KR20110117830A - Plasma resistant member and manufacturing method of the same - Google Patents

Abstract

The present invention includes a substrate and a Y ₂ O ₃ coating film formed on the substrate, wherein the Y ₂ O ₃ coating film is X-ray diffraction at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate X-ray diffraction peak due to the peak and the (222) plane of Y ₂ O ₃ is a film of columnar structure, X-ray at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate the intensity of the diffraction peak relates to a plasma-forming member and a method of manufacturing the intensity of the diffraction peak over the range 0.03 to 4.7 a X- ray due to surface 222 of the Y ₂ O _3. According to the present invention, the plasma characteristics are excellent, contaminant generation is suppressed, there is no crack, and the surface roughness is sufficiently low so as not to be selectively etched by the accelerated particles generated in the plasma, and large pores of 0.1 μm or more And a dense and stable ceramic coating film which does not flow into the reaction gas generated in the plasma may be formed.

Description

Plasma resistant member and manufacturing method of the same

The present invention relates to a plasma member and a method for manufacturing the same, and more particularly, to excellent plasma resistance, suppressed generation of contaminated particles, no cracking, and selective etching by accelerated particles generated in plasma. The present invention relates to a plasma member and a method of manufacturing the same, having a sufficiently low surface roughness, no large pores of 0.1 µm or more, and a dense and stable ceramic coating film in which the reaction gas generated in the plasma does not flow into the interior.

Electrostatic chuck, heater, chamber liner, chemical vapor deposition (CVD) boat and focus ring used in plasma environment of semiconductor device and display process Ceramic materials with high melting point and excellent durability are applied to members such as focus rings and wall liners. However, due to the demand for high integration, the density of plasma is increasing. Accordingly, ceramic members used in the plasma environment have excellent plasma corrosion characteristics and the need for development of ceramic members with low generation of contaminants is on the rise.

The conventional ceramic member mainly used quartz (SiO ₂ ), alumina (Al ₂ O ₃ ), and had a short lifespan due to low process defects and plasma resistance due to particle dropping of the ceramic member. Yttria (Y ₂ O ₃ ) or rare earth-based ceramic materials, which are excellent in corrosion resistance, are used.They are made of plasma-resistant materials by coating yttria or rare earth-based materials on quartz or alumina substrates for ease of manufacture and high price. have.

In general, a plasma spray method is used in which a coating film is formed by spraying powder using a high temperature plasma as a method of forming a coating film. However, the ceramic coating film formed by this method has a high porosity and rough surface roughness due to the unique laminated microstructure of the thermal spraying. Therefore, the reaction gases generated in the plasma environment penetrate into the ceramic coating layer through the pores, thereby promoting the reaction, and shortening the lifespan by selective etching of the particles accelerated in the plasma due to the rough surface.

The ceramic coating film deposited by the ion beam has a dense film and a very flat surface roughness due to the intrinsic columnar microstructure. However, due to the difference in thermal expansion coefficient between the substrate and the ceramic coating film, cracks are formed at a predetermined thickness or more, and thus there is a limit to forming a thick coating film on the substrate. Therefore, there is a need for a technique for forming a thick coating film having a low surface roughness without cracking by relieving stress between the coating film and the substrate.

The problem to be solved by the present invention is excellent plasma resistance, contaminated particle generation is suppressed, there is no crack, has a sufficiently low surface roughness so as not to be selective etching by the accelerated particles generated in the plasma, and larger than 0.1㎛ The present invention provides a plasma member having a dense and stable ceramic coating film having no pores and in which a reaction gas generated in a plasma does not flow into the inside.

Another problem to be solved by the present invention is excellent plasma resistance, contaminated particle generation is suppressed, there is no crack, has a sufficiently low surface roughness so as not to be selective etching by accelerated particles generated in the plasma, 0.1 ㎛ or more The present invention provides a method for manufacturing a plasma member that forms a dense and stable ceramic coating film in which no large pores and no reaction gas generated in a plasma do not flow into the inside.

The present invention includes a substrate and a Y ₂ O ₃ coating film formed on the substrate, wherein the Y ₂ O ₃ coating film is X-ray diffraction at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate X-ray diffraction peak due to the peak and the (222) plane of Y ₂ O ₃ is a film of columnar structure, X-ray at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate A plasma member is provided in which the intensity of diffraction peaks ranges from 0.03 to 4.7 with respect to the intensity of X-ray diffraction peaks due to the (222) plane of Y ₂ O ₃ .

The Y ₂ O ₃ coating film has a thickness in the range of 0.5 to 50㎛, the particle size of the Y ₂ O ₃ coating film is preferably from 5 to 50nm.

The Y ₂ O ₃ coating film is a dense film having an average surface roughness in the range of 1 to 500 nm.

The substrate may be made of a silicon-based, oxide-based, nitride-based, carbide-based, or non-oxide-based ceramic sintered material.

The plasma member may be used as a cathode, a focus ring, an insulator ring, a shield ring, a bellows cover, or a depot shield exposed to a plasma environment generated in a gas atmosphere containing a halogen compound.

