CN110327487B - g-C with light-operated antibacterial function3N4/TiO2Coating and preparation method - Google Patents
g-C with light-operated antibacterial function3N4/TiO2Coating and preparation method Download PDFInfo
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Abstract
The invention relates to g-C with light-operated antibacterial function3N4/TiO2The light-operated antibacterial coating is formed by three-dimensional network TiO2And graphite-like phase carbon nitride (g-C) deposited on the surface thereof3N4) And (4) forming. The g-C with a three-dimensional network structure3N4/TiO2The coating is combined with the surface of a titanium or titanium alloy substrate, rodlike nano-array sodium titanate is constructed on the surface of the substrate through a hydrothermal synthesis method, and is converted into titanium dioxide by utilizing a chemical vapor deposition technology and g-C is deposited simultaneously3N4And (4) preparing the composition. The preparation method comprises the following steps: firstly, a sodium titanate biological coating of a rod-shaped nano array is obtained on the surface of a matrix by adopting a hydrothermal synthesis method; then the mixture is converted into titanium dioxide by using a high-temperature annealing process, and g-C is deposited on the surface of the titanium dioxide by using melamine as a raw material through a chemical vapor deposition technology3N4Finally, g-C with light-operated antibacterial function is prepared3N4/TiO2And (4) coating.
Description
Technical Field
The invention relates to a g-C with light-operated antibacterial function3N4/TiO2A coating and a preparation method, in particular to a sodium titanate biological ceramic coating which selects titanium and titanium alloy as matrix materials, adopts a hydrothermal synthesis method to controllably grow a nano rod-shaped array structure on the surface of the sodium titanate biological ceramic coating, and converts the nano rod-shaped array structure of the sodium titanate into TiO with g-C3N4 nano sheets deposited on the surface by utilizing a high-temperature annealing process and a chemical vapor deposition technology in a tubular furnace2A coating with a three-dimensional network structure and a preparation method thereof belong to the technical field of biomedical materials.
Background
Titanium and titanium alloy have excellent biocompatibility, high obdurability and corrosion resistance, are main raw materials of middle and high-end surgical implants which are commonly used in current clinical treatment, and can be used as a false dental implant, an artificial orthopedic substitute, a blood vessel and soft tissue minimally invasive intervention implant and the like.
Titanium and titanium alloys are biologically inert metal materials, and thin and dense titanium oxide passivation layers on the surfaces of the titanium and titanium alloys can prevent phosphate deposition, so that the implants taking the alloys as the matrix are difficult to form osseointegration and osseointegration with bone tissues, and finally the failure of the implants is caused.
Bacterial organisms often form a bacterial biofilm on the surface of an implant, so that the operation process of interventional therapy is often accompanied with intraoperative infection, and a patient who receives the operation cannot achieve good effect even if treated by antibiotics after the operation, and finally the function of the implant is failed.
TiO2Has good biological activity, can promote the interaction between the surface of the titanium-based alloy and the physiological tissues of a human body, enhances the osseous combination of an implant and the bone tissues and improves the success rate of implantation. At the same time, TiO2Has certain bacteriostasis and sterilization effects, and can play a broad-spectrum antibacterial role under the condition of not consuming the antibacterial agent.
g-C3N4Due to the special two-dimensional structure, the photocatalyst has stronger photocatalysis effect. g-C under visible and near infrared light3N4Can form photoproduction electrons and photoproduction holes, further catalyze oxygen and water in the environment to form superoxide radicals and hydroxyl radicals, thereby destroying cell membranes of bacteria and leading the bacteria to be inactivated, and finally play a role in light control and antibiosis.
g-C3N4The chemical property of the product is stable, the product is nontoxic and pollution-free, the cytotoxicity is almost absent in the organism, and the product has good biocompatibility.
The hydrothermal synthesis method can induce the growth of the sodium titanate nano structure on the surface of the titanium alloy in an alkaline environment. Research shows that the sodium titanate nano structure with the bone-like structure is beneficial to nucleation and growth of the bone-like apatite structure and proliferation, adhesion and differentiation of osteoblasts. In addition, the nano structure with the complex three-dimensional characteristics can greatly improve the specific surface area of the material, thereby providing a place for storing and releasing drugs and biochemical active factors and enhancing the interventional therapy effect and functionality of the implant.
