KR101858160B1 - Producing method and system of graphene - Google Patents
Producing method and system of graphene Download PDFInfo
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- KR101858160B1 KR101858160B1 KR1020160024279A KR20160024279A KR101858160B1 KR 101858160 B1 KR101858160 B1 KR 101858160B1 KR 1020160024279 A KR1020160024279 A KR 1020160024279A KR 20160024279 A KR20160024279 A KR 20160024279A KR 101858160 B1 KR101858160 B1 KR 101858160B1
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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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
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy
Abstract
The present invention relates to a method for producing graphene. The graphene manufacturing method according to the present invention is a graphene manufacturing method using thermal plasma, comprising the steps of (a) preparing graphite (S10), (b) oxidizing graphite (S20), (c) thermal plasma treatment of graphite oxide (S30), and (d) graphene exfoliation.
Description
The present invention relates to a method and system for manufacturing graphene. More particularly, the present invention relates to a graphene manufacturing method and system capable of effectively separating graphene by increasing the distance between graphene layers by subjecting graphite to thermal plasma treatment.
Graphene is a two-dimensional allotropic material made of carbon atoms and has a honeycomb-like hexagonal structure. It has a very large specific surface area (about 2600 m 2 / g) and a very good capacitor property of 550 Fg -1 , It is a material with chemical stability. Graphene has an unlimited potential for applications such as energy storage materials, transparent electrode films, barrier films, graphene / metal composites, and heat dissipation materials.
Examples of the method of peeling the graphene include a mechanical peeling method called scotch tape method, a chemical peeling method in which graphite is oxidized to induce peeling and then graphen is extracted through a reduction process, a nickel / Chemical vapor deposition which forms a graphene crystal structure by crystallizing carbon on the catalyst layer after depositing copper on the substrate, high temperature heat treatment of carbon adsorbed or contained materials such as silicon carbide (SiC) And an epitaxial method for forming a film.
However, the graphene is not easily peeled off due to the van der Waals action between the graphene layers due to the sp 2 carbon bond at the surface, and the graphene peeled using the above method is a single layer, However, there is a problem in that it is mostly present as a thick multi-layer. Even if it is peeled off, it is restacking again. Therefore, it does not utilize the high specific surface area of the single-layer graphene, and it is difficult to form a uniform composite structure, which serves as a factor that hinders the utilization of graphene.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a graphene manufacturing method and system capable of effectively separating graphene by increasing the distance between graphene layers .
It is another object of the present invention to provide a graphene manufacturing method and system capable of improving process productivity by omitting an additional reduction step and a defect removing step after graphen peeling.
It is another object of the present invention to provide a method and system for producing graphene which enables mass production of graphene through a continuous process rather than a one-time process.
It is another object of the present invention to provide a method and system for producing graphene capable of binding metal nanoparticles on the surface of graphene via metal nanoparticles in a thermal plasma treatment process.
The above object of the present invention is achieved by a method for producing graphene using thermal plasma, comprising the steps of: (a) preparing graphite; (b) oxidizing the graphite; (c) subjecting the graphite oxide to thermal plasma treatment; And (d) exfoliating the graphenes.
The above object of the present invention can be also achieved by a method of manufacturing graphene using thermal plasma, comprising the steps of: (a) preparing graphite; (b) oxidizing the graphite; And (c) thermally plasma-treating the mixture of graphite oxide and metal to bond the graphite and the nano-metal particles.
According to an embodiment of the present invention, in the step (c), the thermal plasma process may be performed using a DC plasma.
According to an embodiment of the present invention, in the step (c), the thermal plasma process may be performed using N 2 plasma.
Further, according to an embodiment of the present invention, in the step (c), the distance between graphene layers in the graphite oxide after the thermal plasma treatment may be increased.
According to an embodiment of the present invention, in the step (c), the sp 3 carbon bond structure of the graphite oxide may be decreased and the sp 2 carbon bond structure may be increased after the thermal plasma treatment.
Also, according to an embodiment of the present invention, in the step (c), the temperature change rate of the graphite oxide may be at least 3000 K / sec.
According to an embodiment of the present invention, the nano metal particles are selected from the group consisting of Si, Ni, Ti, Cr, Mn, Fe, Co, Cu, Sn, In, Pt, Au, Mg, ≪ / RTI >
According to an embodiment of the present invention, in the step (c), a graphite-nano metal compound may be formed at the interface between the graphite oxide and the nano-metal particles.
