WO2020242049A1 - Method for manufacturing antibacterial copper nanopowder, and antibacterial copper nanopowder manufactured thereby - Google Patents

Abstract

The present invention pertains to a method for manufacturing an antibacterial copper nanopowder, and an antibacterial copper nanopowder manufactured thereby. More specifically, the present invention pertains to: a method for manufacturing an antibacterial copper nanopowder which is produced by electric wire explosion of a copper wire and has a film layer formed on the surface thereof; and an antibacterial copper nanopowder manufactured by the manufacturing method. The present invention provides: a method for manufacturing an antibacterial copper nanopowder which is produced by electric wire explosion of a copper wire and has a film layer formed on the surface thereof; and an antibacterial copper nanopowder manufactured by the manufacturing method, thus having the effect in which a copper nanopowder having enhanced antibacterial performance, less powder agglomeration, and a lower content of impurities can be mass-produced by a simple and highly energy-efficient process at a lower cost compared to conventional copper nanopowder manufacturing processes. In addition, the present invention has the effect in which a copper nanopowder is highly stable due to having a film layer, which is amorphous or comprises a mixture of amorphous and crystalline phases, formed thereon, and can be highly dispersed without being eluted, even when mixed into yarns or resins and the like.

Description

Manufacturing method of antibacterial copper nanopowder and antibacterial copper nanopowder prepared accordingly

The present invention relates to a method for producing an antibacterial copper nanopowder and an antimicrobial copper nanopowder prepared accordingly, and more particularly, to a method of producing an antibacterial copper nanopowder in which a film layer is formed on the surface, which is produced by an electric wire explosion method of a copper wire. It relates to a method and an antimicrobial copper nanopowder prepared by this method.

Due to the rapid development of modern industrial technology, the need for new materials that can be used for microscopic parts and devices using the same has led to the synthesis and application of nanopowders of several hundreds of nanometers or less, which have superior properties compared to conventional materials of micrometer size. Interest in research is focused.

The manufacturing process of such nano-powder is largely a gas phase synthesis method in which the powder is produced through homogeneous nucleation and condensation processes, a mechanical pulverization method in which the powder is pulverized using a ball mill to make it nano, and a precipitation agent or a reducing agent is added to the aqueous solution of And a liquid phase method for producing oxide powder. The gas phase synthesis method has the advantage of being able to produce high-purity powder, but it has a disadvantage that the powder that can be produced is limited and energy consumption is large. In addition, while the mechanical grinding method or the liquid phase method can be mass-produced, there is a problem of powder contamination by a grinding tool.

In the manufacture of nanopowder, powders with high purity and uniform size that are not contaminated should not be agglomerated with each other. It satisfies these requirements and does not generate any pollutants in the production process, and as an economical metal nanopowder manufacturing technology, there is an electric wire explosion method.

Accordingly,'Korea Patent Registration No. 10-2384003' includes a plating process of plating Cr on a Ti wire, and a process of exploding Ti plated with Cr by the plating process in an electric explosion device (Ti, Cr )N Although a method for producing nanopowder has been disclosed, there is a problem that the nanopowder produced by the disclosed method is not a nanopowder having functionality such as antibacterial properties, but a material that can simply replace titanium.

In modern society, demand for a healthier, safer and more comfortable life is increasing due to highly developed industrial technology and science technology. In particular, as health problems caused by environmental pollution and environmental pollution emerge as sensitive problems worldwide, It has become an essential process to impart antimicrobial properties to various materials used closely with and used in industry. Accordingly, the present invention aims to solve this problem by providing a method of manufacturing a copper nanopowder with antimicrobial properties.

In order to solve the above problems, an object of the present invention is to provide a method of manufacturing an antibacterial copper nanopowder using an electric wire explosion method.

In addition, it is an object of the present invention to provide a copper nanopowder prepared according to a method for producing an antibacterial copper nanopowder.

