CN100346001C - Method of preparing nano-titanium oxide coating layer having bioactivity - Google Patents
Method of preparing nano-titanium oxide coating layer having bioactivity Download PDFInfo
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- CN100346001C CN100346001C CNB2005100231702A CN200510023170A CN100346001C CN 100346001 C CN100346001 C CN 100346001C CN B2005100231702 A CNB2005100231702 A CN B2005100231702A CN 200510023170 A CN200510023170 A CN 200510023170A CN 100346001 C CN100346001 C CN 100346001C
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Abstract
The present invention relates to a preparation method for nano titanium oxide coatings with bioactivity, which belongs to the field of medical bioceramic coatings. The present invention is characterized in that the preparation method comprises the following steps: firstly, nano titanium oxide coatings are prepared by an atmosphere plasma spraying method; then, the sprayed nano titanium oxide coatings are irradiated by ultraviolet light after being cleaned; therefore, the surface of the nano titanium oxide coatings prepared by the plasma spraying method is activated in a biologic way, and bone-like apatite can be induced to form on the surface of the coatings after the surface of the nano titanium oxide coatings contacts with body fluid. Ultraviolet radiation is carried out by that the coatings are dipped in simulated body fluid, or air or water, and the time for the radiation is no less than 12 hours. The present invention uses powder as raw materials, and the powder uses main crystal phases as anatase; after spraying, the main crystal phases of coatings are rutile phases. The offered nano titanium oxide coatings which are deposited on the medical metal base substances and have bioactivity are a new bioactive material for replacing bones.
Description
Technical field
The present invention relates to a kind of method for preparing the nano-titanium oxide coating layer of biologically active, adopt the air plasma spraying method to prepare nano-titanium oxide coating layer more precisely, and then carry out the UV-light bioactivation and handle, belong to the medical bio field of ceramic coatings.
Background technology
In the last thirty years, hydroxyapatite coating layer in plasma spraying obtains extensive concern and application clinical, and this mainly is because hydroxyapatite is the main inorganic composition of skeleton, has good biological activity and biocompatibility.Yet, hydroxyapatite coating layer in plasma spraying has two distinct disadvantage that limit its application, the one, low-crystallinity, low degree of crystallinity is degraded hydroxyapatite coating layer easily in body fluid, thereby reduced its work-ing life [Fazan F, Marquis PM, Dissolutionbehavior of plasma-sprayed hydroxyapatite coatings, J.Mater.Sci.:Mater.Med.2000; 11:787-92]; The 2nd, and relatively low bonding strength between the titanium alloy substrate, low bonding strength can make the patient face danger [the Lamy D of disbonding, Pierrc AC and Heimann RB, Hydroxyapatite coatings with a bond coat of biomedical implants by plasmaprojection, J.Mater.Res., 1996,11:680-686].Although investigators adopt a lot of different post-treating methods to go to overcome and solve this two kinds of shortcomings at present, all do not obtain effect preferably.
TiO
2Have excellent biological compatibility, this has obtained confirming widely, thereby also has been applied gradually in technical field of biological material.Simultaneously, in simulated body fluid, osteoid apatite can form M.Keshmiri and T.Troczynski.Apatite formation on TiO at the anatase octahedrite microsphere surface
2Anatasemicrospheres.J.Non-Cryst.Solids 324 (2003) 289-294], this is a specific index of material biologically active.Also have the investigator to find TiO simultaneously with nanostructure
2Surface energy promotes osteoblastic adhesion, growth and propagation [Thomas J.Webster et al.Enhancedfunctions of osteoblasts on nanophase ceramics, Biomaterials 21 (2000) 1803-1810].This shows nanostructure TiO
2Might both have certain biological activity, have excellent biological compatibility again.This is preparation nanostructure TiO
2Form good synostosis behind the bone substitution material implant into body and between the osseous tissue possibility is provided.But pre-stage test confirms that the routine and the nano-titanium oxide coating layer that adopt plasma spray coating process to obtain all lack biological activity, and in simulated body fluid, osteoid apatite can not form at coatingsurface.
