KR101798301B1 - Method of graphene oxide film - Google Patents
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- KR101798301B1 KR101798301B1 KR1020150186068A KR20150186068A KR101798301B1 KR 101798301 B1 KR101798301 B1 KR 101798301B1 KR 1020150186068 A KR1020150186068 A KR 1020150186068A KR 20150186068 A KR20150186068 A KR 20150186068A KR 101798301 B1 KR101798301 B1 KR 101798301B1
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims description 22
- 238000001035 drying Methods 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims description 71
- 230000037303 wrinkles Effects 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000010408 film Substances 0.000 description 42
- 230000003287 optical effect Effects 0.000 description 6
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000037373 wrinkle formation Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
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- 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
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/123—Ultraviolet light
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
- H01L29/1606—Graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- General Health & Medical Sciences (AREA)
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Abstract
The present invention relates to a method for producing a graphene oxide film having a uniform pattern, comprising the steps of forming a graphene oxide solution by dispersing graphene oxide in a solvent, drying the graphene oxide solution at a predetermined temperature, To form a corrugation of the direction.
Description
The present invention relates to a method for producing a graphene oxide film, and more particularly to a graphene oxide film having wrinkles formed in the process of drying a graphene oxide solution.
Graphene has a structure in which hexagonal carbon bonds are repeated, and has almost two-dimensional structure, so that it has unique and excellent properties that other materials can not have. Graphene Oxide (Graphene Oxide) is a substance which is oxidized by bonding COOH or OH group to graphene. Recently, various studies have been carried out on its own properties. Recently, one of several studies on graphene oxide relates to a method of easily producing graphene by reducing graphene oxide.
Graphene can be easily dispersed in non-toxic solvents such as water, and can achieve electrical characteristics similar to graphene without using expensive equipment such as CVD processes.
In this way, studies that improve electrical properties by reduction with graphene oxide are summarized in Carbon 50 (2012) 3210-3228, The reduction of graphene oxide ".
Apart from various reduction methods, a method is known in which paper is formed after various structures are formed using a two-dimensional structure of graphene oxide or the like. However, this method is mainly used to macroscopically form a two-dimensional structure of graphene oxide, and it is difficult to say that a device using two-dimensional characteristics of graphene oxide has been developed which is more microscopic.
On the other hand, it is known that graphene oxide has a liquid crystal phase recently when it is dispersed in a solvent. In this connection, it is known that graphene oxide particles can be effectively aligned or the density distribution can be changed by various external factors on the liquid crystal of graphene oxide.
The use of a liquid crystal phase is a technique that can be directly applied in various fields such as an optical element, but it is disadvantageous in that it is difficult to use it directly because of the existence of a solvent having a charge for use as an electric element.
An object of the present invention is to produce a graphene oxide film having optical anisotropy.
An object of the present invention is to produce a graphene oxide film having high durability.
An object of the present invention is to manufacture an electric device capable of adjusting electric conductivity.
The method for preparing a graphene oxide film according to an embodiment of the present invention includes the steps of: (a) preparing a graphene oxide solution by dispersing graphene oxide in a solvent; And (b) drying the graphene oxide solution at a predetermined temperature to form wrinkles in a predetermined direction.
In addition, the step (b) may include: providing a substrate; applying the graphene oxide solution on the substrate; And moving the graphene oxide solution applied on the substrate through the blade at a constant speed to dry the graphene oxide solution in a film form.
The drying temperature may be 20 to 100 ° C.
The moving speed of the graphene oxide solution may be 0.0001-0.1 mm / s.
In addition, the refractive index of the graphene oxide film may vary depending on the direction of the corrugation.
In addition, (b) may include disposing a first substrate having a first temperature at a first position and a second substrate having a second temperature lower than the first temperature at a third position; Raising a third substrate over the first substrate and the second substrate; Applying the graphene oxide solution onto the third substrate; And moving the third substrate in a predetermined direction.
In addition, the third substrate may move toward the first substrate from the second substrate.
A method of manufacturing an electric device according to an embodiment of the present invention includes the steps of: (a) dispersing graphene oxide in a solvent to prepare a graphene oxide solution; (b) providing a substrate; (c) applying the graphene oxide solution onto the substrate; And (d) pushing and moving the graphene oxide solution applied on the substrate through the blade at a predetermined drying rate at a constant speed to dry the graphene oxide solution in the form of a film to form a graphene oxide film having wrinkles ; And (e) reducing the graphene oxide film.
In addition, the electric conductivity of the electric device can be controlled by adjusting at least one of the drying temperature and the graphene oxide moving speed.
In the step (e), the graphene oxide film may be irradiated with ultraviolet rays.