In addition, the present invention, mounting the substrate to the substrate holder provided in the chamber of the electron beam deposition apparatus, setting the temperature of the substrate in the range of 400 ~ 800 ℃, and the electron beam scanned from the electron gun of the electron beam deposition apparatus crucible Incident to an evaporation source consisting of Y ₂ O ₃ contained therein; the evaporation source being heated and melted as the electron beam is incident on the evaporation source; and opening the shutter located above the evaporation source to open the evaporation source. Causing the evaporated particles of to proceed upward along the evaporation path and depositing Y ₂ O ₃ on one surface of the substrate mounted on the lower surface of the substrate holder, wherein the power applied to the electron gun through a power supply is set to 1.9~10kW range, and wherein the substrate holder is the type Y ₂ O ₃ coating film on the substrate to be rotated at a speed setting of the range 1~100rpm And, the Y ₂ O ₃ coating layer is a diffraction line attributed to the X- 222 of the X- ray diffraction peak and the Y ₂ O ₃ surface at the 2θ = 52.2 ± 0.5 ° due to the crystal plane of the substrate surface and the horizontal It is a film of columnar structure in which the peak exists, and the intensity of the X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate is due to the (222) plane of Y ₂ O ₃ . Provided is a method for producing a plasma member having a range of 0.03 to 4.7 relative to the intensity of the X-ray diffraction peak.

In addition, the present invention comprises the steps of mounting the substrate to the substrate holder provided in the chamber of the electron beam deposition apparatus, the temperature of the substrate is set in the range of 50 ~ 800 ℃, and the electron beam scanned from the electron gun of the electron beam deposition apparatus is permanent Incident to an evaporation source consisting of Y ₂ O ₃ housed in a crucible and deflected by a magnet; the evaporation source is heated and melted as the electron beam is incident on the evaporation source; and a shutter located above the evaporation source. Open to allow the evaporated particles of the evaporation source to proceed upward along the evaporation path, Y ₂ O ₃ is deposited on one surface of the substrate mounted on the lower surface of the substrate holder, the Y ₂ O ₃ coating film is 0.2 to 5 When the coating is in the thickness range of 탆, the coating is stopped and rested for 10 to 300 minutes, and then the shutter located at the top of the evaporation source is opened to allow Y ₂ O ₃ to be deposited. When the Y ₂ O ₃ coating film is coated with a thickness of 0.2 ~ 5㎛ range to repeat the step of stopping the coating for 10 to 300 minutes to form a Y ₂ O ₃ coating film of the desired thickness, power supply The power applied to the electron gun through the device is set in the range of 1.9 to 10 kW, and the substrate holder is set to rotate at a speed in the range of 1 to 100 rpm to form a Y ₂ O ₃ coating film on the substrate, wherein the Y ₂ O _{3 The} coating film has a columnar structure in which the X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate and the X-ray diffraction peak due to the (222) plane of Y ₂ O ₃ are present. Film, wherein the intensity of the X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate is due to the (222) plane of the Y ₂ O ₃ Provided is a method for producing a plasma member having a range of 0.03 to 4.7 relative to strength.

While the evaporation source is evaporated, it is preferable to allow oxygen to be supplied into the chamber through a gas supply means, and to control the flow rate of the supplied oxygen to be in the range of 0.01 to 20 sccm.

While the evaporation source is evaporated, it is preferable to control the vacuum of the chamber to be in the range of 0.01 to 1 mTorr.

The rate at which the Y ₂ O ₃ coating film is deposited is preferably controlled to achieve a range of 30 to 120 nm / min.

The Y ₂ O ₃ coating film and particle size 5~50㎚ forming the thickness of the Y ₂ O ₃ coating layer is preferably formed to control the 0.5~50㎛ range.

The Y ₂ O ₃ coating film is a dense film having an average surface roughness in the range of 1 to 500 nm.

The substrate may be made of a silicon-based, oxide-based, nitride-based, carbide-based, or non-oxide-based ceramic sintered material.

The plasma member may be used as a cathode, a focus ring, an insulator ring, a shield ring, a bellows cover, or a depot shield exposed to a plasma environment generated in a gas atmosphere containing a halogen compound.

When the coating is stopped, the supply of power applied to the electron gun is cut off, or the evaporation path of the evaporation source is blocked with a shutter, and the temperature of the substrate is constant in the range of 50 to 800 ° C. while the coating is stopped. It is desirable to remain.

According to the present invention, a shrinkage and expansion difference between the substrate and the Y ₂ O ₃ coating film can be alleviated to form a thick coating film having a thickness of 0.5 to 50 µm without cracking.

Also, in order to overcome the critical thickness at which a crack occurs over a certain thickness of the ceramic film, a method of repeatedly depositing a 0.2 to 5 μm ceramic film to form a film at a critical thickness or more without cracking is performed in a high density plasma environment. It is possible to realize a plasma member that is durable and can be used for a long time.

The Y ₂ O ₃ coating film having a columnar structure formed by electron beam evaporation according to the present invention has no large pores of 0.1 μm or more and has an average surface roughness of 500 nm or less, and a YF-based reaction layer is formed on the surface in a plasma environment. Since the layer is stable to chemical reaction, it maintains a stable state in a plasma corrosive environment and thus exhibits excellent etching resistance. Therefore, contaminant particles are not generated and life can be improved even when used as a plasma member. The Y ₂ O ₃ coating film has no crack, has a sufficiently low surface roughness so as not to be selectively etched by the accelerated particles generated in the plasma, does not have large pores larger than 0.1 μm, and the reaction gas generated in the plasma does not flow into the interior. A dense and stable membrane is formed.

