CN109758605A - Mg alloy surface fine acicular hydroxyapatite micro nano structure coating and preparation method - Google Patents

Mg alloy surface fine acicular hydroxyapatite micro nano structure coating and preparation method Download PDF

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Publication number
CN109758605A
CN109758605A CN201910137298.3A CN201910137298A CN109758605A CN 109758605 A CN109758605 A CN 109758605A CN 201910137298 A CN201910137298 A CN 201910137298A CN 109758605 A CN109758605 A CN 109758605A
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coating
magnesium alloy
alloy
micro nano
fine acicular
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孙瑞雪
于文韬
陈克正
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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Abstract

The invention belongs to degradable magnesium alloy implant surface technical field of modification, and in particular to Mg alloy surface fine acicular hydroxyapatite micro nano structure coating and preparation method thereof.Preparation method is the following steps are included: pretreated magnesium alloy substrate is soaked in electrochemical deposition electrolyte solution, using platinum electrode as cathode, magnesium alloy is as anode, connect D.C. regulated power supply, carry out electrochemical deposition, alkali heat-treatment is carried out later, obtains Mg alloy surface hydroxyapatite coating layer.The electrochemical deposition electrolyte prescription that the present invention uses is simple, without adding any promotor or oxidant, and without adjusting electrolyte ph;Using the electrochemical deposition mode of low temperature, low current density, easily controllable, cost is relatively low;Prepared hydroxyapatite coating layer even compact, purity is higher, corrosion resistance and good, and the micro nano structure with fine acicular, is conducive to cell in the adherency and growth of coating surface, that improves magnesium alloy implant is implanted to power.

Description

Mg alloy surface fine acicular hydroxyapatite micro nano structure coating and preparation method
Technical field
The invention belongs to degradable magnesium alloy implant surface technical field of modification, and in particular to Mg alloy surface fine acicular Hydroxyapatite micro nano structure coating and preparation method.
Background technique
Magnesium alloy has good biocompatibility and bioactivity and excellent as a kind of biological and medicinal implant material Biodegradability.Compared with the metal materials such as the common cobalt-base alloys of clinical medicine, stainless steel, titanium alloy, magnesium alloy Elasticity modulus and density are all closest with people's bone, are a kind of ideal bone renovating materials.But since magnesium alloy is in physiologic ring Corrosion resistance under border is poor, and degradation rate is too fast, often will cause implant site local environment pH value is excessively high and hydrogen Short-term a large amount of releases so that implant site healing slow is even resulted in graft failure so as to cause inflammation generation;In addition, too fast Degradation speed keep its mechanical properties decrease during one's term of military service very fast, be not able to satisfy the time requirement of bone tissue healing.Therefore, right It is mesh that medical magnesium alloy, which carries out surface modification treatment to improve its corrosion resistance and biocompatibility in physiological environment, One of the important directions of preceding research.
Hydroxyapatite (Ca10(PO4)6(OH)2, Hydroxyapatite, HAp) be skeleton and tooth main nothing Machine component part has excellent bioactivity and biocompatibility, it is considered to be a kind of most potential human body planting body replaces For material.But because of the disadvantages of HAp brittleness is big, and intensity is low, and toughness is poor, it is largely limited at human bearing position Using.Hydroxyapatite coating layer is prepared in Mg alloy surface, the mechanical property of magnesium alloy and the biology of hydroxyapatite can be made Activity combines.And keyness bonding can be formed with the bone tissue of human body in a short time after being implanted into human body, can also stablize and drop The corrosion rate of low magnesium alloy preferably plays important function of the magnesium alloy in Bone Defect Repari treatment, therefore in Mg alloy surface Hydroxyapatite coating layer is prepared with good development prospect.
