KR101807444B1 - Plasma device part and manufacturing method therefor - Google Patents
Plasma device part and manufacturing method therefor Download PDFInfo
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- KR101807444B1 KR101807444B1 KR1020167013892A KR20167013892A KR101807444B1 KR 101807444 B1 KR101807444 B1 KR 101807444B1 KR 1020167013892 A KR1020167013892 A KR 1020167013892A KR 20167013892 A KR20167013892 A KR 20167013892A KR 101807444 B1 KR101807444 B1 KR 101807444B1
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- Prior art keywords
- oxide
- particles
- yttrium oxide
- lanthanoid
- lanthanoid element
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 212
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 123
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000010419 fine particle Substances 0.000 claims abstract description 15
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 6
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 6
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 5
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract 2
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 111
- 150000002602 lanthanoids Chemical class 0.000 claims description 111
- 238000002485 combustion reaction Methods 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 21
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 11
- 230000003746 surface roughness Effects 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 8
- 238000002441 X-ray diffraction Methods 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 238000000576 coating method Methods 0.000 abstract description 45
- 239000011248 coating agent Substances 0.000 abstract description 43
- 238000005530 etching Methods 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 239000010408 film Substances 0.000 description 119
- 239000000843 powder Substances 0.000 description 22
- 239000002994 raw material Substances 0.000 description 19
- 238000005507 spraying Methods 0.000 description 18
- 230000007797 corrosion Effects 0.000 description 11
- 238000005260 corrosion Methods 0.000 description 11
- 230000007547 defect Effects 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 238000001020 plasma etching Methods 0.000 description 8
- 230000009467 reduction Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006061 abrasive grain Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000005422 blasting Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000011362 coarse particle Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000007750 plasma spraying Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5045—Rare-earth oxides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02299—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment
- H01L21/02312—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment treatment by exposure to a gas or vapour
- H01L21/02315—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment treatment by exposure to a gas or vapour treatment by exposure to a plasma
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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
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Drying Of Semiconductors (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Coating By Spraying Or Casting (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
Ce, Sm, Dy, Gd, Er, Yb (1 to 8 mass%) is added to the yttrium oxide film in the component for a plasma device having a yttrium oxide film containing fine particles having a particle size of 1 m or less formed by the impact sintering method. In which the thickness of the coating film is 10 占 퐉 or more, the density of the coating film is 90% or more, and the grain boundary existing in the unit area of the coating film 20 占 퐉 占 20 占 퐉 can be confirmed Wherein the particles have an area ratio of 0 to 80% and an area ratio of the particles bound with the grain boundaries is 20 to 100%, and a manufacturing method thereof. According to the above configuration, generation of particles can be stably and effectively suppressed during the plasma process, and productivity can be reduced, an increase in etching and film formation costs can be suppressed, and generation of fine particles can be suppressed, Can be prevented and a manufacturing method thereof can be provided.
Description
The present invention relates to a component for a plasma apparatus coated with an oxide film, which is excellent in corrosion resistance against a halogen-based corrosive gas or plasma, and which can be suitably used for parts for plasma devices such as semiconductor and liquid crystal manufacturing.
Among the semiconductor manufacturing apparatuses, parts for devices in an etching process in which a plasma process is a mainstream, a CVD film forming process, and an ashing process for removing a resist are exposed to halogen-based corrosive gases such as fluorine and chlorine which are highly reactive.
For this reason, ceramics materials such as alumina (aluminum oxide), aluminum nitride, yttria (yttria), and YAG are widely used as constituent materials of parts exposed to the halogen plasma in the above process.
For example, Patent Document 1 discloses that a substrate contains ceramics having a metal or metal electrode, tungsten or molybdenum dispersed in an amount of 5 wt% or more and less than 60 wt% relative to yttrium is dispersed in the outermost surface of the substrate, (Electrostatic chuck) having a dielectric layer with a stable low volume resistivity can be obtained by forming an oxide yttrium-based plasma spray coating having a porosity of 5% or less.
However, since the coating of yttrium oxide or aluminum oxide formed by the spraying method is formed by depositing a raw material powder such as yttrium oxide or aluminum oxide in a molten state, when the molten particles solidify rapidly and adhere due to the spraying heat source , A large number of micro cracks are generated in the particles that have become flat and deposited, and deformation caused by rapid cooling and solidification remains in each flat particle to form a coating. When an active radical generated in a plasma discharge is irradiated to a coating film of yttrium oxide or aluminum oxide in such a state, an active radical is attacked by microcracks to promote cracks, and further cracks propagate So that there is a problem that the sprayed coating is broken and particles are generated.
