KR101718412B1 - Thin-film coating apparatus and coating method for graphite surface treatment - Google Patents

Thin-film coating apparatus and coating method for graphite surface treatment Download PDF

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Publication number
KR101718412B1
KR101718412B1 KR1020150049174A KR20150049174A KR101718412B1 KR 101718412 B1 KR101718412 B1 KR 101718412B1 KR 1020150049174 A KR1020150049174 A KR 1020150049174A KR 20150049174 A KR20150049174 A KR 20150049174A KR 101718412 B1 KR101718412 B1 KR 101718412B1
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South Korea
Prior art keywords
vacuum chamber
graphite
vacuum
silicon
crucible
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KR1020150049174A
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Korean (ko)
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KR20160120403A (en
Inventor
황정태
박장식
안상철
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(주)제너코트
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/354—Introduction of auxiliary energy into the plasma
    • C23C14/357—Microwaves, e.g. electron cyclotron resonance enhanced sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635—Carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50—Substrate holders

Abstract

The present invention relates to a thin film coating apparatus for surface treatment of graphite, which comprises a water cooling type cooling plate for preventing cooling by rotating cooling water, a shield plate for preventing adherence of silicon evaporation particles, and a vacuum A chamber; A jig mounting a graphite substrate on an upper portion of the vacuum chamber; A crucible for containing a silicon (Si) material in a lower end of the vacuum chamber; A microwave generator installed to ionize the silicon particles evaporated in the vacuum chamber; A pressure measuring unit for measuring a degree of vacuum in the vacuum chamber through a pressure sensor; The vacuum chamber is filled with a gas selected from the group consisting of SiCl 2 , SiH 2 , tetramethyldisiloxane (TMDSO), and hexamethyldisiloxane (HMDSO) and CH 4 , C 3 H 4 , CCl 4 A gas bomb that supplies any one of the gases; And an exhaust pump for evacuating the vacuum chamber to a vacuum.

Description

[0001] The present invention relates to a thin film coating apparatus and method for surface treatment of graphite,

The present invention relates to a coating apparatus and a method for treating a surface of a graphite substrate with a multilayer thin film.

(Si) gas and carbon (C) gas are introduced into the reactor using a chemical vapor deposition (CVD) apparatus in order to improve the oxidation resistance and abrasion resistance of graphite and to suppress the generation of dust. A chemical reaction was generated in the reaction furnace to deposit on the graphite surface.

However, since the conventional chemical vapor deposition apparatus can not completely remove particles generated from the surface and pores of the graphite mold used for glass molding, defects due to dent or the like occur on the glass surface, and the life of the graphite mold is short .

Korean Patent No. 10-0760336 (2007.09.13)

In order to solve the above problems, an object of the present invention is to prevent particles from being coated on a graphite surface with a multilayer thin film of SiC And to provide a thin film coating apparatus and method for surface treatment of graphite which improves the lifetime of glass molding.

According to an aspect of the present invention, there is provided a thin film coating apparatus for surface treatment of graphite, comprising: a water-cooled cooling plate for preventing cooling by rotating cooling water; a shield plate for preventing adhesion of silicon evaporation particles; A vacuum chamber made of a heater for ensuring a uniform temperature; A jig mounting a graphite substrate on an upper portion of the vacuum chamber; A crucible for containing a silicon (Si) material in a lower end of the vacuum chamber; A microwave generator installed to ionize the silicon particles evaporated in the vacuum chamber; A pressure measuring unit for measuring a degree of vacuum in the vacuum chamber through a pressure sensor; A gas for supplying any one gas of SiCl 2 , SiH 2 , tetramethyldisiloxane (TMDSO), or hexamethyldisiloxane (HMDSO) and CH 4 , C 3 H 4 or CCl 4 to the vacuum chamber bomb; And an exhaust pump for evacuating the vacuum chamber to a vacuum.

In the coating apparatus of the present invention, the heater is a heater rod or a cylinder.

A thin film coating method for surface treatment of graphite according to an embodiment of the present invention is characterized in that a graphite substrate is mounted on a jig at the upper end of a vacuum chamber and a crucible containing a silicon (Si) material is installed at the lower end of the vacuum chamber ; Evacuating a vacuum of the vacuum chamber to 10 -2 to 10 -7 torr and maintaining a temperature of 1200 to 1700 ° C inside the vacuum chamber; Heating the crucible to ionize the evaporated silicon particles and / or the evaporated silicon particles with a microwave generator, and forming a first SiC layer by reacting with the carbon (C) in the surface of the graphite substrate and the carbon in the pores ; And forming a second SiC layer on the first SiC layer by a chemical vapor deposition method.

