CN103536371B - A kind of dentistry implant and preparation method thereof - Google Patents
A kind of dentistry implant and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of dentistry implant and preparation method thereof, the honeycomb nano-titanium oxide rete that described dentistry implant comprises titanio material and surface in situ formation thereof causes described dentistry implant surface to form honeycomb nanotopography, the oxygen content of the nano oxidized titanium layer of wherein said honeycomb increases with thicknesses of layers and successively decreases, and transits to described titanio material gradually.The present invention forms honeycomb nano-titanium oxide rete to form honeycomb nanotopography on described dentistry implant surface at titanio material surface in situ, wherein honeycomb nano-titanium oxide rete is thin, intensity is better, and with titanio material without obvious layering, in conjunction with firm, and the nanostructured of rule effectively can strengthen the expression of mesenchymal stem cells MSCs at the adhesion of implant surface, alkaline phosphatase activities and Bone formation-related gene, embody excellent bone to induction ability, thus improve long-time stability and the success rate of dentistry implant.
Description
Technical field
The present invention relates to dentistry implant Material Field, particularly one surperficial honeycomb nano-pattern dentistry implant and preparation method thereof.
Background technology
Along with the raising of social life level and being on the rise of aged tendency of population, the quantity of dental prosthetic and plastic surgery operations thereof presents sustainable growth trend.Because dentistry planting technology is one of important method of repairing defect of dentition or disappearance, the development of dentistry implant is paid close attention to.A kind of effective promotion Integrated implant is proved to be to implant surface modification and improves the method for implantation body's success rate, research simultaneously shows the nanostructured of implant surface, as nanotube-shaped surface topography can promote osteoblastic attachment and functional expression, can also to the adhesion of people's Gingival Fibroblasts, propagation and albumen, gene expression has significant facilitation (ActaBiomaterialia2011,7 (1): 2686-2696.).Therefore, carrying out making Nano surface modification to tooth implant is the effective means improving implantation body's effect further.
But, because of mastication behind dentistry implant implantation oral cavity, the stress situation born is complicated, active force is large, uneven and the long action time in force part, nano coating prepared by implant surface or thin film can produce because of the effect of this irregular stress dissolving of breaking and come off, and often cause implantation body to loosen and lose efficacy, and finally cause Integrated implant failure.
Summary of the invention
In order to the film strength solving dental implant surface nano modification coating or thin film in prior art is low, film and substrate combinating strength are not good, the problems such as stress fatigue damage, a kind of surface is the object of the present invention is to provide to be dentistry implant of the honeycomb nano-titanium oxide rete of growth in situ and preparation method thereof, thus strengthen film strength and film and substrate combinating strength, and strengthen the adhesion of mesenchymal stem cells MSCs in implant surface, the expression of alkaline phosphatase activities and Bone formation-related gene, strengthen bone to induction ability, thus improve long-time stability and the success rate of dentistry implant.
At this, on the one hand, the invention provides a kind of dentistry implant, the honeycomb nano-titanium oxide rete that described dentistry implant comprises titanio material and surface in situ formation thereof causes described dentistry implant surface to form honeycomb nanotopography, the nano oxidized titanium layer oxygen content of wherein said honeycomb increases with thicknesses of layers and successively decreases, and transits to described titanio material gradually.
The present invention forms honeycomb nano-titanium oxide rete to form honeycomb nanotopography on described dentistry implant surface at titanio material surface in situ, wherein honeycomb nano-titanium oxide rete is thin, intensity is better, and with titanio material without obvious layering, in conjunction with firm, thus described dentistry implant is behind implantation oral cavity, the active force of larger situation complexity can be born and can not to break and dissolving comes off, and the nanostructured of rule effectively can strengthen the adhesion of mesenchymal stem cells MSCs in implant surface, the expression of alkaline phosphatase activities and Bone formation-related gene, embody excellent bone to induction ability, thus improve long-time stability and the success rate of dentistry implant.
Preferably, the thickness of described honeycomb nano-titanium oxide rete is 25 ~ 35nm.
Preferably, described titanio material is medical titanium or titanium alloy.
