CN113102883A - Antibacterial material and preparation method thereof - Google Patents

Antibacterial material and preparation method thereof Download PDF

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Publication number
CN113102883A
CN113102883A CN202110326533.9A CN202110326533A CN113102883A CN 113102883 A CN113102883 A CN 113102883A CN 202110326533 A CN202110326533 A CN 202110326533A CN 113102883 A CN113102883 A CN 113102883A
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China
Prior art keywords
laser
antibacterial
base material
molybdenum
processing
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Chinese (zh)
Inventor
王洁
王盛
李海鹏
陈若涵
张静
游志明
高勇
胡耀程
许章炼
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Xian Jiaotong University
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Xian Jiaotong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/12—Working by laser beam, e.g. welding, cutting or boring in a special atmosphere, e.g. in an enclosure
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Apparatus For Disinfection Or Sterilisation (AREA)

Abstract

The invention discloses an antibacterial material and a preparation method thereof. The preparation method comprises the following steps: and treating the surface of the base material by using laser in an atmosphere containing oxygen and water vapor to enable the surface of the base material to have the hydrophobic structure. The surface of the antibacterial material has a hydrophobic structure, and also has molybdic acid, so that the antibacterial material has good antibacterial and bacteriostatic effects.

Description

Antibacterial material and preparation method thereof
Technical Field
The invention belongs to the field of medical antibiosis, and particularly relates to an antibacterial material and a preparation method thereof.
Background
In the prior art, some metal materials with antibacterial function (such as molybdenum-containing steel) are used in public places and medical places to achieve the purpose of resisting bacteria, but the metal materials with antibacterial function have poor antibacterial effect and insufficient antibacterial property, so that improvement of the materials is urgently needed to improve the antibacterial and bacteriostatic effects.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an antibacterial material and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
an antibacterial and bacteriostatic material comprises a molybdenum-containing matrix material, wherein the surface of the matrix material is provided with a hydrophobic structure, and the surface of the hydrophobic structure contains molybdic acid.
Preferably, the base material is molybdenum, an alloy containing molybdenum, a composite material having a molybdenum layer on the surface thereof, or a composite material having a molybdenum alloy layer on the surface thereof.
Preferably, the molybdenum alloy and the molybdenum alloy layer are made of a molybdenum alloy.
Preferably, the hydrophobic structure is a scale-like nanostructure.
The invention also provides a preparation method of the antibacterial and bacteriostatic material, which comprises the following steps:
and treating the surface of the base material by using laser in an atmosphere containing oxygen and water vapor to enable the surface of the base material to have the hydrophobic structure.
Preferably, during the process of processing the surface of the base material by using laser, the laser scanning mode adopts unidirectional scanning.
Preferably, during the process of processing the surface of the base material by using laser, the laser scanning mode adopts bidirectional cross scanning.
Preferably, the laser power is 0.10W-7.00W during the process of processing the surface of the substrate material by using the laser.
Preferably, the laser scanning interval is 15 μm to 90 μm during the laser processing of the surface of the base material.
Preferably, the laser scanning speed is 4mm/s-4000mm/s during the process of processing the surface of the base material by using laser.
Preferably, the atmosphere is air during the laser processing of the surface of the substrate material.
The surface of the antibacterial and bacteriostatic material has a hydrophobic structure, so that the surface of the antibacterial and bacteriostatic material can inhibit the formation of a biological film, further effectively inhibit the propagation of bacteria on the surface of the antibacterial and bacteriostatic material, and has a good antibacterial effect; meanwhile, the surface of the hydrophobic structure contains molybdic acid (H)2MoO4) Molybdic acid has extraordinary high-efficiency antibacterial performance, so that the antibacterial material has good antibacterial performance, and the antibacterial material has good antibacterial and antibacterial effects.
According to the preparation method of the antibacterial and bacteriostatic material, the hydrophobic structure can be processed on the surface of the matrix material containing molybdenum by using laser, and due to the characteristic of high energy of the laser, molybdenum in the hydrophobic structure reacts with oxygen and water vapor in the atmosphere to generate molybdic acid in the process of treating the surface of the matrix material by using the laser. The preparation method can process the antibacterial and bacteriostatic material with good antibacterial and bacteriostatic effects.
Drawings
FIG. 1(a) shows a laser scanning on a molybdenum metal sheet in a unidirectional scanning manner according to an embodiment of the present invention; fig. 1(b) shows that the laser scans the molybdenum metal sheet in a bidirectional scanning manner in the embodiment of the present invention.
