WO2015151857A1 - Composant résistant au plasma, procédé de fabrication de composant résistant au plasma, et dispositif de dépôt de pellicule servant à fabriquer un composant résistant au plasma - Google Patents

Composant résistant au plasma, procédé de fabrication de composant résistant au plasma, et dispositif de dépôt de pellicule servant à fabriquer un composant résistant au plasma Download PDF

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WO2015151857A1
WO2015151857A1 PCT/JP2015/058458 JP2015058458W WO2015151857A1 WO 2015151857 A1 WO2015151857 A1 WO 2015151857A1 JP 2015058458 W JP2015058458 W JP 2015058458W WO 2015151857 A1 WO2015151857 A1 WO 2015151857A1
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Prior art keywords
oxide
film
plasma
particles
resistant component
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PCT/JP2015/058458
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English (en)
Japanese (ja)
Inventor
佐藤　道雄
高志 日野
仁 中谷
中村　隆
Original Assignee
株式会社東芝
東芝マテリアル株式会社
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Application filed by 株式会社東芝, 東芝マテリアル株式会社 filed Critical 株式会社東芝
Priority to JP2016511538A priority Critical patent/JPWO2015151857A1/ja
Priority to US15/124,477 priority patent/US20170022595A1/en
Priority to CN201580017990.2A priority patent/CN106164325A/zh
Priority to KR1020167024605A priority patent/KR20160119187A/ko
Publication of WO2015151857A1 publication Critical patent/WO2015151857A1/fr

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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
    • 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
    • C23C4/11—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
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • 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
    • C23C4/18—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon

Definitions

  • Embodiments described herein relate generally to a plasma-resistant component, a plasma-resistant component manufacturing method, and a film deposition apparatus used for manufacturing a plasma-resistant component.
  • an insulating film such as SiO 2 is usually formed by a sputtering apparatus or a CVD apparatus, and isotropic etching of Si or SiO 2 by an etching apparatus Fine wiring, electrodes, and the like are formed using anisotropic etching.
  • plasma discharge is used in these apparatuses in order to improve the film formation rate and the etching property.
  • etching apparatus a plasma etching apparatus such as an RIE (Reactive Ion Etching) apparatus is used.
  • RIE reactive Ion Etching
  • the inside of the chamber is brought into a low pressure state, and fluorine gas or chlorine gas is introduced into the chamber to form plasma, and etching is performed.
  • parts such as chambers that are irradiated with plasma have been devised so as not to generate reaction products, and the parts are more likely to be corroded by exposure to plasma.
  • a film having high plasma resistance and corrosion resistance is formed.
  • an oxide coating made of yttrium oxide (Y 2 O 3 ) or aluminum oxide (Al 2 O 3 ) is known. These oxide films are effective in suppressing generation of reaction products and preventing damage to parts due to plasma attack.
  • Patent Document 1 Japanese Patent No. 4084891
  • Patent Document 2 describes a Y 2 O 3 film formed by heat-treating a Y (OH) 3 sol solution applied to a substrate.
  • Patent Document 2 describes an Al 2 O 3 sprayed coating.
  • sprayed oxide coatings such as yttrium oxide and aluminum oxide formed by conventional thermal spraying methods are coatings in which oxide particles such as yttrium oxide and aluminum oxide are deposited, and these particles are molten yttrium oxide and aluminum oxide.
  • the oxide particles collide with the surface of the substrate and rapidly solidify.
  • the particle size of the oxide powder used in the conventional thermal spraying method is as large as about 5 to 45 ⁇ m. For this reason, sprayed oxide coatings such as yttrium oxide and aluminum oxide formed by conventional thermal spraying methods tend to generate many microcracks due to the difference in thermal expansion between the inside and the surface, so that strain tends to remain and durability is poor. There was a technical problem that was enough.
  • oxide particles such as yttrium oxide and aluminum oxide melted by a thermal spraying heat source collide with the surface of the substrate, the thickness is reduced in a direction perpendicular to the substrate surface, and the so-called flattened particles are expanded in a parallel direction.
  • melted flat particles After being deformed into a shape, it is likely to rapidly solidify and become flat particles (hereinafter referred to as “melted flat particles”).
  • microcracks when the average particle diameter of the oxide powder particles is as large as 5 ⁇ m or more, cracks (hereinafter referred to as “microcracks”) mainly observed in the thickness direction perpendicular to the surface of the base material on the surface of the molten flat particles.
  • the flat shape is calculated as an aspect ratio (L / t) from the particle thickness (t) in a direction perpendicular to the substrate surface and the particle length (L) in a direction parallel to the substrate surface. This means that the aspect ratio is 1.5 or more.
