CN112062479A - Laser preparation method of self-cleaning antibacterial glass - Google Patents
Laser preparation method of self-cleaning antibacterial glass Download PDFInfo
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- CN112062479A CN112062479A CN202010960356.5A CN202010960356A CN112062479A CN 112062479 A CN112062479 A CN 112062479A CN 202010960356 A CN202010960356 A CN 202010960356A CN 112062479 A CN112062479 A CN 112062479A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/06—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
- C03C17/10—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals by deposition from the liquid phase
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/02—Re-forming glass sheets
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/251—Al, Cu, Mg or noble metals
- C03C2217/253—Cu
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/251—Al, Cu, Mg or noble metals
- C03C2217/254—Noble metals
- C03C2217/255—Au
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/25—Metals
- C03C2217/251—Al, Cu, Mg or noble metals
- C03C2217/254—Noble metals
- C03C2217/256—Ag
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
Abstract
The invention discloses a laser preparation method of self-cleaning antibacterial glass. Firstly, washing a prepared chemical solution to the surface of a metal substrate, and simultaneously covering the bottom surface of glass with the metal substrate; thirdly, the metal substrate is irradiated by utilizing ultrafast laser to penetrate through the glass, the glass at the interface is melted, the microstructure on the metal is transferred to the glass, meanwhile, the nano particles in the solution are reduced and adsorbed on the glass microstructure, and then, the glass is annealed, so that a double-size micro-nano structure covering the non-polar nano particles is generated on the surface of the glass. The surface has an excellent self-cleaning super-hydrophobic function, oil stains and the like on the surface of glass can be removed by using a small amount of water and labor, water stain residues are almost eliminated, and the cleaning difficulty in the use process is reduced. Moreover, the super-hydrophobic property can resist bacterial adhesion, and the nanoparticles can kill the adhered bacteria, so that the glass surface has excellent antibacterial/bactericidal functions. The preparation method is simple, has universality and is suitable for glass made of various materials. And the prepared glass has unchanged mechanical property and good light transmittance, and is suitable for large-scale commercial production.
Description
Technical Field
The invention relates to a laser preparation method of self-cleaning antibacterial glass, and belongs to the technical field of glass manufacturing.
Background
Along with the gradual improvement of the material and cultural life of people, people pay more and more attention to the environmental sanitation and the cleanliness of human contact surfaces. In the field of using glass as a table top, such as a tea table working table, a dining table working table, a kitchen working table and an electronic scale cover plate installed on an electronic scale, the glass table is easy to contact with various liquids such as oil stains, and in the prior art, the glass table is mainly cleaned by hand wiping, so that the working intensity of a user is high, and the cleaning is not thorough. The surface of the existing self-cleaning glass is mostly super-hydrophilic coated glass, and a good cleaning effect can be realized only under the condition of large water flow.
In addition, the glass platforms in these home areas are often in a humid environment and often contact with food, and are easily infested with microorganisms and bacteria, and viral infections caused by the infested microorganisms and bacteria cause various health problems to people, so that the glass is required to have an antibacterial/bactericidal function. At present, common glass is used for the devices, and the devices have no self-cleaning and antibacterial functions.
With the research and development of high-frequency and high-power industrial ultrafast lasers, ultrafast lasers can be subjected to micro-nano processing on the surfaces of various materials such as silicon, stainless steel, copper, titanium and the like, and are used for preparing superhydrophobic surfaces with self-cleaning functions. Although research has reported that the microstructure can be prepared on the surface of the glass by using the ultrafast laser, the type of the processed microstructure is limited due to the light transmittance of the glass, and after the laser reaches the surface of the glass to perform material removal and structure induction, the residual laser energy passes through the glass to generate a thermal effect on the processing platform, which is easy to cause thermal damage to the surface of the glass. In addition, in order to obtain the antibacterial function of the glass, processes such as film coating and the like need to be added, and the processing difficulty is increased.
