KR20220127411A - Manufacturing method of graphene nano composite powder - Google Patents

Abstract

The present invention relates to a method for producing graphene nanocomposite powder. The method for producing graphene nanocomposite powder comprises the steps of: inserting a metal wire into a mixed solution in which graphene oxide is dispersed; and forming nanopowder containing metal or metal oxide by reacting the graphene oxide with metal powder formed by applying energy to the metal wire loaded in the mixed solution and electrically detonating the metal wire. The step of forming nanopowder includes the processes of: forming reduced graphene oxide in which reduction and defect healing of the graphene oxide are performed due to the exploding metal wire; and forming a composite structure by binding the metal or metal oxide-containing nanopowder with the reduced graphene oxide. According to the present invention, the graphene nanocomposite powder produced thereby contains oxygen in an amount of 5% or less. Therefore, an additional reduction process can be omitted.

Description

Manufacturing method of graphene nano composite powder {Manufacturing method of graphene nano composite powder}

The present invention relates to a method for manufacturing a graphene nanocomposite powder, and more particularly, to a nanocomposite powder made of graphene-metal or graphene-metal oxide using an electric explosion and a method for manufacturing the same.

Recently, by grafting nanotechnology to refine metals (about 100 nm or less), the volume effect due to the increase of the surface area of the metal and new mechanical/physical properties expressed by the interaction between metal particles are attracting attention. In addition, interest in composite powder materials capable of adding new functions or improving electrical properties while maintaining properties through dispersion of inorganic materials in conventional metal powders is growing.

On the other hand, graphene is a layered material composed of one layer of carbon atoms. Graphene is attracting attention as an inorganic material as a reinforcing agent for metal powder because of its excellent thermal conductivity, electrical conductivity, large surface area, high chemical stability and light weight. For this reason, the development of graphene and metal powder or graphene and metal oxide composite material is being studied. In the prior art, a metal salt is provided in a solvent in which graphene oxide is dispersed, and reduced through heat treatment with a reducing agent to prepare a composite powder in which graphene is dispersed between base metal powders. have. However, when using the conventional method, there is a problem in that the process steps are also complicated, and the process cost and time are required accordingly.

An object of the present invention is to solve various problems including the above problems, and an object of the present invention is to provide a method for manufacturing a graphene nanocomposite powder having excellent mechanical/physical properties. However, these problems are exemplary, and the scope of the present invention is not limited thereto.

According to one aspect of the present invention for solving the above problems, there is provided a method for manufacturing a graphene nanocomposite powder. The manufacturing method of the graphene nanocomposite powder comprises: charging a metal wire into a mixed solution in which graphene oxide is dispersed; And the metal powder formed by applying energy to the metal wire charged in the mixed solution to electrically explode the metal wire and the graphene oxide react with each other to form a nanopowder including a metal or a metal oxide; Including, wherein the forming of the nanopowder comprises: forming a reduced graphene oxide in which the reduction and defect healing of the graphene oxide is made due to the exploding metal wire; and combining the nanopowder including the metal or the metal oxide with the reduced graphene oxide to form a composite structure.

In the method of manufacturing the graphene nanocomposite powder, the composite structure may have a structure in which the reduced graphene oxide in the form of a thin film is combined between the nanopowders so that the nanopowder surrounds the reduced graphene.

In the manufacturing method of the graphene nanocomposite powder, the nanopowder may have a size of 100 nm or less (greater than 0).

In the manufacturing method of the graphene nanocomposite powder, the step of forming the nanopowder includes the step of applying a voltage pulse equal to or greater than the energy required for sublimation of the metal wire in consideration of the size of the metal wire charged in the mixed solution. may include

In the method of manufacturing the graphene nanocomposite powder, the voltage pulse may be a voltage (V) calculated in consideration of the sublimation energy of the metal wire and the capacitor capacity (C) of the device.

In the method for producing the graphene nanocomposite powder, the mixed solution is mixed with a stirrer after dispersing the graphene oxide in an organic solvent, and optionally distilled water may be further contained.

