CN105420786A - Preparation method for nano-sodium silicotitanate/titanium dioxide bio-coatings on titanium surfaces - Google Patents
Preparation method for nano-sodium silicotitanate/titanium dioxide bio-coatings on titanium surfaces Download PDFInfo
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- CN105420786A CN105420786A CN201510810386.7A CN201510810386A CN105420786A CN 105420786 A CN105420786 A CN 105420786A CN 201510810386 A CN201510810386 A CN 201510810386A CN 105420786 A CN105420786 A CN 105420786A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/06—Coatings containing a mixture of two or more compounds
Abstract
The invention provides a preparation method for nano-sodium silicotitanate/titanium dioxide bio-coatings on titanium surfaces. The preparation method specifically comprises the following steps of (1) taking an aqueous solution of 0.2M acetate and 0.02M beta-glycerophosphate as an electrolyte, taking titanium and the alloys thereof as an anode, taking stainless steel as a cathode, and carrying out micro-arc oxidation treatment by virtue of a pulse power supply; and (2) taking the mixed solution of soluble silicate and strong base as a reaction solution, and carrying out hydro-thermal treatment on samples subjected to the micro-arc oxidation so as to obtain the nano-sodium silicotitanate/titanium dioxide bio-coatings. According to the preparation, the sodium silicotitanate/titanium dioxide biological composite coatings with nano-fibre, nano-needle and nano-sheet sodium silicotitanate having controllable geometrical configuration, with controllable contents and with high coating bonding strengths having critical load values Lc of 15-30 N can be formed on the surfaces of titanium and the alloys thereof.
Description
Technical field
The present invention relates to titanium and titanium alloys field of surface treatment, be specifically related to a kind of preparation method of titanium nano surface silicon sodium titanate/titanium dioxide biological coating.
Background technology
Titanium and titanium alloys has good biocompatibility and machining property is widely used in bone tissue restoration and replacement, but titanium is bio-inert material, cannot with osseous tissue Chemical bond, do not promote the ability that new bone tissue is formed yet, need to carry out surface biological activation modification.Osseous tissue is primarily of collegen filament and be filled in fibrous bundle and intercellular matrix composition, and in nanofiber form, skeletonization relevant cell is to the response of this structural configuration in uniqueness.
Research shows, the yardstick of nanofiber, spacing and orientation be front or the negative impact attachment of cell, functional expression consumingly, even bio-inert material (as polymkeric substance), certain three-dimensional manometer fibre network also significantly can promote scleroblast attachment, breeding, genetic expression and organization formation.Experiment shows, sodium titanate nanofiber can promote osteoblastic increment, differentiation to a certain extent, improves the new bone formation ability on its surface.Titanium alloy is after hot alkali treatment, and surface can grow sodium titanate nanofiber layer, but this coating can not be firmly attached on titanium alloy substrate, and adopt scratch method evaluated for film film-substrate binding strength, the critical load that coating is peeled off is less than 5mN.Differential arc oxidation is a kind of nonlinear surface treatment process, can obtain the coating of porous, high bond strength on titanium and titanium alloys surface.
In addition, Si, as a kind of element maintaining human normal vital movement, is promoting to have vital role in the regeneration of osseous tissue, healing.Therefore, if build nanofiber silicon sodium titanate/titanium dioxide bioactive coating on differential arc oxidation coating, then can realize promoting that the early stage titanium implant of implantation and host bone form synostosis simultaneously, meet the mechanical property requirements of implant surface coating.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of high preparation method in conjunction with strong degree nano-silicon sodium titanate/titanium dioxide biological coating, improve the integrative biology performance on titanium and titanium alloys surface.
To achieve these goals, technical scheme of the present invention is:
A kind of preparation method of titanium nano surface silicon sodium titanate/titanium dioxide biological coating, first, with the β of the acetate of 0.2M, 0.02M-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, differential arc oxidation process is carried out to titanium and titanium alloys, obtain equally distributed microporous coat, wherein micro-pore diameter is 1 ~ 2 μm; Secondly, with soluble silicate, highly basic mixing solutions for reaction solution, hydrothermal treatment consists is carried out to the sample through differential arc oxidation, grows nanofiber, nanoneedle or nanometer sheet at coatingsurface.
Further, during differential arc oxidation process, pulsed voltage 300V-480V, frequency 50-500Hz, dutycycle 7.5-26%, treatment time 1-3min.
