CN110150317B - PDMS-ZnO/Au sterilization material with noble metal modified semiconductor nano-pillar array structure and preparation method thereof - Google Patents
PDMS-ZnO/Au sterilization material with noble metal modified semiconductor nano-pillar array structure and preparation method thereof Download PDFInfo
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- CN110150317B CN110150317B CN201910461980.8A CN201910461980A CN110150317B CN 110150317 B CN110150317 B CN 110150317B CN 201910461980 A CN201910461980 A CN 201910461980A CN 110150317 B CN110150317 B CN 110150317B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
Abstract
A PDMS-ZnO/Au sterilization material with a noble metal modified semiconductor nano-pillar array structure and a preparation method thereof belong to the technical field of semiconductor sterilization materials. Selecting PDMS as a substrate, growing a ZnO nano-pillar array on the PDMS by a hydrothermal method, and then compounding Au nano-particles on the surface of ZnO by a photoreduction method to obtain the sterilizing material. The prepared sterilization material is used as a bionic nano-column type sterilization surface, structures like spikes are distributed on the sterilization material, and after bacteria are adhered, the micro-nano structure on the surface can inactivate the bacteria by a running mechanism of slowly tearing cell membranes; after the Au nano particles are introduced, the visible light can be utilized, the separation of photo-generated holes and photo-generated electrons can be promoted through the surface plasmon resonance effect, the recombination of current carriers is effectively inhibited, the photocatalytic activity is further improved, and active oxygen radicals generated in the photocatalytic process have a strong sterilization function.
Description
Technical Field
The invention belongs to the technical field of semiconductor sterilization materials, and particularly relates to a PDMS-ZnO/Au sterilization material with a noble metal modified semiconductor nano-pillar array structure and a preparation method thereof.
Background
Under the situation that environmental problems are more and more serious and pathogenic microorganisms are visible everywhere, the development of a novel multifunctional, safe and environment-friendly sterilization material is particularly important. The sterilization materials are various in types, and the photocatalytic sterilization material has strong sterilization activity, is nontoxic and does not release heavy metal ions, so that the photocatalytic sterilization material is concerned. Zinc oxide (ZnO) is considered one of the most promising photocatalytic bactericides due to its good chemical stability, commercial availability, ease of preparation of diverse structures, and the like. When photons larger than the forbidden band gap irradiate ZnO, the photons are excited to generate hole-electron pairs, and then active oxygen groups OH and O with strong oxidizing property are generated2 -They destroy the permeability of the cell wall (membrane) and the structure of DNA of bacteria by oxidizing coenzyme a of bacteria, causing bacteria to die. ZnO is used as a photocatalytic sterilization material, has the characteristic of broad-spectrum sterilization, is only used as a catalyst to participate in the reaction in the sterilization process, is not consumed theoretically, and has lasting sterilization performance. However, the forbidden band gap of ZnO is wide, and can only be excited by ultraviolet light accounting for 4% of solar energy, and the practical application of ZnO is limited due to high recombination rate of semiconductor carriers and low photon efficiency.
At present, there are many methods for improving the photocatalytic efficiency of ZnO, and the scheme of the ZnO-based heterostructure compounded by the noble metal nanoparticles attracts extensive attention of researchers. In the semiconductor/noble metal heterostructure, due to the special energy band structure and the carrier transmission characteristic, hole electron recombination can be effectively inhibited in the photocatalytic reaction, and the catalytic activity of the photocatalyst is improved; and the noble metal nano particles have Surface Plasmon Resonance (SPR) effect, so that the absorption of visible light can be expanded, and the effective utilization of sunlight is realized.
