WO2013133467A1 - 판형 탄소 나노입자 제조방법 및 이를 이용한 알루미늄-탄소 복합재료의 제조방법 - Google Patents
판형 탄소 나노입자 제조방법 및 이를 이용한 알루미늄-탄소 복합재료의 제조방법 Download PDFInfo
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- WO2013133467A1 WO2013133467A1 PCT/KR2012/001888 KR2012001888W WO2013133467A1 WO 2013133467 A1 WO2013133467 A1 WO 2013133467A1 KR 2012001888 W KR2012001888 W KR 2012001888W WO 2013133467 A1 WO2013133467 A1 WO 2013133467A1
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- graphite material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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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- 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
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
Definitions
- the present invention relates to a method for producing a plate-shaped carbon nanoparticles and a method for producing an aluminum-carbon composite material using the same, and more particularly, to a method for producing a plate-shaped carbon nanoparticles consisting of a single layer to several tens of carbon atomic layers and aluminum using the same It relates to a method for producing a carbon composite material.
- Carbon material is a material composed mainly of carbon atoms, and has been widely used in nature and has been used as a carbon material such as charcoal and ink for a long time. Carbon materials are classified into four materials along with metals, ceramics, and polymers, as they are used in high-tech industries because they have properties such as ultra high temperature, light weight, and abrasion resistance.
- the carbon material may have a compound form combined with other elements in addition to the form of carbon alone. Since the electrical and mechanical properties vary depending on the form of bonding with other elements, it can be used in various fields according to the purpose. Therefore, various carbon products are produced at present.
- Carbon alone is a material made of carbon fiber, graphite, nano-carbon materials (carbon nanotubes, graphene, carbon nanoplates, fullerenes, etc.).
- Nanocarbon materials have good thermal, electrical, and mechanical properties and are expected to be applied in as many areas as general carbon materials.
- the two-dimensional structure of graphene or plate-shaped carbon nanoparticles has unique advantages over other carbon allotropees in terms of their electrical and electronic applications, as well as their unique physical properties. That is, due to the two-dimensional structure, there is an advantage that the electronic circuit can be configured by introducing a general semiconductor process of the top-down method represented by printing, etching, and the like.
- Nanocarbon materials have very high specific surface areas and thus have unique physical and chemical properties that are not seen in bulk.
- New concept high-efficiency / multifunctional products that take advantage of the characteristics of these nanomaterials are continuously being developed, and their application fields are gradually expanding.
- Aluminum is used for a variety of purposes, from foils used in kitchens to disposable tableware, windows, cars, aircraft and spacecraft.
- the characteristics of aluminum are as light as 1/3 of the weight of iron, and excellent strength when alloyed with other metals.
- a chemically stable oxide film is present on the aluminum surface, corrosion is prevented from progressing due to moisture, oxygen, or the like.
- aluminum has been used in automobiles and aircraft.
- aluminum parts are lighter than conventional steel parts, thereby reducing their own loads, and this has the effect of gaining benefits that can contribute to reducing fuel consumption by reducing the weight of the vehicle body.
- such aluminum has only about 40% of tensile strength compared to iron, and when used as a structural material, the thickness of the structural aluminum tube or plate becomes very thick, which results in excessive material costs and excessive material costs. Problems will arise.
- a carbon material for example, a carbon nano material
- a carbon material is difficult to disperse due to interactions between van der Waals forces between materials, making it difficult to uniformly disperse in aluminum.
- the carbon material and aluminum is not mixed well due to the difference in surface tension between the carbon material and aluminum.
- One object of the present invention is to provide a method for producing plate-shaped carbon nanoparticles using mechanical shear force.
- Another object of the present invention is to provide an aluminum-carbon composite material using the plate-shaped carbon nanoparticles prepared by the above method.
- the method of manufacturing the plate-shaped carbon nanoparticles for achieving the above object of the present invention is a graphite material and ball mill in a ball mill container rotatably coupled to a disk rotatable in a first direction in a second direction opposite to the first direction.
- Putting the ball ; Rotating the disk and the ball mill container for a predetermined time such that the ball mill ball rubs against the wall surface of the ball mill container so that the ball mill ball itself rotates to apply mechanical shear force to the graphite material; And separating the plate-shaped carbon nanoparticles prepared from the graphite material.
- the graphite material is selected from the group consisting of plate-shaped artificial graphite material, powder-shaped artificial graphite material, lump-shaped artificial graphite material, plate-shaped natural graphite material, powder-shaped natural graphite material and lump-shaped natural graphite material. It may include at least one.
- Rotating the disk and the ball mill container to apply mechanical shear force to the graphite material may be performed in a non-oxidizing atmosphere.
- the ratio of the rotational speed of the ball mill vessel to the rotational speed of the disk may be 30% or more and 70% or less of the critical angular velocity ratio.
- the rotation speed of the disk and the ball mill ball may be 150 rpm or more and 500 rpm or less.
- the release agent may include at least one selected from the group consisting of a surfactant, an organic material, and an inorganic material capable of increasing friction between the graphite material and the ball mill ball.
- the surfactant may include at least one selected from the group consisting of SDS, NaDDBs, and CTAB
- the organic material may include at least one selected from the group consisting of sugar and DNA
- the inorganic material may be aluminum. It may include.
- a method of manufacturing an aluminum-carbon composite material comprising: combining an aluminum powder with a carbon material to produce an aluminum-carbon mixed powder; Applying a mechanical shearing force to the aluminum-carbon mixed powders to produce modified aluminum-carbon mixed powders; And sintering the modified aluminum-carbon mixed powders.
- the preparing of the aluminum-carbon mixed powder may include mixing the carbon material with the solvent and then performing ultrasonic treatment; And adding ultrasonic powder to the ultrasonicated mixed solution and then ultrasonicating the mixture.