In order to solve the above object, the present invention,

A first step of supplying a copper wire into the reaction chamber filled with the mixed gas;

A second step of forming a copper nanopowder by applying energy to the copper wire supplied into the reaction chamber to cause electric explosion; And

It provides a method for producing an antibacterial copper nanopowder comprising a; a third step of forming an amorphous coating layer or a coating layer in which amorphous and crystalline are mixed on the surface of the copper nanopowder.

It is characterized in that the internal pressure of the reaction chamber filled with the mixed gas is 1 to 5 bar.

The copper wire has a diameter of 0.1 to 0.5 mm, and the copper nanopowder has a particle diameter of 50 to 200 nm.

The copper nanopowder is formed by evaporation and condensation of the copper wire to which the energy is applied, and the energy is 1000 to 2000 J.

Antibacterial copper nanopowder is characterized by exhibiting an antibacterial effect of 90 to 99.99% against at least one selected from the group consisting of Escherichia coli, Pseudomonas aeruginosa, pneumonia, MRSA, Bacillus, Candida, streptococcus, and Staphylococcus aureus. .

In order to solve the above other object, the present invention,

It provides an antibacterial copper nanopowder prepared by a method of producing an antibacterial copper nanopowder.

The present invention is produced by the electric wire explosion method of a copper wire, by providing a method for producing an antibacterial copper nanopowder in which a film layer is formed on the surface, and an antibacterial copper nanopowder produced by this method, the conventional copper nanopowder manufacturing process The cost is cheaper, the process is simple, the energy efficiency is excellent, the mass production is possible, the antibacterial performance of the copper nanopowder is strengthened, and the cohesiveness of the powder and the content of impurities are reduced. In addition, since the amorphous or amorphous and crystalline coating layer is formed on the copper nanopowder, stability is high, and even when mixed with yarn or resin, it is not eluted and can be highly dispersed.

1 is a schematic diagram of a reaction chamber for forming a copper nanopowder according to an embodiment of the present invention.

2A is a TEM image of a shape and a surface of a copper nanopowder according to an embodiment of the present invention.

2B is a TEM image showing surface characteristics of a copper nanopowder according to an embodiment of the present invention.

2C is a TEM image showing the surface properties of a copper nanopowder according to a comparative example of the present invention.

3A is an XRD graph of a copper nanopowder according to an embodiment of the present invention.

Figure 3b is a graph confirming the content of copper and copper oxide (Cu ₂ O) according to the XRD result of the copper nanopowder according to an embodiment of the present invention.

Figure 4 shows the results of an antimicrobial test for streptococci of a copper nanopowder according to an embodiment of the present invention.

5 shows the results of an antimicrobial test for Candida bacteria of a copper nanopowder according to an embodiment of the present invention.

6 shows the results of an antimicrobial test for pneumococcal bacteria of a copper nanopowder according to an embodiment of the present invention.

7 shows the results of an antimicrobial test for antibiotic-resistant bacteria (MRSA) of a copper nanopowder according to an embodiment of the present invention.

8 shows the results of an antimicrobial test for Bacillus bacteria of a copper nanopowder according to an embodiment of the present invention.

9 shows the results of an antimicrobial test for E. coli of a copper nanopowder according to an embodiment of the present invention.

10 shows the results of an antimicrobial experiment on Pseudomonas aeruginosa of copper nanopowder according to an embodiment of the present invention.

11 shows the results of an antimicrobial test for Staphylococcus aureus of a copper nanopowder according to an embodiment of the present invention.

12 is an image of a functional fiber yarn in which copper nanopowder is dispersed according to an embodiment of the present invention.

13 is a test report confirming the copper content after washing of a fabric woven with functional fibers according to an embodiment of the present invention.

In the present specification, when a part "includes" a certain component, it means that other components may be further included rather than excluding other components unless otherwise stated.

Hereinafter, the present invention will be described in more detail.

The present invention relates to a method for producing an antimicrobial copper nanopowder produced by an electric wire explosion method of a copper wire and having a film layer formed on the surface thereof, and to an antibacterial copper nanopowder produced by the method.

