KR101792242B1 - Graphene and method for manufacturing the same - Google Patents
Graphene and method for manufacturing the same Download PDFInfo
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- KR101792242B1 KR101792242B1 KR1020150137115A KR20150137115A KR101792242B1 KR 101792242 B1 KR101792242 B1 KR 101792242B1 KR 1020150137115 A KR1020150137115 A KR 1020150137115A KR 20150137115 A KR20150137115 A KR 20150137115A KR 101792242 B1 KR101792242 B1 KR 101792242B1
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Abstract
Graphene having a thickness of 3 to 6 nm and a specific surface area of 150 m 2 / g or more, and spherical graphite particles; Subjecting the spheroidized graphite particles to an acid treatment to produce an intergranular graphite compound; Removing the acid of the graphite intercalation compound and drying it; Expanding the dried graphite intercalation compound to produce an expanded graphite intermediate; And peeling the expanded graphite intermediate material to obtain graphene.
Description
Graphene and a method for producing the same.
Graphene, another name for a graphite monolayer, is typically produced by chemical vapor deposition (CVD) using transition metals (eg, Ni, Cu) as catalyst layers. The catalyst layers are metals which form carbide and carbide alloys well at high temperatures or adsorb carbon well. At this time, a carbon source material such as methane is pyrolyzed and then epitaxially grown to obtain graphene.
The CVD method for the production of single-layer graphene is capable of manufacturing a large-area single-layer graphene up to several tens of centimeters in width depending on the process used. However, there is a problem that the production yield of the graphene film without defects is not high, the process is complicated, and the cost is high.
Multilayer (several to several tens of layers) of similar graphene or graphene platelets apply mechanical forces to natural or artificial graphite flake powders. It is obtained through exfoliation through chemical reaction.
The chemical exfoliation process is generally carried out via a graphite intercalation compound. Alternatively, graphene may be produced by separating the graphite flake powder in the form of a dispersion in solution using energy due to the oxidation and reduction of graphite crystals, or external force such as ultrasonic waves.
Similar graphene or graphene platelets are low cost compared to single layer graphene, and are advantageous for mass production. However, there may be defects due to raw graphite or oxidizing agents used. In addition, there is a problem that the graft plane size of the graphene plate is in the form of small particles of several μm or less than 1 μm in the process of peeling with a sufficiently thin thickness. Therefore, there is a problem that it is difficult to apply to large-area graphene applications such as electric conductivity, thermal conductivity, and barrier properties.
Also, the size of the graphene produced generally correlates with the raw graphite grain size. If the particle size of the raw material graphite is small, sufficient separation due to the intercalant inserted in the graphite intercalation compound does not occur. Thus, there arises a problem that the thickness of the produced graphene platelets becomes thick or graphene is not produced.
Research is underway to solve these problems.
Conventionally, when the size of the raw material graphite particles is small, there arises a problem that the thickness of the graphene becomes thick or graphene is not produced. To solve such a problem, it is desired to provide a graphene having a small thickness and a large specific surface area, and at the same time to provide a graphene manufacturing method with good separation efficiency.
One embodiment of the present invention provides a graphene having a thickness of 3 to 6 nm and a specific surface area of 150 m 2 / g or more.
The graphene may have an average particle diameter of 5 to 50 탆.
The graphene may be one produced by using spherical graphite particles as a raw material.
Specifically, the spherical graphite particles may have a ratio of short diameter to long diameter of 0.50 to 1.0.
Specifically, the spherical graphite particles may have an average particle diameter of 10 to 100 탆.
Another embodiment of the present invention is a method for producing graphite, comprising the steps of: preparing spherical graphite particles; Subjecting the spheroidized graphite particles to an acid treatment to produce an intergranular graphite compound; Removing the acid of the graphite intercalation compound and drying it; Expanding the dried graphite intercalation compound to produce an expanded graphite intermediate; And peeling the expanded graphite intermediate material to obtain graphene.
The spheroidized graphite particles in the step of preparing the spheroidized graphite particles may have pores having a size of 2 μm or less, and the pore volume may be 0.1 mL / g to 0.2 mL / g.