The method that people have developed a variety of Magnesiumalloy surface modifyings at present, common surface coating means mainly have: Sol-gal process, laser melting coating, differential arc oxidation, thermal spraying and electrochemical deposition etc..Wherein, electrochemical deposition method is due to deposition temperature It spends lower and can be deposited on complicated workpiece, therefore receive significant attention.Chinese invention patent (application No. is CN201710881395) " a kind of preparation method of medical magnesium alloy surface active coating " discloses a kind of hydro-thermal electrochemical deposition Method uses the anti-of high temperature and pressure in the preparation method of medical magnesium alloy surface deposition hydroxyapatite coating layer during the preparation process Condition is answered, the HAp coating of preparation is corynebacterium, and purity is higher;Chinese invention patent (application No. is CN201510310437) " one The surface modifying method of kind medical magnesium alloy " discloses a kind of method of pulse electrodeposition in the medical magnesium alloy for having remelted layer The surface of material prepares hydroxyapatite coating layer, completes the modification of medical magnesium alloy surface, uses high-current pulsed electron beam first Medical magnesium alloy matrix surface is irradiated, hydroxyapatite coating layer is then deposited on surface using electrodeposition method, So that HAp coating is formed mechanical closing component structure using the rough surface generated in high-current pulsed electron beam irradiation process, improves painting The bond strength and biocompatibility of layer and matrix;" one kind has Chinese invention patent (application No. is CN201510125339) The method of high bioactivity and low degradation rate biologic medical magnesium or Mg alloy surface electrochemical treatments " discloses a kind of by the differential of the arc Oxidation and electrochemical deposition combine the method for preparing HAp composite coating, improve the corrosion resistance and bioactivity of material.
But the above-mentioned method for preparing hydroxyapatite coating layer in medical magnesium alloy surface often has that the device is complicated, item Part requires height, is formulated the problems such as cumbersome, the reaction condition of high temperature and pressure is such as usually required during preparation, adulterate other adds Add agent to improve coating performance, electrochemical deposition etc. is carried out using pulse current using electrochemical workstation;Some also needs It first carries out surface to magnesium alloy before electrochemical deposition to be modified, so that process is complex.
Summary of the invention
It is an object of the invention to overcome preparation temperature height in the prior art, holiday is more, inadequate even compact, equipment And the disadvantage that formula is complicated, it provides and a kind of prepares fine acicular hydroxyapatite micro nano structure coating in medical magnesium alloy surface Preparation method, without using additive and pulse current, one-step synthesis under the conditions of relatively mild, and the hydroxyapatite prepared The coating is uniform and compact, the micro nano structure with fine acicular, and has good corrosion resistance.
Used technical solution is as follows to solve above-mentioned technical problem by the present invention:
The present invention provides a kind of preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating, described Preparation method the following steps are included:
(1) pretreatment of magnesium alloy substrate: magnesium alloy substrate is polished, and is cleaned, drying;
(2) it prepares electrochemical deposition electrolyte solution: weighing soluble calcium salt, dihydric phosphate, be dissolved separately in In ionized water, so that the concentration of calcium salt is 0.01-0.05mol/L, the concentration of dihydric phosphate is 0.006-0.03mol/L;It is mixed Calcium salt soln and phosphate dihydrogen salt solution are closed, electrochemical deposition electrolyte is obtained;
(3) electrochemical deposition: using platinum electrode as cathode, and magnesium alloy obtains pretreatment in step (1) as anode Magnesium alloy substrate be immersed in electrochemical deposition electrolyte, cathode anode is placed in parallel, connect D.C. regulated power supply, carry out Electrochemical deposition process;
(4) it post-processes: post-depositional magnesium alloy being placed in lye and carries out alkali heat-treatment, then is dried after being rinsed with deionized water It is dry, i.e., one layer of fine and close hydroxyapatite coating layer is formed in the magnesium alloy matrix surface that pretreatment obtains.
Further, the preprocessing process in step (1) be magnesium alloy substrate is successively used 400#, 600#, 800#, The sand paper of 1200# is polished, and the magnesium alloy substrate after polishing is successively clear with ultrasonic wave in dehydrated alcohol, acetone, deionized water Wash instrument ultrasonic cleaning, drying.
