KR20170067274A - Regeneration method of ceramic member for recycle - Google Patents
Regeneration method of ceramic member for recycle Download PDFInfo
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- KR20170067274A KR20170067274A KR1020150173750A KR20150173750A KR20170067274A KR 20170067274 A KR20170067274 A KR 20170067274A KR 1020150173750 A KR1020150173750 A KR 1020150173750A KR 20150173750 A KR20150173750 A KR 20150173750A KR 20170067274 A KR20170067274 A KR 20170067274A
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- ceramic member
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- 239000000919 ceramic Substances 0.000 title claims abstract description 131
- 238000011069 regeneration method Methods 0.000 title claims 3
- 239000000203 mixture Substances 0.000 claims abstract description 69
- 238000000576 coating method Methods 0.000 claims abstract description 46
- 239000004065 semiconductor Substances 0.000 claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011247 coating layer Substances 0.000 claims abstract description 25
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 23
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000001172 regenerating effect Effects 0.000 claims abstract description 19
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims abstract description 19
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008119 colloidal silica Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 14
- -1 yttrium alkoxide Chemical class 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 238000010943 off-gassing Methods 0.000 claims abstract description 12
- 239000003377 acid catalyst Substances 0.000 claims abstract description 10
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 10
- 239000000356 contaminant Substances 0.000 claims abstract description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 9
- 238000004064 recycling Methods 0.000 claims abstract description 7
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- 230000036571 hydration Effects 0.000 claims abstract 2
- 238000006703 hydration reaction Methods 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 40
- 229910010293 ceramic material Inorganic materials 0.000 claims description 23
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052863 mullite Inorganic materials 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- ZXEHLAPOJGDPLC-UHFFFAOYSA-N 1-methoxyethanolate;yttrium(3+) Chemical compound [Y+3].COC(C)[O-].COC(C)[O-].COC(C)[O-] ZXEHLAPOJGDPLC-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000002401 inhibitory effect Effects 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000001771 vacuum deposition Methods 0.000 description 13
- 230000007062 hydrolysis Effects 0.000 description 10
- 238000006460 hydrolysis reaction Methods 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 238000011109 contamination Methods 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 3
- 239000000567 combustion gas Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 230000000887 hydrating effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4803—Insulating or insulated parts, e.g. mountings, containers, diamond heatsinks
- H01L21/4807—Ceramic parts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
- H01L21/02252—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by plasma treatment, e.g. plasma oxidation of the substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4803—Insulating or insulated parts, e.g. mountings, containers, diamond heatsinks
- H01L21/481—Insulating layers on insulating parts, with or without metallisation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S438/00—Semiconductor device manufacturing: process
- Y10S438/974—Substrate surface preparation
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Abstract
The present invention relates to a method of preparing a coating sol composition obtained by hydrolyzing tetraethylorthosilicate, methyltriethoxysilane, dimethyldimethoxysilane and colloidal silica under an acid catalyst, or preparing a coating sol composition comprising an aluminosilicate sol and a yttrium alkoxide A step of preparing a Y 2 O 3 -Al 2 O 3 -SiO 2 sol composition obtained by a polycondensation reaction with hydration, a step of regenerating a ceramic member used in a semiconductor or a display manufacturing process, removing a contaminant generated in a semiconductor or a display manufacturing process Preparing a ceramic member that has been cleaned with acid, alkali, or water in order to make the ceramic member clean; and applying the coating sol composition to the surface of the ceramic member to recover the ceramic member used in a semiconductor or display manufacturing process, Drying the applied ceramic member with the coated sol composition and drying the dried product By separating relates to a recycling method for preventing outgassing and ceramic members, comprising the step of obtaining a coating layer is formed ceramic member for inhibiting the generation of particles. According to the present invention, outgassing generated from a ceramic member used in a semiconductor or a display manufacturing process can be prevented by hard coating, generation of particles can be suppressed, and the surface is smooth, A regenerated ceramic member which is low in moisture adsorption power, high in surface hardness, and can be stably and reliably reused can be obtained.
Description
The present invention relates to a method of regenerating a ceramic member for reuse of a ceramic member, and more particularly, to a method of regenerating a ceramic member for recycling a ceramic member, And a method of regenerating the member.
