CN101928974A - Preparation method and application of magnesium-doped porous nano titanium oxide coating - Google Patents
Preparation method and application of magnesium-doped porous nano titanium oxide coating Download PDFInfo
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- CN101928974A CN101928974A CN 201010225723 CN201010225723A CN101928974A CN 101928974 A CN101928974 A CN 101928974A CN 201010225723 CN201010225723 CN 201010225723 CN 201010225723 A CN201010225723 A CN 201010225723A CN 101928974 A CN101928974 A CN 101928974A
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Abstract
The invention belongs to the technical field of biological ceramics, and in particular relates to a preparation method and application of a magnesium-doped porous nano titanium oxide coating. In the method, in magnesium ion-containing electrolyte, the magnesium-doped porous nano titanium oxide coating is directly generated on the surface of titanium or titanium alloy by one step by microarc oxidation technology, wherein based on the volume of the electrolyte, the magnesium ion concentration range is 0.01-0.5mol/L. The magnesium-doped porous nano titanium oxide coating prepared by the method mainly comprises anatase titanium oxide and rutile titanium oxide or pure anatase; and when the coating is soaked in buffer solution, magnesium ions can be released from the coating in a long time. Osteoblasts can quickly attach to and propagate on the surface of the coating, and have good biocompatibility without cytotoxicity. Compared with undoped titanium oxide coating, the magnesium-doped porous nano titanium oxide coating can obviously improve the propagation rate and activity of the osteoblasts on the surface of the coating.
Description
Technical field
The invention belongs to the biological ceramics technical field, be specifically related to a kind of preparation method and application thereof of magnesium-doped porous nano titanium oxide coating.
Background technology
Titanium and alloy thereof are widely used as bone tissue restoration and replacement material with its lower Young's modulus, excellent biocompatibility, erosion resistance and mechanical property.It is reported one deck thin film of titanium oxide that titanium and alloy excellent biocompatibility thereof and erosion resistance mainly exist naturally owing to its surface.Therefore, titanium oxide ceramics and coated material become the research focus in the technical field of biological material.Especially in recent years, nano-titanium oxide is inducing osteoid apatite to form (referring to Chinese patent ZL 200510029743.2, ZL 200510023170.2, Uchida M, Kim HM, Kokubo T, Fujibayashi S, Nakamura T.Structural dependence of apatite formation on titania gels in simulated body fluid.J.Biomed Mater Res.64A (2003) 164-170) and promote sclerocyte adhere to propagation (referring to Webster TJ, Siegel RW, Bizios R.Enhanced functions of osteoblasts on nanophase ceramics.Biomaterials 21 (2000) 1803-1810.) etc. the outstanding behaviours of aspect more makes it obtain people's concern more and more widely.Yet titanium oxide still remains to be improved in the performance that promotes aspects such as sclerocyte propagation and differentiation, specific proteins absorption and genetic expression, has limited its application clinically.