Further, in step (2) calcium salt soln and phosphate dihydrogen salt solution according to calcium ion and dihydrogen phosphate mole It is mixed than 1.67:1.
Further, cathode anode distance is 2-4cm, current density 0.5-2.5mA/cm in step (3)2, deposition temperature 85 DEG C, sedimentation time 0.5-1.5h of degree, when deposition, carry out magnetic agitation.
Further, the concentration of lye is 0.01-0.1mol/L in step (4), and heat treatment temperature is 70-90 DEG C, at heat The reason time is 2-4h.
Further, calcium salt described in step (2) is Ca (NO3)2·4H2O、CaCl2One of or combinations thereof;Phosphorus Acid dihydride salt is NH4H2PO4、KH2PO4Or NaH2PO4One of or combinations thereof.
Further, the magnesium alloy substrate is medical magnesium alloy, preferably AZ31B magnesium alloy.
The present invention also provides a kind of Mg alloy surface fine acicular hydroxyapatites being prepared by the preparation method Micro nano structure coating.
Technical effect of the invention is as follows:
(1) present invention prepares hydroxyapatite coating layer using the electrochemical deposition method of low temperature, low current density, due to electrification Learning deposition is carried out under low current density, can significantly reduce concentration polarization to the adverse effect of coating, so that coating has There is the structure of even compact;The preparation condition of low temperature can guarantee that the mechanical property of magnesium alloy substrate is unaffected;Electrochemistry is heavy Magnetic agitation is carried out during product, it can be to avoid hydrogen evolution phenomenon, so that the knot between hydroxyapatite coating layer and magnesium alloy substrate It is higher to close intensity.
(2) the electrochemical deposition electrolyte prescription that the present invention uses is simple, is only made of calcium salt and dihydric phosphate, nothing Any promotor or oxidant need to be added, without adjusting electrolyte ph, it is ensured that the growth of hydroxyapatite is not added The influence of agent can be grown along its c-axis, to grow into the micro nano structure of fine acicular.
(3) present invention process is simple, and cost is relatively low, can prepare even compact, hydroxyl with high purity in Mg alloy surface Base apatite coating, and coating has the micro nano structure of fine acicular, while raising magnesium alloy imitates anti-corrosion capability, also Conducive to cell in the adherency and growth of coating surface, to promote being bonded between implantation material and bone tissue, raising is implanted to Power.
Detailed description of the invention
Fig. 1 is the SEM photograph of hydroxyapatite coating layer prepared by the embodiment of the present invention 1;
Fig. 2 is the section SEM photograph of hydroxyapatite coating layer prepared by the embodiment of the present invention 1;
Fig. 3 is the XRD spectrum of hydroxyapatite coating layer prepared by the embodiment of the present invention 1;
Fig. 4 is the SEM photograph of hydroxyapatite coating layer prepared by the embodiment of the present invention 2;
Fig. 5 is Nyquist spectrum of the hydroxyapatite coating layer of the preparation of the embodiment of the present invention 2 in SBF;
Fig. 6 is that Nyquist of the hydroxyapatite coating layer of the preparation of the embodiment of the present invention 2 in SBF is composed in abscissa in 20- 400Ω·cm2Partial enlarged view in range.
Specific embodiment
It is clearly and completely described below in conjunction with the technical solution in the embodiment of the present invention, it is clear that described reality Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general Logical technical staff every other embodiment obtained without making creative work belongs to what the present invention protected Range.