In the method for producing the graphene nanocomposite powder, the organic solvent is acetone, pyridine, methyl ethyl ketone, methyl alcohol, ethyl alcohol, isopropyl alcohol, butyl alcohol, ethylene glycol, polyethylene glycol, tetrahydrofuran, Dimethylformamide, dimethylacetamide, N-methyl-2-pyrrolidone, hexane, cyclohexanone, toluene, chloroform, dichlorobenzene, dimethylbenzene, trimethylbenzene, methylnaphthalene, nitromethane, acrylonitrile, octadecylamine , may include any one selected from aniline and dimethyl sulfoxide, or a mixture of two or more.

In the manufacturing method of the graphene nanocomposite powder, the reduced graphene oxide may have an oxygen content of 5% or less (more than 0).

In the method of manufacturing the graphene nanocomposite powder, the reduced graphene oxide may be grown in the region where the pore defects of the graphene oxide exist, so that 95% or more of the pore defects can be healed.

In the method of manufacturing the graphene nanocomposite powder, the metal wire may have a diameter of 1 mm or less (more than 0), and the length of the metal wire may have a length of 10 cm or less (more than 0).

In the manufacturing method of the graphene nanocomposite powder, the metal wire is manganese (Mn), copper (Cu), chromium (Cr), iron (Fe), nickel (Ni), cobalt (Co), gold (Au) , may include any one or a mixture of two or more of transition metal elements such as silver (Ag) and platinum (Pt).

According to an embodiment of the present invention made as described above, it is possible to provide a method for manufacturing a graphene nanocomposite powder capable of shortening the process cost and process time compared to the conventional graphene composite powder manufacturing process. Since the graphene nanocomposite powder prepared by the above preparation method contains 5% or less of oxygen, it is possible to omit an additional reduction process. In addition, the antioxidative effect of the metal nanopowder can be expected by the improvement of electrical conductivity and graphene. The scope of the present invention is not limited by these effects.

1 is a process flow chart schematically illustrating a method of manufacturing a graphene nanocomposite powder according to an embodiment of the present invention.
2 is a diagram schematically illustrating the structure of an electric explosive device according to an embodiment of the present invention.
Figure 3 is an experimental example of the present invention, (a) Comparative Examples 1 and (b) the graphene oxygen content of Example 1 is the result of analysis by the energy dispersive spectroscopy (EDS) of a transmission electron microscope (TEM) .
4 is an experimental example of the present invention, (a) Comparative Example 1 and (b) an image of the graphene defect distribution of Example 1 analyzed with a transmission electron microscope (TEM).
Figure 5 is an experimental example of the present invention, (a) Examples 1 and (b) is an image of the nano-composite powder form of Example 4 analyzed with a scanning electron microscope.
Figure 6 is an experimental example of the present invention, Examples 1 to 6 and Comparative Example 1 of the nano-composite powder of the analysis results by Raman spectroscopy.
7 is an experimental example of the present invention, the results of analysis of the nanocomposite powder of Examples 1, 3, 4 and 6 by X-ray diffraction (XRD) method.
FIG. 8 is an experimental example of the present invention, showing the results of measuring the conductivity of Examples 1 and 2 by a powder resistance measurement method.
9 is an experimental example of the present invention, and is a result of analyzing the electromagnetic wave shielding characteristics of Examples 1 and 4.

Hereinafter, the present invention will be described in more detail with reference to Examples and the accompanying drawings. These examples are only for illustrating the present invention in more detail, and it will be apparent to those of ordinary skill in the art to which the present invention pertains that the scope of the present invention is not limited by these examples.

Hereinafter, with reference to the drawings, a method of manufacturing a graphene nanocomposite powder using a single process of an electric explosion method will be described in detail.

1 is a process flow chart schematically illustrating a method of manufacturing a graphene nanocomposite powder according to an embodiment of the present invention.

Referring to FIG. 1 , the method (S100) of manufacturing a graphene nanocomposite powder according to an embodiment of the present invention includes a step (S110) of charging a metal wire in a mixed solution in which graphene oxide is dispersed, the charged in the mixed solution. The metal powder formed by applying energy to the metal wire to electrically explode the metal wire and graphene oxide react with each other to form a nanopowder containing a metal or metal oxide (S120), collecting the nanopowder ( S130) may be included.