According to an embodiment of the present invention, immediately after the metal is vaporized, nuclei are grown on the surface of the graphite oxide to bond the graphite and the nanometer metal particles.
Also, according to an embodiment of the present invention, (d) the step of exfoliating the graphene bound to the nanomaterial may be further included.
The above object of the present invention is also achieved by a graphene manufacturing system using a thermal plasma, comprising: a thermal plasma generator; A thermal plasma processing unit installed at one side of the thermal plasma generating unit and thermally plasma-processing the supplied graphite oxide; A filter unit for selectively filtering the thermal plasma treated graphite; And a collector for collecting the thermal plasma treated graphite.
According to the present invention configured as described above, graphene can be effectively stripped by increasing the distance between graphene layers.
Further, after the graphene peeling, the additional reduction step and the defect removing step are omitted, and the process productivity is improved.
In addition, the present invention has an effect of enabling mass production of graphene through a continuous process rather than a one-time process.
Further, there is an effect that the metal nanoparticles can be bonded onto the surface of the graphene via the metal nanoparticles in the thermal plasma treatment process.
1 is a schematic view showing a method of manufacturing graphene according to an embodiment of the present invention.
2 is a schematic diagram illustrating a graphene manufacturing system in accordance with an embodiment of the present invention.
3 is a scanning electron microscope (SEM) photograph of the thermal plasma treatment (FIG. 3 (a)) and after (FIG. 3 (b)) according to an embodiment of the present invention.
4 is a graph showing Raman analysis results of graphite oxide according to an embodiment of the present invention.
FIG. 5 is a graph showing XRD analysis results according to plasma types according to an embodiment of the present invention.
FIG. 6 is a field emission transmission electron microscope (FE-TEM) photograph of graphene according to an embodiment of the present invention and graphene according to a comparative example.
7 is a schematic view showing a method of manufacturing graphene according to another embodiment of the present invention.
8 is a scanning electron microscope (SEM) photograph of the thermal plasma treatment (Fig. 8 (a)) and after (Fig. 8 (b)) according to another embodiment of the present invention.
9 is a graph showing XRD analysis results of graphene decorated with metal nanoparticles according to another embodiment of the present invention.
The following detailed description of the invention refers to the accompanying drawings, which illustrate, by way of illustration, specific embodiments in which the invention may be practiced. These embodiments are described in sufficient detail to enable those skilled in the art to practice the invention. It should be understood that the various embodiments of the present invention are different, but need not be mutually exclusive. For example, certain features, structures, and characteristics described herein may be implemented in other embodiments without departing from the spirit and scope of the invention in connection with an embodiment. It is also to be understood that the position or arrangement of the individual components within each disclosed embodiment may be varied without departing from the spirit and scope of the invention. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is to be limited only by the appended claims, along with the full scope of equivalents to which such claims are entitled, if properly explained. In the drawings, like reference numerals refer to the same or similar functions throughout the several views, and length and area, thickness, and the like may be exaggerated for convenience.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings, so that those skilled in the art can easily carry out the present invention.
1 is a schematic view showing a method of manufacturing graphene according to an embodiment of the present invention.
According to an embodiment of the present invention, a method of manufacturing graphene using a thermal plasma includes the steps of (a) preparing a graphite (S10), (b) oxidizing graphite S20), (c) thermal plasma treatment of graphite oxide (S30), and (d) graphene stripping (S40). Optionally, (e) recovering the graphene may be further included.
Referring to FIG. 1, first, graphite may be prepared (S10). The graphite is preferably granular graphite having a size of several tens of micrometers to several hundreds of micrometers and a purity of 99% or more. Flake-type natural / artificial graphite, lump-type natural / artificial graphite, and the like can be used without limitation.
Next, graphite can be oxidized (S20). The oxidation of graphite can be used without limitation in Hummer's method and the like used in the conventional chemical stripping method. For example, sulfuric acid (H 2 SO 4 ) is added to graphite, followed by stirring and cooling, followed by adding potassium permanganate (KMnO 4 ) to obtain graphite oxide (GO). Graphite oxide is expanded in the c-axis direction by intercalation and can have an accordion-like structure. In this specification, the oxidation of graphite can be understood as a primary expansion between graphene layers.
Next, the graphite oxide can be subjected to thermal plasma treatment (S30). The oxidized graphite can be further expanded after the thermal plasma treatment. That is, the expansion of about 2 to 4 times in the c-axis direction can be further progressed. In this specification, expansion by thermal plasma treatment can be understood as secondary expansion between graphene layers.