In addition, since the component for a plasma apparatus having a ceramic sprayed coating includes a structure in which flat particles are deposited, irregular irregularities remain on the surface even when polishing finish or the like is performed, and the irregular surface irregularities remain on the surface of the dielectric layer , Particles are liable to be removed from the particles, resulting in generation of particles due to these particles.
As described above, since the film of yttria or aluminum oxide formed by spraying is a deposited film in a molten state, it tends to be a source of particles and causes a decrease in product yield. Therefore, It is easy to cause problems in formation.
In addition, in the case of forming the thermal sprayed coating on the component parts, since the thermal sprayed coating is deposited on the surface which is subjected to the blast treatment for spraying the abrasive grains and the substrate surface together with the high pressure solid particles, (Abrasive grains) may remain on the surface of the component, or a fragile fractured layer may be formed on the surface of the component by blasting. Since the thermal sprayed coating is deposited on the surface of the component in this manner, stress acts on the interface between the thermal sprayed part and the thermal sprayed coating due to the thermal stress generated by the temperature change caused by the plasma discharge, and the film separation easily occurs for each thermal sprayed coating. Particularly, when the pressure of the blast treatment and the size of the abrasive grain are increased, the occurrence of film peeling becomes remarkable. Therefore, the lifespan of the thermal spray coating largely depends on the condition of the thermal spray coating itself as well as the constitution of the thermal spray coating itself.
As described above, since there are defects in the yttrium oxide film formed by the spraying method and at the interface with the parts, there is a great problem in terms of longevity of the film formed by the spraying method even in the yttrium oxide film having plasma resistance and corrosion resistance have.
In the case of the plasma spraying, since the particle size of the yttrium oxide powder supplied as the raw material is as large as about 10 to 45 탆, voids (voids) are generated in the formed thermal spray coating at a maximum of about 15%, and the surface roughness It is roughly 6 to 10 mu m in roughness Ra, and it takes a long time to planarize by the polishing treatment. When the electrostatic chuck having such a thermal sprayed coating is used, the plasma etching proceeds through the pores. Further, when the surface roughness is large, the plasma discharge is concentrated on the convex portion of the sprayed surface. As described above, since the plasma attack is concentrated on the internal defects and the sprayed coating is weakened due to surface defects, the amount of particles generated due to the hand damage of the sprayed coating is increased, and the service life of the component for the plasma apparatus is lowered .
Particularly, in a component for a plasma apparatus in which both plasma resistance and resistance to corrosion are required, particles are liable to be generated due to coating defects even in a yttrium oxide film formed by a spraying method, and productivity And an increase in the etching cost.
In recent semiconductor devices, in order to achieve a particularly high degree of integration, narrowing of wiring width (for example, 24 nm, 19 nm) is proceeding. In this narrowed wiring or the element having it, for example, even if very fine particles (fine particles) having a diameter of about 40 nm are mixed, it causes a wiring defect (disconnection) or an element failure (short circuit) It is strongly desired to further suppress the generation of fine particles caused by the component parts.
DISCLOSURE OF THE INVENTION The present invention has been made to solve the above-mentioned conventional problems, and it is an object of the present invention to improve the plasma resistance and corrosion resistance of the coating film itself during the etching process so as to stably and effectively suppress the generation of particles, Which is capable of suppressing film separation and effectively suppressing the generation of fine particles and preventing contamination due to impurities while suppressing an increase in etching rate and film forming cost of a plasma processing apparatus and an apparatus for plasma processing, And it is an object of the present invention to provide a component for a plasma apparatus and a manufacturing method thereof that do not cause corrosion or deformation of the member due to chemical liquid treatment or blast treatment.
The component for a plasma device having a yttrium oxide film formed by the impact sintering method of the present invention is characterized in that the yttrium oxide film contains at least one of lanthanoids selected from La, Ce, Sm, Dy, Gd, Er, Which has a yttrium oxide film containing one kind of oxide in terms of oxide and has a thickness of 10 mu m or more and a coating film density of 90% or more and a coating layer having a unit area of 20 mu m x 20 mu m Characterized in that the area ratio of the particles is 0 to 80% and the area ratio of the particles whose grain boundaries can not be confirmed is 20 to 100%.
The yttrium oxide film containing an oxide of a lanthanoid element preferably has a film thickness of 10 to 200 mu m and a film density of 99% or more and 100% or less. It is preferable that the oxide particles of yttrium oxide and lanthanoid element include fine particles having a particle diameter of 1 占 퐉 or less and yttrium oxide particles capable of confirming the intergranular particle have an average particle diameter of 2 占 퐉 or less. The total average particle diameter of oxide particles of yttrium oxide and lanthanoid-based elements is preferably 5 占 퐉 or less.
