CN102371005A - Zinc-doped porous nano-titanium oxide coating and its preparation method - Google Patents
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Abstract
Belonging to the technical field of biomedical ceramic coatings and nano-materials, the invention relates to a zinc-doped porous nano-titanium oxide coating and its preparation method. The preparation method consists of the steps of: providing a zinc-containing electrolytic solution, and supplementing at least one electrolyte for assisting arc striking, and in the electrolytic solution, taking titanium or titanium alloy as the positive electrode and stainless steel as the negative electrode, conducting microarc oxidation treatment to the titanium or titanium alloy with a direct current pulse power supply, thus obtaining a coating with a porous nano-crystal structure, a pore size of less than 20micrometers and a surface crystal grain scale of less than 100nm. Specifically, the coating phase is anatase titanium oxide or a composite of anatase titanium oxide and rutile titanium oxide, and has zinc content of 0.01-50 wt%. The nano-titanium oxide coating of the invention has better biocompatibility than existing titanium oxide coatings. And osteoblasts on the surface of the coating have faster propagation rate and stronger vigor. Thus, the zinc-doped porous nano-titanium oxide coating in the invention can be used as a replacing material for positions such as thighbones, hip joints, dental implants and others that bear heavy loads.
Description
Technical field
The present invention relates to a kind of zinc doping porous nano titanium oxide coating and preparation method thereof; What relate to or rather is a kind of titanio zinc doping porous nano titanium oxide coating that is used as artificial bone, hip joint or tooth implant and preparation method thereof, belongs to medical bio ceramic coating and technical field of nano material.
Background technology
Titanium and alloy thereof are widely used as bone tissue restoration and alternate material with its lower elastic modelling quantity, excellent biocompatibility, corrosion resistance and mechanical property.It is reported one deck thin film of titanium oxide that titanium and alloy excellent biocompatibility thereof and corrosion resistance mainly exist owing to its surface naturally.Therefore, titanium oxide ceramics and coating 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 [Chinese patent ZL200510029743.2; ZL 200510023170.2; Uchida M; Kim HM; Kokubo T; Fujibayashi S, Nakamura T.Structural dependence of apatite formation on titania gels in simulatedbody fluid.J.Biomed Mater Res.64A (2003) 164-170] and promote osteoblast to adhere to and propagation [Webster TJ, Siegel RW; Bizios R.Enhanced functions of osteoblasts on nanophaseceramics.Biomaterials 21 (2000) 1803-1810.] etc. the outstanding behaviours of aspect, caused that more People more and more pays close attention to widely.Yet; Titanium oxide still remains to be improved in the performance that promotes aspects such as osteoblast propagation and differentiation, specific proteins absorption and gene expression; And titanium oxide does not have antibiotic property, seeming powerless aspect prevention and the treatment implant postoperative infection, has limited its application clinically.