Specifically, the step of forming the nanopowder (S120) is a step of forming a reduced graphene oxide in which the reduction and defect healing of the graphene oxide is made due to the exploding metal wire, and the nano containing the metal or metal oxide. It may include the step of forming a composite structure by combining the powder and the reduced graphene oxide.

Here, the graphene oxide (GO) is based on a carbon structure in the form of a sheet such as graphene. It is known that various oxygen functional groups, for example, a hydroxyl group, an epoxy group, a carboxyl group, and a ketone group, are bonded to the upper surface or end of the sheet.

The metal wire is exploded by receiving a voltage pulse greater than the energy required for sublimation of the metal. At this time, the metal expands by dissipating heat due to high energy, and is dispersed in the mixed solution to form a nanopowder of metal or metal oxide. In this process, the metal or metal oxide nanopowder is combined with the graphene oxide contained in the mixed solution to form a reduced graphene oxide as the oxygen functional groups are broken in the process of being complexed. At this time, the physical and electrical properties of graphene are also restored. The graphene nanocomposite powder prepared in this way can be applied in fields such as electromagnetic wave shielding or anode materials for supercapacitors and heat dissipation films.

The graphene nanocomposite powder implemented by the manufacturing method of the graphene nanocomposite powder according to an embodiment of the present invention may be provided as an electromagnetic wave shielding sheet, a heat dissipation film, and an electrode or electrode contact of an energy storage device, and the application field Since the method applied to them is already known in the art, a detailed description thereof will be omitted.

On the other hand, the reduced graphene oxide may have an oxygen content of 5% or less (more than 0). In the present invention, the reduced graphene oxide may be one in which 95% or more of the pore defects are healed by the growth of graphene in the region where the pore defects of the graphene oxide exist.

The composite structure including the nanopowder has a structure in which the reduced graphene oxide in the form of a thin film is combined between the nanopowders so that the nanopowder surrounds the reduced graphene. The nanopowder has a size of 100 nm or less (greater than 0). Nanopowders containing such reduced graphene oxide have relatively better electrical conductivity compared to metal nanopowders having the same packing density.

Meanwhile, by supplying energy necessary for sublimation of the metal material constituting the metal wire, the metal wire may be exploded in the organic solvent in which the graphene oxide is dispersed to reduce the graphene oxide. Here, the voltage applied to the metal wire applies energy of 1 to 5 times the energy for sublimating the metal wire. At this time, the applied pulse voltage is supplied as much as a value calculated by the following relational expression (1).

[Relational Expression 1]

Considering the size of the metal wire charged in the mixed solution, the voltage (V) is calculated and applied in consideration of the sublimation energy of the metal wire and the capacitor capacity (C) of the device by relation 1 above.

The mixed solution is obtained by dispersing graphene oxide powder in an organic solvent. The organic solvent is acetone, pyridine, methyl ethyl ketone, methyl alcohol, ethyl alcohol, isopropyl alcohol, butyl alcohol, ethylene glycol, polyethylene glycol, tetrahydrofuran, dimethylformamide, dimethylacetamide, N-methyl- Any one selected from 2-pyrrolidone, hexane, cyclohexanone, toluene, chloroform, dichlorobenzene, dimethylbenzene, trimethylbenzene, methylnaphthalene, nitromethane, acrylonitrile, octadecylamine, aniline, dimethylsulfoxide and carbon or a mixture of two or more. In some cases, the degree of reduction of graphene oxide may be controlled by selectively diluting the organic solvent using distilled water.

The metal wire has a diameter of 1 mm or less (greater than 0). The metal wire is, for example, manganese (Mn), copper (Cu), chromium (Cr), iron (Fe), nickel (Ni), cobalt (Co), gold (Au), silver (Ag) and platinum ( It may include any one or a mixture of two or more of transition metal elements such as Pt).

The method of dispersing the graphene oxide in the mixed solution is to stir and disperse the graphene oxide powder in the mixed solution using a magnetic stirrer and ultrasonic grinding. Here, the magnetic stirrer and ultrasonic pulverization are already known techniques, and a detailed description thereof will be omitted. Thereafter, the mixed solution in which graphene oxide is dispersed is filled in the chamber 80 of the electric explosive device 100 shown in FIG. 2 , and the metal wire 30 is charged.

