WO2007108549A1 - Plasma processing apparatus and plasma processing method - Google Patents

Plasma processing apparatus and plasma processing method Download PDF

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Publication number
WO2007108549A1
WO2007108549A1 PCT/JP2007/056130 JP2007056130W WO2007108549A1 WO 2007108549 A1 WO2007108549 A1 WO 2007108549A1 JP 2007056130 W JP2007056130 W JP 2007056130W WO 2007108549 A1 WO2007108549 A1 WO 2007108549A1
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Prior art keywords
plasma
gas
plasma processing
layer
chamber
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PCT/JP2007/056130
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French (fr)
Japanese (ja)
Inventor
Yoshiyuki Kobayashi
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Tokyo Electron Limited
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18After-treatment
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C26/00Coating not provided for in groups C23C2/00 - C23C24/00
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/042Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11Oxides
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32Gas-filled discharge tubes, e.g. for surface treatment of objects such as coating, plating, etching, sterilising or bringing about chemical reactions
    • H01J37/32431Constructional details of the reactor
    • H01J37/32458Vessel
    • H01J37/32477Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
    • H01J37/32495Means for protecting the vessel against plasma

Abstract

Provided is a plasma processing apparatus wherein durability of a part, a member and a component, which are exposed to plasma atmosphere in a chamber used for performing plasma etching in a corrosion resistant gas atmosphere is improved, resistance to plasma erosion of a film formed on the surface of the member and the like in the corrosion resistant gas atmosphere is improved, and furthermore, generation of particles of corrosion resistant products even under high plasma output is prevented. A plasma processing method using such plasma processing apparatus is also provided. In the plasma processing apparatus for processing the surface of a subject which is stored in the chamber to be processed is processed by etching process gas plasma. The part exposed to the plasma generating atmosphere in the chamber or the member arranged inside the chamber or the surface of the component is coated with at least a porous layer composed of a metal oxide and a secondary recrystallized layer of the metal oxide formed on the porous layer.

Description

Burazuma processing apparatus and plasma processing method art

The present invention relates to a plasma processing apparatus and plasma processing method as used in the field of semiconductor processing techniques, in particular halogen gas, inert gas, oxygen walk is and atmosphere such as hydrogen gas containing fluorine and fluorine compounds (hereinafter "F-containing gas" Akira

) And hydrocarbon gas (hereinafter referred to, environmental is consists by atmosphere or the like referred to as "containing CH Gas") or environment, such as those atmosphere is repeatedly formed alternately, plasma etching in a semiconductor device or the like It proposes a plasma processing apparatus and plasma processing method for performing such pressurized manual Engineering. BACKGROUND

Devices used in the fields of semiconductor and liquid crystal is often processed by using a plasma energy of highly corrosive halogen-based corrosive gas. For example, in Etsuchingu processing apparatus using plasma, which is one of the semiconductors processing apparatus, when forming and fine wiring pattern, a strong gas atmosphere Ah Rui corrosive chlorine Ya fluorine system, and these gases generating plasma in a mixed gas atmosphere of inert gas, whereby Etsuchin grayed the semiconductor device by utilizing the strong reactivity of the excited ions and electrons Kaeshi form a wiring pattern or the like.

Such a wall or inside a provided a member Ya unit products such reaction vessels used in the processing (susceptor, electrostatic chuck, electrodes, etc.), susceptibility Les erosion action by plasma energy, therefore, plasma-resistant it is necessary to use a material excellent in erosion resistance. For such requirements, conventionally, such a processing apparatus, corrosion resistance good metal (including alloys), quartz, materials such as alumina have been used. For example, Japanese Unexamined 1 0 4 0 8 3 discloses, the material, the surface of the reaction vessel inside material, corrosion resistance and good metal such coated by PVD or CVD or peripheral Kiritsuhyo of III or forming a film of oxides such a group element, or Y 2 0 3 technology that covers the single crystal is disclosed. Further, in JP-2 0 0 1 1 6 4 3 5 4 and JP-2 0 0 3 2 6 4 1 6 No. 9 in Japanese ,, periodic table III a element belonging to the oxides some Y 2 0 3, by coating the surface of the member by thermal spraying method, a technique for improving the resistance to plasmas erosion ^^ students is disclosed.

However, techniques of coating and metal Sani 匕物 of the Periodic Table Ilia group elements, while indicating relatively good plasma erosion resistance, more severe corrosive atmosphere gas, a high accuracy of machining and the environment in recent years in the field of semiconductor processing technology cleanliness of there is a demand, not in the adequate measures.

Also, members coated with Y 2 O 3 sprayed coating, but has helped to improve the resistance to plasma erosion resistance, processability recent semiconductor member, in addition to more high power plasma Etsuchingu action, working atmosphere corrosive a it is in the strong fluorine-based severe conditions of gas and a hydrocarbon-based gas is used alternately and repeatedly, and further improvement is demanded Me.

In particular, if such are used repeatedly and F-containing gas and containing CH gas alternately, F-containing gas atmosphere, the strong corrosion reaction of the halogen gas specific, although the generation of high off Tsu fluoride vapor pressure occurs, containing CH gas atmosphere, or decomposition is accelerated fluorinated compound produced in F-containing gas, it has the effect of partially raise the reaction to fluorided changed to carbide coating components occurs. Moreover, the plasma environment in which these gases are used, since the above-mentioned reaction is promoted, the more severe corrosive environments. In particular, high when performing Etsuchingu bra Zuma output, the potential difference between the inner wall of the plasma and the plasma processing chamber (chamber) increases, Y 2 0 3 sprayed coating coated on the inner wall surface is corroded, generated in such an environment particles of the corrosion products, fall attached to the integrated circuit surface of a semiconductor product, which since the device damage caused, for conventional member surface processing technology still has been required to further improvement. Disclosure of the Invention

The present invention, a portion exposed to the plasma atmosphere used is Ru chamber in one to the bra Zuma Etsu quenching processed in a corrosive gas atmosphere, members and parts (hereinafter, referred abbreviated as "member etc." a single. we propose a technique for improving the durability of).

