CN104083802B - Improve the method for medical magnesium alloy surface medical bio anchoring strength of coating - Google Patents
Improve the method for medical magnesium alloy surface medical bio anchoring strength of coating Download PDFInfo
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Abstract
A kind of method improving medical magnesium alloy surface medical bio anchoring strength of coating, it is characterized in that first carrying out acid treatment to the magnesium alloy member surface of polishing, the heat effect of optical fiber laser is used to carry out surperficial micro-texture processing to magnesium alloy member subsequently, obtain micro groove array, the stress effect of ultra high energy density pulse laser is used to carry out laser-impact to Mg alloy surface micro groove array pitch place, formed evenly, fine and close also in contraction-like micro structure, the magnesium alloy member finally surface with contraction-like micro groove array is placed in simulated body fluid SBF and soaks, biomimetic growth obtains having hydroxyapatite (HA) biological coating compared with high bond strength.The present invention can promote the biological activity of Mg alloy surface, special contraction-like surface micro-structure makes hydroxyapatite coating layer have mechanical sealed property, thus the adhesion after strengthening implantation between magnesium alloy and bone, overcome medical magnesium alloy implant short for service life, the caducous problem of hydroxyapatite coating layer.
Description
Technical field
The present invention relates to a kind of medical bio technology, especially a kind of technology Laser Processing being used for the surface modification of biomaterial for medical purpose, specifically improved a method for medical magnesium alloy surface medical bio anchoring strength of coating by laser heating power combination process processing machinery closing component structure, which increase implant and hydroxyl apatite biological painting bond strength.
Technical background
Magnesium alloy has the features such as low-density, high strength, excellent processing characteristics, nontoxic and close with human bone elastic modelling quantity, the bio-compatible performance good with human body due to it, becomes the metallic hard tissue implanting material of a new generation.But, owing to there is chloride ion and protein in human body environment, metal material for a long time in fluid environment military service implant surfaces can be caused to corrode, even make that metal ion is free out enters when injected organism tissue, produce when injected organism tissue and go bad; In addition, implant surface biological activity is not good, is unfavorable for the growth of osseous tissue, and these all limit service life and the range of application of medical magnesium alloy.In order to improve the performance of medical magnesium alloy, usually process of surface treatment is utilized to form at Mg alloy surface hydroxyapatite (HA) coating that one deck biological activity is excellent, combination property is good, to improve decay resistance and the biological activity of material, improve the adhesion of osseous tissue and material, reduce the stripping of harmful ion in matrix material simultaneously, reduce the bio-toxicity of material.At present, the multiple method of modifying preparing hydroxyapatite coating layer on Biological magnesium alloy surface has been had, as plasma spraying method, electrochemical deposition method, pulse electrodeposition method, biomimetic method and laser cladding etc.
Document 1 " application number is the Chinese patent of 201110139787.6 " proposes a kind of method of plasma spraying of Ca-P bioactive coating on surface of magnesium alloy, plasma spraying is the coat preparing technology uniquely commercially obtaining large-scale application at present, but, there is coarse grains in its coating prepared, seriously decrystallized, poor with substrate combinating strength, stress is concentrated and is cracked and the problem such as coating degradation, these problems can reduce biocompatibility and the biological activity of coating, and cause coating easily peeling phenomenon to occur in life-time service process, affect implant service life.
Document 2 " application number is the Chinese patent of 201210373185.1 " discloses one and possesses bioactive implantation body preparation method.First select the titanium alloy implant prepared, then implant surface is carried out activation processing, surface spraying hydroxyapatite, finally the implantation body after spraying placed and be immersed in the mixed solution of bone morphogenetic protein and phosphate buffered saline(PBS) formation.The method comes with some shortcomings: what (1) hydroxyapatite coating layer adopted is spraying process, and the high temperature in process easily makes HA coating undergo phase transition and decomposition, produces impurity and amorphous HA in the coating, thus destroys the biological activity of HA coating; (2) easily cause the coating on coarse base surface uneven; (3) coating structure is not fine and close, after implant into body, effectively can not stop the infiltration of physiological tissue's liquid; (4) because interfacial stress remains in coating material, cause coating to crack and make coating loosen or peel off.