  • the active radicals generated by plasma discharge are irradiated to the yttrium oxide film or aluminum oxide film in such a state, the active radicals attack the microcracks to expand the microcracks, and the internal strain is reduced. Microcracks propagate when released. As a result, the thermal spray coating is lost and particles derived from the thermal spray coating are likely to be generated, and the reaction product attached to the upper surface of the thermal spray coating is peeled off to easily generate particles derived from the reaction product. And the generation of particles causes short circuit and disconnection of fine wiring, etc., and lowers the product yield of semiconductor devices, etc., and frequently cleans and replaces parts for plasma devices, lowering productivity and filming cost. Resulting in a rise.
  • the formed sprayed coating has a high porosity of about 15% and many pores are generated.
  • the roughness of the sprayed coating surface becomes as rough as about 6 to 10 ⁇ m in average roughness Ra.
  • the pores (voids) correspond to gaps between particles, and the microcracks indicate a cracked surface shape of molten flat particles.
  • the plasma etching of the substrate proceeds through the pores, shortening the life of the plasma device component and spraying plasma discharge.
  • the sprayed coating becomes brittle by concentrating on the convex portions of the coating and the amount of particles generated increases.
  • the wiring width is being reduced in order to achieve high integration.
  • the narrowing of the wiring width extends to, for example, 32 nm, 19 nm, and even 15 nm or less.
  • a wiring defect or an element defect occurs. For this reason, in recent years, there has been a strong demand for suppressing the generation of even extremely small particles as much as possible.
  • blasting is generally performed as a pretreatment for forming the coating by spraying abrasive grains and the like together with the granules on the surface of the substrate.
  • blasting is performed in this way, residual pieces of abrasive grains as a blasting material are present on the surface of the base material, or a crushed layer is formed on the surface of the base material by blasting.
  • the conventional method of forming the sprayed coating on the surface of the base material of the plasma device component is that the sprayed coating tends to be a source of particles, and the product yield is easily reduced. There has been a problem that the life has changed and the variation in quality has become large for each part.
  • the chemical treatment or blasting process used when peeling the film of yttrium oxide or the like by thermal spraying is applied to the part. Had problems of damage such as corrosion and deformation.
  • the particulate portion deposited without melting there are pores (voids) that are not observed in the molten flat particles and are gaps between the particles deposited without melting. Therefore, further densification is difficult, and further improvement of corrosion resistance is difficult. Furthermore, in the regeneration process in which a film of yttrium oxide or the like is formed again on the inner wall or internal component of the plasma device component, the chemical solution treatment used when peeling the oxide film of yttrium oxide or the like by the impact sintering method is used. In the blast treatment, the voids, which are the gaps between the particles, are less damaged than the conventional thermal spraying method, but still have the problem of causing damage such as corrosion and deformation.
  • One embodiment of the present invention has been made in view of the above circumstances, and can reduce the porosity of the coating to increase the corrosion resistance and strength, thereby preventing generation of particles from the coating and peeling of the coating.
  • Plasma-resistant parts and methods for producing plasma-resistant parts that are stably and effectively suppressed, and that are less likely to cause damage such as corrosion or deformation to the components due to chemical treatment, blast treatment, etc., used when peeling the coating in a regeneration process
  • the oxide such as yttrium oxide constituting the film has internal defects, Internal strain and micro cracks are not substantially generated, and the fine particles are sintered and bonded to each other on the surface of the component base material to form polycrystalline particles, and a dense film with a low porosity is formed as an aggregate. , The corrosion resistance and strength of the coating are increased.
  • the present invention has been completed by finding the formation method and conditions in order to achieve the film structure of the coating.
  • a dense polycrystalline particle in which fine particles are sintered and bonded is obtained by a solid-phase sintering mechanism in which the particles do not melt and the surface of the particles or between the particles. Including both a liquid phase sintering mechanism and a sintered bond that is melted and sintered.
  • the sintered-bonded polycrystalline particles are not single crystal particles, but are particles in which crystal grain boundaries are observed in the microscopic observation, and the coating film of the present invention is similarly observed by microscopic observation of these polycrystalline particles. Observed as a deposited film.
  • Sinter-bonded dense polycrystalline particles obtained in the present invention are non-particulate particles in which grain boundaries separating from the outside are not observed, such as observed by a microscopic observation on a coating formed by, for example, an impact sintering method. Almost no part is observed.
  • the cross section perpendicular to the substrate surface of the coating is observed with a microscope, the area ratio of the non-particulate part where the grain boundary separating from the outside is not confirmed is 10% or less.