Expensive devices or parts such as vacuum deposition chambers are used in the semiconductor manufacturing process or the display manufacturing process. The wall surface of the vacuum deposition chamber is made of a ceramic material such as alumina, and a deposition process is performed using a plasma in a vacuum deposition chamber.
Ceramic materials such as a vacuum deposition chamber exposed to a plasma are damaged or contaminated due to corrosion or physical attack due to a chemical attack or a physical attack depending on a plasma condition. The chemical attack is mainly caused by the radical of the plasma or the like, and the physical attack is mainly caused by ion bombardment due to the floating potential of the plasma or the like. If damage or contamination occurs to a device or part of a ceramic material such as a vacuum deposition chamber, defects may occur and the yield of semiconductors or displays may be reduced.
Therefore, if damage or contamination of the vacuum deposition chamber occurs severely, it should be replaced with a new vacuum deposition chamber, or the vacuum deposition chamber used should be cleaned or replaced with new wall components if damage or contamination is severe. However, the disadvantage is that replacing with a new vacuum deposition chamber or replacing with a new wall part is costly. Therefore, ceramic devices and parts used in actual production of semiconductors and displays are periodically cleaned and reused.
A professional cleaning company that cleans ceramic devices or parts such as vacuum deposition chambers removes various contaminants generated in semiconductor or display manufacturing processes by using acid or alkali, Is recycled and recycled in a semiconductor or display manufacturing process. FIGS. 1 and 2 are scanning electron microscope (SEM) photographs showing a ceramic member of an alumina material constituting a wall surface of a vacuum deposition chamber of a semiconductor manufacturing process after cleaning by a professional cleaning company.
However, the cleaned and regenerated ceramic material devices and parts are surface-damaged by roughening the surface, and pores are formed on the surface, resulting in a high water-absorbing ability and a poor surface hardness. 1 and 2, it can be seen that the cleaned and regenerated ceramic member has a rough and smooth surface.
In addition, when a cleaned and regenerated ceramic material device or component is mounted on a semiconductor or display manufacturing process equipment, it requires at least 6 to 12 hours of gas outgassing to reach the vacuum required for the process operation There is a problem that the productivity is deteriorated due to additional work time.
In order to solve such a problem, a study has been made to reduce the generation time of outgas by applying a polymer such as epoxy to a cleaned and regenerated ceramic material device or part. However, in the case of a semiconductor or a display manufacturing process, Deg.] C, the polymer material of the organic material may generate a combustion gas to provide a cause of the process failure.
SUMMARY OF THE INVENTION The present invention has been made in an effort to solve the above problems, and it is an object of the present invention to provide a method of manufacturing a semiconductor device, which can prevent outgasing generated from a ceramic device or a ceramic member used in a semiconductor or a display manufacturing process, And a regenerated ceramic member having smooth surface, no pore on the surface, low moisture adsorption ability, high surface hardness, and can be stably and reliably reused.
The present invention relates to a method of regenerating a ceramic member for recycling and reusing an apparatus or a part of a ceramic material used in a semiconductor or a display manufacturing process. The method includes the steps of: depositing tetraethyl orthosilicate (TEOS), methyltriethoxysilane preparing a coated sol composition obtained by hydrolyzing methyltriethoxysilane, dimethyldimethoxysilane (DMDMS) and colloidal silica under an acid catalyst, preparing a coating sol composition obtained by subjecting a ceramic used in a semiconductor or display manufacturing process, Preparing a ceramic member that has been cleaned with acid, alkali, or water to regenerate the member and remove contaminants generated in the semiconductor or display manufacturing process, and to recover the ceramic member used in the semiconductor or display manufacturing process Applying the coating sol composition to the surface of the ceramic member Drying the ceramic member coated with the coated sol composition and heat treating the dried product to obtain a ceramic member having a coating layer for preventing outgassing and inhibiting the generation of particles, to provide.
The ceramic member may be made of at least one ceramic material selected from alumina (Al 2 O 3 ), zirconia (ZrO 2 ), mullite, SiC and Si 3 N 4 .
The heat treatment is preferably performed in an oxidizing atmosphere at a temperature of 600 to 1000 ° C.