1 is a view schematically showing an electron beam deposition apparatus.
FIG. 2 is a graph showing X-ray diffraction (XRD) patterns of Y ₂ O ₃ coating films formed according to Example 1, Comparative Example 2, and Comparative Example 3. FIG.
3 is a graph showing an X-ray diffraction (XRD) pattern of the Y ₂ O ₃ coating film formed according to Examples 1 to 4.
FIG. 4 is a scanning electron microscope (SEM) photograph and a transmission electron microscope (SEM) photograph showing a cross section when a Y ₂ O ₃ coating film is formed on a substrate at 600 ° C. in a thickness of 8 μm according to Example 4. FIG. ; TEM) picture.
FIG. 5 is a scanning electron microscope (SEM) photograph showing a cross section when a Y ₂ O ₃ coating film is formed on a substrate at 300 ° C. in a thickness of 4 μm according to Comparative Example 1. FIG.
FIG. 6 is a scanning electron microscope (SEM) photograph showing a cross section when a Y ₂ O ₃ coating film is formed on a substrate at 300 ° C. in a thickness of 4 μm according to Comparative Example 1. FIG.
FIG. 7 is a diagram schematically showing particle distributions that contribute to each X-ray diffraction peak according to the thickness of a Y ₂ O ₃ coating film.
8 is a 30-minute rest after coating the Y ₂ O ₃ coating film to the substrate at 300 ℃ 0.5 ㎛ thickness in accordance with Example 5, again coating the Y ₂ O ₃ coating film to 0.5 ㎛ thickness in 30 minutes The optical microscope photograph of the surface of the Y ₂ O ₃ coating film formed to a thickness of the final 2㎛ by repeating the method of rest.
9 is an optical microscope photograph of the surface of the Y ₂ O ₃ coating film formed in a thickness of 2㎛ continuously without rest in the middle of the substrate at 300 ℃ according to Comparative Example 5.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the following embodiments are provided to those skilled in the art to fully understand the present invention, and may be modified in various forms, and the scope of the present invention is limited to the embodiments described below. It doesn't happen. Like numbers refer to like elements in the figures.

The present invention includes a substrate and a Y ₂ O ₃ coating film formed on the substrate, wherein the Y ₂ O ₃ coating film is X-ray diffraction at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate X-ray diffraction peak due to the peak and the (222) plane of Y ₂ O ₃ is a film of columnar structure, X-ray at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate Presenting a plasma member in which the intensity of the diffraction peak ranges from 0.03 to 4.7 relative to the intensity of the X-ray diffraction peak due to the (222) plane of Y ₂ O ₃ . The Y ₂ O ₃ coating film has a thickness in the range of 0.5 to 50㎛, the particle size of the Y ₂ O ₃ coating film is preferably from 5 to 50nm. The Y ₂ O ₃ coating film is a dense film having an average surface roughness in the range of 1 to 500 nm. The substrate may be made of a silicon-based, oxide-based, nitride-based, carbide-based, or non-oxide-based ceramic sintered material. The plasma member may be used as a cathode, a focus ring, an insulator ring, a shield ring, a bellows cover, or a depot shield exposed to a plasma environment generated in a gas atmosphere containing a halogen compound.

The Y ₂ O ₃ coating film has no large pores of 0.1 μm or more and has an average surface roughness of 500 nm or less, and a YF-based reaction layer is formed on the surface in a plasma environment, and the reaction layer is stable in a chemical reaction, and thus is stable in a plasma corrosion environment. It maintains the state, and thus, contaminant particles are not generated and life can be improved even when used as a plasma member.

Hereinafter, a method of manufacturing the plasma member using the electron beam evaporation method according to a preferred embodiment of the present invention.

The electron beam evaporation method is performed by mounting a substrate on which a coating film is to be deposited in a vacuum chamber maintaining high vacuum, and depositing the object by evaporation from a crucible containing an object (evaporation source) to be deposited on the substrate.

1 is a view schematically showing an electron beam deposition apparatus.

Referring to FIG. 1, the electron beam deposition apparatus includes a vacuum chamber 10 for maintaining a vacuum, an electron gun 20 is installed below the vacuum chamber 10, and an evaporation source in a position adjacent to the electron gun 20. A crucible 30 (crucible) containing an evaporation source is installed. Between the electron gun 20 and the crucible 30 is disposed a permanent magnet (not shown) for deflecting the electron beam irradiated from the electron gun 20 by the magnetic field to enter the evaporation source contained in the crucible 30. The substrate holder 40 is installed on the upper side of the vacuum chamber 10 opposite to the evaporation source, and the substrate 50 on which the evaporation source is melted and deposited is installed on the lower surface of the substrate holder 40. The substrate holder 40 may be rotatably provided for uniform deposition. A shutter 60 is provided on the evaporation source to block the evaporation path to the substrate 50 until the evaporation source is heated and melted. A blocking plate 70 is provided between the evaporation source and the substrate 50 to minimize the damage of the substrate 50 by the secondary electrons generated during the electron beam deposition. The blocking plate 70 is made of a conductive material such as a copper plate and is connected to a direct current power source. In addition, the electron beam deposition apparatus is provided with a sensor 80 for detecting the thickness of the film deposited on the substrate 50, the gas supply means 90 for supplying oxygen (O ₂ ) gas into the vacuum chamber 10 And a valve 95 is provided. In FIG. 1, P / S means a power supply.

