CN103536371A - Dental implant and preparation method thereof - Google Patents
Dental implant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a dental implant and a preparation method thereof. The dental implant comprises a titanium substrate and a honeycomb nano titanium oxide film layer, wherein the honeycomb nano titanium oxide film layer is formed on the surface of the titanium substrate in situ to form a honeycomb nano shape on the surface of the dental implant; the oxygen content of the honeycomb nano titanium oxide film layer is reduced with increase in thickness of the film layer and is gradually transited to the titanium substrate. The honeycomb nano titanium oxide film layer is formed on the surface of the titanium substrate in situ so as to form the honeycomb nano shape on the surface of the dental implant, wherein the honeycomb nano titanium oxide film layer is thin, has better strength, is not obviously layered with the titanium substrate and is firm in combination, and the regular nanostructure can effectively reinforce the adhesion of mesenchymal stem cells to the surface of the implant and the expression of alkaline phosphatase activities and osteogenesis-related genes, and shows superior osteogenic differentiation induction capacity, so that the long-term stability and the success rate of the dental implant are improved.
Description
Technical field
The present invention relates to dentistry implant Material Field, particularly a kind of 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.Due to dentistry planting technology, be one of important method of repairing defect of dentition or disappearance, the development of dentistry implant is paid close attention to.To implant surface, modification is proved to be a kind of method that implantation body's success rate was integrated and improved to effective promotion bone, research simultaneously shows the nanostructured of implant surface, as nanotube-shaped surface topography can promote osteoblastic adhering to and functional expression, adhesion that can also be to people's Gingival Fibroblasts, propagation and albumen, gene expression has significant facilitation (Acta Biomaterialia2011,7 (1): 2686-2696.).Therefore, tooth implant being carried out to making Nano surface modification is the effective means that further improves implantation body's effect.
Yet, dentistry implant is implanted behind oral cavity because of mastication, the stress situation of bearing is complicated, active force is large, inhomogeneous and the long action time in force part, nano coating prepared by implant surface or thin film, because the effect of this irregular stress can produce the dissolving of breaking and come off, tend to cause implantation body to become flexible and lost efficacy, and finally cause bone to integrate unsuccessfully.
Summary of the invention
Low in order to solve the film strength of dental implant surface nano modification coating in prior art or thin film, film and substrate combinating strength are not good, the problems such as stress fatigue damage, the object of the present invention is to provide a kind of surface is the dentistry implant and preparation method thereof of the honeycomb nano-titanium oxide rete of growth in situ, thereby strengthen film strength and film and substrate combinating strength, and strengthen mesenchymal stem cells MSCs in the adhesion of implant surface, the expression of alkaline phosphatase activities and Bone formation-related gene, strengthen bone to induction ability, thereby 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, described dentistry implant comprises that the honeycomb nano-titanium oxide rete that titanio material and surface in situ thereof form causes described dentistry implant surface to form honeycomb nanotopography, the nano oxidized titanium layer oxygen content of wherein said honeycomb increases and successively decreases with thicknesses of layers, transits to gradually described titanio material.
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, thereby described dentistry implant is after implanting oral cavity, can bear and compared with the active force of large situation complexity, can not break and dissolving comes off, and the nanostructured of rule can effectively be strengthened mesenchymal stem cells MSCs in the adhesion of implant surface, the expression of alkaline phosphatase activities and Bone formation-related gene, embody good bone to induction ability, thereby 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 of preparing above-mentioned dentistry implant, comprising:
(1) titanio material dentistry implant is carried out to anodized to be oxidized at surface in situ, thereby make the titanio material dentistry implant that surface is formed with titanium oxide nanotubes thin film; And
(2) take titanio material dentistry implant that described surface is formed with titanium oxide nanotubes thin film as negative electrode carries out electrolysis so that described titanium oxide nanotubes thin film comes off from matrix surface, is the dentistry implant of honeycomb nano-titanium oxide rete thereby make surface.