On the other hand, the present invention also provides a kind of method preparing above-mentioned dentistry implant, comprising:
(1) anodized is carried out to be oxidized at surface in situ to titanio material dentistry implant, thus obtained surface is formed with the titanio material dentistry implant of titanium oxide nanotubes thin film; And
(2) the titanio material dentistry implant being formed with titanium oxide nanotubes thin film with described surface comes off from matrix surface to make described titanium oxide nanotubes thin film for negative electrode carries out electrolysis, thus obtained surface is the dentistry implant of honeycomb nano-titanium oxide rete.
The present invention can obtain the titanium oxide layer of the well-regulated nanostructured of tool (honeycomb) that original position is formed by two one-step electrolysis, thus strengthen film strength and film and substrate combinating strength, and the nanostructured of rule effectively can strengthen the expression of mesenchymal stem cells MSCs at the adhesion of implant surface, alkaline phosphatase activities and Bone formation-related gene, embody excellent bone to induction ability, thus improve long-time stability and the success rate of dentistry implant.
Preferably, the electrolyte that described anodic oxidation adopts is the ethylene glycol solution containing 0.1 ~ 1.0wt% ammonium fluoride and 1 ~ 10vol% water.
Preferably, described anodic oxidation constant voltage DC mode, running voltage is 20 ~ 80V, and oxidization time is 1 ~ 96 hour, and reaction temperature is room temperature.
Preferably, described anodised running voltage is 40 ~ 60V, and oxidization time is 1 ~ 3 hour.
Preferably, in step (2), described electrolysis adopts constant voltage DC mode, and voltage is 2 ~ 5V, and conduction time is 3 ~ 10 minutes, and reaction temperature is room temperature.
Preferably, in step (2), the electrolyte that described electrolysis adopts is the dilution heat of sulfuric acid of 0.5 ~ 2mol/L.
Step of the present invention is simple, with low cost, can obtain the dentistry implant of the honeycomb nano-titanium oxide rete that surface is formed for original position at short notice.
Accompanying drawing explanation
Fig. 1 is pretreated dentistry implant surface topography map in the present invention's example;
Fig. 2 is the titanium oxide nanotubes film surface appearance figure obtained through first step constant voltage DC anodized dentistry implant of the present invention;
Fig. 3 is the surface topography map of the dentistry implant of the present invention's example, and illustration is the figure of enlargement ratio step by step of pattern topology;
Fig. 4 is that the titanium of the dentistry implant surface honeycomb nano-pattern thin layer of the present invention's example, oxygen content are with depth profile curve chart;
Fig. 5 is rat bone marrow mesenchymal stem cells cultivates 4h respectively nucleus (1) and cytoskeleton (2) fluorescence staining picture pure titanium matched group (a) and nano-pattern experimental group (b) surface;
Fig. 6 is the alkaline phosphatase activities result that pure titanium matched group and nano-pattern experimental group surface rat bone marrow mesenchymal stem cells are cultivated 7 days;
Fig. 7 is the gene pyramiding enzyme chain reaction analysis result of Bone Gla protein (OCN), osteopontin (OPN), transcription factor (Runx2) and the bone morphogenetic protein (BMP2) that pure titanium matched group and nano-pattern experimental group surface rat bone marrow mesenchymal stem cells are cultivated 7 days.
Detailed description of the invention
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
Fig. 3 illustrates the surface topography map of the dentistry implant of the present invention's example, with reference to Fig. 3, the dentistry implant of the present invention's example comprises the honeycomb nano-titanium oxide rete that titanio material and surface in situ thereof formed causes described dentistry implant surface to form honeycomb nanotopography.The honeycomb nanotopography of described dentistry implant surface formation can be observed from the figure of enlargement ratio step by step Fig. 3.
Fig. 4 illustrate the dentistry implant surface honeycomb nano-pattern thin layer of the present invention's example through photoelectron spectroscopy detect obtain titanium, oxygen content is with depth profile curve chart, honeycomb nano-pattern chemistry consists of titanium oxide as can be seen from Figure, surface titanium (Ti): oxygen (O) ratio is 1:2, increase with the degree of depth, oxygen content reduces gradually, and superficial oxidation titanium thickness is about 25 ~ 35nm.It can thus be appreciated that the oxygen content of the nano oxidized titanium layer of honeycomb increases with thicknesses of layers and successively decreases, and transits to described titanio material gradually.And illustrate that nano-pattern rete is very thin, with matrix without obvious layering, bond strength is high.