Disclosure of Invention
Aiming at the problems, the invention provides a laser preparation method of self-cleaning antibacterial glass. According to the preparation method of the glass, a hydrophobic material coating is not needed, the bottom surface of the glass is covered with a metal substrate, ultrafast laser penetrates through the glass to irradiate the metal substrate, a micro-nano structure is processed on the surface of the glass, and then annealing treatment is carried out, so that a double-size micro-nano structure covering nonpolar nano particles is generated on the surface of the glass. The surface has an excellent self-cleaning super-hydrophobic function, oil stains and the like on the surface of glass can be removed by using a small amount of water and labor, water stain residues are almost eliminated, and the cleaning difficulty in the use process is reduced. Moreover, the super-hydrophobic property can resist bacterial adhesion, and the nanoparticles can kill the adhered bacteria, so that the glass surface has excellent antibacterial/bactericidal functions. In order to achieve the purpose, the invention is realized by the following technical scheme, which comprises the following specific steps:
step one, performing deoiling cleaning treatment on the surface of glass;
step two, using metal as a substrate, and polishing, deoiling and cleaning the surface of the metal substrate;
thirdly, washing the prepared chemical solution on the surface of the metal matrix, and simultaneously slowly covering the glass in the first step on the surface of the metal substrate in the second step, wherein the liquid film is filled between the glass and the metal;
and step four, processing the micro-nano structure. And (3) carrying out micro-nano processing on the interface of the glass and the metal substrate processed in the step three by adopting ultrafast laser, enabling the laser to penetrate through the glass to manufacture a micro-nano structure on the surface of the metal substrate, melting the glass at the interface, transferring the micro-structure on the metal onto the glass, and simultaneously replacing the nano particles in the chemical solution.
And step five, unloading. And (3) vertically and upwards removing the glass from the metal substrate, forming a mirror image micro-nano structure matched with the metal substrate on the surface of the glass, and randomly distributing the replaced metal nano particles on the surface of the glass micro-nano structure due to the viscosity of the glass.
And step six, annealing. And E, placing the glass treated in the step V into an annealing furnace for annealing, and finishing the preparation of the self-cleaning antibacterial glass.
The glass in the step one is a glass platform material which can be used in the household field, and comprises materials such as common glass, toughened glass and organic glass;
the metal in the second step comprises copper, titanium, aluminum, iron and metal alloy materials thereof;
the chemical solution in the third step comprises metal ion compound solution of gold, silver, copper, titanium and the like;
and fourthly, processing the micro-nano structure on the surface of the material by the ultrafast laser, wherein the specific parameters are as follows: the laser wavelength is 193-1070 nm, the laser power is 0.5-1000W, the pulse frequency is 1 k-5M Hz, the pulse width is 50 fs-100 ns, and the scanning speed is 10-3000 mm/s;
the micro-nano structure graph obtained by laser processing in the fourth and fifth steps comprises the following steps: LIPSS structures, microcone structures, and combinations thereof. The LIPSS period is 600 nm-1 μm; the height of the micro-cone structure is 50 nm-10 μm, and the distance is 50 nm-1 μm;
wherein, the metal nanoparticles described in the fourth and fifth steps are metals capable of releasing antibacterial ions, and comprise: gold, silver, copper, titanium, etc.;
wherein, the hydrophobic structure with the sterilization function and the self-cleaning function is maintained in the sixth step, the contact angle is more than 150 ℃, and the light transmittance is more than 90%;
and sixthly, annealing specifically comprises the following steps: heating to 200 ℃ at the speed of 10-12 ℃/min, preserving the heat for 1 hour, and then cooling to room temperature at the speed of 6-10 ℃/min.
The invention discloses a laser preparation method of self-cleaning antibacterial glass. The metal substrate is covered on the bottom surface of the glass, ultrafast laser penetrates through the glass to irradiate the metal substrate and annealing treatment is carried out, so that a double-size micro-nano structure covered with nonpolar nano particles is generated on the surface of the glass. The surface has an excellent self-cleaning super-hydrophobic function, oil stains and the like on the surface of glass can be removed by using a small amount of water and labor, water stain residues are almost eliminated, and the cleaning difficulty in the use process is reduced. Moreover, the super-hydrophobic property can resist bacterial adhesion, and the nanoparticles can kill the adhered bacteria, so that the glass surface has excellent antibacterial/bactericidal functions.
The invention has the advantages that:
1) the method utilizes laser processing, can adapt to the processing requirements of various glass materials by changing laser parameters.
2) According to the method, the ultrafast laser is used for preparing the micro-nano structure pattern, the heat damage and the heat affected zone are small, various micro-nano patterns can be accurately prepared, and the original mechanical properties of glass can be maintained.
3) The method uses metal as substrate, can fully utilize laser energy, reduce energy loss, and prevent thermal damage caused by overheating of glass bottom surface.
4) The method utilizes the laser to irradiate the chemical solution between the glass and the metal substrate to prepare the bactericidal nano-particles, thereby reducing the process steps.
