US20170029628A1 - Yttrium-base sprayed coating and making method - Google Patents

Yttrium-base sprayed coating and making method Download PDF

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Publication number
US20170029628A1
US20170029628A1 US15/220,652 US201615220652A US2017029628A1 US 20170029628 A1 US20170029628 A1 US 20170029628A1 US 201615220652 A US201615220652 A US 201615220652A US 2017029628 A1 US2017029628 A1 US 2017029628A1
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acid
yttrium
coating
particles
base
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Yasushi Takai
Noriaki Hamaya
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Shin Etsu Chemical Co Ltd
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Shin Etsu Chemical Co Ltd
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Assigned to SHIN-ETSU CHEMICAL CO., LTD. reassignment SHIN-ETSU CHEMICAL CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HAMAYA, NORIAKI, TAKAI, YASUSHI
Publication of US20170029628A1 publication Critical patent/US20170029628A1/en
Priority to US15/600,953 priority Critical patent/US20170253955A1/en
Priority to US18/381,485 priority patent/US20240043983A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C23C4/06—Metallic material
    • 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
    • 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
    • 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
    • C23C4/185—Separation of the coating from the substrate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32458—Vessel
    • H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
    • H01J37/32495—Means for protecting the vessel against plasma
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67063—Apparatus for fluid treatment for etching