Embodiment 1:
(1) AZ31B magnesium alloy substrate successively the pretreatment of magnesium alloy substrate: is used to the sand of 400#, 600#, 800#, 1200# Paper polishing;Magnesium alloy substrate after polishing is successively clear with ultrasonic washing instrument ultrasound in dehydrated alcohol, acetone, deionized water 10min is washed, is dried;
(2) it prepares electrochemical deposition electrolyte solution: weighing Ca (NO3)2·4H2O and NH4H2PO4, it is dissolved separately in In ionized water, so that Ca (NO3)2·4H2The concentration of O is 0.01mol/L, NH4H2PO4Concentration be 0.006mol/L;It will be above-mentioned Two kinds of solution are uniformly mixed in the ratio that calcium phosphorus molar ratio is 1.67 ︰ 1, obtain electrochemical deposition electrolyte;
(3) electrochemical deposition: using platinum electrode as cathode, and magnesium alloy is immersed in electrolyte solution as anode, yin Pole anode is placed in parallel, and is kept at a distance as 2cm, and D.C. regulated power supply is connected, and adjustings current density is 1.5mA/cm2, deposition temperature 85 DEG C, sedimentation time 1h of degree, when deposition, carry out magnetic agitation, revolving speed 500rpm;
(4) it post-processes: post-depositional sample is placed in 80 DEG C of alkali heat-treatment 2h in the NaOH solution of 1mol/L, then by sample It is dried after being rinsed with deionized water, i.e., forms one layer of fine and close hydroxyapatite coating layer in magnesium alloy matrix surface.
The SEM of hydroxyapatite coating layer prepared by the present embodiment is as shown in Figure 1, the coating is uniform and compact, by fine acicular Structure interts into flower-shaped and acanthosphere shape structure, and acicular texture diameter is about 230-670nm, and length is about 2.5-15 μm. The section SEM of the present embodiment hydroxyapatite coating layer is as shown in Fig. 2, uniform coating thickness, about 10 μm, and and basal body interface It is well combined.Fig. 3 is the XRD diagram of prepared coating, through X-ray diffraction analysis as can be seen that prepared coating is hydroxyl Apatite, and purity is higher.
Embodiment 2:
(1) medical magnesium alloy sample successively the pretreatment of magnesium alloy substrate: is used to the sand of 400#, 600#, 800#, 1200# Paper polishing;Magnesium alloy after polishing is successively cleaned by ultrasonic in dehydrated alcohol, acetone, deionized water with ultrasonic washing instrument 15min, drying.
(2) it prepares electrochemical deposition electrolyte solution: weighing CaCl2And KH2PO4, it is dissolved separately in deionized water, So that CaCl2Concentration be 0.05mol/L, KH2PO4Concentration be 0.03mol/L;Above two solution is pressed into calcium phosphorus molar ratio It is uniformly mixed for the ratio of 1.67 ︰ 1, obtains electrochemical deposition electrolyte.
(3) electrochemical deposition: using platinum electrode as cathode, and magnesium alloy is immersed in electrolyte solution as anode, yin Pole anode is placed in parallel, and is kept at a distance as 2cm, connection D.C. regulated power supply, adjusting current density 2.5mA/cm2, depositing temperature 85 DEG C, sedimentation time 0.5h, when deposition, carries out magnetic agitation, revolving speed 500rpm;
(4) it post-processes: post-depositional sample is placed in 80 DEG C of alkali heat-treatment 2h in the NaOH solution of 1mol/L, then by sample It is dried after being rinsed with deionized water, i.e., forms one layer of fine and close hydroxyapatite coating layer in magnesium alloy matrix surface.
The SEM of hydroxyapatite coating layer prepared by the present embodiment is as shown in figure 4, the coating is uniform and compact, by acicular texture It is formed with flower-like structure, acicular texture diameter is about 200-600nm, and length is about 2-13 μm.Fig. 5 is that the present embodiment is made The AC impedance spectroscopy of standby coating, Fig. 6 is the partial enlarged view of AC impedance spectroscopy, and the AC impedance of magnesium alloy bare die is 94ohm·cm2, the AC impedance of Coated With Hydroxyapatite magnesium alloy is 780ohmcm2, corrosion resistance improves significant.