The present invention can obtain the titanium oxide layer of the well-regulated nanostructured of tool (honeycomb) of original position formation by two one-step electrolysis, thereby strengthen film strength and film and substrate combinating strength, and the nanostructured of rule can effectively be strengthened mesenchymal stem cells MSCs in the expression of adhesion, alkaline phosphatase activities and the Bone formation-related gene of implant surface, embody good bone to induction ability, thereby 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 direct current 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 direct current mode, and voltage is 2～5V, and be 3～10 minutes conduction time, and reaction temperature is room temperature.
Preferably, in step (2), the dilution heat of sulfuric acid that the electrolyte that described electrolysis adopts is 0.5～2mol/L.
Step of the present invention is simple, with low cost, can obtain at short notice surface for the dentistry implant of the honeycomb nano-titanium oxide rete of original position formation.
Accompanying drawing explanation
Fig. 1 is pretreated dentistry implant surface topography map in example of the present invention;
Fig. 2 processes through first step constant voltage DC anodizing of the present invention the titanium oxide nanotubes film surface appearance figure that dentistry implant obtains;
Fig. 3 is the surface topography map of the dentistry implant of an example of the present invention, and illustration is the figure of enlargement ratio step by step of pattern pattern;
Fig. 4 is that the titanium, oxygen content of the dentistry implant surface honeycomb nano-pattern thin layer of an example of the present invention is with depth profile curve chart;
Fig. 5 is that rat bone marrow mesenchymal stem cells is cultivated respectively nucleus (1) and cytoskeleton (2) the fluorescence staining picture of 4h on 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 that pure titanium matched group and nano-pattern experimental group surface rat bone marrow mesenchymal stem cells are cultivated Bone Gla protein (OCN), osteopontin (OPN), transcription factor (Runx2) and the bone morphogenetic protein (BMP2) of 7 days.
The specific embodiment
Below in conjunction with accompanying drawing and following embodiment, further illustrate the present invention, should be understood that accompanying drawing and following embodiment are only for the present invention is described, and unrestricted the present invention.
Fig. 3 illustrates the surface topography map of the dentistry implant of an example of the present invention, with reference to Fig. 3, the dentistry implant of an example of the present invention comprises that the honeycomb nano-titanium oxide rete that titanio material and surface in situ thereof form causes described dentistry implant surface to form honeycomb nanotopography.The figure of enlargement ratio step by step from Fig. 3 can observe the honeycomb nanotopography that described dentistry implant surface forms.
The dentistry implant surface honeycomb nano-pattern thin layer that Fig. 4 illustrates an example of the present invention detects the titanium that obtains, oxygen content with depth profile curve chart through photoelectron spectroscopy, honeycomb nano-pattern chemistry consists of titanium oxide as can be seen from Figure, surface titanium (Ti): oxygen (O) ratio is 1:2, with the degree of depth, increase, oxygen content reduces gradually, and top layer titanium oxide thickness is about 25～35nm.Hence one can see that, and the oxygen content of the nano oxidized titanium layer of honeycomb increases and successively decreases with thicknesses of layers, transits to gradually described titanio material.And nano-pattern rete is described as thin as a wafer, without obvious layering, bond strength is high with matrix.
In one example, titanio material can adopt medical titanium or titanium alloy.
The present invention selects medical pure titanium or titanium alloy to be processed into dentistry implant, and adopt constant voltage DC anodizing technique to generate titanium oxide nanotubes thin film in the oxidation of dentistry implant surface in situ, then the nano-tube film that adopts electrochemical means to cause generation comes off completely from matrix surface, and obtaining surface is the dentistry implant of honeycomb nano-pattern.
As example, 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 (for example 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 make dentistry implant matrix is all contained in the present invention.Then dentistry implant is carried out surface finish, cleans pretreatment.Similarly, the polishing of titanio material and cleaning treatment are not particularly limited, can adopt known method, and this pretreatment neither be essential to the invention.The surface topography of pretreated dentistry implant can be referring to Fig. 1, and from scheming, dental implant surface does not have obvious micro structure.