This 宪明 also improved corrosive gas atmosphere, particularly F-containing gas and containing CH gases in the atmosphere is used to repeat alternately, plasma-resistant yellow John of the film formed on the surface of the member such as we propose a technique for.

The present invention also at high plasma power under proposes a plasma processing method capable of preventing the generation of particles corrosion products.

That is, the present invention, the surface of the object accommodated in the chamber of all, in a plasma processing apparatus for processing by etching gas plasma, sites exposed to plasmas generated atmosphere of the chamber one, this chamber one within distribution At least portion material or the surface of the component force, characterized in that it is Manzanillo connexion coated with secondary recrystallized layer of the porous layer and the metal oxide formed on the porous layer of a metal oxide it is a Burazuma processing apparatus.

In the plasma treatment apparatus of the present invention can employ the following configuration.

1. wherein the lower porous layer, providing an undercoat layer comprising a metal-alloy, ceramics or cermets.

2. The etching process, treatment with a fluorine-containing gas plasma is treated repeatedly alternately introduced mixed gas plasma by treatment, or a fluorine-containing gas and a hydrocarbon-containing gas of the fluorine-containing gas and hydrocarbon-containing gas It carried out in one of the methods.

3. The fluorine-containing gas, CF 4, Ji 4?31 gas 8 such, CHF-based gas, HF-based gas, SF-based gas and one selected from among the mixed gas of the these gases 0 2 using the above gas.

4. The hydrocarbon-containing gas, CH 4, C x H y gas, such as C 2 H 2, and H-containing gas and CH 4, such as NH 3 0 2, and CH 3 F and 0 2, CH 2 F 2 using one or more gases selected from among C x H y gas and mixed gas of 0 22.

5. The metal oxide is a metallic oxide containing III a group element such as S c, Y and lanthanoid.

6. The secondary recrystallized layer, by high energy irradiation treatment of the primary transformation metal oxide contained in the porous layer, and forming by the secondary transformation.

7. The secondary recrystallized layer is Natsuta layer tetragonal structure and by connexion secondary transformation porous layer to high energy radiation treatment comprising a crystalline orthorhombic.

8. The high-energy irradiation treatment, an electron beam irradiation treatment or laser beam irradiation process.

9. The chamber of all, the site to be exposed to a plasma atmosphere, and said the member or the front surface of the component Burazuma, has the following potential difference 120 V or 550 V.

10. The potential difference is controlled by the high frequency power applied to the mounting table of the workpiece provided in the chamber in one.

Sites The present invention also the surface of the object which is accommodated in a chamber and foremost, to be exposed in the plasma processing method of processing by etching gas plasma, prior to this process, to a plasma atmosphere of the chamber one not a Well, this chamber one within mounting member or the surface of the component, and the porous layer made of a metal oxide, a composite layer comprising a secondary recrystallization layer of the metal oxide formed on the porous layer coating formed, then, the introduced first gas containing fluorine-containing gas into the chamber, to propose a plasma processing method characterized in that processing by generating a first plasma by exciting the gas .

Further, the present invention is that the surface of the object accommodated in the chamber of all, in a plasma processing method for by connexion processed into plasma etching process gas, prior to this process, first, the chamber one, is exposed to a plasma atmosphere that site, this chamber one the disposed members or parts of the surface, a composite comprising a porous layer made of a metal oxide and a secondary recrystallized layer of the metal oxide has been made form in the porous layer the layers were coated form, then this in the Chiyanba first containing fluorine-containing gas gas to generate a first plasma by exciting After introducing, then a second containing a hydrocarbon gas into the Chiyanba Suggest Burazuma processing method characterized in that processing by generating an excited allowed by second Burazuma After introducing gas.

Incidentally, the plasma processing method of the present invention can employ the following configuration. 1. The fluorine-containing gas is selected from among CF 4, C 4 C x F y gas such as F 8, CHF-based gas, HF-based gas, SF-based gas and these gases and a gas mixture of 0 2 use one or more of the gas.

2. The hydrocarbon-containing gas, CH 4, C 2 H 2 C x H y gas, such as, the H-containing gas and CH 4, such as NH 32, CH 3 F and the 0 2, CH 2 F 2 0 using one or more gases selected C x H y gas 2 such as from among the mixed gas of 0 2.

3. The metal oxide is a metallic oxide containing III a group element such as S c, Y and lanthanoid.

4. The secondary recrystallized layer, by a high energy Noregi irradiation treatment of the primary transformation metal oxide contained in the porous layer, and forming by the secondary transformation.

5. The secondary recrystallized layer is a layer porous layer becomes tetragonal structure with secondary transformation by high-energy radiation treatment comprising a crystalline orthorhombic.

6. The high energy irradiation treatment, an electron beam irradiation treatment or laser beam irradiation process.

7. Of the chamber in one, sites exposed to a plasma atmosphere, and the plasma and the member or the front surface of the component, having the following potential difference 120 V or 550 V.

8. The potential difference is controlled by the high frequency power applied to 载置 base of the object provided in the chamber in one.

According to the present invention, a semiconductor component or a liquid crystal component when plasma etching, plasma atmosphere, in particular halogen, such as F-containing gas atmosphere or F-containing gas atmosphere and the containing CH gas atmosphere is repeatedly formed alternately like under corrosive gas atmosphere, when the flop plasma etching Kae, can be long-term in Wataru connexion improve durability against plasma erosion, such as the chamber first internal member.

