WO2012067469A2 - Procédé de fabrication d'un substrat à l'aide de nanoparticules colloïdales pour prévenir la formation d'un biofilm, substrat ainsi fabriqué, et capteur d'évaluation de la qualité de l'eau présente sur le substrat - Google Patents

Procédé de fabrication d'un substrat à l'aide de nanoparticules colloïdales pour prévenir la formation d'un biofilm, substrat ainsi fabriqué, et capteur d'évaluation de la qualité de l'eau présente sur le substrat Download PDF

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WO2012067469A2
WO2012067469A2 PCT/KR2011/008854 KR2011008854W WO2012067469A2 WO 2012067469 A2 WO2012067469 A2 WO 2012067469A2 KR 2011008854 W KR2011008854 W KR 2011008854W WO 2012067469 A2 WO2012067469 A2 WO 2012067469A2
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substrate
preventing
colloidal nanoparticles
biofilm formation
biofilm
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PCT/KR2011/008854
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English (en)
Korean (ko)
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WO2012067469A3 (fr
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이성호
이도훈
이상호
이낙규
김상용
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한국생산기술연구원
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Priority to CN201180061237.5A priority Critical patent/CN103261886B/zh
Publication of WO2012067469A2 publication Critical patent/WO2012067469A2/fr
Publication of WO2012067469A3 publication Critical patent/WO2012067469A3/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • 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
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units

Definitions

  • the present invention relates to a method for manufacturing a biofilm forming prevention substrate using colloidal nanoparticles, a substrate prepared therefrom, and a water quality inspection sensor including the substrate. More specifically, the colloidal nanoparticles are arranged on a substrate. Thereafter, a hole and a porous structure are formed on the substrate to manufacture a substrate for preventing biofilm formation, the substrate manufactured using the method, a plurality of holes formed on the substrate, and the front and upper surfaces of the substrate and formed on the hole.
  • the present invention relates to a biofilm forming prevention substrate including a porous structure, and a water quality inspection sensor including the substrate.
  • Biofilms are generally referred to as biofilms as structures formed by microorganisms that adhere to and proliferate on the surface of materials in an aqueous system.
  • Such biofilm formation causes a risk by microorganisms and thus causes problems in various industries.
  • biofilm on the surface of the heat exchanger also reduces the heat transfer efficiency.
  • biofilm is formed on the surface of a structure such as a metal surface, it may cause corrosion of the metal and cause decay of the facility. In particular, damages caused by corrosion of materials such as various metals and concrete are not only inconvenient but also costly for reconstruction, which is causing economic difficulties.
  • a method for inhibiting or preventing the growth of the biofilm on the corrosion-sensitive material for example, metal
  • various methods such as pH control, redox potential control, inorganic coating, cathodic protection, and biocide application are performed, but protective coatings such as paints and epoxies are used. They are excessively expensive to apply and maintain, making them impossible to use as effective anti-biofilm formulations.
  • biofilms include: 1) inhibiting the formation of biofilms by coating surfaces with microorganisms or specific chemicals, or 2) decomposing biofilms formed using specific organisms or compounds, 3) There exists a method of inhibiting or disturbing the growth of the microorganisms forming the biofilm, but the research on the technology of preventing the formation of the biofilm by applying a specific form on the surface itself is insufficient.
  • the present inventors do not rely on coating a specific chemical or microorganism or treating the various substances to modify the surface, and thus prevent the production of the biofilm by modifying only the shape of the surface. It is possible to manufacture a substrate comprising a method and a structure manufactured by the method and has been filed with the patent application No. 10-2009-0135754.
  • the inventors of the present invention by coating the specific chemicals or microorganisms using the colloidal nanoparticles, or by modifying the surface by treating the various materials, but only by modifying the shape of the surface of the biofilm itself
  • the present invention has been completed by confirming that a substrate capable of preventing the above-mentioned process can be manufactured, and confirming that the substrate can be coupled to a water quality test sensor to increase the sensitivity and reproducibility of the water quality test sensor.