Definitions

  • This invention relates to an yttrium-base sprayed coating formed by thermally spraying yttrium oxide, yttrium fluoride and/or yttrium oxyfluoride, which is suited as a low dusting coating on parts and articles used in a corrosive plasma atmosphere as encountered in a semiconductor device fabrication process.
  • Typical corrosive halogen-base gases are fluorine-base gases such as SF 6 , CF 4 , CHF 3 , ClF 3 and HF and chlorine-base gases such as Cl 2 , BCl 3 and HCl.
  • the equipment used for such treatment typically includes parts or components having corrosion resistant coatings on their surface. For example, parts or components having coatings formed by spraying yttrium oxide (Patent Document 1) and yttrium fluoride (Patent Documents 2 and 3) to the surface of metallic aluminum and aluminum oxide ceramic substrates are known to be fully corrosion resistant and used in practice.
  • yttrium-base particles may spall off the surface of yttrium-base coatings on the parts during etching treatment and fall onto silicon wafers to interfere with the etching treatment. This causes to reduce the manufacture yield of semiconductor devices. There is a tendency that the number of yttrium-base particles spalling off the yttrium-base coating surface is high at the early stage of etching treatment and decreases with the lapse of etching time.
  • Patent Documents 4 and 5 relating to the spraying technology are also incorporated herein by reference.
  • Patent Document 1 JP 4006596 (U.S. Pat. No. 6,852,433)
  • Patent Document 2 JP 3523222 (U.S. Pat. No. 6,685,991)
  • Patent Document 3 JP-A 2011-514933 (US 20090214825)
  • Patent Document 4 JP-A 2008-133528 (U.S. Pat. No. 8,349,450)
  • Patent Document 5 JP 4591722 (US 20130122218)
  • An object of the invention is to provide an yttrium-base sprayed coating which is formed by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride, capable of substantially preventing yttrium-base particles from spalling off the coating surface during etching or similar treatment, and thus suited for use as a low dusting coating on parts or articles used in a corrosive plasma atmosphere during the semiconductor device fabrication process.
  • a particulate material is melted in a plasma flame into droplets, after which droplets deposit and solidify on a substrate to form a coating. If the size of material particles is too small,, some particles may not enter the flame, but deposit on the coating in the unmelted state. Also, once particles are melted, sometimes droplets may burst on the coating into finer droplets, which will deposit on the coating as finer particles. Such fine (unmelted or burst)
  • Patent Document 5 proposes physical removal of sticky particles (i.e., particles which are not removable by ultrapure water cleaning or ultrasonic cleaning) by polishing or blasting. However, physical removal such as polishing is not so effective because the treatment itself generates fine particles.
  • an improved yttrium-base sprayed coating is obtained by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride to form a coating of 10 to 500 ⁇ m thick, and chemically cleaning the coating with a cleaning liquid in the form of an aqueous solution of organic acid or inorganic acid or a mixture thereof for effectively removing yttrium-base particles anchored to the coating surface until the population of particles having a size of up to 300 nm becomes no more than 5 particles/mm 2 of the coating surface.
  • the resulting yttrium-base sprayed coating prevents yttrium-base particles from spalling off to cause a failure during subsequent etching treatment, it is suitable for use as a low dusting coating on parts and articles used in a corrosive plasma atmosphere in the semiconductor device fabrication process.
  • the invention provides an yttrium-base sprayed coating comprising one or more compounds selected from the group consisting of yttrium oxide, yttrium fluoride, and yttrium oxyfluoride and having a thickness of 10 to 500 ⁇ m, wherein particles with a size of up to 300 nm are present on a coating surface in a population of no more than 5 particles per square millimeters.
  • the yttrium-base sprayed coating has a thickness of 80 to 400 ⁇ m.
  • the yttrium-base sprayed coating is sprayed onto a surface of a substrate of metallic aluminum, aluminum oxide or metallic silicon.
  • the invention provides a method for preparing a yttrium-base sprayed coating, comprising the steps of thermally spraying a particulate spray material comprising at least one compound selected from the group consisting of yttrium oxide, yttrium fluoride, and yttrium oxyfluoride to form a yttrium-base sprayed coating having a thickness of 10 to 500 ⁇ m and chemically cleaning a surface of the coating with a cleaning liquid which is an organic acid aqueous solution, inorganic acid aqueous solution or organic acid/inorganic acid aqueous solution until a population of particles with a size of up to 300 nm is no more than 5 particles per square millimeters of the coating surface.
  • a cleaning liquid which is an organic acid aqueous solution, inorganic acid aqueous solution or organic acid/inorganic acid aqueous solution until a population of particles with a size of up to 300 nm is no more than 5 particles per square millimeter
