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Preparation method of medical titanium surface gradient nanometer silver

A surface gradient and nano-silver technology, which is applied in the direction of surface reaction electrolytic coating, medical science, electrolytic coating, etc., can solve the problems of cytotoxicity and affecting cell activity, and achieve short time consumption, simple process, easy realization and control Effect

Inactive Publication Date: 2019-01-25
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Silver is a broad-spectrum antibiotic, widely used in silver-containing bone cement and other implant materials, but the antibacterial property of silver is a double-edged sword, namely (Li H, Cui Q, Feng B, et al. Antibacterial activity of TiO2 ,nanotubes:Influence of crystal phase,morphology and Ag deposition[J].Applied Surface Science,2013,284(11):179-183) Silver can not only be used as an antibacterial agent, but also affect cells when its content exceeds a certain concentration Activity, that is, cytotoxicity (Arora S, Jain J, Rajwade J M, et al. Cellular responses induced by silvernanoparticles: In vitro, studies[J].Toxicology Letters,2008,179(2):93-100)

Method used

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  • Preparation method of medical titanium surface gradient nanometer silver
  • Preparation method of medical titanium surface gradient nanometer silver
  • Preparation method of medical titanium surface gradient nanometer silver

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Cut the titanium foil into 2.5cm×4cm, ultrasonically clean it with acetone, ethanol, and deionized water for 20 minutes each, then dry it with a hair dryer, and store it in a ziplock bag for use. Prepare 100 ml of electrolytic solution for traditional electrochemical anodic oxidation, which solution contains 0.5 wt% hydrofluoric acid. The titanium foil was submerged in the electrolyte, the voltage was 15V, and the oxidation time was 20min. After the reaction was completed, it was taken out and rinsed with deionized water and dried. At this time, a layer of TiO in a regular array is obtained on the surface of the titanium foil. 2 Nanotubes with a diameter of about 80nm, such as figure 2 shown.

[0038] The titanium foil modified with titanium dioxide nanotubes was cut into 2.5cm×1cm and used as a bipolar electrode. Fix the titanium bipolar electrode horizontally at the bottom of the electrolytic cell, and its two ends are 1mm away from the two platinum electrodes. Po...

Embodiment 2

[0040]Repeat all the steps in Example 1 to prepare gradient nano-silver micropattern samples. The prepared sample was irradiated under ultraviolet light for more than 30 minutes, and the MC3T3-E1 cells were irradiated at a density of 1.0×10 5 Inoculate on the sample at a density of one / ml and incubate in a 37°C incubator for 24h. Fluorescent staining with Calcein-AM, observed with an inverted fluorescence microscope under blue light excitation, as shown in Figure 7-10 As shown, the number of adhered cells gradually increased with the increase of nano-silver particle size.

Embodiment 3

[0042] The gradient nano-silver micropattern sample prepared by repeating all the steps in Example 1. The prepared samples were soaked in alcohol for 30 min and then rinsed with PBS. Staphylococcus aureus at a density of 1.0×10 6 ~1.0×10 7 Inoculate on the sample at a density of one / ml and incubate in a 37°C incubator for 6h. After taking it out, wash it with PBS for 3 times, fix it with 2.5% glutaraldehyde solution in a refrigerator at 4°C for 2 hours, and then use 30%, 50%, 75%, 90%, and 100% absolute ethanol to carry out gradient dehydration successively. The samples were submerged in tert-butanol, frozen in a refrigerator at -20°C, and then placed in a lyophilizer to freeze-dry. The samples were sprayed with gold and observed under a scanning electron microscope. Such as Figures 11-14 As shown, the number of bacteria gradually increased with the increase of nano-silver particle size.

[0043] The present invention cleans the titanium foil and uses an electrochemical ...

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Abstract

The invention provides a preparation method of medical titanium surface gradient nanometer silver, and relates to the field of medical titanium surface coating modification. The method comprises the following steps of performing medical titanium foil surface pretreatment; preparing TiO2 nanometer tubes; preparing silver ion-containing electrolyte; performing bipolar electrochemical reaction experiment to obtain the medical titanium surface gradient nanometer silver. A gradient nanometer silver coating built on a medical titanium surface with a combination of a conventional electrochemical anode oxidization method and a bipolar electrochemical method; by selecting a proper electrolyte formula and controlling electrochemical parameters, the nanometer silver with the variable particle gradient change can be obtained; a prepared TiO2 nanometer tube arrays have a regular array shape; the arrangement is tight. Nanometer silver particles prepared on the surface of the TiO2 nanometer tube array realize the dimension gradient change. In a short time, the gradient nanometer silver particles can be prepared and obtained in one step on the surface of the titanium nanometer tubes by using the bipolar electrochemical method. The characteristics that the process is simple; the time consumption is short; the realization and the control are easy, and the like are achieved. When the preparationmethod is applied to the high-flux screening of nanometer silver particle antibiosis, the characteristics of high efficiency and high speed are realized.

Description

technical field [0001] The invention relates to surface coating modification of medical titanium, in particular to a method for preparing gradient nano silver on the surface of medical titanium by applying a bipolar electrochemical method to controlly construct particle size gradient changes on the surface of medical titanium. Background technique [0002] Medical titanium and its alloys have been widely used as surgical implant materials because of their good biocompatibility. In the initial stage of implantation, medical implant materials are prone to infection due to the growth of bacteria, and even implantation failure. Therefore, in addition to a sterile environment, the antibacterial properties of the implant are very important in the early stage of implantation. Silver is a broad-spectrum antibiotic, widely used in silver-containing bone cement and other implant materials, but the antibacterial property of silver is a double-edged sword, namely (Li H, Cui Q, Feng B, e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26A61L27/30C25D3/46
CPCA61L27/306C25D3/46C25D11/26
Inventor 黄巧玲李艳冉林昌健胡洁洁吴采宇郑锐鸿董元军余平刘向阳
Owner XIAMEN UNIV
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