5) The micro-nano structure in the method plays a role in storing nano particles, can slowly release bactericidal ions and ensures long-acting antibiosis.
6) The glass surface prepared by the method has excellent self-cleaning effect, and the cleaning difficulty in the use process is reduced. Has good antibacterial effect, and can prevent the threat of bacterial growth to human health in household use.
7) In the method, the used metal substrate can be repeatedly used, and the preparation cost is reduced.
8) The size of the nano particles on the glass surface prepared by the method is about 100nm, and according to the Mie scattering theory and the Rayleigh scattering theory, the smaller surface roughness can realize the higher surface anti-scattering function. In the visible light-near infrared spectrum region with the wavelength larger than the surface nano particle size, the optical transmittance of the processed glass is not affected basically, and even the anti-reflection-scattering function in a local range is generated. Therefore, the glass processed by the method has good light transmittance, and the original performance and the aesthetic degree of the glass are ensured.
9) The method has the advantages of simple and flexible processing and high processing speed, and is expected to improve the production efficiency in actual production.
Description of the drawings:
FIG. 1 is a schematic view of the processing of the present invention
FIG. 2 contact Angle of glass surface prepared in example 1
FIG. 3 comparison of antibacterial effect on glass surface prepared in example 1-fluorescence of live bacteria
The specific implementation mode is as follows:
the present invention will be further described with reference to specific examples, which are intended to be illustrative only and not limiting:
example 1
Polishing the surfaces of toughened glass and a copper substrate, ultrasonically cleaning the surfaces for 10 minutes by using alcohol and acetone, and drying;
step two, preparing AgNO3A solution of solubility1.5M；
Thirdly, washing the prepared solution on the surface of the copper substrate by using a water gun, and slowly covering the surface of the copper substrate with toughened glass;
fourthly, placing the tempered glass after surface treatment and a copper substrate sample below the tempered glass under a femtosecond laser (with the wavelength of 1064nm) to perform laser-induced surface micro-nano structure processing, wherein the laser processing parameters are set as follows: the power is 8W, the pulse width is 500fs, the frequency is 400kHz, the scanning speed is 800mm/s, the scanning distance is 35 mu m, and the scanning is carried out for 5 times, so that a micro-cone structure covered with silver nano particles is obtained on the surface of the toughened glass;
step five, vertically and upwardly removing the glass from the metal substrate;
and step six, annealing treatment is carried out, the glass treated in the step five is heated to 200 ℃ at the speed of 10-12 ℃/min and is kept for 1 hour, and then the glass is cooled to room temperature at the speed of 6-10 ℃/min. At this time, the preparation of the self-cleaning antibacterial glass is finished.
Example 2
Grinding and polishing the surfaces of common glass and a titanium substrate, ultrasonically cleaning the surfaces for 10 minutes by using alcohol and acetone, and drying the surfaces;
step two, preparing AuCl4A solution with a solubility of 0.5M;
thirdly, washing the prepared solution on the surface of the titanium substrate by using a water gun, and slowly covering the surface of the copper substrate with common glass;
placing the common glass after surface treatment and a titanium substrate sample below the common glass under a femtosecond laser (with the wavelength of 1064nm) to perform laser-induced surface micro-nano structure processing, wherein the laser processing parameters are set as follows: the power is 5W, the pulse width is 800fs, the frequency is 200kHz, the scanning speed is 1000mm/s, the scanning distance is 30 mu m, and the micro-cone structure covered with gold nano-particles is obtained on the surface of the common glass after 5 times of scanning;
step five, vertically and upwardly removing the glass from the metal substrate;
and step six, annealing treatment is carried out, the glass treated in the step five is heated to 200 ℃ at the speed of 10-12 ℃/min and is kept for 1 hour, and then the glass is cooled to room temperature at the speed of 6-10 ℃/min. At this time, the preparation of the self-cleaning antibacterial glass is finished.