A method of manufacturing an electric device according to another embodiment of the present invention includes the steps of: (a) dispersing graphene oxide in a solvent to prepare a graphene oxide solution; (b) disposing a first substrate having a first temperature at a first location and a second substrate having a second temperature below the first location at a second location; (c) raising a third substrate above the first substrate and the second substrate; (d) applying the graphene oxide solution onto the third substrate; And (e) moving the third substrate in a predetermined direction to dry the graphene oxide solution in a film form to form a wrinkled graphene oxide film; (f) reducing the graphene oxide film.
The predetermined direction may be the first substrate side of the second substrate.
The present invention has the advantage of being able to produce a graphene oxide film having improved durability.
Further, the present invention is advantageous in that a graphene oxide film having optical anisotropy according to the wrinkle direction can be produced.
In addition, the present invention has an advantage in that an electric device capable of controlling the electric conductivity by controlling the wrinkle direction can be produced.
1 is a method for producing a graphene oxide film according to a first embodiment of the present invention.
2 is a wrinkle formed on the graphene oxide film produced by the first embodiment of the present invention.
Figure 3 summarizes the pleats formed on the graphene oxide film produced by the first embodiment of the present invention.
4 is a graph showing the electrical conductivity obtained by reducing the graphene oxide film produced by the first embodiment of the present invention.
5 is a method for producing a graphene oxide film according to a second embodiment of the present invention.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail.
It should be understood, however, that the invention is not intended to be limited to the particular embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
The terms first, second, etc. may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another. For example, without departing from the scope of the present invention, the first component may be referred to as a second component, and similarly, the second component may also be referred to as a first component. And / or < / RTI > includes any combination of a plurality of related listed items or any of a plurality of related listed items.
It is to be understood that when an element is referred to as being "connected" or "connected" to another element, it may be directly connected or connected to the other element, . On the other hand, when an element is referred to as being "directly connected" or "directly connected" to another element, it should be understood that there are no other elements in between.
The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In the present application, the terms "comprises" or "having" and the like are used to specify that there is a feature, a number, a step, an operation, an element, a component or a combination thereof described in the specification, But do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or combinations thereof.
Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the relevant art and are to be interpreted in an ideal or overly formal sense unless explicitly defined in the present application Do not.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In order to facilitate the understanding of the present invention, the same reference numerals are used for the same constituent elements in the drawings and redundant explanations for the same constituent elements are omitted.
The present invention utilizes that a spontaneous structure is formed in the process of drying graphene oxide solution. Here, the graphene oxide solution can be obtained by dispersing graphene oxide in a solvent.
The graphene oxide solution is wrinkled in a predetermined direction on the surface while being dried, or agglomerated at regular intervals. In the present invention, what is gathered at a constant interval is called a thickness modulation.
Among them, the present invention relates to a method for producing a graphene oxide film by using a phenomenon that graphen oxide is formed and wrinkled in a predetermined direction.
1 is a process for producing a graphene oxide film according to a first embodiment of the present invention. According to the first embodiment of the present invention,
Hereinafter, the rate at which the
According to the first embodiment of the present invention, the drying temperature of the
Here, if the drying temperature is lower than 20 ° C, drying may not proceed well, or if the drying temperature exceeds 100 ° C, evaporation of water may occur rapidly and wrinkles may not be formed well.
According to the first embodiment of the present invention, the
The graphene oxide film having wrinkles manufactured through the first embodiment of the present invention can be used as an optical film.
According to the first embodiment of the present invention, the
FIGS. 2 and 3 show the corrugation and thickness modulation formed on the graphene oxide film formed according to the first embodiment of the present invention.
FIG. 2 shows wrinkle formation and thickness modulation by changing the dragging speed v from 0.008 mm / s to 0.1 mm / s at different drying temperatures (55 ° C., 80 ° C. and 95 ° C.) Figure 3 summarizes the observation results of Figure 2.
Referring to FIGS. 2 and 3, the graphene oxide film produced according to the first embodiment of the present invention exhibits a wrinkle direction different depending on a dragging speed (v) and a drying temperature in a drying process, (Thickness Modulation).
3, wrinkles are formed in the graphene oxide film in a direction perpendicular to the moving direction of the
Referring to FIG. 3, the wrinkles formed on the graphene oxide film according to an embodiment of the present invention can control the wrinkle direction according to the drying temperature and the dragging speed v, and when applied to an optical device, There is an advantage that an optical element capable of controlling the refractive index can be manufactured.
4 is a graph of electrical conductivity of a graphene oxide film produced according to the first embodiment of the present invention. Here, the graphene oxide film was produced at a drying temperature of 55 ° C and a dragging speed v of 0.008 mm / s, 0.017 mm / s, 0.033 mm / s, 0.067 mm / s and 0.1 mm / s.
FIG. 4 (a) is a graph showing the electrical conductivity when the graphene oxide film is not reduced, and FIG. 4 (b) is a graph showing the electrical conductivity after reducing graphene oxide. Here, a method of reducing graphene oxide film is a method of irradiating graphene oxide film with ultra violet.
