KR101670780B1 - Diamond-graphite hybrid material, method of manufacturing the same, and heat transfer sheet including the diamond-graphite hybrid material - Google Patents
Diamond-graphite hybrid material, method of manufacturing the same, and heat transfer sheet including the diamond-graphite hybrid material Download PDFInfo
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- KR101670780B1 KR101670780B1 KR1020150060228A KR20150060228A KR101670780B1 KR 101670780 B1 KR101670780 B1 KR 101670780B1 KR 1020150060228 A KR1020150060228 A KR 1020150060228A KR 20150060228 A KR20150060228 A KR 20150060228A KR 101670780 B1 KR101670780 B1 KR 101670780B1
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- C01B31/06—
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- C01B31/04—
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3732—Diamonds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
In a diamond-graphite hybrid material, a method of producing the same, and a heat transfer sheet comprising the diamond-graphite hybrid material, the diamond-graphite hybrid material includes diamond particles and graphite grown on the surface of the diamond particles to cover at least a part of the surface of the diamond particles.
Description
The present invention relates to a diamond-graphite hybrid material, a method for producing the diamond-graphite hybrid material, and a heat transfer sheet comprising the diamond-graphite hybrid material.
Graphite (graphite) is a material belonging to the hexagonal system and composed of almost pure carbon. Graphite is a hexagonal flaky crystal, which is a good conductor for heat and electricity. It has a very low coefficient of friction and is widely used in various industries such as electrodes, carbon rods, refractories, gamma materials, pencils, carbon steel raw materials, have. In recent years, as the heat dissipation increases due to the high integration of electronic devices, and when the electronic devices are damaged, a graphite sheet is applied to electronic devices to induce heat dissipation and thermal diffusion. The graphite sheet is obtained by processing a graphite flake into a sheet, and is very economical because of its excellent mass productivity. In addition, it has a characteristic of rapidly diffusing heat in the in-plane direction, and has conductivity and also has electromagnetic wave shielding performance.
However, the graphite sheet has a disadvantage in that the heat transfer characteristic in the in-plane direction is very good, but the heat transfer characteristic in the vertical direction is low.
On the other hand, as a carbon-based material, diamond has an excellent electrical conductivity, but has an excellent heat conductivity and an isotropic material, and thus has the same characteristics in horizontal and vertical directions. Therefore, nano- or micro- have. At this time, the diamond is used as a filler between other materials, but there is a problem that the heat contact property is deteriorated due to thermal contact resistance.
It is an object of the present invention to provide a novel diamond-graphite hybrid material having an electrically conductive and thermally conductive and mechanically stable structure.
Another object of the present invention is to provide a method for producing the diamond-graphite hybrid material.
Another object of the present invention is to provide a heat transfer sheet comprising the diamond-graphite hybrid material.
A diamond-graphite hybrid material for one purpose of the present invention comprises diamond particles and graphite chemically grown on the surface of the diamond particles to cover at least a portion of the surface of the diamond particles.
In one embodiment, the carbon atoms of the graphite surface may be chemically bonded to the carbon atoms of the diamond particle surface.
In one embodiment, the size of the diamond particles may be between 1 nm and 100 탆.
In one embodiment, the thickness of the graphite may range from 3.5 A to 500 nm.
A method of manufacturing a diamond-graphite hybrid material for another purpose of the present invention includes the steps of cleaning diamond particles by removing impurities on the surface of the diamond particles using hydrogen gas, and supplying carbon source gas to the cleaned diamond particles, And growing graphite on the surface of the diamond particles by vapor deposition.
In one embodiment, the carbon source gas may be a hydrocarbon represented by the following Chemical Formula 1, Chemical Formula 2 or Chemical Formula 3.
≪
≪ Formula 2 > C n H 2n + 2
≪
In the general formulas (1) and (3), n independently represents 2 or more natural numbers, and n in the general formula (2) represents a natural number of 1 or more.