(2) preparation of anodic oxidation electrolyte
The electrolyte adopting can be the ethylene glycol solution of ammonium fluoride, contains a small amount of water, and 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%.For example, can adopt the ammonium fluoride containing 0.25wt%, the ethylene glycol solution of 1vol% water is as electrolyte.
(3) anodic oxidation
Adopt electrolysis mode to carry out anodized to dentistry implant matrix.Take dentistry implant matrix as anode, and negative electrode is not particularly limited, for example, can adopt graphite electrode or platinum plate electrode, and the electrolyte of putting into step (2) preparation carries out electrolysis.Preferably adopt constant voltage direct current mode to carry 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 for example running voltage is 60V, and oxidization time is 1 hour.By the control of reaction condition, can regulate and control pattern, size of titanium oxide nanotubes thin film etc.By anodic oxidation, can be oxidized the surface in situ of dentistry implant matrix, thereby make the titanio material dentistry implant that surface is formed with titanium oxide nanotubes thin film.The surface topography map of this titanium oxide nanotubes thin film can be referring to Fig. 2, and from scheming, dentistry implant surface presents regular nanotube pattern.
(4) preparation of the electrolyte of electrochemical means demoulding
Take water as solvent, preferably take deionized water as solvent, configure the dilution heat of sulfuric acid of 0.5～2mol/L, for example the dilution heat of sulfuric acid of 1mol/L.
(5) electrochemical means demoulding
The nano-tube film that uses electrochemical means to cause generation comes off from matrix surface.The titanio material dentistry implant that surface is formed with titanium oxide nanotubes thin film of take is negative electrode, and anode is not particularly limited, for example, can adopt graphite electrode or platinum plate electrode, and the electrolyte of putting into step (4) preparation carries out electrolysis.Preferably adopt constant voltage direct current mode to carry out electrolysis.Running voltage can be 2～5V, for example, be 5V, can be 3～10 minutes conduction time, for example, be 3 minutes, and 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, after coming off, titanium substrate surface presents honeycomb nano-titanium oxide rete, thereby forms honeycomb nanotopography on dentistry implant surface, obtains dentistry implant of the present invention.Fig. 3 illustrates the surface topography map of the dentistry implant of an example of the present invention, from the figure of enlargement ratio step by step wherein, can observe the honeycomb nanotopography that described dentistry implant surface forms.Again, the dentistry implant surface honeycomb nano-pattern thin layer that Fig. 4 illustrates an example of the present invention detects the titanium that obtains, oxygen content with depth profile curve chart through photoelectron spectroscopy, honeycomb nano-pattern chemistry consists of titanium oxide as can be seen from Figure, surface titanium (Ti): oxygen (O) ratio is 1:2, with the degree of depth, increase, oxygen content reduces gradually, and top layer titanium oxide thickness is about 25～35nm.Hence one can see that, and the oxygen content of the nano oxidized titanium layer of honeycomb increases and successively decreases with thicknesses of layers, transits to gradually described titanio material.And nano-pattern rete is described as thin as a wafer, without obvious layering, bond strength is high with matrix.
< 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 moist CO
2in incubator, at 37 ℃, cultivate.
Cultivate 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 are matched groups, figure a-2 and b-2 are nucleus and the cytoskeleton fluorescence staining picture of experimental group.With the nuclei dyeing chromatic graph sheet contrast of figure a-1 and b-1, the cell quantity that can be observed the adhesion of nano-pattern dental implant surface is more.From figure a-2 and b-2, can find, 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 Osteoblast Differentiation process, is usually used in illustrating the osteogenic activity of cell.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, showed that nanotopography is conducive to the Osteoblast Differentiation of cell.