  • An object of the present invention is to provide a method for producing a substrate for preventing biofilm formation by forming colloidal nanoparticles on a substrate and then forming a hole and a porous structure on the substrate.
  • Another object of the present invention is a substrate produced by the manufacturing method; A plurality of holes formed in an upper portion of the substrate; And a porous structure formed on the upper front surface and the hole of the substrate.
  • Still another object of the present invention is to provide a method of preventing biofilm formation by using the biofilm formation preventing substrate as a surface.
  • Still another object of the present invention is to provide a water quality inspection sensor including the biofilm formation preventing substrate.
  • the present invention provides a method for producing a biofilm forming prevention substrate comprising the following steps.
  • the present invention may further comprise the step of adjusting the interval of the colloidal nanoparticles arranged between the steps 1) and 2) (step 1a).
  • the process of manufacturing a substrate including the structure of the present invention includes: 1) arranging colloidal nanoparticles on a substrate and 2) etching the substrate on which the colloidal nanoparticles are arranged to form holes and porous structures. It may be divided into the step, and optionally may further comprise the step of adjusting the interval of the colloidal nanoparticles arranged between the steps 1) and 2) (step 1a).
  • Step 1 is a step of arranging the colloidal nanoparticles on top of the substrate can be used without limitation methods commonly used in the art, and preferably a method for coating a dispersion containing the colloidal nanoparticles on the substrate It can be performed as.
  • the colloidal nanoparticles used have a size of 100 nm to 100 ⁇ m in consideration of repulsion and aggregation between the colloidal nanoparticles.
  • the colloidal nanoparticles include polystyrene; Silica (SiO 2 ); Nitrides such as Si 3 N 4 ; Oxides or combinations thereof can be used.
  • PS nanobead particles were used as colloidal nanoparticles.
  • the substrate In order to perform the colloidal nanolithography process using PS nanobead particles, the substrate must be changed to a hydrophilic state.
  • silica (SiO 2 ), nitride (Si 3 N 4 ) particles and the like can be adjusted to maintain the appropriate surface state.
  • Step 2 may be used to form a hole and a porous structure on the substrate of the step without limitation, a method commonly used in the art, preferably the hole and the porous structure may be performed by an etching method. .
  • Etching method can also be etched according to the conventional methods used in the art according to the material and material properties of the substrate, the hole and the porous structure of the present invention, if necessary to form a microstructure in units of ⁇ m
  • the chemical etching method is a method of etching using various etching solutions, it is possible to prepare an etching solution of a suitable composition according to the purpose and the needs of those skilled in the art.
  • Electrochemical etching is a method performed in the embodiments of the present specification
  • the discharge machining (EDM (Electro-Discharge Machining)) is a method performed by using a physical, mechanical or electrical action generated when a discharge between the two electrodes. Such electric discharge machining can be performed irrespective of the strength of the material, and is a method of easily processing complex shapes such as planes and solids.
  • the discharge machining can be processed to 0.1 ⁇ m to 0.2 ⁇ m, and in that there is no surface deterioration by heat, it is possible to achieve an object that cannot be achieved by other processing methods.
  • electro-chemical machining produces a metal oxide film, which is an anode product, which hinders the progress of electrochemical dissolution of a metal material.
  • electrolytic processing if a tool made in the shape to be processed is used as a cathode, the material is used as an anode, and both of them are immersed in the electrolyte and the current is passed through, the material is processed like the surface shape of the cathode.
  • the substrate of the present invention can perform the above-described method to form the desired holes and porous structures.
  • the present invention by performing the ECF (electro chemical fabrication) method to apply the structure of the hole and the porous structure to the substrate by etching the remaining portion except the colloidal nano-particles arranged on the substrate to the top of the substrate It was confirmed that the hole can be formed. In addition, it was confirmed that the substrate having the hole structure formed by the above method was etched again using FeCl 3 solution to obtain the structure of the hole and the porous structure of interest in the present invention. In addition, as a result of applying the biofilm-forming microorganisms to the substrate prepared by the method, it was confirmed that the biofilm can be effectively suppressed.