The present according to the invention, plasma etching or fewer particles and the like are markedly members such as the potential corrosion products generated due to the Burazuma in the chamber one, the efficiency of high-quality semiconductor components such as well it is possible to produce. Furthermore, according to the present invention, since the forming characteristic film on the surface of the member such as will be able to increase the output of the plasma up to about 550 V, to improve the effect of velocity and etching of the etching, it can thus reduce the size 'weight of the plasma processing apparatus. BRIEF DESCRIPTION OF THE DRAWINGS

Figure 1 is a diagram showing a schematic configuration of a plasma processing apparatus in accordance with an embodiment of the present invention. 2, the potential applied to the processing chamber within the member or the like, is a diagram showing the relationship between Y 2 0 3 due to dust (Pate Ital) emissions.

3, the potential applied to the processing chamber within the member or the like, is a diagram showing the relationship between Upsilon 2 0 3 due to dust (Pate Ikunore) emissions.

Figure 4 is a cross-sectional view having the film formed by the method according to the prior art (a), member obtained by forming secondary recrystallization layer as the outermost layer by the method of the present invention (b), and Andako member having one bets it is a partial cross-sectional view of (C).

Figure 5 is an X-ray diffraction diagram of the secondary recrystallized layer is formed by Y 2 0 3 sprayed coating (porous layer) and the electron beam irradiation treatment.

Figure 6 is an X-ray diffraction pattern of the electron beam irradiation treatment prior to the state of Upsilon 2 0 3 sprayed coating (porous layer).

Figure 7 is an X-ray diffraction diagram of the state after the electron beam irradiation treatment of Upsilon 2 0 3 sprayed coating (porous layer). - DETAILED DESCRIPTION OF THE EMBODIMENTS

Hereinafter, an example embodiment of the present invention, the details, described with reference to the drawings. Figure 1 is a chamber part sectional view of a plasma processing apparatus to which the present invention is applied. In the plasma treatment apparatus of the present invention is not limited to the structure shown in FIG.

In Figure 1, reference numeral 1 denotes an etching processing chamber one. The Chi Yanba 1, for example, Anoremi having an anodic oxide coating (alumite treatment) to the surface - have a © beam made cylindrical chamber one, a structure that can hold the etching chamber airtight.

The chamber 1 has, in its interior, a lower electrode 2, for holding Coulomb force to be processed object such as a semiconductor the wafer W, the electrostatic Cha click 3 arranged on the upper surface of the lower electrode 2, upper electrode 4 or the like which is arranged at a predetermined distance above the electrostatic chucking 3 is disposed. The electrostatic chuck 3 is for example, between the insulating film ing a polyimide resin or the like, has a structure in which an electrode for an electrostatic chuck, the upper 'lower electrode 2, 4 are respectively similar to the chamber one 1 Les, is preferably be by connexion formed in the material of.

Then, the lower electrode 2 Oyopi electrostatic chucking 3 constitutes a 载置 table 5 for placing the wafer W. The mounting table 5, via a lower matcher 6, connected lower radio frequency power source (RF power source) 7 is, from its lower radio frequency power source 7, such as high-frequency power of a predetermined frequency can be supplied connexion there. Further, the upper electrode 4, through the upper matcher 8, upper radio frequency power source (RF power source) 9 is connected. Its upper electrode 4 is a large number of gas discharge holes 1 0 is provided on its lower surface, whereas the top thereof, the gas supply unit 1 1 is provided.

Wherein the chamber one 1, although not shown in FIG. 1, the exhaust device is connected via a pipe. The Champa in one 1 ^ by the gas device is adjusted for example 1. 3 3 such that P a to 1 3 3 P a degree of pressure. Then, said through the gas inlet 1 1, a predetermined plasma processing gas into the chamber one 1, for example, etching gas made of F-containing gas is introduced.

In this state, a relatively frequency of the low-les from the lower frequency power source 7, a predetermined high-frequency power, for example, with frequency supplies the following frequency power number MH z, from the upper high-frequency power supply 9, a relatively frequency predetermined high frequency power of, for example, by frequency supplying high-frequency power of several tens of MH Z~ hundred MH z, between the upper electrode 4 and the lower electrode 2 can be generated plasma. The treatment Ritai surface such as a semiconductor wafer W can be etched processed by the plasma. It should be noted that the high frequency power supplied from the upper part high-frequency power source 9 to the upper electrode 4, which is used in order to generate Burazuma, whereas, the high frequency power that will be supplied from the lower frequency power source 7 to 载置 stand 5, DC bias is generated and used to control the energy of ions impinging on the semiconductor wafer W.

Incidentally, in the processing chamber one 2, the upper electrode 4 as shown in FIG. 1, other mounting table 5 consists of the lower electrode 2 or the electrostatic chuck 3, the shield ring 1 2, full Oka slings 1 3, Deposhi one Noredo 1 4, Appa one Inshureta 1 5, members and the like, such as the lower one Inshiyureta 1 6 and baffle plate 1 7 is arranged, Shino TOLEDO ring 1 2 and the focus ring 1 3, for example, silicon carbide Ya silicon is intended substantially ring-shaped had it occurred formed, it is disposed so as to surround the outer periphery of each of the upper electrode 4 and the lower electrode 2, semiconductor Weha W plasma generated between the upper electrode 4 and the lower electrode 2 and it is configured to converge to.