Zinc is a kind of important trace element of needed by human body.Discover; Most of zinc in the human body all concentrate in the skeleton, and are playing the part of positive role [Wei X, Ugurlu O in the process of the synthetic in vivo apatite of zinc; Ankit A; Acar HY, Akinc M.Dissolution behavior of Si, Zn-codoped tricalcium phosphates.MaterialsScience and Engineering is (2009) 126-135 C.29]; Zinc to skeletal growth, keep and reparation [the Yamaguchi M that plays an important role; Oishi H, Suketa Y.Stimulatory effect of zinc on bone formationin tissue culture.Biochem Pharmacol 36 (1987) 4007-4012.]; Zinciferous calcium phosphate and hydroxylapatite ceramic can significantly promote osteoblast propagation and alkaline phosphatase expression of enzymes; Promote the osteogen differentiation and enhance bone conduction [the Ikeuchi M of medullary cell; Ito A; Dohi Y, Ohgushi H, Shimaoka H; Yonemasu K, TateishiT.Osteogenic differentiation of cultured rat and human bone marrow cells on thesurface of zinc-releasing calcium phosphate ceramics.J Biomed Mater Res A 67 (2003) 1115-1122.]; Zinc can also promote the osteoblast activity and suppress the absorption of osteoclast; Increase bone protein, calcium and dna content [the Ito A in the osseous tissue; Kawamura H; Otsuka M, Ikeuchi M, et al.Zinc-releasing calciumphosphate for stimulating bone formation.Materials Science and Engineering C 22 (2002) 21-25].On the other hand; Zinc still is a kind of inorganic antiseptic of efficient, cleaning; Various bacteria such as escherichia coli and staphylococcus aureus there is remarkable bacteriostasis and sterilization effect [Yamamoto O; Nakakoshi K, Sasamoto T, NakagawaH.MiuraK.Adsorption and growth inhibition of bacteria on carbon materialscontaining zinc oxide.Carbon 39 (2001) 1643-1651; Wang X, Du Y, Liu H.Preparation, characterization and antimicrobial activity of chitosan-Zn complex.CarbohydratePolymers 56 (2004) 21-26].The doping research of zinc in calcium phosphate and hydroxylapatite ceramic is a lot of, does not but appear in the newspapers but the zinc doping titanium oxide improves the research of its biology performance.Therefore, zinc doping in nano-titanium oxide coating layer, is expected to improve its bone formation performance and antibiotic property, obtains can be applicable to clinical titanium oxide bone tissue restoration and alternate material.
In addition; There are some researches show; Nano material is promoting to show clear superiority aspect osteoblast adhesion, propagation and the differentiation than traditional material; Nano material can significantly promote the absorption [Balasundaram G, Webster TJ.A perspective on nanophase materials fororthopedic implant applications.J Mater Chem 16 (2006) 3737-3745s] of albumen at material surface through the improvement to surface energy and surface texture.On the other hand, porous material, the material that especially 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 [Akin FA; Zreiqat H; Jordan S, Wijesundara MBJ, Hanley L.Preparation and analysis ofmacroporous TiO
2Coatings on Ti surface for bone-tissue implants.J Biomed MaterRes 57 (2001) 588-596.].
Differential arc oxidization technique is claimed plasma electrolytic oxidation again, is a kind of new technique that directly generates ceramic coating in valve metal surface in situ oxidations such as titanium, magnesium, zirconium, aluminum.Its coating is porous and nanostructured, and is high with substrate combinating strength, and do not receive the restriction of workpiece geometric shape, can also be through the adjusting of electrolyte being realized the adjusting of membranous layer ingredient and function.The present invention intends novelty ground through adjusting and control to differential arc oxidation electrolyte, obtains the controlled porous nano titanium oxide coating of zinc doping content, thereby improves the skeletonization and the anti-microbial property of coating.
Summary of the invention
The present invention is based on the excellent biology performance of titanium oxide excellent biological compatibility and zinc element, and differential arc oxidization technique do not limit by the workpiece geometric shape, and coating and matrix bond are firm, and has porous and nanostructured proposes.Also promptly adopt differential arc oxidization technique to select suitable process conditions for use, in certain electrolyte, have porous and nanostructured at titanium or titanium alloy substrate surface preparation, and the zinc doping titanium oxide coating material of coating and matrix strong bonded.
Concrete technical process of the present invention is following:
A, a kind of electrolyte that includes zinc element is provided, and is aided with the electrolyte of at least a auxiliary starting the arc;
B, in above-mentioned specific electrolyte, be anode with titanium or titanium alloy, rustless steel is a negative electrode, adopts direct current pulse power source that titanium or titanium alloy are carried out differential arc oxidation and handles;
C, electric current density 0.1～5A/cm
2, voltage 200～700V, frequency 500～2000Hz, dutycycle 10～80%;
D, differential arc oxidation time are 1～60min;
E, preparation process electrolyte temperature are no more than 60 ℃.
