KR20160107030A - Method for manufacturing graphene and grphene using the methode - Google Patents
Method for manufacturing graphene and grphene using the methode Download PDFInfo
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- KR20160107030A KR20160107030A KR1020150029939A KR20150029939A KR20160107030A KR 20160107030 A KR20160107030 A KR 20160107030A KR 1020150029939 A KR1020150029939 A KR 1020150029939A KR 20150029939 A KR20150029939 A KR 20150029939A KR 20160107030 A KR20160107030 A KR 20160107030A
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- C01B32/15—Nano-sized carbon materials
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Abstract
Description
The present invention relates to a method for producing graphene and to a graphene of a thin film thus produced.
A graphene is a carbon crystal having carbon atoms in a hexagonal honeycomb shape and having a two-dimensional sheet shape, and a plurality of graphene sheets are laminated to form a graphite. Thus, when graphene is exfoliated, it is possible to obtain a sheet-like graphene having one or more layers. Graphene is a material having both metallic and non-metallic properties. It has good electrical conductivity and thermal conductivity as the nature of the metal, and has high thermal stability and chemical inertness as a non-metallic property. Graphene can be applied to various applications such as electric devices, batteries, fuel cells, refractory materials and the like.
Such graphene can be produced by a method such as mechanical exfoliation, epitaxial growth, chemical vapor deposition, graphite oxidation and reduction, graphite intercalation compound, . ≪ / RTI >
The mechanical stripping method can produce high quality graphene by a simple manufacturing process, but the very low yield of the graphene produced and the size of the uneven graphene sheet are not suitable for commercial application.
The graphite oxidation and reduction method is a method of producing graphite oxide by oxidizing graphite with strong acid, then intercalating and separating it in water, and reducing it again to produce graphene. As a result, oxygen atoms can not be completely removed during reduction, There are disadvantages.
Graphene produced by epitaxial and chemical vapor deposition can synthesize graphene sheets which are superior in terms of mechanical, thermal and electrical properties as compared with graphite intercalation compounds produced by extreme oxidation and reduction processes of graphite, High manufacturing costs and low yields due to high temperature processes remain a challenge.
In recent years, graphene has been produced through an intercalation compound of graphite using potassium metal directly. However, when potassium metal is directly used, the metal is expensive and has a high reactivity in air, which is a risk of manufacturing.
To overcome these problems, Korean Patent Publication No. 2011-0106625 proposes a method of producing graphene using an alkali metal salt or an alkaline earth metal salt rather than potassium metal.
It is an object of the present invention to provide a method for effectively expanding each layer of expandable graphite to produce a thin film of graphene.
An object of the present invention is to provide a process for producing graphene which is excellent in process efficiency.
It is another object of the present invention to provide a thin film graphene produced according to the method for producing graphene.
CLAIMS 1. A process for preparing a mixture comprising mixing at least one stripper selected from the group consisting of expandable graphite, cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium dodecylbenzenesulfonate (SDBS) step;
Heating the mixed liquid containing the expandable graphite to 400 to 500 ° C to obtain hydrothermal expanded graphite; And
Applying a shear force to the hydrothermally expanded graphite mixed solution obtained by mixing the hydrothermally expanded graphite with a dispersion medium and a dispersant.
2. The method for producing graphene according to 1 above, wherein said releasing agent is contained in an amount of 50 to 120 parts by weight based on 100 parts by weight of expandable graphite.
3. The process for producing graphene according to 1 above, wherein the water is contained in an amount of 2000 to 6500 parts by weight based on 100 parts by weight of expandable graphite.
4. The method of producing graphene according to 1 above, wherein the step of obtaining the hydrothermally expanded graphite is performed by raising the mixed solution containing the expandable graphite to a temperature of 5 to 20 占 폚 / min.
5. The method of producing graphene according to item 1 above, wherein the heating step is performed for 30 to 90 minutes.
6. The process for producing graphene according to item 1, wherein the apparent density of the hydrothermally expanded graphite is 0.01 to 0.1 g / mm 3 .