Cultivate 7 days Bone Gla protein (OCN), osteopontin (OPN), transcription factor (Runx2) and bone morphogenetic protein (BMP2) gene pyramiding enzyme chain reaction analysis result as shown in Figure 7.OCN, OPN, Runx2 and BMP2 are the important marker of cell Osteoblast Differentiation process, can be used for the Osteoblast Differentiation of characterize cells.The four indices that shows nano-pattern experimental group in figure is all significantly higher than pure titanium matched group, has illustrated that nano-pattern implantation body has the Osteoblast Differentiation ability of 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 nanometer rete as thin as a wafer, presents honeycomb regular pattern.The nanostructured of rule can effectively strengthen the stem cell of cultivation in the expression of adhesion, alkaline phosphatase activities and the relevant osteogenesis gene of implant surfaces, embodies good bone to induction ability, thereby improves long-time stability and the success rate of dentistry implant.
Further exemplify embodiment below 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 only also examples in OK range, and those skilled in the art can be done in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
(1) select pure titanium to be processed into dentistry implant;
(2) by after implant surface polishing, use successively acetone, ethanol and deionized water ultrasonic cleaning 30 minutes, obtain clean uniform outer surface;
(3) preparation anodic oxidation electrolyte: ethylene glycol is solvent, prepares the ethylene glycol solution of 0.25% ammonium fluoride and 1% pure water;
(4) anodizing is prepared 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 preparation electrochemical means demoulding: deionized water is solvent, the dilution heat of sulfuric acid that compound concentration is 1mol/L;
(6) nano-tube film that Applied Electrochemistry mode causes generation comes off completely from matrix.Constant voltage direct current mode, implantation body is negative electrode, and graphite electrode or platinum plate electrode are anode, put into the electrolyte of previous step preparation, and concrete technology parameter is: voltage is 5V, and be 5 minutes conduction time, reaction temperature is room temperature;
(7) clean, after being dried, can obtain dentistry implant of the present invention.
The dentistry implant surface topography map of Fig. 1 for obtaining through step (2).From scheming, dental implant surface does not have obvious micro structure;
Fig. 2 is the titanium oxide nanotubes film surface appearance figure obtaining through step (4).Through anodized, dental implant surface presents regular nanotube pattern;
Fig. 3 is the final dentistry implant surface topography map obtaining.Through amplifying step by step, can observe the honeycomb nano-pattern pattern on dentistry implant surface;
Fig. 4 is that dentistry implant surface honeycomb nano-pattern film surface photoelectron spectroscopy detects the titanium obtaining, 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, with the degree of depth, increases, and oxygen content reduces gradually, and top layer titanium oxide thickness is about 28nm.Nano-pattern rete is described as thin as a wafer, high with substrate combinating strength.
By method mentioned above, carry out biological activity test, test result is referring to Fig. 5,6,7:
Fig. 5 is that the rat bone marrow mesenchymal stem cells of pure titanium matched group and nano-pattern tooth implant experimental group is cultivated nucleus and the cytoskeleton fluorescence staining picture of 4 hours.The nuclei dyeing chromatic graph sheet 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.From figure a-2 and b-2, can find, 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 Osteoblast Differentiation process, is usually used in illustrating the osteogenic activity of cell.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, showed that nanotopography is conducive to the Osteoblast Differentiation of cell;
Fig. 7 is the gene pyramiding enzyme chain reaction analysis result that the rat bone marrow mesenchymal stem cells of pure titanium matched group and nano-pattern tooth implant experimental group is cultivated Bone Gla protein (OCN), osteopontin (OPN), transcription factor (Runx2) and the bone morphogenetic protein (BMP2) of 7 days.OCN, OPN, Runx2 and BMP2 are the important marker of cell Osteoblast Differentiation process, can be used for the Osteoblast Differentiation of characterize cells.The four indices that shows nano-pattern experimental group in figure is all significantly higher than pure titanium matched group, has illustrated that nano-pattern implantation body has the Osteoblast Differentiation ability of good inducing bone mesenchymal stem cell.