Elena P.Ivanova et al discovered that the special nano-pillar structure on the surface of the cicada wing can kill some bacteria attached to the surface of the cicada wing in 2012, and the special sterilization mode provides a thought for developing a novel sterilization material (Small,2012,8(16): 2489-). 2494). Inspired by this, Guingshun Yi et al found that ZnO having a nanopillar array structure can kill bacteria attached to a surface by means of mechanical sterilization (Small,2018, 14(14): 1703159). Meanwhile, ZnO as a photocatalytic sterilization material with excellent performance can be sterilized by releasing active oxygen groups with strong oxidizing property, and Priyanka Sathe et al prepare ZnO nano-pillar arrays on the surface of a fishing net by a hydrothermal method to obtain the photocatalytic sterilization performance (Scientific Reports, 2017,7(1): 3624). At present, the report of combining the physical structure sterilization and the photocatalytic sterilization of the semiconductor nano material does not exist, and the semiconductor nano material is endowed with a special array structure, so that the high-efficiency sterilization is realized, and the defect that the photocatalytic type bactericide can only act after being excited by light is effectively overcome.
Disclosure of Invention
The invention aims to provide a PDMS-ZnO/Au sterilization material with a noble metal modified semiconductor nano-pillar array structure and a preparation method thereof. The film formation of Polydimethylsiloxane (PDMS) can be adjusted by the curing temperature and the curing time; the size of the ZnO nano-column array can be adjusted by the conditions of hydrothermal reaction; the size of the Au nano particles can be adjusted through the concentration of the aqueous solution containing the gold acid and the illumination time; the ratio of ZnO to Au can be adjusted by changing the ratio of the added zinc source and gold source and the illumination time. The PDMS-ZnO/Au composite membrane can show a good sterilization effect by means of a self physical structure through a mechanical sterilization mode under the condition of no light, and combines the physical structure sterilization mode and the photocatalytic sterilization mode under the visible light, so that the PDMS-ZnO/Au composite membrane can show a stronger sterilization effect after being excited by the visible light, and the defect that the photocatalytic sterilization agent can only act after being excited by the light is effectively overcome.
The invention relates to a preparation method of a PDMS-ZnO/Au sterilization material with a noble metal modified semiconductor nano-pillar array structure, which comprises the following steps:
1) and (3) mixing a PDMS monomer and a curing agent according to the ratio of 8-12: 1, uniformly stirring, performing vacuum drying to remove bubbles, and curing at 50-100 ℃ for 1-3 hours to obtain a PDMS sample film;
2) taking 50-100 mL of 10-20 mM zinc salt alcoholic solution, dropwise adding 30-60 mL of 10-50 mM alkali alcoholic solution, and heating and stirring the obtained mixed solution at 50-100 ℃ for 1-3 hours to obtain ZnO seed solution; then soaking the PDMS sample film obtained in the step 1) in the ZnO seed solution for 1-5 min to enable the ZnO seeds to uniformly and compactly cover the surface of the PDMS sample film, and then heating the PDMS sample film at 50-100 ℃ for 30-60 min to enable the bonding force between PDMS and ZnO to be stronger, so as to obtain the PDMS sample film fixed with the ZnO seeds;
3) taking 50-150 mL of 20-60 mM zinc salt aqueous solution, adding 50-100 mL of 20-60 mM Hexamethylenetetramine (HMTA) aqueous solution, stirring at room temperature for 10-30 min, transferring the mixed solution into a reaction kettle, immersing the PDMS sample film fixed with the ZnO seeds obtained in the step 2) into the mixed solution, heating at 80-120 ℃ for 6-12 hours, cooling to room temperature, repeatedly washing with deionized water, and drying to obtain a PDMS-ZnO sample film;
4) placing the PDMS-ZnO sample film obtained in the step 3) into an aqueous solution containing gold acid with the mass fraction of 0.01-0.2%, adjusting the pH to 7-10 by using an aqueous solution of alkali with the mass fraction of 1-5%, illuminating for 20-60 min at room temperature, taking out the sample film after the reaction is finished, repeatedly cleaning by using deionized water, and drying to obtain the PDMS-ZnO/Au sterilization material.