7. The method of claim 1, wherein in the step of applying a shear force to the hydrothermally expanded graphite mixture liquid, the dispersion medium comprises at least one selected from the group consisting of water, an alcohol solvent, dimethylsulfoxide (DMSO) and dimethylformamide In graphene.
8. The method according to 1 above, wherein in the step of applying a shear force to the hydrothermally expanded graphite mixture, the dispersant is composed of cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium dodecylbenzenesulfonate Lt; / RTI > wherein at least one group selected from the group consisting of < RTI ID = 0.0 >
9. The method of producing graphene according to claim 1, wherein the step of applying the shear force to the hydrothermally expanded graphite mixed solution is performed by dispersing the mixture in a high pressure disperser having a pressure of 700 to 200 bar with a nozzle of 50 to 300 mu m.
10. The method of producing graphene according to item 1 above, wherein the step of applying a shear force to the hydrothermally expanded graphite mixed solution is performed by dispersing the bead mill at a speed of 1800 to 2800 rpm.
11. The method for producing graphene according to claim 1, further comprising heating and drying at 100 to 300 DEG C after adding said shearing force.
12. A graphene made according to any one of claims 1 to 11 having a thickness of 0.3 to 5 nm.
The method of manufacturing graphene according to the present invention can effectively expand each layer of expansive graphite through hydrothermal expansion to produce a thin film of graphene.
In the method for producing graphene according to the present invention, by using a specific stripping agent, an intercalation reaction can be effectively performed simultaneously with hydrothermal swelling, so that a graphene of a thin film can be produced.
The process for producing graphene according to the present invention has a mild process condition and excellent process efficiency.
Further, the graphene produced according to the present invention is a thin film structure, and it is easy to apply to an electronic device requiring a thin coating layer using the same.
BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is an exploded perspective view of an expandable graphite used in the present invention. Fig.
2 is an SEM image of hydrothermally expanded graphite produced according to the present invention.
3 shows an SEM image of the heat expandable graphite produced according to Comparative Example 1. Fig.
Fig. 4 schematically shows an AFM image of graphene prepared according to Example 1. Fig.
Fig. 5 shows an AFM image of graphene prepared according to Comparative Example 1. Fig.
6 is a graph showing a change in thickness of graphene produced according to Example 1. Fig.
FIG. 7 is a graph showing a change in thickness of graphene produced according to Comparative Example 1. FIG.
The present invention relates to a method for producing graphene and a graphene produced thereby, and more particularly, to an expandable graphite, cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium Dodecylbenzene sulfonate (SDBS), and water; Heating the mixed liquid containing the expandable graphite to 400 to 500 ° C to obtain hydrothermal expanded graphite; And applying a shear force to the hydrothermally expanded graphite mixed solution obtained by mixing the dispersion medium and the dispersant with the hydrothermally expanded graphite, thereby allowing the hydrothermal expansion and the intercalation reaction to proceed at the same time, effectively expanding each layer of the expandable graphite, Of graphene.
In the present invention, " expandable graphite " refers to a structure before expansion as graphite capable of expanding between the respective layers, and " hydrothermal expanded graphite " means that the expandable graphite is subjected to hydrothermal expansion reaction And graphite in the state where each layer is expanded through the graphite layer.
Expandable graphite is a layered structure. When each layer is exfoliated, it is possible to obtain a graphene sheet in the form of a single layer or multiple layers. Graphene is a material having both metallic and non-metallic properties. It has good electrical conductivity and thermal conductivity as a metal property. It has high thermal stability and chemical inertness as a non-metallic property. . On the other hand, it is important to fabricate graphene with a thin film structure in accordance with recent weight reduction and thinning of electronic devices. For this purpose, it is most important to effectively expand each layer of expandable graphite.
Hereinafter, an embodiment of the present invention will be described in more detail.
First, at least one stripper and water selected from the group consisting of expandable graphite, cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium dodecylbenzene sulfonate (SDBS) are mixed .
Water is a component for effectively expanding the expandable graphite. It dissolves the releasing agents CTAB, TBAOH, and SDBS to help them intercalate between the layers of the expandable graphite, and hydrothermal expansion at a suitable temperature range described later Thereby expanding the respective layers of the expandable graphite and stabilizing the expanded structure.