(1) select medical titanium to be processed into dentistry implant;
(2) by after implant surface polishing, use successively acetone, ethanol and deionized water ultrasonic cleaning 30 minutes, obtain clean uniform outer surface;
(3) preparation anodic oxidation electrolyte: ethylene glycol is solvent, prepares the ethylene glycol solution of 0.25% ammonium fluoride and 1% pure water;
(4) anodizing is prepared 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 preparation electrochemical means demoulding: deionized water is solvent, the dilution heat of sulfuric acid that compound concentration is 1mol/L;
(6) nano-tube film that Applied Electrochemistry mode causes generation comes off completely from matrix.Constant voltage direct current mode, implantation body is negative electrode, and graphite electrode or platinum plate electrode are anode, put into the electrolyte of previous step preparation, and concrete technology parameter is: voltage is 5V, and be 3 minutes conduction time, reaction temperature is room temperature;
(7) clean, after being dried, can obtain tooth implant of the present invention.
(1) select medical titanium to be processed into dentistry implant;
(2) by after implant surface polishing, use successively acetone, ethanol and deionized water ultrasonic cleaning 30 minutes, obtain clean uniform outer surface;
(3) preparation anodic oxidation electrolyte: ethylene glycol is solvent, prepares the ethylene glycol solution of 0.25% ammonium fluoride and 1% pure water;
(4) anodizing is prepared 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 preparation electrochemical means demoulding: deionized water is solvent, the dilution heat of sulfuric acid that compound concentration is 1mol/L;
(6) nano-tube film that Applied Electrochemistry mode causes generation comes off completely from matrix.Constant voltage direct current mode, implantation body is negative electrode, and graphite electrode or platinum plate electrode are anode, put into the electrolyte of previous step preparation, and concrete technology parameter is: voltage is 3V, and be 3 minutes conduction time, reaction temperature is room temperature;
(7) clean, after being dried, can obtain tooth implant of the present invention.
Tooth implant prepared by the present invention has nano surface rete as thin as a wafer, presents honeycomb regular pattern.The nanostructured of rule can effectively be strengthened mesenchymal stem cells MSCs in the expression of adhesion, alkaline phosphatase activities and the Bone formation-related gene of implant surface, embody good bone to induction ability, thereby the long-time stability and the success rate that improve dentistry implant, can be applied to dentistry implant Material Field.
Claims (9)
1. a dentistry implant, it is characterized in that, described dentistry implant comprises that the honeycomb nano-titanium oxide rete that titanio material and surface in situ thereof form causes described dentistry implant surface to form honeycomb nanotopography, the oxygen content of the nano oxidized titanium layer of wherein said honeycomb increases and successively decreases with thicknesses of layers, transits to gradually described titanio material.
2. dentistry implant according to claim 1, is characterized in that, the thickness of described honeycomb nano-titanium oxide rete is 25～35 nm.
3. dentistry implant according to claim 1 and 2, is characterized in that, described titanio material is medical titanium or titanium alloy.
4. a method of preparing the dentistry implant described in any one in claims 1 to 3, is characterized in that, comprising:
(1) titanio material dentistry implant is carried out to anodized to be oxidized at surface in situ, thereby make the titanio material dentistry implant that surface is formed with titanium oxide nanotubes thin film; And
(2) take titanio material dentistry implant that described surface is formed with titanium oxide nanotubes thin film as negative electrode carries out electrolysis so that described titanium oxide nanotubes thin film comes off from matrix surface, is the dentistry implant of honeycomb nano-titanium oxide rete thereby make surface.
5. method according to claim 4, 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.
6. according to the method described in claim 4 or 5, it is characterized in that, described anodized adopts constant voltage direct current mode, and running voltage is 20～80V, and oxidization time is 1～96 hour, and reaction temperature is room temperature.
7. method according to claim 6, is characterized in that, the running voltage of described anodized is 40～60V, and oxidization time is 1～3 hour.
8. according to the method described in any one in claim 4 to 7, it is characterized in that, in step (2), described electrolysis adopts constant voltage direct current mode, and voltage is 2～5V, and be 3～10 minutes conduction time, and reaction temperature is room temperature.
9. according to the method described in any one in claim 4 to 8, it is characterized in that, in step (2), the dilution heat of sulfuric acid that the electrolyte that described electrolysis adopts is 0.5～2mol/L.
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