WO2007111058A1 - Élément structural pour un système de traitement par plasma et son procédé de fabrication - Google Patents

Élément structural pour un système de traitement par plasma et son procédé de fabrication Download PDF

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Publication number
WO2007111058A1
WO2007111058A1 PCT/JP2007/053002 JP2007053002W WO2007111058A1 WO 2007111058 A1 WO2007111058 A1 WO 2007111058A1 JP 2007053002 W JP2007053002 W JP 2007053002W WO 2007111058 A1 WO2007111058 A1 WO 2007111058A1
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Prior art keywords
film
plasma processing
processing apparatus
sol
base material
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PCT/JP2007/053002
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English (en)
Japanese (ja)
Inventor
Tadahiro Ohmi
Masafumi Kitano
Yoshihumi Tsutai
Keisuke Satou
Mabito Iguchi
Original Assignee
Tohoku University
Nihon Ceratec Co., Ltd.
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Publication date
Application filed by Tohoku University, Nihon Ceratec Co., Ltd. filed Critical Tohoku University
Priority to US12/224,784 priority Critical patent/US20090101070A1/en
Priority to KR1020087025800A priority patent/KR101030937B1/ko
Publication of WO2007111058A1 publication Critical patent/WO2007111058A1/fr

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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

  • the present invention relates to a member for a plasma processing apparatus for manufacturing an electronic component such as a semiconductor device or a liquid crystal panel, and a manufacturing method thereof.
  • a ceramic sintered body exhibiting high corrosion resistance against plasma and corrosive gas has been used as a member exposed in a chamber (plasma processing chamber).
  • the electronic component manufacturing apparatus disclosed in Patent Document 1 uses a member using a ceramic sintered body.
  • a member formed by forming a ceramic film on a surface of a metal base material that is low in cost, excellent in workability, and easy to increase in size using a thermal spraying method has been adopted in a plasma processing chamber.
  • Such a member has the same corrosion resistance as the ceramic sintered body.
  • an electronic component manufacturing apparatus disclosed in Patent Document 2 has a member formed by forming a ceramic film (sprayed film) using a thermal spraying method.
  • the thermal spraying method is a high melting point ceramic powder melted by electricity or gas energy. Since the powder is sprayed onto the base material, the ceramic raw material is likely to be insufficiently melted. When the ceramic raw material is insufficiently melted, open pores and continuous pores are formed in the sprayed film. In addition, countless microcracks are generated in the sprayed film due to the rapid cooling of the molten state. When a corrosive gas or plasma comes into contact with the sprayed film in a plasma processing chamber manufactured using a member with a sprayed film, the corrosive gas penetrates through the continuous pores or microcracks of the sprayed film, causing corrosion of the substrate. To do. Eventually, problems such as peeling of the sprayed film occur.
  • the sprayed film is formed with a thickness of 100 / zm or more in order to compensate for defects caused by countless pores and microcracks.
  • the coefficient of linear expansion becomes inconsistent between the thick sprayed film and the metal base material. Due to the mismatch of the linear expansion coefficients, the sprayed film peels off after repeated heating and cooling in the plasma treatment.
  • a sol-gel method which is a conventional technique, and can form a ceramic film having excellent film forming properties, durability, and reliability.
  • Patent Document 1 Japanese Patent No. 3103646
  • Patent Document 2 JP 2001-164354 A
  • Non-patent document 1 "Sintering of ceramics”: written by Keisuke Moriyoshi et al., Published by Uchida Oirakuno, December 15, 1995
  • the use of the sol-gel method as a method for forming a ceramic film of a plasma processing apparatus member has the following problems.
  • the ceramic film of the plasma processing apparatus member is desired to have a purity of 98% or more. Yes.
  • heat treatment at a high temperature eg, 700 ° C or higher
  • a material having A1 force is often used as a base material for a member for a plasma processing apparatus. Substrates with A1 force are prone to deformation and composition changes when exposed to temperatures above 400 ° C due to the low melting point of A1 (approximately 600 ° C).
  • a member for a plasma processing apparatus having excellent film formability, durability, and reliability is obtained.
  • a sol-gel method is used as a method for manufacturing a member for a plasma processing apparatus, a high-purity ceramic film is obtained.
  • an object of the present invention is to solve the problems of the prior art and to provide a member for a plasma processing apparatus that is excellent in film formability, durability, and reliability.
  • Another object of the present invention is to provide a method for manufacturing a member for a plasma processing apparatus, which can manufacture the member for a plasma processing apparatus as described above.
  • the ceramic film has a particle diameter of particles constituting the film of 50 nm or less, A member for a plasma processing apparatus, wherein the amount of water released from the membrane is 10 19 molecules Zcm 2 or less.
  • the base material is also made of metal, ceramics, glass, or a composite material force thereof.
  • the ceramic film is a film composed of at least one element selected from Group 2 to 6 elements, Group 12 to 14 elements, and rare earth elements in the periodic table (1).
  • the ceramic film is a film composed of at least one element selected from Mg, Al, Si, Ti, Cr, Zn, Y, Zr, W, and a rare earth element.
  • a member for a plasma processing apparatus characterized by having a sol-gel film formed on the sprayed film by a sol-gel method.