Further, temperature of reaction 150-250 DEG C during hydrothermal treatment consists, time 4-24h.
Further, acetate used is the mixing solutions of zinc acetate or zinc acetate and lime acetate.
Further, described silicate is that water glass, potassium silicate are wherein a kind of or it is composite.
Further, described highly basic is that sodium hydroxide or potassium hydroxide are wherein a kind of or it is composite.
Further, in water-heat process, strong base concentrations is 0.5M-2M; Silicate concentration 0.05M-0.2M.
The present invention for electrolytic solution, carries out differential arc oxidation process to titanium and titanium alloys with acetate, β-Phosphoric acid glycerol esters disodium salt aqueous solution, obtains the porous TiO containing Zn after process
2ceramic layer; Then, with the soluble silicate of concentration, highly basic mixing solutions for reaction solution, carry out hydrothermal treatment consists, the composite film obtained to the sample through differential arc oxidation, the composite film thickness surface silicone content of gained is 0.5-4.6wt%; Internal layer is poriferous titanium dioxide, adopts scratch method survey film substrate bond strength Lc value to be 15 ~ 30N, and coating is firmly attached on titanium alloy substrate, high with titanium or titanium alloy bonding strength, improves the integrative biology performance on titanium and titanium alloys surface.
The present invention also tool has the following advantages:
1. differential arc oxidation of the present invention, hydrothermal method are easy to control, and micro-arc oxidation electrolyte, hydro-thermal reaction liquid composition are simple, process stabilizing.
2. the thicknesses of layers adopting the present invention to obtain is 5 ~ 20 μm, film thickness can be made to increase further as required by prolongation differential arc oxidation, hydrothermal treatment process; Coatingsurface silicone content can be made to raise further or reduce by adjustment hydrothermal process; Surface and section SEM pattern photo display rete upper strata are nanofiber, nanoneedle or nano-sheet silicon sodium titanate, are porous TiO between silicon sodium titanate and titanium base
2transition layer.
Accompanying drawing explanation
Fig. 1 (a) is the XRD figure spectrum of coating prepared by the embodiment of the present invention 2
Fig. 2 (a) is the SEM photo of coating prepared by the embodiment of the present invention 2
Fig. 2 (b) is the SEM photo of coating prepared by the embodiment of the present invention 3
Fig. 3 (a) is the sectional drawing of the embodiment of the present invention 2 differential arc oxidation
Fig. 3 (b) is the sectional drawing after the embodiment of the present invention 2 hydro-thermal
Fig. 3 (c) is the cut figure of the embodiment of the present invention 2 differential arc oxidation
Fig. 3 (d) is the cut figure after the embodiment of the present invention 3 hydro-thermal
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
The preparation method of titanium nano surface silicon sodium titanate/titanium dioxide biological coating of the present invention:
First, with 0.2M acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 380V-480V, frequency 50-500Hz, dutycycle 7.5-26%, maintain electrolyte temperature at about 25 DEG C, treatment time 1-3min.The porous TiO containing Zn is obtained after process
2ceramic layer.
Then, with the soluble silicate of 0.05M-0.2M, 0.5M-2M highly basic mixing solutions for reaction solution, hydrothermal treatment consists is carried out, temperature of reaction 150-250 DEG C to the sample through differential arc oxidation, time 4-24h.The composite film thickness of gained is 5 ~ 20 μm, and top layer is nanofiber, nanoneedle or nano-sheet silicon sodium titanate, and surface silicon content is 0.5-4.6wt%; Internal layer is poriferous titanium dioxide, scratch method survey film substrate bond strength Lc value is 15 ~ 30N.
Embodiment 1:
The first step: (1) with 0.2M zinc acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 480V, frequency 500Hz, dutycycle 7.5%, maintain electrolyte temperature at about 25 DEG C, treatment time 3min; Or (2) with 0.1M zinc acetate, 0.1M lime acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 480V, frequency 500Hz, dutycycle 7.5%, maintain electrolyte temperature at about 25 DEG C, treatment time 3min.The porous TiO containing Zn is obtained after process
2ceramic layer.
Second step: (1) is with 0.5MNaOH, 0.05MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 200 DEG C, and the time is 10h; Or (2) with 0.5MKOH, 0.05MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 200 DEG C, and the time is 10h; Again or (3) with 0.5MNaOH, 0.05MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 200 DEG C, and the time is 10h.Obtain high bond strength nano-sheet silicon sodium titanate/titanium dioxide bioactive ceramic layer.