Magnesium is the element that contains flow control more than four in the human body, also is one of fundamental element of skeleton.Studies show that, magnesium has vital role (referring to Staiger MP to the metabolism of human body and the formation of natural bone, Pietak AM, Huadmai J, Dias G. Magnesium and its alloys as orthopedic biomaterials:A review.Biomaterials 27 (2006) 1728-1734); Mg content in the Mammals area of new bone is significantly higher than old bone; The content of magnesium is the highest in the early stage calcification stage that bone forms, and deeply reducing along with the calcification stage; Consuming excessively of magnesium can cause sclerocyte and osteoclast activity to reduce in the human body, it is fragile (referring to Chaudhry AA that bone also can become, Goodall J, Vickers M, Cockcroft JK, Rehman I, Knowlesd JC, Darr JA.Synthesis and characterisation of magnesium substituted calcium phosphate bioceramic nanoparticles made via continuous hydrothermal flow synthesis.J Mater Chem 18 (2008) 5900-5908).Research is also found, magnesium can induce osteoid apatite at its surface deposition in simulated body fluid, show that it has certain biological activity (referring to Wan YZ, Huang Y, He E, Wang YL, Zhao ZG, Ding HF.Effect of Mg ion implantation on calcium phosphate formation on titanium.Surf Coat Tech 201 (2006) 2904-2909); Magniferous calcium triphosphate shows the synthetic and excretory characteristics of remarkable promotion cell proliferation and collagenase, magniferous hydroxyapatite then can significantly improve the synosteosis performance (referring to Xu L, Pan F, Yu G, Yang L, Zhang E, Yang K.In vitro and in vivo evaluation of the surface bioactivity of a calcium phosphate coated magnesium alloy.Biomaterials 30 (2009) 1512-1523).In a word, research and the application of magnesium in biomaterial caused people's extensive concern.The existing part report of the doping research of magnesium in calcium phosphate and hydroxylapatite ceramic, but the rarely seen report of the research of magnesium adulterated TiOx pottery.Magnesium is doped in the nano-titanium oxide coating layer, is expected to improve its biology performance, obtain can be applicable to clinical titanium oxide bone tissue restoration and replacement material.
In addition, there are some researches show, nano material is promoting to show clear superiority aspect sclerocyte adhesion, propagation and the differentiation than traditional material, nano material is by the improvement to surface energy and surface tissue, can significantly promote the absorption (referring to Balasundaram G, Webster TJ.A perspective on nanophase materials for orthopedic implant applications.J Mater Chem 16 (2006) 3737-3745s) of albumen at material surface.On the other hand, porous material, especially the material that has the micron order aperture also can significantly promote the adhesion and the propagation of cell, and porous material helps the interior growth of new bone in vivo, strengthens the combination between area of new bone and the implant, quickens patient's rehabilitation (referring to Akin FA, Zreiqat H, Jordan S, Wijesundara MBJ, Hanley L Preparation and analysis of macroporous TiO
2Coatings on Ti surface for bone-tissue implants.J Biomed Mater Res 57 (2001) 588-596.).
Differential arc oxidization technique claims plasma electrolytic oxidation again, is a kind of new technology that directly generates ceramic coating in valve metal surface in situ oxidations such as titanium, magnesium, zirconium, aluminium.The coating of using this technology to make is porous and nanostructure, with the substrate combinating strength height, and is not subjected to the restriction of workpiece geometric shape, can also be by the adjusting of electrolytic solution being realized the adjusting of membranous layer ingredient and function.Yet for this technology, the principal element that influences the differential arc oxidation film-formation result comprises: electrolyte component and concentration thereof, solution temperature, electrical parameter and treatment time etc., wherein, electrolyte component and concentration difference, the current potentials of differential arc oxidation phenomenon such as differential of the arc formation and the speed that moves, the continuous differential of the arc of maintenance etc. are different, voltage and current behavior difference, the color of gained rete, quality, thickness and thing phase composite and electrochemical properties are also different.For how the electrolytic solution by using suitable concn and suitable differential arc oxidization technique parameter can make that to have the active magnesium-doped porous nano titanium oxide coating of good biological then be the problem of the present required solution in this area at titanium and alloy surface thereof in this area, and prior art for the relevant report of this partial content seldom.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, a kind of preparation method and application thereof of magnesium-doped porous nano titanium oxide coating are provided.
The present invention adopts following technical scheme to solve the problems of the technologies described above:
A kind of preparation method of magnesium-doped porous nano titanium oxide coating, this method adopt differential arc oxidization technique in containing the electrolytic solution of magnesium ion, directly generate magnesium-doped porous nano titanium oxide coating at titanium or titanium alloy surface single stage method original position; Wherein, with the volumeter of described electrolytic solution, the concentration range of magnesium ion is 0.01～0.5mol/L.