The optimum content scope of zinc element is 0.01～0.5mol/L in the said electrolyte, and the electrolyte optimum content scope of the auxiliary starting the arc is 0.01～2mol/L.At least a in the preferred zinc acetate of electrolyte, zinc nitrate, zinc sulfate, zinc chloride or other soluble zinc salt of zinc element is provided; At least a in the preferred calcium acetate of electrolyte, sodium glycerophosphate, calcium hydrogen phosphate, sodium hydroxide, potassium hydroxide, phosphoric acid, nitric acid or the acetic acid of the auxiliary starting the arc.
The zinc doping titania coating of method for preparing is porous and nanocrystalline structures form, and the aperture is less than 20 μ m, and the surface microstructure yardstick is less than 100nm; Coating substance mainly is made up of anatase titanium oxide and rutile titanium oxide or pure anatase mutually; Coating and matrix bond are tight; Through adjustment electrolyte composition, concentration and process conditions, can make the content of zinc element in the coating controlled in 0.01～50wt% scope, preferable range is 0.01～35wt%.
When being immersed in coating in the buffer solution, zinc ion can discharge from coating in a long time continuously.Osteoblast can adhere to and breed at this coating surface fast, 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 osteoblast at coating surface.The zinc doping nano-titanium oxide coating layer all has tangible antibacterial effect to the escherichia coli of gram negative bacteria and the staphylococcus aureus of gram positive bacteria.The zinc doping porous nano titanium oxide coating that adopts preparation technology of the present invention to make at titanium or titanium alloy surface can be directly as carrying osseous tissue replacement and repair materials.
The present invention has following outstanding advantage:
1, the zinc doping porous nano titanium oxide coating of the present invention preparation has approaching elastic modelling quantity with sclerotin, and anchoring strength of coating is high, and chemical property is stable, has porous and nanostructured, the growth that helps new bone with combine.
2, the present invention generates the zinc doping porous nano titanium oxide coating in titanium or titanium alloy surface one-step method original position, and can be through adjustment electrolyte composition, concentration and process conditions, makes in the coating zinc element content controlled in 0.01～50wt% scope.
3, the zinc doping porous nano titanium oxide coating of the present invention's preparation has better biocompatibility than existing titania coating; Osteoblast is faster in this coating surface multiplication rate, vigor is stronger, can be used as the alternate material that femur, hip joint and tooth implant etc. bear big load position.
4, the zinc doping porous nano titanium oxide coating of the present invention's preparation all has tangible antibacterial effect to the escherichia coli of gram negative bacteria and the staphylococcus aureus of gram positive bacteria, is expected to effectively prevention and treatment implant postoperative infection.
5, preparation technology of the present invention is simple, quick, easy and simple to handle, controlled, is easy to apply.
Description of drawings
The surface scan electromicroscopic photograph of Fig. 1 zinc doping porous nano titanium oxide coating provided by the invention.(a) 500 times; (b) 50000 times.It is thus clear that coating is porous and nanostructured.
The X ray diffracting spectrum of Fig. 2 zinc doping porous nano titanium oxide coating provided by the invention.It is thus clear that coating is made up of anatase tio2 and rutile TiO2.The characteristic peak of titanium is from the titanio body among the figure.
The surperficial EDS collection of illustrative plates of Fig. 3 zinc doping porous nano titanium oxide coating provided by the invention.It is thus clear that zinc element successfully is doped in the coating.
The cross section scanning electron microscope pattern of Fig. 4 zinc doping porous nano titanium oxide coating provided by the invention.It is thus clear that coating and matrix bond are tight.
The cell quantity of Fig. 5 osteoblast after pure titanium, porous nano titanium oxide coating and zinc doping porous nano titanium oxide coating provided by the invention surface are cultivated 1,4,12 and 24 hour.It is thus clear that the zinc doping porous nano titanium oxide coating more helps the growth and the propagation of osteoblast than other two kinds of materials, shows better cell compatibility.
Specific embodiment
Further illustrate characteristics of the present invention and effect through embodiment below.Limit the present invention absolutely not.