A deposition shield 1 4, which is provided to protect the inner wall of Chiyanba 1, Upper in Shiyu rater 1 5 and the lower one Inshiyureta 1 6, in order to retain the atmosphere in the chamber one 1 provided, the Roi one Inshure motor 1 6 under the baffle plate 1 7, the generated plasma is provided to contain not to flow out from the exhaust port 1 8 located below side of the plasma processing apparatus, these etc. disposed in the Chiyanba the first member, at the time of plasma etching, the or F-containing gas atmosphere, containing F gas and containing CH gas is introduced alternately and repeatedly so that strong corrosive environment of plasma excited It is exposed to the atmosphere.

The F-containing gas atmosphere mainly contains fluorine or a fluorine compound, or may further include an oxygen (0 2). Fluorine is rich in particular reactive among halogen elements (highly corrosive), metal is characterized in that as well react with Sani 匕物 and carbides make high vapor pressure corrosion products. Therefore, if members like the chamber one 1, is subjected to a plasma under highly corrosive atmosphere such as the F-containing gas atmosphere, even it if the metal was filed by well oxide or carbide without generating a protection film for inhibiting the progression of corrosion reaction on the surface, the corrosion reaction will proceed without limit. In this respect, according to where the inventor has knowledge, among these environments, an element belonging to periodic table III a group, i.e., S c and Y, elements of atomic numbers 5 7-7 1 as well as their Sani 匕物for, it was found to exhibit good corrosion resistance.

Meanwhile, in the containing CH gas atmosphere, but not highly corrosive to the CH itself, to constitute an entirely opposite reduction atmosphere and the oxidation reaction proceeding in the F-containing gas atmosphere, relatively stable in F-containing gas metal (alloy) or a metal compound showing a corrosion resistance, then, including

When in contact with the CH gas atmosphere, chemical bonding force tends to be weak. Thus, portion in contact with the free CH gas when exposed to F-containing gas atmosphere again, initial stable compound film is chemically Yabu壌, eventually leading to the phenomenon that the corrosion reaction proceeds.

In particular, in addition to the change of the ambient gas species, in an environment such as a plasma is generated, F, CH both ionized and reactive strong atomic F, C, because H is generated, corrosive and - reducing properties is accelerated by the plasma erosion action further intensified, corrosion products from the surface of such member is easily generated.

Thus the corrosion products formed in the or vaporized in the environment, also you significantly contaminate the Burazuma processing vessel, such as the chamber scratch a fine pore of the particle.

In this regard, in the method of treatment using a plasma processing apparatus according to the present invention, the F-containing gas atmosphere or a mixed gas atmosphere of F-containing gas and containing CH gas, and the F-containing gas atmosphere and containing CH gas atmosphere severe as are alternately repeated, is effective as a corrosion arrangement erosion measures that put in a corrosive environment, it is also effective in generating blocking, suppressing the generation of particles, especially of the corrosion products. Therefore, in the present invention is disposed within the chamber, to the surface of such a member at which is 囉 to the plasma simultaneously plasma processing a root bark processed, a metal oxide containing elemental belonging to III a group comprising a porous layer, the porous layer, Ri by the providing a composite film obtained by forming secondary recrystallization layer obtained by the metal acid I arsenide was allowed to secondary transformation, of the member, such as and to suppress the corrosion reaction. The composite film may be formed on all the member from the chamber one, in particular the plasma density is high, it is needless to say that it may be formed by selecting only the larger part of the damage.

As the F-containing gas, F 2, CF 4, C 4 F S, such as C 4 F 6 and C 5 F 8, other gases represented by one general formula C x F y, CHF 3, CH 2 F 2 and CH 3 CH F-based gas such as F, HF-based gas least one gas selected from a gas mixture of fluorine gas and O 2 represented by CFO system such as SF-based gas and CF 2 0, such as SF 6 it is preferably used.

As examples of the containing CH gas, other H 2, CH 4, C 2 H 2, CH 3 F, etc. CH 2 F 2, CHF 3 C x H y gas, and H-containing gas such as NH 3, the walk-containing CH gas is good preferable to use at least one gas selected from a gas mixture of H-containing gas and 0 2.

Next, the inventors of the composite film-forming material, in particular even in an atmosphere of F-containing gas and containing CH Gas good corrosion resistance Ya environmental pollution of forming on the surface of the member or the like which is disposed in the chamber in one We were examined for the material shown.

As a result, as the metal oxide for forming the porous layer, and excellent compared to the metal oxide power other oxides of the elements belonging to Ilia of the periodic table Te corrosive environment odor resistance to halogen corrosive it was divide showing resistance to plasma erosion property (stain due party cycle of corrosion products).

III The metal oxide of a group element, Sc, Rantanoido Y and atomic number 57~71 (La, Ce, Pr, Nb, Pm, Sra, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, a Sani 匕物 of Lu), particularly for lanthanide, La, Ce, Eu, Dy, rare earth oxides Yb is good suitable. In the present invention, these metal oxides alone or in combination, double oxide, can be used with a eutectic.

In the present invention, a porous layer comprising the metal oxide, as a method of coating formed on the surface on the Jo Tokoro thickness of the member or the like, the spraying method is used as a suitable example. That is, the metal Sani 匕物 of III a group element, an average particle diameter of the thermal spraying material powder consisting of granular material of 5 to 80 mu m by first grinding a predetermined method on the surface of the member such as the thermal spraying material powder in by spraying, to form formed a porous layer made of 50~ 2000 μ ηι thick porous (porosity 5 to 2 about 0%) thermal spray coating.

The thickness of the porous layer 50 is less than mu Itaiota, performance of the coating under the corrosive environment is insufficient, whereas, if the thickness of this layer exceeds 2000 m, the mutual sintering of the sprayed particles on force is weakened, stress generated during film formation (believed to be caused by accumulation and volume shrinkage reaction by quenching of the particles) is large Do connexion, coating is easily damaged.