The spheroidized graphite particles of the spherical graphite particles may have a ratio of the short diameter to the long diameter of 0.50 to 1.0.
The spheroidized graphite particles in the step of preparing the spheroidized graphite particles may have an average particle diameter of 10 to 100 탆.
(H 2 SO 4 ), nitric acid (HNO 3 ), bromic acid (HBrO 3 ), hydrochloric acid (HCl), and chloric acid (HClO 2) in an acidic treatment of the spheroidized graphite particles, 3), perchloric acid (HClO 4), periodic acid (HIO 3), and periodic acid (HIO 4), phosphoric acid (H 3 PO 4), fluorinated antimony acid (HSbF 6), sulfonic acid (FSO 3 H fluorophenyl) thereof . ≪ / RTI >
The step of expanding the dried graphite intercalation compound to prepare an expanded graphite intermediate material is a method in which the acid is removed and the dried graphite intercalation compound is heat-treated in a heating apparatus in an air or inert gas atmosphere .
Specifically, the inert gas may be nitrogen, argon, helium, neon, or a combination thereof.
Specifically, the heat treatment is performed at 700 to 1000 ° C It can be done.
Specifically, the heat treatment may be performed for 30 to 120 minutes.
Separating the expanded graphite intermediate material to obtain graphene, the step of injecting the expanded graphite intermediate material into a solvent to dilute the expanded graphite intermediate material; And dispersing and peeling the diluted expanded graphite intermediate material using a dispersing device.
Specifically, in the dispersing and peeling step, the dispersing device may be an ultrasonic dispersing device.
Specifically, the output of the ultrasonic dispersing device may be 500 to 1400 W.
Specifically, the dispersing and peeling may be performed for 30 minutes to 5 hours.
Peeling the expanded graphite intermediate material to obtain graphene, and then drying the peeled graphene.
Specifically, drying the exfoliated graphene may be performed at 70 to 120 ° C.
The graphene produced according to the above production method may have a thickness of 3 to 6 nm and a specific surface area of 150 m 2 / g or more.
A large graphene having a small thickness and a large specific surface area is provided, and a graphene manufacturing method with good separation efficiency is provided.
1 is a scanning electron microscope (SEM) photograph of expanded graphite particles of spherical graphite raw material.
2 is a scanning electron microscope (SEM) photograph of an expanded graphite material prepared by rapidly heating graphite interlayer compound.
3 is a scanning electron microscope (SEM) photograph of the finally obtained graphene platelet.
Hereinafter, embodiments of the present invention will be described in detail. However, it should be understood that the present invention is not limited thereto, and the present invention is only defined by the scope of the following claims.
As used herein, "average particle diameter" means the average diameter of a spherical substance present in a unit of measurement unless otherwise defined. If the material is an acetal, it means the diameter of the sphere calculated by approximating the spherical material to the spherical shape.
As used herein, "spherical" means a shape with the shortest diameter ratio to the longest diameter of 0.50 to 1.0, unless otherwise defined.
As used herein, "graphene " includes Graphene, similar graphene, and graphene platelets, other names of the graphite monolayer, unless otherwise defined.
Similar graphene or graphene platelet refers to a material in which graphene is laminated in multiple layers.
One embodiment of the present invention provides a graphene having a thickness of 3 to 6 nm and a specific surface area of 150 m 2 / g or more. More specifically, the specific surface area of the graphene may be 150 to 250 m 2 / g.
The average particle size of the graphene may be between 5 and 50 mu m.
The graphene may be made of spherical graphite particles as a raw material.
When spheroidal graphite particles are used, the void volume in the raw graphite particles is increased.
Therefore, when graphene is produced via an intercalated graphite compound, a phenomenon in which an intercalant such as an introduced acid retention moves inside the particle is made of flaky graphite having a particle size similar to that of the raw material Is better than the case.
As a result, it is possible to produce graphene having a thinner thickness and a larger specific surface area than those obtained by using flaky graphite having a similar particle size and having a small loss of intercalant when peeled off by graphene.
The spheroidized graphite particles may have a ratio of the short diameter to the long diameter of 0.50 to 1.0.
