阅读说明：本技术 一种具有AgO纳米颗粒-纳米棒复合结构的抗菌钛板的制备方法 (Preparation method of antibacterial titanium plate with AgO nanoparticle-nanorod composite structure ) 是由 尹永琦 王梦琪 刘潇 白丽娜 付淑芳 周胜 张强 于 2019-11-19 设计创作，主要内容包括：一种具有AgO纳米颗粒-纳米棒复合结构的抗菌钛板的制备方法,本发明涉及一种具有AgO纳米颗粒-纳米棒复合结构的抗菌钛板的制备方法。本发明的目的是为了解决现有湿化学合成方法制备的抗菌钛板存在Ag纳米颗粒易于团聚,均一性差的问题。本发明方法为：一、钛板(Ti)衬底的清洗；二、纳米棒阵列的制备；三、纳米氧化银(AgO)修饰纳米棒阵列的制备。本发明通过物理沉积的方法,在钛基板上形成稳定均一的纳米涂层,可以有效的抑制细菌。本发明应用于医疗和纳米技术领域。(The invention discloses a preparation method of an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure, and relates to a preparation method of an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure. The invention aims to solve the problems that Ag nano particles are easy to agglomerate and the uniformity is poor in an antibacterial titanium plate prepared by the existing wet chemical synthesis method. The method comprises the following steps: firstly, cleaning a titanium plate (Ti) substrate; secondly, preparing a nanorod array; and thirdly, preparing the nano silver oxide (AgO) modified nanorod array. According to the invention, a stable and uniform nano coating is formed on the titanium substrate by a physical deposition method, so that bacteria can be effectively inhibited. The invention is applied to the medical and nanotechnology fields.)

1. A preparation method of an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure is characterized by comprising the following steps:

firstly, cleaning a titanium plate substrate, and then drying;

secondly, preparing a nanorod array on the cleaned titanium plate substrate;

thirdly, preparing the nano silver oxide modified nanorod array: and (3) loading the metal Ag target and the titanium plate substrate with the nanorod array into a growth cavity of a magnetron sputtering device, and carrying out AgO modification on the nanorod array for 10-60min by taking argon as a working gas and oxygen as a reaction gas to obtain the titanium plate with the AgO modified zinc oxide nanorod array.

2. The method for preparing an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure according to claim 1, wherein in the first step, the substrate is ultrasonically cleaned by deionized water with conductivity of 18M Ω and 99.9 wt% ethanol respectively.

3. The method for preparing antibacterial titanium plate with AgO nanoparticle-nanorod composite structure according to claim 1, wherein the drying in the first step is hot-stage drying at 100 ℃.

4. The method for preparing the antibacterial titanium plate with the AgO nano-particle-nanorod composite structure according to claim 1, wherein in the second step, a ZnO nanorod array is prepared on the cleaned titanium plate substrate.

5. The method for preparing the antibacterial titanium plate with the AgO nano-particle-nanorod composite structure according to claim 4, wherein the method for preparing the ZnO nanorod array is as follows:

a. loading the ZnO target and the cleaned titanium plate substrate into a growth cavity of a magnetron sputtering device, introducing argon with the purity of 99.99 percent, introducing the argon at the flow rate of 40sccm, keeping the working pressure at 1Pa, adjusting the radio frequency power to 80W, performing thin film deposition, and obtaining the Ti substrate with the ZnO seed crystal layer, wherein the growth temperature is 350 ℃ and the growth time is 5 min;

b. putting the Ti substrate with the ZnO seed crystal layer into a precursor reaction solution, reacting for 3h under the thermal equilibrium of 90 ℃, then sequentially ultrasonically cleaning with deionized water and absolute ethyl alcohol, and drying at 100 ℃ to obtain a ZnO nanorod array; the precursor reaction solution is prepared from zinc nitrate hexahydrate and hexamethylenetetramine according to a molar ratio of 1: 1 in a certain proportion.

6. The method for preparing an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure according to claim 1, wherein the purity of argon in the third step is 99.99%.

7. The method for preparing the antibacterial titanium plate with the AgO nanoparticle-nanorod composite structure according to claim 1, wherein the working air pressure is 1Pa and the radio frequency power is adjusted to be 20W in the third step.

8. The method for preparing the antibacterial titanium plate with the AgO nano-particle-nanorod composite structure according to claim 1, wherein the flow ratio of oxygen to argon in the third step is 1: 8.

9. the method for preparing the antibacterial titanium plate with the AgO nano-particle-nanorod composite structure according to claim 1, wherein the flow ratio of oxygen to argon in the third step is 8: 1.

Technical Field

The invention relates to a preparation method of an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure.

Background

The titanium material and the titanium alloy have excellent mechanical property and biological stability, so the titanium material and the titanium alloy can be widely applied to implant materials in the medical field. Such as artificial joints in orthopedics, dental implants in dentistry, etc., the main problem of titanium implants at present is that the implants are susceptible to infection. Therefore, it is one of the effective methods to modify a smooth titanium substrate with a nano material having antibacterial properties. Ag has excellent antibacterial performance, and the Ag nano material is usually prepared by a wet chemical method, for example, Ag particles are spin-coated on a titanium sheet by a silane coupling method, so that the smooth titanium surface has the antibacterial performance. Although the wet chemical method is easy to synthesize, in the synthesis process, nano particles are easy to agglomerate, the spin coating loss is large, impurities are easy to introduce by adopting other coupling agents, and the like, and the uniform and stable antibacterial coating is not easy to form. At the same time, it is not suitable for large-scale preparation.

Disclosure of Invention

The invention aims to solve the problems of easy aggregation and poor uniformity of Ag nanoparticles in an antibacterial titanium plate prepared by the existing wet chemical synthesis method, and provides a preparation method of the antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure.

The invention relates to a preparation method of an antibacterial titanium plate with an AgO nanoparticle-nanorod composite structure, which comprises the following steps:

firstly, cleaning a titanium plate substrate, and then drying;

secondly, preparing a nanorod array on the cleaned titanium plate substrate;

thirdly, preparing the nano silver oxide modified nanorod array: and (3) loading the metal Ag target and the titanium plate substrate with the nanorod array into a growth cavity of a magnetron sputtering device, and carrying out AgO modification on the nanorod array for 10-60min by taking argon as a working gas and oxygen as a reaction gas to obtain the titanium plate with the AgO modified zinc oxide nanorod array.

The invention provides an antibacterial titanium plate, which is characterized in that a stable and uniform nano coating is formed on a titanium substrate by a physical deposition method, Ag nano particles are modified on a one-dimensional nanorod array by magnetron sputtering, and the antibacterial titanium plate is beneficial to forming uniformly dispersed Ag nano particles on the surfaces of nanorods and has good uniformity. Through contrast detection, the bacteria can be effectively inhibited. The titanium sheet with the nano composite structure has practical value in the field of medical bone grafting. In the antibacterial activity detection of typical gram-negative bacteria escherichia coli, the diameter of a bacteriostasis ring of an AgO nano structure/ZnO nano rod (high oxygen ratio) can reach 1.937 cm.

Drawings

FIG. 1 is a front phase of a scanning electron microscope of an antibacterial titanium plate with a coating of AgO nanoparticle-ZnO nanorod composite structure prepared in example 1;

FIG. 2 is a side phase of a scanning electron microscope of an antibacterial silicon wafer with a coating of the AgO nanoparticle-ZnO nanorod composite structure prepared in example 1;

FIG. 3 is a graph showing the results of 24 hours of the antibacterial activity test of Escherichia coli, a typical gram-negative bacterium in the example.

Detailed Description