According to an aspect of the present invention, a first step of supplying a copper wire into a reaction chamber filled with a mixed gas; A second step of forming a copper nanopowder by applying energy to the copper wire supplied into the reaction chamber to cause electric explosion; And a third step of forming an amorphous coating layer or a coating layer in which amorphous and crystalline are mixed on the surface of the copper nanopowder. It provides a method of producing an antimicrobial copper nanopowder comprising:

In the present invention, a copper nanopowder can be prepared using an electric wire explosion method. The electric wire explosion method is a method of manufacturing nano powder by using the phenomenon that the metal wire explodes in the form of fine particles or vapors when a high-density current is passed through the metal wire. The production speed is relatively fast and various pure metals, oxides, nitrides, alloys, And it is possible to prepare a nanopowder of the intermetallic compound. In addition, since pulse power is used in the process, energy consumption is low, and there are no by-products other than the powder to be produced, which is environmentally friendly.

The principle of manufacturing nanopowder by electric ray explosion method is as follows. When a strong impact current is applied to the metal wire positioned between the two electrodes, the metal wire becomes molten due to the resistance heating generated at this time, and discharge occurs and vaporizes as the temperature continues to increase thereafter. The vaporized metal gas is confined inside the wire rod, and when the vapor pressure rises above the threshold value, it expands instantaneously to form a shock wave, and metal fine particles and gas are ejected at high speed to form fine particles as a result.

In the present invention, the diameter of the copper wire may be 0.1 to 0.7 mm, and when supplied into the reaction chamber, a copper wire having a length of 80 to 140 nm may be added at a time. The diameter and length of the copper wire may be determined according to the amount of energy applied to the copper wire. If the diameter of the copper wire is less than 0.1 nm, the thickness of the wire is too thin, which may interfere with the continuous production of copper nanopowder. If it exceeds 0.7 mm, the size of the particle increases due to insufficient applied energy. It can be produced by mixing particles and nano-scale particles. Preferably, in the present invention, the diameter of the copper wire, that is, the thickness may be 0.1 to 0.5 mm.

In addition, the internal pressure of the reaction chamber filled with the mixed gas of the present invention may be 1 to 5 bar. If the internal pressure of the reaction chamber filled with the mixed gas is less than 1 bar, the shape or particle size of the copper nanopowder cannot be properly formed. If it exceeds 5 bar, the pressure inside the reaction chamber increases, causing stability problems such as explosion. And the consumption of the mixed gas can be increased. The mixed gas may be a gas in which at least one selected from nitrogen, argon, and oxygen is mixed, and preferably, a mixed gas including argon gas and nitrogen or a mixed gas including argon gas and oxygen.

1 is a view showing a schematic diagram of a reaction chamber for forming a copper nanopowder. According to FIG. 1, a copper wire may be supplied into a reaction chamber filled with a mixed gas through a wire feeding system and then electrically explode to form a copper nanopowder. In the step of forming the copper nanopowder, the mixed gas filled in the reaction chamber is circulated back to the reaction chamber through the injection pipe and discharge pipe and filtering systems 1, 2, and 3 provided in the reaction chamber. And the discharge pipe can be interconnected through a connector. In addition, each filtration system of the connecting pipe may be provided with a collecting powder that collects copper nanopowder formed by an electric explosion, and the container is supplied to the inside of the reaction chamber through an injection pipe and then through a discharge pipe. The discharged mixed gas and copper nanopowder formed by the electric explosion may be discharged and collected.

In the method of manufacturing copper nanopowder, the electric explosion is to evaporate and condense the copper wire by generating a pulse power charged with a capacitor, which is an energy storage device, and instantaneously applying the generated pulse power of 1000 to 3000 J to the copper wire. , As a result of this, a copper nanopowder having a particle diameter of 50 to 200 nm may be formed.

The pulse power applied to the copper wire may be determined according to the diameter and length of the copper wire, and the particle size of the copper nanopowder may be determined due to process factors such as pulse power, application speed, and pressure inside the chamber. In general, the higher the applied energy and the faster the application speed, the higher the rate of generation of small particle diameters. In the method for producing an antibacterial copper nanopowder using the electric wire explosion method of the present invention, a pulse power of 1000 to 3000 J is preferably applied to the copper wire to form a copper nanopowder having a particle diameter of 50 to 200 nm. At this time, the pulse power, that is, the energy may be more preferably 1000 to 2000 J.