The content of water is not particularly limited, but may be, for example, 2000 to 6500 parts by weight, preferably 3200 to 5000 parts by weight, based on 100 parts by weight of expandable graphite. When it is included in the above range, it is judged that hydrothermal swellability is further improved within the temperature range described later.
Cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH), and sodium dodecylbenzene sulfonate (SDBS), when the expandable graphite of layered structure is hydrothermally expanded, the intercalation effect of each expanded layer continues So that the hydrothermally expanded graphite having remarkably improved expansion ratio can be produced.
The content of the releasing agent is not particularly limited, and may be, for example, 50 to 120 parts by weight, preferably 80 to 100 parts by weight, based on 100 parts by weight of the expandable graphite. When it is included in the above range, the intercalation phenomenon can be effectively caused, the expansion ratio can be remarkably improved, and the stability of the expanded structure can be improved.
Next, hydrothermally expanded graphite is obtained through hydrothermal expansion by heating the mixed liquid containing the expandable graphite to 400 to 500 ° C.
Hydrothermal expansion is a reaction for synthesizing or altering minerals in the presence of hot water. In the present invention, when heating a solution containing expandable graphite and the above-mentioned releasing agent in the above-mentioned temperature range, The solution containing the release agent penetrates and is gasified, expanding between the layer and the layer to produce hydrothermal expanded graphite.
When the heating temperature is lower than 400 ° C, the expansion ratio of each layer is not easily peeled in the step of applying a shearing force described later, so that it is difficult to produce the graphene of the thin film. When the heating temperature exceeds 500 ° C, And the process proceeds to an excessively high temperature process, which is costly and the process efficiency is lowered
The thermal expansion for obtaining the hydrothermally expanded graphite may be performed by rapidly heating the mixed liquid containing the expandable graphite to 400 to 500 ° C or by heating to 400 to 500 ° C at a proper rate, Various methods can be applied without any particular limitations as long as they are within the allowable range.
For example, the mixed liquid containing the expandable graphite may be heated at a rate of 5 to 20 ° C / min to 400 to 500 ° C, preferably 10 to 15 ° C / min. When heated in the temperature raising rate range, the exfoliating agent and water effectively penetrate into each layer, and the expansion ratio can be further improved.
After the temperature is reached at 400 to 500 ° C., the heating time is not particularly limited, but can be, for example, 30 to 90 minutes, preferably 50 to 70 minutes. It is judged that the expansion rate is remarkably increased within the temperature and time range.
The properties of hydrothermally expanded graphite produced through the heating step are not particularly limited, but may have an apparent density of 0.01 to 0.1 g / mm 3 , preferably 0.02 to 0.04 g / mm 3 . When the above-mentioned range is satisfied, it is judged that each layer can be effectively peeled off in a step of applying a shearing force described later, whereby a thin film of graphene can be produced.
Thin-film Graphen's Produce
Finally, the graphene of the thin film is prepared by applying a shear force to the hydrothermally expanded graphite mixed with hydrothermal expanded graphite, dispersion medium and dispersant.
The hydrothermally expanded graphite produced is in a state in which each layer is in an expanded state and the interlayer coupling force is weakened. Therefore, when a physical shearing force is applied, each layer is peeled off due to a slip phenomenon between the respective layers to produce graphene.
The step of applying the shearing force may be performed without any particular limitations as long as it is a commonly used method in the art, and may be performed, for example, by dispersing with a high pressure disperser or a bead mill. In this case, the shearing force can be effectively applied to the hydrothermally expanded graphite by the dispersion.
In order to improve the peeling efficiency in the step of applying the shearing force, a dispersant and a dispersant are included, and further used dispersing agent includes cetyltrimethylammonium bromide (CTAB), tetrabutylammonium hydroxide (TBAOH) and sodium At least one compound selected from the group consisting of dodecylbenzene sulfonate (SDBS) can be used.