After the sodium titanate nanorod array structure is controllably constructed on the surface of titanium and titanium alloy in an alkali liquor environment through a hydrothermal synthesis method, the sodium titanate nanorod array structure on the surface of the titanium and titanium alloy is converted into the structure with g-C deposited on the surface by adopting a tube furnace through a high-temperature annealing process and a chemical vapor deposition technology3N4The titanium dioxide coating with the three-dimensional network structure is used for realizing light-operated antibiosis and shows hugePotential for biomedical applications. However, the technique is used to prepare g-C with a similar three-dimensional network structure3N4/TiO2Structural coatings and making use of g-C3N4And TiO2The antibacterial function of the surface of the material is improved, and the method is rarely reported in the technical field of biomedical materials. In view of the above, the invention provides a g-C with light-operated antibacterial function3N4/TiO2A coating and a method for preparing the same.
Disclosure of Invention
The invention aims to overcome the defects of the artificial implant material and provides a g-C with a light-operated antibacterial function3N4/TiO2A coating and a preparation method thereof, and a coating and a preparation method thereof, which can obviously improve the surface bioactivity, the cell regulation and control capability, the surface antibacterial property and various beneficial functions at the early stage of implantation.
The sodium titanate biological ceramic coating with the nano rod-shaped array structure is controllably grown in an alkali liquor environment by a hydrothermal synthesis method, and then the sodium titanate is converted into the coating with g-C deposited on the surface by a high-temperature annealing process and a chemical vapor deposition technology3N4And has a titanium dioxide coating layer of a three-dimensional network structure. In the hydrothermal synthesis process, the sodium titanate active layer is grown in situ on the surface of the TC4 titanium alloy substrate, so that the TiO obtained by the high-temperature annealing process2The biological ceramic coating has high bonding strength with the metal matrix, and the obtained TiO2The nanostructure is also g-C3N4The coating is deposited and grown on the ideal template. g-C3N4Can be deposited on the surface of the TC4 titanium alloy matrix by chemical vapor deposition technology, thereby improving the binding force between the antibacterial coating on the surface of the titanium-based alloy implant material and the matrix, ensuring the durability of the antibacterial performance of the coating, and finally obtaining the g-C3N4/TiO2The three-dimensional network structure has good bioactivity and can promote nucleation and deposition growth of the apatite layer. After fixed implantation in the human body, g-C3N4/TiO2The antibacterial function of the three-dimensional network structure coating is prolonged, and the risk of fixed secondary infection is favorably reduced.
The invention is realized by the following technical scheme:
g-C with light-operated antibacterial function3N4/TiO2The coating and the preparation method are characterized in that the g-C with the light-operated antibacterial function3N4/TiO2The coating is a titanium dioxide coating with three-dimensional network structure characteristics and grown on the surface of a titanium or titanium alloy material, and graphite-like phase carbon nitride g-C chemically deposited on the surface of the titanium dioxide coating3N4The titanium dioxide coating with the three-dimensional network structure characteristic is firmly combined with the surface of a titanium or titanium alloy material, a sodium titanate nanorod array structure is controllably grown on the surface of a matrix in an alkali liquor environment by a hydrothermal synthesis method, and then the sodium titanate nanorod array is converted into a film with g-C deposited on the surface by a high-temperature annealing process and a chemical vapor deposition technology in a tube furnace3N4The titanium dioxide coating with three-dimensional network morphology characteristics; g-C with light-operated antibacterial function3N4/TiO2The preparation method of the coating comprises the following steps:
(1) providing a biomedical material taking titanium or titanium alloy as a matrix;
(2) providing a basic reaction solution containing sodium hydroxide for hydrothermal synthesis;
(3) polishing the surface of the titanium or titanium alloy material, pretreating the surface of the titanium or titanium alloy material by using an advanced oxidation technology, then putting the titanium or titanium alloy material into the alkaline reaction solution obtained in the step (2), and further treating the surface of the material by using a hydrothermal synthesis method to obtain a sodium titanate nanorod array structure;
(4) annealing the sodium titanate nanorod array obtained in the step (3) in Ar atmosphere by using a tube furnace, and simultaneously performing g-C in a high-temperature environment of the annealing process3N4The sodium titanate nanorod array is annealed into titanium dioxide with three-dimensional network structure characteristics, and g-C is deposited on the surface of the titanium dioxide by a chemical vapor deposition technology3N4To obtain g-C with light-operated antibacterial function3N4/TiO2And (4) coating.