Embodiment 1:
(a) use deionized water that the zinc acetate of 0.02mol/L, the calcium acetate of 0.1mol/L and the sodium glycerophosphate of 0.05mol/L are hybridly prepared into electrolyte.(b) be that anode, rustless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 0.5A/cm
2, voltage 400～460V, frequency 800Hz, dutycycle 10% condition under handle 4min, keep electrolyte temperature to be lower than 60 ℃.(c) sample takes out back flushing and natural drying in deionized water.Through detection, the about 5-10 μ of coating layer thickness m, elementary composition Ti, O, Zn, Ca and the P of being mainly, X-ray diffraction analysis show that the coating phase composition is mainly pure anatase TiO
2, EDS result shows that zinc element content is about 3.4wt% in the coating, sem analysis shows that the coating aperture is less than 10 μ m, crystal particle scale 10-100nm.
Embodiment 2:
(a) use deionized water that the zinc acetate of 0.04mol/L, the calcium acetate of 0.1mol/L and the sodium glycerophosphate of 0.05mol/L are hybridly prepared into electrolyte.(b) be that anode, rustless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 0.5A/cm
2, voltage 400～480V, frequency 800Hz, dutycycle 10% condition under handle 4min, keep electrolyte temperature to be lower than 60 ℃.(c) sample takes out back flushing and natural drying in deionized water.Through detection, the about 6-12 μ of coating layer thickness m, elementary composition Ti, O, Zn, Ca and the P of being mainly, X-ray diffraction analysis shows that the coating phase composition is mainly anatase TiO
2With rutile TiO
2, EDS result shows that zinc element content is about 7.3wt% in the coating, sem analysis shows that the coating aperture is less than 10 μ m, crystal particle scale 20-100nm.
Embodiment 3:
(a) use deionized water that the zinc nitrate of 0.08mol/L, the calcium acetate of 0.2mol/L, the sodium glycerophosphate of 0.02mol/L and the sodium hydroxide of 0.1mol/L are hybridly prepared into electrolyte.(b) be that anode, rustless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 1A/cm
2, voltage 500～600V, frequency 1000Hz, dutycycle 30% condition under handle 3min, keep electrolyte temperature to be lower than 60 ℃.(c) sample takes out back flushing and natural drying in deionized water.Through detection, the about 25-35 μ of coating layer thickness m, elementary composition Ti, O, Zn, Ca and the P of being mainly, X-ray diffraction analysis shows that the coating phase composition is mainly anatase TiO
2With rutile TiO
2, EDS result shows that zinc element content is about 15.7wt% in the coating, sem analysis shows that the coating aperture is less than 20 μ m, crystal particle scale 40-100nm.
Embodiment 4:
(a) use deionized water that the zinc acetate of 0.02mol/L and the calcium acetate of 0.1mol/L are hybridly prepared into electrolyte.(b) be that anode, rustless steel are negative electrode with the titanium, adopt direct current pulse power source at constant current density 1A/cm
2, voltage 250～320V, frequency 800Hz, dutycycle 20% condition under handle 5min, keep electrolyte temperature to be lower than 60 ℃.(c) sample takes out back flushing and natural drying in deionized water.Through detecting, the about 3-10 μ of coating layer thickness m, elementary composition Ti, O, Zn and the Ca of being mainly, X-ray diffraction analysis show that the coating phase composition is pure anatase TiO
2, EDS result shows that zinc element content is about 0.9wt% in the coating, sem analysis shows that the coating aperture is less than 1 μ m, crystal particle scale 10-80nm.
Embodiment 5:
(a) use deionized water that the zinc sulfate of 0.1mol/L and the phosphoric acid of 0.15mol/L are hybridly prepared into electrolyte.(b) be that anode, rustless 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 15min, keep electrolyte temperature to be lower than 60 ℃.(c) sample takes out back flushing and natural drying in deionized water.Through detection, the about 15-30 μ of coating layer thickness m, elementary composition Ti, O, Zn, S and the P of being mainly, X-ray diffraction analysis show that the coating phase composition is rutile TiO
2With anatase TiO
2, EDS result shows that zinc element content is about 26.7wt% in the coating, sem analysis shows that the coating aperture is less than 15 μ m, crystal particle scale 10-80nm.
