US20090101070A1 - Member for a Plasma Processing Apparatus and Method of Manufacturing the Same - Google Patents

Member for a Plasma Processing Apparatus and Method of Manufacturing the Same Download PDF

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Publication number
US20090101070A1
US20090101070A1 US12/224,784 US22478407A US2009101070A1 US 20090101070 A1 US20090101070 A1 US 20090101070A1 US 22478407 A US22478407 A US 22478407A US 2009101070 A1 US2009101070 A1 US 2009101070A1
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United States
Prior art keywords
film
plasma processing
processing apparatus
substrate
sol
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US12/224,784
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English (en)
Inventor
Tadahiro Ohmi
Masafumi Kitano
Yoshihumi Tsutai
Keisuke Satou
Mabito Iguchi
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Tohoku University NUC
NTK Ceratec Co Ltd
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Tohoku University NUC
Nihon Ceratec Co Ltd
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Assigned to NIHON CERATEC CO., LTD., TOHOKU UNIVERSITY reassignment NIHON CERATEC CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KITANO, MASAFUMI, OHMI, TADAHIRO, IGUCHI, MABITO, SATOU, KEISUKE, TSUTAI, YOSHIHUMI
Publication of US20090101070A1 publication Critical patent/US20090101070A1/en
Abandoned legal-status Critical Current

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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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid phase
    • 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
    • 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
    • C04B41/5031—Alumina
    • 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
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/042—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/228—Other specific oxides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes

Definitions

  • This invention relates to a member for a plasma processing apparatus for manufacturing an electronic component, such as a semiconductor device and a liquid crystal panel, and to a method of manufacturing the same.
  • a film forming process and a dry etching process which are carried out by plasma processing on a Si wafer and a glass substrate.
  • various corrosive gases are used.
  • a conventional chamber inner wall is made of metal and exposed in an uncovered state inside a chamber.
  • a permissible level of metal contamination is becoming extremely low.
  • plasma having a higher density is used year after year.
  • a ceramic sintered body is becoming used which exhibits high corrosion resistance against the plasma and the corrosive gases.
  • an electronic component manufacturing apparatus disclosed in Patent Document 1 uses a member using the ceramic sintered body.
  • an electronic component manufacturing apparatus disclosed in Patent Document 2 has a member obtained by forming a ceramic film (sprayed film) by using the spraying method.
  • ceramic powder having a high melting point is melted by electric energy or gas energy and sprayed onto a substrate. Therefore, insufficient melting of a ceramic material is easily caused to occur. In case where melting of the ceramic material is insufficient, open pores or consecutive pores are generated on the sprayed film. Also, countless microcracks are generated on the sprayed film due to quenching from a molten state. In a plasma processing chamber manufactured by using the member having the sprayed film, when a corrosive gas and plasma are brought into contact with the sprayed film, the corrosive gas penetrates the consecutive pores or the microcracks of the sprayed film to cause corrosion of the substrate to occur.
  • the sprayed film is formed to have a thickness of 100 ⁇ m or more in order to cover those defects due to the countless pores or microcracks. Between such a thick sprayed film and the metallic substrate, mismatch in linear expansion coefficient occurs. After repetition of temperature rising and cooling in plasma processing, the sprayed film is peeled off due to the mismatch in linear expansion coefficient.
  • the ceramic film by preparing a solution (sol) in which a metallic compound or a fine powder raw material is dispersed, applying the solution to a surface of the substrate by a simple device, such as a spray nozzle, and carrying out heat treatment.
  • a sol-gel method Such a method is called a sol-gel method.
  • the method is a prior and existing technique, it is possible to form a ceramic film excellent in film formability, durability, and reliability.
  • Patent Document 1 JP-B-3103646
  • Patent Document 2 JP-A-2001-164354
  • Non-Patent Document 1 “Sintering of Ceramics” written by Yusuke Moriyoshi et al, published by Uchida Rokakuho on Dec. 15, 1995
  • the ceramic film of the member for a plasma processing apparatus is required to have a purity not less than 98%.
  • heat treatment at a high temperature for example, 700° C. or higher
  • the substrate of the member for a plasma processing apparatus a substrate made of Al is often used. Since Al has a low melting point (approximately 600° C.), the substrate made of Al is susceptible to deformation or composition change if it is exposed to a temperature not lower than 400° C.
  • the sol-gel method in order to execute the sol-gel method at a low temperature capable of preventing deformation or composition change of Al, it is necessary to mix various impurities, such as alkali metal and heavy metal, into a sol or to form a glass layer in the film. In this case, a high purity ceramic film having high corrosion resistance can not be formed. Further, in the ceramic film formed at a comparatively low temperature, bonding strength between granular components is low. Therefore, generation of particles is highly possible.
  • the sol-gel method when used as a method of manufacturing the member for a plasma processing apparatus in order to obtain the member excellent in film formability, durability, and reliability, there is a problem in obtaining a high purity ceramic film and in preventing deformation or composition change of a substrate made of low-melting-point metal.
  • a member for a plasma processing apparatus comprising a substrate and a ceramic film formed thereon and having a purity not less than 98%, in which the ceramic film is constituted by grains having a grain diameter not greater than 50 nm, the amount of moisture released from the film being not more than 10 19 molecules/cm 2 .
  • the member for a plasma processing apparatus comprising, as the ceramic film, a sol-gel film formed by a sol-gel method.
  • the substrate is made of metal, ceramics, glass, or a composite material thereof, the ceramic film being a film comprising at least one kind of element selected from group II-VI elements, group XII-XIV elements, and rare-earth elements in the periodic table.
  • the ceramic film is a film comprising at least one kind of element selected from Mg, Al, Si, Ti, Cr, Zn, Y, Zr, W, and the rare-earth elements.
  • the member for a plasma processing apparatus comprising, as the ceramic film, a sprayed film formed on the substrate by a spraying method and a sol-gel film formed on the sprayed film by a sol-gel method.
  • the member for a plasma processing apparatus comprising, as the ceramic film, a sol-gel film formed on the substrate by a sol-gel method and a sprayed film formed on the sol-gel film by a spraying method.
  • the member for a plasma processing apparatus in which the substrate has a plate-like shape having pores, a tubular shape, or a container shape.
  • a method of manufacturing a member for a plasma processing apparatus comprising the step of forming a ceramic film having a purity not less than 98% on a substrate, in which the forming of the ceramic film is carried out so that grains constituting the film have a grain diameter not greater than 50 nm and the amount of moisture released from the film is not more than 10 19 molecules/cm 2 .