In one embodiment, the step of growing the graphite may be carried out using a carbon source gas containing at least one of methane gas, acetylene gas and ethylene gas under a hydrogen gas atmosphere.
In one embodiment, the step of growing the graphite may be performed at 800 to 1,500 占 폚.
In one embodiment, the step of growing the graphite may be performed at a pressure of 10 mTorr to 500 Torr.
In one embodiment, the size of the diamond particles may be between 1 nm and 100 탆.
A heat transfer sheet for another purpose of the present invention comprises a diamond-graphite hybrid material comprising graphite grown on the surface of the diamond particles to cover at least a portion of the surface of the diamond particles.
In one embodiment, the heat transfer sheet further comprises at least one of graphite flake and graphene, wherein at least a portion of the diamond-graphite hybrid material is interposed between graphite flake yarn, graphene or between graphene flake and graphene. .
According to the diamond-graphite hybrid material of the present invention, the method for producing the diamond-graphite hybrid material, and the heat transfer sheet comprising the same, the diamond-graphite hybrid material including graphite grown on the surface of the diamond particles uses diamond particles having no electric conductivity, And has a structure that has electrical conductivity and thermal conductivity by being hybridized and is mechanically stable.
Such a novel material can be easily formed by a simple process using a chemical vapor deposition method and the heat transfer sheet can have excellent heat radiation and thermal diffusion function and electromagnetic shielding ability by including a diamond-graphite hybrid material as a filler. In particular, the diamond-graphite hybrid material can improve the heat transfer characteristics in the in-plane direction as well as the perpendicular direction intersecting the in-plane direction by lowering the thermal contact resistance in the heat transfer sheet.
1 is a flowchart illustrating a method of manufacturing a diamond-graphite hybrid material according to an embodiment of the present invention.
FIGS. 2A and 2B are views for explaining heat transfer paths of a conventional heat transfer sheet and a heat transfer sheet according to the present invention.
3 is a photograph of
4 is a photograph of Comparative Samples 2-4 and Samples 2-4.
5 is a Raman analysis graph of
Figs. 6 and 7 are TEM photographs of
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. The present invention is capable of various modifications and various forms, and specific embodiments are illustrated in the drawings and described in detail in the text. It is to be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but on the contrary, is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. Like reference numerals are used for like elements in describing each drawing.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In the present application, the term "comprises" or "having ", etc. is intended to specify that there is a feature, step, operation, element, part or combination thereof described in the specification, , &Quot; an ", " an ", " an "
Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.
Diamond-Graphite Hybrid Materials and Manufacturing Method
The diamond-graphite hybrid material according to the present invention comprises diamond particles and graphite grown on the surface of the diamond particles.
Diamond particles are equiaxed carbon crystals composed of carbon. The diamond particles may be those in which the diamond matrix is prepared by grinding or explosive method (Explosive) or grown from a diamond seed. The size of the diamond particles is not limited, but may preferably be 1 nm to 100 탆. Here, the size of the diamond particles may mean a maximum value among a plurality of values defined as a distance between two points at which a virtual straight line passing through the center of gravity of the particle crosses the surface of the diamond particle.
Diamond has low electrical conductivity, but uses nanoscale or micro-sized diamond as a heat transfer material due to its very high thermal conductivity, but its thermal contact resistance is low due to its very high thermal contact resistance when used as a filler between other materials.
The graphite may be formed to cover at least a part of the surface of the diamond particles to lower the heat transfer characteristics of the diamond particles and to enhance the electrical conductivity. Graphite is a hexagonal system carbonaceous material composed of carbon.
The graphite may be formed on a part of the diamond particle surface and may be formed so as to cover the entire surface of the diamond particle. The graphite may be formed to a thickness of 500 nm or less from the surface of the diamond particles. At this time, the graphite may have a thickness of 3.5 ANGSTROM or more. When the thickness of the graphite is less than 3.5 ANGSTROM, graphite is formed on the surface of the diamond particles hardly, and if the graphite is more than 500 ANGSTROM, the surface is covered with the amorphous carbon structure, and the thermal conductivity and electrical conductivity may be lowered.