  • the ceramic film includes a sol-gel film formed on the base material by a sol-gel method and a sprayed film formed on the sol-gel film by a spraying method ( The member for plasma processing apparatus of 1)-(10).
  • a plasma having a step of forming a ceramic film having a purity of 98% or more on a substrate The method of manufacturing a Ma processor member, in the ceramic film formation process, the particle size of the particles constituting the film is not less 50nm or less, and the amount of moisture released from the film and a 10 1 9 molecule ZCM 2 below
  • a method for producing a member for a plasma processing apparatus characterized by comprising:
  • the method includes the step of forming the base material made of a metal, and the step of forming a film formed by passivating the surface of the base material on the surface of the base material.
  • a mode (14) comprising the step of forming the base material made of metal and the step of forming a film formed by heat treatment on the surface of the base material (19)
  • a method for manufacturing a member for a plasma processing apparatus [0040]
  • the ceramic film forming step includes a step of forming a sprayed film on the base material by a spraying method and a step of forming a sol-gel film on the sprayed film by a sol-gel method.
  • the ceramic film forming step includes a step of forming a sol-gel film on the substrate by a sol-gel method, and a step of forming a sprayed film on the sol-gel film by a spraying method.
  • the member for a plasma processing apparatus according to the present invention is excellent in film formability, durability, and reliability!
  • the sol-gel film of the present invention has high plasma resistance in a high-density plasma environment because it is highly dense and smooth. In addition, even in a corrosive gas environment or a chemical solution environment, the film is highly dense and can protect the substrate, and thus exhibits high gas resistance and chemical solution resistance.
  • the conventional technique cannot form a uniform film on a complicated shape or the inner surface of a tube.
  • a film can be easily formed by pouring or dipping a liquid sol. This is possible.
  • the dense sol-gel film blocks the corrosive gas and suppresses the peeling of the sprayed film. be able to.
  • FIG. 1 is a graph for explaining the characteristics of a member for a plasma processing apparatus according to Example 1 of the present invention, and shows measurement data of the amount of water released from a Y 2 O film.
  • FIG. 2 is a graph for explaining the characteristics of a member for a plasma processing apparatus according to Example 1 of the present invention, and shows the amount of moisture released at each temperature rising stage.
  • FIG. 3 is a graph for explaining the characteristics of the plasma processing apparatus member according to Example 1 of the present invention, and shows the relationship between the firing temperature and the amount of moisture released when the temperature is raised to 500 ° C. .
  • FIG. 4 is a schematic cross-sectional view showing a member for a plasma processing apparatus according to Example 2 of the present invention.
  • FIG. 5 is a schematic cross-sectional view showing a member for a plasma processing apparatus according to Example 3 of the present invention.
  • FIG. 6 is a schematic cross-sectional view showing a member for a plasma processing apparatus according to Example 4 of the present invention.
  • FIG. 7 is a schematic cross-sectional view showing a member for a plasma processing apparatus according to Example 5 of the present invention.
  • FIG. 8 is a schematic cross-sectional view showing a member for a plasma processing apparatus according to Example 6 of the present invention.
  • FIG. 9 is a schematic cross-sectional view showing a member for a plasma processing apparatus according to Example 7 of the present invention.
  • FIG. 10 is a table showing the evaluation results of the plasma processing apparatus member according to the present invention together with the evaluation results of the comparative example.
  • FIG. 11 is a drawing for explaining the characteristics of a member for a plasma processing apparatus according to an example of the present invention, and shows the transmittance of sample 10 as an example at a wavelength of visible light of 400 to 800 nm.
  • FIG. 12 is a drawing for explaining the characteristics of a member for a plasma processing apparatus according to an example of the present invention, and shows the transmittance of sample 11 as an example at a wavelength of visible light of 400 to 800 nm.
  • FIG. 13 is a drawing for explaining the characteristics of a member for a plasma processing apparatus according to an example of the present invention, and shows the transmittance of sample 12 as an example at a wavelength of visible light of 400 to 800 nm.
  • FIG. 14 is a drawing for explaining the characteristics of a member for a plasma processing apparatus according to an example of the present invention, and shows the transmittance of sample 37 as a comparative example at a wavelength of visible light of 400 to 800 nm.
  • the member for a plasma processing apparatus has a ceramic film having a purity of 98% or more formed by a sol-gel method and having plasma corrosion resistance and corrosion gas corrosion resistance.
  • the method for producing a member for a plasma processing apparatus is a method of producing a Sorge ceramic film having a purity of 98% or more and having plasma corrosion resistance and corrosion gas corrosion resistance on a substrate.
  • a material generally used as a structural material of metal, ceramics, and glass is used as a base material, and the surface thereof is formed from a 2-6 group element, a 12-14 group element, or a rare earth element.
  • the oxide ceramics can be obtained by applying the sol-gel method, applying it to the substrate using the spray method, dipping method, etc., and heat-treating it in an oxygen-containing atmosphere of 250 ° C or higher. It is.
  • the spray method recommends the use of a nozzle with a special design and optimization, but it is also possible to obtain a similar film using a commercially available airbrush or spray gun. is there.