The heat treatment is performed by raising and maintaining the temperature of the furnace at a heat treatment temperature of 600 to 1000 占 폚 at a heating rate of 15 to 50 占 폚 / min to infiltrate the oxide component of the coated sol composition into the ceramic member And slowly cooling the temperature of the furnace to unload the heat-treated product to obtain a ceramic member having an oxide component forming the coating layer.
The viscosity of the coating sol composition is preferably in the range of 1 to 20 cps (centi poise).
Wherein the coating sol composition comprises the tetraethylorthosilicate (TEOS), the methyltriethoxysilane (MTES), the dimethyldimethoxysilane (DMDMS), and the colloidal silica in a ratio of 1: 0.1 to 10: 0.1 To 10: 0.1 to 10 molar ratio and hydrolyzed in the presence of an acid catalyst.
The colloidal silica may include colloids in which silica particles having a size of 5 to 30 nm are dispersed in water (H 2 O).
The present invention also provides a method of regenerating a ceramic member for recycling and reusing a device or a component of a ceramic material used in a semiconductor or a display manufacturing process. The method includes the steps of: reacting an aluminosilicate sol and a yttrium alkoxide with water preparing a Y 2 O 3 -Al 2 O 3 -SiO 2 sol composition obtained by a polycondensation reaction with a hydrolysis catalyst, and regenerating a ceramic member used in a semiconductor or a display manufacturing process, Preparing a ceramic member that has been cleaned with acid, alkali, or water to remove contamination that has occurred, and applying the coating sol composition to a surface of the ceramic member to regenerate the ceramic member used in a semiconductor or display manufacturing process A step of drying the coated ceramic member; And heat-treating the dried result provides a reproducing method of a ceramic member, comprising the step of obtaining the ceramic member is a coating layer for preventing outgassing and particle generation suppression formed.
The ceramic member may be made of at least one ceramic material selected from alumina (Al 2 O 3 ), zirconia (ZrO 2 ), mullite, SiC and Si 3 N 4 .
The heat treatment is preferably performed in an oxidizing atmosphere at a temperature of 600 to 1000 ° C.
The heat treatment is performed by raising and maintaining the temperature of the furnace at a heat treatment temperature of 600 to 1000 占 폚 at a heating rate of 15 to 50 占 폚 / min to infiltrate the oxide component of the coated sol composition into the ceramic member And slowly cooling the temperature of the furnace to unload the heat-treated product to obtain a ceramic member having an oxide component forming the coating layer.
The viscosity of the coating sol composition is preferably in the range of 1 to 20 cps (centi poise).
The yttrium alkoxide may include yttrium methoxyethoxide prepared by mixing yttrium acetate and 2-methoxyethanol followed by heating at a temperature higher than 125 ° C with stirring.
The aluminosilicate sol can be prepared by partially hydrating distilled Si (OC 2 H 5 ) 4 with deionized water, anhydrous alcohol, and concentrated nitric acid (catalyst), adding Al (OC 4 H 9 ) 3 and isopropanol and reacting them.
According to the present invention, it is possible to prevent outgasing from a device or a component (ceramic member) of a ceramic material used in a semiconductor or a display manufacturing process by hard coating, The occurrence can also be suppressed.
The device or component (ceramic member) of the ceramic material reproduced in accordance with the present invention has smooth surface, no pores on the surface, low water absorption power, high surface hardness, and can be reliably reused.
In addition, according to the present invention, it is possible to reduce the outgasing time without generating combustion gas even when the process temperature of the semiconductor or display manufacturing process exceeds 200 ° C, thereby increasing the productivity.
FIGS. 1 and 2 are scanning electron microscope (SEM) photographs showing a ceramic member of an alumina material constituting a wall surface of a vacuum deposition chamber of a semiconductor manufacturing process after cleaning by a professional cleaning company.
3 is a scanning electron microscope (SEM) photograph showing the surface of an Al 2 O 3 ceramic member on which a coating layer is formed using a coating sol composition.
4 is a scanning electron microscope (SEM) photograph showing a cross section of an Al 2 O 3 ceramic member having a coating layer formed using a coating sol composition.
