WO2018083854A1 - 成膜用材料及び皮膜 - Google Patents
成膜用材料及び皮膜 Download PDFInfo
- Publication number
- WO2018083854A1 WO2018083854A1 PCT/JP2017/028578 JP2017028578W WO2018083854A1 WO 2018083854 A1 WO2018083854 A1 WO 2018083854A1 JP 2017028578 W JP2017028578 W JP 2017028578W WO 2018083854 A1 WO2018083854 A1 WO 2018083854A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- film
- forming material
- less
- film forming
- bulk density
- Prior art date
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/259—Oxyhalides
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/24—Oxygen compounds of fluorine
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/265—Fluorides
-
- 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
- C04B41/5053—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 non-oxide ceramics
- C04B41/5055—Fluorides
-
- 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
- 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
- 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
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the present invention relates to a film forming material and a film containing yttrium oxyfluoride.
- a halogen gas such as a fluorine-based gas or a chlorine-based gas may be used.
- the inside of the etching apparatus is generally coated with a material having high corrosion resistance.
- a material containing a rare earth element typified by yttrium is often used.
- Patent Document 1 discloses a film-forming powder containing a rare earth element oxyfluoride (Ln—O—F), and the powder has an average particle diameter (D 50 ) of 0.1 ⁇ m to 10 ⁇ m, and is intruded with mercury.
- D 50 average particle diameter
- Patent Document 1 describes that high plasma resistance can be obtained by using the film forming powder and the sintered body.
- the demand for plasma corrosion resistance in semiconductor manufacturing equipment and the like has been increasing in recent years, and this is no exception for materials containing yttrium oxyfluoride.
- a film obtained by forming the powder or sintered body described in Patent Document 1 by a PVD method (physical vapor deposition method) using a film-forming material as a film-forming material has higher plasma resistance than before. There was still room for improvement.
- An object of the present invention is to provide a film forming material that can eliminate the various disadvantages of the above-described conventional technology.
- a film-forming material containing yttrium oxyfluoride is a ratio of the Fischer diameter, the tap method bulk density TD, and the stationary method bulk density AD.
- a film-forming material having a specific value of (TD / AD) is that a film having a specific hardness containing yttrium oxyfluoride can be obtained when a film is formed by the PVD method, such as fluorine-based plasma or chlorine-based plasma.
- the present invention has been found.
- the present invention is based on this finding, is a film forming material containing yttrium oxyfluoride, has a Fischer diameter of 1.0 ⁇ m or more and 10 ⁇ m or less, a tap method apparent bulk density TD and a stationary method apparent bulk.
- the present invention provides a film-forming material having a TD / AD ratio of 1.6 to 3.5, which is a ratio to the density AD.
- the present invention also provides a film containing yttrium oxyfluoride having a Vickers hardness of 200HV0.01 or more.
- FIG. 1 is a chart showing the results of subjecting the film forming material obtained in Example 1 to powder X-ray diffraction measurement.
- FIGS. 2A and 2B are scanning electron microscope images of the film forming material obtained in Example 1.
- FIG. 3 is an optical microscope image of the coating obtained in Example 1.
- FIG. 4 is an optical microscope image of the film obtained in Comparative Example 1.
- FIG. 5 is a scanning electron microscope image showing an example of a protrusion.
- FIG. 6 is a chart showing the results of subjecting the coating obtained in Example 1 to X-ray diffraction measurement.
- the film forming material of the present invention (hereinafter sometimes simply referred to as “the material of the present invention”) will be described based on its preferred embodiments.
- Yttrium oxyfluoride is generally represented by YO X F Y (0 ⁇ X and 0 ⁇ Y).
- the film forming material of the present embodiment is preferably in a powder form.
- YO X F Y is a compound composed of yttrium (Y), oxygen (O), and fluorine (F). From the viewpoint of enhancing the effect of obtaining a hard and high plasma-resistant film, 0.04 ⁇ X ⁇ 1.00 is preferable, 0.10 ⁇ X ⁇ 1.00 is more preferable, and 0.30 ⁇ X ⁇ 1.00 is more preferable, and 0.50 ⁇ X ⁇ 1.00 is still more preferable.
- YO X F Y examples include Y 1 O 1 F 1 , Y 5 O 4 F 7 , Y 5 O 6 F 7 , Y 7 O 6 F 9 , Y 17 O 14 F 23 , (YO 0 .826 F 0.17 ) F 1.174 . These can be used alone or in combination of two or more. Hereinafter, in this specification, “YO X F Y ” is also simply referred to as “YOF”.
- a film forming material is formed by evaporating or sublimating a film forming material in a vacuum, and the vapor reaches a workpiece to be deposited.
- the film forming material is required to be efficiently melted, evaporated or sublimated in a powder state in a film forming apparatus.
- the film-forming material of the present embodiment has a larger particle size than the conventional film-forming material containing yttrium oxyfluoride.
- the film forming material of the present embodiment has a Fischer diameter of 1.0 ⁇ m or more, so that the powder can be prevented from being rolled up and the generation of protrusions on the film surface can be suppressed.
- the Fischer diameter of the film forming material is preferably 1.3 ⁇ m or more and 8 ⁇ m or less, and more preferably 1.5 ⁇ m or more and 6 ⁇ m or less.
- the Fisher diameter can be measured by the method described in Examples described later.
- the TD / AD which is the ratio of the apparent bulk density TD of the tap method and the apparent bulk density AD of the stationary method, is in a specific range.
- the present inventors have intensively studied the relationship between the physical properties of the powder containing yttrium oxyfluoride and the hardness of the film obtained from the PVD method, and this TD / AD is an important factor for obtaining a hard film. I found out. By setting the TD / AD of the film forming material containing yttrium oxyfluoride within a certain range, the obtained film becomes sufficiently hard.
- TD / AD is 1.6 or more and 3.5 or less, preferably 1.7 or more and 3.2 or less, and more preferably 1.8 or more and 3.0 or less.
- TD / AD can be measured by the method described in Examples described later.