In one example, titanio material can adopt medical titanium or titanium alloy.
The present invention selects medical pure titanium or titanic alloy machining to become dentistry implant, and adopt constant voltage DC anode oxidation process to generate titanium oxide nanotubes thin film in the oxidation of dentistry implant surface in situ, then the nano-tube film adopting electrochemical means to cause generation comes off completely from matrix surface, obtains the dentistry implant that surface is honeycomb nano-pattern.
Exemplarily, the method for the above-mentioned dentistry implant of preparation of the present invention can adopt following steps.
(1) preparation of dentistry implant matrix
Select titanio material (such as medical pure titanium or titanium alloy) to be processed into dentistry implant matrix, the conventional processing method that can adopt, does not describe in detail at this, as long as should be understood that the processing method that can obtain dentistry implant matrix is all contained in the present invention.Then surface finish, cleaning pretreatment are carried out to dentistry implant.Similarly, the polishing of titanio material and cleaning treatment are not particularly limited, known method can be adopted, and this pretreatment neither be essential to the invention.The surface topography of pretreated dentistry implant can see Fig. 1, and from figure, dental implant surface does not have obvious micro structure.
(2) preparation of anodic oxidation electrolyte
The electrolyte adopted can be the ethylene glycol solution of ammonium fluoride, and containing a small amount of water, the mass percent of ammonium fluoride wherein can be 0.1 ~ 1.0%, and the percent by volume of water can be 1.0 ~ 10%.Such as, can adopt containing 0.25wt% ammonium fluoride, the ethylene glycol solution of 1vol% water is as electrolyte.
(3) anodic oxidation
Electrolysis mode is adopted to carry out anodized to dentistry implant matrix.With dentistry implant matrix for anode, and negative electrode is not particularly limited, such as, can adopt graphite electrode or platinum plate electrode, puts into the electrolyte that step (2) prepares and carries out electrolysis.Preferred employing constant voltage DC mode carries out electrolysis.Running voltage can be 20 ~ 80V, and oxidization time can be 1 ~ 96 hour, and reaction temperature can be room temperature.In a preferred example, running voltage is 40 ~ 60V, and oxidization time is 1 ~ 3 hour, and such as running voltage is 60V, and oxidization time is 1 hour.By the control of reaction condition, the pattern of titanium oxide nanotubes thin film, size etc. can be regulated and controled.By anodic oxidation, can be oxidized the surface in situ of dentistry implant matrix, thus obtained surface is formed with the titanio material dentistry implant of titanium oxide nanotubes thin film.The surface topography map of this titanium oxide nanotubes thin film can see Fig. 2, from figure, and the nanotube pattern of dentistry implant surface presentation rule.
(4) preparation of the electrolyte of electrochemical means demoulding
Taking water as solvent, is preferably solvent with deionized water, the dilution heat of sulfuric acid of configuration 0.5 ~ 2mol/L, the dilution heat of sulfuric acid of such as 1mol/L.
(5) electrochemical means demoulding
The nano-tube film using electrochemical means to cause generation comes off from matrix surface.Be formed with the titanio material dentistry implant of titanium oxide nanotubes thin film for negative electrode with surface, and anode is not particularly limited, such as, can adopt graphite electrode or platinum plate electrode, puts into the electrolyte that step (4) prepares and carry out electrolysis.Preferred employing constant voltage DC mode carries out electrolysis.Running voltage can be 2 ~ 5V, such as, be 5V, can be 3 ~ 10 minutes conduction time, and be such as 3 minutes, reaction temperature can be room temperature.By this one-step electrolysis, the titanium oxide nanotubes thin film on dentistry implant surface comes off from matrix surface, titanio material surface presentation honeycomb nano-titanium oxide rete after coming off, thus form honeycomb nanotopography on dentistry implant surface, namely obtain dentistry implant of the present invention.Fig. 3 illustrates the surface topography map of the dentistry implant of the present invention's example, can observe the honeycomb nanotopography of described dentistry implant surface formation from the figure of enlargement ratio step by step wherein.Again, Fig. 4 illustrate the dentistry implant surface honeycomb nano-pattern thin layer of the present invention's example through photoelectron spectroscopy detect obtain titanium, oxygen content is with depth profile curve chart, honeycomb nano-pattern chemistry consists of titanium oxide as can be seen from Figure, surface titanium (Ti): oxygen (O) ratio is 1:2, increase with the degree of depth, oxygen content reduces gradually, and superficial oxidation titanium thickness is about 25 ~ 35nm.It can thus be appreciated that the oxygen content of the nano oxidized titanium layer of honeycomb increases with thicknesses of layers and successively decreases, and transits to described titanio material gradually.And illustrate that nano-pattern rete is very thin, with matrix without obvious layering, bond strength is high.