FIG. 2(a) is a schematic view of the laser-treated Mo metal surface in example 1 of the present invention;
FIG. 2(b) is a schematic view showing the surface morphology of Mo metal after laser treatment in example 2 of the present invention;
FIG. 2(c) is a schematic view showing the surface morphology of Mo metal after laser treatment in example 3 of the present invention;
FIG. 2(d) is a schematic view of the laser-treated Mo metal surface in example 4 of the present invention;
FIG. 2(e) is a schematic view showing the surface morphology of Mo metal after laser treatment in example 5 of the present invention;
FIG. 2(f) is a schematic view of the laser-treated Mo metal surface in example 6 of the invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
For convenience of experiments, the laser processing is performed on the molybdenum sheet metal in the experiments, and when the base material is an alloy containing molybdenum, a composite material with a molybdenum layer on the surface, or a composite material with a molybdenum alloy layer on the surface, the principle is the same, and the description is omitted in the present invention.
In the following embodiments of the present invention, a femtosecond laser is used to process the surface of a molybdenum metal sheet, and a scaly nanostructure is formed on the surface of the molybdenum metal sheet, wherein the scaly nanostructure is a hydrophobic structure and contains molybdic acid on the surface. Adopting staphylococcus aureus ATCC25923 standard strain, and comparing the OD of the molybdenum metal sheet with that of a blank control group, wherein the surface of the molybdenum metal sheet is processed by laser600And obtaining the antibacterial effect of the laser treatment on the surface of the molybdenum metal sheet by the quotient of the values. In the laser processing, the laser scanning mode is a unidirectional scanning (as shown in fig. 1 (a)) or a cross scanning (as shown in fig. 1 (b)).
When the surface of the molybdenum metal sheet is subjected to laser treatment, the used laser power is 0.10W-7.00W, the laser scanning interval is 15 mu m-90 mu m, and the laser scanning speed is 4mm/s-4000 mm/s. The selection of laser power, laser scanning interval and laser scanning rate is very important for the formation of hydrophobic structures on the surface of the molybdenum metal sheet and the formation of molybdic acid. The laser parameters are favorable for obtaining the hydrophobic molybdenum metal sheet surface structure and are also favorable for the formation of molybdic acid, so that the antibacterial and bacteriostatic properties of the metal sheet surface are improved.
Single colonies were picked and inoculated in MRS liquid medium and shake-cultured at 37 ℃. Adjusting OD of bacterial liquid of strain to be detected600And (5) taking 50 mu l of the bacterial liquid and 150 mu l of blank culture medium based on polyethylene 24-well plates, taking 3 duplicate wells of each group, taking the blank culture medium without adding the bacterial liquid as a negative control, and incubating for 24 hours in an incubator at 37 ℃. After the incubation was completed, the culture solution was gently aspirated off, washed 3 times with sterile PBS, washed free bacteria off, and dried at room temperature; fixing with methanol for 15min, dyeing with 1% crystal violet dye solution for 15min, washing with sterile water for 3 times until the control hole is colorless, and air drying at room temperature. Adding 200 μ l of anhydrous ethanol into each well for dissolving, shaking for 1min, and measuring the light absorption value of each well at 595nm of an enzyme-labeling instrument, wherein Staphylococcus aureus ATCC25923 is a quality control strain.
The processing parameters and results of the examples and comparative examples of the present invention are shown in Table 1,
TABLE 1
Figure BDA0002994874500000041
As can be seen from Table 1, the OD of the sample prepared by example 1 and the blank metal control group600The ratio of the values proves that the laser treatment of the molybdenum surface can actually improve the hydrophobic property of the molybdenum metal sample surface, thereby inhibiting the formation of a biological film. As can be seen from Table 1, the results of comparative example 2 and examples 1 to 4 show that the molybdenum sheets processed by the laser according to the present invention have better antibacterial properties than the original molybdenum sheets. In the invention, the molybdenum metal is processed by laser in the atmosphere to form MoO on the surface3，MoO3Reaction with water to form molybdic acid (H)2MoO4). Under the action of the two effects, the antibacterial performance of the molybdenum metal surface treated by the laser is better.
The topography of the Mo metal surface after laser treatment of each example is shown in fig. 2(a) -2 (f), and it can be seen that the Mo metal surface after laser treatment has a scaly nanostructure.
Compared with the traditional metal or alloy material, the laser treatment of the molybdenum metal surface forms molybdenum oxide on the surface after the laser treatment in the air, and the molybdenum oxide reacts with water to generate molybdate radicals. The molybdenum metal material prepared by the method has the advantages of high repeatability, high yield, simple preparation process, good biocompatibility, good antibacterial performance, high metal strength, corrosion resistance and the like. The material can be used for improving the antibacterial performance of related parts and facilities in public areas (such as toilets, operating tables, medical instruments and the like) in hospitals and the like, and can also be used as a biological implant.

