CN110150317A - A kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure and preparation method thereof - Google Patents
A kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure and preparation method thereof Download PDFInfo
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- CN110150317A CN110150317A CN201910461980.8A CN201910461980A CN110150317A CN 110150317 A CN110150317 A CN 110150317A CN 201910461980 A CN201910461980 A CN 201910461980A CN 110150317 A CN110150317 A CN 110150317A
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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
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Abstract
A kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure and preparation method thereof, belongs to semiconductor sterilization material technical field.It selects PDMS as substrate, ZnO nanopillar array is grown on PDMS by hydro-thermal method, the sterilization material is then obtained in ZnO surface recombination Au nanoparticle using the method for photo-reduction.Sterilization material prepared by the present invention sterilizes surface as a kind of bionic nano column type, is dispersed with the structure such as " shoe tack " thereon, and after bacterial adhesion occurs, the micro nano structure on surface makes inactivation of bacteria by the operating mechanism of slowly tearing cell membrane；After introducing Au nanoparticle, the utilization to visible light may be implemented, the separation of photohole and light induced electron can also be promoted by surface plasma resonance effect, it restrained effectively the recombination of carrier, and then photocatalytic activity is promoted, the producible active oxygen radical of photocatalytic process has powerful sterilizing function.
Description
Technical field
The invention belongs to semiconductor sterilization material technical fields, and in particular to a kind of noble metal decorated semiconductor nano-pillar battle array
PDMS-ZnO/Au sterilization material of array structure and preparation method thereof.
Background technique
Under the situation that environmental problem is on the rise, pathogen microorganism is seen everywhere, novel and multifunctional, safety is developed
The sterilization material of environmental protection is particularly important.Sterilization material it is many kinds of, wherein photocatalyst-type sterilization material due to have compared with
Strong bactericidal activity is nontoxic and do not discharge heavy metal ion and be concerned.Zinc oxide (ZnO) is due to good chemical stabilization
Property, commercial practicability, easily prepared various structure the features such as be considered as one of most potential photocatalyst-type fungicide.When big
When the photon irradiation ZnO of bandgap, it can be excited to generate hole-electron pair, subsequently generate the active oxygen with strong oxidizing property
Group OH and O2 -, they destroy the permeability of the cell wall (film) of bacterium and the structure of DNA by the coacetylase of oxidizing bacteria,
Cause bacterial death.ZnO has the characteristics that broad-spectrum sterilization and is only used as in sterilization process to urge as photo-catalyst material
Agent participates in reaction, does not consume theoretically, has lasting bactericidal property.But the bandgap of ZnO is wider, it can only the occupied sun
The ultraviolet light of energy 4% is excited, and semiconductor carriers recombination rate is high, and photo-quantum efficiency is low, and the reality for limiting ZnO is answered
With.
The method for being used to improve ZnO photocatalysis efficiency at present has very much, wherein the compound zno-based of noble metal nano particles
The scheme of heterojunction structure has caused the extensive concern of scientific research personnel.In semiconductor/noble metal heterojunction structure, due to special energy
Band structure and carrier transmission characteristics effectively can inhibit both hole and electron to recombinate, improve photochemical catalyst in light-catalyzed reaction
Catalytic activity；And there is noble metal nano particles surface plasma body resonant vibration (SPR) effect can expand to visible absorption,
Realize the effective use to sunlight.
The special nanometer rod structure in Elena P.Ivanova in 2012 et al. discovery cicada's wings surface can kill certain attachments
Bacterium on its surface, this special sterilization mode for develop disinfecting material provide thinking (Small, 2012,8
(16):2489-2494).It is inspired by this, the ZnO that Guangshun Yi et al. is found to have nano-pillar array structure can pass through machine
The mode of tool sterilization makes bacterial death (Small, 2018,14 (14): 1703159) for being attached to surface.Meanwhile ZnO is as one
The photo-catalyst material that kind is had excellent performance can have the active oxy group of strong oxidizing property be sterilized by discharging,
ZnO nanopillar array is prepared by hydro-thermal method on fishing net surface in Priyanka Sathe et al., obtains photo-catalyst
Performance (Scientific Reports, 2017,7 (1): 3624).There is presently no by semiconductor nano material physical structure
Semiconductor nano material, is assigned special array structure, not only by the report that sterilization and photo-catalyst two ways combine
It realizes efficient sterilizing, also effectively compensates for photocatalyst-type fungicide and excite the shortcomings that can just acting under light.