- the carbon material may include at least one of a group consisting of graphite plates, graphite fibers, carbon fibers, carbon nanofibers, and carbon nanotubes.
- the aluminum powders may be added such that the carbon material is about 0.1 to 50 wt.% Based on the weight of the aluminum powders.
- the manufacturing of the modified aluminum-carbon mixed powders may include the aluminum-carbon mixed powders and the ball mill ball in a ball mill container rotatably coupled to a disk rotatable in a first direction in a second direction opposite to the first direction. Injecting; And rotating the disc and the ball mill container for a predetermined time such that the ball mill ball rubs against the wall surface of the ball mill container so that the ball mill ball itself rotates to apply mechanical shearing force to the aluminum-carbon mixed powders.
- the ratio of the rotational speed of the ball mill vessel to the rotational speed of the disk may be 30% or more and 70% or less of the critical angular velocity ratio.
- the rotation speed of the disk may be 150 rpm or more and 500 rpm or less.
- the sintering of the modified aluminum-carbon mixed powders may include filling the mold with the modified aluminum-carbon mixed powders; And heating the modified aluminum-carbon mixed powders to a temperature of 500 to 700 ° C. while applying a pressure of 10 MPa to 100 MPa to the modified aluminum-carbon mixed powders filled in the mold.
- the manufacturing method of the plate-shaped carbon nanoparticles according to the embodiment of the present invention it is possible to produce a plate-shaped carbon nanoparticles in a short time in a relatively simple process.
- high temperatures are not required to produce plate-shaped carbon nanoparticles, which can result in a lot of energy savings.
- the carbon material is uniformly dispersed, but also the carbon material and aluminum have a laminated structure, thereby producing an aluminum-carbon composite material having excellent mechanical properties.
- the aluminum-carbon composite material is light in weight, has excellent mechanical strength, and is applicable to automobile parts used in the present, and may also be used as a material for aircraft, spacecraft, ships, and the like requiring high strength.
- FIG. 1 is a flowchart illustrating a method of manufacturing a plate-shaped carbon nanoparticles according to an embodiment of the present invention.
- FIG. 2 is a plan view for explaining a ball mill device.
- Figure 3 is a schematic diagram for explaining the force acting on the ball mill ball injected into the ball mill container.
- FIG. 4 is a flowchart illustrating a method of manufacturing plate-shaped carbon nanoparticles according to another embodiment of the present invention.
- FIG. 5 is an electron micrograph of the graphite material without the ball mill process and the electrons of the graphite material subjected to the ball mill process for 0.5 hours, 1 hour, 2 hours, 4 hours and 6 hours, respectively, according to the method shown in FIG. Micrographs.
- FIG. 6 is an X-ray diffraction measurement graph of plate-shaped carbon nanoparticles prepared by the method shown in FIG. 1.
- FIG. 7 is an electron micrograph of the graphite material without the ball mill process and the electrons of the graphite material subjected to the ball mill process for 0.5 hours, 1 hour, 2 hours, 4 hours and 6 hours, respectively, according to the method shown in FIG. Micrographs.
- FIG. 8 is an X-ray diffraction measurement graph of plate-shaped carbon nanoparticles prepared by the method shown in FIG. 4.
- FIG. 9 is an electron micrograph taken after dispersing the plate-shaped carbon nanoparticles prepared on PET in a spin coating method to see the shape of the plate-shaped carbon nanoparticles made by the method shown in FIG. 4.
- FIG. 11 is a flowchart illustrating a method of manufacturing an aluminum-carbon composite material according to an embodiment of the present invention.
- 16 is electron micrographs (1,000 ⁇ ) of modified aluminum-carbon mixed powders after a ball mill process.
- 17 is a photograph for explaining the microstructure of the aluminum material without carbon material and the aluminum-carbon composite material containing 0.05 wt.% Carbon material.
- FIG. 19 shows a sample of aluminum material (RAW), an aluminum-carbon composite material sample (Al-0.1 wt% C, Example 2) having a carbon material content of 0.1 wt.%, And a carbon material content of 0.3 wt.%. It is a graph showing the result of measuring the tensile strength of the aluminum-carbon composite sample (Al-0.3wt% C, Example 3).
- Example 20 is a graph showing the results of measuring the tensile strength of the aluminum-carbon composite materials prepared according to Comparative Example 1, Example 2, Comparative Example 2 and Example 3.
- first and second 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.
- the first component may be referred to as the second component, and similarly, the second component may also be referred to as the first component.
- FIG. 1 is a flowchart illustrating a method for manufacturing a plate-shaped carbon nanoparticles according to an embodiment of the present invention
- Figure 2 is a plan view for explaining the ball mill device
- Figure 3 is applied to the ball mill ball in the ball mill container It is a schematic diagram to explain the power.
- the graphite material and the ball mill ball are added to the ball mill container 130 rotatably coupled to the disk 110.
- the disk 100 may rotate in a first direction X with respect to a first central axis (hereinafter, referred to as an 'orbital axis') positioned at the center 'O' of the disk 100.
- the ball mill container 130 may be coupled to an edge of the disk 110, and may be coupled to the edge of the disc 110 in a first direction based on a second center axis (hereinafter, referred to as a 'rotation axis') located at the center 'A1' of the ball mill container 130. It can rotate in the 2nd direction Y which is the opposite direction to (X). That is, the ball mill container 130 may revolve with respect to the revolution axis by the rotation of the disc 110, and may be rotated by the rotation of the ball mill container 130 itself with respect to the rotation axis. .
- the graphite material may be artificially produced graphite material or natural graphite material.
- the graphite material applied to the present invention is not particularly limited in the shape and size of the plate-like graphite material, the graphite powder in the form of powder, the graphite material in the form of agglomerate, and the like.
- Graphite materials generally have a hexagonal crystal structure and have a structure in which a plurality of layers are laminated.