The spherical graphite particles may have an average particle diameter of 10 to 100 mu m. If the average particle size is too small, the dissipation rate of the intercalant introduced into the graphite layer increases, and the peeling efficiency may decrease. If the average particle size is too large, the cost of the raw material may increase significantly, which may result in an economical manufacturing process.
According to another embodiment of the present invention, there is provided a method for producing a graphite powder, comprising the steps of: preparing spherical graphite particles; Subjecting the spheroidized graphite particles to an acid treatment to produce an intergranular graphite compound; Removing the acid of the graphite intercalation compound and drying it; Expanding the dried graphite intercalation compound to produce an expanded graphite intermediate; And peeling the expanded graphite intermediate material to obtain graphene.
When spheroidal graphite particles are used, the pore volume in the raw graphite particles is increased.
Therefore, when graphene is produced via an intercalated graphite compound, a phenomenon in which an intercalant such as an introduced acid retention moves inside the particle is made of flaky graphite having a particle size similar to that of the raw material Is better than the case.
As a result, it is possible to produce graphene having a thinner thickness and a larger specific surface area than those obtained by using flaky graphite having a similar particle size and having a small loss of intercalant when peeled off by graphene.
The step of preparing the spherical graphite particles may be a step of sphericalizing the flaky graphite particles by physical milling or grinding.
The spherical graphite particles thus produced may have a structure in which several impression graphite particles are generally combined to form a spherical shape.
The spheroidized graphite particles in the step of preparing the spheroidized graphite particles have pores having a size of 2 μm or less and the pore volume may be 0.1 mL / g to 0.2 mL / g.
If the particle pore volume is too small, the insertion efficiency of the intercalant into the graphite particles may be low and the separation efficiency may be reduced. If the pore volume is too large, the elimination rate of the intercalant during the graphene manufacturing process becomes large, which may cause a problem that the peeling efficiency is reduced.
The spheronized graphite particles of the spheroidized graphite particles may have a ratio of the short diameter to the long diameter of 0.50 to 1.0.
Preparing the spheroidized graphite particles; and spheronizing the graphite particles in the spheroidized graphite particles may have an average particle size of 10 to 100 占 퐉.
If the average particle size is too small, the dissipation rate of the intercalant introduced into the graphite layer increases, and the peeling efficiency may decrease. If the average particle size is too large, the cost of the raw material may increase significantly, which may result in an economical manufacturing process.
(H 2 SO 4 ), nitric acid (HNO 3 ), bromic acid (HBrO 3 ), hydrochloric acid (HCl), chloric acid (HClO 3 ), and the like, , Hydrochloric acid (HClO 4 ), iodic acid (HIO 3 ), periodic acid (HIO 4 ), phosphoric acid (H 3 PO 4 ), fluoroantimonic acid (HSbF 6 ), fluorosulfonic acid (FSO 3 H) Lt; / RTI >
Thereafter, the acid may be removed and dried. The acid may be an excess of acid present primarily on the surface of the graphite intercalation compound.
The step of expanding the dried graphite intercalation compound to prepare an expanded graphite intermediate material may be a method in which the acid is removed and the dried graphite intercalation compound is heat-treated in a heating apparatus in an air or inert gas atmosphere have.
An inert gas is a gas that is difficult to cause a chemical reaction with other substances. Nitrogen is usually used as an inert gas in order to prevent the danger when there is a danger of explosive gas or vapor. In addition to nitrogen, argon, helium, neon, or a combination thereof may be used.
A method of heat-treating a dried graphite intercalation compound in an air or in an inert gas atmosphere, wherein the heating device is an induction or resistance heating type electric furnace, a microwave irradiating device, a gamma ray or electron beam generating device, It can be a combination.
A method for heat-treating a dried graphite intercalation compound in an air or an inert gas atmosphere, wherein the heat treatment is performed at a temperature of 700 to 1000 占 폚 .
If the heating temperature is too low, the graphite intercalation compound does not expand sufficiently and the peeling efficiency may be lowered. If the heating temperature is too high, the oxidation of the graphite intercalation compound proceeds and the quality of the produced graphene may be deteriorated.
In the method of heat-treating the dried graphite intercalation compound in an air or inert gas atmosphere, the heat treatment may be performed for 30 to 120 minutes.