Such, as a method for forming a thermal spray coating formed of a porous layer, atmospheric plasma soluble archery, vacuum is plasma spraying method is preferred, can be applied depending also use conditions such as water plasma spraying method, explosion spraying method is there.

Further, the prior to the formation of the porous layer in advance on the surface of the member such as a metal. Alloy, Serra Mittasu, may be formed a under coat consisting of any of the cermet is a composite material thereof. The formation of the undercoat, the adhesion strength between the porous layer and the substrate is high, the can thus receive preventing the contact to the substrate of the corrosive gas.

The undercoat, Ni and their alloys, Co and its alloys, A1 Oyopiso alloys, Ti Oyopi its alloys, Mo Oyopi its alloys, W and their alloys, Cr and metallic alloys thereof, etc. are preferred coating, the thickness thereof is preferably about 50 to 200 / m.

The role of this undercoat, thereby improving the corrosion resistance by blocking the surface of the member and the like from the corrosive environment is to improve the adhesion between the base and the porous layer. Therefore, the thickness of the undercoat is a sufficient corrosion resistance is less than 50 mu m, not only is a uniform film is difficult, whereas, even thicker than 200 m, the effect of corrosion resistance is saturated to. The ceramic used in the undercoat, oxides Ya borides, nitrides, etc. silicides are suitable, also, these ceramic and the metal - may be a film using a cermet made of an alloy.

As a method of forming the under coat other and air plasma spraying and vacuum-flop plasma spraying method may be a spraying method, such as water Burazuma spraying method, explosion spraying method, or may be formed by vapor deposition method. Is a material of member such as a processing Chiyanpa the member of a plasma processing apparatus according to the present invention, aluminum and its alloys, titanium and its alloys, stainless steel, other special steel of that, metals such as nickel-based alloy (hereinafter other including alloy "metal"), quartz, glass products, carbides, borides, silicides, nitrides and ceramic consisting of mixtures, as a cermet consisting of these ceramics with the metal or the like inorganic materials such, can be used as the plastic. Further, on the surface of a substrate consisting of wood charge, metal plated (electric plated, melt plated, chemical plated) and those, such as those forming the metal deposition film can be used.

The most characteristic configuration in the present invention, parts are exposed directly to the plasma treatment atmosphere position is the presence of the provided relative to the surface of the member such as secondary recrystallization layer. The secondary recrystallization layer, the porous layer, i.e. porous be one that is formed on the thermal spray coating, for example III a metals oxides the porous layer uppermost layer secondary transformation consisting it is a layer formed by.

In general, metal oxide III a group element, for example Sani匕Ittoriumu: For (yttria Y 2 O 3), the crystal structure is a cubic belonging to tetragonal. The oxidation Ittoriu beam (hereinafter, referred to as "yttria") powder and plasma spraying, while being rapidly quenched while the molten particles to fly at high speed towards the substrate and sedimentary collides with the surface of the substrate Occasionally, a primary transformed into a mixed crystal of a crystal structure comprising the addition to monoclinic main crystal structure cubic (C ubic) (monoc 1 inic). This is a metal oxide porous layer. Then, the a secondary crystal layer, wherein the metal oxide has decreased and mixed crystal state including a orthorhombic crystal systems crystals were to be rapid quenching transformation by connexion primary to the time of spraying and tetragonal crystals things porous layer, is that the secondary transformation laminar crystal form of tetragonal by thermal spraying process again.

4, Y 2 0 3 sprayed coating (porous membrane), which Miku port tissue changes near the surface in the composite film having a film and the undercoat layer after the film was electron beam irradiation treatment schematically illustrating it is. Figure 4 in the non-irradiation test piece shown in (a) is present independently sprayed particles constituting the coating, respectively, it is greater roughness of the surface forces, Ru. On the other hand, the electron beam irradiation process shown in FIG. 4 (b), a new layer of different microstructure on the thermal sprayed coating was formed. This layer, the spray particles is engaged S insect mutually, but became less dense layer void. Incidentally, FIG. 4 (c) shows an example having Ann Dakoto.

Under the dense layer formed by electron beam irradiation, there is sprayed coating specific pore-rich film, the layer having excellent heat 衝搫 resistance.

5, a porous layer is Y 2 0 3 sprayed coating, an XRD measurement chart of secondary recrystallized layer formed by electron beam irradiation treatment under the following conditions. Then, 6 and 7, the Upsilon 2 0 3 sprayed coating (porous layer) shows the XRD pattern before and after electron beam irradiation treatment. That is, FIG. 6 is a X-ray diffraction Chiya one bets an enlarged vertical axis of pretreatment, FIG. 7 is an X-ray diffraction Chiya one bets an enlarged vertical axis after treatment. As can be seen from FIG. 6, the Upsilon 2 0 3 spray coating pretreatment, a peak indicating the monoclinic it is observed in the range of especially the 30 to 3 5 °, cubic and monoclinic are mixed situation is seen, contrast, as shown in FIG. 7, the Upsilon 2 0 3 the thermal spray coating was obtained by electron beam irradiation treatment secondary recrystallized layer, Upsilon 2 0 3 particles sharp peak showing the becomes, the peak of the monoclinic is attenuated, plane index (202), (310), such as is ceased confirmed, it can be seen that only cubic. Incidentally, the XRD test is measured using Rigaku Corporation RINT 1 500 X-ray diffractometer.

X-ray diffraction conditions are as follows.

