CN110327487A - Has light-operated antibacterial functions g-C3N4/TiO2Coating and preparation method - Google Patents

Has light-operated antibacterial functions g-C3N4/TiO2Coating and preparation method Download PDF

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CN110327487A
CN110327487A CN201910660038.4A CN201910660038A CN110327487A CN 110327487 A CN110327487 A CN 110327487A CN 201910660038 A CN201910660038 A CN 201910660038A CN 110327487 A CN110327487 A CN 110327487A
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coating
titanium
tio
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preparation
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CN110327487B (en
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饶席
杜陵
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Southwest University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/04Metals or alloys
    • A61L27/06Titanium or titanium alloys
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/30Inorganic materials
    • A61L27/306Other specific inorganic materials not covered by A61L27/303 - A61L27/32
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56Porous materials, e.g. foams or sponges
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

Abstract

The present invention is a kind of light-operated antibacterial functions g-C of tool3N4/TiO2Coating and preparation method, this light-operated antimicrobial coating is by three-dimensional net structure TiO2And its class graphite phase carbon nitride (g-C of surface deposition3N4) composition.The g-C with three-dimensional net structure3N4/TiO2Coating constructs rod-like nano array sodium titanate on its surface by hydrothermal synthesis method in conjunction with titanium or titanium alloy substrate surface, by matrix, is transformed into titanium dioxide using chemical vapour deposition technique and deposits g-C simultaneously3N4It forms.The preparation method comprises the following steps: obtaining the sodium titanate biological coating of rod-like nano array in matrix surface using hydrothermal synthesis method first;It then is transformed into titanium dioxide using high-temperature annealing process, while g-C is deposited in titanium dioxide surface by chemical vapour deposition technique using melamine as raw material3N4, the final g-C that the light-operated antibacterial functions of tool are made3N4/TiO2Coating.

Description

Has light-operated antibacterial functions g-C3N4/TiO2Coating and preparation method
Technical field
The present invention relates to a kind of light-operated antibacterial functions g-C of tool3N4/TiO2Coating and preparation method, more particularly to a kind of choosing Be basis material with titanium and its alloy, using hydrothermal synthesis method its surface controllability growing nano-rod shape array structure metatitanic acid Sodium bio-ceramic coating, by utilizing high-temperature annealing process and chemical vapour deposition technique by sodium titanate nanometer rods in tube furnace Shape array structure is changed into the TiO that surface is deposited with g-C3N4 nanometer sheet2Coating of three-dimensional net structure and preparation method thereof belongs to In biomedical material technology.
Background technique
Titanium or titanium alloy have superior biocompatibility, high-strength tenacity and corrosion resistance, be Present clinical treatment in compared with For the main raw material(s) of common middle and high end surgical implant, artificial tooth planting body, artificial orthopaedics substitute, blood vessel and soft can be used as Organize minimally invasive intervention implant etc..
Titanium or titanium alloy is biologically inert metal material, and the thin and compact titanium oxide passivation layer in surface can prevent phosphate Deposition, and then cause to be difficult to form Integrated implant and synostosis with bone tissue as the implant of matrix using such alloy, finally draw Send out implant failure.
Bacterium living beings usually form bacterial biof iotalm in implant surfaces, so that the surgical procedure of interventional therapy is often with art Middle infection, the patient to undergo surgery are difficult to obtain good result after surgery using antibiotic treatment, eventually lead to implantation Body function failure.
TiO2With good bioactivity, while can promote mutual between titanium-base alloy surface and Human Physiology tissue Effect, enhances the synostosis of implant and bone tissue, and raising is implanted to power.Meanwhile TiO2With certain antibacterial and sterilizing The effect of acting on, broad-spectrum antiseptic can be played in the case where not consuming itself.
g-C3N4Due to its special two-dimensional structure, there is stronger photocatalysis.Under visible light and near infrared light, g-C3N4Light induced electron and photohole can be formed, and further the oxygen in catalytic environment and water form super oxygen group and hydroxyl Free radical finally plays the effect of light-operated antibacterial to destroy the cell membrane of bacterium and lead to its inactivation.
g-C3N4Chemical property itself is stable, nontoxic and pollution-free, almost without cytotoxicity in organism, has good Biocompatibility.