Referring to FIG. 2 , the electric explosive device 100 includes a surplus gas outlet 10 , a high voltage electrode 20 , a metal wire 30 , a wire guide 40 , a ground electrode 50 , an ultrasonic powder dispersing device 70 ) and a chamber 80 , and a mixed solution 60 in which graphene oxide powder is dispersed in the chamber 80 is filled.

Here, at least both of the high voltage electrode 20 and the ground electrode 50 are supported in the mixed solution 60 in which the graphene oxide powder is dispersed, and the metal wire 30 is mixed at a constant speed through the wire guide 40 . It is fed into solution 60 . Thereafter, a pulsed voltage is applied using the high voltage electrode 20 in the chamber 60 filled with the mixed solution 60 to electrically explode the metal wire 30 . At the same time, the metal wire 30 is sublimed in the liquid to form a metal or metal oxide nanopowder and at the same time reduce the graphene oxide powder to form a nanopowder (S120) is performed.

The metal wire 30 is automatically and uniformly supplied with a length of about 2.4 cm by the electric explosive device 100 to connect the anode and the cathode. At this time, the magnitude of the pulse power applied to the metal wire 30 supplies energy that is 1 to 5 times greater than the sublimation energy of the charged metal wire.

In addition, as the pore defects included in the graphene oxide are healed during the reduction process by the electric explosion, the defect density inside the reduced graphene oxide is remarkably reduced. In the reduction step, the carbon source contained in the organic solvent and the energy of the metal or metal oxide nanopowder that explodes at the defect location of the graphene oxide powder reacts to heal the defects inside the graphene oxide during the reduction. It is considered to be because The reduced graphene oxide, in which the defects are healed, exhibits excellent mechanical and chemical properties as well as high electrical conductivity compared to the conventional reduced graphene oxide containing a number of defects therein.

After the step (S120) of forming the nanopowder, a step (S130) of collecting the nanocomposite powder in which the reduced graphene powder and the metal nanopowder are mixed with each other may be performed.

As shown in FIG. 5, the graphene nanocomposite powder has a complex entangled form, and a nanocomposite powder can be obtained by performing dehydration and drying treatment. The nano-composite powder can be used as an electrode material or heat dissipation material for energy storage devices such as batteries and supercapacitors, a conductive composite material for electromagnetic wave shielding, and a sensor.

Hereinafter, embodiments for helping understanding of the present invention will be described. However, the following examples are only provided to help the understanding of the present invention, and the present invention is not limited only to the following examples.

<Example 1_ Graphene/Copper Nano Composite Powder Preparation>

20 ml of a commercial graphene oxide (GO-V50) dispersion solution was mixed with 800 ml of ethanol, and stirred for 30 minutes with an ultrasonic cleaner and magnetic stirrer to prepare a mixed solution. The prepared aqueous solution was filled in the chamber 80 of the electric explosive device 100 shown in FIG. 2, and a copper (Cu) wire having a diameter of 200 μm was connected to the device. The connected copper wire is automatically fed constant by the length of 2.4 cm. After that, the copper wire was supplied with an energy pulse of about 180J when the voltage of 1456V was converted into energy by the two connected electrodes (anode and cathode), and energy 4 times greater than the sublimation energy per unit volume was instantaneously supplied, causing an explosion.

The instantaneously heated and expanded copper wire is dispersed in the liquid phase in the form of nanopowder, and meets with graphene oxide to induce a reduction reaction and a defect healing reaction. At this time, the electric explosion was repeated a thousand times to prepare a graphene/copper nanocomposite powder. Here, the amount of the nanopowder produced by one electric explosion when manufacturing the nanocomposite powder is determined by the length of the charged metal wire, and the electric explosion was repeatedly performed to prepare the nanopowder.

The copper/reduced graphene composite nano powder dispersed in the mixed solution is separated from the powder by using a centrifuge, and then washed with distilled water, washed with a centrifuge, and dried through freeze-drying copper/reduced graphene composite nano A powder was prepared.

<Example 2_Preparation of carbon-coated copper nanopowder>

No graphene oxide was used in the mixed solution, and ethanol was charged into an electric explosive device (see FIG. 2). Thereafter, the connected copper wire was automatically supplied as much as 2.4 cm in length, and an electric explosion was performed with an energy of 1456V (180J) a thousand times to prepare a carbon-coated copper nanopowder.