5A to 5E are diagrams showing energy dispersive spectroscopy (EDS) analysis of an Al 2 O 3 ceramic member having a coating layer formed using a coating sol composition.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, it should be understood that the following embodiments are provided so that those skilled in the art will be able to fully understand the present invention, and that various modifications may be made without departing from the scope of the present invention. It is not.
A recycling method of a ceramic member which recycles and recycles an expensive ceramics device or a part such as a vacuum deposition chamber used in a semiconductor manufacturing process or a display manufacturing process is proposed.
It is possible to prevent outgasing and to prevent generation of particles when a device or a component of a ceramic material used in a semiconductor or a display manufacturing process is reproduced according to the present invention Can also be suppressed. Even if the process temperature of the semiconductor or display manufacturing process exceeds 200 ° C, the outgasing time can be reduced without generating combustion gas, thereby increasing the productivity.
The apparatus or component (regenerated ceramic member) of the ceramic material regenerated in accordance with the present invention has smooth surface, no pores on the surface, low water absorption power, high surface hardness, and can be reliably reused.
A method of regenerating a ceramic member according to a preferred embodiment of the present invention is a method of regenerating a ceramic member for regenerating and reusing an apparatus or a part of a ceramic material used in a semiconductor or a display manufacturing process, A coating sol composition prepared by hydrolyzing tetraethyl orthosilicate, methyltriethoxysilane (MTES), dimethyl dimethoxysilane (DMDMS) and colloidal silica under an acid catalyst is prepared Preparing a ceramic member cleaned with acid, alkali or water to regenerate the ceramic member used in the semiconductor or display manufacturing process and to remove contaminants generated in the semiconductor or display manufacturing process, In order to regenerate the ceramic member used in the process Applying the coating sol composition to the surface of the ceramic member, drying the ceramic member coated with the coated sol composition, and heat treating the dried product to form a ceramic member having a coating layer for preventing outgassing and inhibiting the generation of particles .
The ceramic member may be made of at least one ceramic material selected from alumina (Al 2 O 3 ), zirconia (ZrO 2 ), mullite, SiC and Si 3 N 4 .
The heat treatment is preferably performed in an oxidizing atmosphere at a temperature of 600 to 1000 ° C.
The heat treatment is performed by raising and maintaining the temperature of the furnace at a heat treatment temperature of 600 to 1000 占 폚 at a heating rate of 15 to 50 占 폚 / min to infiltrate the oxide component of the coated sol composition into the ceramic member And slowly cooling the temperature of the furnace to unload the heat-treated product to obtain a ceramic member having an oxide component forming the coating layer.
The viscosity of the coating sol composition is preferably in the range of 1 to 20 cps (centi poise).
Wherein the coating sol composition comprises the tetraethylorthosilicate (TEOS), the methyltriethoxysilane (MTES), the dimethyldimethoxysilane (DMDMS), and the colloidal silica in a ratio of 1: 0.1 to 10: 0.1 To 10: 0.1 to 10 molar ratio and hydrolyzed in the presence of an acid catalyst.
The colloidal silica may include colloids in which silica particles having a size of 5 to 30 nm are dispersed in water (H 2 O).
According to another preferred embodiment of the present invention, there is provided a method of regenerating a ceramic member for regenerating and reusing an apparatus or a part of a ceramic material used in a semiconductor or a display manufacturing process, Preparing a Y 2 O 3 -Al 2 O 3 -SiO 2 sol composition obtained by reacting yttrium alkoxide with hydrolysis and polycondensation; Preparing a ceramic member that has been cleaned with acid, alkali, or water to regenerate the member and remove contaminants generated in the semiconductor or display manufacturing process, and to recover the ceramic member used in the semiconductor or display manufacturing process Applying the coating sol composition to a surface of a ceramic member, Drying the ceramic member coated with the Tingol composition and heat treating the dried product to obtain a ceramic member having a coating layer for preventing outgassing and inhibiting the generation of particles.
The ceramic member may be made of at least one ceramic material selected from alumina (Al 2 O 3 ), zirconia (ZrO 2 ), mullite, SiC and Si 3 N 4 .
The heat treatment is preferably performed in an oxidizing atmosphere at a temperature of 600 to 1000 ° C.