If the heat treatment time is too short, there may arise a problem that the graphite intercalation compound does not sufficiently expand. If the heat treatment time is too long, there may arise a problem of disappearance due to oxidation of the graphite intercalation compound and deterioration of the physical properties of the produced graphene.
Separating the expanded graphite intermediate to obtain graphene, the step of injecting the expanded graphite intermediate into a solvent to dilute; And dispersing and peeling the diluted expanded graphite intermediate material using a dispersing device.
Diluting the expanded graphite intermediate material with a solvent, wherein the solvent can be water or organic solvent, and more specifically, the organic solvent may be methanol, ethanol, ethyl ether.
Dispersing and stripping the diluted expanded graphite intermediate material using a dispersing device, the dispersing device of the step may be an ultrasonic device. More specifically, the output of the ultrasonic dispersing apparatus may be 500 to 1400 W.
If the output is too small, the dispersing force is small and the peeling efficiency may be lowered. If the output is too large, the dispersing power is too large, and the grain size due to the cleavage in the plane direction of the obtained graphene can be greatly reduced.
The step of dispersing and stripping may be performed for 30 minutes to 5 hours.
Peeling the expanded graphite intermediate to obtain graphene, and then drying the peeled graphene. At this time, the drying temperature can be performed at 70 to 120 ° C. The drying time can be performed for 12 to 36 hours.
The graphene produced by the method of the present invention may have a thickness of 3 to 6 nm and a specific surface area of 150 to 250 m 2 / g. Also, the average particle size of the graphene produced according to the above method may be 5 to 50 탆.
Hereinafter, preferred embodiments and comparative examples of the present invention will be described. However, the following examples are only a preferred embodiment of the present invention, and the present invention is not limited to the following examples.
Example
Example One
Spherical graphite particles (manufacturer: Aoyu graphite, hereinafter the same) having an average particle diameter of 50 μm had a ratio of short diameter to long diameter in the range of 0.59 to 0.79.
The spheroidized graphite particles had a pore size of 2 μm or less and a pore volume of 0.16 mL / g. A scanning electron microscope (SEM) photograph of the spherical graphite particles is shown in Fig.
1 g of the spherical graphite particles was immersed in 100 mL of sulfuric acid having a concentration of 99.9%, and maintained for 24 hours to prepare a graphite intercalation compound into which sulfuric acid was introduced.
Thereafter, 1 L of distilled water was added to the prepared graphite intercalation compound, excess sulfuric acid present on the surface of the graphite intercalation compound was removed using a gravitational filter, and then dried in a vacuum oven.
Next, 1 g of the dried sample was placed in a sample container of alumina boat type, introduced into a furnace in a nitrogen atmosphere heated to 850 ° C., and then heat-treated for 1 hour to prepare expanded graphite. A scanning electron microscope (SEM) photograph of the manufactured expanded graphite particles is shown in Fig. The introduction efficiency of sulfuric acid between the graphite layers during the preparation of the graphite intercalation compounds is high and the graphite interlayer spacing varies greatly due to the effective pyrolysis and desorption of sulfuric acid during the rapid heating so that the interlayer spacing is wide and uniform morphology The production of expanded graphite was possible.
Thereafter, 1 g of the expanded graphite was diluted with 100 mL of distilled water and treated for 3 hours by using an ultrasonic dispersing apparatus having an output of 750 W to carry out peeling.
Thereafter, the separated graphene aqueous solution was filtered to remove the distilled water, and the solid matter was recovered.
Finally, the solid material was dried in a vacuum oven at 85 캜 for 24 hours, and a similar graphene platelet was prepared. A scanning electron microscope (SEM) photograph of the prepared similar graphene platelet particles is shown in FIG. The graphene platelet particles produced by using the sphericalized graphite particles as a raw material according to the production method of the present invention are more likely to be peeled off than graphene produced from a raw material of graphite to obtain thinner average thicknesses and wider areas of graphene There are advantages.
Example 2
Spherical graphite particles having an average particle diameter of 34.8 占 퐉 have a ratio of short diameter to long diameter of 0.51 To 0.91.