Plasma can be DC or RF plasma, and N 2 plasma can be used to N doping graphene. The N-doped graphene has an advantage that the electrical conductivity can be improved and the dispersibility in the solution can be increased as the wettability is improved. However, it should be noted that the present invention is not necessarily limited thereto.
The graphite oxide can be thermally plasma treated within 2 seconds by a plasma having a temperature of 6000 K or more. That is, the oxidized graphite has a rapid temperature change of at least 3000 K / sec and can have the best expansion efficiency by thermal plasma treatment.
On the other hand, although it is not strictly considered as a reduction process, as the oxygen atoms are separated and removed from the oxidized graphite (or graphene) by the thermal plasma treatment, the oxidized graphite is reduced in reduced graphite (or graphene , rGO)]. Therefore, the following description does not describe that graphene is peeled off from graphite oxide but graphene is peeled off from graphite.
Next, graphene can be peeled from the secondary expanded graphite (S40). The graphene peeling from the secondary expanded graphite can be used without limitation for the known graphene peeling method. The interlayer distance of graphene increases from oxidation (primary expansion) of graphite, so that the interlayer π-π interaction and the van der Waals force are reduced, and the interlayer distance of graphene is further increased from thermal plasma treatment of graphite oxide , It is possible to obtain an effect that peeling is induced more effectively than conventional graphene peeling. A detailed description thereof will be described later.
In addition, graphene recovery can be completed (S50) by completing recovery of graphene through transfer or the like after peeling of graphene (S50), or further performing impurity removal process or the like on the peeled graphene.
2 is a schematic diagram illustrating a
2, a
The
The thermal
Thermal plasma treatment of the oxidized graphite is performed in the
The
The plasma-treated graphite G flowing into the
The
Conventionally, a method of using microwave to secure the distance between graphene graphite and heat of 700 ° C generated from a heating element such as Super Kanthal has been used. However, microwave generating devices are limited in size, and industrial equipment is very expensive. In addition, a device using a heating element has a problem that a long time of several tens of minutes or more is required for heating and cooling. In both of the above methods, there is a problem that the process is performed by disposing graphite oxide in a closed chamber, and then the chamber is opened to recover the processed graphite oxide, that is, the process is intermittently performed with a single operation. In addition, the graphene peeling effect is weak, and there still remains a problem that impurities remain in graphene.
On the other hand, the present invention has an advantage that the process is completed within a very short time (within 2 seconds) by using a thermal plasma. The graphite directly subjected to the thermal plasma treatment while supplying the graphite oxide into the thermal
Hereinafter, the graphene production method of the present invention will be described based on experimental results.
3 is a scanning electron microscope (SEM) photograph of the thermal plasma treatment (FIG. 3 (a)) and after (FIG. 3 (b)) according to an embodiment of the present invention. Referring to FIG. 3 (a), plate-like graphite in which graphene layers are closely stacked can be identified. Referring to FIG. 3 (b), it can be seen that the oxidized graphite expands after the thermal plasma treatment and expands in an accordion shape, thereby increasing the distance between the graphene layers. It exhibits a volume expansion of about 70-275 times the raw material.
4 is a graph showing Raman analysis results of graphite oxide according to an embodiment of the present invention. And analyzed with a micro Raman spectrometer using a 532 nm laser and a 50x lens for a range of 1200-2800 cm -1 .
Referring to FIG. 4, all the analysis results show a graphene Raman spectrum of a multi-layered structure. A strong G peak appears at around 1585 cm -1 , and a D peak appears at a 2D peak at about 2720 cm -1 and around 1340 cm -1 .
G peak is a result of phonon oscillation of the sp 2 bond structure of carbon (corresponding to the stretching of carbon-carbon bond).
2D peaks are caused by finite size and lattice defects. The double-layer graphene has a pair of π- π * electron bands due to the interlayer interaction, and the 2D-mode has double resonance due to the electronic structure of the graphene. . Therefore, it is known that the position and the half-peak width are related to the number of layers of graphene.
The D peak is a peak showing a defect in the sp 2 crystal structure or a crystal structure of sp 3 , which is observed near the edge of the graphene or in the case of many defects.
Referring again to FIG. 4, graphite (blue line, red line, and yellow line) subjected to thermal plasma treatment than graphite oxide (black line) not subjected to thermal plasma treatment showed G peak and 2D peak increase and D peak decrease Can be confirmed.