  • the method of manufacturing a member for a plasma processing apparatus comprising the steps of forming the substrate made of metal, ceramics, glass, or a composite material thereof; and forming, as the ceramic film, a film comprising at least one kind of element selected from group II-VI elements, group XII-XIV elements, and rare-earth elements in the periodic table.
  • the method of manufacturing a member for a plasma processing apparatus of the aspect (14), comprising the steps of forming the substrate made of metal; and forming, on a surface of the substrate, a film obtained by passivation of the surface of the substrate.
  • the member for a plasma processing apparatus according to the present invention is excellent in film formability, durability, and reliability.
  • the sol-gel film in the present invention is highly dense and highly flat and smooth and therefore has high plasma resistance in a high density plasma environment. Further, also in a corrosive gas environment and in a chemical environment, the sol-gel film exhibits high gas resistance and high chemical resistance because the film is highly dense so as to protect a substrate.
  • film formation is easily performed by pouring a liquid sol or by dipping.
  • FIG. 1 is a graph for describing a characteristic of a member for a plasma processing apparatus according to a first example of the present invention, showing measurement data of the amount of moisture released from an Y 2 O 3 film.
  • FIG. 2 is a graph for describing the characteristic of the member for a plasma processing apparatus according to the first example of the present invention, showing the amount of moisture released at each of temperature rising stages.
  • FIG. 3 is a graph for describing the characteristic of the member for a plasma processing apparatus according to the first example of the present invention, showing a relationship between a firing temperature and the amount of moisture released when a temperature is increased up to 500° C.
  • FIG. 4 is a schematic sectional view showing a member for a plasma processing apparatus according to a second example of the present invention.
  • FIG. 5 is a schematic sectional view showing a member for a plasma processing apparatus according to a third example of the present invention.
  • FIG. 6 is a schematic sectional view showing a member for a plasma processing apparatus according to a fourth example of the present invention.
  • FIG. 7 is a schematic sectional view showing a member for a plasma processing apparatus according to a fifth example of the present invention.
  • FIG. 8 is a schematic sectional view showing a member for a plasma processing apparatus according to a sixth example of the present invention.
  • FIG. 9 is a schematic sectional view showing a member for a plasma processing apparatus according to a seventh example of the present invention.
  • FIG. 10 is a table showing evaluation results for the members for a plasma processing apparatus according to the present invention together with evaluation results for comparative examples.
  • FIG. 11 is a graph for describing a characteristic of the member for a plasma processing apparatus according to the example of the present invention, showing a transmittance of a sample 10 as the example at a visible light wavelength in a range between 400 and 800 nm.
  • FIG. 12 is a graph for describing a characteristic of the member for a plasma processing apparatus according to the example of the present invention, showing a transmittance of a sample 11 as the example at a visible light wavelength in a range between 400 and 800 nm.
  • FIG. 13 is a graph for describing a characteristic of the member for a plasma processing apparatus according to the example of the present invention, showing a transmittance of a sample 12 as the example at a visible light wavelength in a range between 400 and 800 nm.
  • FIG. 14 is a graph for describing a characteristic of the member for a plasma processing apparatus according to the example of the present invention, showing a transmittance of a sample 37 as a comparative example at a visible light wavelength in a range between 400 and 800 nm.
  • a member for a plasma processing apparatus has a ceramic film which is formed by a sol-gel method, which has a purity not less than 98%, and which has plasma resistance and corrosive gas resistance.
  • a method of manufacturing a member for a plasma processing apparatus comprises a step of forming a ceramic film on a substrate by the sol-gel method, which has a purity not less than 98% and has plasma resistance and corrosive gas resistance.
  • a member for a plasma processing apparatus which comprises a substrate made of a material, such as metal, ceramics, and glass, generally used as a structural material and having a surface coated with a ceramic film made of an oxide formed of group II-VI elements, group XII-XIV elements, and rare-earth elements, or a composite oxide formed of two or more kinds of the above-mentioned elements.
  • the sol-gel method is used.
  • the dipping method is a method of coating a substrate surface with a uniform sol film by dipping a substrate into a solution and thereafter pulling out the substrate at a low speed (10 to 50 mm per minute) and at a constant rate.
  • this technique is characterized in that a ceramic thin film having a high purity from 98% to 99.99% can be obtained at such a low temperature of 250° C.
  • the above-mentioned technique is applicable to composite formation by surface coating onto a sprayed film, composite formation by application of a sprayed film after formation of a sol-gel film on a substrate, and a composite film formed by film formation for passivation of a substrate, such as an anodic oxidation film and a fluoride film.
  • a grain diameter of the sol-gel film in the present invention was observed by using a field-emission-type scanning electron microscope (JEM-6700F manufactured by JEOL Ltd.). As a result, it was confirmed that all grains constituting the film had a grain diameter not greater than 50 nm.
  • a grain diameter of a ceramic film is not smaller than 100 nm.
  • the present invention by achieving a grain diameter not greater than 50 nm, it is possible to perform film formation with a high purity (98% or more) and at a low temperature of 250° C.