  • the dipping method is a method in which a uniform sol film is applied to the surface of a substrate by immersing the substrate in a solution and then pulling it up at a low speed (10 to 50 mm / min) and at a constant speed.
  • composite by surface coating on a sprayed film composite by applying a sprayed film after film formation of a sol-gel film on the substrate, and anodized film It can also be applied as a composite film by forming a film such as a fluoride film on the passive material treatment of a base material.
  • the particle size of the sol-gel film in the present invention was observed using a field emission scanning electron microscope (JEM-6700F, manufactured by JEOL Ltd.). As a result, it was confirmed that the particle sizes constituting the film were all 50 nm or less.
  • the ceramic film has a particle diameter of lOOnm or more. In the present invention, the particle diameter is 50 nm, so that high purity (98% or more) and low temperature film formation from 250 ° C can be achieved. It has become possible. This is because when the particle size of the sol-gel film is made finer to 50 nm or less, the sintering temperature is drastically lowered and sintering is started at about 250 ° C.
  • Non-Patent Document 1 the grain boundary diffusion and volume diffusion contributing to sintering increase relatively as the particles become smaller, and this relationship is extremely effective when sintering materials with high vapor pressures that are difficult to densify.
  • the smaller the particle size It is described that the number of contact points per unit volume increases, and the generation and disappearance locations of atoms related to mass transfer increase, leading to a favorable situation for densification. Therefore, it was possible to achieve high purity only by the sol-gel method, despite the processing temperature of less than 700 ° C!
  • Samples 31 to 37 as comparative examples were produced together with samples 1 to 29 as examples of the present invention.
  • Samples 1 to 29, which are examples of the present invention, are films containing at least a sol-gel method on a 50 to 200 mm square substrate surface that has various material strengths shown in the substrate column in the table.
  • a ceramics film is formed by this method.
  • the apparatus used for the formation of the ceramic film by the sol-gel method formed the film by spraying the sol as a raw material onto the substrate by a spray nozzle.
  • An electric furnace was used for heat treatment.
  • the amount of water released from the ceramic film formed on the Si substrate was investigated.
  • the amount of water released was measured with an atmospheric pressure ionization mass spectrometer (APIMS: UG-302P manufactured by Renesas East Japan Semiconductor Co., Ltd.).
  • the sample was placed in a reactor tube made of 1 / 2-inch SUS316L electrolytic polishing tube, and high-purity Ar gas with an impurity concentration of lppb or less was used as the carrier gas.
  • This is a system that allows Ar gas to pass through the sample at a flow rate of 1.2 LZmin and measures the moisture released from the sample with A PIMS.
  • the temperature profile at the time of measuring the amount of moisture released from the ceramic film was set as follows. Hold at 25 ° C for 10 hours, then heat up to 100 ° C in 10 minutes, hold at 100 ° C for 1 hour and 50 minutes, and then step up to 100 ° C to 500 ° C and release The amount of water was measured.
  • FIG. 1 shows measurement data of the amount of water released from the YO membrane.
  • the horizontal axis is measured by APIMS.
  • the fixed time and the vertical axis represent the number of water molecules released from the unit area.
  • Samples were sol-geled and fired in air at 300 ° C, 600 ° C, and 900 ° C, respectively, to a thickness of 1 ⁇ m.
  • FIG. C 100. C, 200. C, 300. C, 400. C, 500.
  • a graph plotting the amount of water released at each temperature increase stage against the reciprocal temperature of C ( ⁇ ) is shown. It was confirmed that the activity energy Ea of water desorption was 0.055 eV regardless of the firing temperature. This suggests that only the effective surface area, which does not change the surface film quality, has decreased. Also, the amount of water released at a temperature up to 500 ° C is 300 ° C calcined sample: 4.23 x 10 18 molecules / cm 2 , 600. C calcined sample: 1.75 x 10 18 molecules / cm 2 , 900. C-fired sample: 6. 31 X 10 17 molecules Zcm 2 was confirmed.
  • FIG. 3 shows the relationship between the firing temperature and the amount of water released when the temperature is raised to 500 ° C. As the calcination temperature increases, the bonding strength at the grain boundaries between the Y 2 O crystal grains increases, and the execution table
  • the amount of water released is greatly reduced.
  • the firing temperature is 300 ° C or higher, the amount of water released from the film is 10 19 molecules Zcm 2 or less.
  • a passivated film or the like is formed on the surface of a substrate made of aluminum (A1) or stainless steel (SUS). Then, a sol-gel film was formed on the base and evaluated.
  • the substrate surface is treated with a passivating treatment made of Cr 2 O, and further on it.
  • a sol-gel film was formed and evaluated.
  • the anodized film whose surface was oxidized by electric field treatment in the solution was used as the base, and a sol-gel film was further formed for evaluation. Carried out.
  • the A1 metal base material of Sample 18 an evaluation was performed by forming a fluorinated MgF film on the base material surface and further forming a sol-gel film.
  • the sprayed film was formed on the sol-gel film as a base.
  • the composite membrane was evaluated.
  • a sprayed film is formed with an anodized film as a base, and a sol-gel film is further formed on the surface.
  • the composite film when the film was formed was evaluated.
  • each sample 31 to 37 as a comparative example was made of various base materials shown in the table of FIG. 10, and a ceramic film was formed using a thermal spraying method, a thermal CVD method, or a conventional sol-gel method.