The zinc salt is one of zinc acetate, zinc sulfate, zinc nitrate or zinc chloride; the aururic acid is one of chloroauric acid, gold acetate, chlorine [ tris (2, 4-di-tert-butylphenyl) phosphite ] gold and the like; the alcohol is one of methanol, ethanol, ethylene glycol or glycerol; the alkali is one of ammonia water, sodium hydroxide, sodium carbonate, potassium hydroxide, hexamethylene tetramine, triethylamine and the like; the light source for illumination is one of simulated sunlight, a mercury lamp, a xenon lamp, an LED lamp and the like, and the wavelength range of the light source is 200-800 nm.
The method for preparing the PDMS-ZnO/Au sterilization material has the advantages of simple equipment, mild conditions and cheap and easily-obtained chemical reagents. Firstly, selecting PDMS with high mechanical property and easy molding as a substrate, growing a ZnO nano-column array on the PDMS by a hydrothermal method, and then compounding Au nano-particles on the surface of ZnO by adopting a photoreduction method to finally obtain the PDMS-ZnO/Au sterilization material. The PDMS-ZnO/Au prepared by the invention is used as a bionic nano-column type sterilization surface, structures like spikes are distributed on the surface, and when bacteria are adhered, the micro-nano structure on the surface can inactivate the bacteria by slowly tearing the operation mechanism of cell membranes; after Au nano particles are introduced to the surface of semiconductor ZnO, on one hand, visible light can be utilized, on the other hand, separation of photo-generated holes and photo-generated electrons can be promoted through the Surface Plasmon Resonance (SPR) effect, recombination of current carriers is effectively inhibited, the photocatalytic activity is further improved, and active oxygen Radicals (ROS) generated in the photocatalytic process have a strong sterilization function. Experimental results show that the PDMS-ZnO/Au has a good sterilization effect. According to the invention, the physical structure sterilization and photocatalytic sterilization modes of the semiconductor nano material are combined for the first time, the prepared PDMS-ZnO/Au has stable and efficient sterilization performance, the raw material cost is low, the preparation method is simple, and mass production can be realized, so that the PDMS-ZnO/Au has a good application prospect in the fields of marine antifouling paint or medical coatings and the like.
Drawings
FIG. 1: scanning electron microscope pictures of the PDMS-ZnO/Au sterilization material prepared in the embodiment 1;
FIG. 2: an X-ray diffraction spectrum of the PDMS-ZnO/Au sterilization material prepared in the embodiment 1;
FIG. 3: the antibacterial effect graphs of the PDMS-ZnO/Au antibacterial material prepared in the application example 1 on escherichia coli under visible light (a) without light (b), under visible light (c) without light (d) and under a control group (e);
Detailed Description
The technical solution of the present invention is described in more detail with the following specific examples, but the examples are not to be construed as limiting the present invention.
Example 1
1) The PDMS monomers and curing agent were mixed as follows 10: 1, stirring uniformly, placing in a vacuum drying oven to remove bubbles, and curing for 1 hour at 80 ℃ to obtain a PDMS sample film;
2) taking 80mL of 10mM zinc acetate ethanol solution, dropwise adding 40mL of 30mM sodium hydroxide ethanol solution into the 10mM zinc acetate ethanol solution, heating and stirring the obtained mixed solution at 60 ℃ for 2 hours to obtain ZnO seed solution, then soaking the PDMS sample film obtained in the step 1) in the ZnO seed solution for 2 minutes to enable ZnO seeds to uniformly and densely cover the surface of PDMS, and then heating the PDMS in a 90 ℃ oven for 30 minutes to enable the bonding force between PDMS and ZnO to be stronger, thus obtaining the PDMS sample film fixed with the ZnO seeds;
3) mixing 100mL of 60mM zinc nitrate aqueous solution and 100mL of 60mM HMTA aqueous solution respectively, stirring at room temperature for 20min, transferring the solution into a reaction kettle, immersing the PDMS sample film fixed with the ZnO seeds into the mixed solution, heating at 90 ℃ for 6 hours, cooling to room temperature, repeatedly washing with deionized water, and drying to obtain a PDMS-ZnO sample film;
4) placing the PDMS-ZnO sample film obtained in the step 3) into a chloroauric acid aqueous solution with the mass fraction of 0.1%, adjusting the pH to 9 with a sodium hydroxide aqueous solution with the mass fraction of 2%, irradiating for 30min with a xenon lamp light source with the wavelength of 350-780 nm at room temperature, taking out the sample after the reaction is finished, repeatedly cleaning with deionized water, and drying to obtain the PDMS-ZnO/Au sterilization material.