Summary of the invention
The object of the present invention is to provide a kind of PDMS- ZnO/Au of noble metal decorated semiconductor nano-pillar array structure to kill
Bacterium material and preparation method thereof.The film forming of dimethyl silicone polymer (PDMS) can be carried out by solidification temperature with curing time
It adjusts；The size of ZnO nanopillar array can be adjusted by the condition of hydro-thermal reaction；The size of Au nanoparticle can be with
It is adjusted by the concentration and light application time of the aqueous solution containing auric acid；The ratio of ZnO and Au can by change be added zinc source and
The ratio and light application time of Jin Yuan is adjusted.PDMS-ZnO/Au can pass through under no light condition by own physical structure
The mode of machinery sterilization shows good bactericidal effect, and PDMS-ZnO/Au composite membrane sterilizes physical structure under visible light
So that it shows stronger bactericidal effect after excited by visible light in conjunction with photocatalyst-type sterilization two ways, effectively make up
Photocatalyst-type fungicide excites the shortcomings that can just acting under light.
A kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure of the present invention
Preparation method, its step are as follows:
1) PDMS monomer and curing agent mixing by the weight ratio of 8~12:1, vacuum drying removes bubble after mixing evenly,
Then solidify 1~3 hour under the conditions of 50~100 DEG C, obtains PDMS sample film；
2) 50~100mL of alcoholic solution for taking 10~20mM zinc salt, is added dropwise 10~50mM alkali alcosol 30 thereto
~60mL, obtained mixed solution obtain ZnO seed solution heating stirring 1~3 hour under conditions of 50~100 DEG C；Then
The PDMS sample film that step 1) obtains is immersed in 1~5min in the ZnO seed solution, is covered on making ZnO seed even compact
PDMS sample film surface then heats 30~60min under the conditions of 50~100 DEG C, makes binding force between PDMS and ZnO more
By force, the PDMS sample film for being fixed with ZnO seed is obtained；
3) 50~150mL of aqueous solution of 20~60mM zinc salt is taken, 20~60mM hexamethylenetetramine is added thereto
(HMTA) mixed solution is transferred in reaction kettle by 50~100mL of aqueous solution after stirring 10~30min at room temperature, and will
The PDMS sample film that step 2) obtained be fixed with ZnO seed is immersed in the mixed solution, is heated under the conditions of 80~120 DEG C
6~12 hours, deionized water repeated flushing was used after being cooled to room temperature, obtains PDMS-ZnO sample film after dry；
4) aqueous solution containing auric acid for PDMS-ZnO sample film will be obtained in step 3) being placed in mass fraction 0.01~0.2%
In, pH to 7~10 is adjusted with the aqueous solution of the alkali of mass fraction 1%~5%, under room temperature 20~60min of illumination, reaction knot
It is cleaned repeatedly after taking out sample film after beam with deionized water, PDMS-ZnO/Au sterilization material of the present invention is obtained after dry
Material.
The zinc salt is one of zinc acetate, zinc sulfate, zinc nitrate or zinc chloride etc.；It is gold chloride, fluorine containing auric acid
One of auric acid, acetic acid gold, chlorine [three (2,4- di-tert-butyl-phenyl) phosphorous acid] gold etc.；Alcohol be methanol, ethyl alcohol, ethylene glycol or
One of glycerine etc.；Alkali is in ammonium hydroxide, sodium hydroxide, sodium carbonate, potassium hydroxide, six methines, four ammonia, triethylamine etc.