Preferable, with the volumeter of described electrolytic solution, the concentration range of described magnesium ion is 0.02～0.1mol/L, and provides the ionogen of described magnesium ion to be selected from magnesium acetate, magnesium nitrate, magnesium chloride or other solubility magnesium salts one or more.
Preferable, also can add assisted electrolysis matter in the described electrolytic solution, with the volumeter of described electrolytic solution, the concentration of described assisted electrolysis matter is 0.01～2mol/L, more preferably 0.1～0.25mol/L; And described assisted electrolysis matter is selected from lime acetate, Sodium Glycerophosphate, sodium hydroxide, potassium hydroxide, phosphoric acid, nitric acid and the acetate one or more.
Preferable, described differential arc oxidization technique is to be anode with titanium or titanium alloy, and stainless steel is a negative electrode, adopts direct current pulse power source that titanium or titanium alloy are carried out differential arc oxidation and handles.
Preferably, described titanium alloy is Ti
6Al
4V.
Further preferred, the parameter of described differential arc oxidization technique is: current density 0.1～5A/cm
2, 0.5～1.5A/cm more preferably
2Voltage 300～700V, more preferably 300～550V; Frequency 500～2000Hz, more preferably 800～1500Hz; Dutycycle 10%～80%, more preferably 10%～50%; The differential arc oxidation time is 1～60min, more preferably 3～30min; The preparation process electrolyte temperature is no more than 60 ℃, more preferably 10～50 ℃.
Magnesium adulterated TiOx coating by method of the present invention makes is porous and nanocrystalline structures form, and coating and matrix bond are tight.Coat-thickness is 2 to 150 microns, and the aperture is less than 20 microns.Coating substance mainly is made up of anatase titanium oxide and rutile titanium oxide or pure anatase octahedrite mutually.By adjusting electrolytic solution composition, concentration and processing condition, can make the content of magnesium elements in the coating controlled in 0～20wt% scope, promptly increase concentration of electrolyte, prolong the differential arc oxidation treatment time or increase and handle current/voltage, magnesium element content raises in the coating.When being immersed in coating in the buffered soln, magnesium ion can discharge from coating in a long time continuously.Sclerocyte can adhere to and breed fast at this coatingsurface, demonstrates excellent biological compatibility, does not have cytotoxicity.Compare with adulterated TiOx coating not, this coating can significantly improve multiplication rate and the vigor of sclerocyte at coatingsurface.The magnesium-doped porous nano titanium oxide coating that adopts preparation technology of the present invention to make at titanium or titanium alloy surface can directly be replaced and repair materials as the carrying osseous tissue, for example be used to prepare artificial femur, hip joint and root of the tooth.
The present invention has following outstanding advantage:
1, the magnesium-doped porous nano titanium oxide coating of the present invention preparation has approaching Young's modulus with sclerotin, the anchoring strength of coating height, chemical property is stable, has porous and nanostructure, the growth that helps new bone with combine.
2, the present invention generates magnesium-doped porous nano titanium oxide coating in titanium or titanium alloy surface single stage method original position, and can be by adjusting electrolytic solution composition, concentration and processing condition, makes in the coating magnesium element content controlled in 0～20wt.% scope.
3, the magnesium-doped porous nano titanium oxide coating of the present invention's preparation has better biocompatibility than existing titania coating, sclerocyte is faster in this coatingsurface multiplication rate, vigor is stronger, can be used as bone tissue restoration and replacement material that femur, hip joint and root of the tooth etc. bear big load position.
4, preparation technology of the present invention is simple, quick, easy and simple to handle, controlled, is easy to apply.
The present invention intends obtaining the controlled porous nano titanium oxide coating of magnesium doping content by adjusting and control to differential arc oxidation electrolytic solution, thereby improves the biology performance of coating.The present invention is based on the biology performance of titanium oxide excellent biological compatibility and magnesium elements excellence, and differential arc oxidization technique do not limit by the workpiece geometric shape, coating and matrix bond are firm, and have porous and nanostructure proposes.Also promptly adopt differential arc oxidization technique to select suitable process conditions for use, in certain electrolytic solution, have porous and nanostructure at titanium or titanium alloy substrate surface preparation, and the magnesium adulterated TiOx coated material of coating and matrix mortise.