Hydrothermal synthesis method can induce the growth of titanium alloy surface sodium titanate nanostructure in alkaline environment.Studies have shown that The advantageous bone-like apatite stone structure forming core of sodium titanate nanostructure, growth and osteoblastic proliferation with class bone structure, stick and Differentiation.In addition, the specific surface area of material can be greatly improved in the nanostructure with complex three-dimensional stereoscopic features, thus for drug and The storage and release of the biochemical activity factor provide place, enhance the interventional therapeutic effect and functionality of planting body.
Sodium titanate nano bar-shape battle array is constructed in titanium and its alloy surface controllability in Hydroxyapatite Coatings in Alkaline Solution by hydrothermal synthesis method After array structure, utilize high-temperature annealing process and chemical vapour deposition technique by the sodium titanate of titanium and its alloy surface using tube furnace Nano bar-shape array structure is converted into surface and is deposited with g-C3N4The coating of titanium dioxide with three-dimensional net structure to realize light Antibacterial is controlled, shows huge biomedical applications potentiality.However, there is similar three-dimensional net structure using technique preparation G-C3N4/TiO2Structure coating, and utilize g-C3N4And TiO2Material surface antibacterial functions are improved, in bio-medical material technology Field is also rarely reported.In consideration of it, the present invention provides a kind of g-C for having light-operated antibacterial functions3N4/TiO2Coating and its preparation Method.
Summary of the invention
The purpose of the present invention is being directed to the above-mentioned deficiency of Artificial Intervention material, a kind of g- for having light-operated antibacterial functions is proposed C3N4/TiO2Coating and preparation method thereof, and implantation initial stage surface bioactive, cell ability of regulation and control, table can be significantly improved Face anti-microbial property and the coating of multiple beneficial function and preparation method thereof.
Using hydrothermal synthesis method, controllability growth has the sodium titanate biology of nano bar-shape array structure in Hydroxyapatite Coatings in Alkaline Solution Ceramic coating, then surface is converted for sodium titanate by high-temperature annealing process and chemical vapour deposition technique and is deposited with g-C3N4And Coating of titanium dioxide with three-dimensional net structure.Since during hydrothermal synthesis, sodium titanate active layer is in TC4 titanium alloy Matrix surface carries out growth in situ, so that the TiO obtained by high-temperature annealing process2Bio-ceramic coating is in conjunction with metallic matrix Intensity is high, while TiO obtained2Nanostructure is also g-C3N4The ideal template of coating deposition growing.g-C3N4It can lead to simultaneously It crosses chemical vapour deposition technique to be deposited on TC4 titanium alloy substrate surface, to make titanium-base alloy implantation material surface antibacterial Coating is improved with basal body binding force, to guarantee the persistence of the anti-microbial property of coating, and the g-C finally obtained3N4/TiO2 Three-dimensional net structure has good bioactivity and can promote the forming core and deposition growing of apatite layer.Fixed implantation people After body, g-C3N4/TiO2The antibacterial functions of three-dimensional net structure coating are extended, and the wind of fixed superinfection is advantageously reduced It is dangerous.
The present invention is realized especially by following technical scheme:
A kind of light-operated antibacterial functions g-C of tool3N4/TiO2Coating and preparation method, which is characterized in that the light-operated antibacterial function of the tool The g-C of energy3N4/TiO2Coating is by the titanium dioxide with three-dimensional net structure feature in titanium or the growth of titanium alloy material surface Titanium coating and the class graphite phase carbon nitride g-C of its surface chemistry vapor deposition3N4Composition, described has three-dimensional net structure The coating of titanium dioxide and titanium of feature or titanium alloy material surface are firmly combined, using hydrothermal synthesis method in base in Hydroxyapatite Coatings in Alkaline Solution Body surface face controllability grows sodium titanate nanometer stick array structure, and high-temperature annealing process and chemical gaseous phase are then utilized in tube furnace Deposition technique converts surface for sodium titanate nanometer stick array and is deposited with g-C3N4The titanium dioxide with three-dimensional network appearance feature Titanium coating;The g-C of the light-operated antibacterial functions of tool3N4/TiO2The preparation method of coating, includes the following steps:
(1) a kind of titanium is provided or titanium alloy is the bio-medical material of matrix;
(2) provide it is a kind of include sodium hydroxide hydrothermal synthesis alkaline reaction solution;
(3) by titanium or titanium alloy material surface polishing, its surface is pre-processed using high-level oxidation technology, then It is put into the alkaline reaction solution of step (2), is further processed material surface using hydrothermal synthesis method, obtains sodium titanate nanometer rods Array structure;
(4) tube furnace is used, in an ar atmosphere, the sodium titanate nanometer stick array that step (3) obtains anneal and sharp simultaneously G-C is carried out with the hot environment of annealing process3N4Chemical vapor deposition, the sodium titanate nanometer stick array, which is annealed into, to be had The titanium dioxide of three-dimensional net structure feature, surface deposited g-C by chemical vapour deposition technique3N4, obtain having light-operated anti- The g-C of bacterium function3N4/TiO2Coating.