When the yttrium oxide film containing the oxide of the lanthanoid element is subjected to XRD analysis, the ratio (Im / Ic) of the strongest peak Im of monoclinic to the strongest peak Ic of the cubic crystal is preferably 0.2 to 0.6. The yttrium oxide film containing the oxide of the lanthanoid element is preferably subjected to a polishing treatment so that the surface roughness Ra is 0.5 m or less.
A method of manufacturing a component for a plasma device in which a yttrium oxide film containing an oxide of a lanthanoid element is formed by the impact sintering method of the present invention includes the steps of supplying a slurry containing oxide particles to a combustion flame, And lanthanoid element oxide particles at a jetting rate of 400 to 1000 m / sec.
Here, the average particle size of the oxide particles of the yttrium oxide particles and the lanthanoid-based elements is preferably 0.05 to 5 mu m. It is preferable that the yttrium oxide film containing an oxide of the lanthanoid element is 10 mu m or more in film thickness. It is preferable to supply a slurry containing yttrium oxide particles and oxide particles of lanthanoid-based elements to the center of the combustion flame.
According to the yttrium oxide film containing an oxide of a lanthanide element using the impact sintering method in which a supply powder containing fine particles having an average particle diameter of 5 mu m or less and a particle diameter of 1 mu m or less at the time of film formation is deposited without melting as in the present invention , Flat-shaped molten particles are hardly generated, and fine particles having a particle diameter of 1 탆 or less are also deposited, whereby minute voids can be reduced to reduce surface defects.
The yttrium oxide film containing an oxide of a lanthanoid element such as La, Ce, Sm, Dy, Gd, Er, or Yb in the coating film can achieve higher densification and smoothening of the surface as compared with yttrium oxide, The internal defects of the coating film can be reduced. Thereby, the densification of the film is improved as compared with the coating containing yttrium alone, and the stability of the crystal structure of the oxide constituting the coating is improved, so that the chemical stability of the coating can be improved and the plasma resistance and corrosion resistance can be improved .
The lanthanoid element may be suitably used as any of complex oxides of metals, oxides and Y 2 O 3 . Preferably, it is an oxide or a composite oxide. If it is an oxide or a composite oxide, it is possible to further improve the corrosion resistance.
By applying such an oxide film to a component for a plasma apparatus using a plasma discharge, the plasma resistance of the component can be improved, the amount of particles generated and the amount of impurity contamination can be suppressed, and chemical treatment or blasting It is possible to drastically reduce the number of times of device cleaning and parts replacement since the processing does not damage the member by corrosion or deformation. The reduction of the amount of generated particles greatly contributes to the improvement of the yield of various thin films subjected to the plasma etching treatment, and further, the devices and parts using the thin films. Further, reduction in the number of times of device cleaning and parts replacement greatly contributes to improvement in productivity and reduction in etching cost and film formation cost.
According to the present invention, it is possible to stably and effectively suppress the generation of fine particles generated from a component, to suppress the productivity and the component cost associated with frequent cleaning and replacement of components, and to provide a highly integrated semiconductor device It is possible to provide a component for a plasma apparatus and a manufacturing method thereof that can be applied to manufacture and reduce etch or film formation cost by improving the operating rate.
1 is a cross-sectional view schematically showing a cross-sectional structure of a component for a plasma apparatus according to the present invention.
2 is a microscope organization chart showing an example of a yttrium oxide film containing a lanthanoid oxide.
Hereinafter, embodiments for carrying out the present invention will be described.
The component for a plasma device having the yttrium oxide film formed by the impact sintering method of the present invention is characterized in that an oxide of a lanthanoid element selected from La, Ce, Sm, Dy, Gd, Er, Wherein the coating layer has a thickness of 10 占 퐉 or more, a coating density of 90% or more, and an area ratio of particles in which the grain boundary existing in a unit area of 20 占 퐉 to 20 占 퐉 is 0 to 80 %, While the area ratio of the particles whose grain boundaries can not be confirmed is 20 to 100%.
Fig. 1 shows a structural example of a part for an electrostatic chuck as a part for a plasma apparatus according to the present invention. In the figure, reference numeral 1 denotes a component for a plasma apparatus, 2 denotes a yttrium oxide film containing an oxide of a lanthanoid element, and 3 denotes a base.
Ce, Sm, Dy, Gd, Er, Al, and the like, which are resistant to chlorine-based plasma attack, fluorine-based plasma attack and radical attack (for example, active F radicals or Cl radicals) When the oxide of the lanthanoid element selected from Yb is contained in the yttrium oxide in a proportion of 1 to 8 mass%, the corrosion resistance can be further improved.