The spheroidized graphite particles had a pore size of 2 μm or less and a pore volume of 0.14 mL / g.
1 g of the spherical graphite particles was immersed in 100 mL of sulfuric acid having a concentration of 99.9%, and maintained for 24 hours to prepare a graphite intercalation compound into which sulfuric acid was introduced.
Thereafter, 1 L of distilled water was added to the prepared graphite intercalation compound, excess sulfuric acid present on the surface of the graphite intercalation compound was removed using a gravitational filter, and then dried in a vacuum oven.
Next, 1 g of the dried sample was placed in a sample container of alumina boat type, introduced into a furnace in a nitrogen atmosphere heated to 850 ° C., and then heat-treated for 1 hour to prepare expanded graphite.
Thereafter, 1 g of the expanded graphite was diluted with 100 mL of distilled water and treated for 3 hours by using an ultrasonic dispersing apparatus having an output of 750 W to carry out peeling.
Thereafter, the separated graphene aqueous solution was filtered to remove the distilled water, and the solid matter was recovered.
Finally, the solid material was dried in a vacuum oven at 85 캜 for 24 hours, and a similar graphene platelet was prepared.
Example 3
The spherical graphite particles having an average particle size of 19.6 占 퐉 have a ratio of short diameter to long diameter of 0.55 To 0.63.
The spheroidized graphite particles had a pore size of 2 μm or less and a pore volume of 0.16 mL / g.
1 g of the spherical graphite particles was immersed in 100 mL of sulfuric acid having a concentration of 99.9%, and maintained for 24 hours to prepare a graphite intercalation compound into which sulfuric acid was introduced.
Thereafter, 1 L of distilled water was added to the prepared graphite intercalation compound, excess sulfuric acid present on the surface of the graphite intercalation compound was removed using a gravitational filter, and then dried in a vacuum oven.
Next, 1 g of the dried sample was introduced into a tube furnace in a nitrogen atmosphere heated to 900 ° C. in an alumina boat type sample container, followed by heat treatment for 1 hour to prepare expanded graphite. Thereafter, 1 g of the expanded graphite was diluted with 100 mL of distilled water, treated with an output 750 W ultrasonic dispersing apparatus for 3 hours, and peeled.
Thereafter, the separated graphene aqueous solution was filtered to remove the distilled water, and the solid matter was recovered.
Finally, the solid material was dried in a vacuum oven at 85 캜 for 24 hours, and a similar graphene platelet was prepared.
Comparative Example
Comparative Example One
A similar graphene platelet was prepared in the same manner as in Example 1 except that impression graphite having an average particle size of 52 占 퐉 (manufacturer: Asbury Carbons, hereinafter the same) was used as a raw material.
Comparative Example 2
A similar graphene platelet was prepared in the same manner as in Example 1 except that impression graphite having an average particle size of 31 μm was used as a raw material.
Experimental Example
Experimental Example One : Specific surface area Measure
A BET specific surface area meter (Micrometrics, model ASAP 2000 surface area analyzer) was used for the analysis of the specific surface area. The specific relative surface area (P / P 0 ) range was from 0.0025 to less than 0.05 and the specific surface area was calculated using standard nitrogen adsorption (temperature 77K).
The measurement results are shown in Table 1 below.
(m 2 / g)
(nm)
It was confirmed that the specific surface area of graphene (Examples 1 to 3) prepared from raw graphite particles as raw materials was much higher than the specific surface area of graphene (Comparative Example 1 and Comparative Example 2) made of impression graphite as a raw material I could.
Graphene grains (Examples 1 to 3) prepared by using spherical graphite grains as raw materials were also found to have a theoretical thickness calculated by the formula: graphene thickness = [(2630 / measurement specific surface area) - 1] x 0.3354 It was confirmed that the graphene was thinner than the graphene produced (Comparative Example 1 and Comparative Example 2).
As the thickness of the graphene becomes thinner, the aspect ratio of the graphene having the same width increases, thereby improving the barrier effect when the coating layer is formed. Since the graphene film has a high specific surface area, it can be applied to a catalyst or a catalyst carrier There is an advantage that the reaction efficiency can be improved.
