CN100508116C - Plasma treating apparatus and plasma treating method - Google Patents

Plasma treating apparatus and plasma treating method Download PDF

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CN100508116C
CN100508116C CNB2007101006931A CN200710100693A CN100508116C CN 100508116 C CN100508116 C CN 100508116C CN B2007101006931 A CNB2007101006931 A CN B2007101006931A CN 200710100693 A CN200710100693 A CN 200710100693A CN 100508116 C CN100508116 C CN 100508116C
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gas
plasma
plasma processing
chamber
metal oxide
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CN101042996A (en
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小林义之
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Tokyo Electron Ltd
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Tokyo Electron Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18—After-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/3065—Plasma etching; Reactive-ion etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating 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
    • C23C28/04—Coating 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
    • C23C28/042—Coating 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11—Oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32458—Vessel
    • H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
    • H01J37/32495—Means for protecting the vessel against plasma

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

Plasma processing apparatus and method of plasma processing
Technical field
The present invention relates to be used for the plasma processing apparatus and the method for plasma processing in semiconductor processing technology field.Be particularly related under the environment that constitutes by the atmosphere of halogen gas, inactive gas, oxygen or hydrogen etc., the atmosphere etc. of gas (hereinafter referred to as " containing F gas ") and hydrocarbon system gas (hereinafter referred to as " containing CH gas ") that contains fluorine and fluorine compounds, perhaps form under the environment of these atmosphere alternately repeating, be used for semiconductor element etc. is carried out the plasma processing apparatus and the method for plasma processing of plasma etching processing etc.
Background technology
The device that is used for semiconductor and field of liquid crystals is adding man-hour, and utilizing the high halogen of corrosivity mostly is the energy of plasma of etchant gas.For example, in plasma etch process (processing) device as one of semiconductor processing, in the mixed-gas atmosphere of the strong gas atmosphere of the corrosivity of chlorine system or fluorine system or these gas and inactive gas, produce plasma, by utilizing the ion that excites this moment and the strong reactivity of electronics, semiconductor element is carried out etching and processing.
Under the situation of this process technology, the corrosiveness that the member of at least a portion of reaction vessel wall or portion's setting within it or parts class (pedestal, electrostatic chuck, electrode etc.) are subjected to energy of plasma easily, therefore, it is very important using the material of anti-plasma corrosivity excellence.For such requirement, all be to use the metal (comprising alloy) of good corrosion resistance and inorganic material such as quartz, aluminium oxide etc. in the past.For example, open in the flat 10-4083 communique the spy and to disclose following technology: utilize PVD method or CVD method on the surface of above-mentioned reaction vessel interior part, to cover these materials, and form the dense film that constitutes by the oxide of the IIIB family element in the periodic table of elements etc., perhaps cover Y 2O 3Monocrystalline.In addition, open in 2001-164354 communique and the Te Kai 2003-264169 communique the spy and disclose following technology: utilize the metallikon will be as the Y of the oxide of the element of the IIIB family that belongs to the periodic table of elements 2O 3Cover on the parts surface, improve anti-plasma corrosivity thus.
; cover periodic table of elements IIIB family element metal oxide etc. open disclosed technology in the flat 10-4083 communique the spy; though demonstrate better anti-plasma corrosivity; but in harsh more aggressive atmosphere gas, require in the semiconductor processing technology field in recent years of high-precision processing and clean environment degree, in fact be not sufficient countermeasure.
In addition, open disclosed in 2001-164354 communique and the Te Kai 2003-264169 communique, covering Y the spy 2O 3The parts of sputtered films of bismuth, improve the corrosive effect of anti-plasma though played, but, the processing of nearest semiconductor device, except the plasma etching effect of higher output, also be in processing atmosphere and alternately reuse under the exacting terms that the strong fluorine of corrosivity is gas and hydrocarbon system gas, still require further to improve.