- the apparent bulk density TD of the film forming material of the present embodiment is 1.0 g / cm 3 or more and 2.0 g / cm 3 or less. Preferably, it is 1.2 g / cm 3 or more and 1.8 g / cm 3 or less.
- the film forming material of the present embodiment preferably has a pore volume with a pore diameter of 100 ⁇ m or less by a mercury intrusion method within a specific range.
- the pore volume is affected not only by the particle size of the film forming material but also by the shape of the constituent particles of the film forming material. For this reason, even if it is a powder with the same particle size, the said pore volume is not necessarily the same.
- the film forming material of the present embodiment preferably has a pore volume of 1.0 cm 3 / g or less. When the pore volume is within this range, a film that is harder and more resistant to plasma can be formed by the PVD method.
- the pore volume of the film forming material of the present invention is more preferably at most 0.9 cm 3 / g, more preferably not more than 0.8 cm 3 / g.
- the lower limit of the pore volume is not particularly defined, but is usually 0.1 cm 3 / g or more.
- the pore volume can be measured by the method described in Examples described later.
- the film forming material of the present embodiment preferably has a repose angle of a certain level or more. Since a material having a large angle of repose has low fluidity, it is possible to perform stable film formation in the PVD method, which is advantageous in terms of hardness and fracture toughness, and provides an advantage that it is easy to obtain a film with few protrusions. .
- the angle of repose of the film-forming material of this embodiment is preferably 40 ° or more, more preferably 43 ° or more, and further preferably 45 ° or more.
- the upper limit of the angle of repose is not particularly limited and is usually 60 ° or less. The angle of repose can be measured by the method described in Examples described later.
- a film forming material having specific values of the Fischer diameter, the tap method bulk density TD and the stationary method bulk density AD (TD / AD), the pore volume, and the angle of repose is suitable for the production of this embodiment described later. It can be obtained by producing a film forming material by a method.
- the oxygen content of the film forming material is preferably 0.3% by mass or more and 13% by mass or less, more preferably 3% by mass or more and 13% by mass or less, and more preferably 6% by mass or more. 13 mass% or less is still more preferable.
- the oxygen content can be measured by the method described in Examples described later.
- the film forming material of this embodiment when this is subjected to X-ray diffraction measurement, the X-ray diffraction peak of YOF is observed.
- an X-ray diffraction peak derived from YF 3 may or may not be observed.
- the height of the main peak of X-ray diffraction of YF 3 is preferably 20% or less with respect to the height of the main peak of X-ray diffraction.
- X-ray diffraction measurement of the film-forming material can be performed by the method described in the examples described later.
- a PVD method (physical vapor deposition method) may be mentioned.
- the PVD method may be an ion plating method (IP method).
- IP method ion plating method
- a vaporized particle is passed through the plasma in a decompressed container to carry a positive charge, and a negative charge is applied to the workpiece to attract and deposit the evaporated particle to form a film.
- the PVD method may be a vacuum vapor deposition method which is a physical vapor deposition method without using plasma.
- an inert gas such as argon is introduced into the processing apparatus chamber.
- the ion plating method is particularly preferable from the viewpoint that a dense and hard film having excellent plasma resistance can be obtained.
- the gas pressure is 0.01 Pa or more and 0.1 Pa or less.
- the EB output is preferably 0.4 kW to 10 kW, and the RF output is preferably 0.2 kW to 3.0 kW.
- Step-second step Step-second step and the powder dry mixed in powder and yttrium fluoride of yttrium oxide (Y 2 O 3) (YF 3): calcining a mixture obtained in the first step
- the BET specific surface area (S) of the Y 2 O 3 powder used for mixing is preferably 1 m 2 / g or more and 30 m 2 / g or less.
- the BET specific surface area (S) of the YF 3 powder used for mixing is preferably 0.1 m 2 / g or more and 5 m 2 / g or less.
- the BET specific surface area (S) can be measured by a BET one-point method using a fully automatic specific surface area meter Macsorb (registered trademark) model-1201 (manufactured by Mountec).
- the gas used for the measurement can be a nitrogen-helium mixed gas (nitrogen 30 vol%).
- Y 2 O 3 powder and YF 3 powder are dry mixed.
- the means for dry mixing is not particularly limited, and may be by stirring in a container, or a W cone mixer, a V-type mixer, a Henschel mixer, or the like may be used.
- ammonium fluoride (NH 4 F) is contained in the mixture of Y 2 O 3 powder and YF 3 powder because low-temperature firing is possible.
- the mixing ratio of Y 2 O 3 powder, YF 3 powder and ammonium fluoride (NH 4 F) is 2.6 mass for Y 2 O 3 powder, assuming that the total of the three components is 100 mass% or less. % To 61.9% by mass, YF 3 powder from 36.0% to 96.2% by mass, and ammonium fluoride (NH 4 F) from 1.2% to 2.1% by mass. Is preferred.
- the mixture obtained in the first step is baked.
- an oxygen-containing atmosphere such as an air atmosphere or an inert atmosphere such as argon or nitrogen can be used, and an oxygen-containing atmosphere is preferable from the viewpoint of sufficiently generating YO X F Y.
- the firing temperature is preferably 450 ° C. or higher and lower than 750 ° C. By baking at a temperature in this range, the film forming material of the present invention can be obtained more efficiently.
- the firing temperature is more preferably 500 ° C. or more and 700 ° C. or less, and particularly preferably 550 ° C. or more and 650 ° C. or less.
- the firing time is preferably 1 hour or more and 100 hours or less, more preferably 5 hours or more and 50 hours or less, and particularly preferably 10 hours or more and 30 hours or less, provided that the firing temperature is in the above range.
- the film forming material obtained as described above is preferably used for obtaining the film of the present embodiment.
- the base material to be deposited for example, various metals such as aluminum, various alloys such as aluminum alloy, various ceramics such as alumina, quartz, and the like are used.
- a film in which a corrosion-resistant film is formed in advance may be used.
