KR101797145B1 - Manufacturing method for reduced graphene oxides - Google Patents

Manufacturing method for reduced graphene oxides Download PDF

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KR101797145B1
KR101797145B1 KR1020150153559A KR20150153559A KR101797145B1 KR 101797145 B1 KR101797145 B1 KR 101797145B1 KR 1020150153559 A KR1020150153559 A KR 1020150153559A KR 20150153559 A KR20150153559 A KR 20150153559A KR 101797145 B1 KR101797145 B1 KR 101797145B1
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South Korea
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graphene
aqueous solution
reduced
oxidized graphene
present
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KR1020150153559A
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Korean (ko)
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KR20170051896A (en
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박진홍
유광위
박형열
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성균관대학교산학협력단
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/21—After-treatment
    • C01B32/23—Oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F1/00—Methods of preparing compounds of the metals beryllium, magnesium, aluminium, calcium, strontium, barium, radium, thorium, or the rare earths, in general
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides

Abstract

The present invention relates to a method for producing reduced oxidized graphene, and a method for producing reduced oxidized graphene according to an embodiment of the present invention includes mixing photoresist particles in an aqueous solution of oxidized graphene; And exposing light corresponding to the absorption wavelength of the photosensitive particles contained in the aqueous solution to reduce the oxidized graphene.

Description

TECHNICAL FIELD [0001] The present invention relates to a method for producing reduced oxidized graphene,

The present invention relates to a method for producing reduced oxidized graphene.

Graphene has very good strength and conductivity, and is made of honeycomb lattice with a thickness of one atom. Such graphene has been applied in various fields such as transistors, transparent electrodes, energy storage materials, sensors, and polymer complexes. However, pure graphene, unlike semiconductors such as silicon, has a zero band gap and is therefore not suitable for digital circuits used in most of the integrated circuits.

In order to overcome the above-mentioned problems and to impart more performance to graphene, researches on chemically modifying graphene have been actively conducted. Among them, the reduced graphene graphene is a high quality graphene material close to graphene, showing its applicability to various fields due to its unique chemical properties.

Generally, reduced graphene graphene is produced through reduction of oxidized graphene, and a method of reducing graphene oxide by using a reducing agent or reducing at high temperature is used. At this time, the reducing agent of the oxidized graphene generally has a strong toxicity such as hydrazine (N 2 H 4), sodium hydroxide (NaOH), potassium hydroxide (KOH), and hydrogen iodide Materials are being used. Further, since the method of reducing the graphene oxide at a high temperature is performed at a high temperature of 200 ° C or more, the use of a substrate having a high flexibility is limited, and energy consumption is a problem.

Korean Patent Laid-Open No. 10-2014-0093930 (entitled Reduced Oxidized Graft Pine and Method for Producing the Same) discloses a method of providing graphene oxide, applying a reducing agent to at least a portion of the graphene oxide, Discloses a method for producing graphene oxide.

Some embodiments of the present invention seek to provide a process for producing reduced oxidized graphene that is environmentally friendly and capable of a low temperature process.

It should be understood, however, that the technical scope of the present invention is not limited to the above-described technical problems, and other technical problems may exist.

According to an aspect of the present invention, there is provided a method of preparing reduced oxidized graphene, comprising: mixing photosensitive grains in an aqueous solution of graphene oxide; And exposing light corresponding to the absorption wavelength of the photosensitive particles contained in the aqueous solution to reduce the oxidized graphene.

According to the above-mentioned problem solving means of the present invention, in the case of the example proposed in the present invention, it is possible to produce an environmentally-friendly reduced graphene oxide.

In addition, it is possible to produce reduced graphene grains on a substrate having a high flexibility since a low temperature process is possible.

FIG. 1 is a flowchart illustrating a method for manufacturing reduced oxidized graphene according to an embodiment of the present invention. Referring to FIG.
2 schematically illustrates a method for producing reduced oxidized graphene according to an embodiment of the present invention.
3 is a graph showing the results of absorption spectra of reduced oxidized graphene prepared according to an embodiment of the present invention.
4 is a graph showing the results of infrared absorption spectroscopic analysis of reduced oxidized graphene prepared according to an embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.