Especially, contain F gas and contain under the situation of CH gas alternately reusing, in containing the F gas atmosphere, utilize the distinctive deep-etching reaction of halogen gas, generate the high fluoride of vapour pressure, on the other hand, containing under the CH gas atmosphere, the decomposition of the fluorine compounds that generate in containing F gas obtains promoting that the part of film component becomes carbide, has the effect that the reaction of materialization is fluoridized in further raising.And under plasma environment, these reactions obtain promoting, therefore become very harsh corrosive environment.Especially, carrying out under the etched situation with high plasma output, it is big that the potential difference of the inwall of plasma and container for plasma treatment (chamber) becomes, and covers the Y on the internal face 2O 3Sputtered films of bismuth can be corroded.Therefore, the particle of the corrosivity product that generates under such environment can fall and integrated circuit surface attached to semiconductor article on, this just becomes the reason of device damage.
Summary of the invention
The objective of the invention is to improve the durability that is used for carrying out the position that is exposed to plasma atmosphere, member and the parts (below, only be called " parts etc. " simply) of the chamber of plasma etching processing itself in corrosive gas atmosphere.
Another object of the present invention is to improve the anti-plasma corrosivity of the film that forms in corrosive gas atmosphere, on the surface of parts etc.
Even another purpose of the present invention is to provide a kind of method of plasma processing that also can prevent to produce the particle of corrosion product under high plasma output.
Means as realizing above-mentioned purpose the invention provides a kind of plasma processing apparatus, and it comprises accommodates the chamber that utilizes the handled object that the etch processes gaseous plasma processes; With being exposed to position that plasma generates atmosphere, being arranged on member or parts in this chamber of this chamber itself, on surface more than in above-mentioned position, above-mentioned member or above-mentioned parts any, be provided with composite bed, this composite bed comprises the secondary recrystallization layer of porous layer that is made of metal oxide and this metal oxide that forms on this porous layer.
Plasma processing apparatus of the present invention can adopt following structure.
1. below above-mentioned porous layer, the priming coat (undercoat) that is made of metal, alloy, pottery or cermet is set.
2. the processing that above-mentioned etch processes is carried out with the processing that utilizes the fluoro-gas plasma to carry out, the mixed gas plasma that utilizes fluoro-gas and gas containing hydrocarbon or alternately repeat imports fluoro-gas and gas containing hydrocarbon and any mode in the processing carried out is carried out.
3. above-mentioned fluoro-gas uses and is selected from CF 4, C 4F 8Deng C xF yGas, CHF are that gas, HF are that gas, SF are gas and these gas and O 2Mist in the gas more than a kind.
4. above-mentioned gas containing hydrocarbon uses and is selected from CH 4, C 2H 2Deng C xH yGas, NH 3Deng containing H gas and CH 4With O 2, CH 3F and O 2, CH 2F 2With O 2Deng C xH yGas and O 2Mist in the gas more than a kind.
5. above-mentioned metal oxide is the metal oxide that contains IIIB family elements such as Sc, Y and lanthanide series.
6. above-mentioned secondary recrystallization layer forms its secondary metamorphosis by the once abnormal metal oxide that contains in the porous layer being carried out the high energy radiation processing.
7. above-mentioned secondary recrystallization layer for the porous layer that contains the orthorhombic system crystallization by high energy radiation handle, secondary abnormal become behind the tetragonal system tissue layer.
8. above-mentioned high energy radiation is treated to the electron beam treatment with irradiation or laser beam irradiation is handled.
9. making the surface and the potential difference between the above-mentioned plasma of the position that is exposed to plasma atmosphere, member or the parts of above-mentioned chamber is below the above 550V of 120V.
10. the High frequency power that the mounting table of above-mentioned potential difference by the handled object in being arranged on above-mentioned chamber applies is controlled.
In addition, the invention provides a kind of method of plasma processing, it is a plasma treatment of utilizing the plasma of etch processes gas that the surface that is housed in the handled object in the chamber is processed, comprise: at first, at the position that is exposed to plasma atmosphere of described chamber itself, be arranged on the surface of member in this chamber or parts, cover the operation that forms composite bed in advance, this composite bed comprises the secondary recrystallization layer of porous layer that is made of metal oxide and the above-mentioned metal oxide that forms on this porous layer; With in this chamber, import first gas comprise fluoro-gas, this gas is excited, produce first plasma, the operation of handling.