  • the conventional sol-gel method is a method in which the structure and purity of the ceramic film are outside the scope of the present invention.
  • the sol-gel films in Samples 1 to 29, which are examples of the present invention, have a purity of 99% or more.
  • the conventional sol-gel films in Comparative Samples 31 and 32 contain a large amount of alkali metal in order to technically enable low-temperature film formation, so the purity is about 85%. Yes, less than 98%.
  • the sprayed film in the comparative samples 33 and 34 has a purity of 99%, and the CVD film in the comparative samples 35 to 37 has a purity of 95%.
  • a parallel plate type RIE etching chamber is equipped with a 6-inch silicon wafer and a mirror-polished specimen, and CF +0 plasma for 10 hours.
  • Corrosion test by exposure was conducted. At that time, a part of the polished surface was masked with a polyimide tape and a silicon wafer, and the step between the portion with and without the mask was measured by a stylus method to calculate the etching rate.
  • the ceramic used as an example this time is an oxide that is relatively resistant to plasma, the etching amount on the surface is very small.
  • the number of particles having a size of 0.5 microns or more was measured using a particle counter (Surfscan 6420 manufactured by Tencor).
  • the sol-gel film which is a dense and flat film, has better results than other film forming methods.
  • the samples 19 to 23, which are examples of the present invention have a sprayed film on the outermost surface, so that the number of particles is increased as in the samples 33 and 34, which are comparative examples.
  • samples 19 to 23 and 26 and 27, which are examples of the present invention in which a sol-gel film is formed on the surface of the sprayed film have an increased number of particles compared to the sol-gel alone film, but only the sprayed film. The number of particles is about 1/3 compared to Decrease in degrees. Therefore, a particle reduction effect was obtained by applying a sol-gel film.
  • the membrane in each example was changed to C1 gas.
  • test piece was installed in a cell for sample installation, C1 gas 100%, 0.3 MPa
  • a 24-hour gas exposure test was conducted in a stream of pressure.
  • the temperature inside the cell was 100 ° C.
  • the surface condition after gas exposure was confirmed, and the presence or absence of surface corrosion or peeling was used as the evaluation standard.
  • the conventional sol-gel film can be formed flexibly with respect to a relatively complicated shape, but when the film is formed with a corner or a sharp R shape.
  • the film had poor adhesion and delamination.
  • a CVD film is not formed unless the surface on which the film is formed is completely exposed to the supplied source gas, and when both parallel and right-angle surfaces exist on the film formation surface, both of them are formed. Since the film rate changed extremely, uniform film formation was impossible.
  • the inner surface of the small-diameter cylinder, the inside of the porous body, and the inside of the fibrous filter were fired after passing through the raw material solution (sol) and drying.
  • sol-gel method it was possible to form a film on a member having the above-mentioned shape, which was impossible with the prior art.
  • the thermal spraying method and the CVD method shown in the comparative example were unable to form a film on the entire surface.
  • the conventional sol-gel method is used, a film can be formed, but the purity and the viewpoint of particles are difficult to apply to a member for a plasma processing apparatus.
  • the transmittance in the visible light region is less than 80% by visual observation, the film starts to appear cloudy. Also, when the transmittance is below 60%, the film appears to be cloudy. Therefore, when it is applied to a member that requires translucency, a transmittance of 80% or more is required to obtain good translucency.
  • the transmittance usually decreases as the film thickness increases.
  • the sol-gel film of the present invention has a film thickness of 1 ⁇ as shown in Figs. If it is ⁇ 5 / ⁇ ⁇ , almost no decrease in transmittance occurs in the visible light region.
  • the transmittance is maintained at about 90% in the entire wavelength range. 4mm thick stone as the base material Considering that the UK transmittance is about 93% over the entire wavelength range, it can be seen that if the transmittance of the film alone is calculated, it will be about 97%.
  • the transmittance of the CVD film is remarkably reduced to about 50 to 80% at 1 ⁇ m. Also, sprayed films and conventional sol-gel films do not show translucency because they contain many pores and are thick.
  • the sol-gel monolayer film of Samples 1 to 18 which is an example of the present invention or a multilayer composite film not including a sprayed film, and Samples 31 to 37 which are comparative examples have excellent etching rates of lOnm / min or less.
  • a comprehensive evaluation was given for films that showed plasma corrosion resistance, low dust generation with 50 or fewer particles, and that can be applied to complex shapes.
  • the composite film with the sol-gel film including the sprayed film of Samples 19 to 29 as an example of the present invention the film number and the chlorine gas exposure characteristics are improved as compared with the sprayed film alone. Comprehensive evaluation. It was.
  • the present invention is not limited to electronic component manufacturing apparatuses such as semiconductor elements and liquid crystal panels, but can be applied to members used in all apparatuses that perform plasma processing and the like with corrosive atmospheres, and manufacturing methods thereof. .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Structural Engineering (AREA)
  • Thermal Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Chemically Coating (AREA)
  • Drying Of Semiconductors (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