Further, NaOH of the hydrothermal synthesis of the step (2) with alkaline reaction solution comprising 1-10 mol/L.
Further, the parameter of the high-level oxidation technology of the step (3) are as follows: the hydrogen peroxide solution concentration used is 5- 30 wt.%, the wavelength using ultraviolet lamp are 254 nm, and oxidation treatment time is 2-6 h.
Further, the response parameter of the hydrothermal synthesis method of the step (3) are as follows: reaction temperature is 80-180 DEG C, instead It is 4-12 h between seasonable.
Further, the sodium titanate nanometer stick array of the step (4) anneal and while utilizing annealing process Hot environment carries out g-C3N4Chemical vapor deposition, include the following steps: for melamine to be placed in ceramic boat bottom, utilize The face-down frame of growth of titanium or titanium alloy of the wire netting by surface with sodium titanate nanometer stick array structure is on melamine Side, is subsequently placed in CVD tube furnace, and heating rate is 3-8 DEG C/min, and the working time is 10-60 min, and operating temperature is 500-650 ℃。
Beneficial effect
(1) surface of the present invention has the g-C of light-operated antibacterial functions3N4/TiO2Three-dimensional net structure coating is by titanium and its alloy material Material surface is deposited with g-C3N4TiO2Bio-ceramic coating is constituted, which has good bioactivity, cell adjusting, antibacterial Equal beneficial effects and induced osteogenesis effect, can safely form in conjunction with firm physiology with bone tissue in a short time.
(2) TiO on surface2Bio-ceramic coating and metallic matrix bond strength are high, and have three-dimensional net structure, with gold The coating that metal surface is in contact is fine and close, bioactivity is high and can promote the deposition growing of apatite layer;Has the coating of nanostructure It is the ideal place of cell adhesion, proliferation, can induce neoblast and guidance is divided into histocyte to facilitate group around It knits to be formed.The g-C of titanium and its alloy material surface deposition3N4Coating can generate first more under visible light and near infrared range Strong oxidizing property photohole, while the super oxygen group and hydroxyl radical free radical that further generate can make inactivation of bacteria.In titanium And its alloy surface depends on the g-C of three-dimensional net structure deposition3N4Coating is remarkably improved it in the bon e formation energy at implantation initial stage Power and anti-microbial property.
Detailed description of the invention
Fig. 1 is coating surface form of the titanium alloy surface with sodium titanate nano bar-shape array structure in embodiment 1 Scanning electron microscope (SEM) picture of low (height) again.
Fig. 2 is that the titanium alloy surface in embodiment 1 has g-C3N4/TiO2The scanning of low (height) of coating surface form times Electronic Speculum (SEM) picture.
Fig. 3 is that the titanium alloy surface in embodiment 2 has g-C3N4/TiO2The x-ray photoelectron spectroscopy (XPS) of coating.
Fig. 4 is that the titanium alloy surface in embodiment 1 and embodiment 2 has g-C3N4/TiO2The antibacterial (Escherichia coli) of coating Experimental result.
Specific embodiment
Embodiment 1
(1) TC4 titanium alloy is selected first.
(2) pre-process: by titanium-base alloy implantation materials'use label be followed successively by the abrasive paper for metallograph of 600#, 800#, 1000# by Coarse sand is to fine sand sanding and polishing step by step, then with acetone, 70% alcohol, distilled water ultrasonic cleaning, dried for standby.