In addition, the present invention also provides a kind of method of plasma processing, it is a plasma treatment of utilizing the plasma of etch processes gas that the surface that is housed in the handled object in the chamber is processed, comprise: at first, at the position that is exposed to plasma atmosphere of above-mentioned chamber itself, be arranged on the surface of member in this chamber or parts, cover the operation that forms composite bed in advance, this composite bed comprises the secondary recrystallization layer of porous layer that is made of metal oxide and the above-mentioned metal oxide that forms on this porous layer; After importing comprises first gas of fluoro-gas in this chamber, it is excited, produce the operation of first plasma; With, then, after importing comprises second gas of appropriate hydrocarbon gas in this chamber, it is excited, produce second plasma, the operation of handling.
In addition, above-mentioned method of plasma processing of the present invention can adopt following structure.
1. above-mentioned fluoro-gas uses and is selected from CF 4, C 4F 8Deng C xF yGas, CHF are that gas, HF are that gas, SF are gas and these gas and O 2Mist in the gas more than a kind.
2. above-mentioned gas containing hydrocarbon uses and is selected from CF 4, C 2H 2Deng C xH yGas, NH 3Deng containing H gas and CH 4With O 2, CH 3F and O 2, CH 2F 2With O 2Deng C xH yGas and O 2Mist in the gas more than a kind.
3. above-mentioned metal oxide is the metal oxide that contains IIIB family elements such as Sc, Y and lanthanide series.
4. above-mentioned secondary recrystallization layer forms its secondary metamorphosis by the once abnormal metal oxide that contains in the porous layer being carried out the high energy radiation processing.
5. above-mentioned secondary recrystallization layer for the porous layer that contains the orthorhombic system crystallization by high energy radiation handle, secondary abnormal become behind the tetragonal system tissue layer.
6. above-mentioned high energy radiation is treated to the electron beam treatment with irradiation or laser beam irradiation is handled.
7. making the surface and the potential difference between the above-mentioned plasma of the position that is exposed to plasma atmosphere, member or the parts of above-mentioned chamber is below the above 550V of 120V.
8. the High frequency power that the mounting table of above-mentioned potential difference by the handled object in being arranged on above-mentioned chamber applies is controlled.
The present invention according to said structure, in that being carried out plasma etching, semiconductor device or Liquid crystal component add man-hour, for at plasma atmosphere, particularly contain under the F gas atmosphere or alternately repeat to form the plasma etching of the parts that contain in F gas atmosphere and the chamber that contains under the etchant gas atmosphere such as the such halogen of CH gas atmosphere etc., can make it have durability for a long time.
In addition, according to the present invention, the particle of the corrosion product that produces owing to the potential difference between parts in plasma etch process or the chamber etc. and the plasma etc. obviously reduces, and can produce high-quality semiconductor device etc. expeditiously.
In addition, according to the present invention, because on the surface of parts etc., form unique film, so the output of plasma can be brought up to about 550V, can obtain etching speed and etch effect and improve, and then can realize the light-weighted effect of miniaturization of plasma processing apparatus.
Description of drawings
Fig. 1 is the figure of schematic configuration of the plasma processing apparatus of expression an embodiment of the invention.
Fig. 2 be the current potential of expression treatment chamber inner part etc. with by Y 2O 3The figure of the relation between the dust that causes (dust) (particle) generation.
Fig. 3 be the current potential of expression treatment chamber inner part etc. with by Y 2O 3The figure of the relation between the dust that causes (particle) generation.
Fig. 4 is sectional view (a) with film that the method for the prior art utilized forms, utilize the inventive method to form the secondary recrystallization layer on outermost layer and the partial section of the parts (b) that form and parts (c) with priming coat.