Embodiment 2:
The process of the first step differential arc oxidation is identical with embodiment 1.
Second step: (1) is with 1MNaOH, 0.05MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 220 DEG C, and the time is 24h; Or (2) with 1MKOH, 0.05MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 220 DEG C, and the time is 24h; Again or (3) with 1MNaOH, 0.05MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 220 DEG C, and the time is 24h.Obtain high bond strength nano whiskers silicon sodium titanate/titanium dioxide bioactive ceramic layer.
Shared by Fig. 1 (a) Si, weight percent is 0.66, obtains the needle-like rete that spacing is 600 ran as shown in Fig. 2 (a).
As Fig. 3 (a), 3 (b) are respectively the sectional drawing after the sectional drawing of differential arc oxidation and hydro-thermal, micro-arc oxidation films layer thickness is approximately 10 μm, and can find out and adopt two-step approach to obtain special structure, thicknesses of layers slightly reduces.
As the cut figure after Fig. 3 (c), 3 (d) the cut figure that is differential arc oxidation and hydro-thermal, after showing hydro-thermal, its bonding strength is still very high, relative to differential arc oxidation not too large change.
Embodiment 3:
The process of the first step differential arc oxidation is identical with embodiment 1.
Second step: (1) is with 1MNaOH, 0.2MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 220 DEG C, and the time is 24h; Or (2) with 1MKOH, 0.2MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 220 DEG C, and the time is 24h; Again or (3) with 1MNaOH, 0.2MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 220 DEG C, and the time is 24h.Obtain high bond strength nano-sheet silicon sodium titanate/titanium dioxide bioactive ceramic layer.
As shown in Fig. 2 (b), obtain sheet rete, Si weight percent contained by it is 1.99.
Embodiment 4:
The first step: (1) with 0.2M zinc acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 300V, frequency 250Hz, dutycycle 18%, maintain electrolyte temperature at about 25 DEG C, treatment time 2.0min; Or (2) with 0.1M zinc acetate, 0.1M lime acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 300V, frequency 250Hz, dutycycle 18%, maintain electrolyte temperature at about 25 DEG C, treatment time 2.0min.The porous TiO containing Zn is obtained after process
2ceramic layer.
Second step: (1) is with 1.5MNaOH, 0.5MKOH, 0.10MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 250 DEG C, and the time is 4h; Or (2) with 0.5MNaOH, 1.5MKOH, 0.10MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 250 DEG C, and the time is 4h; Again or (3) with 2.0MNaOH, 0.05MK
2siO
3, 0.05MNa
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 250 DEG C, and the time is 4h.Obtain high bond strength nano-sheet silicon sodium titanate/titanium dioxide bioactive ceramic layer.
Embodiment 5:
The first step: (1) with 0.2M zinc acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 400V, frequency 50Hz, dutycycle 26%, maintain electrolyte temperature at about 25 DEG C, treatment time 1.0min; Or (2) with 0.1M zinc acetate, 0.1M lime acetate, 0.02M β-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, pure titanium is anode, stainless steel is negative electrode, the pulse power is adopted to carry out differential arc oxidation process under the condition of voltage 400V, frequency 50Hz, dutycycle 26%, maintain electrolyte temperature at about 25 DEG C, treatment time 1.0min.The porous TiO containing Zn is obtained after process
2ceramic layer.
Second step: (1) is with 1.2MNaOH, 0.06MNa
2siO
3, 0.06MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 150 DEG C, and the time is 20h; Or (2) with 1.2MKOH, 0.06MNa
2siO
3, 0.06MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 150 DEG C, and the time is 20h; Again or (3) with 0.6MNaOH, 0.6MKOH, 0.06MNa
2siO
3, 0.06MK
2siO
3mixing solutions is reaction solution, carries out hydrothermal treatment consists to the sample through differential arc oxidation, temperature of reaction 150 DEG C, and the time is 20h; .Obtain high bond strength nano-sheet silicon sodium titanate/titanium dioxide bioactive ceramic layer.