In general, metals such as copper form a crystal phase having a regular crystal structure in which atoms are arranged at room temperature, and can be said to be an aggregate of fine crystals. Crystals theoretically mean that the arrangement of atoms has a three-dimensional, regular pattern, and the state in which these crystals have properties is called crystalline.

On the other hand, amorphous (amorphous) is a state in which the arrangement of a plurality of atoms or molecules is regular or non-periodic, and has superior properties such as toughness, battery resistance, hardness, abrasion resistance, corrosion resistance, strength, biocompatibility, and processability compared to crystalline . In order to utilize the amorphous material exhibiting such mechanical and chemical properties, an alloy or metal itself may be manufactured in an amorphous form, but this may be an ineffective and uneconomical method. Accordingly, by coating an amorphous material on the surface of the base material, it is possible to manufacture a metallic material that is more efficient and economical and exhibits excellent amorphous properties.

Copper nanopowder does not originally contain a surface layer, and if a surface layer, that is, a film layer, is not formed, it may explode due to the high reactivity of the copper nanopowder itself. Therefore, in order to use the copper nanopowder in the industrial field, a surface layer must be formed arbitrarily.

In the present invention, in order to prevent corrosion due to the high explosiveness and oxidation properties of the copper nanopowder at room temperature or in the atmosphere, and to secure stability, a film layer having a thickness of several nanometers is formed on the surface to passivate it (passivation). have. In addition, a coating layer may be formed on the surface of the copper nanopowder through a process of injecting air into the copper nanopowder formed by an electric explosion and collected in a container and then leaving it for 12 to 24 hours.

The coating layer formed at this time is an amorphous or a mixture of amorphous and crystalline, and can prevent oxidation of the copper nanopowder, and thus the surface of the finally prepared antibacterial copper nanopowder is 1 to 10 nm, preferably 1 to 3 nm. A coating layer of may be formed. Unlike the crystalline coating layer, this coating layer does not peel off, so that the surface of the copper nanopowder can be stably coated. The coating layer of the present invention may be formed through an oxidation process, and may also be referred to as an oxide film.

The antibacterial copper nanopowder prepared according to the manufacturing method of the present invention is 90 to 99.99% with respect to at least one selected from the group consisting of E. coli, Pseudomonas aeruginosa, pneumonia, MRSA, Bacillus, Candida, streptococcus, and Staphylococcus aureus. It can exhibit the antibacterial effect of.

In addition, the antimicrobial copper nanopowder of the present invention is copper oxide having an amorphous or amorphous and crystalline surface layer (Cu ₂ O) unlike the copper oxide nanopowder having a crystalline surface layer (CuO) formed by the conventional electric ray explosion method. The nanopowder exhibits excellent amorphous properties (stability, storage), and the surface layer is made of Cu ₂ O, which exhibits excellent antimicrobial properties, and thus can exhibit superior antimicrobial properties than conventional copper or copper oxide nanopowder.

According to another aspect of the present invention, there is provided an antibacterial copper nanopowder prepared by a method for producing an antibacterial copper nanopowder.

The antibacterial copper nanopowder comprises a first step of supplying a copper wire into a reaction chamber filled with a mixed gas; A second step of forming a copper nanopowder by applying energy to the copper wire supplied into the reaction chamber to cause electric explosion; And a third step of forming an amorphous coating layer or a coating layer in which amorphous and crystalline mixtures are mixed on the surface of the copper nanopowder. It can be prepared through a method of manufacturing an antibacterial copper nanopowder comprising.

The diameter of the supplied copper wire may be 0.1 to 0.7 mm, preferably 0.1 to 0.5 mm, and when supplied into the reaction chamber, a copper wire having a length of 80 to 140 nm may be added at one time. The diameter and length of the copper wire may be determined according to the amount of energy applied to the copper wire. If the diameter of the copper wire is less than 0.1 nm, the thickness of the wire is too thin, which may interfere with the continuous production of copper nanopowder. If it exceeds 0.7 mm, the size of the particle increases due to insufficient applied energy. It can be produced by mixing particles and nano-scale particles.