Graphite can be formed on the surface of the diamond particles by chemically bonding the carbon atoms of the graphite to the carbon atoms of the diamond particles.
The diamond has excellent thermal conductivity, high strength and low electrical conductivity, but the diamond-graphite hybrid material according to the present invention has excellent thermal conductivity and electric conductivity and can be widely used in various fields.
1 is a flowchart illustrating a method of manufacturing a diamond-graphite hybrid material according to an embodiment of the present invention.
Referring to FIG. 1, first, the surface of the diamond particles is cleaned (step S100).
In the cleaning process, impurities and / or amorphous carbon structures present on the surface of the diamond particles can be removed. The cleaning process may be performed under a hydrogen gas atmosphere. At this time, the cleaning process can be performed at a high temperature of 800 DEG C or more. For example, it can be carried out at 1,000 ° C to 1,100 ° C.
After the cleaning step, graphite is grown on the surface of the diamond particles (step S200).
The diamond particles may be provided with a carbon source gas under a hydrogen gas atmosphere to form graphite through chemical vapor deposition (CVD).
As the carbon source gas, hydrocarbons (C n H 2n , C n H 2n + 2, C n H 2n-2 ) which are generally composed of carbon and hydrogen may be used. For example, a gas such as methane (CH 4 ), ethylene (C 2 H 4 ), acetylene (C 2 H 2 ) or the like can be used. In addition to the hydrocarbon, gas including carbon such as CO and CO 2 can be used.
Providing a carbon source gas to the diamond particles may form a seed comprising carbon atoms chemically bonded to the carbon atoms of the diamond particles on the surface of the diamond particles. Subsequently, by providing a carbon source gas, carbon can be grown into hexagonal crystal from the seed to form graphite.
In one embodiment, when methane gas is used as the carbon source gas in the step of growing the graphite, the ratio of hydrogen gas to methane gas may be set at 1: 1 to 1:30. Alternatively, when acetylene gas is used as the carbon source gas, the ratio of the hydrogen gas to the acetylene gas may be 1: 1 to 1:10.
On the other hand, the step of growing the graphite can be carried out in a temperature range of 800 ° C to 1500 ° C. The pressure condition may also be between 10 mTorr and 500 Torr.
After the graphite is formed, an additional cooling step can be performed.
Through such a process, a diamond-graphite hybrid material in which diamond and graphite are chemically bonded is produced.
Heat transfer sheet
The heat transfer sheet according to the present invention comprises a diamond-graphite hybrid material.
The diamond-graphite hybrid material is substantially the same as that described above, including diamond particles and graphite grown on the surface of the diamond particles. Therefore, redundant detailed description will be omitted.
The heat transfer sheet comprises graphite flakes and / or graphene with good heat transfer properties in the in-plane direction. The diamond-graphite hybrid material is interposed between graphite flakes and graphene or between graphene flakes and graphene to improve heat transfer characteristics in a direction perpendicular to the in-plane direction and the in-plane direction of the heat transfer sheet.
That is, the diamond-graphite hybrid material may become a filler of a heat transfer sheet comprising graphite flakes and / or graphene to connect the graphite flakes and / or graphene in a direction perpendicular to the in-plane direction and in- Therefore, the heat transfer characteristic in the in-plane direction and the perpendicular direction can be improved.
The heat transfer sheet according to the present invention can be produced by adding a diamond-graphite hybrid material to graphite flakes and / or graphenes, dispersing them, drying and pressing them. At this time, graphite flakes can be produced by expanding graphite impression.
FIGS. 2A and 2B are views for explaining heat transfer paths of a conventional heat transfer sheet and a heat transfer sheet according to the present invention.
FIG. 2A illustrates a heat transfer path in a conventional heat transfer sheet, and FIG. 2B illustrates a heat transfer path of the heat transfer sheet according to the present invention.
The graphical representation of the diamond-graphite hybrid material in dotted form in FIG. 2b is graphite flake and / or graphene.