- the material of the ball mill ball is not particularly limited, but a ball mill ball made of polyimide may be used to effectively apply friction to the graphite material and not excessively damage the graphite material.
- the size of the ball mill ball may be appropriately selected in consideration of the shear force to be applied to the graphite material.
- the ball mill ball may have a diameter of about 3 to 50mm. If the size of the ball mill ball is less than 3mm, there may be a problem that the mass of the ball mill ball is too small so that the mechanical shear force applied to the graphite material is smaller than the required value. On the contrary, when the size of the ball mill ball exceeds 50 mm, excessively large shear force or impact may be applied to the graphite material, thereby causing a problem in that the graphite material is broken.
- the mixing amount of the graphite material and the ball mill ball may be appropriately controlled, it is preferable to mix the graphite material and the ball mill ball so that the weight of the ball mill ball is larger than the weight of the graphite material in order to apply mechanical shear force to the whole graphite material.
- the disk 110 and the ball mill container 130 may be rotated such that the ball mill ball introduced into the ball mill container 130 applies a mechanical shear force to the graphite material.
- the ball mill ball in the ball mill vessel 130 may (i) make motion with another ball mill ball, graphite material or inner wall of the ball mill vessel 130, or (ii) another ball mill ball, graphite material or ball mill vessel.
- the state of contact with the inner wall of the 130 may be a friction motion by the rotation of the ball mill ball, that is, a motion to apply a mechanical shear force.
- the above-mentioned forces are controlled so that the ball mill ball applies mechanical shear force to the graphite material. Control of these forces can be controlled by adjusting the rotational speed of the disk 110 and the ball mill container 130.
- the ball mill ball is subjected to various movements by the action of the forces described above. Specifically, when the rotation speed of the ball mill container 130 is gradually increased while rotating the ball mill container 130 while the disk 110 rotates at a constant speed, the rotation speed of the ball mill container 130 is the first speed. In the first section below, the second section below the first speed and above the second speed, and the third section above the second speed, the ball mill ball may perform different movements.
- the first centrifugal force Fr due to the revolution of the ball mill container 130 acts largely on the ball mill ball.
- the rotational movement is made about the revolution axis at the point farthest from the revolution axis.
- the inner wall of the ball mill container 130 applies a friction force to the ball mill ball by the rotation of the ball mill container 130, the ball mill ball rotates itself.
- the first centrifugal force due to the revolution of the ball mill container 130 and the second centrifugal force due to the rotation of the ball mill container 130 interact with each other.
- the ball mill ball is moved to the space inside the ball mill container 130 to make a motion to collide with the wall surface of the ball mill container.
- the second centrifugal force due to the rotation of the ball mill container 130 is largely actuated so that the ball mill ball is rotated in contact with the wall surface of the ball mill container 130.
- the rotational movement is based on. In this case, since friction between the inner wall of the ball mill container 130 and the ball mill ball hardly occurs, rotation of the ball mill ball itself hardly occurs.
- the ball mill ball is moved in the same manner as the first section to control the rotational speed of the disk 110 and the ball mill container 130 to apply a mechanical shear force to the graphite material.
- the ball mill ball acts on the ball mill ball located closest to the revolution axis in the space inside the ball mill container 130.
- the revolution centrifugal force (Fr) should be greater than the rotation centrifugal force (Fp).
- the orbital centrifugal force (Fr) acting on the ball mill ball located closest to the revolving axis of the ball mill vessel 130 may be represented by Equation 1 below, and the ball mill vessel 130 is located closest to the revolving axis of the ball mill vessel 130.
- the rotating centrifugal force (Fp) acting on the ball mill ball can be expressed by the following Equation 2.
- Equation 1 and 2 'm' represents the weight of the ball mill ball, 'R' represents the distance between the revolution axis and the rotation axis, that is, the revolution radius, 'Lc' ball mill ball at the radius of the ball mill vessel
- w1 is the rotational angular velocity
- w2 is the rotational angular velocity
- 'w2 / w1' is the critical angular velocity ratio 'rc'
- the critical angular velocity ratio 'rc' may be derived from Equations 1 and 2 and may be expressed as Equation 3 below.
- the ratio of the rotation speed to the idle speed can be controlled to be about 30 to 70% of the critical angular velocity ratio.
- the ratio of the rotation speed to the revolution speed (w2 / w1) is the critical angular velocity ratio (rc Should be about 70% or less). That is, when the ratio of the rotational speed to the rotational speed (w2 / w1) exceeds 70% of the critical angular velocity ratio (rc), the influence of the centrifugal force caused by the rotation increases, which causes the ball mill ball to mainly collide with the graphite material.
- the ratio of the rotation speed to the revolution speed (w2 / w1) is less than 30% of the critical angular velocity ratio (rc)
- the rotational speed of the ball mill ball itself is low, the mechanical shear force applied to the graphite material is too small, As a result, the graphite material may not be peeled off.
- the mechanical shear force applied to the graphite material by the ball mill ball is affected by the rotational speed of the ball mill ball itself, which is determined by the rotational speed. That is, as the rotation speed of the ball mill container increases, the rotation speed of the ball mill ball itself increases.
- the mechanical shearing force applied to the graphite material by the ball mill ball is also affected by the pressure at which the ball mill ball presses the graphite material, which is influenced by the revolving speed of the ball mill container 130. That is, as the revolution speed of the ball mill container 130 increases, the pressure for the ball mill ball to pressurize the graphite material increases.
- the revolution speed of the ball mill vessel can be adjusted to be about 150 to 500 rpm.
- the ball mill vessel 130 interior is preferably maintained in a non-oxidizing atmosphere during the ball mill process.
- the inside of the ball mill vessel may be maintained in a non-oxidizing atmosphere by purging argon (Ar) gas after being maintained in a vacuum.
- the prepared plate carbon nanoparticles may be separated and recovered.