In addition, the internal pressure of the reaction chamber filled with the mixed gas of the present invention may be 1 to 5 bar. If the internal pressure of the reaction chamber filled with the mixed gas is less than 1 bar, the shape or particle size of the copper nanopowder cannot be properly formed. If it exceeds 5 bar, the pressure inside the reaction chamber increases, causing stability problems such as explosion. And the consumption of the mixed gas can be increased. The mixed gas may be a gas in which at least one selected from nitrogen, argon, and oxygen is mixed, and preferably, a mixed gas including argon gas and nitrogen or a mixed gas including argon gas and oxygen.

During the manufacturing process, the electric explosion generates a pulse power charged with a capacitor, which is an energy storage device, and instantaneously applies the generated pulse power to the copper wire to evaporate and condense the copper wire, resulting in a particle diameter of 50 to 200. nm copper nanopowder can be formed.

The pulse power applied to the copper wire may be determined according to the diameter and length of the copper wire, and the particle size of the copper nanopowder may be determined due to process factors such as pulse power, application speed, and pressure inside the chamber. In general, the higher the applied energy and the faster the application speed, the higher the rate of generation of small particle diameters.

The antibacterial copper nanopowder prepared by the method for producing the antibacterial copper nanopowder of the present invention may be prepared through the above manufacturing process, and may be formed using the reaction chamber of FIG. 1. In order to prevent corrosion of the formed copper nanopowder from high explosiveness and oxidation caused by oxidation at room temperature or in the atmosphere, and to secure stability, a film layer having a thickness of several nanometers can be formed on the surface to be passivated (passivation). In addition, a coating layer may be formed on the surface of the copper nanopowder through a process of injecting air into the copper nanopowder formed by an electric explosion and collected in a container and then leaving it for 12 to 24 hours.

The coating layer formed at this time is an amorphous or a mixture of amorphous and crystalline, and can prevent oxidation of the copper nanopowder, and thus the surface of the finally prepared antibacterial copper nanopowder is 1 to 10 nm, preferably 1 to 3 nm A coating layer of may be formed. Unlike the crystalline coating layer, this coating layer does not peel off, so that the surface of the copper nanopowder can be stably coated. The coating layer of the present invention may be formed through an oxidation process, and may also be referred to as an oxide film.

Such antibacterial copper nanopowder may exhibit an antimicrobial effect of 90 to 99.99% against at least one selected from the group consisting of Escherichia coli, Pseudomonas aeruginosa, pneumonia, MRSA, Bacillus, Candida, streptococcus, and Staphylococcus aureus. In addition, unlike copper oxide nanopowder having a crystalline surface layer (CuO) formed by the conventional electric ray explosion method, it is a copper oxide nanopowder having an amorphous or amorphous and crystalline surface layer (Cu ₂ O) with excellent amorphous properties ( Stability and preservation), and the surface layer is made of Cu ₂ O showing excellent antimicrobial properties, so that it can exhibit superior antimicrobial properties than conventional copper or copper oxide nanopowder.

Hereinafter, examples will be described in detail in order to describe the present specification in detail. However, the embodiments according to the present specification may be modified in various forms, and the scope of the present specification is not construed as being limited to the embodiments described below. The embodiments of the present specification are provided to more completely describe the present specification to those of ordinary skill in the art.

<Example>

Example 1-Copper nanopowder formation (electric wire explosion method)

A copper wire with a diameter of 0.4 mm and a length of 80 mm was supplied to the inside of the reaction chamber filled with mixed gas at a pressure of 3 bar, and then the pulse power charged with the capacitor was instantaneously applied to the copper wire by 2000 J. It was evaporated and then condensed to form a copper nanopowder.

Example 2-Passivation of copper nanopowder

In order to increase the stability of the copper nanopowder formed according to Example 1, air was injected into the container in which the copper nanopowder was collected at a rate of 5 cc/min and left for 24 hours to form a film layer on the surface of the copper nanopowder. Made it.