- the film of the present embodiment contains yttrium oxyfluoride represented by YO X F Y (0 ⁇ X and 0 ⁇ Y) (hereinafter also simply referred to as “YO X F Y ” or “YOF”). This is one of the characteristics.
- YO X F Y is a compound composed of yttrium (Y), oxygen (O), and fluorine (F).
- 0.04 ⁇ X ⁇ 1.00 is preferable, 0.10 ⁇ X ⁇ 1.00 is more preferable, and 0.30 ⁇ X ⁇ 1.00.
- YO X F Y include Y 1 O 1 F 1 , Y 5 O 4 F 7 , Y 5 O 6 F 7 , Y 7 O 6 F 9 , Y 17 O 14 F 23 , (YO 0 .826 F 0.17 ) F 1.174 . These can be used alone or in combination of two or more.
- the film of this embodiment contains YOF and has a Vickers hardness of 200HV0.01 or more. By having such hardness, it has excellent corrosion resistance against various plasmas such as halogen plasma. Such a hard film containing YOF is difficult to obtain from conventional film forming materials.
- the Vickers hardness of the coating is preferably 220 HV 0.01 or more, more preferably 250 HV 0.01 or more, and even more preferably 280 HV 0.01 or more.
- the film forming material of this embodiment may be formed by the PVD method. In particular, when a film is formed by an ion plating method, a hard film is more easily obtained. The Vickers hardness can be measured by the method described in Examples described later.
- the film of the present embodiment preferably has a fracture toughness of 1.0 ⁇ 10 2 Pa ⁇ m 1/2 or more from the viewpoint of a film having excellent plasma resistance. From these points, the fracture toughness is more preferably 1.0 ⁇ 10 3 Pa ⁇ m 1/2 or more, still more preferably 1.0 ⁇ 10 4 Pa ⁇ m 1/2 or more. It is more preferably 0 ⁇ 10 5 Pa ⁇ m 1/2 or more, and further preferably 1.0 ⁇ 10 6 Pa ⁇ m 1/2 or more. Fracture toughness can be measured by the method described in Examples described later. In order to make the fracture toughness of the film within this range, the film forming material of this embodiment may be used for film formation by the PVD method.
- the film of the present embodiment preferably has a film thickness of 3 ⁇ m or more from the viewpoint of enhancing the plasma corrosion resistance and the coverage of the unevenness of the substrate.
- the film thickness is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more.
- the film forming material of this embodiment may be used for film formation by the PVD method. The film thickness can be measured by the method described in Examples described later.
- the number of protrusions per area of 1.0 cm ⁇ 1.0 cm is preferably 10 or less, more preferably 8 or less, and further preferably 4 or less. Preferably, it is more preferably 2 or less. “The number of protrusions per area of 1.0 cm ⁇ 1.0 cm” refers to the number of protrusions observed in one square area of 1.0 cm in length and 1.0 cm in width on the film surface.
- the conventional film-forming material containing yttrium oxyfluoride has a small particle size and is light, so that when the film is formed by the PVD method, the material powder is likely to roll up and adhere to the film being manufactured. was there.
- Vapor deposition proceeds on the powder adhering to the film being manufactured, thereby forming protrusions. If a film having such protrusions is provided in a semiconductor manufacturing apparatus or the like that performs plasma etching, the protrusions are selectively etched by plasma, causing particles. On the other hand, since the film of this embodiment has very few protrusions, it is further excellent in plasma corrosion resistance.
- a protrusion means the convex part which exists in the membrane
- the maximum length is the maximum length of the shape of the convex portion when viewed from the projecting side of the convex portion orthogonal to the coating surface, and is the length of the longest line segment among the line segments crossing this shape. .
- the maximum length is the diameter of the convex portion when the shape is a circle. The number of protrusions can be measured by the method described in Examples described later.
- the X-ray diffraction peak of YOF is observed.
- the height of the main peak of the X-ray diffraction of YF 3 is preferably 20% or less with respect to the height of the main peak.
- the X-ray diffraction measurement of the film can be performed by the method described in the examples described later.
- the oxygen content of the film is preferably 0.3% by mass or more and 15% by mass or less, more preferably 3% by mass or more and 14% by mass or less, and further preferably 6% by mass or more and 13% by mass or less.
- the oxygen content can be measured by the method described in Examples below.
- the film of this embodiment makes use of its excellent plasma resistance, and is used for coating the inside of a semiconductor manufacturing apparatus such as a vacuum chamber in an etching apparatus, a sample stage, a chuck, a focus ring, and an etching gas supply port in the chamber and its constituent members. be able to.
- a semiconductor manufacturing apparatus such as a vacuum chamber in an etching apparatus, a sample stage, a chuck, a focus ring, and an etching gas supply port in the chamber and its constituent members.
- the film of the present embodiment can be used for various plasma processing apparatuses and chemical plant components in addition to the inside of the semiconductor manufacturing apparatus and its component members.
- the film of this embodiment exhibits excellent resistance to both fluorine-based plasma and chlorine-based plasma as described in the examples described later.
- the film of this embodiment exhibits excellent resistance to oxygen plasma, NF 3 plasma, oxygen / NF 3 plasma, ammonia plasma, NF 3 / oxygen plasma, nitrogen plasma, hydrogen plasma, and the like, and plasma etching using these.
- the surface properties are almost unchanged.
- Y 2 O 3 yttrium oxide
- YF 3 yttrium fluoride
- NH 4 F ammonium fluoride
- Y 2 O 3 yttrium oxide
- YF 3 yttrium fluoride
- Y 2 O 3 Japanese yttrium oxide yttrium oxide
- YF 3 yttrium fluoride Japan
- NH 4 F ammonium fluoride
- Comparative Example 1 produced a film forming material in the same manner as Example 9 described in Patent Document 1.
- the obtained mixture was put into an alumina dish and baked in an electric furnace at 950 ° C.