- the manufactured plate carbon nanoparticles may have a thickness of about 20 to 1000 nm. In order to manufacture such plate-shaped carbon nanoparticles, when the ball mill process is performed by adding only the graphite material and the ball mill ball to the ball mill vessel, it is preferable to proceed with the ball mill process for about 6 hours or more.
- FIG. 4 is a flowchart illustrating a method of manufacturing plate-shaped carbon nanoparticles according to another embodiment of the present invention.
- the stripping agent is further mixed in addition to the graphite material and the ball mill ball, and these are added to a ball mill container (S210), and the prepared plate carbon nanoparticles are washed.
- S240 is substantially the same as the manufacturing method of the plate-shaped carbon nanoparticles described with reference to FIG. Therefore, hereinafter, the peeling activator and the cleaning step will be mainly described, and the description of the remaining steps will be omitted.
- the release activator can increase the friction between the graphite material and the ball mill ball.
- the release agent may be a surfactant, an organic material, or an inorganic material that can increase the friction between the graphite material and the ball mill ball.
- the surfactant that can be used as the release agent may be selected from SDS, NaDDBs, CTAB, etc.
- the organic material that may be used as the release agent may be selected from sugar, DNA, etc., may be used as the release agent
- the inorganic material may be aluminum.
- the plate-shaped carbon nanoparticles can be produced even if the ball mill process is performed for a short time.
- the plate-shaped carbon nanoparticles may be prepared by performing a ball mill process for about 4 hours or more.
- the plate-shaped carbon nanoparticles produced through the ball mill process may have a small amount of peeling activator. Therefore, the plate-shaped carbon nanoparticles prepared through the ball mill process may be cleaned to remove the stripping activator.
- the plate-shaped carbon nanoparticles prepared through the ball mill process may remove the stripping activator.
- the solvent and the stripping activator may be removed by filtering into a soluble solvent and then filtering. For example, when sugar is used as the peeling activator, the plate-shaped carbon nanoparticles prepared through the ball mill process may be added to distilled water (H20) to dissolve the sugar and then filtered to clean the plate-shaped carbon nanoparticles.
- 5 is an electron micrograph of the graphite material without the ball mill process, and an electron micrograph of the graphite material subjected to the ball mill process for 0.5 hours, 1 hour, 2 hours, 4 hours and 6 hours, respectively, according to the method described above.
- 6 is an X-ray diffraction measurement graph of carbon nanoplates prepared by the above method.
- the graphite material is peeled off as the execution time of the ball mill process is produced plate carbon nanoparticles. Since the graphite material has a hexagonal lamination structure, a peak appears in the crystal plane [002] direction when the X-ray diffraction (XRD) is measured. The higher the peak intensity in the [002] direction, the better the crystallinity of the interlayer bonding structure of the graphite. The lower the peak intensity in the [002] direction, the more the graphite material is peeled off and the poorer the crystallinity of the interlayer bonding structure. it means.
- XRD X-ray diffraction
- the peak intensity in the [002] direction decreases as the ball mill process execution time increases.
- the peak in the [002] direction hardly appears, which is a plate-shaped carbon nanostructure of a structure in which the graphite material is almost completely peeled off so that a single layer or several layers are laminated. It means that the particles are produced.
- 7 is an electron micrograph of the graphite material without the ball mill process, and an electron micrograph of the graphite material subjected to the ball mill process for 0.5 hours, 1 hour, 2 hours, 4 hours and 6 hours, respectively, according to the method described above.
- 8 is an X-ray diffraction measurement graph of the plate-shaped carbon nanoparticles prepared by the above method.
- FIG. 9 is an electron micrograph taken after dispersing the plate-shaped carbon nanoparticles prepared on PET in a spin coating method to see the shape of the plate-shaped carbon nanoparticles made by the above method.
- the carbon nanoplay was photographed at 50,000x and 100,000x, and it was confirmed that plate-shaped carbon nanoparticles having a size of about 100 to 200nm were prepared.
- a plate-shaped nanoparticle was prepared in the same manner as in Example 2 except that the rotation speed was 400 rpm.
- carbon nanoparticles were prepared in the same manner as in Example 2, except that zirconia (ZrO 2 ) balls having a diameter of 5 mm were used as the ball mill balls.
- zirconia (ZrO 2 ) balls having a diameter of 5 mm were used as the ball mill balls.
- the carbon nanoparticles prepared according to Comparative Example 2 is much thicker than the carbon nanoparticles shown in Figure 10 (b). This is due to the interaction between the centrifugal force due to the revolution and the centrifugal force due to the rotation, and the ball mill ball transfers the force mainly due to the collision rather than the mechanical shear force to the graphite material, and as a result, the graphite material was not effectively peeled off.
- the ratio of the rotating angular velocity to the rotating angular velocity in Comparative Example 2 is '400/300'. That is, the ratio of the rotating angular velocity to the rotating angular velocity in Comparative Example 2 corresponds to about 95.2% of the ratio rc of the critical angular velocity.
- the carbon nanoparticles prepared according to Comparative Example 3 have a very high degree of damage compared to the carbon nanoparticles shown in FIG. 10 (b). This is because the ball mill ball density of the polyimide material is 1.43 g / cm 3 , whereas the ball mill ball density of the zirconia material is 6.0 g / cm 3 , and a strong impact is transmitted to the graphite material by the zirconia ball mill.
- FIG. 11 is a flowchart illustrating a method of manufacturing an aluminum-carbon composite material according to an embodiment of the present invention
- FIG. 12 is a plan view illustrating a ball mill device
- FIG. 13 is a ball mill ball inserted into a ball mill container. It is a schematic diagram to explain the power.
- an aluminum-carbon mixed powder may be manufactured by bonding a carbon material to aluminum powders (S110).
- the carbon material may first be dispersed in a solvent, and then the dispersion solution may be sonicated.
- the carbon material at least one or more of graphite plates, graphite fibers, carbon fibers, carbon nanofibers, and carbon nanotubes may be used.