Embodiment 3:
(1) medical magnesium alloy sample successively the pretreatment of magnesium alloy substrate: is used to the sand of 400#, 600#, 800#, 1200# Paper polishing;Magnesium alloy after polishing is successively cleaned by ultrasonic in dehydrated alcohol, acetone, deionized water with ultrasonic washing instrument 10min, drying;
(2) it prepares electrochemical deposition electrolyte solution: weighing Ca (NO3)2·4H2O and NH4H2PO4, it is dissolved separately in In ionized water, so that Ca (NO3)2·4H2The concentration of O is 0.0417mol/L, NH4H2PO4Concentration be 0.025mol/L;It will be upper It states two kinds of solution to be uniformly mixed in the ratio that calcium phosphorus molar ratio is 1.67 ︰ 1, obtains electrochemical deposition electrolyte;
(3) electrochemical deposition: using platinum electrode as cathode, and magnesium alloy is immersed in electrolyte solution as anode, yin Pole anode is placed in parallel, and is kept at a distance as 4cm, connection D.C. regulated power supply, adjusting current density 0.5mA/cm2, depositing temperature 85 DEG C, sedimentation time 1.5h, when deposition, carries out magnetic agitation, revolving speed 500rpm;
(4) it post-processes: post-depositional sample is placed in 70 DEG C of alkali heat-treatment 2h in the NaOH solution of 1mol/L, then by sample It is dried after being rinsed with deionized water, i.e., forms one layer of fine and close hydroxyapatite coating layer in magnesium alloy matrix surface.
Embodiment 4:
(1) medical magnesium alloy sample successively the pretreatment of magnesium alloy substrate: is used to the sand of 400#, 600#, 800#, 1200# Paper polishing;Magnesium alloy after polishing is successively cleaned by ultrasonic in dehydrated alcohol, acetone, deionized water with ultrasonic washing instrument 10min, drying;
(2) it prepares electrochemical deposition electrolyte solution: weighing Ca (NO3)2·4H2O and NH4H2PO4, it is dissolved separately in In ionized water, so that Ca (NO3)2·4H2The concentration of O is 0.0417mol/L, NH4H2PO4Concentration be 0.025mol/L;It will be upper It states two kinds of solution to be uniformly mixed in the ratio that calcium-phosphorus ratio is 1.67 ︰ 1, obtains electrochemical deposition electrolyte;
(3) electrochemical deposition: using platinum electrode as cathode, and magnesium alloy is immersed in electrolyte solution as anode, yin Pole anode is placed in parallel, and is kept at a distance as 2cm, connection D.C. regulated power supply, adjusting current density 1mA/cm2, depositing temperature 85 DEG C, sedimentation time 1h, when deposition, carries out magnetic agitation, revolving speed 500rpm;
(4) it post-processes: post-depositional sample is placed in 90 DEG C of alkali heat-treatment 2h in the NaOH solution of 1mol/L, then by sample It is dried after being rinsed with deionized water, i.e., forms one layer of fine and close hydroxyapatite coating layer in magnesium alloy matrix surface.
Embodiment 5:
(1) medical magnesium alloy sample successively the pretreatment of magnesium alloy substrate: is used to the sand of 400#, 600#, 800#, 1200# Paper polishing;Magnesium alloy after polishing is successively cleaned by ultrasonic in dehydrated alcohol, acetone, deionized water with ultrasonic washing instrument 10min, drying;
(2) it prepares electrochemical deposition electrolyte solution: weighing Ca (NO3)2·4H2O and NH4H2PO4, it is dissolved separately in In ionized water, so that Ca (NO3)2·4H2The concentration of O is 0.0417mol/L, NH4H2PO4Concentration be 0.025mol/L;It will be upper It states two kinds of solution to be uniformly mixed in the ratio that calcium-phosphorus ratio is 1.67 ︰ 1, obtains electrochemical deposition electrolyte;
(3) electrochemical deposition: using platinum electrode as cathode, and magnesium alloy is immersed in electrolyte solution as anode, yin Pole anode is placed in parallel, and is kept at a distance as 2cm, connection D.C. regulated power supply, adjusting current density 1.5mA/cm2, depositing temperature 85 DEG C, sedimentation time 1h, when deposition, carries out magnetic agitation, revolving speed 500rpm;
(4) it post-processes: post-depositional sample is placed in 80 DEG C of alkali heat-treatment 4h in the NaOH solution of 0.1mol/L, then by sample Product are dried after being rinsed with deionized water, i.e., form one layer of fine and close hydroxyapatite coating layer in magnesium alloy matrix surface.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention Various changes and improvements, should all fall into claims of the present invention determine protection scope in.