- the obtained fired product was dry pulverized with an atomizer, mixed with the same amount of pure water, and pulverized with a bead mill using yttria-stabilized zirconia balls (YSZ) having a diameter of 2 mm for 2 hours. Thereafter, the mixture was pulverized for 0.5 hours by a bead mill using yttria-stabilized zirconia balls (YSZ) having a diameter of 1.2 mm to obtain a wet pulverized slurry. The obtained wet pulverized slurry was dried at 120 ° C. for 12 hours to obtain a film forming material of Comparative Example 1.
- TD/AD> Using the multi-functional powder physical property measuring device Multi Tester MT-1001k type (manufactured by Seishin Enterprise Co., Ltd.), the tap method apparent bulk density TD (g / cc) and the stationary method apparent bulk density AD (g / cc) are measured. And the ratio was calculated
- the tap method apparent bulk density TD (g / cc) was measured according to JIS Z 2512, and the static method apparent bulk density AD (g / cc) was measured according to JIS K 5101.
- Pore volume> The measurement was performed according to JIS R 1655 using Autopore IV (manufactured by Micromeritics).
- the oxygen content of the film forming materials of Example 1, Example 2, and Example 3 is set to the above 5.
- the results of measurement by the methods were 12% by mass, 9% by mass, and 6% by mass, respectively.
- the oxygen content of the film forming material of Comparative Example 1 measured by the same method was 10% by mass.
- the chart obtained by the X-ray diffraction measurement of Example 1 is shown in FIG.
- films were produced by the following method.
- the films obtained from the film forming materials of Examples 1 to 3 and Comparative Example 1 are referred to as Examples 1 to 3 and Comparative Example 1, respectively.
- [Manufacture of film] A 100 mm square plate made of alumina ceramic (thickness: 2 mm) was prepared as a base material, and a film was formed on the surface of the base material by an ion plating method. Film formation conditions were an argon gas pressure of 0.04 Pa, an EB output of 4.0 kW, and an RF output of 2.0 kW.
- Vickers hardness and fracture toughness> Vickers hardness is based on JIS Z 2244.
- Fracture toughness is based on JIS R1607.
- the indenter indentation load is 1.96 ⁇ 10 ⁇ 4 N
- the elastic modulus is 1.8 ⁇ 10 11 Pa.
- Fracture toughness 0.018 ⁇ (E / HV) 1/2 (P / C 3/2 )
- the number of protrusions (projections having a maximum length of 5 ⁇ m or more) on the surface of the film having an actual size in the range of 1.0 cm ⁇ 1.0 cm was determined by observation with an optical microscope (magnification 250 times). The average value was obtained by observing the same size range at three locations.
- An optical microscope image of the film of Example 1 is shown in FIG. 3, and an optical microscope image of the film of Comparative Example 1 is shown in FIG.
- the protrusions appear as white spots in the film of FIG. 4, for example.
- One of the SEM images is shown in FIG.
- the protrusion shown in FIG. 5 has a substantially circular shape when viewed from above.
- the X-ray diffraction chart of the film of Example 1 is shown in FIG.
- Oxygen content of film> Using an oxygen / nitrogen analyzer EMGA-550 (manufactured by Horiba, Ltd.), measurement was performed by an inert gas-impulse heating and melting method. When the oxygen content of the film of Example 1, Example 2, and Example 3 was measured, they were 13% by mass, 10% by mass, and 7% by mass, respectively. On the other hand, the oxygen content of the film of Comparative Example 1 was 18% by mass.