L'invention concerne un élément structural pour un système de traitement par plasma, qui possède des propriétés filmogènes, une durabilité et une fiabilité excellentes. L'élément structural comprend un substrat et un film céramique déposé sur le substrat, le film céramique présentant une pureté de 98 % ou plus. Les particules constituant le film céramique présentent un diamètre de particules de 50 nm ou moins, et la quantité d'humidité s'échappant du film est de 1019 molécules/cm2 ou moins.
PCT/JP2007/053002 2006-03-27 2007-02-20 Élément structural pour un système de traitement par plasma et son procédé de fabrication WO2007111058A1 (fr)

Priority Applications (2)

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US12/224,784 US20090101070A1 (en) 2006-03-27 2007-02-20 Member for a Plasma Processing Apparatus and Method of Manufacturing the Same
KR1020087025800A KR101030937B1 (ko) 2006-03-27 2007-02-20 플라즈마 처리 장치용 부재 및 그 제조 방법

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JP2006084543A JP5014656B2 (ja) 2006-03-27 2006-03-27 プラズマ処理装置用部材およびその製造方法

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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
FR2988404B1 (fr) * 2012-03-21 2015-02-13 Centre Techn Ind Mecanique Procede de depot d'un revetement anticorrosion
EP2980265A4 (fr) * 2013-03-28 2016-11-30 Osg Corp Film dur pour outils d'usinage et outil d'usinage de métal revêtu de film dur
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
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
KR20230005107A (ko) * 2021-06-28 2023-01-09 주식회사 히타치하이테크 내벽 부재의 재생 방법

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US20090101070A1 (en) 2009-04-23
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CN101432461A (zh) 2009-05-13
KR20080111086A (ko) 2008-12-22
JP5014656B2 (ja) 2012-08-29

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