Claims (9)

1. a kind of preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating, which is characterized in that described Preparation method the following steps are included:
(1) pretreatment of magnesium alloy substrate: magnesium alloy substrate is polished, and is cleaned, drying;
(2) it prepares electrochemical deposition electrolyte solution: weighing soluble calcium salt, dihydric phosphate, be dissolved separately in deionization In water, so that the concentration of calcium salt is 0.01-0.05mol/L, the concentration of dihydric phosphate is 0.006-0.03mol/L;Calcium mixture Salting liquid and phosphate dihydrogen salt solution obtain electrochemical deposition electrolyte;
(3) electrochemical deposition: use platinum electrode as cathode, magnesium alloy is as anode, by the magnesium that pretreatment obtains in step (1) Alloy substrate is immersed in electrochemical deposition electrolyte, and cathode anode is placed in parallel, and connects D.C. regulated power supply, carries out electrification Learn deposition process;
(4) it post-processes: post-depositional magnesium alloy being placed in lye and carries out alkali heat-treatment, then is dried after being rinsed with deionized water, One layer of fine and close hydroxyapatite coating layer is formed in the magnesium alloy matrix surface that pretreatment obtains.
2. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 1, It is characterized in that, the preprocessing process in step (1) is the sand that magnesium alloy substrate is successively used to 400#, 600#, 800#, 1200# Paper polishing, the magnesium alloy substrate after polishing is successively clear with ultrasonic washing instrument ultrasound in dehydrated alcohol, acetone, deionized water It washes, dries.
3. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 1, It is characterized in that, calcium salt soln and phosphate dihydrogen salt solution are according to calcium ion and dihydrogen phosphate molar ratio 1.67 in step (2): 1 is mixed.
4. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 1, It is characterized in that, cathode anode distance is 2-4cm, current density 0.5-2.5mA/cm in step (3)2, 85 DEG C of depositing temperature, Sedimentation time 0.5-1.5h, when deposition, carry out magnetic agitation.
5. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 1, It is characterized in that, the concentration of lye is 0.01-0.1mol/L in step (4), heat treatment temperature is 70-90 DEG C, heat treatment time For 2-4h.
6. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 3, It is characterized in that, calcium salt described in step (2) is Ca (NO3)2·4H2O、CaCl2One of or combinations thereof;Biphosphate Salt is NH4H2PO4、KH2PO4Or NaH2PO4One of or combinations thereof.
7. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 1, It is characterized in that, the magnesium alloy substrate is medical magnesium alloy.
8. the preparation method of Mg alloy surface fine acicular hydroxyapatite micro nano structure coating according to claim 1, It is characterized in that, the hydroxyapatite coating layer is the hydroxyapatite micro nano structure coating of fine acicular.
9. a kind of Mg alloy surface fine acicular hydroxy-apatite being prepared by the described in any item preparation methods of claim 1-8 Stone micro nano structure coating.
CN201910137298.3A 2019-02-25 2019-02-25 Mg alloy surface fine acicular hydroxyapatite micro nano structure coating and preparation method Pending CN109758605A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021115872A1 (en) 2019-12-11 2021-06-17 Universita' Degli Studi Di Palermo Process for the surface treatment of magnesium alloys for biomedical applications

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WO2021115872A1 (en) 2019-12-11 2021-06-17 Universita' Degli Studi Di Palermo Process for the surface treatment of magnesium alloys for biomedical applications

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