Claims (7)
1. the preparation method of titanium nano surface silicon sodium titanate/titanium dioxide biological coating, it is characterized in that: first, with the β of the acetate of 0.2M, 0.02M-Phosphoric acid glycerol esters disodium salt aqueous solution for electrolytic solution, differential arc oxidation process is carried out to titanium and titanium alloys, obtain equally distributed microporous coat, wherein micro-pore diameter is 1 ~ 2 μm; Secondly, with soluble silicate, highly basic mixing solutions for reaction solution, hydrothermal treatment consists is carried out to the sample through differential arc oxidation, grows nanofiber, nanoneedle or nanometer sheet at coatingsurface.
2. method according to claim 1, is characterized in that: during differential arc oxidation process, pulsed voltage 300V-480V, frequency 50-500Hz, dutycycle 7.5-26%, treatment time 1-3min.
3. method according to claim 1, is characterized in that: temperature of reaction 150-250 DEG C during hydrothermal treatment consists, time 4-24h.
4. method according to claim 1, is characterized in that: acetate used is the mixing solutions of zinc acetate or zinc acetate and lime acetate.
5. method according to claim 1, is characterized in that: described silicate is that water glass, potassium silicate are wherein a kind of or it is composite.
6. method according to claim 1, is characterized in that: described highly basic is that sodium hydroxide or potassium hydroxide are wherein a kind of or it is composite.
7. method according to claim 1, is characterized in that: in water-heat process, strong base concentrations is 0.5M-2M; Silicate concentration 0.05M-0.2M.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637348A (en) * | 2016-09-23 | 2017-05-10 | 西安交通大学 | Preparation method of titanium surface ferrotitanium stone type oxide/ titanium dioxide bio-coating |
| CN106637347A (en) * | 2016-09-08 | 2017-05-10 | 西安交通大学 | Preparation method of tin dioxide electroactive biological ceramic coating composited on surface of micro-arc oxidation titanium |
| CN108517517A (en) * | 2018-04-16 | 2018-09-11 | 江苏科技大学 | A method of preparing titanium phosphate zinc chemical conversion film on titanium surface |
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| CN102146577A (en) * | 2010-02-05 | 2011-08-10 | 佳木斯大学 | Pure-titanium metal surface micro-arc oxidation treatment electrolyte and antimicrobial bioactive coating preparation method thereof |
| CN102371005A (en) * | 2010-08-13 | 2012-03-14 | 中国科学院上海硅酸盐研究所 | Zinc-doped porous nano-titanium oxide coating and its preparation method |
| CN104498915A (en) * | 2014-12-25 | 2015-04-08 | 西安交通大学 | Preparation method of nanofiber-strip-shaped calcium silicate/titanium dioxide bioactive coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102146577A (en) * | 2010-02-05 | 2011-08-10 | 佳木斯大学 | Pure-titanium metal surface micro-arc oxidation treatment electrolyte and antimicrobial bioactive coating preparation method thereof |
| CN102371005A (en) * | 2010-08-13 | 2012-03-14 | 中国科学院上海硅酸盐研究所 | Zinc-doped porous nano-titanium oxide coating and its preparation method |
| CN104498915A (en) * | 2014-12-25 | 2015-04-08 | 西安交通大学 | Preparation method of nanofiber-strip-shaped calcium silicate/titanium dioxide bioactive coating |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637347A (en) * | 2016-09-08 | 2017-05-10 | 西安交通大学 | Preparation method of tin dioxide electroactive biological ceramic coating composited on surface of micro-arc oxidation titanium |
| CN106637347B (en) * | 2016-09-08 | 2019-03-01 | 西安交通大学 | A kind of preparation method of the electroactive bio-ceramic coating of differential arc oxidation titanium surface recombination stannic oxide |
| CN106637348A (en) * | 2016-09-23 | 2017-05-10 | 西安交通大学 | Preparation method of titanium surface ferrotitanium stone type oxide/ titanium dioxide bio-coating |
| CN106637348B (en) * | 2016-09-23 | 2019-02-05 | 西安交通大学 | Titanium surface ferrotitanium stone-type oxide/titanium dioxide biological coating preparation method |
| CN108517517A (en) * | 2018-04-16 | 2018-09-11 | 江苏科技大学 | A method of preparing titanium phosphate zinc chemical conversion film on titanium surface |
| CN108517517B (en) * | 2018-04-16 | 2019-09-20 | 江苏科技大学 | A method of titanium phosphate zinc chemical conversion film is prepared on titanium surface |
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