  • the fine particles having a particle size of 3 ⁇ m or less present in the oxide deposited film according to the present invention have an area ratio of 10% or less when the cross section perpendicular to the substrate surface of the film is observed with a microscope.
  • the molten flat particles present therein are 10% or less in area ratio when a cross section perpendicular to the substrate surface of the film is observed with a microscope, and are hardly observed anyway.
  • a processing object holding means for holding a processing object in the chamber, and a plasma generation means for converting the gas introduced into the chamber into plasma, using the generated plasma
  • a plasma apparatus for processing the processing object is provided.
  • An oxide film is formed on the inner wall of the chamber and the surface of the component in the chamber on the side of the plasma generation region generated by the plasma generation means. This oxide film is a deposited film made of oxide particles such as yttrium oxide.
  • the deposited film is a deposited film formed as an aggregate of fine particles having a particle diameter of 0.05 to 3 ⁇ m that are sintered and bonded to each other on the surface of the base material of the component. Is 10 ⁇ m or more and 200 ⁇ m or less, and the film density is 90% or more. In the deposited film, fine particles (raw material particles) having a particle size of 3 ⁇ m or less are present in an area ratio of 10% or less. However, since the aggregate of polycrystalline particles is densely formed, plasma resistance is increased. Is well retained.
  • the oxide film may be configured with a base film. That is, it has an oxide deposited film in which oxide particles are deposited on a conventional oxide sprayed coating such as yttrium oxide formed as a base film, and comprises the base film (sprayed coating) and the oxide deposited film.
  • the total thickness of the laminated film may be 20 ⁇ m or more and 300 ⁇ m or less, and the film density of the oxide deposited film may be 90% or more.
  • the oxide film comprises an oxide film formed by, for example, anodizing the surface of the base material, a base film formed on the surface of the oxide film, and an oxide deposited film formed on the surface of the base film.
  • a three-layer structure may be used. That is, the oxide film is formed on a conventional oxide sprayed film such as yttrium oxide formed as a base film on the surface of the substrate on which the oxide film is formed.
  • the total film thickness of the laminated film is 20 ⁇ m or more and 200 ⁇ m or less, and the oxide deposited film has a film density of 90% or more.
  • the film laminating apparatus is a film laminating apparatus used for manufacturing the plasma-resistant component including a base material and an oxide deposition film that covers the surface of the base material, and a plasma arc, A generation chamber for generating a high temperature plasma jet or a high temperature gas, a raw material slurry supply port for supplying a raw material slurry containing oxide raw material powder to the center of the high temperature plasma jet or high temperature gas, and a fuel or oxygen gas in the generation chamber A fuel supply port for supplying, a gas supply port for supplying a working gas to the generation chamber, a raw material slurry is gasified by the working gas and fuel or oxygen gas, and the oxide raw material in the gas is below the boiling point of the oxide and An injection nozzle that controls the state in which the raw material oxide is heated to a temperature below the sublimation point and sprayed onto the surface of the base material so that the spray speed is 400 to 1000 m / sec. Characterized in that it comprises a and.
  • the spray distance between the tip of the spray nozzle for spraying the oxide raw material onto the surface of the substrate and the surface of the substrate is 100 to 400 mm.
  • the content of the oxide raw material powder in the raw material slurry is preferably 30 to 80% by volume.
  • the plasma-resistant component manufacturing method and the film deposition apparatus used for manufacturing the plasma-resistant component according to the present invention the plasma resistance is improved and the generation of particles is stably and effectively suppressed.
  • the manufacturing method and the film deposition apparatus used for the manufacturing can be provided.
  • FIG. 1 is a cross-sectional view showing an example of a component mounted on the plasma apparatus of the embodiment.
  • FIG. 2 is a photomicrograph (enlarged photograph) showing the structure of an aluminum oxide film having a cross section perpendicular to the substrate surface as an example of an oxide film formed by a conventional thermal spraying method.
  • FIG. 3 shows a schematic diagram as an example of an aggregate of molten flat particles of an oxide film formed by a conventional thermal spraying method. Molten flat particles 5 are deposited on the substrate 4, and microcracks 6 that are mainly cracked in the thickness direction perpendicular to the substrate surface are observed on the surface of the molten flat particles 5. A large number of pores 7 that are gaps between the particles are observed.
  • FIG. 1 is a cross-sectional view showing an example of a component mounted on the plasma apparatus of the embodiment.
  • FIG. 2 is a photomicrograph (enlarged photograph) showing the structure of an aluminum oxide film having a cross section perpendicular to the substrate surface as an example of an oxide film formed by
  • FIG. 4 is a photomicrograph (enlarged photograph) showing the structure of the aluminum oxide film having a cross section perpendicular to the substrate surface as an example of the oxide film according to the embodiment.