Output: 40 k V

Run 查速 degree: 20 / min

4, reference numeral 41 denotes a substrate, 42 is porous layers (spray particle deposition layer) 43 is vapor hole (void) 44 particle interface, 45 through pores 46 Te cowpea electron beam irradiation treatment the resulting secondary recrystallized layer, and 47 is an undercoat. Even by the laser beam irradiation process, results of observation with an optical microscope, similar Miku port tissue changes and the electron beam irradiation surface is observed.

Thus, in the present invention, Te cowpea that mainly the porous layer of III a metals oxides ing from the crystal structure of the primary transformation was orthorhombic mainly to high-energy radiation treatment, the porous layer processed heated volume spray particles at least above the melting point, the layers were again transformed (secondary transformation), the crystal structure of the tetragonal to be crystallographically stabilized back to 袓織it was was.

At the same time, in the present invention, when the primary transformation by spraying, heat distortion and mechanical strain accumulated in the spray particle deposition layer to release a physical, chemical stabilize its properties, the accompanying Chikaratsu molten it was decided to also realize densification and smoothing of the layer. As a result, the secondary recrystallization layer made of a metal oxide of Iotapai a group element will dense and smooth layer than the layer that remains spraying.

Therefore, the secondary recrystallization layer had a porosity of less than 5%, preferably with a densified layer of less than 2%, surface 0.1 in average roughness (Ra) 8~3. 0 m, the maximum roughness is (R y) at 6~16 μιη, it becomes approximately. 3 to 14 mu m in 10-point average roughness (Rz), becomes remarkably different layers as compared with the porous layer. The control of the maximum roughness (Ry) is determined in terms of environmental pollution resistance. This is because, by plasma ions and electrons excited in etching atmosphere, the surface of the container member is scraped off, when generating particles, appeared well to the value of the maximum roughness of the impact surface (Ry) When this value is larger, because the particle generation opportunity increases. Next, a description will be given high energy irradiation method performed to form the secondary recrystallization layer. How employed in the present invention, an electron beam irradiation treatment, the laser irradiation process, such as C0 2 laser and YAG laser is preferably used, but the invention is not limited to these methods.

(1) electron beam irradiation treatment: The conditions of this process, the irradiation chamber was evacuated of air, and introducing an inert gas such as A r gas, for example, it is processed by the irradiation conditions as shown below recommended.

Irradiation atmosphere: O~0.0005Pa (Ar gas)

Beam radiation output: 0. l~8kW

Processing speed: l~30mm / s

Of course, these conditions are not intended to be limited to the above range is an illustration of a suitable conditions for obtaining a suitable secondary recrystallization layer, as long as the desired effects of the present invention is obtained, It is not limited only to these conditions.

Metal oxides including electron beam irradiation treated Ilia group elements, the molten state reaches above the melting point and eventually the temperature from the surface above the temperature to. The melting behavior, or by increasing the electron beam irradiation power, or to increase the number of times of irradiation, and because we extends to the film inside gradually by the child long irradiation time, the depth of the irradiation melt layer, these by varying the irradiation conditions can be controlled. Practically the secondary recrystallized layer meet the above objects of the present invention if there is penetration ilr depth of 1 / Γη~50μηι. The (2) laser beams, YAG laser also utilizing YAG crystal, when medium quality is gas, it is possible to use the C_〇 2 gas laser or the like. The irradiation process of the lasers one beam, the following conditions are recommended.

Laser output: 0. l~10kW

Les Zabimu area: 0.01 to 2500瞧2

Processing speed: 5-1000 瞧 / s

Said electron beam irradiation treatment and laser beam irradiation processed layers is directed to that described above, and hot transformation precipitated secondary recrystallization upon cooling, the changes to the physicochemically stable crystalline form, of the film reforming proceeds at a unit of the crystal level. For example, in the gamma 2 o 3 film formed by atmospheric plasma spraying method, as described above, while in the spraying state orthorhombic mainly varies almost cubic after electron beam irradiation. Hereinafter, it summarizes the characteristics of the secondary recrystallized layer of a metal oxide of high energy radiation treated Periodic Table Ilia group elements.

a. the secondary recrystallized layer to generate is high energy radiation treatment, as was further secondary transform the porous layer composed of a metal oxide such as a primary transformation layer under, or oxide particles of the lower layer it forces et al., which is heated above the melting point, at least a portion of the pores are densified to disappearance.

b. secondary recrystallized layer to generate is high energy radiation treatment, particularly when a layer obtained by a porous layer comprising a lower layer of metallic oxides is further secondary transformation, formed particularly it by spraying method when the thermal spray coating was unmelted particles during spraying it is also completely melted, and because the surface becomes a mirror surface state, so that the easily projections plasma etched is extinguished.

c the a, the effect of b, the porous layer, for secondary recrystallization layer to generate Te cowpea high energy irradiation treatment, through pores are blocked, the internal (group through these through pores eliminates the corrosive gas from entering the wood), as well as improved corrosion resistance, exhibits strong resistance against plasma etching action to have 緻 densification, excellent corrosion resistance and resistance to plasma erosion resistance over extended periods exhibit.

d. the secondary recrystallization layer are the physical I human studies stable crystal modification can be achieved in the crystal level. Moreover, at this time, the heat distortion introduced during spraying also becomes stable layer is released simultaneously. e. the thickness of the secondary crystal layer produced by high-energy irradiation treatment, it is preferable that the thickness of about 1 ~50 μ ιη from the surface. The reason is that there is no effect of the film formation is less than, on the other hand, if thicker than 50 m, together with the burden of high energy irradiation treatment is greatly, because the effect of the deposition is saturated.