< biological activity test >
Choose pure titanium as a control group, dentistry implant of the present invention is experimental group, by rat bone marrow mesenchymal stem cells kind at sample surfaces, at the CO of humidity
2cultivate at 37 DEG C in incubator.
Cultivate the nucleus after 4 hours and cytoskeleton fluorescence staining picture as shown in Figure 5, wherein scheme nucleus and cytoskeleton fluorescence staining picture that a-1 and b-1 is matched group, figure a-2 and b-2 is nucleus and the cytoskeleton fluorescence staining picture of experimental group.Contrast with the nuclear targeting picture of figure a-1 and b-1, the cell quantity that can be observed the adhesion of nano-pattern dental implant surface is more.Can find from figure a-2 and b-2, nano-pattern implant surface cell has obvious stretching form and more filopodia stretches, and illustrates that honeycomb nano-pattern pattern can stimulate the adhesion of mesenchymal stem cells MSCs and the growth of migration and filopodia.
Cultivate the alkaline phosphatase activities result of 7 days as shown in Figure 6.Alkali phosphatase is the product of cell osteogenic differentiation process, is usually used in the osteogenic activity that cell is described.Visible in figure, through the cultivation of 7 days, the alkaline phosphatase activities of nano-pattern implant surface cell was significantly higher than pure titanium matched group, shows that nanotopography is conducive to the Osteoblast Differentiation of cell.
Cultivate the gene pyramiding enzyme chain reaction analysis result of the Bone Gla protein (OCN) of 7 days, osteopontin (OPN), transcription factor (Runx2) and bone morphogenetic protein (BMP2) as shown in Figure 7.OCN, OPN, Runx2 and BMP2 are the important marker of cell osteogenic differentiation process, can be used for the Osteoblast Differentiation characterizing cell.The four indices showing nano-pattern experimental group in figure is all significantly higher than pure titanium matched group, describes the Osteoblast Differentiation ability that nano-pattern implantation body has good inducing bone mesenchymal stem cell.
As from the foregoing, the dental implant surface after PROCESS FOR TREATMENT of the present invention is a kind of surface with honeycomb nano-pattern, it is characterized by very thin nanometer rete, presents honeycomb regular pattern.The nanostructured of rule effectively can strengthen the expression of the adhesion of stem cell at implant surfaces of cultivation, alkaline phosphatase activities and relevant osteogenesis gene, embodies good bone to induction ability, thus improves long-time stability and the success rate of dentistry implant.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The concrete concentration of following example, voltage, time etc. are also only examples in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
(1) pure titanium is selected to be processed into dentistry implant;
(2) by after implant surface polishing, use acetone, ethanol and deionized water ultrasonic cleaning 30 minutes successively, obtain clean uniform outer surface;
(3) anodic oxidation electrolyte is prepared: ethylene glycol is solvent, prepares the ethylene glycol solution of 0.25% ammonium fluoride and 1% pure water;
(4) anodizing prepares regular titanium oxide nanotubes thin film: adopt constant voltage DC anodizing technology, dentistry implant is anode, and graphite electrode or platinum plate electrode are negative electrode, puts into the electrolyte of previous step preparation; Running voltage is 50V, and oxidization time is 2 hours, and reaction temperature is room temperature;
(5) electrolyte of electrochemical means demoulding is prepared: deionized water is solvent, and compound concentration is the dilution heat of sulfuric acid of 1mol/L;
(6) nano-tube film that Applied Electrochemistry mode causes generation comes off completely from matrix.Constant voltage DC mode, implantation body is negative electrode, and graphite electrode or platinum plate electrode are anode, and put into the electrolyte of previous step preparation, concrete technology parameter is: voltage is 5V, and conduction time is 5 minutes, and reaction temperature is room temperature;
(7) clean, after drying, dentistry implant of the present invention can be obtained.