  • ECF electro chemical fabrication
  • the biofilm formation inhibitory effect was compared between ECF alone treatment and the combination treatment of ECF and FeCl 3 , and as a result, it was confirmed that the combination treatment of ECF and FeCl 3 was more effective in inhibiting biofilm formation.
  • the effect of inhibiting biofilm formation was compared by varying the treatment time of FeCl 3 performed after ECF from 1 minute to 5 minutes. As a result, treating FeCl 3 after ECF for 1 minute was most effective in inhibiting biofilm formation. Confirmed.
  • the contact angle of the porous structure may be changed according to the needs of those skilled in the art or according to the type of biofilm to be prevented, and various methods of changing the contact angle, including a method of treating with an etchant, may be performed.
  • the type and concentration of the etchant used may be determined by those skilled in the art according to the purpose, and the time and number of times of exposure to the etchant may also be determined by conventional methods.
  • the inventors have found that when the time and number of times exposed to the etchant increases, the contact angle of the porous structure can be increased.
  • the present inventors have made a lot of experiments, and as a result of diligent efforts, it was confirmed that as the contact angle increases, microbial adhesion is reduced, as a result that the biofilm can be further suppressed.
  • the present invention provides a method for manufacturing a biofilm forming prevention substrate comprising the following steps.
  • the present invention may further comprise the step of adjusting the interval of the colloidal nanoparticles arranged between the steps 1) and 2) (step 1a).
  • the process of manufacturing a substrate including the structure of the present invention comprises: 1) arranging colloidal nanoparticles on top of the substrate, 2) coating a protective material on the substrate of the step, 3) the substrate of the step Removing colloidal nanoparticles from and 4) forming holes and porous structures in the colloidal nanoparticles removed from the upper part of the substrate, optionally in steps 1) and 2 It may further comprise the step (step 1a) of adjusting the spacing of the colloidal nanoparticles arranged between the steps.
  • Steps 1 and 1a are as described in the method of manufacturing the biofilm formation preventing substrate.
  • Step 2 is a step of coating the substrate with a protective material to protect the substrate so that the hole and the porous structure is not formed in the step of forming a hole and the porous structure to be performed as a step of coating a protective material on the substrate.
  • an oxide film or a nitride film may be used as the protective material, but is not limited thereto.
  • Step 3 is a step of removing the colloidal nanoparticles from the substrate to remove the colloidal nanoparticles from the substrate to secure a region for forming holes and porous structures.
  • a method that can be used to remove colloidal nanoparticles includes a removal method using a chemical solution, but is not limited thereto.
  • Step 4 is a step of forming a hole and a porous structure in the colloidal nano-particles removed portion of the upper substrate, the specific method is the same as described in step 2 of the manufacturing method of the biofilm formation prevention substrate.
  • the present inventors arrange the colloidal nanoparticles on the substrate as described above, then coat the protective material, remove the colloidal nanoparticles, and then form a hole and a porous structure in the portion where the colloidal nanoparticles are removed.
  • the biofilm-forming microorganisms it was confirmed that the biofilm can be effectively suppressed.
  • the present invention is a substrate; A plurality of holes formed in an upper portion of the substrate; And it provides a substrate for preventing biofilm formation comprising a porous structure formed in the upper front and the hole of the substrate.
  • the substrate including the hole and the porous structure of the present invention can form a microstructure having a superhydrophobic surface due to the above structural features, and can have a composite structure of nano-micro multi-scale, As a result, biofilm formation by the growth and proliferation of microorganisms can be prevented or suppressed.
  • the "substrate” of the present invention is not limited as long as it is a material capable of forming the hole and the porous structure of the present invention, as long as it has a material or material that can prevent the formation of biofilm by treating the surface with the above structure. It is not limited.
  • examples of the material include metal, polymer, glass, and the like, but the types of materials to which the surface structure of the present invention is applicable are not limited by the above examples.
  • the substrate may be a flexible substrate that can be easily implemented in various forms.