It is a kind of；The light source of illumination is one of simulated solar irradiation, mercury lamp, xenon lamp, LED light etc., the wave-length coverage of light source is 200~
800nm。
The method equipment that the present invention prepares PDMS-ZnO/Au sterilization material is simple, mild condition, and chemical reagent used is cheap
It is easy to get.Selection mechanical performance first is high, and PDMS easy to form grows ZnO nano by hydro-thermal method as substrate on PDMS
Then column array is finally obtained the PDMS-ZnO/Au and killed using the method for photo-reduction in ZnO surface recombination Au nanoparticle
Bacterium material.PDMS-ZnO/Au prepared by the present invention sterilizes surface as a kind of bionic nano column type, is dispersed with thereon such as " shoes
Structure as nail ", after bacterial adhesion occurs, the micro nano structure on surface is made by the operating mechanism of slowly tearing cell membrane
Inactivation of bacteria；After the surface semiconductor ZnO introduces Au nanoparticle, the utilization to visible light, another party on the one hand may be implemented
Face can promote the separation of photohole and light induced electron, restrained effectively current-carrying by surface plasma resonance (SPR) effect
The recombination of son, and then photocatalytic activity is promoted, the producible active oxygen radical of photocatalytic process (ROS) has powerful sterilization
Function.The experimental results showed that PDMS-ZnO/Au has good bactericidal effect.The present invention is for the first time by semiconductor nano material physics
Structure sterilization is combined with photo-catalyst mode, and the PDMS-ZnO/Au being prepared presents the bactericidal property of stability and high efficiency,
Its low raw-material cost, preparation method is simple, can mass production, make PDMS-ZnO/Au in marine antifouling coating or medical coating
There is good application prospect in equal fields.
Detailed description of the invention
Fig. 1: the scanning electron microscopic picture for the PDMS-ZnO/Au sterilization material that embodiment 1 is prepared；
Fig. 2: the X-ray diffraction spectrogram for the PDMS-ZnO/Au sterilization material that embodiment 1 is prepared；
Fig. 3: the PDMS-ZnO/Au sterilization material that Application Example 1 is prepared is under (a) is unglazed under visible light (b),
The PDMS fungistatic effect figure of (d) and control group (e) to Escherichia coli under (c) is unglazed under visible light；
Specific embodiment
More detailed description is done to technical solution of the present invention with specific embodiment below, but the example is not constituted to this
The limitation of invention.
Embodiment 1
1) PDMS monomer and curing agent are mixed by the weight ratio of 10:1, puts remove in a vacuum drying oven after mixing evenly
Bubble then solidifies 1 hour under the conditions of 80 DEG C, obtains PDMS sample film；
2) the ethanol solution 80mL for taking the zinc acetate of 10mM, is added dropwise the ethanol solution of 30mM sodium hydroxide thereto
40mL, obtains ZnO seed solution, then by step 1) at obtained mixed solution 2 hours of heating stirring under conditions of 60 DEG C
Obtained PDMS sample film is immersed in 2 min in ZnO seed solution, is covered on the surface PDMS with making ZnO seed even compact, then
30 min are heated in 90 DEG C of baking ovens, keep the binding force between PDMS and ZnO stronger, obtain the PDMS sample for being fixed with ZnO seed
Product film；
3) each 100mL mixing of the HMTA aqueous solution of the zinc nitrate aqueous solution and 60mM that take 60mM, stirs 20min at room temperature
The solution is transferred in reaction kettle afterwards, and the PDMS sample film for being fixed with ZnO seed is immersed in the mixed solution,
It is heated 6 hours under the conditions of 90 DEG C, deionized water repeated flushing is used after being cooled to room temperature, obtains PDMS-ZnO sample film after dry；
4) PDMS-ZnO sample film will be obtained in step 3) to be placed in the aqueous solution of chloraurate that mass fraction is 0.1%, use
The sodium hydrate aqueous solution that mass fraction is 2% adjusts pH to 9, uses the xenon source of 350~780nm of wavelength under room temperature
30min is irradiated, after reaction take out sample and is cleaned repeatedly with deionized water, PDMS-ZnO/Au sterilization is obtained after dry
Material.