  • Non-Patent Document 1 describes that, as grains become smaller, grain boundary diffusion and volume diffusion contributing to sintering are relatively increased and this relationship is extremely effective when a material having a high steam pressure and difficult to be densified is sintered and that, when a grain diameter becomes smaller, the number of contact points per unit volume is increased and the number of generation points and disappearance points of atoms involved in mass transfer is increased, thereby providing a state preferable for densification.
  • a high purity can be achieved only by the sol-gel method.
  • Samples 1 to 29 as examples of the present invention and samples 31 to 37 as comparative examples were manufactured. For those samples, some characteristics were verified and evaluated. Results thereof are shown in a table of FIG. 10 .
  • Each of the samples 1 to 29 as the examples of the present invention comprises a substrate made of one of various materials shown in a substrate-column in the table and having a 50 to 200 mm square size and a ceramic film formed on a surface of the substrate by a film formation method including at least a sol-gel method.
  • film formation was carried out by spraying a sol as a raw material onto the substrate by a spray nozzle. Further, an electric furnace was used for heat treatment.
  • the amount of moisture released from a ceramic film formed on a Si substrate was observed.
  • the amount of released moisture was measured by an atmospheric pressure ionization mass spectrometry device (APIMS: UG-302P manufactured by Renesas Eastern Japan Semiconductor, Inc.).
  • Each sample is placed in a reactor tube manufactured by using an electrolytically-polished pipe of SUS316L having a size of 1 ⁇ 2 inch.
  • a high-purity Ar gas having an impurity concentration of 1 ppb or less is used as a carrier gas. This is a system in which the Ar gas is made to pass over the sample at a flow rate of 1.2 L/min and the amount of moisture released from the sample is measured by the APIMS.
  • a temperature profile at a time of measurement of the amount of moisture released from the ceramic film was set as follows. After the ceramic film was kept at a temperature of 25° C. for 10 hours, the temperature was increased up to 100° C. in 10 minutes. Then, the ceramic film was kept at 100° C. for 1 hour and 50 minutes. Thereafter, the temperature was increased stepwise by every 100° C. up to 500° C. During the above-mentioned period, the amount of released moisture was measured.
  • FIG. 1 shows measurement data of the amount of moisture released from an Y 2 O 3 film.
  • a horizontal axis shows a measurement time by the APIMS and a vertical axis shows the number of water molecules released per unit area.
  • the samples were prepared by firing at 300° C., 600° C., and 900° C. in the atmosphere and had a film thickness of 1 ⁇ m.
  • FIG. 2 shows a graph plotting the amount of released moisture at each temperature rising stage with respect to temperature reciprocals (1/K) for 25° C., 100° C., 200° C., 300° C., 400° C., and 500° C. It was confirmed that an activation energy Ea of moisture desorption was 0.055 eV regardless of a firing temperature. This suggests that a film quality of a surface is not changed at all and only an effective surface area is decreased. Further, it was confirmed that the amount of moisture released during the temperature rising up to 500° C. was 4.23 ⁇ 10 18 molecules/cm 2 for the samples fired at 300° C., 1.75 ⁇ 10 18 molecules/cm 2 for the samples fired at 600° C., and 6.31 ⁇ 10 17 molecules/cm 2 for the samples fired at 900° C.
  • FIG. 3 shows a relationship between the firing temperature and the amount of moisture released when the temperature is raised up to 500° C.
  • the firing temperature As the firing temperature is increased, a bonding strength at a grain boundary between Y 2 O 3 crystal grains is increased and the effective surface area is decreased. Hence, it is understood that the amount of released moisture is significantly decreased. Further, it is understood that, with the firing temperature not lower than 300° C., the amount of moisture released from the film is not more than 10 19 molecules/cm 2 .
  • a passivation film or the like was formed as a base on a surface of a substrate made of aluminum (Al) or stainless steel (SUS) and a sol-gel film was formed on the base, as shown in FIG. 5 . Then, evaluation was performed. With respect to a SUS substrate of the sample 15, a passivation film made of Cr 2 O 3 was formed as a base on a surface of the substrate and a sol-gel film was further formed thereon. Then, evaluation was performed.
  • an anodic oxidation film was formed as a base by oxidizing Al of a substrate surface by electric field treatment in a solution and a sol-gel film was further formed. Then, evaluation was performed.
  • a MgF 2 film was formed as a base by fluoridizing a substrate surface, and a sol-gel film was further formed. Then, evaluation was performed.
  • evaluation was performed on a composite film obtained by forming the sprayed film and thereafter forming the sol-gel film on a surface thereof, as shown in FIG. 6 .
  • evaluation was performed on a composite film having a sandwich structure obtained by forming a sol-gel film as a base, forming a sprayed film thereon, and forming another sol-gel film on a surface thereof, as shown in FIG. 8 .
  • evaluation was performed on a composite film obtained by forming an anodic oxidation film as a base, forming the sprayed film thereon, and further forming a sol-gel film formed on a surface thereof, as shown in FIG. 9 .
  • the samples 31 to 37 as comparative examples were made of various substrates shown in the table of FIG. 10 and ceramic films were formed by using the spraying method, a thermal CVD method, or a conventional sol-gel method.
  • the conventional sol-gel method is a method in which a structure and a purity of the ceramic film are out of the scope of the present invention.
  • GDMS low-discharge mass spectrometry
  • VG9000 manufactured by Fl. Elemental was used as an analyzer.
  • a plasma processing apparatus requires severer impurity control with miniaturization of a printed circuit and so on. Hence, in order to improve a yield of an electronic component, a higher-purity ceramic film is required.