- the obtained yttrium oxyfluoride film has a hardness of a specific value or more, and the plasma corrosion resistance of this film is excellent.
- the film forming material of the present invention When the film forming material of the present invention is formed using the PVD method, it is hard and a film having excellent resistance to various plasmas such as fluorine plasma and chlorine plasma can be obtained.
- the film of the present invention has excellent corrosion resistance against various plasmas such as fluorine plasma and chlorine plasma.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Ceramic Engineering (AREA)
- Wood Science & Technology (AREA)
- Geology (AREA)
- Structural Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Physical Vapour Deposition (AREA)
- Drying Of Semiconductors (AREA)
Abstract
Description
また、特許文献1には希土類元素のオキシフッ化物(Ln-O-F)を含有する成膜用焼結体が記載されており、この焼結体を成膜用材料としてPVD法にて成膜することが記載されている。
しかしながら、半導体製造装置等におけるプラズマ耐食性に対する要求は、近年、ますます高まっており、これはイットリウムのオキシフッ化物を含む材料に対しても例外ではない。この点に関し、特許文献1に記載の粉末や焼結体を成膜用材料として、PVD法(物理蒸着法)にて成膜して得られる膜は、従来よりも更に高いプラズマ耐性を得る点でなお改善の余地があった。
以下、本明細書では、「YOXFY」を、単に「YOF」とも記載する。
この観点から、本実施形態の成膜用材料の粒径は従来のイットリウムのオキシフッ化物を含む成膜用材料に比べて大きい。具体的には、本実施形態の成膜用材料はフィッシャー径が1.0μm以上であることで粉末の巻き上がりが防止され、膜表面の突起物の発生を抑制することが可能である。一方、フィッシャー径が10μm以下であることで、一定速度以上で溶融、蒸発ないし昇華して、安定した成膜を行うことが可能である。これらの観点から成膜用材料のフィッシャー径は、1.3μm以上8μm以下であることが好ましく、1.5μm以上6μm以下であることがより好ましい。フィッシャー径は後述する実施例に記載の方法にて測定できる。
本実施形態の成膜用材料の好適な製造方法としては、以下の第1工程及び第2工程を有するものである。以下、各工程について詳述する。
・第1工程:酸化イットリウム(Y2O3)の粉末とフッ化イットリウム(YF3)の粉末とを乾式混合する工程
・第2工程:第1工程で得られた混合物を焼成する工程
混合に供するY2O3粉末のBET比表面積(S)は、1m2/g以上30m2/g以下が好ましい。混合に供するYF3粉末のBET比表面積(S)は、0.1m2/g以上5m2/g以下が好ましい。BET比表面積(S)は、全自動比表面積計Macsorb(登録商標)model―1201(マウンテック社製)を用いてBET1点法にて測定することができる。測定の際使用するガスは、窒素ヘリウム混合ガス(窒素30vol%)とすることができる。
第2工程では第1工程で得られた混合物を焼成する。焼成雰囲気としては、大気雰囲気等の酸素含有雰囲気やアルゴンや窒素等の不活性雰囲気を使用でき、YOXFYを十分に生成する観点から酸素含有雰囲気が好ましい。焼成温度は、好ましくは450℃以上750℃未満とする。この範囲の温度で焼成することによって、本発明の成膜用材料をより一層効率よく得ることができる。焼成温度は、500℃以上700℃以下が更に好ましく、550℃以上650℃以下が特に好ましい。
焼成時間は、焼成温度が上記範囲であることを条件に1時間以上100時間以下が好ましく、5時間以上50時間以下が更に好ましく10時間以上30時間以下が特に好ましい。
本実施形態の皮膜は、YOXFY(0<X、かつ0<Y)で表されるイットリウムのオキシフッ化物(以下、単に「YOXFY」又は「YOF」とも記載する)を含有することを特徴の一つとしている。YOXFYは、イットリウム(Y)、酸素(O)、フッ素(F)からなる化合物である。硬く耐プラズマ性の高い膜を得るためには、0.04≦X≦1.00であることが好ましく、0.10≦X≦1.00であることがより好ましく、0.30≦X≦1.00であることが更に好ましく、0.50≦X≦1.00であることが一層好ましい。代表的なYOXFYの例としては、Y1O1F1、Y5O4F7、Y5O6F7、Y7O6F9、Y17O14F23、(YO0.826F0.17)F1.174が挙げられる。これらは1種又は2種以上を組み合わせて用いることができる。
突起物の個数は、後述する実施例に記載の方法で測定できる。
日本イットリウム社製酸化イットリウム(Y2O3)粉末(BET比表面積S=3.1m2/g)65gと、日本イットリウム社製フッ化イットリウム(YF3)粉末(BET比表面積S=0.4m2/g)28gと、フッ化アンモニウム(NH4F)7gとを乾式混合した。この混合物を、アルミナ製容器に入れ、電気炉で大気雰囲気中700℃で10時間焼成し、実施例1の成膜用材料を得た。
日本イットリウム社製酸化イットリウム(Y2O3)粉末(BET比表面積S=3.1m2/g)64gと、日本イットリウム社製フッ化イットリウム(YF3)粉末(BET比表面積S=0.4m2/g)29gと、フッ化アンモニウム(NH4F)7gとを乾式混合した。この混合物を、アルミナ製容器に入れ、電気炉で大気雰囲気中650℃で12時間焼成し、実施例2の成膜用材料を得た。
日本イットリウム社製酸化イットリウム(Y2O3)粉末(BET比表面積S=3.1m2/g)39gと、日本イットリウム社製フッ化イットリウム(YF3)粉末(BET比表面積S=0.4m2/g)39gと、フッ化アンモニウム(NH4F)12gとを乾式混合した。この混合物を、アルミナ製容器に入れ、電気炉で大気雰囲気中550℃で16時間焼成し、実施例3の成膜用材料を得た。
〔比較例1〕
日本イットリウム社製酸化イットリウム(Y2O3)粉末(BET比表面積S=20m2/g、D50:0.24μm)47gと日本イットリウム社製フッ化イットリウム(YF3)粉末(BET比表面積S=0.4m2/g、D50:7.4μm)53gとを混合した(YF3/Y2O3モル比1.74)。得られた混合物を、アルミナ製の皿に入れ、電気炉で大気雰囲気中950℃にて8時間焼成した。得られた焼成物をアトマイザーにて乾式粉砕後、同質量の純水と混合し、直径2mmのイットリア安定化ジルコニアボール(YSZ)を用いたビーズミルにて2時間粉砕した。その後、直径1.2mmのイットリア安定化ジルコニアボール(YSZ)を用いたビーズミルにて0.5時間粉砕して湿式粉砕スラリーを得た。得られた湿式粉砕スラリーを、120℃で12時間乾燥させて比較例1の成膜用材料を得た。
Fisher Model 95 Sub Sieve Sizer (Fisher Scientific 製)を用い、JIS H 2116に準拠して測定した。
多機能型粉体物性測定器マルチテスターMT-1001k型(株式会社セイシン企業製)を用い、タップ法見掛け嵩密度TD(g/cc)と静置法見掛け嵩密度AD(g/cc)を測定し、その比を求めた。タップ法見掛け嵩密度TD(g/cc)の測定はJIS Z 2512に準拠し、静置法見掛け嵩密度AD(g/cc)の測定はJIS K 5101に準拠して行った。