Experimental Example 2: Particle size analysis
A laser particle size analyzer (CILAS, model particle size analyzer 920) was used for particle size analysis of the obtained graphene. The dispersive solvent used is isopropyl alcohol, and the average particle size of the sample was analyzed by dynamic light scattering of a solution in which graphene was well dispersed at a concentration of 0.5 wt%.
The analysis results are shown in Table 2 below
(μm)
The average particle size of the graphene thus produced was also larger than that of graphene (Examples 1 to 3) produced from spheroidized graphite particles as raw materials (Comparative Examples 1 and 2) .
If the graphene particle size is large, there is an advantage that a graphene-based coating layer having excellent properties such as barrier properties, electrical conductivity, and thermal conductivity can be manufactured.
The present invention provides a method for producing graphene having a sufficient particle size while using a spherical graphite particle as a raw material for graphene, thereby reducing the thickness of the graphene. As a result, it is possible to increase the peeling efficiency in the production of graphene. In addition, graphene that can be applied to applications where the use of large area graphene, such as electrical conductivity, thermal conductivity, and barrier properties, is desirable.
It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims. As will be understood by those skilled in the art. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Claims (21)
Graphene is produced using spherical graphite particles as raw materials,
Wherein the spheroidized graphite particles have a short diameter ratio to a long diameter of from 0.50 to 1.0.
Wherein the graphene has an average particle diameter of 5 to 50 占 퐉.
Wherein said spheroidized graphite particles have an average particle size of 10 to 100 占 퐉.
Subjecting the spheroidized graphite particles to an acid treatment to produce an intergranular graphite compound;
Removing the acid of the graphite intercalation compound and drying it;
Expanding the dried graphite intercalation compound to produce an expanded graphite intermediate; And
Peeling the expanded graphite intermediate material to obtain graphene;
Lt; / RTI >
Preparing the spheroidized graphite particles;
Wherein the spheroidized graphite particles have a ratio of a short diameter to a long diameter of 0.50 to 1.0.
Preparing the spheroidized graphite particles;
Wherein the spheroidized graphite particles have pores having a size of 2 탆 or less and a pore volume of 0.1 mL / g to 0.2 mL / g.
Preparing the spheroidized graphite particles;
Wherein the spheroidized graphite particles have an average particle diameter of 10 to 100 占 퐉.
Treating the spheroidized graphite particles with an acid to prepare an intergranular graphite compound;
The acid is sulfuric acid (H 2 SO 4), nitric acid (HNO 3), boric acid (HBrO 3), hydrochloric acid (HCl), acid (HClO 3), perchloric acid (HClO 4), periodic acid (HIO 3), and periodic acid (HIO 4 ), phosphoric acid (H 3 PO 4 ), fluorantimonic acid (HSbF 6 ), fluorosulfonic acid (FSO 3 H), or a combination thereof.
Expanding the dried graphite intercalation compound to produce an expanded graphite intermediate,
Wherein the acid is removed and the dried graphite intercalation compound is heat-treated in a heating apparatus in an air or inert gas atmosphere.
Wherein the inert gas is nitrogen, argon, helium, neon, or a combination thereof.
The heat treatment is performed at 700 to 1000 ° C Lt; RTI ID = 0.0 > (I). ≪
Wherein the heat treatment is performed for 30 to 120 minutes.
Peeling the expanded graphite intermediate material to obtain graphene,
Diluting the expanded graphite intermediate material with a solvent; And
Dispersing and peeling the diluted expanded graphite intermediate material using a dispersing device;
≪ / RTI >
The dispersing and peeling step
Wherein the dispersing device is an ultrasonic dispersing device.
And the output of the ultrasonic dispersing apparatus is 500 to 1400 W.
Wherein the dispersing and peeling comprises:
Lt; RTI ID = 0.0 > 5 < / RTI >
Peeling the expanded graphite intermediate material to obtain graphene,
And drying the exfoliated graphene.
Drying the exfoliated graphene;
Lt; RTI ID = 0.0 > 120 C < / RTI >
The produced graphene has a thickness of 3 to 6 nm and a specific surface area of 150 m 2 / g or more.
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