Claims (10)

1. An antibacterial and bacteriostatic material is characterized by comprising a matrix material containing molybdenum, wherein the surface of the matrix material is provided with a hydrophobic structure, and the surface of the hydrophobic structure contains molybdic acid.
2. An antibacterial and bacteriostatic material according to claim 1, wherein the base material is molybdenum, an alloy containing molybdenum, a composite material with a molybdenum layer on the surface or a composite material with a molybdenum alloy layer on the surface.
3. An antibacterial and bacteriostatic material according to claim 1 or 2 wherein the hydrophobic structure is a scaly nanostructure.
4. A method for preparing an antibacterial and bacteriostatic material according to any one of claims 1 to 3, which is characterized by comprising the following steps:
and treating the surface of the base material by using laser in an atmosphere containing oxygen and water vapor to enable the surface of the base material to have the hydrophobic structure.
5. The preparation method according to claim 4, wherein the laser scanning mode adopts unidirectional scanning during the process of processing the surface of the base material by the laser.
6. The method according to claim 4, wherein the laser scanning is bidirectional criss-cross scanning during the processing of the surface of the base material with the laser.
7. The method according to any one of claims 4 to 6, wherein the laser power is 0.10W to 7.00W during the processing of the surface of the base material with the laser.
8. The method according to any one of claims 4 to 6, wherein the laser scanning pitch is 15 μm to 90 μm during the processing of the surface of the base material with the laser.
9. The method according to any one of claims 4 to 6, wherein the scanning speed of the laser is 4mm/s to 4000mm/s during the processing of the surface of the base material with the laser.
10. The method according to any one of claims 4 to 6, wherein air is used as an atmosphere during the laser processing of the surface of the base material.
CN202110326533.9A 2021-03-26 2021-03-26 Antibacterial material and preparation method thereof Pending CN113102883A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101219506A (en) * 2008-01-07 2008-07-16 江苏大学 Laser production method for metal base ultra-hydrophobicity micro-structure surface
CN103433618A (en) * 2013-07-25 2013-12-11 长春理工大学 Method for controlling size and distribution of metal surface micro-nanostructure
DE102012017483A1 (en) * 2012-09-04 2014-03-06 Hochschule für angewandte Wissenschaften München Structuring first thin layer using laser, comprises applying first thin layer made of first material, on further second layer made of second material, in which first- and second materials exhibit different optical absorption coefficients
CN104439708A (en) * 2014-11-18 2015-03-25 清华大学 Super-hydrophobic high-adhesion metal surface and manufacturing method thereof
CN106141438A (en) * 2015-04-03 2016-11-23 长春理工大学 A kind of method utilizing laser plasma filament to prepare metal multifunction surface
US20200009687A1 (en) * 2018-09-20 2020-01-09 Beihang University Preparation of antimicrobial surface for medical devices
CN111774731A (en) * 2020-06-24 2020-10-16 北京航空航天大学 Ultrafast laser preparation method for bacteriostatic surface of public article

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101219506A (en) * 2008-01-07 2008-07-16 江苏大学 Laser production method for metal base ultra-hydrophobicity micro-structure surface
DE102012017483A1 (en) * 2012-09-04 2014-03-06 Hochschule für angewandte Wissenschaften München Structuring first thin layer using laser, comprises applying first thin layer made of first material, on further second layer made of second material, in which first- and second materials exhibit different optical absorption coefficients
CN103433618A (en) * 2013-07-25 2013-12-11 长春理工大学 Method for controlling size and distribution of metal surface micro-nanostructure
CN104439708A (en) * 2014-11-18 2015-03-25 清华大学 Super-hydrophobic high-adhesion metal surface and manufacturing method thereof
CN106141438A (en) * 2015-04-03 2016-11-23 长春理工大学 A kind of method utilizing laser plasma filament to prepare metal multifunction surface
US20200009687A1 (en) * 2018-09-20 2020-01-09 Beihang University Preparation of antimicrobial surface for medical devices
CN111774731A (en) * 2020-06-24 2020-10-16 北京航空航天大学 Ultrafast laser preparation method for bacteriostatic surface of public article

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