Further, the hydrothermal synthesis of the step (2) comprises 1-10 mol/L NaOH with an alkaline reaction solution.
Further, the parameters of the advanced oxidation technology in the step (3) are as follows: the concentration of the hydrogen peroxide solution is 5-30 wt.%, the wavelength of an ultraviolet lamp is 254 nm, and the oxidation treatment time is 2-6 h.
Further, the reaction parameters of the hydrothermal synthesis method in step (3) are as follows: the reaction temperature is 80-180 ℃, and the reaction time is 4-12 h.
Further, annealing the sodium titanate nanorod array in the step (4) and simultaneously performing g-C by utilizing a high-temperature environment of the annealing process3N4Comprises the following steps: the melamine is placed at the bottom of the ceramic boat, the growing surface of the titanium or titanium alloy with the sodium titanate nanorod array structure on the surface is erected on the melamine downwards by using a wire mesh, and then the melamine is placed in a CVD (chemical vapor deposition) tube furnace, wherein the heating rate is 3-8 ℃/min, the working time is 10-60 min, and the working temperature is 500-650 ℃.
Advantageous effects
(1) The surface of the invention has g-C with light-operated antibacterial function3N4/TiO2The three-dimensional network structure coating is formed by depositing g-C on the surface of titanium and alloy materials thereof3N4Of TiO 22The biological ceramic coating has good biological activity, cell regulation, antibiosis and other beneficial effects and induces osteogenesis effect, and can safely form firm physiological combination with bone tissues in a short time.
(2) Surface TiO2The biological ceramic coating has high bonding strength with a metal matrix, has a three-dimensional network structure, is compact in coating contacted with the metal surface, has high biological activity and can promote the deposition and growth of the apatite layer; the nanostructured coating is an ideal site for cell adhesion and proliferation, and can induce undifferentiated cells and direct differentiation into tissue cells to promote the formation of surrounding tissues. g-C deposited on surface of titanium and alloy material thereof3N4A coating capable of generating more photo-generated holes with strong oxidizing property in visible light and near infrared rangeBoth superoxide radicals and hydroxyl radicals produced further can inactivate bacteria. g-C deposited by attaching three-dimensional network structure on surface of titanium and titanium alloy3N4The coating can obviously improve the bone forming capability and the antibacterial performance of the coating in the early stage of implantation.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of the low (high) power of the morphology of the coated surface of the titanium alloy having the sodium titanate nanorod array structure on the surface in example 1.
FIG. 2 is a graph showing that the surface of the titanium alloy in example 1 has g-C3N4/TiO2Scanning Electron Microscope (SEM) pictures of low (high) power of the coating surface morphology.
FIG. 3 shows the surface of the titanium alloy of example 2 having g-C3N4/TiO2X-ray photoelectron spectroscopy (XPS) of the coating.
FIG. 4 shows that the titanium alloy surfaces of examples 1 and 2 have g-C3N4/TiO2Results of the coating antibacterial (E.coli) test.
Detailed Description
Example 1
(1) The TC4 titanium alloy is selected firstly.
(2) Pretreatment: the titanium-based alloy implant material is gradually ground and polished from coarse sand to fine sand by using metallographic abrasive paper with the serial numbers of 600#, 800#, and 1000#, then is ultrasonically cleaned by acetone, 70% alcohol and distilled water, and is dried for later use.
(3) Chemical polishing: preparing 40 ml of polishing solution containing hydrofluoric acid and concentrated nitric acid, wherein the volume ratio is as follows: h2O：HF：HNO3=5:1: 4; and (3) polishing the TC4 titanium alloy in a chemical polishing solution for 3 min.