  • the cleaning liquid is preferably an aqueous solution of an acid selected from the group consisting of a monofunctional carboxylic acid, difunctional carboxylic acid, trifunctional carboxylic acid, hydroxy acid, sulfonic acid, nitric acid, sulfuric acid, carbonic acid, hydrofluoric acid, and acidic ammonium fluoride or a mixture thereof.
  • the monofunctional carboxylic acid is formic acid or acetic acid
  • the difunctional carboxylic acid is maleic: acid, tartaric acid or phthalic acid
  • the trifunctional carboxylic acid is citric acid
  • the hydroxy acid is lactic acid
  • the sulfonic acid is methanesulfonic acid.
  • the chemical cleaning step includes immersing the yttrium-base sprayed coating in the cleaning liquid to dissolve the coating to a depth of at least. 0.01 ⁇ m from its surface for thereby removing particles with a size of up to 300 nm on the coating surface.
  • the yttrium-base sprayed coating of the invention exhibits high corrosion resistance during treatment in a corrosive halogen-base gas plasma atmosphere, and prevents dusting as a result of yttrium-base particles spalling off during etching or similar treatment in the semiconductor device fabrication process, which is effective for improving the fabrication yield of semiconductor devices.
  • the yttrium-base sprayed coating is thus suitable for use as a low dusting coating on parts and articles which are exposed to a corrosive plasma atmosphere.
  • FIGS. 1, 2, 3 and 4 are SEM images of the surface of yttrium-base sprayed coatings in Examples 1, 2, 3 and 4, respectively.
  • FIGS. 5 and 6 are SEM images of the surface of yttrium-base sprayed coatings in Comparative Examples 1 and 2, respectively.
  • the yttrium-base sprayed coating of the invention is formed by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride.
  • Thermal spraying to a substrate is desirably atmospheric plasma spraying or vacuum plasma spraying.
  • the plasma gas used herein may be nitrogen/hydrogen, argon/hydrogen, argon/helium, argon/nitrogen, argon alone, or nitrogen gas alone, but not limited thereto.
  • the substrate subject to thermal spraying include, but are not limited to, substrates of stainless steel, aluminum, nickel, chromium, zinc, and alloys thereof, metal silicon, aluminum oxide, aluminum nitride, silicon nitride, silicon carbide, and quartz, glass when parts or components of the semiconductor fabrication equipment are contemplated.
  • the conditions under which yttrium oxide, yttrium fluoride or yttrium oxyfluoride is thermally sprayed are not particularly limited.
  • the thermal spraying conditions may be determined as appropriate depending on the identity of substrate, the particle size and composition of spray material, and a particular application of the resulting sprayed component.
  • an yttrium oxide coating when an yttrium oxide coating is formed on a metal aluminum substrate, it may be deposited by argon/hydrogen atmospheric plasma spraying using yttrium oxide powder having an average particle size D50 of about 20 ⁇ m and a gas mixture of 40 L/min of argon and 5 L/min of hydrogen.
  • the thermal spraying conditions including a spray distance, current value and voltage value may be determined as appropriate depending on a particular application of the sprayed component.
  • the feed rates of argon and hydrogen gases may be suitably adjusted.
  • the sprayed coating i.e., yttrium-base sprayed coating should have a thickness of 10 to 500 ⁇ m.
  • a coating of less than 10 ⁇ m thick may be less corrosion resistant or allow the substrate surface to be partly exposed in the cleaning step to be described below.
  • a coating of more than 500 ⁇ m thick may simply add to the cost because no further improvement in corrosion resistance is expectable.
  • the thickness of the coating is preferably 80 to 400 ⁇ m, more preferably 100 to 400 ⁇ m, and even more preferably 100 to 300 ⁇ m.
  • the surface of the yttrium-base sprayed coating is then cleaned with a preselected cleaning liquid to remove yttrium-base particles anchored thereto until the population (or number) of yttrium-base particles with a size of up to 300 nm becomes no more than 5 particles/square millimeters (mm 2 ) of the coating surface. It is, of course, most preferred that the population of yttrium-base particles with a size of up to 300 nm on the coating surface be 0. As long as the population is no more than 5 particles/mm 2 , dusting to such an extent as to invite a substantial loss of production yield does not occur during etching treatment in the semiconductor device fabrication process.
  • the “size” of yttrium-base particles refers to the maximum diameter of individual particles measured by microscopy under a scanning electron microscope (SEM) or the like. As seen from the images of FIGS. 5 and 6 , no or only a few particles with a size in excess of 300 nm are present on the sprayed coating surface. Removal of particles with a size of up to 300 nm means removal of substantially all inhibitory particles.
  • the cleaning liquid is an aqueous solution of organic acid, aqueous solution of inorganic acid or aqueous solution of mixed organic: and inorganic acids.
  • the organic acid is not particularly limited as long as it is water-soluble.