  • the sol-gel film in each of the samples 1 to 29 as the examples of the present invention has a purity not less than 99%.
  • the conventional sol-gel film in each of the samples 31 and 32 as the comparative examples contains a large amount of alkali metal for the purpose of technically enabling low-temperature film formation. Accordingly, the purity is about 85% and does not reach 98% or more.
  • the sprayed film in each of the samples 33 and 34 as the comparative examples has a purity of 99%.
  • the CVD film in each of the samples 35 to 37 as comparative examples has a purity of 95%.
  • a 6-inch silicon wafer was placed and a mirror-polished test specimen was placed thereon. Then, a corrosion test was performed by plasma exposure in plasma of CF 4 +O 2 for 10 hours. During the test, a part of a polished surface was masked with a polyimide tape and a silicon wafer. A difference in level between the masked part and an unmasked part was measured by a stylus method to calculate an etching rate.
  • Ceramics used herein as the examples is an oxide comparatively resistant against the plasma. Therefore, the amount of etching of its surface is very small.
  • the number of grains having a size of 0.5 micron or more was measured by using a particle counter (Surfscan6420 manufactured by Tencor).
  • the number of particles With respect to the number of particles, an excellent result was obtained by the sol-gel film which is a dense and flat film in comparison with other film formation methods. It is noted here that, since each of the samples 19 to 23 as the examples of the present invention has the sprayed film as the outermost surface, the number of particles is increased similarly to the samples 33 and 34 as the comparative examples. However, in each of the samples 19 to 23 and 26 and 27 as the examples of the present invention in which the sol-gel film is formed on a surface of the sprayed film, the number of particles is decreased to about one third of that of the samples with the sprayed film only, although the number of particles is increased in comparison with the simple sol-gel films. Thus, by applying the sol-gel film, an effect of decreasing the particles was obtained.
  • an apparatus for manufacturing a semiconductor device has an internal environment constantly exposed to a corrosion gas in each process.
  • a film in each of the examples was exposed to a Cl 2 gas to evaluate corrosion gas resistance.
  • test specimen was placed in a sample mounting cell and a gas exposure test was carried out in an air stream containing 100% Cl 2 gas and having a pressure of 0.3 MPa for 24 hours.
  • a temperature in the cell was kept at 100° C.
  • a surface condition after the gas exposure was checked and presence or absence of surface corrosion or presence or absence of peeling was used as an evaluation criterion.
  • Judgment was made about whether or not film formation is possible onto a complicated configuration, such as two or more steps and an inner surface of a box shape, an inner surface of a cylinder having a small diameter (for example, a gas pipe having an inner diameter of about 5 mm), an inside of a porous body, and an inside of a fibrous filter.
  • a complicated configuration such as two or more steps and an inner surface of a box shape, an inner surface of a cylinder having a small diameter (for example, a gas pipe having an inner diameter of about 5 mm), an inside of a porous body, and an inside of a fibrous filter.
  • the conventional sol-gel film could flexibly be formed onto a comparatively complicated configuration.
  • film formation with corners or a sharp R shape film peeling occurred due to low adhesion.
  • film formation is performed only in a region where a frame with a sprayed material melted thereon can be linearly irradiated. Therefore, film formation was impossible onto a substrate with a shaded part formed therein.
  • the CVD film is not formed unless a surface on which a film is to be formed is completely exposed to a material gas supplied. Further, in case where a film formation surface has both a parallel plane and an orthogonal plane, film formation rates thereof are extremely widely varied. Therefore, uniform film formation was impossible.
  • a material solution (sol) was supplied to pass therethrough, dried, and thereafter fired.
  • sol-gel method film formation was possible onto those members having the above-mentioned configurations although it was impossible by the conventional technique.
  • spraying method and the CVD method in the comparative examples film formation throughout the entire surface was impossible in principle.
  • film formation was possible by using the conventional sol-gel method, application to the member for a plasma processing apparatus is difficult in view of purity and particles.
  • the substrates themselves exhibit translucency. Therefore, a transmittance at a visible light wavelength between 400 and 800 nm was measured. In the measurement, a self-recording spectrophotometer (U-3500 manufactured by Hitachi, Ltd.) was used. Results of transmittances of the samples 10 to 12 are shown in FIGS. 11 to 13 , respectively. As a comparative example, a transmittance of the CVD film is shown in FIG. 14 .
  • a transmittance decreases.
  • decrease in transmittance in a visible light range does not substantially occur if a film thickness is between 1 ⁇ m and 5 ⁇ m, as shown in FIGS. 11 to 13 .
  • the transmittance is kept at about 90% throughout an entire wavelength range. Considering that 4 mm thick quartz as a substrate has a transmittance of about 93% throughout an entire wavelength range, it is understood that a transmittance of the film alone is calculated to about 97%.
  • the CVD film has a transmittance which remarkably decreases to about 50 to 80% at a film thickness of 1 ⁇ m. Further, the sprayed film and the conventional sol-gel film do not exhibit translucency because a large number of pores are contained and the film is thick.
  • the present invention is applicable not only to an electronic component manufacturing apparatus, such as a semiconductor element and a liquid crystal panel, but also to a member for use in all apparatuses for conducting plasma processing or the like with a corrosive atmosphere and to a method of manufacturing the same.