In the coating method of the present invention, the second SiC layer may be formed of any one of SiCl 2 , SiH 2 , tetramethyldisiloxane (TMDSO), and hexamethyldisiloxane (HMDSO) and CH 4 , C 3 H 4 , CCl 4 The gas is formed by using any one of the following gases.

According to this aspect, the present invention forms a multilayer thin film of SiC on the surface of a graphite mold for glass molding, thereby improving the durability and surface roughness of the mold, thereby increasing the lifetime of the graphite mold and preventing defects such as dents caused by glass molding .

1 is a view showing a thin film coating apparatus for surface treatment of graphite according to an embodiment of the present invention.
2A to 2C are cross-sectional views of graphite surface-treated by a thin film coating method for surface treatment of graphite according to an embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.

Hereinafter, a thin film coating apparatus and method for surface treatment of graphite according to an embodiment of the present invention will be described with reference to the accompanying drawings.

1 is a view showing a thin film coating apparatus for surface treatment of graphite according to an embodiment of the present invention.

Referring to FIG. 1, a thin film coating apparatus for surface treatment of graphite according to the present invention includes a water cooling type cooling plate 10 for preventing cooling water from being heated to rotate, and a vaporized silicon (Si) A vacuum chamber 100 composed of a shield plate 11 made of graphite felt to prevent adhesion to the inner wall of the vacuum chamber 100 and eight or 12 heaters (16).
Here, the heater 16 may be a heater rod or a cylinder (not shown).
A graphite substrate 13 as a product to be coated is mounted on a jig (not shown) on the upper part of the inside of the vacuum chamber 100 and a crucible 14 ).
The degree of vacuum in the vacuum chamber 100 is measured by a pressure gauge 20 through a pressure sensor 17. Here, the pressure sensor 17 is installed between the vacuum chamber 100 and the shield plate 11.
A microwave generator (21) is installed in the vacuum chamber (100) to activate the evaporation particles of silicon (15) by ionization. At this time, the microwave generator 21 supplies a microwave power source 22 of 0.5 to 50 Kw to generate a frequency of 2.45 GHz.
The vacuum chamber 100 evacuates to a vacuum through an exhaust pump 19.
The gas of the gas cylinder 18 is injected into the vacuum chamber 100 through a gas pipe of SUS material connected to the graphite gas pipe 12 having heat resistance.
2A to 2C are cross-sectional views of graphite surface-treated by a thin film coating method for surface treatment of graphite according to an embodiment of the present invention.

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2A, a graphite substrate 13 is mounted on a jig at an upper end of the vacuum chamber 100 and a crucible 14 containing a silicon (Si) 15 material is disposed at the lower end of the vacuum chamber 100 Install it. Here, the graphite substrate 13 generally includes a pore 30.
Subsequently, the vacuum of the vacuum chamber 100 is evacuated to 10 -2 to 10 -7 torr by the exhaust pump 19, and the temperature of the chamber interior 100 is maintained at 1200 to 1700 ° C.

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Subsequently, the temperature of the crucible 14 is raised to 1600 ° C to evaporate the silicon (Si) 15 material contained in the crucible 14. Here, the silicon (15) material starts to melt at 1410 캜 and evaporates.

At this time, the vaporized silicon (15) particles react with the carbon (C) in the surface of the graphite substrate 13 and the pores to form the first SiC layer 40 as shown in FIG.

The vaporized silicon 15 particles are ionized by the microwave generator 21 according to sample preparation conditions and reacted with the carbon (C) in the surface of the graphite substrate 13 and the pores to form a first SiC layer 40 are formed.

In this case, the evaporation particles of the silicon (15) react with the graphite substrate (13) to form the first SiC layer (40) because of the reactivity, so that the carbon (C) on the surface of the graphite substrate (13) The thickness of the SiC thin film on the surface of the graphite substrate 13 is 5 占 퐉 or less. Therefore, the first SiC layer 40 can not be formed entirely on the graphite surface and the pores by the silicon (Si) evaporated particles.