Comparative Example 1-Copper nanopowder formation (plasma method)

In the process of injecting various inorganic materials such as metals, ceramics, oxides, etc. into the ultra-high temperature plasma region around 10,000 ^o C to obtain nano powders through the steps of vaporization, nuclear growth, and rapid cooling, a plasma method of forming metal nano powders is used. The prepared copper nanopowder was used as a comparative example of Example 1.

Preparation Example 1-Preparation of a masterbatch containing copper nanopowder

Air was injected into the container in which the copper nanopowder formed according to Examples 1 and 2 was collected, and allowed to stand for 24 hours while injecting air at a rate of 5 cc/min to form an oxide film on the surface of the copper nanopowder. 50 g of copper nanopowder stabilized through a passivation process and 450 g of polyethylene terephthalate (PET) were mixed at 90 rpm at 280°C using a compressor to obtain a masterbatch containing 10 wt% of copper nanopowder. Was prepared.

In the present invention, as an example, a master batch containing copper nanopowder was prepared, and then fiber yarn and fabric were produced, and excellent dispersibility and adhesion of the copper nanopowder through the fiber yarn and fabric were confirmed. At this time, the master batch may be prepared and used without limitation, as long as it is a thermoplastic resin, and polyethylene terephthalate was used as a manufacturing example.

Preparation Example 2-Preparation of functional fiber yarn containing copper nanopowder

250 g of the masterbatch containing the copper nanopowder prepared according to Examples 1 to 3 was mixed with 4,750 g of PET, spun according to the conditions shown in Table 1 below, and finally contained 0.5 wt% of the copper nanopowder. To prepare a functional fiber yarn.

Contents	Conception		Unit	PET + Cu → 0.5wt%
Chip	Chip		kind	PET SD + 8wt% Cu M/B
Extruder	Heater Temp. #1~4		℃	278	286	286	285
	Melting Temp.		℃	287
	Die Head Temp.		℃	285
	Spin Pack Temp.		℃	282
	MP Speed		rpm	8 (MP capacity: 0.6cc/rev)
	Die Head Pressure			Bar	20
Godet R/O		GR 1	Speed	m/min	170
			Temp.	℃	85
	GR 2	Speed	m/min	420
		Temp.	℃	82
	Draw ratio		-	2.47
Quenching	Air volume			%	30
	Temp.		℃	15
Winder	Speed		rpm	1,250 (approx. 450 m/min)

Preparation Example 3-Fabric weaving of functional fiber yarn

The fabric was woven using the yarn manufactured according to the same method as in the above example, and the used yarn is shown in Table 3 below.

division	Used yarn	T/M	Year direction	Main
slope		PET SD 50/36	450	Z	9,600
Weft	PET +　Cu yarn 115/18	450	Z	One

Using the warp and weft of Table 3, a functional fiber fabric containing 0.5 wt% of copper nanopowder was woven according to the weaving conditions of Table 4 below.

division			Condition
Speaker	Covering	T/M	450
		Year direction	Z
Weaving	slope		density	90 sheets/inch
		Main	9,600 copies
	Weft		80 sheets/inch
	Weaving density		80T/inch
	Fabric tissue		Plain weave
	Weaving quantity		5yds

<Experimental Example>

Experimental Example 1-Analysis of copper nanopowder transmission electron microscopy

In order to measure the shape and properties of the copper nanopowder according to the above example, it was measured under the conditions of 300 kV Extraction Voltage and 36 μA FEG Emiision using FEI's Tecnai G2 F30 S-TWIN.

Experimental Example 2-Copper nanopowder X-ray diffraction analysis

In order to analyze the crystal structure and composition of the copper nanopowder according to the above example, it was measured under the conditions of an angle of 20-100 ^o , a Step Size of 0.04, and a Timp per Step 0.5 using PANalytical's Empyrean.