Therefore, efficient, that low cost, bond strength are high, even, the fine and close biological coating preparation method of development of new is urgent need to solve the problem in bio-medical industry, is also the study hotspot in domestic and international biological coating field.
Laser surface texturing is the conventional process of surface pretreatment in field of thermal spray in recent years, it utilizes laser to go out micro asperities or the pattern of various micron/submicron level in body surface moulding, and the excellent biological coating of preparation that develops into of this technique provides new thinking.By adjusting the pulse of laser beam, difform surface texture pattern can be realized: circle dimple-shaped, square dimple-shaped, strip indenture shape and latticed indenture shape etc.Compared with traditional heat treatment method, Laser Processing have processing heat affected area little, can accurately the width of control treatment layer and the degree of depth, be applicable to the advantages such as manufacture in enormous quantities.Therefore the present invention proposes to adopt optical fiber laser to prepare square micro groove array at material surface, micro-texture can increase the effective bond area between coating and matrix on the one hand, make coating material be absorbed in concavo-convex middle formation hook and connect state, the wellability of matrix can be improved on the other hand.Due to surface irregularity, coating can infiltrate matrix surface pit, play the effect of mechanical interlock, but micro-texture is open type after solidification, and be unfavorable for the mechanical snap of coating at pit and matrix surface, coating and substrate combinating strength are still undesirable.
Laser impact intensified is that a kind of laser blast wave that utilizes carries out the technology of modification to material surface.Light laser and matter interaction produce strong shock wave, it has high pressure (GPa-TPa magnitude), high energy (GW/ magnitude), ultrafast (tens nanoseconds) and Under High Strain rate four distinguishing features, shock wave pressure is far longer than the dynamic yield strength of material, thus make material produce surrender and plastic deformation, produce residual compressive stress in plastic deformation area simultaneously, improve the fatigue of material, abrasion and corrosion performance.Light laser shock wave is utilized to make material produce the feature of plastic deformation, laser-impact is carried out to micro groove spacing, be the micro-texture of shrinkage type by micro-for open type texture development, the sealed property of machinery of the micro-texture of shrinkage type can improve the direction of coating layer portion contractility, reduce the stress along matrix surface direction, thus the bond strength strengthened between coating and implant surfaces, weaken the tendency of biological coating cracking.
The present invention proposes the method that laser heating power combination process processing machinery closing component structure improves HA biological coating bond strength first, utilize the micro-texture of laser surface in conjunction with the heating power combination process of laser-impact, in medical magnesium alloy surface preparation evenly, fine and close also in contraction-like micro structure, magnesium alloy member surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, biomimetic growth obtains the hydroxyapatite coating layer can filling completely contraction-like surface groove micro structure, coating structure is even, fine and close, the mechanical self-latching of micro structure enhances the bond strength of implant and hydroxyl apatite biological painting simultaneously.
By consulting domestic and foreign literature, not finding to use laser heating power combination process processing machinery closing component structure to improve the method for HA biological coating bond strength, thus improving the bond strength of HA and magnesium alloy.
Summary of the invention
The bond strength that the present invention seeks to biological coating and the matrix produced for existing Mg alloy surface is not high, extremely caducous problem in use procedure, invent a kind of elder generation in medical magnesium alloy surface utilize laser secondary operations to be formed method that up-small and down-big snap close groove growth in next life coating realizes mechanical sealed increase bond strength, it effectively can improve hydroxyapatite coating layer and implant poor bonding strength, coating skewness, the problems such as manufacturing process is complicated, improve the wear resistance and corrosion resistance of magnesium alloy in addition, biocompatibility and biological activity, extend service life.