These lanthanoid oxide particles improve the grain strength by bonding yttrium oxide particles and also exhibit an effect of eliminating the particle step in polishing finish and the like, and also the volume resistivity of the coating film can be adjusted. When the amount of the oxide of the lanthanoid element is less than 1% by mass, the above effect is not sufficiently exhibited. On the other hand, if the addition amount is more than 8 mass%, the grain boundary layer becomes thick, the film strength is lowered, and the grain step becomes remarkable. A more preferable addition amount is 2 to 6 mass%.
The yttrium oxide film containing an oxide of a lanthanide element has yttrium oxide particles containing an oxide of a lanthanoid element. For example, when a film is formed by a general spraying method, yttrium oxide particles containing an oxide of a lanthanoid element are melted and deposited. As a result, yttrium oxide particles containing an oxide of a lanthanoid element are flat. On the other hand, in the present invention, the area ratio of the particles present in the unit area of 20 mu m x 20 mu m in the coating film is 0 to 80%, while the area ratio of the particles in which the grain boundary can not be confirmed is 20 to 100% .
The yttrium oxide particles containing an oxide of a lanthanoid element capable of confirming the grain boundary can be confirmed by an enlarged photograph. For example, an enlarged photograph of 5000 times is taken by a scanning electron microscope photograph.
Fig. 2 is a drawing (enlarged view) showing an example of a yttrium oxide film containing an oxide of a lanthanoid-based element. In the figure,
&Quot; Grains capable of confirming grain boundaries " can confirm the grain boundaries of individual grains by the difference in contrast. On the other hand, " particles whose grain boundaries can not be confirmed " can not confirm the grain boundaries of individual particles by bonding adjacent particles. The unit area of the coating film was 20 mu m x 20 mu m. Further, arbitrary three sites are measured with respect to this unit area, and the average value is defined as the area ratio of the " particle capable of confirming the grain boundary " and the " grain containing the oxide of the lanthanoid element not capable of confirming grain boundary. &Quot; In Fig. 2, a particle group of " particles capable of confirming the grain boundary " and a grain group of " grain boundary can not be confirmed " are mixed.
The impact sintering method is a coating method in which particles are sprayed by a flame of a combustion flame, and the particles collide with each other at a high speed, and are sintered and bonded by the heat of the collision of the particles. As a result, the yttrium oxide particles in the yttrium oxide film containing the oxide of the lanthanide element tend to form a film in a crushed form rather than the particle shape of the raw material powder.
Further, by accelerating the jet velocity of the yttrium oxide particles containing an oxide of the lanthanoid element at a high speed and accelerating the particle velocity beyond the critical velocity at which the particles begin to deposit, the yttria particles containing the oxide of the lanthanoid element are not melted It is possible to obtain a yttrium oxide film containing an oxide of a lanthanoid-based element having a high film density and almost retaining the particle shape of the raw material powder. Since the impact sintering method enables high-speed injection, it is easy to obtain a structure in which "grains capable of confirming grain boundaries" and "grains that can not be confirmed grain boundaries" are mixed.
When the sum of the area ratios of "grains capable of confirming grain boundaries" and "grains not recognizable grain boundaries" is 100%, the area ratio of "grains capable of confirming grain boundaries" is 0 to 80% Can not be confirmed "is 20 to 100%.
The impact sintering method is a film formation method in which yttria particles containing an oxide of a lanthanoid element are jetted at high speed and particles are deposited by the fracture heat at the time of collision with the substrate. The yttrium oxide particles containing the oxide of the lanthanoid element are bonded by heat when the deposition is carried out by the destructive heat, thereby forming the yttrium oxide particle containing the oxide of the lanthanoid element which can not confirm the grain boundaries.
In addition, by performing the high-speed injection, the raw material powder is not dissolved and sprayed like a spray, so that it can be deposited while maintaining the powder shape of the yttrium oxide particles containing the oxide of the lanthanoid-based element as the raw material powder. As a result, it is possible to form a coating film which is dense and has a strong bonding force without generating stress in the film.
If the area ratio of the " particles capable of confirming grain boundaries " exceeds 80%, the heat of fracture due to the impact is insufficient, so that the coating is rapidly cooled down in the deposition and the density and bonding force of the film are lowered. Occurs. The area ratio of " particles capable of confirming grain boundaries " is preferably 0 to 50%. This means that the area ratio of the " particles whose grain boundaries can not be confirmed " is preferably in the range of 50 to 100%.