- the carbon material may be a plate-shaped carbon nanoparticles prepared according to the method described above.
- the solvent at least one or more of water, hexane, ethanol, methanol, propanol, ethylene glycol, amine and phenol may be used. Sonication may be performed for about 0.5 to 60 minutes.
- This sonication not only uniformly disperses the carbon material but also can make functional groups including oxygen in the carbon material, for example, hydroxyl groups and the like.
- the aluminum powders may then be added to the sonicated dispersion and sonicated again to precipitate the aluminum-carbon mixed powders.
- the aluminum powders may have a diameter of about 100 nm to 1 mm.
- Aluminum powders may be added so that the carbonaceous material is about 0.1 to 50 wt.% Relative to the weight of the aluminum powders.
- Sonication to precipitate the aluminum-carbon mixed powders may be performed for about 0.5 to 60 minutes. This sonication may induce a bond between the aluminum and the functional group containing oxygen formed in the carbon material.
- the precipitated aluminum-carbon mixed powders can then be separated and dried.
- the modified aluminum-carbon mixed powders may be prepared by applying mechanical shearing force to the aluminum-carbon mixed powders (S120).
- the aluminum-carbon mixed powders and the ball mill ball are placed in a ball mill container 130 rotatably coupled to the disk 110. You can put in.
- the disk 110 may rotate in a first direction X with respect to a first central axis (hereinafter, referred to as an 'idle axis') positioned at the center 'O' of the disk 110.
- the ball mill container 130 may be coupled to an edge of the disk 110, and may be coupled to the edge of the disc 110 in a first direction based on a second center axis (hereinafter, referred to as a 'rotation axis') located at the center 'A1' of the ball mill container 130. It can rotate in the 2nd direction Y which is the opposite direction to (X). That is, the ball mill container 130 may revolve with respect to the revolution axis by the rotation of the disc 110, and may be rotated by the rotation of the ball mill container 130 itself with respect to the rotation axis. .
- the material of the ball mill ball is not particularly limited, but a ball mill ball made of zirconia may be used to effectively apply friction to aluminum-carbon mixed powders.
- the size of the ball mill ball may be appropriately selected in consideration of the shear force to be applied to the aluminum-carbon mixed powders.
- the ball mill ball may have a diameter of about 3 to 50mm.
- the size of the ball mill ball is less than 3 mm, the mass of the ball mill ball is so small that the mechanical shear force applied to the aluminum-carbon mixed powders becomes smaller than the required value, and as a result, the carbon material bonded to the aluminum powder is oriented in a certain direction. Problems may arise that it is not possible or impossible to deform the aluminum powder into a constant plate shape.
- the disk 110 and the ball mill container 130 may be rotated such that the ball mill ball introduced into the ball mill container 130 applies a mechanical shear force to the aluminum-carbon mixed powders.
- the ball mill ball introduced into the ball mill container 130 is rotated by the first centrifugal force Fr and the ball mill container 130 due to the revolution of the ball mill container 130.
- the second centrifugal force Fp is caused to act.
- the first centrifugal force Fr acts in the direction away from the ball axis
- the second centrifugal force Fp acts in the direction away from the axis.
- the magnitude or direction of action of the first and second centrifugal forces Fr and Fp depends on the position of the ball mill ball.
- the ball mill container 130 rotates while the disk 110 rotates, the ball mill ball rotates in the same direction as the ball mill container 130 by the friction force between the ball mill ball and the wall surface of the ball mill container 130.
- the ball mill ball in the ball mill vessel 130 may (i) make motion with another ball mill ball, aluminum-carbon mixed powder or the inner wall of the ball mill vessel 130, or (ii) other ball mill ball, aluminum- In the state of contact with the carbon mixed powder or the inner wall of the ball mill container 130, it is possible to perform a rubbing motion by the rotation of the ball mill ball, that is, to apply a mechanical shear force.
- the force is controlled so that the ball mill ball applies a mechanical shear force to the aluminum-carbon mixed powder while the ball mill ball is in contact with the aluminum-carbon mixed powder. Control of these forces can be controlled by adjusting the rotational speed of the disk 110 and the ball mill container 130.
- the ball mill ball is subjected to various movements by the action of the forces described above. Specifically, when the rotation speed of the ball mill container 130 is gradually increased while rotating the ball mill container 130 while the disk 110 rotates at a constant speed, the rotation speed of the ball mill container 130 is the first speed. In the first section below, the second section below the first speed and above the second speed, and the third section above the second speed, the ball mill ball may perform different movements.
- the first centrifugal force Fr due to the revolution of the ball mill container 130 acts largely on the ball mill ball.
- the rotational movement is made about the revolution axis at the point farthest from the revolution axis.
- the inner wall of the ball mill container 130 applies a friction force to the ball mill ball by the rotation of the ball mill container 130, the ball mill ball rotates itself.
- the first centrifugal force due to the revolution of the ball mill container 130 and the second centrifugal force due to the rotation of the ball mill container 130 interact with each other.
- the ball mill ball is moved to the space inside the ball mill container 130 to make a motion to collide with the wall surface of the ball mill container.
- the second centrifugal force due to the rotation of the ball mill container 130 is largely actuated so that the ball mill ball is rotated in contact with the wall surface of the ball mill container 130.
- the rotational movement is based on. In this case, since friction between the inner wall of the ball mill container 130 and the ball mill ball hardly occurs, rotation of the ball mill ball itself hardly occurs.
- the ball mill ball moves in the same manner as the first section to control the rotational speed of the disk 110 and the ball mill container 130 to apply a mechanical shear force to the aluminum-carbon mixed powder.
- the ball mill ball acts on the ball mill ball located closest to the revolution axis in the space inside the ball mill container 130.
- the revolution centrifugal force (Fr) should be greater than the rotation centrifugal force (Fp).