Technical scheme of the present invention is:
A kind of method improving medical magnesium alloy surface medical bio anchoring strength of coating, it is characterized in that utilizing laser heating power combination process even, fine and close also in contraction-like micro structure in medical magnesium alloy surface preparation, the magnesium alloy member subsequently surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, and biomimetic growth obtains hydroxyapatite (HA) biological coating that bond strength meets the demands.
Concrete steps of the present invention are:
Step one, carries out polishing, acidification to medical magnesium alloy matrix;
Step 2, adopts optical fiber laser to carry out the micro-texture of laser to the medical magnesium alloy matrix surface through polishing, acidification, obtains micro groove array on medical magnesium alloy part surface;
Step 3, uses the stress effect impact micro groove array pitch surface of laser, is formed even, fine and close also in contraction-like surface micro-structure;
Step 4, prepares simulated body fluid SBF, and medical magnesium alloy part surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, and biomimetic growth obtains the hydroxyapatite coating layer can filling completely contraction-like surface micro-structure.
Described acidification refers to that the medical magnesium alloy after by polishing puts into 8-12 %HF+4-6 %HNO
3take out sample after mixed solution 8-15s, then use anhydrous alcohol ultrasonic cleaning 4-6 min, natural drying.
During the micro-texture process of described surface laser, adopt pulse optical fiber to carry out the micro-texture of concave groove type, its design parameter is: optical maser wavelength
λ 1 =1064 nm, pulsewidth
τ 1 =100 ns, frequency
f 1 =20 kHz, laser power is 6-16 W, groove width 100 μm after processing, separation 120 μm, groove depth 140 μm.
During described laser-impact medical magnesium alloy surface micro groove array, adopt nanosecond pulse Nd:YAG solid state laser, its design parameter is: optical maser wavelength
λ 2 =1064 nm, pulsewidth
τ 2 =8 ns, frequency
f 2 =10 Hz, pulsed laser energy is 0.5 ~ 1 J, spot diameter is 200 μm, hot spot overlapping rate is 50%, because groove is contraction-like structure after laser-impact, groove upper surface groove width 50 μm, lower surface groove width 100 μm, groove depth 125 μm, contraction-like surface groove micro structure makes hydroxyapatite coating layer have mechanical sealed property.
Described simulated body fluid uses the preparation of Kokubo T formula, medical magnesium alloy part surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, HA coatings growth is full of the micro-texture of whole shrinkage type and at material surface with uniform coating, the mechanical self-latching of micro structure enhances the bond strength of medical magnesium alloy and hydroxyl apatite biological painting.
The invention has the beneficial effects as follows:
1. first the present invention utilizes laser thermal effect to prepare micro forming at material surface, has the advantages such as controllability is high, heat affected area is little, pollution-free.
2. present invention utilizes induced with laser super high impact wave pressure, material surface is made to produce plastic deformation, by stress reinforced and build up, useful residual compressive stress can be introduced at material surface, not only can eliminate the residual tension that laser thermal effect produces, and avoid the surface crack defect melting and cause due to tension in process of setting, force crack closure, improve fatigue life in addition, improve the wear-resisting erosion resistance of magnesium alloy.
3. invention introduces the heating power combination process of laser, the basis of the micro-texture of laser surface is carried out laser impact intensified, strengthening position is micro groove spacing place, micro groove due to laser thermal effect be the micro-texture of open type, through stiffened region and the zone of influence of laser-impact stress effect, the micro-texture of open type changes, and changes the micro-texture of shrinkage type into.The sealed property of machinery of the micro-texture of shrinkage type can improve the direction of coating layer portion contractility, reduces the stress along matrix surface direction, thus strengthens the bond strength between coating and implant surfaces, weakens the tendency of biological coating cracking.
