阅读说明：本技术 一种改善Ag微纳薄膜生物相容性的方法及其膜的应用 (Method for improving biocompatibility of Ag micro-nano film and application of Ag micro-nano film ) 是由 宋忠孝 陈东圳 朱晓东 钱旦 于 2019-11-04 设计创作，主要内容包括：本发明公开了一种改善Ag微纳薄膜生物相容性的方法及其膜的应用,包括清洗硅片、制备Ta@Ag双金属薄膜；通过调整磁控溅射沉积设备的温度,电压,控制Ag靶和Ta靶的电流,将Ta相按照比例与Ag在烘干的硅片上进行两相共溅射,即制备出Ta@Ag双金属薄膜。所制得的Ta@Ag双金属薄膜为金属晶体结构,表面有1.5nm厚的顶部氧化层,控制生物细胞在薄膜上,生物细胞的存活率为95～99％。本发明通过采用真空物理气相沉积技术掺杂金属Ta元素,从而改善了Ag微纳薄膜的生物相容性。(The invention discloses a method for improving biocompatibility of an Ag micro-nano film and application of the Ag micro-nano film, which comprises the steps of cleaning a silicon wafer and preparing a Ta @ Ag bimetallic film; the Ta @ Ag bimetallic film is prepared by adjusting the temperature and voltage of magnetron sputtering deposition equipment, controlling the current of an Ag target and a Ta target and carrying out two-phase co-sputtering on a Ta phase and Ag on a dried silicon wafer according to a proportion. The prepared Ta @ Ag bimetallic film is of a metal crystal structure, a top oxidation layer with the thickness of 1.5nm is arranged on the surface of the Ta @ Ag bimetallic film, and the survival rate of biological cells on the film is controlled to be 95-99%. According to the invention, the metal Ta element is doped by adopting a vacuum physical vapor deposition technology, so that the biocompatibility of the Ag micro-nano film is improved.)

1. A method for improving biocompatibility of an Ag micro-nano film is characterized by comprising the following steps:

step 1: cleaning a silicon wafer:

soaking the cleaned silicon wafer substrate in ethanol or acetone solution and deionized water in sequence, and drying;

step 2: preparing a Ta @ Ag bimetallic film:

adjusting the temperature of magnetron sputtering deposition equipment to be 25-150 ℃, controlling the voltage to be 360-400V, controlling the current of an Ag target and a Ta target to be 0.5-6A, keeping vacuum, introducing argon, and carrying out two-phase co-sputtering on a dried silicon wafer with 5-90% of Ta phase and Ag according to the mass percentage to prepare the Ta @ Ag bimetallic film.

2. The method for improving the biocompatibility of the Ag micro-nano film according to claim 1, wherein in the step 1, the cleaned silicon wafer substrate is immersed in an ethanol and acetone solution for 2-5 min and is immersed in deionized water for 2-5 min.

3. The method for improving the biocompatibility of the Ag micro-nano film according to claim 1, wherein the current ratio of the Ag target to the Ta target is 0.2: 1-1: 1.

4. The method for improving the biocompatibility of the Ag micro-nano film according to claim 1, wherein the temperature of the magnetron sputtering deposition equipment is 25-150 ℃, the voltage is 360-380V, the current of the Ta target and the Ag target is 1.8-4A, and the mass percent of the Ta element is 25-75%.

5. The method for improving the biocompatibility of the Ag micro-nano film according to claim 1, wherein the temperature of the magnetron sputtering deposition equipment is 25-150 ℃, the voltage is 360-380V, the current of the Ta target and the Ag target is 0.5-5.5A, and the mass percent of the Ta element is 30-45%.

6. The method for improving the biocompatibility of the Ag micro-nano film according to claim 1, wherein the temperature of the magnetron sputtering deposition equipment is 25-150 ℃, the voltage is 360-380V, the current of the Ta target and the Ag target is 2-4A, and the mass percent of the Ta element is 60-80%.

7. The method for improving the biocompatibility of the Ag micro-nano film according to the claim 1, wherein the temperature of the magnetron sputtering deposition equipment is 150 ℃, the voltage is 370V, the current of the Ag target and the Ta target is 3A, and the mass percent of the Ta element is 47%.

8. The method for improving the biocompatibility of the Ag micro-nano film according to any one of claims 1 to 7, wherein the Ta @ Ag bimetallic film is of a metal crystal structure, a top oxide layer with the thickness of 1.5nm is arranged on the surface of the Ta @ Ag bimetallic film, and the survival rate of biological cells on the film is controlled to be 95-99%.