In addition, the thickness of the yttrium oxide film containing the oxide of the lanthanoid element is required to be 10 占 퐉 or more. If the film thickness is less than 10 탆, the effect of providing a yttrium oxide film containing an oxide of a lanthanoid element is not sufficiently obtained, which may cause film peeling.
Although the upper limit of the thickness of the yttrium oxide film containing the oxide of the lanthanoid element is not particularly limited, even if the yttrium oxide film is excessively thick, the above effect can not be obtained and the cost can also be increased. Therefore, the thickness of the yttrium oxide film containing an oxide of a lanthanoid element is in the range of 10 to 200 占 퐉, and more preferably in the range of 50 to 150 占 퐉.
In addition, the density of the film is required to be 90% or more. The density of the film is the opposite of the porosity, and the porosity of 90% or more means the same as 10% or less.
In the measurement of the film density, an enlarged photograph of a 500-fold magnification is taken by an optical microscope of a cross-sectional structure photograph of a yttrium oxide film containing an oxide of a lanthanoid element in the film thickness direction, and the area ratio of the pore to be imaged thereon is calculated . Specifically,
&Quot; Film density (%) = 100-area ratio of pores "
The film density is calculated by the equation of " At the time of calculating the film density, the area of the unit area of the tissue of 200 mu m x 200 mu m will be analyzed. When the film thickness is thin, a plurality of points are measured until the total unit area becomes 200 탆 x 200 탆.
The film density is preferably 90% or more, more preferably 95% or more, further preferably 99% or more and 100% or less.
When voids (voids) are present in a yttrium oxide film containing an oxide of a lanthanoid element, erosion such as plasma attack progresses from the pore to lower the lifetime of the yttrium oxide film containing an oxide of a lanthanoid element . Particularly, it is important that the surface of the yttrium oxide film containing the oxide of the lanthanoid element is small in the pores.
The surface roughness of the yttrium oxide film containing an oxide of a lanthanoid element is preferably set to a surface roughness Ra of 0.5 mu m or less by polishing. When the surface roughness after polishing is Ra of 0.5 mu m or less, the wafer adheres closely to the dielectric layer to improve the uniformity of etching. On the other hand, when the surface roughness after polishing is more than Ra 0.5 탆, the wafer is deformed to deteriorate the adhesiveness, the etching property becomes uneven, and particles are liable to be generated.
The average particle diameter of the yttrium oxide particles containing the oxide of the lanthanide element capable of confirming the grain boundary is 2 탆 or less and the total lanthanide series including the yttrium oxide particles containing the oxide of the lanthanide element, The average particle diameter of the yttrium oxide particles containing the oxide of the element is preferably 5 占 퐉 or less.
As described later, yttrium oxide powder containing an oxide of a lanthanoid element as a raw material powder using the impact sintering method preferably has an average particle diameter of 0.05 to 5 mu m. When the average particle diameter of the yttrium oxide particles containing the oxide of the lanthanoid element as the raw material powder exceeds 5 mu m, it is difficult to form a film due to scattering without collapsing when the particles collide with each other, There is a possibility of causing cracks.
When the yttrium oxide particle containing the oxide of the lanthanoid element is not more than 5 mu m, the particles are appropriately crushed when the particles collide with each other, so that particle bonding is promoted by the heat generated by the crushing, and the coating is easily formed. The formed coating has a large bonding force between the particles, so that the amount of generated particles due to plasma attack and radical attack is reduced, and the plasma resistance is improved.
More preferably, the particle size of the particles is from 0.05 to 3 m. When the particle size is less than 0.05 m, the particles are hardly broken and the coating film is formed as a coating film. However, Therefore, the application range of the particle size of the fine particles is preferably 0.05 to 5 mu m. However, if the fine particles of less than 0.05 占 퐉 are less than 5% of the total yttrium oxide particles containing an oxide of the lanthanoid-based element, the coating formation does not deteriorate. Therefore, powders containing fine particles of less than 0.05 占 퐉 may be used.
The average particle size is determined by using an enlarged photograph as shown in Fig. Particles that can identify grain boundaries are the longest diagonal line of the individual particles to be photographed. Particles whose grain boundaries can not be confirmed use their hypothetical sources to set their diameters to particle diameters. This operation is carried out for each of 50 particles (100 particles in total), and the average value is taken as the average particle diameter.
Further, when the yttrium oxide film containing an oxide of a lanthanoid element is subjected to XRD analysis (X-ray diffraction analysis), the ratio of the peak intensity Im of monoclinic to the strongest peak Ic of the cubic intensity Im / Ic) is 0.2 to 0.6.