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  • Chemical Vapour Deposition (AREA)
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PCT/JP2007/053002 WO2007111058A1 (ja) 2006-03-27 2007-02-20 プラズマ処理装置用部材およびその製造方法

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FR2988404A1 (fr) * 2012-03-21 2013-09-27 Ct Tech Des Ind Mecaniques Procede de depot d'un revetement anticorrosion
US9551062B2 (en) 2013-03-28 2017-01-24 Osg Corporation Hard film for machining tools and hard film-coated metal machining tool

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JP5411460B2 (ja) * 2008-06-24 2014-02-12 一般財団法人ファインセラミックスセンター バリア性能評価方法及びバリア性能評価装置
KR101290539B1 (ko) * 2013-04-15 2013-07-31 와이엠씨 주식회사 아노다이징 필름 제조 방법
CN103639157B (zh) * 2013-11-15 2016-06-08 广州福耀玻璃有限公司 玻璃附件的表面处理方法
TW201546007A (zh) * 2014-06-11 2015-12-16 Creating Nano Technologies Inc 玻璃結構之製造方法與設備
TWI709653B (zh) * 2018-02-15 2020-11-11 日商京瓷股份有限公司 電漿處理裝置用構件及具備其之電漿處理裝置
CN113272474A (zh) * 2019-01-10 2021-08-17 日本碍子株式会社 散热部件
JP2020132947A (ja) * 2019-02-20 2020-08-31 日本特殊陶業株式会社 膜付き部材及びその製造方法
WO2023275958A1 (ja) * 2021-06-28 2023-01-05 株式会社日立ハイテク 内壁部材の再生方法

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US9551062B2 (en) 2013-03-28 2017-01-24 Osg Corporation Hard film for machining tools and hard film-coated metal machining tool

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JP5014656B2 (ja) 2012-08-29
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WO2007111058A1 (ja) 2007-10-04
CN101432461A (zh) 2009-05-13
KR101030937B1 (ko) 2011-04-28

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