Referring to FIG. 4, the graphene oxide film (a) having no ultraviolet rays but having no electric conductivity has a different electric conductivity depending on the dragging speed (v) .
In FIG. 4, the electric conductivity is obtained by measuring the electric conductivity in the vertical (⊥) direction and the horizontal (∥) direction according to the dragging speed (v), respectively, and normalizing the difference between the electric conductivity in the horizontal direction and the electric conductivity in the horizontal direction.
Referring to the results of FIG. 4, when the dragging speed v is low, the electrical conductivity in the horizontal direction is large. In addition, it can be seen that as the dragging speed (v) becomes lower, the electric conductivity decreases, but the difference in the electric conductivity with the difference in the moving speed decreases gradually. Therefore, it can be seen that it is possible to manufacture an electric device capable of maximizing the difference in electric conductivity between the horizontal direction and the vertical direction when the dragging speed v is appropriately adjusted.
FIG. 5 illustrates a method of manufacturing a graphene oxide film according to a second embodiment of the present invention.
According to the second embodiment of the present invention, the
Thereafter, the
For example, as shown in FIG. 5, the
Figures 2 to 4 show the dynamic low, optical, and electrical anisotropic behavior of graphene oxide films. Referring to FIG. 2, it can be seen that the X-axis and Y-axis directions have different degree of wrinkle formation. Therefore, a birefringence phenomenon occurs in which the refractive index differs depending on the direction. In addition, the electrical conductivity also varies with direction.
Claims (12)
(b) drying the graphene oxide solution at a predetermined temperature to form wrinkles in a predetermined direction,
Wherein the refractive index of the graphene oxide film is different depending on the direction of the corrugation.
Providing a substrate;
Applying the graphene oxide solution onto the substrate; And
And pushing and moving the graphene oxide solution applied on the substrate through the blade at a constant speed to dry the graphene oxide solution in the form of a film.
Wherein the drying temperature is 20 to 100 ° C.
Disposing a first substrate having a first temperature at a first position and a second substrate having a second temperature lower than the first temperature at a third position;
Raising a third substrate over the first substrate and the second substrate;
Applying the graphene oxide solution onto the third substrate; And
And moving the third substrate in a predetermined direction.
(b) providing a substrate;
(c) applying the graphene oxide solution onto the substrate; And
(d) pushing and moving the graphene oxide solution applied on the substrate through the blade at a predetermined rate at a constant speed to dry the graphene oxide solution in the form of a film to form a graphene oxide film having wrinkles step; And
(e) reducing the graphene oxide film.
(b) disposing a first substrate having a first temperature at a first position and a second substrate having a second temperature lower than the first temperature at a second position;
(c) raising a third substrate above the first substrate and the second substrate;
(d) applying the graphene oxide solution onto the third substrate; And
(e) moving the third substrate in a predetermined direction to dry the graphene oxide solution in a film form to form a graphene oxide film having wrinkles;
(f) reducing the graphene oxide film.
Wherein the predetermined direction is the first substrate side in the second substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150186068A KR101798301B1 (en) | 2015-12-24 | 2015-12-24 | Method of graphene oxide film |
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| KR1020150186068A KR101798301B1 (en) | 2015-12-24 | 2015-12-24 | Method of graphene oxide film |
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| KR20170076156A KR20170076156A (en) | 2017-07-04 |
| KR101798301B1 true KR101798301B1 (en) | 2017-11-15 |
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| KR1020150186068A KR101798301B1 (en) | 2015-12-24 | 2015-12-24 | Method of graphene oxide film |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358197B (en) * | 2018-02-12 | 2020-04-14 | 杭州高烯科技有限公司 | Preparation method and application of highly-folded graphene oxide film |
| KR102309500B1 (en) * | 2019-11-26 | 2021-10-06 | (주)에버켐텍 | Debonding Layer and Method for Manufacturing the Same, Information Display Element and Method for Manufacturing the Same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140331920A1 (en) | 2011-09-23 | 2014-11-13 | Chung-Ang University Industry-Academy Cooperation Foundation | Production device for a graphene thin film |
| WO2015112122A1 (en) | 2014-01-21 | 2015-07-30 | Empire Technology Development Llc | Graphene membranes and methods for making and using the same |
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- 2015-12-24 KR KR1020150186068A patent/KR101798301B1/en active IP Right Grant
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140331920A1 (en) | 2011-09-23 | 2014-11-13 | Chung-Ang University Industry-Academy Cooperation Foundation | Production device for a graphene thin film |
| WO2015112122A1 (en) | 2014-01-21 | 2015-07-30 | Empire Technology Development Llc | Graphene membranes and methods for making and using the same |
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