- the orbital centrifugal force (Fr) acting on the ball mill ball located closest to the revolving axis of the ball mill vessel 130 may be represented by Equation 4 below, and the ball mill vessel 130 is located closest to the revolving axis of the ball mill vessel 130.
- the rotating centrifugal force (Fp) acting on the ball mill ball may be expressed by the following Equation 5.
- Equations 4 and 5 'm' represents the weight of the ball mill ball, 'R' represents the distance between the revolution axis and the rotation axis, that is, the idle radius, 'Lc' ball mill ball at the radius of the ball mill vessel Where w1 is the rotational angular velocity and w2 is the rotational angular velocity.
- 'w2 / w1' is the critical angular velocity ratio 'rc'
- the critical angular velocity ratio 'rc' may be derived from Equations 1 and 2 and expressed as shown in Equation 6 below.
- the ratio of the rotation speed to the revolution speed of the ball mill container 130 may be controlled to be about 30 to 70% of the critical angular velocity ratio.
- the rotational centrifugal force rather than the rotating centrifugal force acts on the ball mill ball.
- w1 should be about 70% or less of the critical angular velocity ratio rc. That is, when the ratio of the rotational speed to the rotational speed (w2 / w1) exceeds 70% of the critical angular velocity ratio (rc), the influence of the centrifugal force due to the rotation increases, so that the ball mill ball is mainly composed of aluminum-carbon mixed powders.
- the mechanical shearing force applied to the aluminum-carbon mixed powder by the ball mill ball is also affected by the pressure at which the ball mill ball presses the aluminum-carbon mixed powder. ) Is affected by the idle speed. That is, as the revolution speed of the ball mill container 130 increases, the pressure for the ball mill ball to pressurize the graphite material increases.
- the rotation speed of the disk in order for the ball mill ball to apply an appropriate size mechanical shear force to the aluminum-carbon mixed powder, can be adjusted to be about 150 to 500 rpm.
- the inside of the ball mill vessel 110 is preferably maintained in an inert gas atmosphere during the ball mill process.
- the ball mill process may be performed for about 5 minutes to 6 hours.
- the aluminum-carbon mixed powders may be deformed to have a shape close to the plate shape, and the carbon material bonded to the aluminum powder surface may be in one direction. Can be aligned to extend.
- the modified aluminum-carbon mixed powders may be sintered.
- the modified aluminum-carbon mixed powders may first be filled into a mold. Subsequently, the modified aluminum-carbon mixed powders filled in the mold were sintered at a temperature of about 500 to 700 ° C. for about 1 minute to about 1 hour while applying a pressure of about 10 MPa to 100 MPa in a vacuum atmosphere to fill the mold. The modified aluminum-carbon mixed powders can be plastically modified. The final aluminum-carbon composite can then be separated from the mold. 14 is a schematic view of a sintering molding machine for sintering the modified aluminum-carbon mixed powders.
- Aluminum powder and carbonaceous material were added to 20 ml of Hexane solvent and sonicated with a horn-type sonicator to prepare aluminum-carbon mixed powders. 2 g of aluminum powder was added, and carbon materials were added by 0.05 wt.% (Example 3), 0.1 wt.% (Example 4) and 0.3 wt.% (Example 5), respectively, based on the weight of the aluminum powder.
- As the aluminum powder an aluminum powder product having a size of 3 ⁇ m purchased from the Japan Institute of High Purity Chemistry was used.
- As a carbon material a nano graphite plate having a size of 100 to 500 nm manufactured by itself was used.
- the modified aluminum-carbon mixed powders were put in a mold, and the upper and lower punches were fixed, compressed using a hydraulic press at a pressure of 50 MPa, and sintered at a temperature of 600 ° C. for about 30 minutes to prepare an aluminum-carbon composite material.
- the atmosphere inside the mold sintering chamber was carried out in a vacuum of 10 -2 torr. 14 is a schematic view of a molding sintering machine.
- FIG. 15 are electron micrographs of ultrasonic samples of aluminum.
- the upper left photograph of FIG. 15 is an electron microscope photograph of a powder composed of only aluminum
- the upper right, lower left and lower right photographs of FIG. 5 each have a concentration of 0.05 wt.% Of the nanographite plate (Example 3 )
- the nanographite plate is uniformly dispersed and bonded to the surface of the aluminum powder.
- FIG. 16 is an electron micrograph (1,000 ⁇ ) of a modified aluminum-carbon mixed powder after the ball mill process.
- FIG. 16 is an electron micrograph of a modified aluminum-carbon mixed powder having a concentration of 0.1 wt.% (Example 4) of the nanographite plate.
- the modified aluminum-carbon mixed powder may be formed by a ball mill ball. It can be seen that the shape is deformed into a plate shape due to the application of mechanical shear force.
- FIG. 17 is a photograph for describing a microstructure of an aluminum material without a carbon material and an aluminum-carbon composite material containing 0.05 wt.% (Example 3). Specifically, the left photograph of FIG. 17 is a microstructure photograph (Olympus, GC51F) of the aluminum material without the carbon material, and the right photograph of FIG. 17 is a microstructure of the aluminum-carbon composite material containing 0.05 wt.% Of the carbon material. Structure picture. Referring to FIG. 17, in the aluminum-carbon composite material prepared according to Example 3 of the present invention, it was confirmed that the aluminum and the carbon material form a laminated structure.
- Figure 18 (a) is a result of the confocal Raman (Witec, CRM 200) measurement of the aluminum-carbon composite material prepared by performing a ball mill process under the condition that the ball mill ball mainly impacts the aluminum-carbon mixed powder
- 18 (b) is a confocal Raman (Witec Co., Ltd.) of an aluminum-carbon composite material manufactured by performing a ball mill process in which a ball mill ball applies mechanical shear force mainly to an aluminum-carbon mixed powder according to Example 3 of the present invention.
- CRM 200 is the measurement result.