The XRD analysis is performed by the 2? Method, a Cu target, a tube voltage of 40 kV, and a tube current of 40 mA. The strongest peak of the cubic is detected between 28 and 30 degrees, while the strongest peak of the monoclinic is detected between 30 and 33 degrees. Normally, commercially available yttrium oxide particles are cubic. It is preferable to increase the monoclinicity since the plasma is changed by the breakage heat of the impact sintering method and the monoclinicity is increased to improve the plasma resistance.
Next, a method of manufacturing a component for a plasma apparatus of the present invention will be described.
A method of manufacturing a component for a plasma apparatus in which a yttrium oxide film containing an oxide of a lanthanoid element is formed by the impact sintering method of the present invention includes a step of forming a yttrium oxide layer containing an oxide of a lanthanoid- And a step of jetting the yttrium oxide particles containing an oxide of the lanthanoid element to the substrate at an injection speed of 400 to 1000 m / sec.
The average particle diameter of the yttrium oxide particles containing an oxide of the lanthanoid element is preferably 0.05 to 5 mu m. It is also preferable that the yttrium oxide particle containing an oxide of a lanthanoid element is 10 mu m or more in film thickness. It is preferable that the slurry containing yttria particles containing an oxide of a lanthanoid element is supplied to the center of the combustion flame.
The impact sintering method is a film formation method for supplying yttrium oxide particles containing an oxide of a lanthanoid element at high speed by supplying a slurry containing yttrium oxide particles containing an oxide of a lanthanoid element in a combustion flame.
The film forming apparatus for effecting the impact sintering method has a combustion source supply port for supplying a combustion source and a combustion chamber connected thereto. By burning the combustion source in the combustion chamber, a combustion flame is generated in the combustion flame. A slurry supply port is disposed in the vicinity of the combustion flame. A yttrium oxide particle slurry containing an oxide of a lanthanoid element supplied from the slurry supply port is injected from the combustion flame to the substrate through a nozzle to form a film.
Oxygen, acetylene, kerosene and the like are used as the combustion source, and two or more kinds may be used if necessary. The combustion conditions such as the mixing ratio of the combustion source and the amount of the cooling gas are adjusted so that the temperature of the combustion flame is less than the boiling point of the yttrium oxide particles containing the oxide of the lanthanoid element to be formed.
When the temperature of the combustion flame is equal to or higher than the boiling point of the raw material particles, the yttria particles containing an oxide of a lanthanoid element to be supplied as a slurry are evaporated, decomposed or melted and do not deposit, or Even if it is deposited, it becomes a form similar to a warrior.
In the case of forming a yttrium oxide film containing an oxide of a lanthanoid element by the impact sintering method, it is preferable that the jetting rate of the yttrium oxide particle containing an oxide of a lanthanoid element is in a range of 400 m / sec to 1000 m / sec Do. If the spraying speed is slower than 400 m / sec, pulverization at the time of collision of particles becomes insufficient, and there is a fear that a film with high film density may not be obtained. If the jetting speed exceeds 1000 m / sec, the impact force becomes excessive, and the blast effect due to the yttria particles containing the oxide of the lanthanoid element tends to occur, and the desired film is hardly obtained.
When the yttrium oxide particle slurry containing the oxide of the lanthanoid element is put into the slurry feed port, it is preferable that the slurry is supplied to the center of the flame of the combustion flame.
When the yttrium oxide particle slurry is supplied outside the combustion flame, the injection speed is not stabilized. Yttrium oxide particles containing an oxide of a part of the lanthanoid-based element are injected outside the combustion flame and some of them reach the center and then are injected. Even at the same combustion flame, the combustion temperature is slightly different on the outside and inside. It is possible to control the structure including the " particles capable of confirming grain boundaries " and the " grain boundaries can not be confirmed " by forming the film at the same temperature condition and at the same jetting rate as possible.
The impact sintering method is a coating method in which particles are sprayed by a flame of a combustion flame, and the particles collide with each other at a high speed, and are sintered and bonded by the heat of the collision of the particles. As a result, yttria particles containing an oxide of a lanthanoid element in the coating tend to form a film in a crushed form rather than a particle shape of the raw material powder.
Further, by accelerating the jet velocity of the yttrium oxide particles containing the oxide of the lanthanoid element at a high speed and accelerating the particle velocity beyond the critical velocity at which the particles begin to deposit, the yttria yttrium oxide particles containing the oxide of the lanthanoid element are melted It is possible to obtain a yttrium oxide film containing an oxide of a lanthanum element having a high film density. Since the impact sintering method enables high-speed injection, it is easy to obtain " particles whose grain boundaries can not be confirmed ". The yttrium oxide film containing an oxide of a lanthanide element having an area ratio of particles which can be confirmed as grain boundaries of 0 to 80% and an area ratio of particles whose grain boundaries can not be confirmed is 20 to 100% .