Example 3
Firstly, polishing the surfaces of organic glass and a stainless steel substrate, ultrasonically cleaning the surfaces for 10 minutes by using alcohol and acetone, and drying;
preparing a CuCl solution with the solubility of 1.0M;
thirdly, washing the prepared solution on the surface of the stainless steel substrate by a water gun, and slowly covering the organic glass on the surface of the copper substrate;
placing the organic glass subjected to surface treatment and a stainless steel substrate sample below the organic glass under a femtosecond laser (with the wavelength of 1064nm) to perform laser-induced surface micro-nano structure processing, wherein the laser processing parameters are set as follows: the power is 7W, the pulse width is 100fs, the frequency is 300kHz, the scanning speed is 1500mm/s, the scanning distance is 40 mu m, scanning is carried out for 10 times, and a micro-cone structure covered with copper nano particles is obtained on the surface of toughened glass;
step five, vertically and upwardly removing the glass from the metal substrate;
and step six, annealing treatment is carried out, the glass treated in the step five is heated to 200 ℃ at the speed of 10-12 ℃/min and is kept for 1 hour, and then the glass is cooled to room temperature at the speed of 6-10 ℃/min. At this time, the preparation of the self-cleaning antibacterial glass is finished.
Claims (8)
1. A laser preparation method of self-cleaning antibacterial glass is characterized by comprising the following steps:
step one, performing deoiling cleaning treatment on the surface of glass;
step two, using metal as a substrate, and polishing, deoiling and cleaning the surface of the metal substrate;
thirdly, washing the prepared chemical solution on the surface of the metal matrix, and simultaneously slowly covering the glass in the first step on the surface of the metal substrate in the second step, wherein the liquid film is filled between the glass and the metal;
and step four, processing the micro-nano structure. And (3) carrying out micro-nano processing on the interface of the glass and the metal substrate processed in the step three by adopting ultrafast laser, enabling the laser to penetrate through the glass to manufacture a micro-nano structure on the surface of the metal substrate, melting the glass at the interface, transferring the micro-structure on the metal onto the glass, and simultaneously replacing the nano particles in the chemical solution.
And step five, unloading. And (3) vertically and upwards removing the glass from the metal substrate, forming a mirror image micro-nano structure matched with the metal substrate on the surface of the glass, and randomly distributing the replaced metal nano particles on the surface of the glass micro-nano structure due to the viscosity of the glass.
And step six, annealing. And E, placing the glass treated in the step V into an annealing furnace for annealing, and finishing the preparation of the self-cleaning antibacterial glass.
2. The glass according to claim 1 is a glass platform material which can be used in the household field, and comprises materials such as common glass, tempered glass and organic glass.
3. The metal substrate of claim 1 comprising copper, titanium, aluminum, iron, and metal alloy materials thereof.
4. The method for processing the micro-nano structure on the surface of the material by using the ultrafast laser according to claim 1, wherein the specific parameters are as follows: the laser wavelength is 193-1070 nm, the laser power is 0.5-1000W, the pulse frequency is 1 k-5M Hz, the pulse width is 50 fs-100 ns, and the scanning speed is 10-3000 mm/s.
5. The micro-nano structure graph obtained by utilizing laser processing according to claim 1, comprising: LIPSS structures, microcone structures, and combinations thereof. The LIPSS period is 600 nm-1 μm; the height of the micro-cone structure is 50 nm-10 μm, and the distance is 50 nm-1 μm.
6. The metal nanoparticle of claim 1, being an antimicrobial ion releasable metal nanoparticle comprising: gold, silver, copper, titanium, and the like.
7. The obtained hydrophobic structure with bactericidal function while maintaining self-cleaning function according to claim 1, having a contact angle >150 ℃ and a light transmittance > 90%.
8. The annealing according to claim 1, performed in particular by: heating to 200 ℃ at the speed of 10-12 ℃/min, preserving the heat for 1 hour, and then cooling to room temperature at the speed of 6-10 ℃/min.
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Cited By (4)
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| CN113210347A (en) * | 2021-03-25 | 2021-08-06 | 广东工业大学 | Amorphous alloy antibacterial surface and manufacturing method thereof |
| CN113210362A (en) * | 2021-03-25 | 2021-08-06 | 广东工业大学 | Cleaning method for antibacterial surface of alloy microstructure |
| CN113636760A (en) * | 2021-09-02 | 2021-11-12 | 青岛理工大学 | Antifogging self-cleaning glass and preparation method thereof |
| CN113967796A (en) * | 2021-10-26 | 2022-01-25 | 江苏大学 | Method for preparing super-hydrophobic surface by laser shock imprinting of micro-nano particles on surface of aluminum alloy |
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| CN113967796B (en) * | 2021-10-26 | 2023-09-22 | 江苏大学 | Method for preparing superhydrophobic surface by laser impact imprinting of micro-nano particles on aluminum alloy surface |
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