  • FIG. 5 is a cross-sectional view showing an example of an aggregate of polycrystalline particles of an oxide film according to the embodiment.
  • the polycrystalline particle 8 is a particle in which a crystal grain boundary 9 is seen in the particle, not a single fine particle 10, and the coating of the present invention is a coating in which these polycrystalline particles 8 are deposited on the substrate 4. ing.
  • FIG. 6 is a cross-sectional view schematically showing an injection port of the film laminating apparatus used for manufacturing the plasma device component according to the embodiment, and the raw material slurry supply port 15 is operated in the plasma arc generation chamber or the hot gas generation chamber 11.
  • FIG. 7 is a cross-sectional view schematically showing an injection port of the film laminating apparatus used for manufacturing the plasma device component according to the embodiment, in which the raw material slurry supply port 15 is a working gas in the plasma arc generation chamber or the high temperature gas generation chamber 11.
  • the structural example installed in the place near the supply port 13 and the fuel or oxygen gas supply port 14 is shown.
  • the plasma-resistant component according to the present invention is a component including a base material and an oxide film such as yttrium oxide that covers at least a part of the surface of the base material.
  • the base material used in the plasma-resistant component is a member covered with an oxide film such as yttrium oxide among the components.
  • Examples of the substrate include members exposed to plasma and radicals generated during the plasma treatment among the members of the plasma resistant component.
  • Examples of such members include wafer placement members, inner wall portions, deposition shields, insulator rings, upper electrodes, baffle plates, focus rings, shield rings, bellows covers, which are members of semiconductor manufacturing apparatuses and liquid crystal device manufacturing apparatuses. Is mentioned.
  • Examples of the material of the base material include ceramics such as quartz and metals such as aluminum.
  • the oxide film such as yttrium oxide used in the plasma-resistant component of the embodiment is an oxide deposition film formed by using fine particles having an average particle diameter of 0.05 to 3 ⁇ m and covering the surface of the substrate. Consisting of a single layer of material deposition coating, or consisting of two layers of an oxide spray coating formed after coating a substrate with a conventional spray coating as a base film, or the substrate surface The film is formed of three layers: an oxide film formed by oxidizing the film, a conventional sprayed coating formed on the surface of the oxide film, and an oxide deposited film covering the surface of the sprayed coating.
  • One embodiment is a plasma apparatus equipped with a plasma-resistant component having an oxide film formed with fine particles having an average particle diameter of 0.05 to 3 ⁇ m.
  • the oxide film is made of oxide particles. Is a deposited film.
  • the deposited film is an oxide deposited film formed as an aggregate of fine particles having an average particle diameter of 0.05 to 3 ⁇ m that are sintered and bonded to each other on the surface of a component substrate.
  • the film thickness of this oxide deposited film is 10 ⁇ m or more and 200 ⁇ m or less, and the film density is 90% or more.
  • a laminate composed of the foundation film and the oxide deposition film in the case of a two-layer structure having the oxide deposition film on a general oxide sprayed film such as yttrium oxide formed as the foundation film, a laminate composed of the foundation film and the oxide deposition film.
  • the total film thickness of the film is 30 ⁇ m or more and 200 ⁇ m or less, and the film density of the oxide deposited film is 90% or more.
  • FIG. 1 is a cross-sectional view showing an example of components mounted on the plasma apparatus of the first embodiment.
  • 1 is a component for a plasma processing apparatus (plasma-resistant component)
  • 2 is an oxide deposited film
  • 3 is a substrate. If the oxide deposited film 2 is made of, for example, yttrium oxide, it has strong resistance to plasma attack, radical attack (for example, active F radical) and fluorine-based plasma.
  • the purity of oxide raw material particles such as yttrium oxide is preferably 99.9% or more. If there are many impurities in the oxide particles, they may cause impurities to be mixed in the semiconductor manufacturing process. For this reason, it is more preferable to use oxide particles having a purity of 99.99% or more.
  • oxide particles such as yttrium oxide are injected in a molten state with coarse particles having a particle size of about 5 to 45 ⁇ m, and are formed into a flat shape. Cracks are likely to occur.
  • the average particle size is 0.05 ⁇ m to 3 ⁇ m and fine particles, the heat conduction between the inside and the surface of the particles is fast even when the film is formed on the base material. There is almost no stress inside the film due to the difference in thermal expansion between the inside and the surface, and cracks and the like due to rapid solidification do not occur.
  • the fine particle deposition film is a film formed by depositing a film by heating a fine particle with a plasma jet or high temperature gas jetting at a high speed and depositing a film heated to a temperature lower than the boiling point and sublimation temperature of 400 m / second. This is a method of forming a film by injecting at a high speed and colliding with the substrate and bonding at the contact portion of the deposited particles.