  • the substrate may be stainless steel, in a preferred embodiment of the present invention to form the structure of the present invention by using a stainless steel used in a variety of everyday life, such as water pipes, while the substrate comprising the structure is bio It was confirmed that film formation can be suppressed.
  • the substrate may be implemented in a cylindrical shape by winding the substrate.
  • the cylindrical substrate is a stainless steel having a nano and micro porous structure, and has a nano and micro porous structure formed by using ECF, FeCl 3 etching method inside the cylinder.
  • the thickness of the cylindrical substrate may be from several ⁇ m to several hundred mm.
  • hole of the present invention means a hole-shaped structure formed on the surface of the substrate, the diameter, spacing and depth of the hole can be appropriately adjusted by those skilled in the art as needed. This range is preferably set in the direction of suppressing the growth of microorganisms constituting the biofilm.
  • the size of the hole applied on the substrate may or may not be uniform, it is preferable to form holes of various sizes and structures as long as it can suppress the formation of the biofilm.
  • the spacing of holes formed on the substrate may be uniform or not uniform, and may be adjusted using an oxygen plasma or the like.
  • the spacing of the holes is preferably 10 nm to 10 ⁇ m, and the depth of the holes is preferably 10 nm to 50 ⁇ m.
  • the lower diameter is preferably set to be smaller than the size of the target microorganism to prevent the formation of the biofilm.
  • the size of the microorganisms known to form a biofilm is 0.1 ⁇ m to 10 ⁇ m, and the size of the microorganisms is known to be 1 ⁇ m to 3 ⁇ m in many microorganisms. desirable.
  • porous structure of the present invention is meant a form present on the surface of the substrate, the porous structure may be formed on all or part of the surface as required by those skilled in the art.
  • the porous structure is not limited in the form and number to the extent that the various microorganisms known to form a biofilm can be prevented or inhibited from adhering to and proliferating on the surface, and the porous structure has a regular distribution or irregularity such as holes. It may be configured in any form such as distribution.
  • Such a structure can be formed into a structure in which substances such as water droplets required for growth conditions of microorganisms and other microorganisms cannot be stagnated.
  • the diameter of the porous structure may be 100 nm to 100 ⁇ m, the spacing between the porous structures is 10 nm to 10 ⁇ m, depth may be formed in the range of 1 ⁇ m to 1000 ⁇ m.
  • the porous structure formed on the entire surface including the substrate, the holes formed on the surface of the substrate, and the holes prevents water droplets necessary for the survival of the microorganisms from adhering to the substrate, that is, forms microstructures having a superhydrophobic surface.
  • the microorganism itself can be attached to the surface of the substrate, grow, and block the process of proliferation.
  • the present invention also relates to a method for preventing biofilm formation by using the biofilm formation preventing substrate as a surface.
  • the substrate including the hole and the porous structure of the present invention When the substrate including the hole and the porous structure of the present invention is used, contamination and corrosion by various microorganisms or organisms known to form a biofilm can be suppressed or prevented.
  • the microorganisms forming the biofilm that can be suppressed in the present invention include all the biofilm forming microorganisms known in the art, for example, Pseudomonas aeruginosa , Staphylococcus epidermidis , Delisea pulchra , Methicillin resistant staphylococcus aureus (MRSA), Leigonella pneumophila , Serratia , Vibrio fischeri , Vibrio harveyi , Kleb Microorganisms such as Klebsiella oxytica and Enterobacter cloacae , enterobacteria including E.
