactic acid/calcium series phosphatating object composite coating interface bond strength the relevant technologies also lack very much.This makes polylactic acid and calcium system
The bond strength of phosphide becomes the serious resistance that polylactic acid/calcium series phosphatating object composite coating realizes clinical application on bone implant
Hinder.
Summary of the invention
It is compound using silane coupler modified polylactic acid/calcium series phosphatating object that the problem to be solved by the invention is to provide a kind of
Polylactic acid/calcium series phosphatating object composite film interface binding power and anti-corrosion can be improved in the processing technique of film layer, the processing technique
Property.
Technical proposal that the invention solves the above-mentioned problems is：It is a kind of to utilize silane coupler modified polylactic acid/calcium series phosphatating
The processing method of object composite film, it is characterised in that：It using AZ60 magnesium alloy as substrate, first polishes magnesium alloy, drops
Low surface roughness, then ultrasonic cleaning removes surface grease stain；A certain amount of calcium phosphorus conversion fluid is prepared, magnesium alloy is immersed it
In, single layer calcium series phosphatating film is obtained on surface；A certain proportion of KH550 coupling agent hydrating solution is prepared again, at the solution
Manage resulting calcium series phosphatating film；The dichloromethane solution for finally preparing a certain amount of polylactic acid, using dip-coating method in its table
Wheat flour obtains polylactic acid layers.
It is above-mentioned using silane coupler modified polylactic acid/calcium series phosphatating object composite film processing method, specifically include with
Lower step：
A, it pre-processes：AZ60 magnesium alloy stick is successively polished with the sand paper of 240-1000 mesh respectively.It will polish later
Magnesium alloy block be cleaned by ultrasonic oil removing in acetone, it is dry in case subsequent processing.
B, the preparation of calcium series phosphatating film：A certain amount of calcium nitrate and phosphoric acid are added in 1L distilled water, uniform stirring is to make
Standby calcium phosphorus conversion fluid.The pH value of prepared calcium phosphorus conversion fluid is adjusted to 2.7 again.Then by pretreated AZ60 magnesium alloy
It is dipped at 37 DEG C in prepared calcium phosphorus conversion solution, obtains single layer calcium series phosphatating film.Finally, with distilled water flushing and
Air drying.
C, KH550 modification：First it is made 1:The ethanol water of 9 (ethyl alcohol: water) ratios, then by a certain amount of KH550
Coupling agent is dissolved in ethanol solution, obtain the mixed solution of 6% volume fraction.After hydrolyzing a few houres, phosphorating treatment will be passed through
Magnesium alloy impregnated in the hydrolyzate prepared, be then sintered and spontaneously dry.
D, polylactic acid coats：Particles of polylactic acid is added in methylene chloride and is uniformly mixed, the mixed of 10% mass fraction is obtained
Close solution.Then KH550 treated magnesium alloy is immersed in prepared solution, and is pulled out with constant speed, finally in room
The lower drying of temperature.
Compared with the prior art, the present invention has the advantage that：
1. the present invention carries out Mg alloy surface polylactic acid/calcium series phosphatating object composite film by KH550 silane coupling agent
Its corrosion resistance in body fluid is substantially improved in modification.Electro-chemical test shows：Modified polylactic acid/calcium system phosphorus
Compound composite film corrosion potential is obviously improved, and corrosion current then accordingly declines.
2. the present invention carries out Mg alloy surface polylactic acid/calcium series phosphatating object composite film by KH550 silane coupling agent
Modification greatly improves its organic/inorganic interface binding power.Cross-hatching adhesive tape test shows：The binding force of composite film
1 grade is risen to from 4 grades, coating is close to without damaged state.
3. method of the invention is simple, convenient and efficient, to human body and environmentally friendly, cost is relatively low, is a kind of easy to spread
The novel artistic used.
Detailed description of the invention
Fig. 1 is to shine without the modified polylactic acid/calcium series phosphatating object composite membrane scanning electron microscope of Silane coupling agent KH550
Piece；
Fig. 2 is the polylactic acid/calcium series phosphatating object composite membrane stereoscan photograph modified by Silane coupling agent KH550；
Fig. 3 is embodiment 1 and the polylactic acid/calcium series phosphatating object composite membrane pole modified without Silane coupling agent KH550
Change curve comparison figure；
Fig. 4 is embodiment 1 and the polylactic acid/calcium series phosphatating object composite membrane resistance modified without Silane coupling agent KH550
Anti- comparison diagram；
Fig. 5 is that embodiment 1 is drawn with without the modified polylactic acid/calcium series phosphatating object composite membrane of Silane coupling agent KH550
Lattice experimental comparison figure.