(4) Advanced oxidation: preparing a 5 wt% hydrogen peroxide solution, putting the TC4 titanium alloy into an oxidizing solution, and irradiating the outer surface of the titanium alloy with an ultraviolet lamp with a wavelength of 254 nm, wherein the oxidizing treatment time is 4 h.
(5) Hydrothermal synthesis treatment: carrying out hydro-thermal synthesis on the TC4 titanium alloy subjected to advanced oxidation by using a sodium hydroxide solution with the concentration of 4 mol/L, wherein the working temperature is 120 ℃, and the reaction time is 7 h; so that the surface of the titanium alloy is provided with a coating with a sodium titanate nanorod array structure; the surface morphology is shown in the Scanning Electron Microscope (SEM) picture of fig. 1.
（6）g-C3N4-TiO2Preparing a coating: 0.4 g of melamine is weighed as an evaporation source and placed at the bottom of a ceramic boat, the TC4 titanium alloy with the surface having the sodium titanate nanorod array structure is erected above the melamine with the growing surface facing downwards by using a wire mesh, and then the titanium alloy is placed in a CVD tube furnace at the working temperature of 550 ℃, the heating rate of 5 ℃/min and the working time of 30 min. g-C with light-operated antibacterial function can be obtained3N4/TiO2Coating; the surface morphology is shown in the Scanning Electron Microscope (SEM) picture of fig. 2.
FIGS. 4 (a 1) and (a 2) are the results of the antibacterial (E.coli) test of TC4 titanium alloy samples, (C1) and (C2) are the titanium alloy samples of example 1 having g-C on the surface3N4/TiO2Results of the coating antibacterial (E.coli) test.
Example 2
(1) The TC4 titanium alloy is selected firstly.
(2) Pretreatment: the titanium-based alloy implant material is gradually ground and polished from coarse sand to fine sand by using metallographic abrasive paper with the serial numbers of 600#, 800#, and 1000#, then is ultrasonically cleaned by acetone, 70% alcohol and distilled water, and is dried for later use.
(3) Chemical polishing: preparing 40 ml of polishing solution containing hydrofluoric acid and concentrated nitric acid, wherein the volume ratio is as follows: h2O：HF：HNO3=5:1: 4; and (3) polishing the TC4 titanium alloy in a chemical polishing solution for 3 min.
(4) Advanced oxidation: preparing a 5 wt% hydrogen peroxide solution, putting the TC4 titanium alloy into an oxidizing solution, and irradiating the outer surface of the titanium alloy with an ultraviolet lamp with a wavelength of 254 nm, wherein the oxidizing treatment time is 3 h.
(5) Hydrothermal synthesis treatment: carrying out hydrothermal reaction on the titanium alloy bone nail subjected to advanced oxidation by using a sodium hydroxide solution with the concentration of 5 mol/L, wherein the working temperature is 120 ℃, and the working time is 6 hours.
（6）g-C3N4-TiO2Preparing a coating: 0.2 g of melamine is weighed as an evaporation source and placed at the bottom of a ceramic boat, the TC4 titanium alloy with the surface having the sodium titanate nanorod array structure is erected above the melamine with the growing surface facing downwards by using a wire mesh, and then the titanium alloy is placed in a CVD tube furnace at the working temperature of 550 ℃, the heating rate of 5 ℃/min and the working time of 20 min.
FIG. 3 shows the surface of the titanium alloy of example 2 having g-C3N4/TiO2X-ray photoelectron Spectroscopy (XPS) of the coating, FIG. 4 shows that the surface of the titanium alloy of example 2 has g-C3N4/TiO2Results of the coating antibacterial (E.coli) test.
FIGS. 4 (a 1) and (a 2) are the results of the antibacterial (E.coli) test of TC4 titanium alloy samples, and (b 1) and (b 2) are the titanium alloy samples of example 2 having g-C on the surface3N4/TiO2Results of the coating antibacterial (E.coli) test.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. It will be apparent to those skilled in the art that other variations and modifications may be made in the foregoing disclosure, without departing from the spirit or essential characteristics of the invention, and it is intended to cover all such modifications and variations as fall within the true spirit and scope of the invention.