4. adopt biomimetic method to carry out biomimetic growth hydroxyapatite to the magnesium alloy with the micro-texture of shrinkage type, micro-texture increases the contact area of implant and HA on the one hand, also improves bond strength.On the other hand, cell has selectivity in the configuration of surface of growth to material of material surface, the micro-texture of channel form is conducive to the growth of cell, the present invention is by the sample after biomimetic method immersion treatment, not only obtain uniform coating at material surface, and HA can be filled up in micro groove, the implant therefore after micro forming has better biological activity.
Accompanying drawing explanation
Fig. 1 is that laser thermal effect of the present invention prepares micro-texture schematic diagram.
Fig. 2 is that laser-impact material surface of the present invention produces mechanical sealed structural representation.
Fig. 3 is machinery of the present invention sealed structural material surface biomimetic growth HA schematic diagram.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, this method is further described.
As Figure 1-3.
A kind of method improving medical magnesium alloy surface medical bio anchoring strength of coating, first form micro groove array by matrix surface laser thermal effect, then laser-impact material surface is utilized to form contraction-like micro structure, finally biomimetic growth medical (HA) coating in simulated body fluid, contraction-like micro structure is utilized to make HA coating formation closing component structure, improve the bond strength of coating and matrix, coating performance and uniformity, as Fig. 1 ~ 3.Enforcement detailed process is as follows:
1) experiment material selects bio-medical AZ31B magnesium alloy.First use successively abrasive paper for metallograph 280#, 320#, 600#, 800#, 1200# to AZ31B magnesium alloy materials sanding and polishing, finally with dehydrated alcohol at room temperature ultrasonic cleaning 8 min, remove surface impurity, natural air drying after taking out.Magnesium alloy after polishing is put into 8-12 %HF+4-6 %HNO
3take out sample after mixed solution 8-15s, then use anhydrous alcohol ultrasonic cleaning 4-6 min, natural drying, obtains shaggy magnesium alloy sample.
2) adopt YLP-HP-100 type to mix ytterbium pulse optical fiber and the micro-texture of laser is carried out to material surface.Laser parameter is optical maser wavelength
λ 1 =1064 nm, pulsewidth
τ 1 =100 ns, frequency
f 1 =20 kHz, laser power is 10 W, nc program input required processing nick groove width 100 μm, separation 120 μm, groove depth 140 μm.Because the power density of laser is high, pulse width is extremely short, and after focusing on material surface, material is rapidly heated to vapourizing temperature, directly with gas evaporation, forms nick hole (the rightest figure of Fig. 1).In the course of processing, the cross-couplings such as optics, mechanics, calorifics is carried out power conversion and is made material surface generation physicochemical change, thus produces the micro-texture of open type.Rough surface adds effective contact area between coating and matrix, can improve the adhesive force of coating.
3) ultra high energy density (GW/cm is used
2magnitude) Pulse Nd: YAG solid state laser impact nick hole between material surface.Wherein, pulsed laser energy is 0.8J, and spot diameter is 200 μm, and spot separation is 100 μm (micro-pit diameter).Under the super high impact power effect of induced with laser, material surface produces plastic deformation, the micro-texture of above-mentioned open type is made to become the micro-texture of shrinkage type, groove upper surface groove width 50 μm, lower surface groove width 100 μm, groove depth 125 μm (Fig. 2 rightmost side figure), contraction-like surface groove micro structure makes hydroxyapatite coating layer have mechanical sealed property, be conducive to the mechanical snap of coating at pit and implant, fundamentally improve the bond strength of coating and implant.In addition, under the impact of strong shock wave, there is the change of slippage, distortion and spacing in implant crystal lattices simultaneously, dislocation density in crystal grain is caused to increase, make material surface refinement, material surface is in compressive stress state, is conducive to the combination of coating and implant surfaces.Due to laser impact intensified non-thermal characteristics, coating surface is compressive stress state, avoids the surface crack defect caused due to tension in Melting And Solidification process.Simultaneously, uneven owing to impacting rear surface, the direction of coating layer portion contractility can be upset, reduce the stress along matrix surface direction, thus make the bond strength between coating and matrix surface higher than the bond strength of smooth surface, reduce the tendency that coating produces cracking.