Note that the lower layer of the porous layer is present as a layer having excellent heat 衝墜 resistance, the layer is characterized responsible for buffering action between an upper layer. That is, through the function of relaxing the thermal shock that Kuwawa dense electrolyte secondary crystal layer of the upper layer, is effective to alleviate the thermal shock applied to the entire film. In this sense, has a porous layer made of the thermal spray coating in the lower layer, when the composite film to the upper layer of laminated secondary recrystallized layer, by connexion synergistically combined action of these two layers effects the durability of the coating is improved occur.

Further, as described above, when the etching at high plasma power, the potential difference between the members and the like and Burazuma in the chamber is increased, spray coating or the like the gamma 2 o 3 which covering the like member is corroded, by it connexion particle mosquito resulting corrosion products falling onto the surface of the object to be processed, leading to device failure by deposition. However, in the plasma processing apparatus of the present invention, by erosion of the coating formed on the surface of the member or the like is on improvement, if the plasma power, the potential difference between the members and the like and the plasma is increased until about 550V in also becomes can thus receive possible to suppress the generation of particles. Incidentally, the potential difference between the members and the like and Burazuma is controlled by the power applied from the high frequency power supply 7 of FIG. 1 in 载置 table 5, preferably 550V or less, and more preferably less 550V or 120V. Example

(Example 1)

On the front surface of the chamber inner wall member (aluminum baffle) of the plasma processing apparatus shown in FIG. 1, Υ 2 0 3 (or more purity 95 mass%) Examples of III a metals oxides that sprayed with film-forming (Comparative and example B), Υ 2 0 3 'After sprayed with film forming, its surface is secondary transformation by irradiating an electron beam to form the shape as a (Inventive Alpha) with secondary crystal layer. The respective chambers in one, plasma treatment is introduced repeatedly to F-containing gas and containing CH gases alternately, after weakening the Upsilon 2 0 3 sprayed coating is to be bra Zuma processed semiconductor by controlling the application amount of the high-frequency power to the mounting table of the wafer, by changing the potential difference between the chamber first wall potential and the plasma to 200V~300V, generation of dust (particles) onto the semiconductor wafer at each potential It was measured. The results are shown in Figure 2.

As a result, in Comparative Example B, other semiconductor wafers due to dust with increasing potential difference, while the film (Ittoriumu) caused dust occurs, in invention sample A, although the semiconductor wafer due to dust was observed , coating component (Itsutoriumu) the generation of resulting in the Particle is not observed at all, it did not occur little force.

(Example 2)

The plasma processing chamber inner wall member (aluminum lower in Shiyu regulator, baffles, deposition shield) and to investigate the limit value of the potential difference between the plasma (film (Itsutoriumu) range generation can be suppressed in due dust), Example 1 similar to the surface of the processing container inner wall material, Y 2 0 3 that sprayed with film forming (Comparative example beta), After film formation by spraying the Upsilon 23, further the surface and electron beam irradiation treatment is secondary transformation was prepared that form the secondary crystal layer (invention examples Alpha). Each of the processing container, plasma treatment by repeatedly introducing a F-containing gas and containing CH gases alternately, after weakening the Upsilon 2 0 3 coating, to control the application amount of the high-frequency power to the lower electrode in particular by changing the potential difference between the members and the like and Burazuma Te cowpea were measured amount of generated Dust onto the semiconductor wafer at each potential. The results are shown in Figure 3.

As a result, in Comparative Example beta, with an increase of the potential difference, while the yttrium due dust proportion is 增加 thereto, the invention example Alpha, we have found no occurrence of Itto helium due dust even at the time of 550V . Thus, the plasma treatment equipment of the present invention, even in case of increasing to a maximum 550V potential difference, generation of dust Itsutoriumu attributable was divide that it is possible to suppress. Available 个生 on the industry

Technique of the present invention, members used in a general semiconductor processing equipment, parts and the like as well as used as a surface processing technique for a plasma processing apparatus members more precise and sophisticated processing of these days is required. In particular, the present invention is the deposition shield for a semiconductor processing apparatus for plasma processing in a severe atmosphere such as to use the F-containing gas and containing CH gas alternately and repeatedly device or these gases for use in, respectively alone, baffle plate is suitable focus ring upper 'Roi one insulator, sealing Doringu, bellows cover, electrode, members such as the solid derivatives, as a surface treatment technology to parts. Further, the present invention can be applied as a surface treatment technology of the liquid crystal device manufacturing apparatus member.