1 performance test of embodiment
PDMS-ZnO/Au sterilization material is immersed in the medicinal alcohol of volume fraction 75% and is carried out disinfection, after 24 hours
Taking-up is put into super-clean bench and is dried up with sterile wind, draws 100 μ L E. coli suspensions (10 with sterile pipette tips6CFU/mL, ATCC
25922) it gently beats on sterilization material surface, after under visible light or being placed 30 minutes under no light condition, extremely by its global transfer
In the physiological saline of sterilizing, vortex oscillation 8 seconds, takes out 200 μ L bacterium solutions and be coated in the LB solid being contained in culture dish with three angle rods
On culture medium, culture dish inversion is placed in 37 DEG C of incubators and counts after culture 12h to colony count, and evaluates its sterilization
Performance.The result shows that using whole Escherichia coli can be killed in short under visible light conditions 30 minutes PDMS-ZnO/Au,
The sterilizing rate of PDMS-ZnO/Au under no light condition is also up to 65.5%, and it is excellent to illustrate that the PDMS- ZnO/Au of preparation has
Different bactericidal property.
The electron scanning micrograph for the PDMS-ZnO/Au sterilization material that attached drawing 1 is.It prepares as shown in the figure
ZnO nano column is uniformly modified on PDMS film, and nanometer column length is 2 μm, and diameter is 100 nm, and wherein Au nano particle is equal
Even modification is 40 nm in ZnO nano column surface, the diameter of Au nano particle.
The X-ray diffraction spectrogram for the PDMS-ZnO/Au sterilization material that attached drawing 2 is.Wurtzite ZnO as shown in the figure
Diffraction maximum it is high-visible, illustrate synthesis ZnO be wurtzite structure, Au is face-centered cubic crystal form.
Attached drawing 3 be PDMS-ZnO/Au sterilization material under visible light (a), it is unglazed under (b), PDMS (c) nothing under visible light
The fungistatic effect figure of (c) to Escherichia coli under the conditions of (d) and control group under light.According to bacteriostasis rate calculation formula: Eb=(Nb-
Nc)/Nb* 100%, (NbFor the average colony number of the control sample of no fungicide；NcIt is flat after sterilization material acts on
Equal colony count) it is calculated and distinguishes in visible light according to the sterilizing rate under 30 minutes and no light condition using PDMS- ZnO/Au
It is 100.0% and 65.5%, PDMS is 31.5% He respectively according to the sterilizing rate under 30 minutes and no light condition in visible light
0.5%, illustrate that the PDMS-Zn/Au composite membrane of preparation has excellent bactericidal property.
Embodiment 2
Such as each step operation of embodiment 1, the difference is that the condition of hydro-thermal reaction is 90 DEG C of items in the step 3) of embodiment 1
It is heated 6 hours under part；And the condition of hydro-thermal reaction is heated 12 hours under the conditions of 90 DEG C in embodiment 2.The composite membrane is visible
Sterilizing rate under illumination 30 minutes is 100.0%.
Embodiment 3
Such as each step operation of embodiment 1, the difference is that the time of illumination is 30 min in the step 4) of embodiment 1；And
The time of illumination is 60min in embodiment 3.The composite membrane is 100.0% according to the sterilizing rate under 30 minutes in visible light.
Embodiment 4
Such as each step operation of embodiment 1, the difference is that PDMS-ZnO sample film is placed in matter in the step 4) of embodiment 1
In the aqueous solution containing auric acid for measuring score 0.1%；It and is that PDMS-ZnO sample film is placed in mass fraction 0.01% in embodiment 4
The aqueous solution containing auric acid in.The composite membrane is 98.2% according to the sterilizing rate under 30 minutes in visible light.