4) use Kokubo T formula to obtain simulated body fluid SBF, each ion concentration is respectively Na
+142.0, K
+5.0, Mg
2+1.5, Ga
2+2.5, Cl
-147.8, HCO
3 -4.2, HPO
4 2-1.0, SO
4 2-0.5 mmol/L, close with inorganic ions composition in blood of human body.Be flat on by test specimen in plastic containers, test specimen does not contact with container inner wall, and add 40-100 ml simulated body fluid, and flood test specimen completely, sealed membrane is closed, and 36.5 ± 1.5 DEG C of constant temperature preserve 10-15 days.With the sample of micro-texture after the immersion of simulated body fluid, can form more HA crystallization on its surface, coating is full of the micro-texture of whole shrinkage type and at material surface with uniform coating, shows the ability of induction HA deposition preferably, as shown in Figure 3.
According to the residual stress result that XRD diffractometer detects, after utilizing process coating of the present invention, the residual stress of coating is the residual compressive stress of-87 MPa, compared with the residual stress (about 1 GPa) of the coating prepared with sedimentation, significantly improves the mechanical property of coating.According to the test result of adhesive force detector, the coating utilizing the present invention to prepare and the adhesive force of matrix are 82.7 MPa, and compared with the adhesive force (20 ~ 40 MPa) of the coating prepared with sedimentation, adhesive force improves 2 times nearly.
Fig. 1 is that laser thermal effect prepares micro-texture schematic diagram.Because the power density of laser is high, pulse width is extremely short, and after focusing on material surface, material is rapidly heated to vapourizing temperature, directly with gas evaporation, forms nick hole.Fig. 2 is that laser-impact material surface produces mechanical sealed structural representation.Under the super high impact power effect of induced with laser, material surface produces plastic deformation, make the micro-texture of above-mentioned open type become the micro-texture of shrinkage type, be beneficial to the mechanical snap of coating at pit and matrix, depth direction makes depth of groove reduce owing to there is plastic deformation.Fig. 3 is mechanical sealed structural material surface biomimetic growth HA schematic diagram.Micro-texture implant, after simulated body fluid soaks, grows full HA, and goes out the even HA coating of one deck in superficial growth in micro-texture groove.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.
Claims (4)
1. one kind is improved the method for medical magnesium alloy surface medical bio anchoring strength of coating, it utilizes laser heating power combination process even, fine and close also in contraction-like micro structure in medical magnesium alloy surface preparation, the magnesium alloy member subsequently surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, and biomimetic growth obtains hydroxyapatite (HA) biological coating that bond strength meets the demands; It is characterized in that it comprises the following steps:
Step one, carries out polishing, acidification to medical magnesium alloy matrix;
Step 2, adopts optical fiber laser to carry out the micro-texture of laser to the medical magnesium alloy matrix surface through polishing, acidification, obtains micro groove array at medical magnesium alloy matrix surface;
Step 3, uses the stress effect impact micro groove array pitch surface of laser, is formed even, fine and close also in contraction-like surface micro-structure;
Step 4, prepares simulated body fluid SBF, and medical magnesium alloy part surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, and biomimetic growth obtains the hydroxyapatite coating layer can filling completely contraction-like surface micro-structure;
During described laser-impact medical magnesium alloy surface micro groove array, adopt nanosecond pulse Nd:YAG solid state laser, its design parameter is: optical maser wavelength
λ 2 =1064 nm, pulsewidth
τ 2 =8 ns, frequency
f 2 =10 Hz, pulsed laser energy is 0.5 ~ 1 J, spot diameter is 200 μm, hot spot overlapping rate is 50%, because groove is contraction-like structure after laser-impact, groove upper surface groove width 50 μm, lower surface groove width 100 μm, groove depth 125 μm, contraction-like surface groove micro structure makes hydroxyapatite coating layer have mechanical sealed property.