In each of Figs. 2A and 2B, the size of the arrow indicates the amount of heat.
Referring to FIG. 2A, in a conventional heat transfer sheet, that is, a heat transfer sheet including graphite flake and / or graphen, heat transfer occurs in the in-plane direction in the horizontal direction and heat transfer occurs in the vertical direction crossing the in- It happens.
On the other hand, referring to FIG. 2B, in the case of the heat transfer sheet according to the present invention, the diamond-graphite hybrid material is further included as a mediator by further including the diamond-graphite hybrid material, thereby improving the heat transfer characteristic. The graphite flakes contained in the heat transfer sheet can be artificial graphite or the heat transfer properties of the heat transfer sheet in the vertical direction can be improved due to the addition of the diamond-graphite hybrid material regardless of the natural graphite.
Particularly, when the heat transfer sheet uses natural graphite, the diamond-graphite hybrid material is dispersed among the graphite flakes to mediate them while lowering the thermal contact resistance of the graphite flakes, so that the heat transfer property in both the in- Can be improved.
Hereinafter, a diamond-graphite hybrid material according to the present invention and a method for producing the diamond-graphite hybrid material will be described in detail with reference to specific experimental examples.
Preparation of
A diamond powder composed of diamond particles having a size of 500 nm was prepared. Hydrogen gas was added to the diamond powder to remove surface impurities and amorphous carbon structure of the diamond particles.
Then, graphite was formed on the surface of the diamond particles by chemical vapor deposition (CVD) using acetylene gas as a carbon source gas in a hydrogen gas atmosphere. At this time, the process pressure was 1 Torr, and the ratio of acetylene gas to hydrogen gas flow rate was 5: 1. This process was performed at 1,050 占 폚 for about 60 minutes to synthesize graphite and perform a cooling process for 35 minutes to prepare
Appearance evaluation of
A diamond powder composed of diamond particles having a size of 500 nm was prepared as a
3 is a photograph of
3, (a) is a photograph of
Referring to FIG. 3, it can be visually confirmed that
Preparation of Samples 2 to 4
Sample 2 was prepared by substantially the same method as that of
Appearance evaluation of Comparative Samples 2 to 4 and Samples 2 to 4
Diamond powders composed of diamond particles having sizes of 1 mu m, 5 mu m, and 70 mu m, respectively, were prepared as comparative samples 2 to 4, respectively, and the appearance was compared with the samples 2 to 4 through photographs.
4 is a photograph of Comparative Samples 2-4 and Samples 2-4.
In FIG. 4, (a) is a photograph of Comparative Samples 2 to 4 and (b) is a photograph of Samples 2 to 4.
Referring to FIG. 4, it can be seen that Comparative Sample 2 before forming graphite shows light gray,
Raman analysis
For each of
5 is a Raman analysis graph of
5, (a) is a graph of
Referring to FIG. 5, it can be seen that in both (a) and (b), a D peak appears at about 1,360 cm -1 and a G peak appears at about 1,580 cm -1 in (b). It can be seen that the D peak appears by the presence of the diamond having the sp 3 bond structure of the carbon-carbon and the sp 2 bond structure of the carbon-carbon exists by the presence of the G peak. That is, it can be confirmed that graphite is formed by the G peak of the Raman analysis graph.
TEM analysis
Transmission Electron Microscope (TEM) analysis was performed for each of
Figs. 6 and 7 are TEM photographs of
FIG. 6 is an enlarged TEM photograph of the surface of the diamond particles, and FIG. 7 is a TEM image of the graphite of FIG. 6 further enlarged.
Referring to FIG. 6, graphite having a thickness of about 20 nm is formed on the surface of the diamond particles. As shown in FIGS. 6 and 7, it can be seen that the graphite is formed by stacking layers of several layers. The distance between the layers is calculated to be about 3.36 Å. That is, based on the theory that the interlayer spacing of the graphite is 3.35 Å, it can be confirmed that the carbon structure having an actual interlayer distance of 3.36 Å is graphite.