  • the fine particles having an average particle size of 3 ⁇ m or less are bonded to each other, the heat conduction inside the particles and the surface is fast, and the stress inside the film due to the difference in thermal expansion between the inside and the surface in the deposited state is Almost no generation, sintering bonding on the surface of the base material of the parts to form polycrystalline particles, and as an aggregate, form an oxide deposit film such as yttrium oxide with high density (high film density) and strong bonding strength Can do.
  • the film thickness of the oxide deposit film such as yttrium oxide needs to be 10 ⁇ m or more. If it is less than 10 ⁇ m, the effect of plasma resistance cannot be obtained sufficiently, and the film may be peeled off.
  • the upper limit of the thickness of the oxide deposited film is not particularly limited, but if it is excessively thick, no further effect can be obtained, and cracks are likely to occur due to the accumulation of internal stress, which may cause a cost increase. Become. Therefore, the thickness of the oxide deposited film is 10 to 200 ⁇ m, preferably 30 to 150 ⁇ m.
  • the film density (relative density) of the oxide deposited film needs to be 90% or more.
  • the film density is a term opposite to the porosity, and the film density of 90% or more has the same meaning as the porosity of 10% or less.
  • an area of a unit area of 200 ⁇ m ⁇ 200 ⁇ m is analyzed. When the film thickness is small, measurement is made at a plurality of locations until the total unit area becomes 200 ⁇ m ⁇ 200 ⁇ m.
  • the film density of the oxide deposited film needs to be 90% or more, more preferably 95% or more, and further preferably 99% or more and 100% or less. If there are many pores (voids) in the oxide deposited film, erosion such as plasma attack proceeds from the pores and the life of the oxide film is reduced. Therefore, it is particularly desirable that there are few pores on the surface of the oxide deposited film.
  • the surface roughness Ra of the oxide deposited film is preferably 3 ⁇ m or less. If the surface roughness of the oxide deposited film is large, plasma attacks and the like are likely to concentrate, which may reduce the life of the deposited film.
  • the surface roughness Ra is measured in accordance with JIS-B-0601-1994.
  • the surface roughness Ra is 2 ⁇ m or less.
  • the oxide powder as the raw material powder using fine particles preferably has an average particle size in the range of 0.05 to 3 ⁇ m.
  • the formed deposited film has a high bonding force between the particles, reduces wear due to plasma attack and radical attack, reduces the amount of particles generated, and improves plasma resistance. If the average particle size of the oxide particles as the raw material powder exceeds 3 ⁇ m, when particles are deposited on the substrate, cracks due to rapid solidification are likely to occur in each particle, and the deposited film may be damaged and cracks may occur. There is.
  • the more preferable value of the average particle diameter of the particles is 0.05 ⁇ m or more and 1 ⁇ m or less.
  • the average particle diameter of the particles is less than 0.05 ⁇ m, the particles cannot obtain a high speed, and even when they are deposited, a low-density coating is formed, and the plasma resistance and corrosion resistance are lowered.
  • the average particle size is less than 0.05 ⁇ m and the particle size is less than 5% of the entire oxide particle, the film formation is not deteriorated. Therefore, a powder containing small particles less than 0.05 ⁇ m may be used. .
  • the manufacturing method of the plasma-resistant component in which the oxide deposit film is formed of the fine particles according to the embodiment includes supplying a slurry containing oxide particles such as yttrium oxide in a high-temperature plasma jet or high-temperature gas, and boiling the oxide particles such as yttrium oxide. A step of heating to a temperature below the sublimation point and spraying onto the substrate at a spraying speed of 400 to 1000 m / sec.
  • the heating operation is performed at a temperature equal to or higher than the melting point temperature of the oxide and lower than the boiling point and the sublimation point temperature, and the injection speed is 500 to 1000 m / sec.
  • the average particle diameter of oxide particles such as yttrium oxide is preferably 0.05 to 3 ⁇ m. More preferably, it is 0.05 to 1 ⁇ m.
  • a film deposition apparatus that performs deposition using fine particles includes a high-temperature plasma jet or high-temperature gas supply port and a plasma torch or high-temperature gas generation chamber connected thereto.
  • the high-temperature plasma jet or high-temperature gas generation chamber has a slurry supply port, and yttrium oxide slurry such as yttrium oxide supplied from the slurry supply port is jetted from the high-temperature plasma jet or high-temperature gas generation chamber to the substrate through the nozzle. Then the film is formed.
  • a combustion flame using oxygen, acetylene, ethanol, kerosene, or the like may be used.