オートポアIV(マイクロメリティクス社製)を用い、JIS R 1655に準拠して測定した。
多機能型粉体物性測定器マルチテスター MT-1001k型(株式会社セイシン企業製)を用い、JIS R 9301に準拠して測定した。
酸素・窒素分析装置EMGA-550(株式会社堀場製作所製)を用い、不活性ガス-インパルス加熱融解法にて測定した。
(X線回折の測定方法)
・装置:UltimaIV(株式会社リガク製)
・線源:CuKα線
・管電圧:40kV
・管電流:40mA
・スキャン速度:2度/min
・ステップ:0.02度
・スキャン範囲:2θ=0~70度
また実施例1の成膜用材料を走査型電子顕微鏡による観察に供したところ、図2の画像を得た。
〔皮膜の製造〕
基材として100mm角のアルミナセラミックス製の板(厚さ2mm)を用意し、この基材の表面にイオンプレーティング法により成膜を行った。成膜条件はアルゴンガス圧力0.04Pa、EB出力4.0kW、RF出力2.0kWとした。
ビッカース硬度はJIS Z 2244に基づき、試験機:ミツトヨ社製HM-220(測定圧子:ダイヤモンド正四角錐圧子、対面角136°)にて試験力:0.01kgf、保持時間10秒、大気中25℃にて測定した。試料をビッカース硬度計にセットし、上記荷重でダイヤモンド圧子を押し込み、試験片の表面に圧痕を付け、圧痕面積に基づき硬度を測定した。
破壊靭性はJIS R1607に基づき、上記のビッカース硬度測定の際に生じた亀裂の長さを測定圧子を用い、圧子押込み荷重1.96×10-4N、弾性率:1.8×1011Paとして求めた。具体的には、ビッカース硬度測定で得られた圧痕の四つの角から発生している亀裂の長さを走査型電子顕微鏡で観察して測定した。破壊靭性の値は下記式にて求めた。
破壊靭性=0.018×(E/HV)1/2(P/C3/2)
E:弾性率(Pa)
HV:ビッカース硬度(Pa)
P:押し込み荷重(N)
C:クラック長さの平均の半分(m)
なお、ビッカース硬度の算出は次式による。
HV=1.8544×P/(2a)2
a:圧痕の対角線長さの平均の半分(m)
ビッカース硬度及び破壊靭性は測定点数3点とし、その平均値とした。
測定機器として東京精密社製サーフコムを用いて測定した。
光学顕微鏡(倍率250倍)による観察により、実寸で1.0cm×1.0cmの範囲の皮膜表面における突起物(最大長さ5μm以上の突起物)の数を求めた。同サイズの範囲を3箇所観察して平均値を求めた。実施例1の皮膜の光学顕微鏡像を図3に示し、比較例1の皮膜の光学顕微鏡像を図4に示す。突起物は、例えば図4の皮膜において白い点として表れている。そのうちの一つのSEM画像を図5に示す。図5に示す突起物は、上面視略円形の形状をしている。
各実施例の皮膜に対し、下記条件にてX線回折測定を行ったところ、各実施例において、2θ=0~70°の範囲に観察されるメーンピークはYOFに由来するものであった。また各実施例における、2θ=0~70度の範囲におけるYF3のX線回折のメーンピークは、2θ=0~70度の範囲におけるYOFのX線回折のメーンピーク高さに対して20%以下であった。また各実施例において2θ=0~70度の範囲におけるY2O3のX線回折のメーンピークは、2θ=0~70度の範囲におけるYOFのX線回折のメーンピーク高さに対して40%以下であった。実施例1の皮膜のX線回折チャートを図6に示す。
(X線回折の測定方法)
・装置:UltimaIV(株式会社リガク製)
・線源:CuKα線
・管電圧:40kV
・管電流:40mA
・スキャン速度:2度/min
・ステップ:0.02度
・スキャン範囲:2θ=0~70度
酸素・窒素分析装置EMGA-550(株式会社堀場製作所製)を用い、不活性ガス-インパルス加熱融解法にて測定した。
実施例1、実施例2、実施例3の皮膜の酸素含有量をそれぞれ測定したところ13質量%、10質量%、7質量%であった。一方、比較例1の皮膜の酸素含有量は18質量%であった。
上記の実施例及び比較例で得られた皮膜について、以下の方法にてハロゲン系プラズマに対する耐食性を調べた。結果を表3に示す。
(パーティクルの発生数の評価方法)
上記成膜方法で成膜した100mm角のアルミナセラミックス製基材における膜にプラズマエッチングを行った。プラズマエッチングを行うに際しては、チャンバー内には直径3インチのシリコンウエハーを載置しておいた。エッチング作用によって削られて飛散し、シリコンウエハーの表面に付着したパーティクルのうち、粒径が約0.1μm以上のものの数を、拡大鏡を用いて計測した。プラズマエッチング条件は以下の通り、フッ素系プラズマとした。
・雰囲気ガス CHF3:Ar:O2=80:160:100mL/min
・高周波電力:1300W
・圧力:4Pa
・温度:60℃
・エッチング時間:50時間
また、雰囲気ガスのCHF3をHClに変更して塩素系プラズマとした場合についても同様の計測を実施した。
Claims (12)
- イットリウムのオキシフッ化物を含む成膜用材料であって、フィッシャー径が1.0μm以上10μm以下であり、タップ法見掛け嵩密度TDと静置法見掛け嵩密度ADとの比率であるTD/ADが1.6以上3.5以下である成膜用材料。
- 水銀圧入法により測定した直径100μm以下の細孔の容積が1.0cm3/g以下である、請求項1に記載の成膜用材料。
- 安息角が40°以上である、請求項1または2に記載の成膜用材料。
- イットリウムのオキシフッ化物を含む皮膜であって、ビッカース硬度が200HV0.01以上である皮膜。
- 前記皮膜の破壊靭性が1.0×102Pa・m1/2以上である、請求項4に記載の皮膜。
- 1.0cm×1.0cmの面積当たりの突起物の個数が10個以下である、請求項4又は5に記載の皮膜。
- 膜厚が3μm以上である請求項4~6の何れか一項に記載の皮膜。
- 請求項4~7の何れか一項に記載の皮膜の製造方法であって、
イットリウムのオキシフッ化物を含み、フィッシャー径が1.0μm以上10μm以下であり、タップ法見掛け嵩密度TDと静置法見掛け嵩密度ADとの比率であるTD/ADが1.6以上3.5以下である成膜用材料をPVD法により成膜する、皮膜の製造方法。 - 請求項8に記載の皮膜の製造方法であって、
前記成膜用材料として、水銀圧入法により測定した直径100μm以下の細孔の容積が1.0cm3/g以下である成膜用材料を用いる、皮膜の製造方法。 - 請求項8又は9に記載の皮膜の製造方法であって、
前記成膜用材料として、安息角が40°以上である成膜用材料を用いる、皮膜の製造方法。 - PVD法がイオンプレーティング法である、請求項8~10の何れか一項に記載の皮膜の製造方法。
- イットリウムのオキシフッ化物を含み、フィッシャー径が1.0μm以上10μm以下であり、タップ法見掛け嵩密度TDと静置法見掛け嵩密度ADとの比率であるTD/ADが1.6以上3.5以下である粉末の成膜用材料としての使用。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2017559715A JP6388188B1 (ja) | 2016-11-02 | 2017-08-07 | 成膜用材料及び皮膜 |
CN201780062561.6A CN109844166B (zh) | 2016-11-02 | 2017-08-07 | 成膜用材料及皮膜 |
KR1020197010372A KR102407119B1 (ko) | 2016-11-02 | 2017-08-07 | 성막용 재료 및 피막 |
US16/343,945 US11414325B2 (en) | 2016-11-02 | 2017-08-07 | Film-forming material and film |
US17/457,695 US11691889B2 (en) | 2016-11-02 | 2021-12-06 | Film-forming material and film |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2016-215615 | 2016-11-02 | ||