Increase in the G peak thermal plasma processing after Yes many more in the pin carbon-carbon bond structure (sp 2 carbon bond increased structure) represents a formed, reduction of the D-peak is yes shrink impurities or defects in the pin (sp 3 carbon Bond structure reduction). That is, the increase of the G peak and the decrease of the D peak by the thermal plasma treatment suggest that the purity of graphene is improved and an additional reduction process for eliminating impurities is unnecessary. Accordingly, the present invention has an advantage in that process productivity can be improved by omitting an additional reduction process and a defect removing process after graphen peeling.
The increase in the 2D peak suggests that the oxidized graphite expands further and that there is a small amount of graphene even within the same thickness. Accordingly, the present invention has an advantage that a smaller number of multi-layered or single-layer graphenes can be produced, and a high specific surface area can be utilized.
FIG. 5 is a graph showing XRD analysis results according to plasma types according to an embodiment of the present invention. Referring to FIG. 5, it can be seen that the treatment with DC plasma shows a higher crystallinity of carbon than with the treatment with RF plasma.
FIG. 6 is a field emission transmission electron microscope (FE-TEM) photograph of graphene according to an embodiment of the present invention and graphene according to a comparative example. 6 (a) and 6 (b) are comparative examples using microwave, and Fig. 6 (c) is an embodiment of the present invention using thermal plasma. When graphene is peeled off using a microwave, about 15-40 layers and about 20-60 layers of graphene can be peeled off. On the contrary, when graphene is peeled off using thermal plasma, about 2-7 layers It is possible to peel off the laminated graphene, and it can be confirmed that the peeling effect of the present invention is superior.
7 is a schematic view showing a method of manufacturing graphene according to another embodiment of the present invention.
According to another embodiment of the present invention, a method of manufacturing graphene using thermal plasma includes the steps of (a) preparing a graphite (S10 '), (b) oxidizing graphite (S20 ') and (c) a step (S30') of subjecting the mixture of graphite and metal to a thermal plasma treatment to bond the graphite and the nano-metal particles. Alternatively, the method may further include (d) a step (S40 ') of exfoliating graphene bound with the nano-metal particles, and (e) a step (S50') of recovering the graphene. Hereinafter, steps S10 ', S20', and S50 'are the same as steps S10, S20, and S50 of FIG. 1, and thus description thereof will be omitted and differences between steps S30' and S40 'will be described.
First, graphite is prepared (S10 ') and graphite can be oxidized (S20').
Next, the mixture of graphite oxide and metal may be subjected to thermal plasma treatment (S30 '). The graphite and nano-metal particles can be bonded by thermal plasma treatment. The metal has a size of several tens of micrometers and may be a metal selected from the group consisting of Si, Ni, Ti, Cr, Mn, Fe, Co, Cu, Sn, In, Pt, Au, Mg and combinations thereof.
The oxidized graphite can be further expanded after the thermal plasma treatment. That is, the expansion of about 2 to 4 times in the c-axis direction can be further progressed. In this specification, expansion by thermal plasma treatment can be understood as secondary expansion between graphene layers.
On the other hand, during the thermal plasma treatment, the metal can be vaporized by the high temperature plasma. Immediately after the vaporization, the metal can grow nuclei from the surface of the oxidized graphite. In other words, graphite-nanometallic compounds can be produced at the interface of graphite oxide and nanometallic particles. Nanometer metal particles have a size of less than 100 nm and can be generated between graphene layers.
The graphite oxide can be thermally plasma treated within 2 seconds by a plasma having a temperature of 6000 K or more. That is, the oxidized graphite has a rapid temperature change of at least 3000 K / sec and can have the best expansion efficiency by thermal plasma treatment.
According to another embodiment of the present invention, a nano-fusion of graphite (graphene) and metal is formed by thermal plasma treatment of a mixture of graphite oxide and metal to grow metal nuclei on the surface between the graphene interlayers in oxidized graphite can do.
In addition, graphene bound to the nano-metal particles from the secondary expanded graphite can be stripped (S40 '). The separation of the graphene bound with the nanometer metal particles from the secondary expanded graphite can be carried out without limitation using a known graphene separation method.
Graphene has excellent mechanical and electrical properties in the horizontal direction, but poor vertical characteristics. However, the graphene nano-fusion material in which nano-sized metal particles are crystallized at high density according to another embodiment of the present invention has an advantage that mechanical and electrical characteristics in the vertical direction can be improved.