  • Suitable organic acids include, but are not limited to, monofunctional carboxylic acids such as formic acid and acetic acid, difunctional carboxylic acids such as maleic acid, tartaric acid and phthalic acid, trifunctional carboxylic acids such as citric acid, hydroxy acids such as lactic acid, and sulfonic acids such as methanesulfonic acid. Inter alia, tartaric acid and citric acid are preferred because they are edible, nontoxic and easy to handle.
  • the inorganic acid is not particularly limited as long as it is water-soluble. Suitable inorganic acids include nitric acid, sulfuric acid, carbonic acid, hydrofluoric acid, and acidic ammonium fluoride.
  • the cleaning technique is not particularly limited.
  • a part or component in the form of a substrate having the yttrium-base sprayed coating formed on its surface is wholly immersed in the cleaning liquid because this technique is effective and efficient.
  • the area of the substrate that should avoid corrosion with acid is desirably masked with resin tape or sheet when a strong acid is used for cleaning. Cleaning without masking is possible when a weak organic acid is used for cleaning, for example, a carboxylic acid or hydroxy acid such as phthalic acid, tartaric acid or citric acid.
  • a buffer solution based on a combination of acid and salt may be used as the cleaning liquid.
  • the yttrium-base sprayed coating is chemically cleaned with the cleaning liquid to dissolve a thin layer from the coating surface for removing particles with a size of up to 300 nm which become a source of dusting.
  • the dissolution depth is preferably at least 0.01 ⁇ m from the original coating surface. Although the upper limit of dissolution depth is not critical, the dissolution depth is preferably up to 20 ⁇ m. More preferably the dissolution depth is 1 to 20 ⁇ m from the coating surface. A dissolution depth of less than 0.01 ⁇ m may be insufficient to remove particles with a size of up to 300 nm and fail to reach a population of no more than 5 particles/mm 2 . A dissolution depth in excess of 20 ⁇ m may simply make the coating thinner without further improvements in particle removal.
  • the coating is rinsed with ultrapure water to thoroughly remove the acid and dried in vacuum or under atmospheric pressure.
  • yttrium-base particles having a size of up to 300 nm on the coating surface are detectable. According to the invention, yttrium-base particles are removed from the coating surface by the cleaning step until the population of particles reaches no more than 5 particles/mm 2 of the surface.
  • An yttrium-base sprayed coating was obtained by thermally spraying the coating material shown in Table 1 onto a surface of a substrate of the material shown in Table 1, immersing the coated substrate in a cleaning liquid, which was an aqueous solution of the cleaning agent shown in Table 1, to clean the coating surface, thoroughly rinsing with ultrapure water, and vacuum drying.
  • the surface of the yttrium-base coating thus obtained was observed under SEM, and yttrium-base particles having a size of up to 300 nm on the surface were inspected and counted.
  • the results are shown in Table 1 and SEM images are shown in FIGS. 1 to 6.
  • the yttrium-base sprayed coating was formed by atmospheric plasma spraying using a gas mixture of 40 L/min of argon and 8 L/min of hydrogen.
  • Example Comparative Example 1 2 3 4 1 2 Spray material Y 2 O 3 Y 2 O 3 + YF 3 YF 3 YOF Y 2 O 3 YF 3 Coating thickness, 200 300 100 200 200 200 ⁇ m Substrate material Al Al 2 O 3 Si Al Al Al Al Cleaning Cleaning agent tartaric citric hydrofluoric lactic no no conditions acid acid acid + acid cleaning cleaning acidic ammonium fluoride Concentration, 2 1 0.05 + 0.1 2 — — mol/L Temperature, ° C.
  • the yttrium-base sprayed coatings in Examples 1 to 4 bear no particles on their surface whereas numerous particles are on the yttrium-base sprayed coatings in Comparative Examples 1 and 2 which omit cleaning with an aqueous solution of acid or cleaning agent. It is readily presumed that these particles cause dust generation during etching treatment.
  • dusting as a result of yttrium-base particles spalling off during etching treatment in a semiconductor device fabrication process is substantially prevented. This will eventually improve the fabrication yield of semiconductor devices.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Drying Of Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • ing And Chemical Polishing (AREA)
  • Weting (AREA)
US15/220,652 2015-07-31 2016-07-27 Yttrium-base sprayed coating and making method Abandoned US20170029628A1 (en)

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US15/600,953 US20170253955A1 (en) 2015-07-31 2017-05-22 Yttrium-based sprayed coating and making method
US18/381,485 US20240043983A1 (en) 2015-07-31 2023-10-18 Yttrium-based sprayed coating and making method

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JP2015151568A JP6500681B2 (ja) 2015-07-31 2015-07-31 イットリウム系溶射皮膜、及びその製造方法
JP2015-151568 2015-07-31

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US (3) US20170029628A1 (ja)
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190017333A (ko) * 2017-08-11 2019-02-20 (주)단단 Yof계 분말의 제조방법
US10443125B2 (en) 2017-05-10 2019-10-15 Applied Materials, Inc. Flourination process to create sacrificial oxy-flouride layer
CN110499486A (zh) * 2018-05-18 2019-11-26 信越化学工业株式会社 喷涂材料、喷涂部件和制造方法
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