Throughout the specification, when a part is referred to as being "connected" to another part, it includes not only "directly connected" but also "electrically connected" with another part in between . Also, when an element is referred to as "comprising ", it means that it can include other elements as well, without departing from the other elements unless specifically stated otherwise.

Hereinafter, a method for manufacturing reduced oxidized graphene according to an embodiment of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a flowchart illustrating a method for manufacturing reduced oxidized graphene according to an embodiment of the present invention. Referring to FIG.

2 schematically illustrates a method for producing reduced oxidized graphene according to an embodiment of the present invention.

Referring to FIG. 1, a method for preparing reduced oxidized graphene according to an embodiment of the present invention comprises: mixing photoreceptive particles in an aqueous solution of oxidized graphene (S110); Reducing the graphene oxide contained in the aqueous solution (S120), and drying the aqueous solution containing the reduced oxidized graphene (S130).

Referring to FIGS. 1 and 2, a method of producing reduced oxidized graphene 200 according to an embodiment of the present invention includes the steps of mixing oxidized graphene A pin aqueous solution 100 may be prepared. At this time, the oxidized graphene aqueous solution 100 can be obtained by a well-known method such as a modified hummers method. For example, an aqueous solution of oxidized graphene can be obtained by mixing graphite with an oxidizing agent containing (100) sulfuric acid or nitric acid.

First, the photosensitive particles 50 are mixed with the prepared aqueous solution 100 of graphene oxide. Here, the photosensitive particles 50 are substances sensitive to light and can absorb photons and transfer electrons. Specifically, the photosensitive particles 50 decompose water molecules present in the aqueous solution by a photocatalytic reaction, and simultaneously absorb photons of light to emit electrons. Therefore, the electrons emitted from the photosensitive particles 50 cause the reduction of the oxidized graphene. The photosensitive particles 50 may include, but not limited to, one or more of, for example, a lanthanide ion, a divalent metal ion, a metal nanoparticle, a titanium oxide nanoparticle, or a zinc peroxide nanoparticle. The concentration of the photoconductive particles 50 mixed in the aqueous solution 100 may be approximately 0.01 mM / L to 1 M / L, but may be varied depending on the degree of reduction of the oxidized graphene. .

Next, in the step of reducing the graphene oxide contained in the aqueous solution (S120), the graphene oxide aqueous solution 150 mixed with the photosensitive particles can be exposed for about several seconds to several minutes in the light of the intensity of 0.1 mW to 10 mW . Thus, the graphene oxide contained in the aqueous solution can be reduced. At this time, the light used for exposure is light having a wavelength corresponding to the absorption wavelength of the photosensitive particles, and may be any one of ultraviolet rays, visible rays, and infrared rays, and is not limited to a specific wavelength band. That is, the wavelength and intensity of the light to be exposed may be varied in the concentration of the photosensitive particles, the kind thereof, and the process of designing the process, and are not limited to any one.

Finally, the aqueous solution 150 containing reduced oxidized graphene can be dried. At this time, the drying method may be any one of a near-infrared heating method, an infrared heating method, a room temperature drying method, and a drying oven heating method, but is not limited thereto.

On the other hand, in the step of drying the aqueous solution containing the graphene oxide (S130), the reduced graphene graphene is formed in a thin film form by coating the substrate or the flexible substrate with an aqueous solution of the graphene oxide (150) . Alternatively, it is also possible to produce a desired shape using a mold. In other words, the reduced oxidized graphene can be designed and manufactured in various shapes depending on the use, and is not limited to any one shape.

10 mT / L of terbium (Tb) ion, a kind of lanthanide ion, was mixed with an aqueous solution of oxidized graphene and then exposed for 5 minutes using light of 520 nm, 655 nm, and 785 nm, respectively. At this time, the intensity of the exposed light is 1 mW.

Then, the absorption spectrum was measured using ultraviolet rays, visible rays, and infrared rays to confirm changes in absorption spectra before and after the reduction of the reduced graphene graphene.

3 is a graph showing the results of absorption spectra of reduced oxidized graphene prepared according to an embodiment of the present invention.