In the electron beam deposition apparatus having the structure as described above, the electron beam scanned from the electron gun 20 is deflected by the permanent magnet and is incident on the evaporation source made of Y ₂ O ₃ contained in the crucible 30, and thus the evaporation source is heated. Melting In this case, since the shutter 60 is positioned above the evaporation source, the evaporation path of the evaporation particles is blocked. The shutter 60 opens the evaporation path, and the evaporated particles of the evaporation source travel upward along the evaporation path and are deposited on one surface of the substrate 50 mounted on the lower surface of the substrate holder 40.

Hereinafter, a method of manufacturing the plasma member using the electron beam evaporation method will be described in detail.

Suitable substrates for forming the ceramic coating film using the electron beam evaporation method are silicon, oxide-based, nitride-based carbide, non-oxide-based ceramic sintered bodies, and the like. In addition, in the case of the plasma material for manufacturing a semiconductor device or display, quartz, which is widely used for members such as a chamber liner, a CVD boat, a focus ring, and a wall liner (SiO ₂ ) and silicon (Si), and the like, and ceramics such as alumina (Al ₂ O ₃ ) and aluminum nitride (AlN) used in electrostatic chucks and heaters. Material may be applied.

In order to form a ceramic coating film, it is preferable that the surface of the substrate is subjected to mirror polishing to treat Y ₂ O ₃ after the average surface roughness Ra has a surface roughness of 100 nm or less. This is because when the average surface roughness Ra of the substrate is 100 nm or more, the surface roughness adversely affects the microstructure and surface roughness of the Y ₂ O ₃ coating film. The Y ₂ O ₃ coating film coated on the substrate is preferably formed to a thickness of 0.5 ~ 50㎛. The reason is that the life of the plasma member is short in the case of 0.5 μm or less, and the coating film may fall off due to cracks caused by the thermal stress difference between the substrate and the coating layer in the case of 50 μm or more, which may cause serious problems during the plasma process.

The Y ₂ O ₃ coating film coated on the substrate for use as the plasma member exhibits excellent etching resistance in a plasma environment containing halogen gas. According to the researches of the present inventors, Y ₂ O ₃ maintains a stable state in a plasma corrosion environment because a YF-based reaction layer is formed on the surface in a fluorine-based plasma environment having strong bonding force with oxygen and the reaction layer is stable to chemical reaction.

Since the Y ₂ O ₃ coating film formed by the conventional spraying method has a surface roughness of 5000 nm or more and contains a lot of pores therein, the reaction gas penetrates into the coating film through the pores, thereby increasing the frequency of contaminating particles and increasing the surface. The roughness causes selective etching, which is a major cause of shortening the life of the plasma member.

Hereinafter, a method of manufacturing the plasma member according to a preferred embodiment of the present invention.

The substrate is mounted on a substrate holder provided in the chamber of the electron beam evaporation apparatus, and the temperature of the substrate is set in the range of 400 to 800 ° C. The substrate holder is set to rotate at a speed in the range of 1 to 100 rpm.

The electron beam scanned from the electron gun of the electron beam deposition apparatus is deflected by the permanent magnet to be incident to the evaporation source consisting of Y ₂ O ₃ contained in the crucible. The power applied to the electron gun through the power supply is set in the range of 1.9 to 10 kW.

As the electron beam is incident on the evaporation source, the evaporation source is heated and melted.

The shutter positioned above the evaporation source is opened to allow evaporated particles of the evaporation source to proceed upward along the evaporation path and to deposit Y ₂ O ₃ on one surface of the substrate mounted on the lower surface of the substrate holder. While the evaporation source is evaporated, oxygen is supplied into the chamber through a gas supply means, and the flow rate of the supplied oxygen is controlled to be in a range of 0.01 to 20 sccm. While the evaporation source is evaporated, it is preferable to control the vacuum of the chamber to be in the range of 0.01 to 1 mTorr. The rate at which the Y ₂ O ₃ coating film is deposited is controlled to achieve a range of 30 to 120 nm / min, and the thickness of the Y ₂ O ₃ coating film is controlled to achieve a range of 0.5 to 50 μm.

Hereinafter, a method of manufacturing the plasma member according to another preferred embodiment of the present invention.

The substrate is mounted on a substrate holder provided in the chamber of the electron beam evaporation apparatus, and the temperature of the substrate is set in the range of 50 to 800 ° C. The substrate holder is set to rotate at a speed in the range of 1 to 100 rpm.

The electron beam scanned from the electron gun of the electron beam deposition apparatus is deflected by the permanent magnet to be incident to the evaporation source consisting of Y ₂ O ₃ contained in the crucible. The power applied to the electron gun through the power supply is set in the range of 1.9 to 10 kW.

As the electron beam is incident on the evaporation source, the evaporation source is heated and melted.