The heat treatment is performed by raising and maintaining the temperature of the furnace at a heat treatment temperature of 600 to 1000 占 폚 at a heating rate of 15 to 50 占 폚 / min to infiltrate the oxide component of the coated sol composition into the ceramic member And slowly cooling the temperature of the furnace to unload the heat-treated product to obtain a ceramic member having an oxide component forming the coating layer.
The viscosity of the coating sol composition is preferably in the range of 1 to 20 cps (centi poise).
The yttrium alkoxide may include yttrium methoxyethoxide prepared by mixing yttrium acetate and 2-methoxyethanol followed by heating at a temperature higher than 125 ° C with stirring.
The aluminosilicate sol can be prepared by partially hydrating distilled Si (OC 2 H 5 ) 4 with deionized water, anhydrous alcohol, and concentrated nitric acid (catalyst), adding Al (OC 4 H 9 ) 3 and isopropanol and reacting them.
Hereinafter, a method of regenerating a ceramic member according to a preferred embodiment of the present invention will be described in more detail.
A coating sol composition for regenerating a ceramic member according to a preferred embodiment of the present invention may be prepared by mixing tetraethyl orthosilicate (TEOS), methyltriethoxysilane (MTES), dimethyldimethoxysilane (DMDMS; dimethyldimethoxysilane and colloidal silica by hydrolysis under an acid catalyst. As the solvent for hydrolysis, water, water (H 2 O), ethanol and the like can be used. The amount of the tetraethyl orthosilicate (TEOS), the methyltriethoxysilane (MTES), the dimethyldimethoxysilane (DMDMS), and the colloidal silica is 1: 0.1 to 10: 0.1 to 10: 10 in a molar ratio and hydrolyzed under an acid catalyst. The temperature for carrying out the hydrolysis is preferably about room temperature to about 60 ° C. The viscosity of the coating sol composition is preferably about 1 to 20 cps (centi poise). The colloidal silica may be a colloid in which silica particles having a size of 5 to 30 nm, more specifically, 10 to 20 nm, are dispersed in water (H 2 O).
A coating sol composition for regenerating a ceramic member according to another preferred embodiment of the present invention comprises Y 2 O 3 -Al (aluminosilicate) obtained by reacting an aluminosilicate sol with a yttrium alkoxide by hydrolysis and polycondensation, 2 O 3 -SiO 2 (YAS) sol composition. The viscosity of the coating sol composition is preferably about 1 to 20 cps (centi poise).
Hereinafter, the method for synthesizing the Y 2 O 3 -Al 2 O 3 -SiO 2 (YAS) sol composition will be described in more detail.
Soluble yttrium alkoxide is synthesized. The synthesis of yttrium alkoxide is suitable for homogeneous gel preparation.
The yttrium alkoxide can be synthesized as follows. For example, yttrium methoxyethoxide, a kind of yttrium alkoxide, is prepared by mixing yttrium acetate and 2-methoxyethanol (OCH 3 C 2 H 5 OH) The yttrium methoxyethoxide thus prepared is quite stable and can be stored at room temperature for a long time.
The composition of the three-component eutectic Y 2 O 3 -Al 2 O 3 -SiO 2 (ternary eutectic YAS) can be successfully synthesized by controlling the hydrolysis and polycondensation reaction rates.
For example, distilled Si (OC 2 H 5 ) 4 is partially hydrated using deionized water, anhydrous alcohol, and concentrated nitric acid (catalyst), and stirred at 40 to 70 캜 (preferably 60 캜) 4 H 9 ) 3 and isopropanol are added and reacted to obtain an aluminosilicate sol that remains clear as water without precipitation products such as AlO (OH) or Al (OH) 3 When the yttrium alkoxide synthesized by continuously stirring the aluminosilicate sol thus obtained at 40 to 70 ° C (preferably 60 ° C) is added and reacted, the Y 2 O 3 -Al 2 O 3- SiO 2 (YAS) sol can be obtained. According to the above-described method, the formation of an alkoxide complex which is generated in the insoluble Y 2 O 3 .2SiO 2 system can be avoided, and the clear Y 2 O 3 -Al 2 having a color similar to that of yttrium alkoxide can be avoided O 3 -SiO 2 (YAS) sol can be obtained.
The coating sol composition described above is coated on the surface of a ceramic member cleaned with acid, alkali, water (H 2 O) or the like to prevent outgasing and to suppress the generation of particles have.