Embodiment 5
Such as each step operation of embodiment 1, the difference is that the condition of hydro-thermal reaction is 90 DEG C of items in the step 3) of embodiment 1
It is heated 6 hours under part；And the condition of hydro-thermal reaction is heated 8 hours under the conditions of 90 DEG C in embodiment 2.The composite membrane is visible
Sterilizing rate under illumination 30 minutes is 100.0%.
Claims (7)
1. a kind of preparation method of the PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure, step
It is rapid as follows:
1) PDMS monomer and curing agent are mixed by the weight ratio of 8~12:1, vacuum drying removes bubble after mixing evenly, then
Solidify 1~3 hour under the conditions of 50~100 DEG C, obtains PDMS sample film；
2) 50~100mL of alcoholic solution for taking 10~20mM zinc salt, be added dropwise thereto 10~50mM alkali alcosol 30~
60mL, obtained mixed solution obtain ZnO seed solution heating stirring 1~3 hour under conditions of 50~100 DEG C；Then will
The PDMS sample film that step 1) obtains is immersed in 1~5min in the ZnO seed solution, is covered on making ZnO seed even compact
PDMS sample film surface then heats 30~60min under the conditions of 50~100 DEG C, makes binding force between PDMS and ZnO more
By force, the PDMS sample film for being fixed with ZnO seed is obtained；
3) 50~150mL of aqueous solution of 20~60mM zinc salt is taken, the aqueous solution of 20~60mM hexamethylenetetramine is added thereto
The mixed solution is transferred in reaction kettle after stirring 10~30min at room temperature, and consolidates what step 2) obtained by 50~100mL
Surely there is the PDMS sample film of ZnO seed to be immersed in the mixed solution, heated 6~12 hours under the conditions of 80~120 DEG C, it is cooling
Deionized water repeated flushing is used after to room temperature, obtains PDMS-ZnO sample film after dry；
4) PDMS-ZnO sample film will be obtained in step 3) to be placed in the aqueous solution containing auric acid of mass fraction 0.01~0.2%,
PH to 7~10 is adjusted with the aqueous solution of the alkali of mass fraction 1%~5%, 20~60min of illumination, reaction terminate under room temperature
It is cleaned repeatedly after sample film is taken out afterwards with deionized water, obtains PDMS-ZnO/Au sterilization material after dry.
2. a kind of PDMS-ZnO/Au of noble metal decorated semiconductor nano-pillar array structure as described in claim 1 sterilizes material
The preparation method of material, it is characterised in that: the zinc salt is one of zinc acetate, zinc sulfate, zinc nitrate or zinc chloride.
3. a kind of PDMS-ZnO/Au of noble metal decorated semiconductor nano-pillar array structure as described in claim 1 sterilizes material
The preparation method of material, it is characterised in that: described is gold chloride, fluorine auric acid, acetic acid gold, chlorine [three (2,4- di-t-butyls containing auric acid
One of phenyl) phosphorous acid] gold.
4. a kind of PDMS-ZnO/Au of noble metal decorated semiconductor nano-pillar array structure as described in claim 1 sterilizes material
The preparation method of material, it is characterised in that: the alcohol is one of methanol, ethyl alcohol, ethylene glycol or glycerine.
5. a kind of PDMS-ZnO/Au of noble metal decorated semiconductor nano-pillar array structure as described in claim 1 sterilizes material
The preparation method of material, it is characterised in that: the alkali is ammonium hydroxide, sodium hydroxide, sodium carbonate, potassium hydroxide, six methines, four ammonia
Or one of triethylamine.
6. a kind of PDMS-ZnO/Au of noble metal decorated semiconductor nano-pillar array structure as described in claim 1 sterilizes material
The preparation method of material, it is characterised in that: the light source of illumination is one of simulated solar irradiation, mercury lamp, xenon lamp or LED light, light source
Wave-length coverage be 200~800nm.
7. a kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure, it is characterised in that: be by
Method described in claim 1~6 any one is prepared.
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