8 is a scanning electron microscope (SEM) photograph of the thermal plasma treatment (Fig. 8 (a)) and after (Fig. 8 (b)) according to another embodiment of the present invention.
Figure 8 (a) shows a mixture of graphite oxide and metal. It can be seen that graphite and Si of several tens of μm are mixed. Fig. 8 (b) shows that the nano-metal particles are bonded to the surface of the graphite after the thermal plasma treatment. It can be confirmed that the nano metal particles are grown through nucleation immediately after vaporization and are bound to graphite in a size of nm level.
9 is a graph showing XRD analysis results of graphene decorated with metal nanoparticles according to another embodiment of the present invention. Referring to FIG. 9, graphite-nano metal compound was generated at the interface between graphite and nano-metal particles since 80.72% of graphite, 18.26% of Si and 1.02% of SiC exist after thermal plasma treatment .
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is clearly understood that the same is by way of illustration and example only and is not to be taken in conjunction with the present invention. Variations and changes are possible. Such variations and modifications are to be considered as falling within the scope of the invention and the appended claims.
10: Graphene manufacturing system
100: thermal plasma generating unit
200: Plasma gas supply part
300:
400: thermal plasma processing unit
500:
600: collecting section
700: Vacuum pump
Claims (20)
(a) preparing graphite;
(b) oxidizing the graphite;
(c) subjecting the graphite oxide to thermal plasma treatment; And
(d) step of exfoliating graphene
Lt; / RTI >
Wherein the graphene layer in the oxide graphite after the step (b) and the step (c) is increased in length, and the graphene laminated in the layer less than ten layers in the step (d) Way.
(a) preparing graphite;
(b) oxidizing the graphite; And
(c) subjecting the mixture of graphite and metal to a thermal plasma treatment to bond the graphite and the nano-metal particles; And
(d) a step of exfoliating graphene bound with the nano-metal particles
Including the
Wherein the graphene layer in the oxide graphite after the step (b) and the step (c) is increased in length, and the graphene laminated in the layer less than ten layers in the step (d) Way.
In the step (c), the thermal plasma treatment is performed using a DC plasma.
In the step (c), the thermal plasma treatment is performed using N 2 plasma.
In the step (c), after the thermal plasma treatment, the sp 3 carbon bond structure of the oxidized graphite decreases and the sp 2 carbon bond structure increases.
In the step (c), the rate of temperature change of the graphite oxide is at least 3000 K / sec.
Wherein the nano metal particles are at least one particle selected from the group consisting of Si, Ni, Ti, Cr, Mn, Fe, Co, Cu, Sn, In, Pt, Au, Mg and combinations thereof.
In the step (c), a graphite-nano metal compound is formed at the interface between the graphite oxide and the nano-metal particles.
And immediately after the metal is vaporized, nuclei are grown on the surface of the graphite oxide to bond the graphite and the nano-metal particles.
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CN111039282A (en) * | 2019-12-27 | 2020-04-21 | 中国科学院合肥物质科学研究院 | Preparation method of graphene material and application of graphene material in preparation of lithium ion battery |
CN111453719B (en) * | 2020-04-24 | 2022-05-24 | 湖北航天化学技术研究所 | High-quality graphene and preparation method thereof |
CN112408383A (en) * | 2020-11-17 | 2021-02-26 | 成都爱敏特新能源技术有限公司 | Plasma stripping graphite material and preparation method thereof |
KR102240358B1 (en) * | 2020-11-19 | 2021-04-14 | 주식회사 케이비엘러먼트 | Continuous mass manufacturing method of graphene using high temperature plasma spinning and graphene manufactured by using the same |
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KR101330227B1 (en) | 2012-06-28 | 2013-11-18 | 재단법인 철원플라즈마 산업기술연구원 | A graphene-nano particle composite which nano particles are highy densified thereon |
KR101573241B1 (en) | 2014-05-08 | 2015-12-01 | 한국화학연구원 | Three-dimensional Grapheene Structure and Manufacturing method of Thereof and Elctrode using thereof |
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KR101330227B1 (en) | 2012-06-28 | 2013-11-18 | 재단법인 철원플라즈마 산업기술연구원 | A graphene-nano particle composite which nano particles are highy densified thereon |
KR101573241B1 (en) | 2014-05-08 | 2015-12-01 | 한국화학연구원 | Three-dimensional Grapheene Structure and Manufacturing method of Thereof and Elctrode using thereof |
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