  • Pseudomonas aeruginosa Staphylococcus epidermidis , Delisea pulchra , Methicillin resistant staphylococcus aureus (MRSA), Leigonella pneumophila , Serratia , Vibrio fischeri , Vibrio harveyi , Kle
  • coli fungi such as Candida albicans , and as marine organisms, Barnacles Emphitreat, Balanus Emphitreat Community, Balanus Elegantidegatus, Megavalanus Antylene , Ctamalus malensis, ctamalus withersi, and la pas anatifera, algae (diatoms: Dunaliella, Nizshua, Skeletonema, Caesoseros genus, and Dunaliella teriorecta , Skeleto-themed Costatium species), speckled antlers, tubular monopods, red algae, molluscs, shellfish, red and brown moss, ascidian, cocci, mussels, hydroworms, vertebrates, oysters, wolves (ulba), enteromorpha, ectocorpus, ostrea, mytilus, slime; Although it includes organisms such as sea lettuce, green laver and marine spirogyra, the kind of biofilm that can be suppressed in the present invention
  • the method of suppressing the present invention is to prevent the survival and reproduction of living organisms by physical structure, rather than the method of using the microorganism-specifically reacting chemicals or another microorganism to form a biofilm, and thus, the kind of such microorganisms Without limitation, growth and proliferation can be effectively suppressed.
  • the present invention provides a water quality inspection sensor including the biofilm formation prevention substrate.
  • the method for bonding the biofilm formation preventing substrate into the water quality inspection sensor may be used without limitation the methods commonly used in the art.
  • the substrate can be wound and implemented in a cylindrical shape, and also nano and microporous structures are formed on the inner wall of the cylindrical stainless steel by using ECF and FeCl 3 methods.
  • ECF and FeCl 3 methods By implementing the cylindrical substrate having the nano- and micro-porous structure can be easily coupled in the water quality inspection sensor.
  • the cylindrical substrate is made of stainless steel having nano and micro porous structures, and nano and micro porous structures may be manufactured using ECF and FeCl 3 etching methods in a cylinder.
  • the thickness of the cylindrical substrate may be from several ⁇ m to several hundred mm.
  • the biofilm formation preventing substrate of the present invention When the biofilm formation preventing substrate of the present invention is bonded to a water quality test sensor, the biofilm is formed on the surface of the water quality test sensor to prevent or suppress contamination and corrosion by microorganisms or marine organisms. This can increase the sensitivity and reproducibility of the sensor for inspecting water contamination.
  • FIG. 1 is a diagram schematically illustrating a process of coating PS nanobeads on a surface of a flexible stainless substrate.
  • FIG. 2 is a view showing the appearance of PS nanobead coated on a flexible stainless substrate.
  • FIG. 3 is a process diagram briefly illustrating a process of etching a flexible stainless substrate without removing the PS nanobeads.
  • FIG. 4 is a process diagram briefly illustrating a process of removing PS nanobeads and etching a flexible stainless substrate.
  • FIG. 5 is a view schematically showing the structure of a water quality inspection sensor manufactured using the flexible film for preventing biofilm formation of the present invention.
  • (a) is a brief view showing the overall appearance of the structure in which the flexible substrate is packaged integrally to the water quality inspection sensor,
  • (b) is to enlarge the surface structure of the substrate used as the sensor protection net.
  • FIG. 6 is an SEM image showing the surface shape of the flexible substrate for preventing biofilm formation of the present invention.
  • (a) shows that only ECF etching is performed without removing the PS nanobeads
  • (b) shows that if both ECF and FeCl 3 etching are performed without removing the PS nanobeads
  • (c) shows PS nanobeads.
  • (d) shows the case of removing the PS nanobead and performing both the ECF and FeCl 3 etching.
  • FIG. 7 shows the results of performing microbial culture and biofilm formation experiments with respect to the flexible film for preventing biofilm formation of Examples 4 to 6 with a correlation.
  • (a) is Example 4
  • (b) is Example 5
  • (c) is a flexible substrate for preventing biofilm formation of Example 6.
  • 11 is a view showing the degree of microbial adhesion according to the change in contact angle.
  • a stainless steel (SUS304) product was polished to a thickness of several tens of micrometers through a chemical mechanical polishing (CMP) process to produce a flexible substrate.
  • CMP chemical mechanical polishing
  • the dispersion solution in which the nanobead particles were dispersed was coated on the above-described flexible substrate to arrange the nanobead particles in a single layer. After washing with acetone, the flexible stainless surface was dried using D.I and nitrogen. The process of coating the PS nanobeads on the surface of the flexible stainless substrate is shown in FIG. 1, and the appearance of the PS nanobeads coated on the flexible stainless substrate is shown in FIG. 2.