On the other hand, TiO
2With advantages such as its moderate energy gap, advantages of high catalytic activity, anti-photoetch and nontoxic, good stabilities, become the photocatalyst important research object.TiO
2Under the irradiation of certain wavelength light, the valence band electronics can be energized into conduction band, and produces electron-hole pair, and this electron-hole pair has stronger redox ability, majority of organic pollutants in the oxidable environment.Along with the development of nanotechnology, nano-titanium oxide begins to substitute conventional titanium oxide and is applied in photocatalysis field.The grain-size of nanostructure titanium oxide is little, when its particle diameter little when a certain threshold value, it is remarkable that quantum size effect becomes, energy gap broadens, and the energy that illumination produces electronics and hole is higher, has higher redox ability, and along with reducing of particle diameter, the compound minimizing in light induced electron and hole can effectively improve the productive rate of electron-hole pair, thereby has better catalytic capability when making nano-titanium oxide as photocatalyst.Simultaneously, under UV-irradiation, form a large amount of activity hydroxy groups on the nano-titanium oxide surface, in simulated body fluid, this helps the formation of osteoid apatite.So, cause the present invention.
Summary of the invention
The object of the invention is to provide a kind of method for preparing the nano-titanium oxide coating layer of biologically active.It is based on, and the photocatalysis characteristic of plasma spraying nano-titanium oxide coating layer and biological characteristics propose.Purpose is to utilize plasma spraying technology, with the nano-titanium oxide powder deposition on the medical metal matrix, and adopt the post-treating method of UV-irradiation to improve the biological activity and the biocompatibility of plasma spraying nano-titanium oxide coating layer, thereby develop novel biological activity bone substitution material.
The plasma spraying nano-titanium oxide coating layer is expected to solve the dissolving of artificial bone coating and peels off problem.Because the affinity of titania coating and titanium alloy substrate is better, and very high bonding strength is arranged between plasma spraying titania coating and the titanium alloy substrate, can reach 2～3 times of hydroxyapatite coating layer.In addition, titanium oxide is the extraordinary material of a kind of erosion resistance, and very low solubility rate is arranged in body fluid, so titania coating just can have very long work-ing life in vivo.Limit the major cause that titania coating uses clinically is that it lacks biological activity before.By the UV-light aftertreatment, can make plasma spraying nanostructure titania coating have good biological activity, and titanium oxide is a kind of biocompatible materials that gains public acceptance.Therefore, adopt method of the present invention, will obtain a kind of artificial bone coated material with high comprehensive performance.
Specific embodiment is as follows:
With particle diameter is nano oxidized ti powder below the 100nm, and forming aggregate particle size behind mist projection granulating is micron-sized spherical powder.Adopt plasma spraying technology, the nano-titanium oxide powder deposition after the granulation on the medical metal matrix, is prepared titania coating.Under the optimized parameters (seeing Table 1) titanium dioxide powder is being sprayed on the medical metal matrix that cleans with sandblast.The cleaning of metallic matrix and sandblast are technology commonly used in the general Plasma Spraying Process Using, and its processing parameter need not at this detailed description, and one of ordinary skill in the art all can be grasped and be known.
Table 1 spray parameters
| Plasma gas Ar plasma gas H 2Spray distance | 30～80slpm *? 6～12slpm 90～120mm | Powder carrier gas Ar powder feeding rate electric current | 2.5～4.5 |
*Slpm: standard liter/min
Principal crystalline phase be the nano oxidized ti powder of anatase octahedrite after the plasma flame high-temperature fusion, high speed deposition forms coating to titanium alloy-based surface after the condensation cured.In this process, the partial oxidation titanium undergoes phase transition, and is phase-changed into the rutile phase from anatase octahedrite, under different spray parameters, can obtain the coating of different anatase octahedrite content, the coating principal crystalline phase with good microtexture all is the rutile phase, and coatingsurface is made up of less than the nano particle of 50nm particle diameter.With the ultrasonic cleaning 5 minutes in acetone of the titania coating that obtains, then coating is soaked in and carries out UV-irradiation in the simulated body fluid simultaneously, UV-light can be produced by the UV-lamp of various models, and concrete power has range of choice widely, and the UV-irradiation synoptic diagram is seen Fig. 1.In simulated body fluid, if the UV-irradiation sufficiently long time, osteoid apatite can directly form at coatingsurface.In addition, UV-irradiation also can be in simulated body fluid, and in water or air in advance through the short period of time UV-irradiation, irradiation time 12 hours or be not less than 12 hours, coating does not continue to be immersed in the simulated body fluid under having the situation of UV-irradiation then, osteoid apatite also can form on the nano-titanium oxide coating layer surface, and this shows that the nano-titanium oxide coating layer surface after UV-irradiation is handled has good biological activity.Employed medium can be selected according to actual needs when ultra-violet lamp power, UV-irradiation time and irradiation.(seeing embodiment for details)
In sum, method feature provided by the invention is at first to prepare nano-titanium oxide coating layer with the air plasma spraying method, use to be principal crystalline phase be spraying raw material as the titanium dioxide powder of anatase octahedrite, nano-titanium oxide coating layer after will spraying then carries out UV-irradiation after cleaning, thereby make the activation of nano-titanium oxide coating layer surface biological, with can bring out osteoid apatite after body fluid contacts and form at coatingsurface, the air plasma spraying processing parameter is as shown in table 1.