Experimental Example 3-Copper nanopowder antibacterial evaluation

In order to confirm the antimicrobial properties of the copper nanopowder according to the above example, an experiment was conducted according to the test standard of KCL-FIR-1002:2011. Test strains include Streptococcus mutans ATCC 25175, Candida, Candida albicans ATCC 10231 , Klebisiella pneumoniae ATCC 4352, a pneumococcus, Staphylococcus aureus subsp. aureus ATCC 33591, Bacillus cereus 11778, and E. Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 15442, and Staphylococcus aureus ATCC 6538 were used, respectively, 3.7×10 ⁶ CFU/ml, 3.9×10 ⁶ CFU/ml, 1.0×10 ⁶ CFU for each medium. /ml, 1.1×10 ⁶ CFU/ml, 1.2×10 ⁶ CFU/ml, 1.0×10 ⁶ CFU/ml, 2.0×10 ⁶ CFU/ml, and 1.0×10 ⁶ CFU/ml. Using the culture medium inoculated with the bacteria, a medium containing 4 g of copper nanopowder and a medium containing nothing were cultured in an incubator at about 37° C. for 24 hours to measure the concentration of the bacteria.

Experimental Example 4-Copper nanopowder anti-mold evaluation

In order to confirm the antifungal efficacy of the copper nanopowder according to the above embodiment, the test strain mixed spore solution was inoculated in 100 ml of distilled water to which 4g of copper nanopowder was added, reacted for 24 hours, and then cultured in a solid medium for 5 days to grow mold. Check the presence or absence. Aspergillus brasiliensis ATCC 9642, Penicillium pinophilum ATCC 11797, Chaetomium globosum ATCC 6205, Trichoderma virens ATCC 9645, and Aureobasidium pullulans ATCC 15233 were used as test strains.

Experimental Example 5-Image measurement of functional fiber yarn in which copper nanopowder was dispersed (SEM)

A PET fiber yarn containing 0.5 wt% of copper nanopowder prepared according to the above Examples and Preparation Examples was used with a LYRA3 scanning electron microscope to obtain a SEM (Scanning Electron Microscope) image under the conditions of an acceleration voltage of 10 kV, a working distance of 9 mm, and an intensity of 10. Photographed.

Experimental Example 6-Copper nanopowder dissolution test of functional fiber fabric

In order to check the elution amount of the copper nanopowder before and after washing (30 times) of the functional fabric prepared according to the above Examples and Preparation Examples, the copper content was measured before and after washing the fabric according to KS K ISO 6330:2011.

<Evaluation and results>

Results 1-Transmission electron microscopy analysis of copper nanopowder

The copper nanopowder according to the Examples and Comparative Examples was observed according to Experimental Example 1, and the results are shown in FIGS. 2A to 2C.

In Figure 2a, the shape of the copper nanopowder formed according to the embodiment could be confirmed through a TEM image measured based on 100 nm, and 1 to 3 nm on the surface of the copper nanopowder through a TEM image measured based on 5 nm It was confirmed that an amorphous coating layer was formed. In addition, in FIG. 2B, it was confirmed that amorphous and crystalline film layers were simultaneously formed on the surface of the copper nanopowder according to the embodiment. Accordingly, it was found that the copper nanopowder of the present invention forms an amorphous coating layer or a coating layer in which amorphous and crystalline are mixed on the surface.

On the other hand, it was confirmed that the surface of the copper nanopowder formed according to the comparative example formed a crystalline film layer through the TEM image measured based on 5 nm in FIG. 2C.

Results 2-X-ray diffraction analysis of copper nanopowder

According to the above Examples and Experimental Example 2, the components of the copper nanopowder were analyzed through X-Ray Diffraction (XRD), and the results are shown in FIGS. 3A and 3B.

In the XRD graph of the copper nanopowder, the peaks of Cu and Cu ₂ O were detected, and it was confirmed that Cu and Cu ₂ O in the copper nanopowder were contained in 93.4 wt% and 6.6 wt%, respectively. In addition, in the XRD graph, the graph line was shown to have very severe noise, indicating that the coating layer of the copper nanopowder was formed including the amorphous coating layer.