Claims (4)
1. g-C with light-operated antibacterial function3N4/TiO2The preparation method of the coating is characterized in that the g-C with the light-operated antibacterial function3N4/TiO2The coating is a titanium dioxide coating with three-dimensional network structure characteristics and grown on the surface of a titanium or titanium alloy material and g-C chemically deposited on the surface of the titanium dioxide coating3N4The titanium dioxide coating with the three-dimensional network structure characteristic is firmly combined with the surface of a titanium or titanium alloy material, and a sodium titanate nanorod array grows on the surface of a matrix in an alkali liquor environment in a controllable manner by using a hydrothermal synthesis methodA column structure, then a high-temperature annealing process and a chemical vapor deposition technology are utilized in a tube furnace to convert the sodium titanate nanorod array into a structure with g-C deposited on the surface3N4The titanium dioxide coating with three-dimensional network morphology characteristics; g-C with light-operated antibacterial function3N4/TiO2The preparation method of the coating comprises the following steps:
(1) providing a biomedical material taking titanium or titanium alloy as a matrix;
(2) providing a basic reaction solution containing sodium hydroxide for hydrothermal synthesis;
(3) polishing the surface of the titanium or titanium alloy material, pretreating the surface of the titanium or titanium alloy material by using an advanced oxidation technology, then putting the titanium or titanium alloy material into the alkaline reaction solution obtained in the step (2), and further treating the surface of the material by using a hydrothermal synthesis method to obtain a sodium titanate nanorod array structure; the parameters of the advanced oxidation technology are as follows: the concentration of the used hydrogen peroxide solution is 5-30 wt.%, the wavelength of an ultraviolet lamp is 254 nm, and the oxidation treatment time is 2-6 h;
(4) annealing the sodium titanate nanorod array obtained in the step (3) in Ar atmosphere by using a tube furnace, and simultaneously performing g-C in a high-temperature environment of the annealing process3N4The sodium titanate nanorod array is annealed into titanium dioxide with three-dimensional network structure characteristics, and g-C is deposited on the surface of the titanium dioxide by a chemical vapor deposition technology3N4To obtain g-C with light-operated antibacterial function3N4/TiO2And (4) coating.
2. The light-operated antibacterial g-C as claimed in claim 13N4/TiO2The preparation method of the coating is characterized in that the hydrothermal synthesis in the step (2) comprises 1-10 mol/L NaOH by using an alkaline reaction solution.
3. The light-operated antibacterial g-C as claimed in claim 13N4/TiO2The preparation method of the coating is characterized in that the hydrothermal method in the step (3)The reaction parameters of the synthesis method are as follows: the reaction temperature is 80-180 ℃, and the reaction time is 4-12 h.
4. The light-operated antibacterial g-C as claimed in claim 13N4/TiO2The preparation method of the coating is characterized in that the sodium titanate nanorod array in the step (4) is annealed, and simultaneously g-C is carried out in a high-temperature environment of the annealing process3N4Comprises the following steps: the melamine is placed at the bottom of the ceramic boat, the growing surface of the titanium or titanium alloy with the sodium titanate nanorod array structure on the surface is erected on the melamine downwards by using a wire mesh, and then the melamine is placed in a CVD (chemical vapor deposition) tube furnace, wherein the heating rate is 3-8 ℃/min, the working time is 10-60 min, and the working temperature is 500-650 ℃.
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| CN111870737B (en) * | 2020-06-15 | 2021-11-23 | 江汉大学附属湖北省第三人民医院 | Preparation method of titanium alloy-based antibacterial film |
| CN115245594B (en) * | 2021-04-26 | 2023-04-07 | 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 |
| CN113797398A (en) * | 2021-09-26 | 2021-12-17 | 苏州纽创医疗科技有限公司 | Preparation method of titanium alloy stent with anticoagulant coating and stent |
| CN114875458B (en) * | 2022-05-19 | 2023-04-18 | 西安泰金新能科技股份有限公司 | Noble metal anode for electrolytic copper foil and preparation method thereof |
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