The kind of the dispersion medium is not particularly limited, but at least one compound selected from the group consisting of water, an alcohol solvent, dimethylsulfoxide (DMSO) and dimethylformamide (DMF) may be used.
In the step of applying the shear force to the hydrothermally expanded graphite mixture, when the high-pressure disperser is used, the pressure is not particularly limited, but may be, for example, 700 to 2000 bar, preferably 1000 to 1500 bar, , The shearing force is sufficient and the interlayer can be effectively peeled off.
When the high-pressure disperser is used, the size of the nozzle is not particularly limited. For example, the size of the nozzle may be 50 to 300 μm, preferably 100 to 200 μm. . ≪ / RTI >
In the step of applying the shear force to the hydrothermally expanded graphite mixed solution, when the bead mill is dispersed, the size of the beads used in the above step is not particularly limited, but may be, for example, 0.05 to 0.3 mm , In which case it is judged to be more effective for the production of the thin film graphene.
When the bead mill is used, the dispersion speed is not particularly limited, but may be, for example, 1800 to 2800 rpm, preferably 2200 to 2500 rpm. When the bead mill is rotated in the above range, By applying a frictional force to graphite, each layer can be effectively peeled off.
The present invention relates to graphene produced according to the above-described method, and the produced graphene is formed into a thin film structure of 0.3 to 5 nm.
The graphene according to the present invention is formed in a thin film structure, and is easily applied to an electronic device requiring a thin coating layer. In particular, the graphen is preferably applied to a sealing material of a display as a coating layer.
It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to be illustrative of the invention and are not intended to limit the scope of the claims. It will be apparent to those skilled in the art that such variations and modifications are within the scope of the appended claims.
Example And Comparative Example
Example One
100 g of expandable graphite was charged into a stripper containing 100 g of CTAB and 3200 g of water and heated to 450 캜 at a rate of 10 캜 / min and then heated at 450 캜 for 70 minutes to prepare hydrothermally expanded graphite. A sectional SEM photograph of the graphite is shown in Fig. Thereafter, a polyimide bead mill was charged into a mixture of 20 g of hydrothermally expanded graphite, 20 g of CTAB and 1980 g of water and dispersed at 2500 rpm to prepare a graphene peeling solution.
The prepared graphene stripping solution is dried at 120 ° C. for 24 minutes through a drying step to obtain a solid graphene.
Comparative Example One
Expanded graphite was heated at 450 캜 without addition of water or exfoliating liquid to prepare expanded graphite. A sectional SEM photograph of the produced expanded expanded graphite is shown in Fig. Thereafter, a polyimide bead mill was charged into a mixture of 20 g of expanded graphite, 20 g of CTAB and 1980 g of water and dispersed at 2500 rpm to prepare a graphene peeling solution.
The prepared graphene stripping solution is dried at 120 ° C. for 24 minutes through a drying step to obtain a solid graphene.
Test Methods
(1) Measurement of apparent density of expandable graphite
The apparent density (g / mm < 3 >) of expandable graphite prepared according to Examples and Comparative Examples was measured using a scalpel cylinder and a balance, and the results are shown in Table 1.
(2) Grapina Thickness measurement
AFM images of graphene prepared according to Examples and Comparative Examples were photographed (Figs. 4 and 5), and their thickness ranges were measured according to the above images. The results are shown in the graphs of Figs. 6 and 7 and in Table 1 .
Referring to Table 1, it can be seen that Example 1 according to the present invention has a smaller density than hydrothermally expanded graphite due to a uniform expansion effect by hydrothermal swelling. It was also confirmed that the thickness of the graphene thus produced was very thin.