It is also effective to adjust the spraying distance L from the nozzle to the substrate as a control method of the generation ratio of "particles capable of confirming grain boundaries" and "grain particles not capable of confirming grain boundaries". As described above, the impact sintering method is a method in which yttria particles containing an oxide of a lanthanoid element are sprayed at high speed using a combustion flame, and sintering is performed using the heat of destruction of the particles at the time of impact.
In order to form the yttria particles containing the oxide of the lanthanoid element heated by the flame of the combustion flame without forming the molten flattened shape, it is preferable to adjust the jetting distance L to 100 to 400 mm. If the spraying distance L is less than 100 mm, the distance is too close, so yttria particles containing the oxide of the lanthanoid element are not broken and it is difficult to obtain a sintered coating. On the other hand, if the spraying distance L exceeds 400 mm, since it is excessively spaced, the impact force is weakened and it is difficult to obtain a yttrium oxide film containing an oxide of the desired lanthanoid element. By controlling the yttria particle size including the above-described jetting speed and the oxide of the lanthanoid element as the raw material powder, the structure of melting and unmelting can be controlled. Preferably, the spraying distance L is 100 to 200 mm.
The yttrium oxide particle slurry containing an oxide of a lanthanoid element is preferably a slurry containing yttrium oxide particles containing an oxide of a lanthanoid element having an average particle diameter of 0.05 to 5 mu m as a raw material powder. The solvent for slurrying is preferably a solvent that is relatively volatile, such as methyl alcohol or ethyl alcohol.
It is preferable that the yttrium oxide particles containing an oxide of a lanthanoid element are sufficiently pulverized to be free of coarse particles and then mixed with a solvent. For example, when coarse particles having a particle diameter of 20 탆 or more are present, it is difficult to obtain a uniform film. The yttrium oxide particles in the slurry are preferably 30 to 80 vol%. The slurry having an appropriate fluidity is smoothly supplied to the supply port and the supply amount is stabilized, so that a uniform film can be obtained.
By using this impact sintering method, the crystal structure of the raw material powder (yttrium oxide particle slurry containing an oxide of the lanthanoid-based element) can constitute a yttrium oxide film containing an oxide of a lanthanoid-based element changed into monoclinic . For example, yttria is cubic at room temperature. The crystal structure changes when exposed to high temperatures such as a flame of a combustion flame. Since the impact sintering method can be sprayed at a high speed, it can be changed to a monoclinic state to form a yttrium oxide film containing an oxide of a lanthanoid element having high plasma resistance .
According to the above configuration, the plasma resistance in a component for a plasma etching apparatus is remarkably improved, and the reduction of particles, the reduction of impurity contamination, and the longevity of parts use are enabled. Therefore, in the case of the plasma etching apparatus using such components for the plasma etching apparatus, generation of particles and the number of parts replacement can be reduced in the plasma etching process.
Further, since the particles are sprayed at a high speed by the impact sintering method and the particles are deposited by the impact energy, blasting treatment is not required when depositing a coating film on the constituent parts, and no residual blast material or surface defects are generated , The adhesion of the film is improved. This is because the surface oxide film of the component is broken by the high-speed collision of the particles, and the active surface is exposed, so that a film is formed directly on the surface of the component, the subsequent particle collision causes bonding due to heat generation due to particle breakage, As shown in Fig.
Therefore, generation of particles due to peeling of the yttrium oxide film deposited on the component can be effectively suppressed, and the number of times of device cleaning and parts replacement can be greatly reduced. In addition, the reduction in the amount of generated particles greatly contributes to the improvement of the yield of various thin films to be etched or deposited in the semiconductor manufacturing apparatus, and further, the devices and parts using the thin films. Further, the number of times of device cleaning and the number of parts replacement are reduced, and the service life of the parts is increased by eliminating the necessity of blast treatment, which contributes greatly to the improvement of the productivity and the reduction of the etching cost.
<Examples>
Hereinafter, embodiments of the present invention will be described in more detail with reference to the following embodiments.
(Examples 1 to 8 and Comparative Example 1)
Various oxide ceramics were added to yttrium oxide on the alumina base material (300 mm x 3 mm) under the conditions shown in Table 1 by the impact sintering method using the combustion flame injection device to form a film, thereby forming a part for a plasma apparatus. The solvent of the yttrium oxide particles and the other oxide particle slurry was all ethyl alcohol. In addition, high purity oxide particles having a purity of 99.9% or more were used as raw material powders to be used. The Y 2 O 3 particles as the raw material powder were cubic, and raw material powders free of coarse particles exceeding 10 μm by sufficient pulverization and sieving were used.