Claims

The scope of the claims
1. The surface of the object accommodated in the chamber in one, in the plasma processing apparatus to by connexion processed into etching gas plasma,
Site exposed to the plasma generation atmosphere of the chamber one, this chamber one within mounting member or the surface of the component, at least, the metal oxide formed on the porous layer and its porous layer of a metal oxide the plasma processing apparatus characterized by being covered by a secondary recrystallized layer of the object.
2. Wherein the lower porous layer, a metal. Alloy, plasma processing apparatus according to claim 1, wherein, characterized in that it comprises an undercoat layer made of ceramic or cermet.
3. The etching process, treatment with a fluorine-containing gas plasma and processes repeatedly alternately introduced mixed gas plasma by treatment, or a fluorine-containing gas and a hydrocarbon-containing gas of the fluorine-containing gas and hydrocarbon-containing gas the plasma processing apparatus according to claim 1, wherein to feature that either.
4. The fluorine-containing gas, C x F y gas, CHF-based gas, HF-based gas one or more gases der Rukoto selected from among a mixed gas of ¾ and SF-based gas and these gases the plasma processing apparatus according to claim 3, wherein, wherein.
5. The hydrocarbon-containing gas, according to which is a C x H y gas, one or more gases selected from among H containing gas and C x H y gas and mixed gas of 0 2 Burazuma processing apparatus according to claim 3.
6. The metal oxide plasma processing device according to claim 1, billed, which is a metal oxide containing III a group element.
7. The secondary recrystallized layer, metal oxide primary transformation contained in the porous layer by high energy irradiation treatment, to claim 1, wherein, characterized in that one which is formed by the secondary transformation the plasma processing apparatus according.
8. The secondary recrystallized layer, and wherein the porous layer including crystals of the orthorhombic system is tissue Natsuta layer of tetragonal and by connexion secondary transformation to high-energy radiation treatment the plasma processing apparatus according to claim 1, wherein the.
9. The high energy irradiation treatment, plasma processing apparatus according to claim 7 claims, characterized in that an electron beam irradiation treatment or laser beam irradiation process.
1 0. The high-energy irradiation treatment, plasma processing apparatus according to claim 8 claims, characterized in that an electron beam irradiation treatment or laser beam irradiation elevation process.
1 1. site to be 嗨 to a plasma atmosphere of the chamber one, the said a member or component of a surface plasma, plasma treatment according to claim 1 請 nucleophilic, characterized in that it comprises the following potential difference 120 V or 550V apparatus.
1 2. The potential difference, plasma treatment according to claim 1 1, wherein wherein the and is controlled by the high-frequency power applied to the mounting table of the workpiece provided in the chamber in one apparatus.
1 3. the surface of the object accommodated in the chamber in one, in the plasma processing method for a result processed into etching gas plasma, prior to this process, a portion is first exposed to a plasma atmosphere of the Chang bar, in this Chiyanba distribution the portion material or the surface of the component, a composite layer formed by coating including a porous layer made of a metal oxide and a secondary recrystallized layer of the metal oxide formed on the porous layer, then, the plasma processing method introducing a first gas containing fluorine-containing gas into the Chiyanba, characterized in that for processing the gas to generate a first bra Zuma by exciting a.
14. The fluorine-containing gas, it is C x F y gas, CHF-based gas, HF-based gas, SF-based gas and at least one gas selected from among a mixed gas containing 〇 2 and these gases the plasma processing method according to claim 1 3 claims, wherein.
1 5. The metal oxide plasma processing method according to claim 1 3 claims, characterized in that a metal oxide containing III a group element.
1 6. The secondary recrystallized layer by Koko energy irradiation of the primary transformation metal oxide contained in the porous layer, the claims characterized in that which is formed by the secondary transformation the plasma processing method according to 1 3.
1 7. The secondary recrystallized layer, and wherein the porous layer including crystals of the orthorhombic a layer became tissue tetragonal and by connexion secondary transformation to high-energy radiation treatment the plasma processing method according to claim 1 3 billed for.
1 8. The high-energy irradiation treatment, plasma treatment method according to claim 1 6 claims, characterized in that the electron beam irradiation treatment or laser beam irradiation.
1 9. The high-energy irradiation treatment, plasma treatment method according to claim 1 7 claims, characterized in that the electron beam irradiation treatment or laser beam irradiation.
2 0. Of the chamber in one, sites exposed to a plasma atmosphere, and is the a member or component of a surface Burazuma, in the range 1 3 claims you characterized by the following potential difference 120 V or 550 V plasma processing method described.
2 1. The potential difference, plasma processing method according to claim 2 0 claims, characterized in that the control by the high-frequency power applied to the mounting table of the workpiece provided in the chamber in one.
2 2. The surface of the object accommodated in the chamber in one, in the plasma processing method of processing by plasma etching process gas, prior to this process, the first said Chiya members, sites exposed to a plasma atmosphere, this chamber one on the surface of the inner mounting member or part products, the composite layer formed by coating including a porous layer made of a metal oxide and a secondary recrystallized layer of the metal oxide formed on the porous layer, Thereafter, the chamber in one to generate a first plasma by exciting After introducing the first gas containing fluorine-containing gas and then, guiding the second gas containing a hydrocarbon gas into the chamber in one flop plasma processing method characterized in that processing by generating a second plasma by exciting After entering.
2 3. The fluorine-containing gas, C x F y gas, CHF-based gas, HF-based gas, SF-based Gas Yopi one or more gases selected from among the mixed gas containing the these gases 0 2 the plasma processing method according to claim 2 2 claims, characterized in that it.
2 4. Gas containing the hydrocarbon, and characterized by a C x H y gas, one or more gases selected from among a mixed gas of H-containing gas and C x H y gas and O 2 the plasma processing method according to claim 2 2 claims to be.
2 5. The metal oxide plasma processing method according to claim 2 2 claims, characterized in that a metal oxide containing III a group element.
2 6. The secondary recrystallized layer, claims by Koko energy irradiation of the primary transformation metal oxide contained in the porous layer, characterized in that which is formed by the secondary transformation the plasma processing method according to 2 2.
2 7. The secondary recrystallized layer, and wherein the porous layer including crystals of the orthorhombic a layer became tissue tetragonal and by connexion secondary transformation to high-energy radiation treatment Burazuma processing method according to claim 2 2 billed for.
2 8. The high energy irradiation treatment, plasma treatment method according to claim 2 6 claims, characterized in that the electron beam irradiation treatment or laser beam irradiation.
2 9. The high energy irradiation treatment, plasma treatment method according to claim 2 7 claims, characterized in that the electron beam irradiation treatment or laser beam irradiation.
3 0. of the chamber in one, sites exposed to a plasma atmosphere, and said a member or component of a surface plasma, in the range 2 2 according you characterized by the following potential difference 120 V or 550 V plasma processing method described.
3 1. The potential difference, plasma processing method according to claim 3 0 of claims and controlling the high frequency power applied to the mounting table of the workpiece provided in the chamber in one.
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