JP2016215615 | 2016-11-02 |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US16/343,945 A-371-Of-International US11414325B2 (en) | 2016-11-02 | 2017-08-07 | Film-forming material and film |
US17/457,695 Division US11691889B2 (en) | 2016-11-02 | 2021-12-06 | Film-forming material and film |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2018083854A1 true WO2018083854A1 (ja) | 2018-05-11 |
Family
ID=62076842
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2017/028578 WO2018083854A1 (ja) | 2016-11-02 | 2017-08-07 | 成膜用材料及び皮膜 |
Country Status (6)
Country | Link |
---|---|
US (2) | US11414325B2 (ja) |
JP (1) | JP6388188B1 (ja) |
KR (1) | KR102407119B1 (ja) |
CN (1) | CN109844166B (ja) |
TW (1) | TWI746617B (ja) |
WO (1) | WO2018083854A1 (ja) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020090528A1 (ja) * | 2018-10-31 | 2020-05-07 | 日本イットリウム株式会社 | コールドスプレー用材料 |
JP2020092151A (ja) * | 2018-12-04 | 2020-06-11 | 東京エレクトロン株式会社 | 基板載置台、基板処理装置及び基板載置台の製造方法 |
JP7154517B1 (ja) | 2022-02-18 | 2022-10-18 | Agc株式会社 | イットリウム質保護膜およびその製造方法ならびに部材 |
TWI811397B (zh) * | 2018-07-17 | 2023-08-11 | 日商信越化學工業股份有限公司 | 膜形成粉末、膜形成方法、及膜形成粉末製備方法 |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20180327892A1 (en) * | 2017-05-10 | 2018-11-15 | Applied Materials, Inc. | Metal oxy-flouride films for chamber components |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004197181A (ja) * | 2002-12-19 | 2004-07-15 | Shin Etsu Chem Co Ltd | フッ化物含有膜及び被覆部材 |
JP2016211071A (ja) * | 2015-05-08 | 2016-12-15 | 東京エレクトロン株式会社 | 溶射用材料、溶射皮膜および溶射皮膜付部材 |
JP2016211070A (ja) * | 2015-05-08 | 2016-12-15 | 東京エレクトロン株式会社 | 溶射用材料、溶射皮膜および溶射皮膜付部材 |
JP2016211072A (ja) * | 2015-05-08 | 2016-12-15 | 東京エレクトロン株式会社 | 溶射用材料、溶射皮膜および溶射皮膜付部材 |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6677262B2 (en) * | 2000-07-05 | 2004-01-13 | Shin-Etsu Chemical Co., Ltd. | Rare earth oxide, basic rare earth carbonate, making method, phosphor, and ceramic |
EP1239055B1 (en) * | 2001-03-08 | 2017-03-01 | Shin-Etsu Chemical Co., Ltd. | Thermal spray spherical particles, and sprayed components |
US8357262B2 (en) * | 2005-08-31 | 2013-01-22 | Kyocera Corporation | Corrosion-resistant member, treatment apparatus and sample treatment method using the member, and method for manufacture of corrosion-resistant member |
JP4996868B2 (ja) | 2006-03-20 | 2012-08-08 | 東京エレクトロン株式会社 | プラズマ処理装置およびプラズマ処理方法 |
US9017765B2 (en) * | 2008-11-12 | 2015-04-28 | Applied Materials, Inc. | Protective coatings resistant to reactive plasma processing |
JP5939084B2 (ja) * | 2012-08-22 | 2016-06-22 | 信越化学工業株式会社 | 希土類元素オキシフッ化物粉末溶射材料の製造方法 |
KR101865232B1 (ko) | 2015-02-10 | 2018-06-08 | 닛폰 이트륨 가부시키가이샤 | 성막용 분말 및 성막용 재료 |
CN107250082B (zh) | 2015-03-05 | 2018-10-12 | 日本钇股份有限公司 | 烧结用材料以及用于制造烧结用材料的粉末 |
KR20160129457A (ko) | 2015-04-30 | 2016-11-09 | 방소윤 | 사면 바람 선풍기용 날개 구조 |
US10138167B2 (en) | 2015-05-08 | 2018-11-27 | Tokyo Electron Limited | Thermal spray material, thermal spray coating and thermal spray coated article |
TWI751106B (zh) | 2015-05-08 | 2022-01-01 | 日商東京威力科創股份有限公司 | 熔射用材料、熔射被膜及附熔射被膜之構件 |
US10106466B2 (en) | 2015-05-08 | 2018-10-23 | Tokyo Electron Limited | Thermal spray material, thermal spray coating and thermal spray coated article |
CN105505392B (zh) | 2015-12-09 | 2018-02-02 | 中国科学院福建物质结构研究所 | 稀土氟氧化物纳米材料及其制备方法和应用 |
-
2017
- 2017-08-07 WO PCT/JP2017/028578 patent/WO2018083854A1/ja active Application Filing
- 2017-08-07 CN CN201780062561.6A patent/CN109844166B/zh active Active
- 2017-08-07 JP JP2017559715A patent/JP6388188B1/ja active Active
- 2017-08-07 US US16/343,945 patent/US11414325B2/en active Active
- 2017-08-07 KR KR1020197010372A patent/KR102407119B1/ko active IP Right Grant