Specific embodiment
The present invention is described in further details with Figure of description combined with specific embodiments below.The implementation case with
Implemented under premised on the technology of the present invention, it is of the invention to illustrate now to provide detailed embodiment and specific operating process
Creativeness, but protection scope of the present invention embodiment not limited to the following.
Embodiment 1
It is a kind of using KH550 polydactyl acid/calcium series phosphatating object composite film processing method, include the following steps：
A, it pre-processes：AZ60 magnesium alloy stick is successively beaten with the sand paper of 240 mesh, 600 mesh, 800 mesh and 1000 mesh respectively
Mill.The magnesium alloy block polished is cleaned by ultrasonic 10 minutes in 20ml acetone later, it is dry in case subsequent processing.
B, the preparation of calcium series phosphatating film：The phosphoric acid of the calcium nitrate of 23.6g and 34.2ml are added in 1L distilled water, uniformly stirred
It mixes to prepare calcium phosphorus conversion fluid.The pH value of prepared calcium phosphorus conversion fluid is adjusted to 2.7 with strong caustic again.Then
Pretreated AZ60 magnesium alloy is immersed in prepared calcium phosphorus conversion solution 20 minutes at 37 DEG C, obtains single layer calcium system phosphorus
Change film.Finally, drying with distilled water flushing and in air.
C, KH550 modification：45ml water and 5ml alcohol are mixed to prepare 1:The ethyl alcohol of 9 (ethyl alcohol: water) ratios is water-soluble
Liquid, then 3mlKH550 coupling agent is dissolved in ethanol solution, obtain the mixed solution of 6% volume fraction.After hydrolysis 6 hours,
2min will be impregnated in the hydrolyzate prepared by parkerized magnesium alloy, be then sintered at 100 DEG C 1 hour and natural
It is dry.
D, polylactic acid coats：5g particles of polylactic acid is added in 45g methylene chloride liquid and is uniformly mixed, 10% mass is obtained
The mixed solution of score.Then KH550 treated magnesium alloy is immersed in prepared solution, and with the constant of 240 μm/s
Speed pulls out, and is finally dried at room temperature for.
Fig. 1, Fig. 2 are the polylactic acid/calcium series phosphatating object composite membrane scanning electricity modified without Silane coupling agent KH550 respectively
Mirror photo and the polylactic acid/calcium series phosphatating object composite membrane stereoscan photograph modified through Silane coupling agent KH550.Compare this two
Kind composite coating is it can be found that the modified composite coating surface of Silane coupling agent KH550 is more uniform consistent, without larger
Volt, structure more compact, defect significantly reduce, and without obvious hole and crackle.
Polarization curve is carried out to unmodified polylactic acid/calcium series phosphatating object composite membrane and embodiment 1 with electrochemical workstation
And testing impedance, specific test use three-electrode system, use saturated calomel electrode for reference electrode, platinum black electrode is to electricity
Pole, sample are working electrode, and corrosive medium is simulated body fluid, and the work area of sample exposure is 1cm2, as a result such as Fig. 3, Fig. 4 institute
Show.The composite membrane after silane coupler modified has compared to unmodified higher corrosion resistance as can be seen from Figure 3,
Corrosion potential is obviously improved, and corrosion current is then in contrast, declines.Fig. 4 also shows that same trend, modified
Composite membrane has higher polarization resistance resistance value, illustrates that its corrosion resistance significantly improves.