- G mode shows a peak inherent in carbon material (G mode) as a yellow dot.
- the aluminum-carbon composite material of FIG. 18B is not only uniformly dispersed in the carbon material as compared with the aluminum-carbon composite material of FIG. 18A, but also forms a laminated structure of aluminum and carbon material. Can be.
- Table 3 shows a sample of aluminum material (RAW), a sample of aluminum-carbon composite material (Al-0.1wt% C, Example 4) having a carbon content of 0.1 wt.%, And a content of 0.3 wt.% Of a carbon material.
- the tensile strength of the aluminum-carbon composite material sample (Al-0.3wt% C, Example 5) was measured.
- FIG. 19 shows a sample of aluminum material (RAW) and aluminum having a content of 0.1 wt.% Aluminum.
- Tensile strength of the carbon composite material sample (Al-0.1wt% C, Example 4) and the aluminum-carbon composite material sample (Al-0.3wt% C, Example 5) having a carbon content of 0.3 wt.% It is a graph showing the result of a measurement.
- the specimen was extruded to ⁇ 2mm and processed into a test piece of 20mm gauge and a diameter of 1.3mm, and the resultant was tensioned at a speed of 0.1mm / min using a universal tensile tester (LLOYD instrument, LR30K). Measured.
- Table 4 below shows the results of measuring the tensile strength of the aluminum-carbon composites prepared according to Comparative Example 4, Example 4, Comparative Example 5 and Example 5,
- Figure 20 is Comparative Example 4,
- Example 4 , Comparative Example 5 and Example 5 is a graph showing the results of measuring the tensile strength of the aluminum-carbon composite materials prepared.
- the tensile strength was increased by 11.55% and the elongation was increased by 28.17% than the aluminum-carbon composite material according to Comparative Example 4.
- the tensile strength was increased by 52.73% and the elongation was increased by 33.92% than the aluminum-carbon composite material according to Comparative Example 5. Therefore, it can be seen that the aluminum-carbon composite material according to the embodiment of the present invention has significantly improved mechanical properties than the aluminum-carbon composite material according to the comparative example.
- the plate-shaped carbon nanoparticles can be manufactured in a large amount in a short time through a relatively simple process.
- high temperatures are not required to produce plate-shaped carbon nanoparticles, which can result in a lot of energy savings.
- the manufacturing method of the aluminum-carbon composite material described above it is possible to manufacture the aluminum-carbon composite material in a large amount through a relatively simple process.
- the aluminum-carbon composite material prepared according to the above-described manufacturing method has a tensile strength strengthened due to the uniformly dispersed and carbon material forming a laminated structure with aluminum. Therefore, when using the aluminum-carbon composite material as a structural material, it is possible to manufacture a lightweight structure.
Abstract
Description
공전축과 자전축 사이의 거리, R | 170 mm |
볼밀 용기 반경, r | 60 mm |
공전 속도 | 300 rpm |
자전 속도 | 200 rpm |
공전축과 자전축 사이의 거리, R | 170 mm |
볼밀 용기 반경, r | 60 mm |
공전 속도 | 300 rpm |
자전 속도 | 200 rpm |
Sample | TensileStress(MPa) | 인장강도증가율(%) | Elongation(%) | 연신률 증가율(%) |
Raw 1(600℃, 0.5h) | 142.76 | - | 8.93 | - |
Al-0.1wt%C(630℃, 0.5h) | 164.30 | 15.09 | 12.92 | 44.68 |
Raw 2(600℃, 3.0h) | 172.85 | - | 11.86 | - |
Al-0.3wt%C(600℃, 3.0h) | 233.07 | 34.84 | 12.24 | 3.20 |
Sample | TensileStress(MPa) | 인장강도증가율(%) | Elongation(%) | 연신률 증가율(%) |
비교예 4 | 147.29 | - | 8.93 | - |
실시예 4 | 164.30 | 11.55 | 12.92 | 28.17 |
비교예 5 | 152.60 | - | 11.86 | - |
실시예 5 | 233.07 | 52.73 | 12.24 | 33.92 |
Claims (17)
- 제1 방향으로 회전 가능한 디스크에 상기 제1 방향과 반대 방향인 제2 방향으로 회전 가능하게 결합된 볼밀 용기에 흑연재료 및 볼밀볼을 투입하는 단계;상기 볼밀볼이 상기 볼밀 용기의 벽면과 마찰하여 상기 볼밀볼 자체가 회전하여 상기 흑연재료에 기계적 전단력을 인가하도록 상기 디스크 및 상기 볼밀 용기를 소정 시간동안 회전시키는 단계; 및상기 흑연 재료로부터 제조된 탄소 나노입자를 분리하는 단계를 포함하는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제1항에 있어서, 상기 흑연 재료는 판 형상의 인조 흑연 재료, 분말 형상의 인조 흑연재료, 덩어리 형상의 인조 흑연재료, 판 형상의 천연 흑연재료, 분말 형상의 천연 흑연 재료 및 덩어리 형상의 천연 흑연재료로 이루어진 그룹으로부터 선택된 적어도 하나 이상을 포함하는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제1항에 있어서, 상기 디스크 및 상기 볼밀 용기를 회전시켜 상기 흑연재료에 기계적 전단력을 인가하는 단계는 비산화 분위기에서 수행되는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제1항에 있어서, 상기 디스크의 회전속도에 대한 상기 볼밀 용기의 회전 속도의 비는 임계 각속도 비의 30% 이상 70% 이하인 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제4항에 있어서, 상기 디스크의 회전 속도는 150 rpm 이상 500 rpm 이하인 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제1항에 있어서, 상기 볼밀 용기에 상기 흑연재료 및 상기 볼밀볼을 투입하는 단계에 있어서, 상기 흑연재료와 상기 볼밀볼 사이의 마찰력을 증가시키는 박리활성제를 더 투입하는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제6항에 있어서, 상기 박리활성제는 상기 흑연재료와 상기 볼밀볼 사이의 마찰력을 증가시킬 수 있는 계면활성제, 유기물질 및 무기물질로 이루어진 그룹으로부터 선택된 적어도 하나를 포함하고,상기 계면활성제는 SDS, NaDDBs 및 CTAB로 이루어진 그룹으로부터 선택된 적어도 하나를 포함하고,상기 유기물질은 설탕(sugar) 및 DNA로 이루어진 그룹으로부터 선택된 적어도 하나를 포함하며,상기 무기물질은 알루미늄을 포함하는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제7항에 있어서, 상기 분리된 판형 탄소 나노입자를 상기 박리 활성제를 용해할 수 있는 용매를 이용하여 세정하는 단계를 더 포함하는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 제7항에 있어서, 상기 디스크 및 상기 볼밀 용기는 4시간 이상 회전되는 것을 특징으로 하는 판형 탄소 나노입자의 제조방법.