  • a method for manufacturing a component for a plasma etching apparatus includes a step in which a raw material slurry containing oxide raw material powder is supplied to the center of a high temperature plasma jet or high temperature gas (oxide raw material powder supply step), and a high temperature plasma jet or high temperature gas.
  • the oxide raw material powder is heated to below the boiling point and sublimation point temperature and sprayed onto the surface of the base material at an injection speed of 400 to 1000 m / sec (oxide raw material powder spraying step).
  • the raw material slurry When the slurry concentration is in the range of 30 to 80% by volume, the raw material slurry has an appropriate fluidity and is smoothly supplied to the slurry supply port, so that the supply amount of the raw material slurry to the high temperature gas is stable. Therefore, there is an advantage that the film thickness and composition of the oxide deposited film become uniform.
  • the slurry supply port of the film deposition apparatus is usually provided so as to supply the raw material slurry to the central portion of the high temperature plasma jet or the high temperature gas. Further, the high temperature plasma jet or the high temperature gas has a high injection speed.
  • the injection speed of the oxide raw material powder in the high temperature plasma jet or the high temperature gas is stabilized to the injection speed. It is preferable because variations are difficult to occur, and the temperature of the high-temperature plasma jet or the high-temperature gas is constant and the structure of the oxide deposited film can be easily controlled.
  • the oxide raw material powder in the raw material slurry is supplied to the center of the high temperature plasma jet or the high temperature gas flow.
  • the oxide raw material powder in the raw material slurry is centered from the side of the high temperature plasma jet or the high temperature gas flow. It means that it is supplied to the part.
  • the central portion of the high temperature plasma jet or the high temperature gas means a central portion in this cross section when a cross section perpendicular to the injection direction of the high temperature plasma jet or the high temperature gas is taken.
  • the oxide raw material powder in the raw slurry is not supplied to the central portion of the high temperature plasma jet or the high temperature gas flow, but is supplied to the side surface of the high temperature plasma jet or the high temperature gas flow or outside the high temperature plasma jet or the high temperature gas flow. If it stays, the injection speed of the oxide raw material powder in the high temperature plasma jet or the high temperature gas is not stable, and the injection speed is likely to vary, and the temperature variation of the high temperature plasma jet or the high temperature gas flow is large. It becomes difficult to control the organization.
  • the position adjustment of the raw material slurry supply port, the supply amount of the raw material slurry to the high temperature plasma jet or the high temperature gas, and the supply speed are adjusted.
  • the method of adjustment etc. are mentioned.
  • the high-temperature plasma jet or high-temperature gas and oxide raw material powder prepared in the above process are sprayed from the spray nozzle of the film deposition apparatus toward the substrate.
  • the injection state of the high temperature plasma jet or the high temperature gas and the oxide raw material powder is controlled. Examples of the controlled injection state include the injection speed of the oxide raw material powder.
  • the spray nozzle of the film deposition apparatus is usually provided so as to spray a high temperature plasma jet or a high temperature gas and oxide raw material powder in the lateral direction.
  • the substrate is usually arranged such that the surface of the substrate is positioned on the extension of the lateral spray nozzle of the film deposition apparatus.
  • the spray speed of the oxide particles is in a range of 400 m / sec to 1000 m / sec.
  • the injection speed is as low as less than 400 m / second, the deposition when the particles collide is insufficient, and a film having a high film density may not be obtained.
  • the injection speed exceeds 1000 m / sec, the impact force is too strong, and the blast effect by the oxide particles is generated, and it is difficult to obtain the target oxide deposited film.
  • the oxide particle slurry is preferably a slurry containing oxide particles having an average particle diameter of 0.05 to 3 ⁇ m as a raw material powder.
  • the solvent to be slurried is preferably a solvent that is relatively volatile, such as methyl alcohol and ethyl alcohol.
  • the oxide particles are preferably mixed with a solvent after being sufficiently pulverized so that coarse particles do not exist. For example, if there are coarse particles having an average particle size exceeding 3 ⁇ m, it is difficult to obtain a uniform deposited film.
  • the content of oxide particles in the slurry is 30 to 80 vol. % Range is preferred.
  • the slurry having an appropriate fluidity is more smoothly supplied to the supply port and the supply amount is stabilized, so that a uniform deposited film can be obtained.
  • a more preferable content is 50 to 80 vol. %.
  • the plasma device parts as described above can be applied to various plasma devices.
  • microfabrication of various thin films such as insulating films, electrode films, and wiring films formed on Si wafers and substrates is performed by using a high-frequency voltage applied between electrodes or a halogen gas by the interaction between a microwave electric field and a magnetic field. It can be carried out using a RIE (Reactive Ion Etching) apparatus that converts the plasma into plasma and processes the generated ions and radicals.