Description of drawings
The surface scan electromicroscopic photograph of Fig. 1 magnesium-doped porous nano titanium oxide coating provided by the invention.(a) 1000 times; (b) 50000 times.
The X ray diffracting spectrum of Fig. 2 magnesium-doped porous nano titanium oxide coating provided by the invention.
The surperficial EDS collection of illustrative plates of Fig. 3 magnesium-doped porous nano titanium oxide coating provided by the invention.
The cross section pattern of Fig. 4 magnesium-doped porous nano titanium oxide coating provided by the invention and distribution diagram of element spectrum.
Fig. 5 sclerocyte MC3T3-E1 is at pure titanium surface (a) and the laser co-focusing photo after magnesium-doped porous nano titanium oxide coating provided by the invention surface (b) is cultivated 12 hours.
Embodiment
Further describe technical scheme of the present invention below by specific embodiment.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.
Embodiment 1:
(a) use deionized water that the magnesium acetate of 0.04mol/L, the lime acetate of 0.1mol/L and the Sodium Glycerophosphate of 0.05mol/L are hybridly prepared into electrolytic solution.(b) be that anode, stainless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 0.5A/cm
2, voltage 390～460V, frequency 800Hz, dutycycle 10% condition under handle 4min, keep electrolyte temperature to be lower than 60 ℃ (being 50 ℃).(c) sample takes out back flushing and seasoning in deionized water.After testing, the about 8-15 μ of coat-thickness m, elementary composition Ti, O, Mg, Ca and the P of being mainly, X-ray diffraction analysis show that the coating phase composite is mainly pure anatase octahedrite TiO
2With rutile TiO
2, EDS result shows that magnesium element content is about 1.3wt% in the coating, sem analysis shows that the coating aperture is less than 10 μ m, crystal particle scale 10-80nm.
The surface scan electromicroscopic photograph of the magnesium-doped porous nano titanium oxide coating that Fig. 1 makes for present embodiment, coating is porous and nanostructure as can be seen from Fig. 1.The X ray diffracting spectrum of the magnesium-doped porous nano titanium oxide coating that Fig. 2 makes for present embodiment, coating is by anatase octahedrite TiO as can be seen from Fig. 2
2With rutile TiO
2Form, the characteristic peak of titanium comes the titanium matrix among Fig. 2.The surperficial EDS collection of illustrative plates of the magnesium-doped porous nano titanium oxide coating that Fig. 3 makes for present embodiment, magnesium elements successfully is doped in the coating as can be seen from Fig. 3.Fig. 4 composes (b) for the cross section pattern (a) and the distribution diagram of element of the magnesium-doped porous nano titanium oxide coating that present embodiment makes, and coating and matrix bond are tight as can be seen from Fig. 4, and magnesium elements is uniformly dispersed in coating.Fig. 5 is that sclerocyte MC3T3-E1 is at pure titanium surface (a) and the laser co-focusing photo after the magnesium-doped porous nano titanium oxide coating surface (b) that present embodiment makes is cultivated 12 hours, as seen sprawl more abundant in the cellular form on magnesium-doped porous nano titanium oxide coating surface among Fig. 5, the Actin muscle of contained green is more, demonstrates excellent cell compatibility.
Embodiment 2:
(a) use deionized water that the magnesium acetate of 0.08mol/L, the sodium hydroxide of 0.1mol/L, the lime acetate of 0.1mol/L and the Sodium Glycerophosphate of 0.05mol/L are hybridly prepared into electrolytic solution.(b) be that anode, stainless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 1A/cm
2, voltage 400～480V, frequency 800Hz, dutycycle 10% condition under handle 3min, keep electrolyte temperature to be lower than 60 ℃ (being 50 ℃).(c) sample takes out back flushing and seasoning in deionized water.After testing, the about 15-25 μ of coat-thickness m, elementary composition Ti, O, Mg, Ca and the P of being mainly, X-ray diffraction analysis shows that the coating phase composite is mainly anatase octahedrite TiO
2With rutile TiO
2, EDS result shows that zinc element content is about 3.2wt% in the coating, sem analysis shows that the coating aperture is less than 15 μ m, crystal particle scale 20-100nm.