(3) chemical polishing: 40 ml of configuration contain the polishing solution of hydrofluoric acid, concentrated nitric acid, volume ratio are as follows: H2O:HF:HNO3= 5:1:4;TC4 titanium alloy is put into chemical polishing solution and polishes 3 min.
(4) advanced oxidation: TC4 titanium alloy is put into oxidation solution by the hydrogenperoxide steam generator of 5 wt% of configuration, and with 254 Its outer surface of the ultraviolet light irradiation of nm, oxidation treatment time are 4 h.
(5) hydrothermal synthesis is handled: by the TC4 titanium alloy after advanced oxidation, the sodium hydroxide solution for being 4 mol/L with concentration Hydrothermal synthesis is carried out, operating temperature is 120 DEG C, and the reaction time is 7 h;So that titanium alloy surface has sodium titanate nano bar-shape The coating of array structure;Its configuration of surface is as shown in scanning electron microscope (SEM) picture of Fig. 1.
(6) g-C3N4-TiO2Coating preparation: weighing 0.4 gram of melamine and be placed in ceramic boat bottom as evaporation source, There is the TC4 titanium alloy of sodium titanate nanometer stick array structure to grow face-down frame in melamine using wire netting above-mentioned surface It above amine, is subsequently placed in CVD tube furnace, operating temperature is 550 DEG C, and heating rate is 5 DEG C/min, and the working time is 30 min.It can obtain the g-C for having light-operated antibacterial functions3N4/TiO2Coating;Scanning electron microscope (SEM) figure of its configuration of surface such as Fig. 2 Shown in piece.
Fig. 4 (a1) and (a2) are antibacterial (Escherichia coli) experimental result of TC4 titanium alloy sample, and (c1) and (c2) is to implement Titanium alloy surface in example 1 has g-C3N4/TiO2Antibacterial (Escherichia coli) experimental result of coating.
Embodiment 2
(1) TC4 titanium alloy is selected first.
(2) pre-process: by titanium-base alloy implantation materials'use label be followed successively by the abrasive paper for metallograph of 600#, 800#, 1000# by Coarse sand is to fine sand sanding and polishing step by step, then with acetone, 70% alcohol, distilled water ultrasonic cleaning, dried for standby.
(3) chemical polishing: 40 ml of configuration contain the polishing solution of hydrofluoric acid, concentrated nitric acid, volume ratio are as follows: H2O:HF:HNO3= 5:1:4;TC4 titanium alloy is put into chemical polishing solution and polishes 3 min.
(4) advanced oxidation: TC4 titanium alloy is put into oxidation solution by the hydrogenperoxide steam generator of 5 wt% of configuration, and with 254 Its outer surface of the ultraviolet light irradiation of nm, oxidation treatment time are 3 h.
(5) hydrothermal synthesis is handled: molten with the sodium hydroxide that concentration is 5 mol/L by the titanium alloy bone nail after advanced oxidation Liquid carries out hydro-thermal reaction, and operating temperature is 120 DEG C, and the working time is 6 h.
(6) g-C3N4-TiO2Coating preparation: weighing 0.2 gram of melamine and be placed in ceramic boat bottom as evaporation source, There is the TC4 titanium alloy of sodium titanate nanometer stick array structure to grow face-down frame in melamine using wire netting above-mentioned surface It above amine, is subsequently placed in CVD tube furnace, operating temperature is 550 DEG C, and heating rate is 5 DEG C/min, and the working time is 20 min。
Fig. 3 is that the titanium alloy surface in embodiment 2 has g-C3N4/TiO2The x-ray photoelectron spectroscopy (XPS) of coating, figure 4 have g-C for the titanium alloy surface in embodiment 23N4/TiO2Antibacterial (Escherichia coli) experimental result of coating.
Fig. 4 (a1) and (a2) are antibacterial (Escherichia coli) experimental result of TC4 titanium alloy sample, and (b1) and (b2) is to implement Titanium alloy surface in example 2 has g-C3N4/TiO2Antibacterial (Escherichia coli) experimental result of coating.