  • the spacing of the PS nanobead particles was adjusted to 10 nm to 5 ⁇ m using an oxygen plasma.
  • the substrate on which the PS nanobead particles were arranged was etched by ECF (Electro Chemical Fabrication) to prepare a flexible substrate for preventing biofilm formation of the present invention.
  • ECF Electro Chemical Fabrication
  • a stainless steel (SUS304) product was polished to a thickness of several tens of micrometers through a chemical mechanical polishing (CMP) process to produce a flexible substrate.
  • CMP chemical mechanical polishing
  • the dispersion solution in which the nanobead particles were dispersed was coated on the above-described flexible substrate to arrange the nanobead particles in a single layer. After washing with acetone, the flexible stainless surface was dried using D.I and nitrogen. The process of coating the PS nanobeads on the surface of the flexible stainless substrate is shown in FIG. 1, and the appearance of the PS nanobeads coated on the flexible stainless substrate is shown in FIG. 2.
  • the spacing of the PS nanobead particles was adjusted to 10 nm to 5 ⁇ m using an oxygen plasma.
  • the substrate on which the PS nanobead particles are arranged is etched by ECF (Electro Chemical Fabrication), and then etched for 1 minute using FeCl 3 solution to prepare a flexible film for preventing biofilm formation of the present invention. It was.
  • the overall manufacturing process of the flexible substrate for preventing biofilm formation is shown in FIG. 3.
  • a stainless steel (SUS304) product was polished to a thickness of several tens of micrometers through a chemical mechanical polishing (CMP) process to produce a flexible substrate.
  • CMP chemical mechanical polishing
  • the dispersion solution in which the nanobead particles were dispersed was coated on the above-described flexible substrate to arrange the nanobead particles in a single layer. After washing with acetone, the flexible stainless surface was dried using D.I and nitrogen. The process of coating the PS nanobeads on the surface of the flexible stainless substrate is shown in FIG. 1, and the appearance of the PS nanobeads coated on the flexible stainless substrate is shown in FIG. 2.
  • the spacing of the PS nanobead particles was adjusted to 10 nm to 5 ⁇ m using an oxygen plasma.
  • the substrate on which the PS nanobead particles were arranged was then treated with oxygen plasma to coat the substrate with a protective material, and then the PS nanobead particles were removed from the substrate.
  • the substrate from which the PS nanobead particles were removed was etched by ECF (Electro Chemical Fabrication) to prepare a flexible substrate for preventing biofilm formation.
  • ECF Electro Chemical Fabrication
  • a stainless steel (SUS304) product was polished to a thickness of several tens of micrometers through a chemical mechanical polishing (CMP) process to produce a flexible substrate.
  • CMP chemical mechanical polishing
  • the dispersion solution in which the nanobead particles were dispersed was coated on the above-described flexible substrate to arrange the nanobead particles in a single layer. After washing with acetone, the flexible stainless surface was dried using D.I and nitrogen. The process of coating the PS nanobeads on the surface of the flexible stainless substrate is shown in FIG. 1, and the appearance of the PS nanobeads coated on the flexible stainless substrate is shown in FIG. 2.
  • the spacing of the PS nanobead particles was adjusted to 10 nm to 5 ⁇ m using an oxygen plasma.
  • the substrate on which the PS nanobead particles were arranged was then treated with oxygen plasma to coat the substrate with a protective material, and then the PS nanobead particles were removed from the substrate.
  • substrate for preventing biofilm formation of this invention of 6 was produced.
  • the overall manufacturing process of the flexible substrate for preventing biofilm formation is shown in FIG. 4.
  • a water quality inspection sensor was manufactured as shown in FIG. 5 using the biofilm formation preventing flexible substrate manufactured in any one of Examples 1 to 6.
  • FIG 5 (a) is a simplified view of the overall structure of the structure in which the flexible substrate is packaged to be integrated into the water quality inspection sensor, (b) is an enlarged view of the surface structure of the substrate used as the sensor protection net.