Description of drawings
Fig. 1 UV-irradiation synoptic diagram
The XRD figure of Fig. 2 plasma spraying nano-titanium oxide coating layer
R represents rutile among the figure, and A represents anatase octahedrite
Fig. 3 (a) plasma spraying nano-titanium oxide coating layer surface topography;
(b) plasma spraying nano-titanium oxide coating layer cross section pattern.
In simulated body fluid, soak the surface topography after 168 hours under Fig. 4 (a) plasma spraying nano-titanium oxide coating layer UV-irradiation; (b) in simulated body fluid, soak cross section pattern after 168 hours under the plasma spraying nano-titanium oxide coating layer UV-irradiation
In simulated body fluid, soak the surface topography after 168 hours under the conventional titania coating UV-irradiation of Fig. 5 (a) plasma spraying; (b) the plasma spraying nano-titanium oxide coating layer soaks the surface topography (not having UV-irradiation) after 28 days in simulated body fluid.
Concrete implementation step
Further illustrate characteristics of the present invention and effect below by embodiment.Limit the present invention absolutely not.
Embodiment 1: with particle diameter is nano oxidized ti powder (principal crystalline phase is an anatase octahedrite) about 30nm, and forming aggregate particle size behind mist projection granulating is micron-sized spherical powder.Adopt plasma spraying technology, the nano-titanium oxide powder deposition after the granulation on titanium alloy substrate, is prepared into titania coating.Concrete spray parameters sees Table 2.The XRD analysis that obtains coating under this spray parameters is seen Fig. 2, and the result shows that the coating principal crystalline phase is a rutile.Coatingsurface scanning electron microscope analysis confirmation coatingsurface mainly is made up of less than the nano particle of 50nm particle diameter, sees Fig. 3 a, is coated with layer cross section (Fig. 3 b) and shows that coating combines better with titanium alloy substrate, does not have obvious crack, and coating internal fissure and pore are all less.
With the ultrasonic cleaning 5 minutes in acetone of the titania coating that obtains, coating is soaked in as shown in Figure 1 carries out UV-irradiation, irradiation time 168 hours in the simulated body fluid simultaneously then.UV-light produces (GGZ-125 straight tube shape, Shanghai Yaming Lamp Bulb Factory Co., Ltd. produces) by ultraviolet high-pressure mercury lamps, the mercury lamp center to sample apart from 30-40mm.Scanning electron microscopic observation finds that osteoid apatite can form on plasma spraying nano-titanium oxide coating layer surface, and as shown in Figure 4, this shows that the UV-irradiation processing can improve the biological activity of plasma spraying nano-titanium oxide coating layer.Simultaneous test confirms that in simulated body fluid, through the identical time of UV-irradiation, osteoid apatite can not form on conventional titania coating (adopting conventional titanium dioxide powder plasma spraying to form) surface, shown in Fig. 5 (a); Test simultaneously also confirms there is not UV-irradiation, is immersed in the simulated body fluid after 4 weeks, does not still have osteoid apatite to be formed on the nano-titanium oxide coating layer surface, shown in Fig. 5 (b).
Table 2 spray parameters
| Plasma gas Ar plasma gas H 2Spray distance | 40slpm *12slpm 100mm | Powder carrier gas Ar powder feeding rate electric current | 3.5slpm 6g/min 600A |
*Slpm: standard liter/min
Embodiment 2: with particle diameter is nano oxidized ti powder (principal crystalline phase is an anatase octahedrite) about 50nm, and forming aggregate particle size behind mist projection granulating is micron-sized spherical powder.Adopt plasma spraying technology, the nano-titanium oxide powder deposition after the granulation on titanium alloy substrate, is prepared titania coating.Concrete spray parameters sees Table 2.With the ultrasonic cleaning 5 minutes in acetone of the titania coating that obtains, coating is soaked in carries out UV-irradiation, irradiation time 168 hours in the simulated body fluid simultaneously then.Scanning electron microscopic observation finds that osteoid apatite can form on the titania coating surface.All the other are with embodiment 1.