Characteristic evaluation: Conductivity
For each of
As a result, it was confirmed that the electric resistance was not measured in the
Preparation and characterization of heat transfer sheet
The graphite flakes were expanded by expanding the inner graphite, and the
Also, the
As a conventional heat transfer sheet for comparison, except for
For each of the prepared Examples 1 and 2 and Comparative Examples for comparison, the thermal conductivity was measured using a LFA 467 instrument of NETZCH (company name). The results are shown in Table 1.
Referring to Table 1, the thermal conductivity of Comparative Example is only 372 W / mK, whereas the thermal conductivity of Example 1 according to the present invention is 433 W / mK and the thermal conductivity of Example 2 is 455 W / mK It can be confirmed that the thermal conductivity is remarkably increased as compared with the example.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the present invention as defined by the following claims. It can be understood that it is possible.
Claims (12)
And graphite grown on the surface of the diamond particles to cover at least a portion of the surface of the diamond particles,
Wherein the graphite grown on the surface of the diamond particles has a hexagonal system structure in which a plurality of carbon layers are laminated outward from the surface of the diamond particles.
Diamond-graphite hybrid material.
Characterized in that carbon atoms on the surface of the graphite are chemically bonded to the carbon atoms on the surface of the diamond particles.
Diamond-graphite hybrid material.
Characterized in that the size of the diamond particles is from 1 nm to 100 탆.
Diamond-graphite hybrid material.
Wherein the thickness of the graphite is 3.5 ANGSTROM or more and 500 nm or less.
Diamond-graphite hybrid material.
And providing carbon source gas to the cleaned diamond particles under a hydrogen gas atmosphere to grow graphite on the surface of diamond particles at 1,000 to 1,100 ° C by chemical vapor deposition,
Wherein the graphite grown on the surface of the diamond particles has a hexagonal system structure in which a plurality of carbon layers are laminated outward from the surface of the diamond particles.
A process for producing a diamond-graphite hybrid material.
The carbon source gas
Is a hydrocarbon represented by the following formula (1), (2) or (3)
A method for producing a diamond-graphite hybrid material;
≪ Formula 1 > C n H 2n
≪ Formula 2 > C n H 2n + 2
≪ Formula 3 > C n H 2n-2
In the general formulas (1) and (3), n independently represents 2 or more natural numbers, and n in the general formula (2) represents a natural number of 1 or more.
The carbon source gas
And at least one of methane gas, acetylene gas, and ethylene gas.
A process for producing a diamond-graphite hybrid material.
The step of growing the graphite
Is performed at a pressure of 10 mTorr to 500 Torr.
A process for producing a diamond-graphite hybrid material.
Characterized in that the size of the diamond particles is from 1 nm to 100 탆.
A process for producing a diamond-graphite hybrid material.
Heat transfer sheet.
Further comprising at least one of graphite flake and graphene,
Characterized in that at least a portion of the diamond-graphite hybrid material is interposed between graphite flake yarn, graphene or between graphene flake and graphene.
Heat transfer sheet.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20210099902A (en) * | 2020-02-05 | 2021-08-13 | 한국과학기술연구원 | Method of manufacturing and modularizing assembled thermal management material based on diamond-graphene hybrid structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004363432A (en) | 2003-06-06 | 2004-12-24 | Matsushita Electric Ind Co Ltd | Heat conduction sheet and heat dissipation structure employing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004363432A (en) | 2003-06-06 | 2004-12-24 | Matsushita Electric Ind Co Ltd | Heat conduction sheet and heat dissipation structure employing same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210099902A (en) * | 2020-02-05 | 2021-08-13 | 한국과학기술연구원 | Method of manufacturing and modularizing assembled thermal management material based on diamond-graphene hybrid structure |
| KR102333477B1 (en) | 2020-02-05 | 2021-12-02 | 한국과학기술연구원 | Method of manufacturing and modularizing assembled thermal management material based on diamond-graphene hybrid structure |
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