  • RIE Reactive Ion Etching
  • the plasma device component which is one of the embodiments can be applied anywhere as long as it is exposed to plasma. For this reason, not only a wafer placement member such as an electrostatic chuck, but also any part that is exposed to plasma, such as an inner wall portion, can be applied.
  • the base material on which the oxide deposited film is formed is not limited to quartz, and may be provided on a metal member or a ceramic base material.
  • it is a technology that can be applied to deposition shields, insulator rings, upper electrodes, baffle plates, focus rings, shield rings, bellows covers, etc. that are exposed to plasma among the parts used in plasma devices.
  • the present invention is not limited to this, and can be applied to parts of a plasma apparatus such as a liquid crystal device.
  • the plasma resistance of the plasma device parts is remarkably improved, and it is possible to reduce particles and extend the service life of the parts. For this reason, if it is a plasma apparatus using such a plasma-resistant component, it is possible to reduce particles during the plasma processing and reduce the number of parts replacement.
  • an insulating member may be used in order to maintain insulation from a high-frequency voltage applied for plasma generation.
  • a general oxide sprayed film is formed on it, and oxide fine particles by high-speed particle deposition method are formed thereon.
  • a three-layer coating with a deposited film is effective.
  • an aluminum oxide film formed by fine particle deposition may be formed in addition to the anodized film.
  • a two-layer coating in which a highly insulating aluminum oxide film (alumite) is deposited and then an yttrium oxide deposited film is formed thereon is effective.
  • the thickness of the aluminum oxide film it is important to adjust the thickness of the aluminum oxide film and to form a high-density film. Especially when an ⁇ -structured aluminum oxide film is densely formed, a further effect is exhibited. It is preferable to set the conditions equivalent to the formation of the yttrium film.
  • the underlayer is an yttrium oxide film, other oxides or a mixture thereof may be used, and it is preferable to select a material according to necessary characteristics.
  • the upper limit of the total film thickness is preferably 500 ⁇ m or less.
  • the underlayer is an aluminum oxide film, but other oxides or a mixture thereof may be used, and it is preferable to select a material according to the required characteristics.
  • the upper limit of the film thickness is preferably 500 ⁇ m or less.
  • the present invention it is possible to suppress the generation of particles due to the peeling of the deposits deposited on the plasma device components, and to greatly reduce the number of times of device cleaning and component replacement. Reduction of the amount of generated particles greatly contributes to defects in etching processing in semiconductor manufacturing, defects in the film during film formation of various thin films, and improvement in the yield of elements and components using the defects. In addition, reducing the number of times of device cleaning, part replacement, and extending the service life of parts greatly contribute to the improvement of productivity and the reduction of running costs.
  • Deposition conditions of the oxide fine particles (Examples 1 to 7) shown in Table 1 and the yttrium oxide film formed by the conventional thermal spraying method (Comparative Example 1) are shown.
  • thermal spraying after forming an yttrium oxide film by plasma spraying treatment, the conditions shown in Table 1 are applied to the surface of the aluminum substrate (100 mm ⁇ 200 mm) by the fine particles emitted by using a plasma type film spraying device.
  • a yttrium oxide deposited film was formed by using a plasma device component (plasma-resistant component).
  • the solvent of the yttrium oxide particle slurry was ethyl alcohol.
  • the raw material powder used was high-purity oxide particles having a purity of 99.99% or higher.
  • yttrium oxide (Y 2 O3) particles as a raw material powder were cubic crystals, and there were no coarse particles exceeding 3 ⁇ m by sufficient pulverization and sieving.
  • an yttrium oxide sprayed coating was formed by plasma spraying.
  • Table 1 shows the film density regarding each example and comparative example of the yttrium oxide film formed under each condition.
  • the film density was obtained from the ratio of pores appearing in an enlarged photograph (500 times) so that the total unit area of the film cross section was 200 ⁇ m ⁇ 200 ⁇ m.
  • the surface roughness Ra of the deposited film of each plasma-resistant component according to Examples 1 to 7 was 3 ⁇ m or less. Furthermore, in Comparative Example 1, the surface roughness Ra of the yttrium oxide sprayed coating was 6.3 ⁇ m.
  • Table 2 shows the evaluation results of the plasma resistance of each of the plasma-resistant parts according to Examples 1 to 7 and the comparative example. That is, the plasma resistant component on which the yttrium oxide deposited film or the sprayed film shown in each example and comparative example of Table 1 is formed is placed in a plasma etching processing apparatus (RIE), and CF 4 (flow rate: 80 sccm) + O 2 (20 sccm). ) + Ar (100 sccm) in a mixed gas stream was exposed to and exposed to plasma.