Obviously, the above embodiment of the present invention is just for the sake of clearly illustrating examples made by the present invention, and being not is pair The restriction of embodiments of the present invention.It for those of ordinary skill in the art, can also be on the basis of the above description It makes other variations or changes in different ways, there is no need and unable to be exhaustive to all embodiments, and these belong to Spiritual changes and variations that derived from of the invention are still in protection scope of the present invention.

Claims (5)

1. a kind of light-operated antibacterial functions g-C of tool3N4/TiO2Coating and preparation method, which is characterized in that the light-operated antibacterial of the tool The g-C of function3N4/TiO2Coating is by the dioxy with three-dimensional net structure feature in titanium or the growth of titanium alloy material surface Change the g-C of titanium coating and the vapor deposition of its surface chemistry3N4Composition, the titanium dioxide with three-dimensional net structure feature Titanium coating and titanium or titanium alloy material surface are firmly combined, using hydrothermal synthesis method in matrix surface controllability in Hydroxyapatite Coatings in Alkaline Solution Sodium titanate nanometer stick array structure is grown, then utilizes high-temperature annealing process and chemical vapour deposition technique by titanium in tube furnace Sour sodium nanometer stick array is converted into surface and is deposited with g-C3N4The coating of titanium dioxide with three-dimensional network appearance feature;It is described The light-operated antibacterial functions of tool g-C3N4/TiO2The preparation method of coating, includes the following steps:
(1) a kind of titanium is provided or titanium alloy is the bio-medical material of matrix;
(2) provide it is a kind of include sodium hydroxide hydrothermal synthesis alkaline reaction solution;
(3) by titanium or titanium alloy material surface polishing, its surface is pre-processed using high-level oxidation technology, then It is put into the alkaline reaction solution of step (2), is further processed material surface using hydrothermal synthesis method, obtains sodium titanate nanometer rods Array structure;
(4) tube furnace is used, in an ar atmosphere, the sodium titanate nanometer stick array that step (3) obtains anneal and sharp simultaneously G-C is carried out with the hot environment of annealing process3N4Chemical vapor deposition, the sodium titanate nanometer stick array, which is annealed into, to be had The titanium dioxide of three-dimensional net structure feature, surface deposited g-C by chemical vapour deposition technique3N4, obtain having light-operated anti- The g-C of bacterium function3N4/TiO2Coating.
2. a kind of g-C for having light-operated antibacterial functions according to claim 13N4/TiO2Coating and preparation method, feature It is, NaOH of the hydrothermal synthesis of the step (2) with alkaline reaction solution comprising 1-10 mol/L.
3. a kind of g-C for having light-operated antibacterial functions according to claim 13N4/TiO2Coating and preparation method, feature It is, the parameter of the high-level oxidation technology of the step (3) are as follows: the hydrogen peroxide solution concentration used is 5-30 wt.%, is used The wavelength of ultraviolet lamp is 254 nm, and oxidation treatment time is 2-6 h.
4. a kind of g-C for having light-operated antibacterial functions according to claim 13N4/TiO2Coating and preparation method, feature It is, the response parameter of the hydrothermal synthesis method of the step (3) are as follows: reaction temperature is 80-180 DEG C, reaction time 4-12 h。
5. a kind of g-C for having light-operated antibacterial functions according to claim 13N4/TiO2Coating and preparation method, feature It is, the sodium titanate nanometer stick array of the step (4) anneal and while being carried out using the hot environment of annealing process g-C3N4Chemical vapor deposition, include the following steps: for melamine to be placed in ceramic boat bottom, using wire netting by surface The face-down frame of growth of titanium or titanium alloy with sodium titanate nanometer stick array structure is subsequently placed to above melamine In CVD tube furnace, heating rate is 3-8 DEG C/min, and the working time is 10-60 min, and operating temperature is 500-650 DEG C.
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CN111870737A (en) * 2020-06-15 2020-11-03 江汉大学附属湖北省第三人民医院 Preparation method of novel titanium alloy-based antibacterial film
CN115245594A (en) * 2021-04-26 2022-10-28 中国科学院上海硅酸盐研究所 Graphene oxide/graphite phase carbon nitride/titanium dioxide composite coating and preparation method and application thereof
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