<Example 3_Copper and Copper Oxide Nanopowder Preparation>

Graphene oxide and ethanol were not used, and distilled water was charged in an electric explosive device (see FIG. 2). After that, the connected copper wire was automatically supplied as much as a length of 2.4 cm, and an electric explosion was performed a thousand times with an energy of 1456V (180J) to prepare pure copper nanopowder.

<Example 4_ Graphene/Nickel Nano Composite Powder Preparation>

After preparing the same mixed solution as in Experimental Example 1, it was charged in the chamber of the electric explosive device (refer to FIG. 2), and a nickel (Ni) wire having a diameter of 200 μm was connected to the device. An electric explosion was performed with an energy of 1415V (170J) to prepare a nickel/reduced graphene composite nanopowder. Except for the above-mentioned conditions, the remaining experimental variables were carried out in the same manner as in Experimental Example 1.

<Example 5_ Carbon-coated nickel nanopowder production>

In the same manner as in Example 2, ethanol was charged in an electric explosive device (see FIG. 2). After changing to a nickel wire instead of a copper wire, an electric explosion was performed with an energy of 1415V (170J) to prepare a carbon-coated nickel nanopowder. Except for the above-mentioned conditions, the remaining experimental parameters were carried out in the same manner as in Experimental Example 2.

<Example 6_Nickel and Nickel Oxide Nanopowder Preparation>

In the same manner as in Example 3, distilled water was charged in the electric explosive device (see FIG. 2). After changing to a nickel wire instead of a copper wire, an electric explosion was performed with an energy of 1415V (170J) to prepare pure nickel nanopowder. Except for the above-mentioned conditions, the remaining experimental variables were carried out in the same manner as in Experimental Example 3.

<Comparative Example 1_ Graphene Oxide>

Commercially available graphene oxide (GO-V50) was dispersed in distilled water to prepare a graphene oxide dispersion solution having a concentration of 0.5 mg/ml. By performing energy dispersive spectroscopy (EDS) of a transmission electron microscope (TEM), the oxygen content of graphene oxide through the microstructure image is shown in FIG. 3 , and the defect distribution of graphene oxide is shown in FIG. 4 .

<Evaluation of reduced graphene oxide>

Table 1 below summarizes the oxygen content of each position for each sample shown in FIG. 3 in a table. Hereinafter, GO is graphene oxide and rGO is reduced graphene oxide.

Comparative Example 1 GO (%) Experimental Example 1
rGO (%) O ₁ 11.15 0.62 O ₂ 11.25 0.28 O ₃ 10.09 0.32

Referring to FIG. 3 and Table 1, in the analysis results of graphene oxide of Comparative Example 1 sample, the oxygen ratio was measured to be 11.15% in the O ₁ region, 11.25% in the O ₂ region, and 10.09% in the O ₃ region. The reduced graphene of Experimental Example 1 had an oxygen ratio of 0.62% in the O ₁ region, 0.28% in the O ₂ region, and 0.32% oxygen content in the O ₃ region, confirming that the oxygen content dropped to 1% or less through electric explosion. could

Through the above results, it was confirmed that the electric explosion process is effective in reducing graphene oxide. It is believed that when the copper wire is instantaneously applied with energy, sublimated and exploded, and dispersed in the liquid phase as a powder with a size of several tens of nanometers, it reacts with graphene oxide in the liquid phase in a state with high thermal energy, and oxygen is removed.

Referring to FIG. 4 , it was confirmed that the graphene oxide sample of Comparative Example 1 had many defects in the form of voids. However, it can be seen that the reduced graphene of the sample of Example 1 forms a complete sheet without visible pore defects. Ethanol (C ₂ H ₅ OH) used as a dispersion is a precursor for supplying carbon, and the moment copper nanopowder formed by electric explosion meets graphene oxide, graphene is formed at the defect location of graphene oxide. Therefore, since the pore defects are cured by the graphene formed at the defect positions, it is determined that the pore type defects cannot be found in the sample of Example 1.