Embodiment 3: with particle diameter is nano oxidized ti powder (principal crystalline phase is an anatase octahedrite) about 30nm, and forming aggregate particle size behind mist projection granulating is micron-sized spherical powder.Adopt plasma spraying technology, the nano-titanium oxide powder deposition after the granulation on titanium alloy substrate, is prepared titania coating.Concrete spray parameters sees Table 3.With the ultrasonic cleaning 5 minutes in acetone of the titania coating that obtains, coating is soaked in carries out UV-irradiation, irradiation time 12 hours in the simulated body fluid simultaneously then.Stop UV-irradiation, directly be soaked in 2 weeks in the simulated body fluid of no UV-irradiation after the coating of handling is taken out from original simulated body fluid.Scanning electron microscopic observation is found, osteoid apatite can form on the titania coating surface, this shows, in simulated body fluid, UV-irradiation can make the activation of plasma spraying nano-titanium oxide coating layer surface biological in 12 hours, biologically active is with formation and the growth that can bring out osteoid apatite after body fluid contacts.All the other are with embodiment 1.
Table 3 spray parameters
| Plasma gas Ar plasma gas H 2Spray distance | 35slpm * 6slpm 110mm | Powder carrier gas Ar powder feeding rate electric current | 3.5slpm 8g/min 600A |
*Slpm: standard liter/min
Table 4 spray parameters
| Plasma gas Ar plasma gas H 2Spray distance | 50slpm * 10slpm 90mm | Powder carrier gas Ar powder feeding rate electric current | 4slpm 8g/min 650A |
*Slpm: standard liter/min
Embodiment 4: with particle diameter is nano oxidized ti powder (principal crystalline phase is an anatase octahedrite) about 30nm, and forming aggregate particle size behind mist projection granulating is micron-sized spherical powder.Adopt plasma spraying technology, the nano-titanium oxide powder deposition after the granulation on titanium alloy substrate, is prepared titania coating.Concrete spray parameters sees Table 4.With the ultrasonic cleaning 5 minutes in acetone of the titania coating that obtains, coating is soaked in carries out UV-irradiation in the deionized water simultaneously then, irradiation time is 12 hours.Stop UV-irradiation, directly be soaked in 4 weeks in the simulated body fluid of no UV-irradiation after the coating of handling is taken out from deionized water.Scanning electron microscopic observation finds that osteoid apatite can form on the titania coating surface, and this shows that in deionized water, UV-irradiation can make the coatingsurface activation in 12 hours, can bring out the formation and the growth of osteoid apatite after being immersed in the simulated body fluid.Therefore, in deionized water, carry out UV-irradiation and can give the plasma spraying bioactivity of nanometer titania coating.All the other are with embodiment 1.
Embodiment 5: with particle diameter is nano oxidized ti powder (principal crystalline phase is an anatase octahedrite) about 30nm, and forming aggregate particle size behind mist projection granulating is micron-sized spherical powder.Adopt plasma spraying technology, the nano-titanium oxide powder deposition after the granulation on titanium alloy substrate, is prepared into titania coating.Concrete spray parameters sees Table 5.With the ultrasonic cleaning 5 minutes in acetone of the titania coating that obtains, then coating is carried out UV-irradiation in atmosphere, irradiation time 12 hours.Stop UV-irradiation, postradiation coating is soaked in 4 weeks in the simulated body fluid of no UV-irradiation.Scanning electron microscopic observation finds that osteoid apatite can form on the titania coating surface, and this shows that in atmosphere, UV-irradiation can make the coatingsurface activation in 12 hours, can bring out the formation and the growth of osteoid apatite after being immersed in the simulated body fluid.Therefore, in atmosphere, carry out UV-irradiation and can give the plasma spraying bioactivity of nanometer titania coating.When concrete surgical operation, can directly when being carried out uv sterilisation, implant make the activation of plasma spraying nano-titanium oxide coating layer, simplified processing step.All the other are with embodiment 1.