The dentistry implant surface topography map of Fig. 1 for obtaining through step (2).From figure, dental implant surface does not have obvious micro structure;
Fig. 2 is the titanium oxide nanotubes film surface appearance figure obtained through step (4).Through anodized, dental implant surface presents the nanotube pattern of rule;
Fig. 3 is the final dentistry implant surface topography map obtained.Through amplifying step by step, the honeycomb nano-pattern pattern on dentistry implant surface can be observed;
Fig. 4 is that dentistry implant surface honeycomb nano-pattern film surface photoelectron spectroscopy detects the titanium obtained, and oxygen content is with depth profile curve chart.Abscissa is the degree of depth, and vertical coordinate is atom percentage concentration.Honeycomb nano-pattern chemistry consists of titanium oxide as can be seen from Figure, surperficial titanium (Ti): oxygen (O) ratio is 1:2, and increase with the degree of depth, oxygen content reduces gradually, and superficial oxidation titanium thickness is about 28nm.Illustrate that nano-pattern rete is very thin, high with substrate combinating strength.
Carry out biological activity test by method mentioned above, test result is see Fig. 5,6,7:
Fig. 5 is nucleus and the cytoskeleton fluorescence staining picture that the rat bone marrow mesenchymal stem cells of pure titanium matched group and nano-pattern tooth implant experimental group is cultivated 4 hours.The nuclear targeting picture of comparison diagram a-1 and b-1, the cell quantity that can be observed the adhesion of nano-pattern dental implant surface is more.Can find from figure a-2 and b-2, nano-pattern implant surface cell has obvious stretching form and more filopodia stretches, and illustrates that honeycomb nano-pattern pattern can stimulate the adhesion of mesenchymal stem cells MSCs and the growth of migration and filopodia;
Fig. 6 is the alkaline phosphatase activities result that the rat bone marrow mesenchymal stem cells of pure titanium matched group and nano-pattern tooth implant experimental group is cultivated 7 days.Alkali phosphatase is the product of cell osteogenic differentiation process, is usually used in the osteogenic activity that cell is described.Visible in figure, through the cultivation of 7 days, the alkaline phosphatase activities of nano-pattern implant surface cell was significantly higher than pure titanium matched group, shows that nanotopography is conducive to the Osteoblast Differentiation of cell;
Fig. 7 is the gene pyramiding enzyme chain reaction analysis result of Bone Gla protein (OCN), osteopontin (OPN), transcription factor (Runx2) and the bone morphogenetic protein (BMP2) that the rat bone marrow mesenchymal stem cells of pure titanium matched group and nano-pattern tooth implant experimental group is cultivated 7 days.OCN, OPN, Runx2 and BMP2 are the important marker of cell osteogenic differentiation process, can be used for the Osteoblast Differentiation characterizing cell.The four indices showing nano-pattern experimental group in figure is all significantly higher than pure titanium matched group, describes the Osteoblast Differentiation ability that nano-pattern implantation body has good inducing bone mesenchymal stem cell.
Embodiment 2
(1) medical titanium is selected to be processed into dentistry implant;
(2) by after implant surface polishing, use acetone, ethanol and deionized water ultrasonic cleaning 30 minutes successively, obtain clean uniform outer surface;
(3) anodic oxidation electrolyte is prepared: ethylene glycol is solvent, prepares the ethylene glycol solution of 0.25% ammonium fluoride and 1% pure water;
(4) anodizing prepares regular titanium oxide nanotubes thin film: adopt constant voltage DC anodizing technology, dentistry implant is anode, and graphite electrode or platinum plate electrode are negative electrode, puts into the electrolyte of previous step preparation; Running voltage is 60V, and oxidization time is 1 hour, and reaction temperature is room temperature;
(5) electrolyte of electrochemical means demoulding is prepared: deionized water is solvent, and compound concentration is the dilution heat of sulfuric acid of 1mol/L;
(6) nano-tube film that Applied Electrochemistry mode causes generation comes off completely from matrix.Constant voltage DC mode, implantation body is negative electrode, and graphite electrode or platinum plate electrode are anode, and put into the electrolyte of previous step preparation, concrete technology parameter is: voltage is 5V, and conduction time is 3 minutes, and reaction temperature is room temperature;
(7) clean, after drying, tooth implant of the present invention can be obtained.