Embodiment 6:
(a) use deionized water that the zinc chloride of 0.04mol/L, the sodium hydroxide of 0.1mol/L and the sodium glycerophosphate of 0.05mol/L are hybridly prepared into electrolyte.(b) be that anode, rustless steel are negative electrode with the Nitinol, adopt direct current pulse power source at constant current density 1.5A/cm
2, voltage 480～550V, frequency 600Hz, dutycycle 30% condition under handle 30min, keep electrolyte temperature to be lower than 60 ℃.(c) sample takes out back flushing and natural drying in deionized water.Through detection, the about 35-50 μ of coating layer thickness m, elementary composition Ti, O, Zn, Na, P and the Ni of being mainly, X-ray diffraction analysis shows that the coating phase composition is mainly anatase TiO
2With rutile TiO
2, EDS result shows that zinc element content is about 33.6wt% in the coating, sem analysis shows that the coating aperture is less than 20 μ m, crystal particle scale 20-100nm.
Claims (6)
1. a zinc doping porous nano titanium oxide coating is characterized in that, coating is porous nano crystalline texture form, and the aperture is less than 20 μ m, and the surface microstructure yardstick is less than 100nm; Coating substance is anatase titanium oxide mutually, or anatase titanium oxide and rutile titanium oxide is compound; The content of zinc element is at 0.01～50wt% in the coating.
2. by the described a kind of zinc doping porous nano titanium oxide coating of claim 1, it is characterized in that the content of zinc element is at 0.01～35wt%.
3. the method for preparing of a zinc doping porous nano titanium oxide coating is characterized in that, comprises the steps:
(1) a kind of electrolyte that includes zinc element is provided, and is aided with the electrolyte of at least a auxiliary starting the arc;
(2) in above-mentioned specific electrolyte, be anode with titanium or titanium alloy, rustless steel is a negative electrode, adopts direct current pulse power source that titanium or titanium alloy are carried out the differential arc oxidation processing.
4. by the method for preparing of the described a kind of zinc doping porous nano titanium oxide coating of claim 3, it is characterized in that the differential arc oxidation treatment conditions are control electric current density 0.1～5A/cm
2, voltage 200～700V, frequency 500～2000Hz, dutycycle 10～80%; Control arc oxidization time is 1～60min; The control electrolyte temperature is no more than 60 ℃.
5. press the method for preparing of claim 3 or 4 described a kind of zinc doping porous nano titanium oxide coatings; It is characterized in that; The content range of zinc element is 0.01～0.5mol/L in the electrolyte; The electrolytical content range of the auxiliary starting the arc is 0.01～2mol/L, provides the electrolyte of zinc element to comprise at least a in zinc acetate, zinc nitrate, zinc sulfate, zinc chloride or other soluble zinc salt; The electrolyte of the auxiliary starting the arc comprises at least a in calcium acetate, sodium glycerophosphate, calcium hydrogen phosphate, sodium hydroxide, potassium hydroxide, phosphoric acid, nitric acid or the acetic acid.
6. a zinc doping porous nano titanium oxide coating is in the application of artificial bone, hip joint or tooth implant.