Table 5 spray parameters
| Plasma gas Ar plasma gas H 2Spray distance | ?60slpm *?8slpm ?100mm | Powder carrier gas Ar powder feeding rate electric current | 4.5slpm 8g/min 500A |
*Slpm: standard liter/min
Claims (7)
1. method for preparing the biologically active nano-titanium oxide coating layer, it is characterized in that at first preparing nano-titanium oxide coating layer with the air plasma spraying method, nano-titanium oxide coating layer after will spraying then carries out UV-irradiation after cleaning, thereby make plasma spraying nano-titanium oxide coating layer surface biological activation, and can bring out osteoid apatite after body fluid contacts and form at coatingsurface; Described atmospheric plasma spraying technology processing parameter is: plasma gas is Ar and H
2Mixed gas, wherein Ar is 30～80 standard liter/min and H
2Be 6～12 standard liter/min, spray distance is 90～120 millimeters, and the powder carrier gas is that Ar is 2.5～4.5 standard liter/min, and powder feeding rate is 5～15 gram/minute, and spraying current is 400～650A; And the employing principal crystalline phase is that the titanium dioxide powder of anatase octahedrite is a spraying raw material.
2. press the method for the nano-titanium oxide coating layer of the described preparation biologically active of claim 1, the particle diameter that it is characterized in that described spraying raw material is less than 100nm, the surface that obtains this coating behind plasma spraying is that principal crystalline phase is the coating of rutile, by the granulometric composition less than 50nm.
3. press the method for the nano-titanium oxide coating layer of the described preparation biologically active of claim 1, it is characterized in that UV-irradiation is coatings prepared to be immersed in carry out UV-irradiation in the simulated body fluid simultaneously, bring out osteoid apatite and form and growth at coatingsurface.
4. press the method for the nano-titanium oxide coating layer of the described preparation biologically active of claim 1, it is characterized in that UV-irradiation is coatings prepared to be immersed in carry out UV-irradiation in the deionized water simultaneously, make the coatingsurface bioactivation, be immersed in then in the simulated body fluid, can bring out osteoid apatite and form and growth at coatingsurface.
5. press the method for the nano-titanium oxide coating layer of the described preparation biologically active of claim 1, it is characterized in that UV-irradiation is that coatings prepared is carried out UV-irradiation in atmosphere, make the coatingsurface bioactivation, be immersed in then in the simulated body fluid, can bring out osteoid apatite and form and growth at coatingsurface.
6. by the method for the nano-titanium oxide coating layer of each preparation biologically active in the claim 1,3,4 or 5, it is characterized in that the UV-light of using is to be produced by high voltage mercury lamp, the UV-irradiation time was not less than 12 hours.
7. press the method for the nano-titanium oxide coating layer of claim 1 or 2 described preparation biologically actives, earlier the nano level titanium dioxide powder being formed aggregate particle size behind mist projection granulating before it is characterized in that spraying is micron-sized spherical powder.
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| US6433154B1 (en) | 1997-06-12 | 2002-08-13 | Bristol-Myers Squibb Company | Functional receptor/kinase chimera in yeast cells |
| CN1830536A (en) | 2000-05-16 | 2006-09-13 | 明尼苏达大学评议会 | High mass throughput particle generation using multiple nozzle spraying |
| CN100368027C (en) * | 2005-09-16 | 2008-02-13 | 中国科学院上海硅酸盐研究所 | Hydrogen ion implantation process of raising bioactivity of nanometer titania coating |
| CA2637883C (en) | 2006-01-31 | 2015-07-07 | Regents Of The University Of Minnesota | Electrospray coating of objects |
| US9108217B2 (en) | 2006-01-31 | 2015-08-18 | Nanocopoeia, Inc. | Nanoparticle coating of surfaces |
| US9248217B2 (en) | 2006-01-31 | 2016-02-02 | Nanocopocia, LLC | Nanoparticle coating of surfaces |
| US9040816B2 (en) | 2006-12-08 | 2015-05-26 | Nanocopoeia, Inc. | Methods and apparatus for forming photovoltaic cells using electrospray |
| CN104027839B (en) * | 2014-06-17 | 2015-09-09 | 浙江大学 | A kind of method in pure titanium surface preparation with biologically active nanometer structure |
| CN106958014B (en) * | 2017-04-06 | 2019-05-17 | 西南交通大学 | In the method for pure magnesium surface building hybrid inorganic-organic function and service coating |
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| CN1184626A (en) * | 1997-11-19 | 1998-06-17 | 化南理工大学 | Method for preparing artificial joint with bio-active gradient coating |
| JP2004169077A (en) * | 2002-11-19 | 2004-06-17 | Nippon Steel Corp | Method for manufacturing locally alloyed metal product |
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