Results 3-Evaluation of antimicrobial properties of copper nanopowder

The antimicrobial properties of the copper nanopowder were confirmed according to the above Examples and Experimental Example 3, and the results are shown in FIGS. 4 to 11.

As a result, in the medium without any treatment, the strain concentration increased or showed an insignificant reduction rate, but in the medium containing copper nanopowder, all eight strains compared to the initial test strain concentration, when compared to the initial test strain concentration, more than 99.9% bacteria It showed a reduction rate.

In Figures 4 to 11 (a), which is the result of including the copper nanopowder, the growth of the bacteria could not be confirmed with the naked eye, but the control group without any treatment in Figures 4 to 11 (b) shows that the bacteria were grown. I could confirm.

Results 4-Copper nanopowder anti-fungal evaluation

As a result of confirming the antifungal properties of the copper nanopowder according to the above Examples and Experimental Example 4, it was confirmed that all five fungal strains did not grow in the medium, and that the copper nanopowder of the present invention has antifungal efficacy in addition to antibacterial properties. Could know.

Results 5-Image of functional fiber yarn with copper nanopowder dispersed

According to the above Example and Experimental Example 5, the fiber yarn in which the copper nanopowder was dispersed was magnified to take an SEM image, and the results are shown in FIG. 12.

When the yarn was enlarged, it was confirmed that functional copper nanoparticles were evenly dispersed on the surface of the yarn, and through this, it was found that the functional fiber yarn of the present invention can exhibit the properties of the antibacterial copper nanopowder.

Results 6-Copper nanopowder dissolution test result of functional fiber fabric

The elution amount of the copper nanopowder before and after washing the functional fabrics prepared according to the above Examples and Preparation Examples was confirmed according to Experimental Example 6, and the test report is shown in FIG. 13.

As a result, the content of copper nanopowder, which was 5.489 mg/kg before washing, was measured as 5.428 mg/kg after washing 30 times (detection limit 10 mg/kg), and the elution amount of copper in the fabric was about 0.98 wt%. When comparing this with a commercially available copper-containing fabric (CuS-containing), it was found that the commercially available K company's copper-containing fabric had an elution amount of 46 wt% of copper, and that the copper elution amount of the fabric according to the present invention was very small. .

Therefore, the copper nanopowder of the present invention is hardly eluted during the process of spinning a fiber yarn using a master batch and weaving a fabric using a fiber yarn, and is added to various materials due to such excellent adhesion to It was confirmed that a functional material exhibiting characteristics could be manufactured.

Claims (8)

1. A first step of supplying a copper wire into the reaction chamber filled with the mixed gas;

   A second step of forming a copper nanopowder by applying energy to the copper wire supplied into the reaction chamber to cause electric explosion; And

   A third step of forming an amorphous coating layer or a coating layer in which amorphous and crystalline are mixed on the surface of the copper nanopowder.
2. The method of claim 1,

   The method for producing antibacterial copper nanopowder, characterized in that the internal pressure of the reaction chamber filled with the mixed gas is 1 to 5 bar.
3. The method of claim 1,

   The method for producing antibacterial copper nanopowder, characterized in that the diameter of the copper wire is 0.1 to 0.5 mm.
4. The method of claim 1,

   The method for producing an antibacterial copper nanopowder, characterized in that the particle diameter of the antibacterial copper nanopowder is 50 to 200 nm.
5. The method of claim 1,

   The antibacterial copper nanopowder is formed by evaporation and condensation of the copper wire to which the energy is applied.
6. The method according to claim 1 or 5,

   The energy is 1000 to 2000 J method for producing an antibacterial copper nanopowder, characterized in that.
7. The method of claim 1,

   The antimicrobial copper nanopowder is characterized in that it exhibits an antibacterial effect of 90 to 99.99% against at least one selected from the group consisting of Escherichia coli, Pseudomonas aeruginosa, pneumococcal, MRSA, Bacillus, Candida, streptococcus, and Staphylococcus aureus. Method for producing antibacterial copper nanopowder.
8. Antibacterial copper nanopowder prepared by the manufacturing method according to claim 1.

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