Embodiment 3
(1) medical titanium is selected to be processed into dentistry implant;
(2) by after implant surface polishing, use acetone, ethanol and deionized water ultrasonic cleaning 30 minutes successively, obtain clean uniform outer surface;
(3) anodic oxidation electrolyte is prepared: ethylene glycol is solvent, prepares the ethylene glycol solution of 0.25% ammonium fluoride and 1% pure water;
(4) anodizing prepares regular titanium oxide nanotubes thin film: adopt constant voltage DC anodizing technology, dentistry implant is anode, and graphite electrode or platinum plate electrode are negative electrode, puts into the electrolyte of previous step preparation; Running voltage is 75V, and oxidization time is 1 hour, and reaction temperature is room temperature;
(5) electrolyte of electrochemical means demoulding is prepared: deionized water is solvent, and compound concentration is the dilution heat of sulfuric acid of 1mol/L;
(6) nano-tube film that Applied Electrochemistry mode causes generation comes off completely from matrix.Constant voltage DC mode, implantation body is negative electrode, and graphite electrode or platinum plate electrode are anode, and put into the electrolyte of previous step preparation, concrete technology parameter is: voltage is 3V, and conduction time is 3 minutes, and reaction temperature is room temperature;
(7) clean, after drying, tooth implant of the present invention can be obtained.
Tooth implant prepared by the present invention has very thin nano surface rete, presents honeycomb regular pattern.The nanostructured of rule effectively can strengthen the expression of mesenchymal stem cells MSCs at the adhesion of implant surface, alkaline phosphatase activities and Bone formation-related gene, embody excellent bone to induction ability, thus improve long-time stability and the success rate of dentistry implant, dentistry implant Material Field can be applied to.
Claims (8)
1. prepare the method for dentistry implant for one kind, it is characterized in that, the honeycomb nano-titanium oxide rete that described dentistry implant comprises titanio material and surface in situ formation thereof causes described dentistry implant surface to form honeycomb nanotopography, the oxygen content of the nano oxidized titanium layer of wherein said honeycomb increases with thicknesses of layers and successively decreases, transit to described titanio material gradually, described method comprises:
(1) anodized is carried out to be oxidized at surface in situ to titanio material dentistry implant, thus obtained surface is formed with the titanio material dentistry implant of titanium oxide nanotubes thin film; And
(2) the titanio material dentistry implant being formed with titanium oxide nanotubes thin film with described surface comes off from matrix surface to make described titanium oxide nanotubes thin film for negative electrode carries out electrolysis, thus obtained surface is the dentistry implant of honeycomb nano-titanium oxide rete.
2. method according to claim 1, is characterized in that the thickness of described honeycomb nano-titanium oxide rete is 25 ~ 35nm.
3. method according to claim 1, is characterized in that, described titanio material is medical titanium or titanium alloy.
4. method according to claim 1, is characterized in that, the electrolyte that described anodic oxidation adopts is the ethylene glycol solution containing 0.1 ~ 1.0wt% ammonium fluoride and 1 ~ 10vol% water.
5. method according to claim 1, is characterized in that, described anodized adopts constant voltage DC mode, and running voltage is 20 ~ 80V, and oxidization time is 1 ~ 96 hour, and reaction temperature is room temperature.
6. method according to claim 5, is characterized in that, the running voltage of described anodized is 40 ~ 60V, and oxidization time is 1 ~ 3 hour.
7. method according to claim 1, is characterized in that, in step (2), described electrolysis adopts constant voltage DC mode, and voltage is 2 ~ 5V, and conduction time is 3 ~ 10 minutes, and reaction temperature is room temperature.
8. the method according to any one of claim 4 to 7, is characterized in that, in step (2), the electrolyte that described electrolysis adopts is the dilution heat of sulfuric acid of 0.5 ~ 2mol/L.
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| CN109485459B (en) * | 2018-12-12 | 2023-09-05 | 中国人民解放军总医院第八医学中心 | Zirconium dioxide nanotube film coating plated on surface of zirconium oxide ceramic, and preparation method and application thereof |
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