  • the surface of the flexible film for preventing biofilm formation prepared in Examples 1 to 4 was observed by scanning electron microscope (SEM).
  • the surfaces (b and d) of Examples 2 and 4 which performed the combination treatment of ECF and FeCl 3 , were more effective than the surfaces (a and c) of Examples 1 and 3, which performed only the ECF treatment. It can be seen that relatively rough and nano-sized pores are formed.
  • the Ra value was measured as (a) at 0.28 ⁇ m, (b) at 2.99 ⁇ m, (c) at 0.05 ⁇ m, and (d) at 2.23 ⁇ m, respectively.
  • Pseudomonas aeruginosa (KCTC 1750) was used as the microorganism. After culturing a solid medium (nutrient agar) and single colony (single colony) separation was carried out liquid culture (M9 medium) for 12 hours at 37 °C. In order to form a biofilm on the chip surface, the chip was placed in a Petri dish, and then 30 ml of microbial culture solution (OD ⁇ 0.1) was poured and incubated at 37 ° C. for 3-4 days.
  • M9 medium liquid culture
  • a non-patterned flexible substrate was prepared by not using nanobeads as a control, and the non-patterned flexible substrate was not etched, and those prepared by etching with FeCl 3 for 1 minute, 3 minutes, and 5 minutes, respectively, were prepared. Microbial culture experiment was performed under the conditions.
  • each substrate was observed with an optical microscope to investigate the degree of biofilm formation.
  • FIG. 8 50 magnification
  • FIG. 9 150 magnification
  • FIG. 10 600 magnification
  • Example 4 As a result, in Example 4, it was 74.2 ° (No. 5), Example 5 was 49.8 ° (No. 6), and Example 6 was 22.6 ° (No. 7).
  • the etching time of the FeCl 3 is shorter and accordingly the contact angle is higher, the adhesion degree of the microorganisms in the flexible substrate for preventing biofilm formation of Example 4 was found to be lower.

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Abstract

Cette invention concerne un procédé de fabrication d'un substrat à l'aide de nanoparticules colloïdales pour prévenir la formation d'un biofilm, le substrat ainsi fabriqué, et un capteur d'évaluation de la qualité de l'eau présente sur le substrat. Plus particulièrement, cette invention concerne un procédé de fabrication d'un substrat pour prévenir la formation d'un biofilm par agencement de nanoparticules colloïdales sur le substrat et formation de trous et d'une structure poreuse sur ledit substrat. Cette invention concerne également un substrat pour prévenir la formation d'un biofilm constitué d'un substrat, d'une pluralité de trous formés sur la surface supérieure du substrat, et d'une structure poreuse formée sur la totalité de la surface supérieure du substrat, trous compris. Un capteur d'évaluation de la qualité de l'eau présente sur le substrat selon l'invention est, en outre, décrit.
PCT/KR2011/008854 2010-11-19 2011-11-18 Procédé de fabrication d'un substrat à l'aide de nanoparticules colloïdales pour prévenir la formation d'un biofilm, substrat ainsi fabriqué, et capteur d'évaluation de la qualité de l'eau présente sur le substrat WO2012067469A2 (fr)

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CN201180061237.5A CN103261886B (zh) 2010-11-19 2011-11-18 使用胶体纳米颗粒的用于防止生物膜形成的基板及其制备方法

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KR10-2010-0115886 2010-11-19
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KR101755469B1 (ko) * 2015-12-08 2017-07-07 현대자동차 주식회사 미세 물질 측정 센서
US20220233992A1 (en) * 2019-06-28 2022-07-28 Korea Institute Of Industrial Technology Fine particle aggregation method and apparatus
TWI797837B (zh) 2021-11-17 2023-04-01 財團法人工業技術研究院 光學式水質檢測設備

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KR20120054554A (ko) 2012-05-30
CN103261886B (zh) 2015-08-19
KR101275305B1 (ko) 2013-06-17
WO2012067469A3 (fr) 2012-07-19
CN103261886A (zh) 2013-08-21

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