Example 1 Performance testing
Soaking the PDMS-ZnO/Au sterilization material in 75% volume fraction medical alcohol for sterilization, taking out after 24 hours, placing in a super clean bench, drying with sterile wind, and sucking 100 μ L of Escherichia coli suspension (10 μ L) with a sterile gun head6CFU/mL, ATCC 25922) is lightly hammered on the surface of the sterilization material, the sterilization material is placed for 30 minutes under visible light or no light, the whole is transferred into sterilized normal saline, vortex oscillation is carried out for 8 seconds, 200 mu L of bacterial liquid is taken out and coated on a culture dish by a triangular rodThe colony number was counted after the culture dish was placed upside down in a 37 ℃ incubator for 12 hours on the LB solid medium, and the bactericidal performance was evaluated. The result shows that the PDMS-ZnO/Au can kill all escherichia coli within 30 minutes in short time under the condition of visible light, and the sterilization rate of the PDMS-ZnO/Au under the condition of no light is up to 65.5 percent, which indicates that the prepared PDMS-ZnO/Au has excellent sterilization performance.
FIG. 1 is a scanning electron micrograph of the PDMS-ZnO/Au sterilization material obtained. The ZnO nano-column prepared as shown in the figure is uniformly modified on a PDMS film, the length of the nano-column is 2 μm, the diameter of the nano-column is 100 nm, Au nano-particles are uniformly modified on the surface of the ZnO nano-column, and the diameter of the Au nano-particles is 40 nm.
FIG. 2 is an X-ray diffraction spectrum of the obtained PDMS-ZnO/Au sterilization material. As shown in the figure, the diffraction peak of the wurtzite structure ZnO is clearly visible, which indicates that the synthesized ZnO is the wurtzite structure, and Au is the face-centered cubic crystal form.
FIG. 3 is a graph showing the bacteriostatic effect of PDMS-ZnO/Au on Escherichia coli under visible light (a) and dark (b), under visible light (c) and dark (d), and under the control group condition (c). Calculating a formula according to the bacteriostatic rate: eb＝(Nb-Nc)/Nb*100％，(NbThe average colony number of the control group sample without the bactericide; n is a radical ofcThe average number of colonies acted by the sterilization material) to obtain that the sterilization rates of PDMS-ZnO/Au under the conditions of visible light for 30 minutes and no light are 100.0% and 65.5% respectively, and the sterilization rates of PDMS under the conditions of visible light for 30 minutes and no light are 31.5% and 0.5% respectively, which indicates that the prepared PDMS-Zn/Au composite membrane has excellent sterilization performance.
Example 2
The operations were carried out in the same manner as in example 1 except that the hydrothermal reaction in step 3) of example 1 was carried out at 90 ℃ for 6 hours; the hydrothermal reaction in example 2 was carried out at 90 ℃ for 12 hours. The sterilization rate of the composite film under the condition of visible light irradiation for 30 minutes is 100.0%.
Example 3
The operations were carried out in the same manner as in example 1 except that the time for light irradiation in step 4) of example 1 was 30 min; while the time of light irradiation in example 3 was 60 min. The sterilization rate of the composite film under the condition of visible light irradiation for 30 minutes is 100.0%.
Example 4
The procedure of example 1 was followed, except that the PDMS-ZnO sample film was placed in an aqueous solution containing gold acid at a mass fraction of 0.1% in step 4) of example 1; in example 4, the PDMS-ZnO sample film is placed in a gold acid-containing aqueous solution with the mass fraction of 0.01%. The sterilization rate of the composite film under the visible light for 30 minutes is 98.2%.