<Evaluation of properties of reduced graphene/metal nano composite powder>

5 is an image of (a) Example 3 metal and metal oxide nanopowders and (b) Example 1 graphene-metal nanocomposite powders analyzed with a scanning electron microscope (SEM).

Referring to FIG. 5 , it can be seen that both the metal and metal oxide powder of Example 3 and the nanocomposite powder of Example 1 have a size distribution of several tens of nanometers. In addition, in the SEM image of the graphene-metal nanocomposite powder of Example 1, it can be confirmed that graphene combined with the metal nanopowder.

6 is a result of analyzing the nanocomposite powder of Examples 1 to 6 and the graphene oxide of Comparative Example 1 by Raman spectroscopy.

6, in the Raman spectra of Examples 1 and 4, three main D peaks (1354.9 cm ^-1 ), G peaks (1580.2 cm ^-1 ), and 2D peaks (2693.3 cm ^-1 ) of graphene are All were observed. Through this, it can be confirmed that the film covering the metal nanopowder in FIG. 5 is graphene.

In the case of the copper and copper oxide nanopowders of Example 3 and the nickel and nickel oxide nanopowders of Example 6, carbon-related G peaks were not detected, and metal oxide-related peaks were detected. In the case of the carbon-coated copper nanopowder of Example 2, metal oxide-related peaks appeared, and at the same time, the D peak (1354.9 cm ^-1 ) and G peak (1580.2 cm ^-1 ) appearing in the carbon material appeared together with the fluorescence peak.

In addition, in the case of the carbon-coated nickel nanopowder of Example 5, graphene D peak (1354.9 cm ^-1 ) and G peak (1580.2 cm ^-1 ) were detected without metal oxide and fluorescence peaks. Summarizing the above results, in the case of Examples 2 and 5, a carbon layer is formed on the metal nanopowder through electric explosion, but the 2D peak signal shown by the double resonance of graphene is weak, so the crystallinity is can be seen falling.

In the case of the nanocomposite powders of Experimental Examples 1 and 4, a strong 2D peak was shown, indicating good crystallinity of graphene. This is consistent with the results of the transmission electron microscope image of FIG. 4, which confirmed that defect healing occurred in the manufacturing process of reduced graphene by electric explosion.

7 is an experimental example of the present invention, the results of analysis of the nanocomposite powder of Examples 1, 3, 4 and 6 by X-ray diffraction (XRD) method.

7, (a) In the case of Experimental Examples 1 and 3, the metal nanopowder was composed of copper oxide (Cu ₂ O) and copper (Cu). (b) In the case of Experimental Examples 4 and 6, it was confirmed that the metal nanopowder was composed of a nanopowder of nickel oxide (NiO) and nickel (Ni).

In the case of Examples 3 and 6 in which no organic solvent was used, the specific gravity of the metal oxide was relatively large. In the case of Examples 1 and 4 using the organic solvent, the specific gravity of the metal oxide decreased as the metal nanopowder was complexed with the reduced graphene. That is, it can be seen that when the composite nanopowder is prepared by the electric explosion method of the present invention, the specific gravity of the metal oxide can be controlled by controlling the mixed solution.

8 is an experimental example of the present invention, showing the results of measuring the conductivity of Examples 1 and 2 by the powder resistance measurement method, and the powder resistance measurement result was linearized with a change in conductivity according to the density of the powder (plot).

Referring to FIG. 8 , the carbon-coated copper nanopowder of Example 2 showed a conductivity value of 73.2 S/m at a density of 3.5 g/cc. On the other hand, in the case of the graphene-copper nanocomposite powder of Example 1, the conductivity value was 166.2 S/m at the same density of 3.5 g/cc.

This is an increase in conductivity by about 127%. As shown in the image shown in the structure of the nanocomposite powder in FIG. 5, reduced graphene connects the gaps between the copper nanopowders to create a path for the current to flow while lowering the resistance to increase the conductivity. considered to be improved.

On the other hand, Example 3 is copper and copper oxide nanopowder, and since it contains copper oxide, the resistance is high, and the conductivity was not measured by the powder resistance measurement method.