In Comparative Example 1, yttrium oxide powder having an average particle size of 14 占 퐉 was used as a raw material, and the film was formed by the plasma spraying method.
Next, with respect to each yttrium oxide film formed in each of the examples and the comparative examples, the film density, the area ratio of the particles whose grain boundaries can be confirmed, the area ratio of the particles whose grain boundaries can not be confirmed, and the grain boundaries within each yttrium oxide film The average particle size and crystal structure of the particles were analyzed.
The film density was determined by taking an enlarged photograph (500 times) such that the total unit area of the film cross-section was 200 占 퐉 占 200 占 퐉 and the ratio of the pores to the area. The area ratio of the particles which can confirm the grain boundaries and the grain boundaries that can not be confirmed can be obtained by taking an enlarged photograph (magnification: 5000 times) of the unit area of 20 μm × 20 μm on the coating surface, And the area ratio was calculated by referring to "particles that can identify the grain boundary" and "grain boundaries that can not be identified by combining the grain boundary". This operation was carried out at arbitrary three sites, and the average value thereof was defined as the area ratio (%) of the "particles capable of confirming grain boundaries" and "grain particles not identifiable". Further, the same enlarged photograph was used to determine the average grain size of " grains capable of confirming grain boundaries ".
The crystal structure was also investigated by XRD analysis. XRD analysis was carried out using a Cu target under the conditions of a tube voltage of 40 kV and a tube current of 40 mA, and the ratio (Im / Ic) of the strongest peak Im to the strongest peak Ic of the cubic crystal was examined. The results are shown in Table 2 below.
As apparent from the results shown in Table 2, the yttrium oxide film containing the oxide of the lanthanoid element according to each Example had a high film density and a ratio (area ratio) of " To 80%. Further, by using the impact sintering method, the particles were slightly smaller than the size of the raw material powder. Further, since it was not melted more than necessary, the crystal structure was the same as that of the raw material powder.
The surface roughness Ra of the yttrium oxide coating films in Examples 1 to 8 was 0.5 m or less. The surface roughness Ra of the coating film in Comparative Example 1 was 3.1 占 퐉.
Subsequently, the parts for the plasma etching apparatuses according to each of the examples and the comparative examples were placed in a plasma etching apparatus and exposed to mixed etching gas of CF 4 (50 sccm) + O 2 (20 sccm) + Ar (50 sccm). The inside of the etching chamber was set at 10 mTorr, and the sample was continuously operated for 2 hours at an output of 300 W (bias of 100 W). Then, the adhesion area ratio of the detacking adhered particles was measured for each yttrium oxide film by a tape peeling method . Specifically, after the conductive carbon tape was attached to each yttrium oxide film, the tape was removed and the tape was observed by SEM to measure the area of each yttrium oxide particle present in the field of view of 125 mu m x 95 mu m. Further, the change in weight of the part before and after the above test was measured, and the weight loss per unit area was obtained. The results are shown in Table 3 below.
The volume resistivity of each yttrium oxide film was measured by a four-terminal method (in accordance with JIS K 7194) at room temperature (25 ° C), and was found to be in the range of 1.2 to 1.5 × 10 12 Ω · cm.
As is clear from the results shown in Table 3, it was found that the components for plasma devices according to the respective Examples had strong resistance to plasma attack and radical attack. Plasma attack and strong resistance to radical attack means that generation of particles can be effectively suppressed when used in a dry etching apparatus. These effects were further improved when lanthanum oxide was added to yttrium oxide.
In the above examples, the case where the base material contains alumina ceramics is exemplified, but it has been confirmed by experiments that the same effect is exhibited even when a metal base material is used.
INDUSTRIAL APPLICABILITY As described above, according to the component for a plasma apparatus according to the present invention, particles generated from component parts can be stably and effectively prevented. In addition, since corrosion of the coating film against the active radical of the corrosive gas is suppressed, it is possible to prevent the generation of particles from the coating film, and it is possible to suppress the generation of particles due to prevention of fallout as well as reduction of corrosion products. Therefore, it is possible to reduce the number of times of cleaning and parts replacement of the plasma device parts.
1: Parts for plasma processing apparatus
2: Yttrium oxide film containing an oxide of a lanthanoid-based element
3: substrate
4: Yttrium oxide particles containing an oxide of a lanthanoid-based element whose grain boundaries can not be confirmed
5: Yttrium oxide particles containing an oxide of a lanthanoid element capable of confirming grain boundaries
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