By opening the shutter located above the evaporation source to allow the evaporation particles of the evaporation source to proceed upward along the evaporation path, Y ₂ O ₃ is deposited on one surface of the substrate mounted on the lower surface of the substrate holder, Y ₂ O ₃ coating film when coated to a thickness of 0.2~5㎛ range to stop the coating to be 10-300 minutes at rest, and again opening the shutter is located at an upper side of the evaporation source, Y ₂ O ₃ is deposited for Y ₂ O _{3 When the} coating film is coated to a thickness of 0.2 ~ 5㎛ range to stop the coating and repeat for 10 to 300 minutes to form a Y ₂ O ₃ coating film of the desired thickness. While the evaporation source is evaporated, oxygen is supplied into the chamber through a gas supply means, and the flow rate of the supplied oxygen is controlled to be in a range of 0.01 to 20 sccm. While the evaporation source is evaporated, it is preferable to control the vacuum of the chamber to be in the range of 0.01 to 1 mTorr. The rate at which the Y ₂ O ₃ coating film is deposited is controlled to achieve a range of 30 to 120 nm / min, and the thickness of the Y ₂ O ₃ coating film is controlled to achieve a range of 0.5 to 50 μm.

When the coating is stopped, the supply of power applied to the electron gun is cut off or the evaporation path of the evaporation source is shuttered, and the temperature of the substrate is constant in the range of 50 to 800 ° C. while the coating is stopped. It is desirable to remain.

The thus formed Y ₂ O ₃ coating film had an X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to a crystal plane parallel to the surface of the substrate and an X-ray diffraction due to the (222) plane of Y ₂ O ₃ . It is a film of columnar structure in which the peak exists, and the intensity of the X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate is due to the (222) plane of Y ₂ O ₃ . The intensity of the X-ray diffraction peak ranges from 0.03 to 4.7, and the particle size of the Y ₂ O ₃ coating layer is about 5 to 50 nm. The Y ₂ O ₃ coating film is a dense film having an average surface roughness in the range of 1 to 500 nm.

The Y ₂ O ₃ coating film formed by the method according to the preferred embodiment of the present invention has no large pores of 0.1 μm or more and has a surface roughness of 500 nm or less, and a YF-based reaction layer is formed on the surface in a plasma environment and the reaction layer is chemically formed. Since it is stable to the reaction, it maintains a stable state in a plasma corrosive environment, so that contaminant particles are not generated and life can be improved even when used as a plasma member.

Hereinafter, the embodiments of the present invention will be described in more detail, and the present invention is not limited to the following examples.

≪ Example 1 >

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 600 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source move upward along the evaporation path by opening the shutter located above the evaporation source, and the substrate mounted on the bottom surface of the substrate holder. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 58nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 4㎛.

<Example 2>

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 600 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source travel upward along the evaporation path by opening the shutter located above the evaporation source. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 60nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 1㎛.

<Example 3>

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 600 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source move upward along the evaporation path by opening the shutter located above the evaporation source, and the substrate mounted on the bottom surface of the substrate holder. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 61nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 2㎛.

<Example 4>

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 600 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source travel upward along the evaporation path by opening the shutter located above the evaporation source. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 60nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 8㎛.

In order to more easily understand the characteristics of the above Examples 1 to 4 are presented comparative examples that can be compared with the embodiments of the present invention.

Comparative Example 1

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 300 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source move upward along the evaporation path by opening the shutter located above the evaporation source, and the substrate mounted on the bottom surface of the substrate holder. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 63nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 4㎛.

Comparative Example 2

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 80 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source travel upward along the evaporation path by opening the shutter located above the evaporation source. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 60nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 4㎛.

Comparative Example 3

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 300 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source travel upward along the evaporation path by opening the shutter located above the evaporation source. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 59nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 2㎛.

<Comparative Example 4>

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 80 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source move upward along the evaporation path by opening the shutter located above the evaporation source, and the substrate mounted on the bottom surface of the substrate holder. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 62nm / min. The Y ₂ O ₃ coating film deposited on the substrate was formed to a thickness of 2㎛.

An X-ray diffraction pattern was observed for the Y ₂ O ₃ coating film formed according to Examples 1 to 4 and Comparative Examples 1 to ₂ using the X-ray diffraction method. 2 and FIG. 3. In Figure 2 (a) is an X-ray diffraction pattern of the Y ₂ O ₃ coating film formed in a thickness of 4㎛ on a substrate of 600 ℃ in accordance with Example 1, (b) is a substrate at 300 ℃ according to Comparative Example 1 X-ray diffraction pattern of the Y ₂ O ₃ coating film formed to a thickness of 4㎛, (c) is X-ray diffraction pattern of the Y ₂ O ₃ coating film formed to a thickness of 4㎛ on a substrate of 80 ℃ according to Comparative Example 2 to be. In Figure 3 (a) is an X-ray diffraction pattern of the Y ₂ O ₃ coating film formed in a thickness of 8㎛ on a substrate of 600 ℃ according to Example 4, (b) is a substrate of 600 ℃ according to Example 1 X-ray diffraction pattern of the Y ₂ O ₃ coating film formed to a thickness of 4㎛, (c) is X-ray diffraction pattern of the Y ₂ O ₃ coating film formed to a thickness of 2㎛ on a substrate at 600 ℃ according to Example 3 (D) is an X-ray diffraction pattern of the Y ₂ O ₃ coating film formed on the substrate at 600 ° C. in a thickness of 1 μm according to Example 2.

Comparative Example 1, as also shown in 2 and Comparative Example 2, 400, 222, direction texturing is generated 2θ = 52.2 ± at 0.5 ° in the first embodiment than the diffraction peak does not substantially observed Y ₂ O, respectively _In the case of ₃ coating film, strong diffraction peak was found at 2θ = 52.2 ± 0.5 °.