Figure 9 is an experimental example of the present invention, using the nanocomposite powder of Examples 1 and 4 is a result of analyzing the electromagnetic wave shielding properties. In the electromagnetic wave shielding characteristic analysis method, the electromagnetic wave shielding rate was measured in the high frequency region (X band) of 8 GHz to 12 GHz after the powder of each sample was compressed into a disk shape having a diameter of 3 cm and a thickness of 1000 mm. As a result, the graphene-nickel nanocomposite powder of Example 4 showed an average shielding efficiency of 83.1 dB.

As described above, the method for producing a graphene nanocomposite powder according to an embodiment of the present invention can prepare a graphene nanocomposite powder that is healed to 95% or more in a single process simply by using an underwater electric explosive device. By reducing the process steps of graphene nanocomposite powder compared to the prior art, it is possible to save process cost and time. In addition, by implementing reduced graphene in which most of the defects are healed compared to the prior art, the conductivity is improved significantly compared to the metal nanopowder, so that it can be applied as a conductive filling material.

Although the present invention has been described with reference to the embodiment shown in the drawings, which is merely exemplary, it will be understood by those skilled in the art that various modifications and equivalent other embodiments are possible therefrom. Therefore, the true technical protection scope of the present invention should be determined by the technical spirit of the appended claims.

10: surplus gas outlet
20: high voltage electrode
30: conductive wire (explosive part)
40: wire guide
50: ground electrode
60: mixed solution in which graphene oxide powder is dispersed
70: ultrasonic powder dispersing device
80: chamber
100: electric explosive device

Claims (11)

charging a metal wire into a mixed solution in which graphene oxide is dispersed; and
The metal powder formed by applying energy to the metal wire loaded in the mixed solution to electrically explode the metal wire and the graphene oxide react with each other to form a nanopowder containing a metal or a metal oxide; including; do,
The step of forming the nanopowder,
forming a reduced graphene oxide in which the reduction and defect healing of the graphene oxide is made due to the exploding metal wire; and forming a composite structure by combining the nanopowder with the metal or metal oxide and the reduced graphene oxide.
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
The composite structure is
The reduced graphene oxide in the form of a thin film is bonded between the nanoparticles so that the nanopowder has a structure surrounding the reduced graphene oxide,
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
The nanopowder has a size of 100 nm or less (greater than 0),
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
The step of forming the nanopowder,
Including the step of applying a voltage pulse equal to or greater than the energy required for sublimation of the metal wire in consideration of the size of the metal wire charged in the mixed solution,
Method for manufacturing graphene nanocomposite powder. 5. The method of claim 4,
The voltage pulse is a voltage (V) calculated in consideration of the sublimation energy of the metal wire and the capacitor capacity (C) of the device,
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
The mixed solution is mixed using a stirrer after dispersing the graphene oxide in an organic solvent, optionally further containing distilled water,
Method for manufacturing graphene nanocomposite powder. 7. The method of claim 6,
The organic solvent is acetone, pyridine, methyl ethyl ketone, methyl alcohol, ethyl alcohol, isopropyl alcohol, butyl alcohol, ethylene glycol, polyethylene glycol, tetrahydrofuran, dimethylformamide, dimethylacetamide, N-methyl- Any one or two selected from 2-pyrrolidone, hexane, cyclohexanone, toluene, chloroform, dichlorobenzene, dimethylbenzene, trimethylbenzene, methylnaphthalene, nitromethane, acrylonitrile, octadecylamine, aniline and dimethylsulfoxide containing a mixture of more than one,
A method for producing graphene nanocomposite powder. The method of claim 1,
The reduced graphene oxide has an oxygen content of 5% or less (greater than 0),
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
In the reduced graphene oxide, graphene grows in the region where the pore defects of the graphene oxide exist, and 95% or more of the pore defects are healed,
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
The metal wire has a diameter of 1 mm or less (more than 0), and the length of the metal wire has a length of 10 cm or less (more than 0),
Method for manufacturing graphene nanocomposite powder. The method of claim 1,
The metal wire includes manganese (Mn), copper (Cu), chromium (Cr), iron (Fe), nickel (Ni), cobalt (Co), gold (Au), silver (Ag) and platinum (Pt). Including any one or a mixture of two or more of the transition metal elements,
Method for manufacturing graphene nanocomposite powder.

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