Claims (12)
Heating the mixed liquid containing the expandable graphite to 400 to 500 ° C to obtain hydrothermal expanded graphite; And
Applying a shear force to the hydrothermally expanded graphite mixed solution obtained by mixing the hydrothermally expanded graphite with a dispersion medium and a dispersant.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180039194A (en) * | 2016-10-07 | 2018-04-18 | 전자부품연구원 | Anode for a lithium secondary battery and method of the same and lithium secondary battery using the same |
| KR20180082737A (en) | 2017-01-11 | 2018-07-19 | 에스케이이노베이션 주식회사 | Dispersive agent for carbon allotrope and conductive composition including the same |
| WO2019107860A1 (en) * | 2017-11-30 | 2019-06-06 | 전자부품연구원 | Graphene-current collector-integrated negative electrode for lithium secondary battery, and method for manufacturing same |
| CN110610814A (en) * | 2019-08-12 | 2019-12-24 | 中北大学 | Nano-scale electrochemical expansion graphite paper conductive matrix and preparation method thereof |
| CN110963485A (en) * | 2019-11-22 | 2020-04-07 | 贵州明志典成科技有限公司 | Production device and production method of high-conductivity graphene nanoplatelets |
| KR20200086036A (en) * | 2019-01-08 | 2020-07-16 | 주식회사 아이피씨 | Graphene sponge sheet and manufacturing method thereof |
| CN112225209A (en) * | 2020-11-17 | 2021-01-15 | 山东建筑大学 | Method for preparing graphene by using expandable graphite |
| KR20210084051A (en) | 2019-12-27 | 2021-07-07 | 주식회사 서현테크켐 | Carbon nanotube solution and fabricating method of the same |
| KR20220146199A (en) * | 2021-04-23 | 2022-11-01 | 주식회사 지에버 | Dry and wet graphene flake-based thermal ink and its manufacturing method |
| CN115465860A (en) * | 2022-07-06 | 2022-12-13 | 山东海科创新研究院有限公司 | Preparation method of low-oxygen high-stripping graphene oxide and application of obtained product |
Citations (1)
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| KR20110106625A (en) | 2010-03-23 | 2011-09-29 | 한국과학기술원 | Method of forming high-quality graphene using multi component eutectic point system |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110106625A (en) | 2010-03-23 | 2011-09-29 | 한국과학기술원 | Method of forming high-quality graphene using multi component eutectic point system |
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| KR20180039194A (en) * | 2016-10-07 | 2018-04-18 | 전자부품연구원 | Anode for a lithium secondary battery and method of the same and lithium secondary battery using the same |
| KR20180082737A (en) | 2017-01-11 | 2018-07-19 | 에스케이이노베이션 주식회사 | Dispersive agent for carbon allotrope and conductive composition including the same |
| WO2019107860A1 (en) * | 2017-11-30 | 2019-06-06 | 전자부품연구원 | Graphene-current collector-integrated negative electrode for lithium secondary battery, and method for manufacturing same |
| KR20190063592A (en) * | 2017-11-30 | 2019-06-10 | 전자부품연구원 | Graphene-current collecting integrated anode for lithium secondary battery and method for manufacturing the same |
| KR20200086036A (en) * | 2019-01-08 | 2020-07-16 | 주식회사 아이피씨 | Graphene sponge sheet and manufacturing method thereof |
| CN110610814A (en) * | 2019-08-12 | 2019-12-24 | 中北大学 | Nano-scale electrochemical expansion graphite paper conductive matrix and preparation method thereof |
| CN110963485A (en) * | 2019-11-22 | 2020-04-07 | 贵州明志典成科技有限公司 | Production device and production method of high-conductivity graphene nanoplatelets |
| KR20210084051A (en) | 2019-12-27 | 2021-07-07 | 주식회사 서현테크켐 | Carbon nanotube solution and fabricating method of the same |
| CN112225209A (en) * | 2020-11-17 | 2021-01-15 | 山东建筑大学 | Method for preparing graphene by using expandable graphite |
| KR20220146199A (en) * | 2021-04-23 | 2022-11-01 | 주식회사 지에버 | Dry and wet graphene flake-based thermal ink and its manufacturing method |
| CN115465860A (en) * | 2022-07-06 | 2022-12-13 | 山东海科创新研究院有限公司 | Preparation method of low-oxygen high-stripping graphene oxide and application of obtained product |
| CN115465860B (en) * | 2022-07-06 | 2023-06-16 | 山东海科创新研究院有限公司 | Preparation method of low-oxygen and high-stripping graphene oxide and application of obtained product |
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