Embodiment 3:
(a) use deionized water that the magnesium nitrate of 0.02mol/L and the lime acetate of 0.1mol/L are hybridly prepared into electrolytic solution.(b) be that anode, stainless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 0.9A/cm
2, voltage 300～350V, frequency 1000Hz, dutycycle 30% condition under handle 5min, keep electrolyte temperature to be lower than 60 ℃ (being 40 ℃).(c) sample takes out back flushing and seasoning in deionized water.After testing, the about 3-8 μ of coat-thickness m, elementary composition Ti, O, Mg and the Ca of being mainly, X-ray diffraction analysis show that the coating phase composite is pure anatase octahedrite TiO
2, EDS result shows that magnesium element content is about 0.7wt% in the coating, sem analysis shows that the coating aperture is less than 1 μ m, crystal particle scale 10-80nm.
Embodiment 4:
(a) use deionized water that the magnesium chloride of 0.1mol/L and the phosphoric acid of 0.15mol/L are hybridly prepared into electrolytic solution.(b) be that anode, stainless steel are negative electrode with Ti6Al4V, adopt direct current pulse power source at constant current density 1.5A/cm
2, voltage 450～530V, frequency 1500Hz, dutycycle 50% condition under handle 20min, keep electrolyte temperature to be lower than 60 ℃ (being 50 ℃).(c) sample takes out back flushing and seasoning in deionized water.After testing, the about 15-30 μ of coat-thickness m, elementary composition Ti, O, Mg, P and the Al of being mainly, X-ray diffraction analysis show that the coating phase composite is rutile TiO
2With anatase octahedrite TiO
2, EDS result shows that magnesium element content is about 10.8wt% in the coating, sem analysis shows that the coating aperture is less than 15 μ m, crystal particle scale 10-80nm.
Embodiment 5:
(a) use deionized water that the magnesium acetate of 0.1mol/L, the sodium hydroxide of 0.1mol/L and the Sodium Glycerophosphate of 0.05mol/L are hybridly prepared into electrolytic solution.(b) be that anode, stainless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 1A/cm
2, voltage 480～550V, frequency 800Hz, dutycycle 10% condition under handle 30min, keep electrolyte temperature to be lower than 60 ℃ (being 10 ℃).(c) sample takes out back flushing and seasoning in deionized water.After testing, the about 30-40 μ of coat-thickness m, elementary composition Ti, O, Mg, Na and the P of being mainly, X-ray diffraction analysis shows that the coating phase composite is mainly rutile TiO
2With anatase octahedrite TiO
2, EDS result shows that magnesium element content is about 14.5wt% in the coating, sem analysis shows that the coating aperture is less than 20 μ m, crystal particle scale 20-100nm.
Claims (10)
1. the preparation method of a magnesium-doped porous nano titanium oxide coating, this method adopt differential arc oxidization technique in containing the electrolytic solution of magnesium ion, directly generate magnesium-doped porous nano titanium oxide coating at titanium or titanium alloy surface single stage method original position; Wherein, with the volumeter of described electrolytic solution, the concentration range of magnesium ion is 0.01～0.5mol/L.
2. the preparation method of the magnesium-doped porous nano titanium oxide coating described in claim 1 is characterized in that, provides the ionogen of described magnesium ion to be selected from magnesium acetate, magnesium nitrate, magnesium chloride or other solubility magnesium salts one or more.