Fig. 5 is Y 2O 3Sputtered films of bismuth (porous layer) and utilize the X-ray diffractogram of the secondary recrystallization layer that the electron beam treatment with irradiation forms.
Fig. 6 is Y 2O 3The X-ray diffractogram of the state before the electron beam treatment with irradiation of sputtered films of bismuth (porous layer).
Fig. 7 is Y 2O 3The X-ray diffractogram of the state after the electron beam treatment with irradiation of sputtered films of bismuth (porous layer).
Embodiment
Below, with reference to accompanying drawing, describe an example of embodiments of the present invention in detail.Fig. 1 is the sectional view of a part of using the chamber of plasma processing apparatus of the present invention.In addition, plasma processing apparatus of the present invention is not only limited to structure shown in Figure 1.
In Fig. 1, the chamber that symbol 1 expression etch processes is used.This chamber 1 for example for having the cylindric chamber of aluminum of anodic oxidation overlay film (pellumina processing) from the teeth outwards, has the structure that can keep etch process chamber airtightly.
Inside at this chamber 1 is provided with: lower electrode 2; Be used to utilize the Coulomb force keep handled object such as semiconductor wafer W, be configured in this lower electrode 2 top on electrostatic chuck 3; With above this electrostatic chuck 3, separate the upper electrode 4 of predetermined distance configuration etc.In addition, above-mentioned electrostatic chuck 3 for example has be provided with the structure of electrostatic chuck with electrode between the dielectric film that is made of polyimide resin etc., and above-mentioned upper electrode lower electrode 2,4 is preferably respectively by forming with chamber 1 identical materials.
And bottom high frequency electric source (RF power supply) 7 is connected with the mounting table 5 that is made of lower electrode 2 and electrostatic chuck 3 by bottom adaptation 6, supplies with the High frequency power of assigned frequency from this bottom high frequency electric source 7.In addition, top high frequency electric source (RF power supply) 9 is connected with upper electrode 4 by top adaptation 8.
In addition, in upper electrode 4, be provided with a plurality of gas squit holes 10 in its lower section, on the other hand,, be provided with gas supply part 11 at its top.
In addition, although not shown among Fig. 1, exhaust apparatus is connected with chamber 1 by pipe arrangement, utilizes this exhaust apparatus to be adjusted into for example interior pressure about 1.33Pa～133Pa in this chamber 1.Then, in this chamber 1, import the plasma processing gas of stipulating from above-mentioned gas introduction part 11, for example by containing the etching gas that F gas constitutes.
Then, under this state, supplying with lower regulation High frequency power, for example frequency of frequency from bottom high frequency electric source 7 is the High frequency power below several MHz, and supplying with higher regulation High frequency power, for example frequency of frequency from top high frequency electric source 9 is the High frequency power of tens MHz～100 MHz, thus, can between upper electrode 4 and lower electrode 2, produce plasma, and utilize double handled object surface such as wafer conductor W of this plasma to carry out etching and processing.In addition, the High frequency power of supplying with to upper electrode 4 from top high frequency electric source 9 is used to produce plasma, on the other hand, the High frequency power of supplying with to mounting table 5 from bottom high frequency electric source 7 is used to produce the DC bias voltage, with the energy of ions of control with the semiconductor wafer W collision.
In addition, in treatment chamber 1, as shown in Figure 1, the mounting table 5 that constitutes except above-mentioned upper electrode 4, by lower electrode 2 or electrostatic chuck 3, also be provided with parts such as shading ring (shieldring) 12, focusing ring 13, deposit shield 14, top insulator (upper insulator) 15, lower isolator (lower insulator) 16 and baffle plate 17 etc.
Shading ring 12 and focusing ring 13 for example are the parts of the roughly ring-type that formed by carborundum or silicon, mode with the periphery of surrounding upper electrode 4 and lower electrode 2 disposes respectively, and the plasma that will produce between upper electrode 4 and lower electrode 2 converges on the semiconductor wafer W.