Example 5
The operations were carried out in the same manner as in example 1 except that the hydrothermal reaction in step 3) of example 1 was carried out at 90 ℃ for 6 hours; the hydrothermal reaction in example 2 was carried out at 90 ℃ for 8 hours. The sterilization rate of the composite film under the condition of visible light irradiation for 30 minutes is 100.0%.
Claims (7)
1. A preparation method of a PDMS-ZnO/Au sterilization material with a noble metal modified semiconductor nano-pillar array structure comprises the following steps:
1) and (3) mixing a PDMS monomer and a curing agent according to the ratio of 8-12: 1, uniformly stirring, performing vacuum drying to remove bubbles, and curing at 50-100 ℃ for 1-3 hours to obtain a PDMS sample film;
2) taking 50-100 mL of 10-20 mM zinc salt alcoholic solution, dropwise adding 30-60 mL of 10-50 mM alkali alcoholic solution, and heating and stirring the obtained mixed solution at 50-100 ℃ for 1-3 hours to obtain ZnO seed solution; then soaking the PDMS sample film obtained in the step 1) in the ZnO seed solution for 1-5 min to enable the ZnO seeds to uniformly and compactly cover the surface of the PDMS sample film, and then heating the PDMS sample film at 50-100 ℃ for 30-60 min to enable the bonding force between PDMS and ZnO to be stronger, so as to obtain the PDMS sample film fixed with the ZnO seeds;
3) taking 50-150 mL of 20-60 mM zinc salt aqueous solution, adding 50-100 mL of 20-60 mM hexamethylenetetramine aqueous solution, stirring at room temperature for 10-30 min, transferring the mixed solution into a reaction kettle, immersing the PDMS sample film fixed with ZnO seeds obtained in the step 2) into the mixed solution, heating at 80-120 ℃ for 6-12 hours, cooling to room temperature, repeatedly washing with deionized water, and drying to obtain a PDMS-ZnO sample film;
4) placing the PDMS-ZnO sample film obtained in the step 3) into an aqueous solution containing gold acid with the mass fraction of 0.01-0.2%, adjusting the pH to 7-10 by using an aqueous solution of alkali with the mass fraction of 1-5%, illuminating for 20-60 min at room temperature, taking out the sample film after the reaction is finished, repeatedly cleaning by using deionized water, and drying to obtain the PDMS-ZnO/Au sterilization material.
2. The method for preparing the PDMS-ZnO/Au sterilization material with the noble metal modified semiconductor nano-pillar array structure according to claim 1, wherein the method comprises the following steps: the zinc salt is one of zinc acetate, zinc sulfate, zinc nitrate or zinc chloride.
3. The method for preparing the PDMS-ZnO/Au sterilization material with the noble metal modified semiconductor nano-pillar array structure according to claim 1, wherein the method comprises the following steps: the aururic acid is one of chloroauric acid, gold acetate and gold [ tris (2, 4-di-tert-butylphenyl) phosphite ] chloride.
4. The method for preparing the PDMS-ZnO/Au sterilization material with the noble metal modified semiconductor nano-pillar array structure according to claim 1, wherein the method comprises the following steps: the alcohol is one of methanol, ethanol, glycol or glycerol.
5. The method for preparing the PDMS-ZnO/Au sterilization material with the noble metal modified semiconductor nano-pillar array structure according to claim 1, wherein the method comprises the following steps: the alkali is one of ammonia water, sodium hydroxide, sodium carbonate, potassium hydroxide, hexamethylene tetramine or triethylamine.
6. The method for preparing the PDMS-ZnO/Au sterilization material with the noble metal modified semiconductor nano-pillar array structure according to claim 1, wherein the method comprises the following steps: the light source for illumination is one of simulated sunlight, a mercury lamp, a xenon lamp or an LED lamp, and the wavelength range of the light source is 200-800 nm.
7. A PDMS-ZnO/Au sterilization material with a noble metal modified semiconductor nano-pillar array structure is characterized in that: is prepared by the method of any one of claims 1 to 6.
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