Referring to FIG. 3, it was confirmed that the absorption spectrum of the visible and infrared regions was increased in the aqueous solution of graphene oxide mixed with the photosensitive particles exposed to light of 520 nm in the absorption wavelength band of Tb ions. This is due to the recovery of the CC bond due to the formation of the oxidized graphene graphene oxide graphene, and it can be confirmed that the graphene oxide is reduced by the light of the absorption wavelength band of the mixed photosensitive particles and the exposed Tb ion .

4 is a graph showing the results of infrared absorption spectroscopic analysis of reduced oxidized graphene prepared according to an embodiment of the present invention.

Infrared absorption spectroscopy was performed to analyze the change in the redox composition of the oxidized graphene. As shown in FIG. 4, when the absorbance around 1050 cm-1 indicating CO bonding was observed, a relatively low signal was detected at 405 nm, 520 nm, and 655 nm near the absorption wavelength band of Tb ion, It can be confirmed that it is detected. In other words, it can be seen that there is a difference in the degree of reduction of the graphene oxide depending on the type of the mixed photosensitive particles and the light to be exposed.

As described above, the reduced graphene graphene fabrication method according to an embodiment of the present invention is a method of manufacturing reduced graphene grains by mixing photoresist grains into an oxidized graphene aqueous solution and exposing light in the absorption wavelength band of the photoresist grains, It is possible to produce graphene oxide. In addition, it is possible to manufacture reduced graphene grains on a substrate having a high flexibility since a low temperature process is possible.

It will be understood by those skilled in the art that the foregoing description of the present invention is for illustrative purposes only and that those of ordinary skill in the art can readily understand that various changes and modifications may be made without departing from the spirit or essential characteristics of the present invention. will be. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.

The scope of the present invention is defined by the appended claims rather than the detailed description and all changes or modifications derived from the meaning and scope of the claims and their equivalents are to be construed as being included within the scope of the present invention do.

50: Photosensitive particles
100: aqueous solution of graphene oxide
150: An aqueous solution of graphene oxide containing photosensitive particles
200: reduced oxidized graphene

Claims (6)

In the method for producing reduced oxidized graphene,
Mixing photosensitive grains with an aqueous solution of graphene oxide; And
And exposing light corresponding to the absorption wavelength of the photosensitive particles contained in the aqueous solution to reduce the oxidized graphene,
Wherein the graphene oxide aqueous solution comprises any one of lanthanide ions, divalent metal ions, metal nanoparticles, and zinc peroxide nanoparticles as the photosensitive particles. The method according to claim 1,
And drying the aqueous solution containing the reduced oxidized graphene to produce reduced oxidized graphene.
Wherein the reduced graphene graphene is produced. 3. The method of claim 2,
The step of producing the reduced oxidized graphene
Further comprising the step of coating an aqueous solution containing the reduced graphene oxide on a substrate. delete delete delete
KR1020150153559A 2015-11-03 2015-11-03 Manufacturing method for reduced graphene oxides KR101797145B1 (en)

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CN115738950A (en) * 2022-12-14 2023-03-07 中国科学技术大学 Micro-fluidic-based graphene continuous preparation and assembly micro-system and application

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010248066A (en) 2009-04-16 2010-11-04 Northrop Grumman Systems Corp Graphene oxide deoxygenation
JP2013151398A (en) 2012-01-26 2013-08-08 Dowa Electronics Materials Co Ltd Method for reducing graphene oxide, and method for producing electrode material using the method
US20140054490A1 (en) 2012-08-25 2014-02-27 Indian Institute Of Technology Madras Graphene composites with dispersed metal or metal oxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010248066A (en) 2009-04-16 2010-11-04 Northrop Grumman Systems Corp Graphene oxide deoxygenation
JP2013151398A (en) 2012-01-26 2013-08-08 Dowa Electronics Materials Co Ltd Method for reducing graphene oxide, and method for producing electrode material using the method
US20140054490A1 (en) 2012-08-25 2014-02-27 Indian Institute Of Technology Madras Graphene composites with dispersed metal or metal oxide

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