9. The Ta @ Ag bimetallic film prepared by the method for improving the biocompatibility of the Ag micro-nano film according to the claim 8 is applied to active biological cell detection and biomedical equipment coatings.

Technical Field

The invention belongs to the technical field of film coatings, and particularly relates to a method for improving biocompatibility of a silver (Ag) micro-nano film and application of the film.

Background

The Ag micro-nano structure film has good dielectric property, higher plasma activity and lower cost, thereby being widely concerned by people. In various metals, the nanostructure rich in silver can maintain an extremely strong surface plasma polarization mode, and the characteristic is the key to the realization of the applications of plasma sensing, catalysis and the like. (C.Gao, Y.Hu, M.Wang, M.Chi, Y.yin, J.Am.chem.Soc.2014,136, 7474.). In gold (Au) and Ag plasma metal, the optical section of the Ag nano structure is larger, and the manufacturing cost is low. However, the biocompatibility of the Ag micro-nano structure film is poor, and the application of the Ag micro-nano structure film in biochemical analysis, biomedical equipment and the like is hindered. The construction of a bimetallic system is an effective strategy for improving the biocompatibility of the Ag micro-nano film. Bimetallic systems exhibit better performance than single element systems by combining immiscible metals of different functional properties. The metal Ta has good biocompatibility, corrosion resistance and fracture toughness. Researches show that the Ta modified surface with the micro-nano structure can activate focal adhesion kinase and enhance the interaction between cells and the surface. (H.Cao, F.Meng, X.Liu, J.Vac.Sci.Technol.A.2016,34,04C 102; H.L.Huang, Y.Y.Chang, H.J.Chen, Y.K.Chou, J.Vac.Sci.Technol.A.2014,32,02B117.) therefore, the design and preparation of Ta @ Ag bimetallic films can improve the biocompatibility of high-purity Ag micro-nano structure films.

Disclosure of Invention

In order to solve the defects in the prior art, the invention aims to provide a method for improving the biocompatibility of an Ag micro-nano film and application of the Ag micro-nano film, the method solves the problem of poor biocompatibility of the existing pure Ag micro-nano film, Ta element is controlled to be doped in the Ag micro-nano film, Ta and Ag are mechanically mixed to generate composition, and a Ta @ Ag bimetallic film is formed.

The invention is realized by the following technical scheme.

A method for improving biocompatibility of an Ag micro-nano film comprises the following steps:

step 1: cleaning a silicon wafer:

soaking the cleaned silicon wafer substrate in ethanol or acetone solution and deionized water in sequence, and drying;

step 2: preparing a Ta @ Ag bimetallic film:

adjusting the temperature of magnetron sputtering deposition equipment to be 25-150 ℃, controlling the voltage to be 360-400V, controlling the current of an Ag target and a Ta target to be 0.5-6A, keeping vacuum, introducing argon, and carrying out two-phase co-sputtering on a dried silicon wafer with 5-90% of Ta phase and Ag according to the mass percentage to prepare the Ta @ Ag bimetallic film.

With respect to the above technical solutions, the present invention has a further preferable solution:

preferably, in the step 1, the silicon wafer substrate is immersed in an ethanol and acetone solution for 2-5 min and immersed in deionized water for 2-5 min.

Preferably, the current ratio of the Ag target to the Ta target is 0.2:1 to 1: 1.

Preferably, the temperature of the magnetron sputtering deposition equipment is 25-150 ℃, the voltage is 360-380V, the current of the Ta target and the Ag target is 1.8-4A, and the mass percent of the Ta element is 25-75%.

Preferably, the temperature of the magnetron sputtering deposition equipment is 25-150 ℃, the voltage is 360-380V, the current of the Ta target and the Ag target is 0.5-5.5A, and the mass percent of the Ta element is 30-45%.

Preferably, the temperature of the magnetron sputtering deposition equipment is 25-150 ℃, the voltage is 360-380V, the current of the Ta target and the Ag target is 2-4A, and the mass percent of the Ta element is 60-80%.

Preferably, the temperature of the magnetron sputtering deposition equipment is 150 ℃, the voltage is 370V, the current of the Ag target and the Ta target is 3A, and the mass percent of the Ta element is 47%.