In addition, in the case of the Y ₂ O ₃ coating film formed at 600 ℃ according to Examples 1 to 4 as shown in Figure 3 as the thickness increases to 1 ~ 8㎛ diffraction peak and Y at 2θ = 52.2 ± 0.5 ° The ratio of diffraction peak intensity on the ₂ 0 ₃ (222) plane tends to increase.

FIG. 4 is a scanning electron microscope (SEM) photograph and a transmission electron microscope (SEM) photograph showing a cross section when a Y ₂ O ₃ coating film is formed on a substrate at 600 ° C. in a thickness of 8 μm according to Example 4. FIG. ; TEM) picture. FIG. 5 is a scanning electron microscope (SEM) photograph showing a cross section when a Y ₂ O ₃ coating film is formed on a substrate at 300 ° C. in a thickness of 4 μm according to Comparative Example 1, and FIG. 6 is 300 ° C. according to Comparative Example 2. Scanning electron microscope (SEM) photograph showing a cross section of the case where the Y ₂ O ₃ coating film is formed on the substrate of 4㎛ thickness.

4 to 6, when the microstructure of the cross section was observed through the scanning electron microscope, it was confirmed that the dense film of the columnar structure was formed without cracking as shown in FIG. On the other hand, when coated at a substrate temperature of 300 ° C. as in Comparative Example 1 and at a substrate temperature of 80 ° C. as in Comparative Example 2, the interface of the substrate from the surface was 4 μm or less as shown in FIGS. 5 and 6. Deep cracks were formed until. This difference is understood to be the case in Example 4 that the strong diffraction peaks appearing at 2θ = 52.2 ± 0.5 ° improve the durability of Y ₂ O ₃ coated on the substrate.

In addition, through the transmission electron microscope (TEM) analysis shown in Figure 4 it was confirmed the particle size of the Y ₂ O ₃ coating membrane.

Using the alpha step, the average surface roughness Ra of the Y ₂ O ₃ coating film was determined under the condition of a profile length of 10 mm. The Y ₂ O ₃ coating film formed under the same process conditions by the electron beam deposition method was able to obtain a small particle size of 5 ~ 20nm and a low average surface roughness of 4 ~ 64nm.

Table 1 below shows the average surface roughness, diffraction peak intensity ratio, and presence of cracks according to temperature, deposition rate, and thickness of the Examples and Comparative Examples.

Substrate temperature (℃) Coating film thickness (㎛) Deposition rate (nm / min) Average Surface Roughness Ra (nm) I _{2θ = 52.2 ± 0.5 °} / I _{Y2O3 (222)} Crack presence Example 1 600 4 58 10 2.7 radish Example 2 600 One 60 5 0.03 radish Example 3 600 2 61 11 0.4 radish Example 4 600 8 60 14 4.7 radish Comparative Example 1 300 4 63 4 0.00 U Comparative Example 2 80 4 60 64 0.00 U Comparative Example 3 300 2 59 5 0.00 U Comparative Example 4 80 2 62 24 0.00 U

Referring to Table 1, in the case of Examples 1 to 4, as the thickness of the Y ₂ O ₃ coating film increased to 1, 2, 4, and 8 μm, 2θ = 52.2 ± The intensity of the X-ray diffraction peak at 0.5 ° is compared to the intensity of the X-ray diffraction peak due to the (222) plane of Y ₂ O ₃ (I _{2θ = 52.2 ± 0.5 °} / I Y ₂ O _{3 (222)} ) from 0.03 to 4.7 As shown in FIG. 7, it can be inferred that the particle distribution contributing to each X-ray diffraction peak varies depending on the thickness of the Y ₂ O ₃ coating film as shown in FIG. 7. That is, Y ₂ O ₃ when the thickness of the coating film 1㎛ or less, a Y ₂ O ₃ (222) thickness of the X- ray is mainly distributed particles that contribute to the diffraction peak, and Y ₂ O ₃ coating film due to the surface of the second As it increases to 4, 8 μm, it is found that more and more particles contribute to the X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to the crystal plane parallel to the surface of the substrate.

Hereinafter, other embodiments of the present invention will be described in detail, and the present invention is not limited to the following examples.

Example 5

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 300 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source travel upward along the evaporation path by opening the shutter located above the evaporation source. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 60nm / min. After coating the Y ₂ O ₃ coating film with a thickness of 0.5 μm, the coating was stopped for 30 minutes, and again, the same method was used to coat the Y ₂ O ₃ coating film with a thickness of 0.5 μm for 30 minutes. Repeatedly, the final thickness of the Y ₂ O ₃ coating film was 2㎛. The process of stopping the coating for 30 minutes by stopping the coating was performed by shutting off the supply of power applied to the electron gun or by shuttering the evaporation path of the evaporation source.

<Example 6>

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 300 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source move upward along the evaporation path by opening the shutter located above the evaporation source, and the substrate mounted on the bottom surface of the substrate holder. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 61nm / min. Y ₂ O at rest for 30 minutes and then coated to a thickness of the coating film ₃ to 0.5㎛ and coated to a thickness of Y ₂ O ₃ coating film by the same method as 0.5㎛ again and repeat the method of tissue for 30 minutes and Y ₂ The final thickness of the O ₃ coating film was 4 μm. The process of stopping the coating for 30 minutes by stopping the coating was performed by shutting off the supply of power applied to the electron gun or by shuttering the evaporation path of the evaporation source.