- 알루미늄 분말들에 탄소재료를 결합시켜 알루미늄-탄소 혼합 분말을 제조하는 단계;상기 알루미늄-탄소 혼합 분말들에 기계적 전단력을 인가하여 변형 알루미늄-탄소 혼합 분말들을 제조하는 단계; 및상기 변형 알루미늄-탄소 혼합분말들을 소결성형하는 단계를 포함하는 알루미늄-탄소 복합재료의 제조 방법.
- 제10항에 있어서, 상기 알루미늄-탄소 혼합 분말을 제조하는 단계는,용매에 탄소 재료를 혼합한 후 초음파 처리하는 단계; 및상기 초음파 처리된 혼합용액에 알루미늄 분말을 첨가한 후 초음파 처리하는 단계를 포함하는 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
- 제11항에 있어서, 상기 탄소재료는 흑연판, 흑연섬유, 탄소섬유, 탄소나노섬유 및 탄소나노튜브로 이루어진 그룹 중 적어도 하나를 포함하는 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
- 제11항에 있어서, 상기 알루미늄 분말들은 상기 탄소재료가 상기 알루미늄 분말들의 중량에 대해 약 0.1 내지 50 wt.% 정도가 되도록 첨가되는 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
- 제10항에 있어서, 상기 변형 알루미늄-탄소 혼합 분말들을 제조하는 단계는,제1 방향으로 회전 가능한 디스크에 상기 제1 방향과 반대 방향인 제2 방향으로 회전 가능하게 결합된 볼밀 용기에 상기 알루미늄-탄소 혼합 분말들 및 볼밀볼을 투입하는 단계; 및상기 볼밀볼이 상기 볼밀 용기의 벽면과 마찰하여 상기 볼밀볼 자체가 회전하여 상기 알루미늄-탄소 혼합 분말들에 기계적 전단력을 인가하도록 상기 디스크 및 상기 볼밀 용기를 소정 시간동안 회전시키는 단계를 포함하는 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
- 제14항에 있어서, 상기 디스크의 회전속도에 대한 상기 볼밀 용기의 회전 속도의 비는 임계 각속도 비의 30% 이상 70% 이하인 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
- 제15항에 있어서, 상기 디스크의 회전 속도는 150 rpm 이상 500 rpm 이하인 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
- 제14항에 있어서, 상기 변형 알루미늄-탄소 혼합분말들을 소결성형하는 단계는,상기 변형 알루미늄-탄소 혼합 분말들을 금형에 충진하는 단계; 및상기 금형에 충진된 상기 변형 알루미늄-탄소 혼합 분말들에 10MPa 내지 100MPa의 압력을 인가한 상태에서 상기 변형 알루미늄-탄소 혼합 분말들을 500 내지 700℃의 온도로 가열하는 단계를 포함하는 것을 특징으로 하는 알루미늄-탄소 복합재료의 제조 방법.
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EP12805555.5A EP2687485A4 (en) | 2012-03-09 | 2012-03-15 | METHOD FOR PRODUCING PLANAR CARBON NANOPARTICLES, AND PROCESS FOR PRODUCING ALUMINUM / CARBON COMPOSITE MATERIAL USING THE SAME |
CN201280001011.0A CN103562130A (zh) | 2012-03-09 | 2012-03-15 | 板状碳纳米粒子的制造方法及利用其的铝-碳复合材料的制造方法 |
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CN105776196A (zh) * | 2016-03-22 | 2016-07-20 | 中国石油大学(北京) | 一种快速剥离装置及生产石墨烯的方法 |
CN108817381A (zh) * | 2018-05-14 | 2018-11-16 | 兰州交通大学 | 一种低膨胀片状石墨/碳纳米管/铝复合材料的制备方法 |
KR20200050549A (ko) * | 2018-11-02 | 2020-05-12 | 현대자동차주식회사 | 리튬공기전지용 양극, 그 제조방법 및 이를 포함하는 리튬공기전지 |
CN114875261B (zh) * | 2022-06-02 | 2022-10-28 | 哈尔滨工业大学 | 耐蚀铝碳复合材料及其制备方法 |
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KR20090114091A (ko) * | 2008-04-29 | 2009-11-03 | 성균관대학교산학협력단 | 급속 가열 방법을 이용한 알루미늄과 탄소 재료 복합체 및이의 제조방법 |
KR20090075651A (ko) * | 2009-06-08 | 2009-07-08 | 성균관대학교산학협력단 | 알루미늄과 탄소재료 간의 공유결합을 형성하는 방법, 알루미늄과 탄소재료 복합체를 제조하는 방법 및 그 방법에 의하여 제조된 알루미늄과 탄소재료 복합체 |
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JP2014519461A (ja) | 2014-08-14 |
EP2687485A4 (en) | 2015-12-16 |
EP2687485A1 (en) | 2014-01-22 |
CN103562130A (zh) | 2014-02-05 |
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