The Ta @ Ag bimetallic film is of a metal crystal structure, the top oxidation layer with the thickness of 1.5nm is arranged on the surface of the Ta @ Ag bimetallic film, biological cells are controlled on the Ta @ Ag bimetallic film, and the survival rate of the biological cells is 95-99%.

Due to the adoption of the technical scheme, the invention has the following beneficial effects:

according to the method for improving the biocompatibility of the Ag micro-nano film, good cell surface interaction can be generated according to the excellent biocompatibility, corrosion resistance and fracture toughness of the metal Ta. Therefore, the temperature and the voltage of the magnetron sputtering deposition equipment and the current ratio of the Ta target to the Ag target are adjusted, the Ta element is doped in the Ag micro-nano film by controlling, the component proportion of the Ta @ Ag bimetallic film is controlled, the Ta and the Ag are mechanically mixed to generate compounding, the Ta @ Ag bimetallic film is formed, and the biocompatibility of the Ag film can be effectively improved.

The prepared Ta @ Ag bimetallic film is of a metal crystal structure, a top oxidation layer with the thickness of 1.5nm is arranged on the surface of the Ta @ Ag bimetallic film, and the survival rate of biological cells on the film is controlled to be 95-99%. The Ta @ Ag bimetallic film prepared by the method for improving the biocompatibility of the Ag micro-nano film can be applied to active biological cell detection and biomedical equipment coatings.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:

FIG. 1 is a high-resolution transmission electron micrograph of a Ta @ Ag bimetallic film section in a method for improving biocompatibility of an Ag micro-nano film according to the invention;

FIG. 2 is a scanning electron microscope image of a Ta @ Ag bimetallic film prepared by doping Ta element at 81% by mass according to a method for improving biocompatibility of an Ag micro-nano film of the present invention;

FIG. 3 is an XRD (X-ray diffraction) pattern of a Ta @ Ag bimetallic film prepared by doping Ta with about 81% by mass in the method for improving the biocompatibility of the Ag micro-nano film;

FIG. 4 is a scanning electron microscope image of a Ta @ Ag bimetallic film prepared by doping Ta element at about 45.25% by mass according to a method for improving biocompatibility of an Ag micro-nano film of the invention;

FIG. 5 is a scanning electron microscope image of pure Ag film in a method for improving biocompatibility of Ag micro-nano film according to the invention;

FIG. 6 is an XRD pattern of a pure Ag film in a method for improving biocompatibility of an Ag micro-nano film according to the invention;

FIG. 7 is a test chart of biological cell culture on the surface of a Ta @ Ag bimetallic film (9% doped with Ta element) in the method for improving the biocompatibility of the Ag micro-nano film according to the invention;

FIG. 8 is a test chart of biological cell culture on the surface of a Ta @ Ag bimetallic film (81% Ta element doped) in a method for improving the biocompatibility of an Ag micro-nano film according to the invention;

fig. 9 is a test chart of culturing biological cells on the surface of a pure Ag film in the method for improving the biocompatibility of the Ag micro-nano film according to the present invention.

Detailed Description

The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.

The invention provides a method for improving biocompatibility of an Ag micro-nano film, which specifically comprises the following steps:

step 1: cleaning a silicon wafer:

soaking the cleaned silicon wafer substrate in an ethanol and acetone solution for 2-5 minutes, taking out the soaked silicon wafer, soaking the silicon wafer in deionized water for 2-5 minutes, and then taking out and drying the soaked silicon wafer;

step 2: preparing a Ta @ Ag bimetallic film by using a physical vapor deposition technology:

adjusting the temperature of the magnetron sputtering deposition equipment to be 25-150 ℃, the voltage to be 360-400V, controlling the current of the Ta target and the Ag target to be 0.5-6A, and controlling the current ratio of the Ag target to the Ta target to be 0.2: 1-1: 1. And (2) putting the silicon wafer dried in the step (1) into magnetron sputtering deposition equipment, keeping the magnetron sputtering deposition equipment in vacuum, introducing argon, and carrying out two-phase co-sputtering on 5-90% of Ta target and Ag according to the mass percentage to prepare the Ta @ Ag bimetallic film.

The Ta @ Ag bimetallic film is a Ta element doped Ag micro-nano composite film.

According to the method for improving the biocompatibility of the Ag micro-nano film, the Ta @ Ag bimetallic film is constructed by doping the Ta element, so that the biocompatibility of the pure Ag micro-nano film is improved.

The method for improving the biocompatibility of the Ag micro-nano film is described in detail by specific examples.