Comparative Example 5

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 300 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source move upward along the evaporation path by opening the shutter located above the evaporation source, and the substrate mounted on the bottom surface of the substrate holder. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 59nm / min. Unlike Example 5 and Example 6, a Y ₂ O ₃ coating film was continuously deposited on the substrate to form a 2 μm thick Y ₂ O ₃ coating film.

Comparative Example 6

An evaporation source consisting of Y ₂ O ₃ housed in a crucible by mounting a 50 mm diameter silicon substrate mirror-polished to an average surface roughness of 10 nm or less on a substrate holder of an electron beam deposition apparatus, and the electron beam scanned from the electron gun is deflected by a permanent magnet. It was made to enter. At this time, the power applied to the electron gun through the power supply was set to 1.9 ~ 2.9kW. The distance between the substrate and the evaporation source was about 480 mm. The temperature of the substrate was set to 300 ° C., and the substrate holder was set to rotate at a speed of about 5 rpm. The flow rate of oxygen introduced into the vacuum chamber through the gas supply means was set to about 1 sccm. The vacuum degree of the vacuum chamber was set in the range of 0.1 mTorr.

As the electron beam enters the evaporation source, the evaporation source is heated and melted, and the evaporation particles of the evaporation source travel upward along the evaporation path by opening the shutter located above the evaporation source. It was to be deposited on one side of. The deposition rate of the Y ₂ O ₃ coating film deposited on the substrate surface was detected by the sensor, the deposition rate measured by the sensor was about 63nm / min. Examples 5 and 6 and is different in that Y ₂ O ₃ coating layer is continuously deposited on the substrate to form a coating film of a Y ₂ O ₃ 4㎛ thickness.

8 is a 30-minute rest after coating the Y ₂ O ₃ coating film to the substrate at 300 ℃ 0.5 ㎛ thickness in accordance with Example 5, again coating the Y ₂ O ₃ coating film to 0.5 ㎛ thickness in 30 minutes The optical microscope photograph of the surface of the Y ₂ O ₃ coating film formed to a thickness of the final 2㎛ by repeating the manner of rest, the optical microscope picture, Figure 9 is continuously without rest in the middle of the substrate at 300 ℃ according to Comparative Example 5 It is an optical microscope photograph of the surface of the Y ₂ O ₃ coating film formed to a thickness of 2㎛.

8 and 9, when the microstructure of the surface was observed through an optical microscope, cracks did not exist as shown in FIG. 8. However, as in Comparative Example 5, the Y ₂ O ₃ coating film continuously formed at a thickness of 2 μm on a 300 ° C. substrate can be seen that cracks are formed on the surface as shown in FIG. 9, and 300 ° C. as in Comparative Example 6 Cracks were also formed on the surface of the Y ₂ O ₃ coating film formed continuously on the substrate with a thickness of 4 μm.

After coating the Y ₂ O ₃ to a predetermined thickness by which a tissue to freeze the coating for a predetermined time (e.g., 10-300 minutes), then, a method of repeating the step of coating and the rest is again the Y ₂ coated on the substrate It can be seen that it plays a major role in forming the coating film without cracking beyond the critical thickness of O ₃ .

Table 2 below shows the average surface roughness Ra and crack presence according to the substrate temperature, deposition rate, and thickness of the Examples and Comparative Examples.

Substrate temperature (℃) Coating film thickness (㎛) Deposition rate
(Nm / min) Average surface roughness (nm) Crack presence Example 5 300 2 60 5 radish Example 6 300 4 61 6 radish Comparative Example 5 300 2 59 5 U Comparative Example 6 300 4 63 4 U

As mentioned above, although preferred embodiment of this invention was described in detail, this invention is not limited to the said embodiment, A various deformation | transformation by a person of ordinary skill in the art within the scope of the technical idea of this invention is carried out. This is possible.

10: vacuum chamber 20: electron gun
30: crucible 40: substrate holder
50: substrate 60: shutter
70: blocking plate 80: sensor
90: gas supply means 95: valve

Claims (15)