2. the method for raising medical magnesium alloy surface medical bio anchoring strength of coating according to claim 1, is characterized in that described acidification refers to that the medical magnesium alloy matrix after by polishing puts into 8-12 %HF+4-6 %HNO
3take out sample after mixed solution 8-15s, then use anhydrous alcohol ultrasonic cleaning 4-6 min, natural drying.
3. the method for raising medical magnesium alloy surface medical bio anchoring strength of coating according to claim 1, when it is characterized in that the micro-texture process of described surface laser, adopt pulse optical fiber to carry out the micro-texture of concave groove type, its design parameter is: optical maser wavelength
λ 1 =1064 nm, pulsewidth
τ 1 =100 ns, frequency
f 1 =20 kHz, laser power is 6-16 W, groove width 100 μm after processing, separation 120 μm, groove depth 140 μm.
4. the method for raising medical magnesium alloy surface medical bio anchoring strength of coating according to claim 1, it is characterized in that described simulated body fluid uses the preparation of Kokubo T formula, medical magnesium alloy part surface with contraction-like micro structure is placed in simulated body fluid SBF and soaks, HA coatings growth is full of the micro-texture of whole shrinkage type and at material surface with uniform coating, the mechanical self-latching of micro structure enhances the bond strength of medical magnesium alloy and hydroxyl apatite biological painting.
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| DE102015101626B4 (en) * | 2015-02-04 | 2019-06-27 | Kulzer Gmbh | Coating of dental prosthetic surfaces with a distinct layer of a synthetic hydroxyapatite |
| CN104707170B (en) * | 2015-04-02 | 2017-06-30 | 山东大学齐鲁医院 | Titanium surface prepares nano-grade hydroxy apatite layer load rapamycin drug method |
| CN104962970A (en) * | 2015-06-08 | 2015-10-07 | 太原理工大学 | Surface modification method of medical magnesium alloy |
| CN106119750A (en) * | 2016-06-22 | 2016-11-16 | 浙江工业大学 | Laser-impact and differential arc oxidation are combined in Mg alloy surface and prepare biological coating method |
| CN106392332B (en) * | 2016-10-11 | 2018-06-22 | 北京航空航天大学 | A kind of laser-graining method for improving medical implant surfaces cell adhesion |
| CN107009027A (en) * | 2017-05-27 | 2017-08-04 | 江苏大学 | The micro- texture of hair follicle type and its processing method of a kind of high bond strength |
| WO2019082160A1 (en) * | 2017-10-26 | 2019-05-02 | Universidade Do Minho | Dental implant with functional gradient and its production process |
| CN109045351B (en) * | 2018-06-26 | 2021-03-23 | 哈尔滨工业大学 | Magnesium alloy and silk fibroin connection method based on surface treatment |
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| CN110878414A (en) * | 2019-12-10 | 2020-03-13 | 江苏微纳激光应用技术研究院有限公司 | Method and structure for realizing laser coating of heterogeneous material |
| CN112144001B (en) * | 2020-10-19 | 2022-08-23 | 有研工程技术研究院有限公司 | Pretreatment method for enhancing bonding strength of VW75 magnesium alloy thermal barrier coating and substrate |
| CN114798394A (en) * | 2022-06-27 | 2022-07-29 | 吉林大学 | Method for improving binding force of polycaprolactone coating based on nanosecond laser processing |
| CN115429940B (en) * | 2022-08-30 | 2024-01-26 | 电子科技大学 | Method for enhancing stability of bioactive coating |
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| US8039038B2 (en) * | 2007-08-20 | 2011-10-18 | Council Of Scientific And Industrial Research | Process for the preparation of protein mediated calcium hydroxyapatite (HAp) coating on metal substrate |
| CN103060528A (en) * | 2013-01-14 | 2013-04-24 | 温州大学 | Laser compound strengthening technology |
| CN103146892B (en) * | 2013-03-07 | 2014-04-09 | 江苏大学 | Femtosecond laser surface pretreatment method for improving bonding state of layer base or film base |
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