A stroke lattice tape test has been carried out according to ASTM standard D3359-963, it is compound to compare polylactic acid/calcium series phosphatating object
Coating and silane coupler modified polylactic acid/calcium series phosphatating object composite coating interface binding power.Fig. 5 be embodiment 1 with without
It crosses the modified polylactic acid/calcium series phosphatating object composite membrane of Silane coupling agent KH550 and draws lattice experimental comparison figure.It is compound to compare two classes
Film, it can be found that modified composite film surface only has the polylactic acid membrane in only a few grid to fall off, and it is unmodified compound
The polylactic acid membrane of film surface nearly 2/3rds falls off.This illustrates that KH550 modified technique can greatly improve polylactic acid/calcium series phosphatating
The interface binding power of object composite coating alleviates polylactic acid/calcium series phosphatating object composite coating and interfacial separation occurs under soaking conditions
The case where.
Claims (6)
1. a kind of method of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550, it is characterised in that：Using
AZ60 magnesium alloy first polishes to magnesium alloy as substrate, reduces surface roughness, then ultrasonic cleaning removal surface oil
Stain；A certain amount of calcium phosphorus conversion fluid is prepared, magnesium alloy is immersed, obtains single layer calcium series phosphatating film on surface；One is prepared again
The KH550 coupling agent hydrating solution of certainty ratio handles resulting calcium series phosphatating film using the solution；It finally prepares a certain amount of poly-
The dichloromethane solution of lactic acid covers polylactic acid layers on its surface using dip-coating method.
2. a kind of side of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 according to claim 1
Method, which is characterized in that specifically include following steps：
A, it pre-processes：AZ60 magnesium alloy stick is successively polished with the sand paper of 240-1000 mesh respectively, the magnesium that will have been polished later
Alloy block is cleaned by ultrasonic oil removing in acetone, dry in case subsequent processing；
B, the preparation of calcium series phosphatating film：A certain amount of calcium nitrate and phosphoric acid are added in 1L distilled water, uniform stirring is to prepare calcium
Phosphorus conversion fluid, then the pH value of prepared calcium phosphorus conversion fluid is adjusted to 2.7, then by pretreated AZ60 magnesium alloy 37
It is dipped at DEG C in prepared calcium phosphorus conversion solution, obtains single layer calcium series phosphatating film；Finally, with distilled water flushing and in air
Middle drying；
C, KH550 modification：First it is made 1:The ethanol water of 9 (ethyl alcohol: water) ratios, then a certain amount of KH550 is coupled
Agent is dissolved in ethanol solution, obtains the mixed solution of 6% volume fraction, after hydrolyzing a few houres, will pass through parkerized magnesium
Alloy impregnates in the hydrolyzate prepared, is then sintered and spontaneously dries；
D, polylactic acid coats：Particles of polylactic acid is added in methylene chloride and is uniformly mixed, the mixing for obtaining 10% mass fraction is molten
Then KH550 treated magnesium alloy is immersed in prepared solution, and is pulled out with constant speed by liquid, finally at room temperature
It is dry.
3. a kind of side of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 according to claim 1
Method, it is characterised in that：Step A, the sand paper mesh number are followed successively by 240 mesh, 600 mesh, 800 mesh and 1000 mesh, when ultrasonic cleaning
Between be 10min.
4. a kind of side of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 according to claim 1
Method, it is characterised in that：Step B, the calcium nitrate quality are 23.6g, and phosphoric acid volume is 34.2ml, and magnesium alloy is converted in calcium phosphorus
Soaking time in liquid is 20min.
5. a kind of side of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 according to claim 1
Method, it is characterised in that：Step C, the volume of the ethyl alcohol are 5ml, and distilled water 45ml, KH550 silane coupling agent is 3ml,
Hydrolysis time is 6 hours, and magnesium alloy soaking time in hydrolyzate is 2min.
6. a kind of side of the modified Mg alloy surface polylactic acid/calcium series phosphatating object composite membrane of KH550 according to claim 1
Method, it is characterised in that：Step D, the polylactic acid quality are 5g, and methylene chloride quality is 45g, and constant pull-out speed is 240 μ
m/s。
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| CN113384751A (en) * | 2021-06-15 | 2021-09-14 | 重庆理工大学 | Magnesium alloy gradient composite coating and application thereof |
| CN115708896A (en) * | 2022-11-16 | 2023-02-24 | 南京友德邦医疗科技有限公司 | Degradable magnesium alloy composite material and preparation method thereof |
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| CN113384751A (en) * | 2021-06-15 | 2021-09-14 | 重庆理工大学 | Magnesium alloy gradient composite coating and application thereof |
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Application publication date: 20181130 |