A substrate and a Y ₂ O ₃ coating film formed on the substrate, wherein the Y ₂ O ₃ coating film has a X-ray diffraction peak and Y ₂ at 2θ = 52.2 ± 0.5 ° due to a crystal plane parallel to the surface of the substrate. A film of columnar structure in which an X-ray diffraction peak due to the (222) plane of O ₃ exists, and the intensity of the X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to a crystal plane parallel to the surface of the substrate. The plasma member is characterized in that the range of 0.03 to 4.7 compared to the intensity of the X-ray diffraction peak due to the (222) plane of Y ₂ O ₃ .
The method of claim 1 wherein said Y ₂ O ₃ coating layer is a plasma member, characterized in that a thickness of 0.5~50㎛ range, and wherein the particle size forming the Y ₂ O ₃ coating layer is 5~50㎚.
The plasma member of claim 1, wherein the Y ₂ O ₃ coating film is a dense film having an average surface roughness of 1 to 500 nm.
The plasma member of claim 1, wherein the substrate is made of a silicon-based, oxide-based, nitride-based, carbide-based, or non-oxide-based ceramic sintered material.
The method of claim 1, wherein the plasma member is used as a cathode, a focus ring, an insulator ring, a shield ring, a bellows cover, or a depot shield exposed to a plasma environment generated in a gas atmosphere containing a halogen compound. No plasma resistance.
Mounting a substrate to a substrate holder provided in a chamber of an electron beam deposition apparatus, and setting a temperature of the substrate to a range of 400 to 800 ° C;
Causing the electron beam scanned from the electron gun of the electron beam deposition apparatus to be incident on an evaporation source consisting of Y ₂ O ₃ contained in the crucible;
Heating and melting the evaporation source as the electron beam is incident on the evaporation source; And
Opening the shutter located above the evaporation source to allow evaporated particles of the evaporation source to proceed upward along the evaporation path, and depositing Y ₂ O ₃ on one surface of the substrate mounted on the lower surface of the substrate holder. Include,
The power applied to the electron gun through the power supply is set in the range of 1.9 ~ 10kW, the substrate holder is set to rotate at a speed of 1 ~ 100rpm to form a Y ₂ O ₃ coating film on the substrate,
The Y ₂ O ₃ coating film has an X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to a crystal plane parallel to the surface of the substrate and an X-ray diffraction peak attributable to the (222) plane of Y ₂ O ₃ . X-ray diffraction peak intensity at 2θ = 52.2 ± 0.5 ° due to the crystal phase parallel to the surface of the substrate, which is a film of columnar structure present, due to the (222) plane of Y ₂ O ₃ A method for producing a plasma member comprising a range of 0.03 to 4.7 relative to the intensity of the line diffraction peak.
Mounting a substrate to a substrate holder provided in a chamber of an electron beam deposition apparatus, wherein the temperature of the substrate is set in a range of 50 to 800 ° C;
Causing the electron beam scanned from the electron gun of the electron beam deposition apparatus to be deflected by the permanent magnet and incident to an evaporation source consisting of Y ₂ O ₃ contained in the crucible;
Heating and melting the evaporation source as the electron beam is incident on the evaporation source; And
By opening the shutter located above the evaporation source to allow the evaporation particles of the evaporation source to proceed upward along the evaporation path, Y ₂ O ₃ is deposited on one surface of the substrate mounted on the lower surface of the substrate holder, Y ₂ O ₃ coating film when coated to a thickness of 0.2~5㎛ range to stop the coating to be 10-300 minutes at rest, and again opening the shutter is located at an upper side of the evaporation source, Y ₂ O ₃ is deposited for Y ₂ O _{When the} coating film is coated with a thickness of 0.2 ~ 5㎛ range to stop the coating to repeat for 10 to 300 minutes to repeat the step of forming a Y ₂ O ₃ coating film of the desired thickness,
The power applied to the electron gun through the power supply is set in the range of 1.9 ~ 10kW, the substrate holder is set to rotate at a speed of 1 ~ 100rpm to form a Y ₂ O ₃ coating film on the substrate,
The Y ₂ O ₃ coating film has an X-ray diffraction peak at 2θ = 52.2 ± 0.5 ° due to a crystal plane parallel to the surface of the substrate and an X-ray diffraction peak attributable to the (222) plane of Y ₂ O ₃ . X-ray diffraction peak intensity at 2θ = 52.2 ± 0.5 ° due to the crystal phase parallel to the surface of the substrate, which is a film of columnar structure present, due to the (222) plane of Y ₂ O ₃ A method for producing a plasma member comprising a range of 0.03 to 4.7 relative to the intensity of the line diffraction peak.
The method according to claim 6 or 7, wherein the oxygen is supplied into the chamber through a gas supply means while the evaporation source is evaporated, and the flow rate of the supplied oxygen is controlled to be in the range of 0.01 to 20 sccm. Method of manufacturing a plasma member.
The method of claim 6 or 7, wherein the vacuum degree of the chamber is controlled to be in a range of 0.01 to 1 mTorr while the evaporation source is evaporated.
The method of claim 6 or 7, wherein the deposition rate of the Y ₂ O ₃ coating film is controlled to achieve a range of 30 to 120nm / min.
In the sixth or claim 7, wherein the Y ₂ O ₃ particle size forming the coating film is 5~50㎚, in characterized in that the control is formed to a thickness 0.5~50㎛ range of the Y ₂ O ₃ coating film Method of manufacturing a plasma member.
The method of claim 6 or 7, wherein the Y ₂ O ₃ coating film is a dense film having an average surface roughness in the range of 1 to 500 nm.
The method of manufacturing a plasma member according to claim 6 or 7, wherein the substrate is made of a silicon-based, oxide-based, nitride-based, carbide-based, or non-oxide-based ceramic sintered material.
The method of claim 6 or 7, wherein the plasma member is used as a cathode, a focus ring, an insulator ring, a shield ring, a bellows cover, or a depot shield exposed to a plasma environment generated in a gas atmosphere containing a halogen compound. Method for producing a plasma member, characterized in that.
The method of claim 7, wherein the supply of power applied to the electron gun is interrupted when the coating is stopped, or the evaporation path of the evaporation source is shuttered, and the temperature of the substrate is 50 while the coating is stopped. A method for producing a plasma member, which is kept constant in the range of -800 ° C.

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