In addition; deposit shield 14 is provided with for the inwall of protecting chamber 1; top insulator 15 and lower isolator 16 are provided with in order to keep the atmosphere in the chamber 1; baffle plate 17 below this lower isolator 16 is set; be plasma sealing, it can not flowed out from the exhaust outlet 18 that is positioned at the plasma processing apparatus below in order to produce.
These are configured in parts in the chamber 1 etc., add man-hour carrying out plasma etching, are exposed to the above-mentioned F of containing gas atmosphere or alternately repeat to import to contain F gas and contain plasma exciatiaon atmosphere under such strong corrosive environment of CH gas.
Usually, the above-mentioned F of containing gas atmosphere mainly contains fluorine, fluorine compounds, perhaps also contains aerobic (O sometimes 2).Fluorine has following feature: be imbued with reactivity (corrosivity is strong) especially in halogens, do not say metal, also can react with oxide or carbide and generate the high corrosion product of vapour pressure.Therefore; if the parts in the above-mentioned chamber 1 etc. are exposed to the plasma under the severe corrosive atmosphere such as the above-mentioned F of containing gas atmosphere, then do not say metal, even oxide or carbide; also can not generate from the teeth outwards and be used to suppress the diaphragm that corrosion reaction is carried out, corrosion reaction is unrestrictedly carried out.This point, according to inventor's understanding as can be known, even in such environment, belong to periodic table of elements IIIB family element, be the element of Sc, Y, atom sequence number 57～71 and their oxide, also demonstrate good anti-corrosion.
On the other hand, contain in the CH gas atmosphere above-mentioned, this CH itself does not have severe corrosive, constitute and the antipodal reduction reaction atmosphere of oxidation reaction of in containing the F gas atmosphere, carrying out, therefore, in containing F gas, show the metal (alloy) or the metallic compound of more stable corrosion resistance, when after this when containing the CH gas atmosphere and contact, the trend that also has chemical bond power to die down.Thereby, when with contain part that CH gas contacts and be exposed to once more when containing the F gas atmosphere, initial stable compound film is chemically destroyed, and finally causes corrosion reaction to continue the phenomenon of development.
Especially, except the kind change of atmosphere gas, in the environment of plasma generation, the equal ionization of F, CH, produce F, C, the H of hyperergic atom shape, therefore, corrosivity and reproducibility are accelerated, the plasma etching effect is stronger, and easily the surface from parts etc. generates corrosion product.
The corrosion product of Sheng Chenging vaporize in this environment like this, and, form fine particle, the inside of the container for plasma treatment of chamber etc. is polluted significantly.
This point, in the method for utilizing plasma processing apparatus of the present invention to handle, as at the above-mentioned F of containing gas atmosphere, to contain F gas be effectively with containing the mixed atmosphere of CH gas or alternately repeating to contain the F gas atmosphere with containing etch-proof countermeasure under the such harsh corrosive environment of CH gas atmosphere, in the generation that stops corrosion product, particularly to suppress aspect the generation of particle be effective.
Therefore, in the present invention, for the surface that is configured in above-mentioned parts of in the chamber, when handled object is carried out plasma treatment, being exposed to this plasma simultaneously etc., composite membrane is set, this composite membrane comprises the porous layer that is made of the metal oxide that contains the element that belongs to IIIB family and make the abnormal and secondary recrystallization layer that obtains of this metal oxide secondary on this porous layer, suppresses the corrosion reaction of above-mentioned parts etc. thus.This composite membrane can form on parts in all chambers etc., can certainly only select plasma density height, the big part of damage especially and forms.
In addition, as the above-mentioned F gas that contains, the preferred use is selected from F 2, CF 4, C 4F 8, C 4F 6And C 5F 8Deng by general formula C xF yGas, the CHF of expression 3, CH 2F 2And CH 3CHF such as F are that gas, HF are gas, SF 6Deng SF is gas and by CF 2The fluorine gas and the O of the expression of CFO such as O system 2Mist in the gas more than a kind.