  • RIE plasma etching processing apparatus
  • the pressure in the RIE chamber was set to 20 mTorr, the RF output was set to 100 W, and after 12 hours (“20 minutes discharge ⁇ 10 minutes cooling” ⁇ 24 times) continuously operated, the amount of yttrium oxide coating particles was scotched. It was investigated by peeling evaluation according to the method (Scotch tape is a registered trademark of 3M).
  • a conventional yttrium oxide sprayed coating is formed on the surface of each substrate, and then an yttrium oxide deposited coating with fine particles is formed, or an yttrium oxide deposited coating with fine particles is formed directly on the substrate.
  • at least one insulating film such as aluminum oxide is formed between the base material surface of the component and the yttrium oxide deposited film, and the yttrium oxide deposited film of fine particles is formed on the outermost surface.
  • the corrosion of the deposited film against the radical of the corrosive gas is suppressed, and the stability of each component and the film itself is improved. Therefore, the generation of particles from parts and coatings can be suppressed. Furthermore, since the use of parts is prolonged and the products generated by corrosion are reduced, the number of parts exchanges and the number of cleanings can be reduced.
  • the yttrium oxide sprayed coating formed by the plasma spraying method is blasted to remove the adhered product on the sprayed surface, and the yttrium oxide deposited film of fine particles is deposited on the yttrium oxide sprayed coating.
  • the recycling process can be carried out smoothly, damage to parts is reduced, parts can be recycled, and part costs can be reduced.
  • an RIE (plasma etching) apparatus has been exemplified as the plasma apparatus.
  • the present invention is not limited to the components used for these apparatuses, and plasma CVD (Chemical Vapor Deposition) apparatus is also available.
  • the parts having the oxide deposited film of the above embodiment can be applied to all apparatuses that perform processing by generating plasma.
  • SYMBOLS 1 Plasma apparatus parts (plasma-resistant parts), 2 ... Yttrium oxide deposition coating, 3 ... Base material, 4 ... Base material, 5 ... Molten flat particle, 6 ... Micro crack, 7 ... Pore (void), 8 ... Many Crystal grains, 9 ... Grain boundary, 10 ... Fine particles, 11 ... Plasma arc generation chamber or high temperature gas generation chamber, 12 ... Injection nozzle, 13 ... Working gas supply port, 14 ... Fuel or oxygen gas supply port, 15 ... Raw material Slurry supply port

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  • Organic Chemistry (AREA)
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  • Metallurgy (AREA)
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  • Chemical Vapour Deposition (AREA)
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Abstract

　Selon un mode de réalisation, la présente invention concerne un composant résistant au plasma et son procédé de fabrication, caractérisé : en ce qu'un revêtement d'oxyde d'un composant de plasma est un revêtement de dépôt d'oxyde qui est formé comme un agrégat de particules polycristallines qui sont obtenues en joignant de très petites particules mesurant entre 0,05 et 3 µm par frittage sur la surface d'un substrat de composant ; en ce que l'épaisseur de pellicule est comprise entre 10 et 200 μm ; et en ce que la densité de pellicule est supérieure ou égale à 90 %. La configuration ci-dessus rend possible l'obtention d'un composant résistant au plasma et d'un procédé de fabrication d'un composant résistant au plasma selon lequel la génération de particules provenant du revêtement est inhibée de manière stable et efficace et les modes de dommages comme la corrosion et la déformation se produisent rarement pendant le processus de régénération.
PCT/JP2015/058458 2014-03-31 2015-03-20 Composant résistant au plasma, procédé de fabrication de composant résistant au plasma, et dispositif de dépôt de pellicule servant à fabriquer un composant résistant au plasma WO2015151857A1 (fr)

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JP2016511538A JPWO2015151857A1 (ja) 2014-03-31 2015-03-20 耐プラズマ部品及び耐プラズマ部品の製造方法及び耐プラズマ部品の製造に用いる膜堆積装置
US15/124,477 US20170022595A1 (en) 2014-03-31 2015-03-20 Plasma-Resistant Component, Method For Manufacturing The Plasma-Resistant Component, And Film Deposition Apparatus Used For Manufacturing The Plasma-Resistant Component
CN201580017990.2A CN106164325A (zh) 2014-03-31 2015-03-20 耐等离子体部件、耐等离子体部件的制造方法以及耐等离子体部件的制造中使用的膜沉积装置
KR1020167024605A KR20160119187A (ko) 2014-03-31 2015-03-20 내플라즈마 부품 및 내플라즈마 부품의 제조 방법 및 내플라즈마 부품의 제조에 사용하는 막 퇴적 장치

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