The ceramic member may be made of a ceramic material such as alumina (Al 2 O 3 ), zirconia (ZrO 2 ), mullite, SiC or Si 3 N 4 . The ceramic member may be a ceramic member cleaned using acid, alkali, water (H 2 O) or the like in a professional cleaning company to remove various contaminants generated in a semiconductor or a display manufacturing process.
The coated sol composition is coated on the surface of the ceramic member to form a coating layer. The coated sol composition is coated on the surface of the ceramic member, dried, and then subjected to a heat treatment process, thereby forming a coating layer on the ceramic member to prevent outgassing and to suppress the generation of particles. By forming the coating layer on the ceramic member using the coating sol composition, the outgassing can be prevented and generation of particles can be suppressed when the recycled ceramic member is reused in a semiconductor or a display process.
Hereinafter, a method of regenerating a ceramic member by a glass infiltration method using a coated sol composition according to a preferred embodiment of the present invention will be described in further volume.
A ceramic member cleaned with acid, alkali, water (H 2 O) or the like is prepared for regenerating the ceramic member used in the semiconductor or display manufacturing process.
The coated sol composition is applied on the ceramic member by dip, spray, brushing, printing, dispensing, flow coating or the like. The ceramic member may be made of a ceramic material such as alumina (Al 2 O 3 ), zirconia (ZrO 2 ), mullite, SiC or Si 3 N 4 . The ceramic member removes various contaminants (particularly, contaminants generated in a semiconductor or a display manufacturing process) on the surface of the ceramic member, acid, alkali, water (H 2 O), or the like. The printing may be a screen printing method or an inkjet printing method. The coating thickness of the coated sol composition is adjusted in consideration of the thickness after the heat treatment, and is appropriately applied in accordance with the viscosity of the coating sol composition.
After the coated sol composition is applied, a drying step is performed. The drying step may be carried out, for example, at 60 to 180 DEG C for 10 minutes to 24 hours. By this drying step, the solvent (or solvent) component is volatilized.
The ceramic member coated with the coated sol composition and subjected to the drying process is charged into a furnace to perform heat treatment.
Hereinafter, the heat treatment process will be described in more detail.
The ceramic member to which the coated sol composition is applied and the drying process is performed is charged into a furnace.
The temperature of the furnace is raised to a target heat treatment temperature using a heating means provided in the furnace and maintained for a predetermined time (for example, 1 minute to 12 hours). If the rate of temperature rise of the furnace is slower than 15 ° C / min, it takes a long time to lower the productivity, and due to the decrease of moisture on the surface of the ceramic member, If the rate of temperature rise of the furnace is higher than 50 DEG C / min, thermal stress may be applied due to a rapid temperature rise. Therefore, it is preferable to raise the temperature of the furnace at the temperature raising rate within the above range. The heat treatment temperature is preferably 600 to 1000 占 폚, and more preferably 700 to 900 占 폚. The heat treatment is preferably performed in an oxidizing atmosphere such as oxygen (O 2 ) and air. When maintained at the heat treatment temperature, the oxide component of the coating sol composition is infiltrated into the ceramic member. The organic components contained in the coating sol composition burn up during the heating process and the heat treatment process.
After performing the heat treatment process, the furnace temperature is slowly cooled to unload the heat-treated product (the ceramic member having the coating layer formed thereon). The furnace cooling may be performed by shutting down the furnace power source to cool slowly in a natural state, or to set the temperature to a predetermined lowering rate (for example, 1 to 20 ° C / min).
If the coated sol composition is coated on the ceramic member to form a coating layer, outgassing can be prevented and generation of particles can be suppressed even if the ceramic member is reused in a semiconductor or a display process.
The present invention will be explained in more detail with reference to the following experimental examples, which are not intended to limit the present invention.
Hydrolysis of tetraethyl orthosilicate (TEOS), methyltriethoxysilane (MTES), dimethyl dimethoxysilane (DMDMS), and colloidal silica under an acid catalyst To obtain a coating sol composition. The tetraethylorthosilicate (TEOS), the methyltriethoxysilane (MTES), the dimethyldimethoxysilane (DMDMS), and the colloidal silica were mixed in a molar ratio of 0.2: 0.3: 0.3: 0.2 Hydrolyzed under hydrochloric acid (HCl) catalyst. Water (H 2 O) and ethanol were used as the solvent for the hydrolysis. The temperature for carrying out the hydrolysis was about 30 캜. The viscosity of the coating sol composition was on the order of 8.5 cps (centi poise).