Finally, the graphite substrate 13 surface and coating the pores, and in order to improve the surface roughness as the surface planarization of claim 1 SiC layer 40, the upper SiCl 2, SiH 2, a chemical vapor deposition (CVD) method for the tetramethyl- The second SiC layer 41 is formed as shown in FIG. 2B by using any one gas of disiloxane (TMDSO) and hexamethyldisiloxane (HMDSO) and CH 4 , C 3 H 4 and CCl 4 do.

By the reactivity of the particles of the present invention and the chemical vapor deposition method, SiC is formed on the surface and pores of the graphite, dust generation can be prevented and the durability of the graphite mold can be improved

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, It belongs to the scope of right.

10: water cooled cooling plate 11: shield plate
12: graphite gas pipe 13: graphite substrate
14: Crucible 15: Silicon
16: heater 17: pressure sensor
18: Gas cylinder 19: Exhaust pump
20: Pressure meter 21: Microwave generator
22: microwave power source 30: porosity
40: first SiC layer 41: second SiC layer

Claims (4)

A thin film coating apparatus for treating SiC on a graphite surface,
A cooling chamber composed of a water-cooled cooling plate for rotating the cooling water to prevent heating, a shield plate for preventing deposition of silicon evaporation particles, and a heater for securing a uniform temperature;
A jig mounting a graphite substrate on an upper portion of the vacuum chamber;
A crucible for containing a silicon (Si) material in a lower end of the vacuum chamber;
A microwave generator installed to ionize the silicon particles evaporated in the vacuum chamber;
A pressure measuring unit for measuring a degree of vacuum in the vacuum chamber through a pressure sensor;
A gas for supplying any one gas of SiCl 2 , SiH 2 , tetramethyldisiloxane (TMDSO), or hexamethyldisiloxane (HMDSO) and CH 4 , C 3 H 4 or CCl 4 to the vacuum chamber bomb; And
And an exhaust pump for evacuating the vacuum chamber to a vacuum state. The method according to claim 1,
Wherein the heater is a heater rod or a cylinder. A thin film coating method for treating SiC on a graphite surface,
Installing a graphite substrate on the top of the inside of the vacuum chamber and installing a crucible containing a silicon (Si) material in the bottom of the vacuum chamber;
Evacuating a vacuum of the vacuum chamber to 10 -2 to 10 -7 torr and maintaining a temperature of 1200 to 1700 ° C inside the vacuum chamber;
Heating the crucible to ionize the evaporated silicon particles and / or the evaporated silicon particles with a microwave generator, and forming a first SiC layer by reacting with the carbon (C) in the surface of the graphite substrate and the carbon in the pores ; And
And forming a second SiC layer on the first SiC layer by a chemical vapor deposition method. The method of claim 3,
The second SiC layer may be formed of any one of SiCl 2 , SiH 2 , tetramethyldisiloxane (TMDSO), and hexamethyldisiloxane (HMDSO) and one of CH 4 , C 3 H 4 and CCl 4 Wherein the coating layer is formed on the surface of the graphite.
KR1020150049174A 2015-04-07 2015-04-07 Thin-film coating apparatus and coating method for graphite surface treatment KR101718412B1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101947485B1 (en) 2017-07-06 2019-02-13 김석진 Method for SiC Coating of Graphite Base Substrate
KR102053160B1 (en) * 2018-01-10 2019-12-06 (주)새한나노텍 Manufacturing method of carbon mold impregnating silicone
KR102084841B1 (en) 2018-03-22 2020-03-09 주식회사 티엠비 Surface treating method for controlling surface roughness of carbon material
CN108588671B (en) * 2018-05-22 2020-03-24 桑尼光电技术（安徽）有限公司 Multifunctional vacuum coating machine
CN116695089B (en) * 2023-08-09 2023-10-24 通威微电子有限公司 Relay ring tantalum carbide coating device and method

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KR20020084538A (en) * 2001-05-02 2002-11-09 김명한 Brown rice germination method and brown rice germination device
KR100760336B1 (en) 2006-06-22 2007-09-20 (주)글로벌코센테크 Method for improving graphite's surface property using chemical vapor response
US8372489B2 (en) * 2007-09-28 2013-02-12 Tel Epion Inc. Method for directional deposition using a gas cluster ion beam
KR101272844B1 (en) * 2011-01-31 2013-06-11 한국기초과학지원연구원 Device and mothod for SiC coating on graphite pebble
KR101459187B1 (en) * 2012-08-24 2014-11-07 한국기초과학지원연구원 CVD equipments for the uniformity coating of spherical form

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