- 2017-08-15 TW TW106127663A patent/TWI746617B/zh active
-
2021
- 2021-12-06 US US17/457,695 patent/US11691889B2/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2004197181A (ja) * | 2002-12-19 | 2004-07-15 | Shin Etsu Chem Co Ltd | フッ化物含有膜及び被覆部材 |
JP2016211071A (ja) * | 2015-05-08 | 2016-12-15 | 東京エレクトロン株式会社 | 溶射用材料、溶射皮膜および溶射皮膜付部材 |
JP2016211070A (ja) * | 2015-05-08 | 2016-12-15 | 東京エレクトロン株式会社 | 溶射用材料、溶射皮膜および溶射皮膜付部材 |
JP2016211072A (ja) * | 2015-05-08 | 2016-12-15 | 東京エレクトロン株式会社 | 溶射用材料、溶射皮膜および溶射皮膜付部材 |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TWI811397B (zh) * | 2018-07-17 | 2023-08-11 | 日商信越化學工業股份有限公司 | 膜形成粉末、膜形成方法、及膜形成粉末製備方法 |
US11851768B2 (en) | 2018-07-17 | 2023-12-26 | Shin-Etsu Chemical Co., Ltd. | Film-forming powder, film forming method, and film-forming powder preparing method |
WO2020090528A1 (ja) * | 2018-10-31 | 2020-05-07 | 日本イットリウム株式会社 | コールドスプレー用材料 |
JPWO2020090528A1 (ja) * | 2018-10-31 | 2021-09-16 | 日本イットリウム株式会社 | コールドスプレー用材料 |
US11773493B2 (en) | 2018-10-31 | 2023-10-03 | Nippon Yttrium Co., Ltd. | Material for cold spraying |
JP7380966B2 (ja) | 2018-10-31 | 2023-11-15 | 日本イットリウム株式会社 | コールドスプレー用材料 |
JP2020092151A (ja) * | 2018-12-04 | 2020-06-11 | 東京エレクトロン株式会社 | 基板載置台、基板処理装置及び基板載置台の製造方法 |
JP7241519B2 (ja) | 2018-12-04 | 2023-03-17 | 東京エレクトロン株式会社 | 基板載置台、基板処理装置及び基板載置台の製造方法 |
JP7154517B1 (ja) | 2022-02-18 | 2022-10-18 | Agc株式会社 | イットリウム質保護膜およびその製造方法ならびに部材 |
WO2023157849A1 (ja) * | 2022-02-18 | 2023-08-24 | Agc株式会社 | イットリウム質保護膜およびその製造方法ならびに部材 |
JP2023120943A (ja) * | 2022-02-18 | 2023-08-30 | Agc株式会社 | イットリウム質保護膜およびその製造方法ならびに部材 |
Also Published As
Publication number | Publication date |
---|---|
KR102407119B1 (ko) | 2022-06-10 |
JPWO2018083854A1 (ja) | 2018-11-01 |
US20190241746A1 (en) | 2019-08-08 |
JP6388188B1 (ja) | 2018-09-12 |
US11414325B2 (en) | 2022-08-16 |
CN109844166A (zh) | 2019-06-04 |
CN109844166B (zh) | 2021-11-19 |
TWI746617B (zh) | 2021-11-21 |
US11691889B2 (en) | 2023-07-04 |
TW201829810A (zh) | 2018-08-16 |
KR20190075059A (ko) | 2019-06-28 |
US20220089451A1 (en) | 2022-03-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP6388188B1 (ja) | 成膜用材料及び皮膜 | |
JP5071856B2 (ja) | 酸化イットリウム材料及び半導体製造装置用部材 | |
JP5927656B2 (ja) | 皮膜付き基材、その製造方法、その皮膜付き基材を含む半導体製造装置部材 | |
TWI724797B (zh) | 半導體製造裝置用構件及具備半導體製造裝置用構件之半導體製造裝置以及顯示器製造裝置 | |
TWI750156B (zh) | 附皮膜之基材、電漿蝕刻裝置用零件及該等之製造方法 | |
JP7154517B1 (ja) | イットリウム質保護膜およびその製造方法ならびに部材 | |
JP2023533712A (ja) | 酸化イットリウム系のコーティング及びバルク組成物 | |
JP2017061738A (ja) | 溶射材料 | |
JP2018082155A (ja) | 構造物 | |
JP2009029686A (ja) | 耐食性部材およびその製造方法ならびに処理装置 | |
JP2023521164A (ja) | 酸化イットリウム系コーティング組成物 | |
WO2023162741A1 (ja) | 複合構造物および複合構造物を備えた半導体製造装置 | |
TWI777504B (zh) | 複合結構物及具備複合結構物之半導體製造裝置 | |
WO2024038674A1 (ja) | イットリウム質保護膜およびその製造方法ならびに部材 | |
WO2023162743A1 (ja) | 複合構造物および複合構造物を備えた半導体製造装置 | |
TWI778587B (zh) | 複合結構物及具備複合結構物之半導體製造裝置 | |
TW202346240A (zh) | 複合結構物及具備複合結構物之半導體製造裝置 | |
JP2023124889A (ja) | 複合構造物および複合構造物を備えた半導体製造装置 | |
JP2023124888A (ja) | 複合構造物および複合構造物を備えた半導体製造装置 | |
TW202238998A (zh) | 複合結構物及具備複合結構物之半導體製造裝置 | |
JP2023124887A (ja) | 複合構造物および複合構造物を備えた半導体製造装置 | |
JP2023124886A (ja) | 複合構造物および複合構造物を備えた半導体製造装置 | |
JP4410607B2 (ja) | 酸素ラジカル発生電極 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 2017559715 Country of ref document: JP |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 17868436 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 20197010372 Country of ref document: KR Kind code of ref document: A |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 17868436 Country of ref document: EP Kind code of ref document: A1 |