A ceramic member made of Al 2 O 3 (hereinafter referred to as "Al 2 O 3 ceramic member") was washed with deionized water and used.
The coating sol composition obtained according to Experimental Example was coated on an Al 2 O 3 ceramic member by a flow coating method in which the angle of inclination of the Al 2 O 3 ceramic member was about 80 °, The posterior state was maintained for about 3 minutes. After the coated sol composition was applied, a drying process was performed at a temperature of about 100 DEG C for 30 seconds.
The Al 2 O 3 ceramic member coated with the coating sol composition and dried was subjected to a heat treatment process to form a coating layer. The temperature of the furnace was raised to a heat treatment temperature (900 DEG C) at a heating rate of 20 DEG C / min using a heating means provided in a furnace, and maintained at a heat treatment temperature for 60 minutes.
After the heat treatment process, the furnace temperature was lowered to unload the heat-treated product, and the furnace was allowed to cool slowly.
3 is of Al 2 O coating layer is formed by coating a sol composition 3 is a scanning electron microscope, showing a surface of a ceramic member (SEM) picture, 4 is Al 2 O coating layer is formed by coating a sol composition 3 ceramic members 5A to 5E are graphs showing energy dispersive spectroscopy (EDS) analysis of an Al 2 O 3 ceramic member on which a coating layer is formed using a coating sol composition. FIG. 5A is a scanning electron microscope (SEM)
3 to 5E, it can be seen that the Al 2 O 3 ceramic member in which the coating layer is formed has a smooth surface and no pores on the surface.
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, but, on the contrary, This is possible.
Claims (10)
Preparing a coating sol composition obtained by hydrolyzing tetraethyl orthosilicate, methyltriethoxysilane, dimethyldimethoxysilane, and colloidal silica in the presence of an acid catalyst;
Preparing a ceramic member washed with acid, alkali, or water to regenerate the ceramic member used in the semiconductor or display manufacturing process and to remove contaminants generated in the semiconductor or display manufacturing process;
Applying the coating sol composition to a surface of the ceramic member to regenerate the ceramic member used in a semiconductor or display manufacturing process;
Drying the ceramic member coated with the coating sol composition; And
And a step of heat treating the dried product to obtain a ceramic member having a coating layer for preventing outgassing and for suppressing the generation of particles.
Preparing a Y 2 O 3 -Al 2 O 3 -SiO 2 sol composition obtained by polycondensation reaction of an aluminosilicate sol and a yttrium alkoxide with hydration;
Preparing a ceramic member washed with acid, alkali, or water to regenerate the ceramic member used in the semiconductor or display manufacturing process and to remove contaminants generated in the semiconductor or display manufacturing process;
Applying the coating sol composition to a surface of the ceramic member to regenerate the ceramic member used in a semiconductor or display manufacturing process;
Drying the ceramic member coated with the coating sol composition; And
And a step of heat treating the dried product to obtain a ceramic member having a coating layer for preventing outgassing and for suppressing the generation of particles.
Raising and maintaining the temperature of the furnace at a heat treatment temperature of 600 to 1000 占 폚 at a heating rate of 15 to 50 占 폚 / min to infiltrate the oxide component of the coated sol composition into the ceramic member; And
And slowly cooling the temperature of the furnace to unload the heat treated product to obtain a ceramic member having an oxide component forming the coating layer.
Distilled Si (OC 2 H 5 ) 4 was partially hydrated using deionized water, anhydrous alcohol, and concentrated nitric acid (catalyst), and Al (OC 4 H 9 ) 3 and isopropanol And a sol which is obtained by reacting the ceramic member with a solvent.
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| KR20200104811A (en) * | 2019-02-27 | 2020-09-04 | 토토 가부시키가이샤 | Member for semiconductor manufacturing device and semiconductor manufacturing device with member for semiconductor manufacturing device and display manufacturing device |
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