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| CN102732882A (en) * | 2012-07-13 | 2012-10-17 | 东南大学 | Artificial joint with micro-nano graded topological surface structure and preparation method of artificial joint |
| CN102995092A (en) * | 2012-11-23 | 2013-03-27 | 北京星航机电设备厂 | Blue titan-alloy microarc oxidation coloring solution and preparation method thereof |
| CN103526261A (en) * | 2013-10-17 | 2014-01-22 | 赵全明 | Preparation method of zinc-containing micro-arc oxidation electrolyte and zinc-containing biological ceramic membrane |
| CN103911644A (en) * | 2014-04-09 | 2014-07-09 | 江西科技师范大学 | Micro-arc oxidation electrolyte and micro-arc oxidation method for titanium alloys |
| CN105420786A (en) * | 2015-11-19 | 2016-03-23 | 西安交通大学 | Preparation method for nano-sodium silicotitanate/titanium dioxide bio-coatings on titanium surfaces |
| CN105648497A (en) * | 2016-01-13 | 2016-06-08 | 西安交通大学 | Zinc titanate-titanium oxide composite antibacterial coating on surface of titanium and preparation method of zinc titanate-titanium oxide composite antibacterial coating |
| CN110965108A (en) * | 2019-12-27 | 2020-04-07 | 沈兰兰 | Zn-TiO2Method for producing a coating |
| CN111467572A (en) * | 2020-04-09 | 2020-07-31 | 上海交通大学医学院附属第九人民医院 | Implant material and preparation method and application thereof |
| CN111839768A (en) * | 2020-07-28 | 2020-10-30 | 中日友好医院(中日友好临床医学研究所) | Zinc-modified implant and preparation method thereof |
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| CN102732882B (en) * | 2012-07-13 | 2014-08-13 | 东南大学 | Artificial joint with micro-nano graded topological surface structure and preparation method of artificial joint |
| CN102732882A (en) * | 2012-07-13 | 2012-10-17 | 东南大学 | Artificial joint with micro-nano graded topological surface structure and preparation method of artificial joint |
| CN102995092A (en) * | 2012-11-23 | 2013-03-27 | 北京星航机电设备厂 | Blue titan-alloy microarc oxidation coloring solution and preparation method thereof |
| CN103526261A (en) * | 2013-10-17 | 2014-01-22 | 赵全明 | Preparation method of zinc-containing micro-arc oxidation electrolyte and zinc-containing biological ceramic membrane |
| CN103911644B (en) * | 2014-04-09 | 2016-10-05 | 江西科技师范大学 | Titanium alloy micro-arc oxidation electrolyte and differential arc oxidation method |
| CN103911644A (en) * | 2014-04-09 | 2014-07-09 | 江西科技师范大学 | Micro-arc oxidation electrolyte and micro-arc oxidation method for titanium alloys |
| CN105420786A (en) * | 2015-11-19 | 2016-03-23 | 西安交通大学 | Preparation method for nano-sodium silicotitanate/titanium dioxide bio-coatings on titanium surfaces |
| CN105648497A (en) * | 2016-01-13 | 2016-06-08 | 西安交通大学 | Zinc titanate-titanium oxide composite antibacterial coating on surface of titanium and preparation method of zinc titanate-titanium oxide composite antibacterial coating |
| CN105648497B (en) * | 2016-01-13 | 2018-06-26 | 西安交通大学 | A kind of titanium surface zinc titanate-titanium oxide composite antibacterial coating and preparation method thereof |
| CN110965108A (en) * | 2019-12-27 | 2020-04-07 | 沈兰兰 | Zn-TiO2Method for producing a coating |
| WO2021168917A1 (en) * | 2020-02-25 | 2021-09-02 | 北京爱康宜诚医疗器材有限公司 | Antibacterial three-dimensional porous bone implant material and preparation method therefor |
| CN111467572A (en) * | 2020-04-09 | 2020-07-31 | 上海交通大学医学院附属第九人民医院 | Implant material and preparation method and application thereof |
| CN111839768A (en) * | 2020-07-28 | 2020-10-30 | 中日友好医院(中日友好临床医学研究所) | Zinc-modified implant and preparation method thereof |
| CN112813478A (en) * | 2020-12-30 | 2021-05-18 | 西比里电机技术(苏州)有限公司 | Method for performing thermoelectric chemical oxidation on surface of niobium-titanium alloy and electrolyte |
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