3. the preparation method of the magnesium-doped porous nano titanium oxide coating described in claim 1 is characterized in that, also contains assisted electrolysis matter in the described electrolytic solution, and with the volumeter of described electrolytic solution, the concentration of assisted electrolysis matter is 0.01～2mol/L.
4. the preparation method of the magnesium-doped porous nano titanium oxide coating described in claim 3 is characterized in that, described assisted electrolysis matter is selected from one or more in lime acetate, Sodium Glycerophosphate, sodium hydroxide, potassium hydroxide, phosphoric acid, nitric acid and the acetate.
5. as the preparation method of arbitrary described magnesium-doped porous nano titanium oxide coating in the claim 1～4, it is characterized in that, described differential arc oxidization technique is to be anode with titanium or titanium alloy, and stainless steel is a negative electrode, adopts direct current pulse power source that titanium or titanium alloy are carried out differential arc oxidation and handles.
6. the preparation method of the magnesium-doped porous nano titanium oxide coating described in claim 5 is characterized in that, described titanium alloy is Ti
6Al
4V.
7. the preparation method of the magnesium-doped porous nano titanium oxide coating described in claim 5 is characterized in that, the parameter of described differential arc oxidization technique is: current density 0.1～5A/cm
2, voltage 300～700V, frequency 500～2000Hz, dutycycle 10～80%, differential arc oxidation time is that 1～60min, preparation process electrolyte temperature are no more than 60 ℃.
8. a magnesium-doped porous nano titanium oxide coating is made by arbitrary described method in the claim 1～7.
9. the magnesium-doped porous nano titanium oxide coating described in the claim 8 is in the application of biomedical materials field.
10. the application described in claim 9 is characterized in that, described magnesium-doped porous nano titanium oxide coating is replaced and repair materials as the carrying osseous tissue.
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| CN103251984A (en) * | 2013-05-13 | 2013-08-21 | 上海交通大学 | Porous titanium microsphere bone filling material |
| GB2513575A (en) * | 2013-04-29 | 2014-11-05 | Keronite Internat Ltd | Corrosion and erosion-resistant mixed oxide coatings for the protection of chemical and plasma process chamber components |
| CN107829123A (en) * | 2017-10-09 | 2018-03-23 | 深圳市中科摩方科技有限公司 | A kind of aluminium alloy of surface duplex coating and its preparation method and application |
| CN109371443A (en) * | 2018-11-01 | 2019-02-22 | 赵全明 | A kind of preparation method of electrolyte solution and titanium implant surface magnesium/titanium dioxide micropore ceramics coating and preparation method thereof |
| CN110565144A (en) * | 2018-11-01 | 2019-12-13 | 赵全明 | Porous biological ceramic coating with antibacterial and bone-promoting functions and preparation method and application thereof |
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| GB2513575B (en) * | 2013-04-29 | 2017-05-31 | Keronite Int Ltd | Corrosion and erosion-resistant mixed oxide coatings for the protection of chemical and plasma process chamber components |
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| CN103251984A (en) * | 2013-05-13 | 2013-08-21 | 上海交通大学 | Porous titanium microsphere bone filling material |
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| CN109371443A (en) * | 2018-11-01 | 2019-02-22 | 赵全明 | A kind of preparation method of electrolyte solution and titanium implant surface magnesium/titanium dioxide micropore ceramics coating and preparation method thereof |
| CN110565144A (en) * | 2018-11-01 | 2019-12-13 | 赵全明 | Porous biological ceramic coating with antibacterial and bone-promoting functions and preparation method and application thereof |
| CN115444980A (en) * | 2021-06-08 | 2022-12-09 | 中国科学院上海硅酸盐研究所 | Metal ion doped titanium dioxide nano coating, preparation method and application thereof in nerve and bone tissue repair |
| CN115055697A (en) * | 2022-06-08 | 2022-09-16 | 佳木斯大学 | Preparation method of super-hydrophilic micro-nano surface of nickel-titanium implant for 3D printing |
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Application publication date: 20101229 |