In addition, as the above-mentioned CH gas that contains, the preferred use is selected from H 2, CH 4, C 2H 2, CH 3F, CH 2F 2, CHF 3Deng C xH yGas, NH 3Deng containing H gas and the above-mentioned CH of containing gas or containing H gas and O 2Mist in the gas more than a kind.
Then, the inventor has studied the above-mentioned composite membrane that forms on the surface of parts in being configured in above-mentioned chamber etc. and has formed and use material, is particularly containing F gas, is containing the material that shows good anti-corrosion, anti-environmental pollution in the atmosphere of CH gas.
The result shows, as the metal oxide that is used to form above-mentioned porous layer, the metal oxide of element that belongs to the IIIB family of the periodic table of elements is compared with other oxide, shows excellent halogen resistant corrosivity, anti-plasma corrosivity (stain resistance of the particle of corrosion product) in corrosive atmosphere.In addition, the metal oxide of IIIB family element is the oxide of the lanthanide series (La, Ce, Pr, Nb, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) of Sc, Y and atom sequence number 57～71, especially, for lanthanide series, be preferably the rare-earth oxide of La, Ce, Eu, Dy, Yb.In the present invention, these metal oxides can use or use mixture more than 2 kinds, composite oxides, eutectic thing etc. separately.
In the present invention, as the method that on the surface of above-mentioned parts etc., covers the porous layer that constitutes by above-mentioned metal oxide that forms specific thickness,, use metallikon as preferred example.Therefore, when spraying plating is handled, at first the powder body that the metal oxide of IIIB family element is become by average grain diameter 5～80 μ m by pulverizing constitutes the depositing materials powder, the method of utilizing regulation on the surface of parts etc., forms the porous layer that the sputtered films of bismuth by the thick porous matter of 50～2000 μ m (porosity is about 5～20%) constitutes with this depositing materials powder spraying plating.
When the thickness of this porous layer during less than 50 μ m, the performance as film under above-mentioned corrosive environment is insufficient, on the other hand, when the thickness of this layer during greater than 2000 μ m, not only the power of mutually combining of spraying plating particle dies down, and the stress that produces during film forming (thinking that reason is the contractile response of the volume that causes of the chilling because of particle and gathers) becomes big, and film is damaged easily.
As the method that forms the sputtered films of bismuth that is made of this porous layer, preferred atmosphere plasma spraying method, decompression plasma spraying method can also be answered water plasma spraying method or blast metallikon etc. according to service condition.
In addition, also can be before forming above-mentioned porous layer, on the surface of parts etc., form in advance by metal, alloy, pottery with as any priming coat that constitutes in their cermet of composite material.By forming this priming coat, the adherence strength of porous layer and base material improves, and can stop corrosive gas to contact with base material.
Above-mentioned priming coat is preferably Ni and metallic films such as alloy, Co and alloy thereof, Al and alloy thereof, Ti and alloy thereof, Mo and alloy thereof, W and alloy thereof, Cr and alloy thereof thereof, and its thickness is preferably about 50～200 μ m.
The effect of this priming coat is to make the surface of parts etc. and above-mentioned corrosive atmosphere to cut off to improve corrosion resistance and to improve the adherence of base material and porous layer.Thereby when the thickness of this priming coat during less than 50um, not only corrosion resistance is insufficient, and is difficult to even film forming, and on the other hand, when its thickness surpassed 200 μ m, the effect of corrosion resistance was saturated.As the pottery that is used for this priming coat, preferred oxides, boride, nitride, silicide etc. in addition, also can be to use the cermet that is made of these potteries and above-mentioned metal, alloy and the film that forms.
As the formation method of this priming coat, except atmosphere plasma metallikon and decompression plasma spraying method etc., can also make metallikons such as water plasma spraying method or blast metallikon, in addition, also can utilize formation such as vapour deposition method.
Material as parts in the treatment chamber of plasma processing apparatus of the present invention etc., except metals such as aluminium and alloy, titanium and alloy thereof, stainless steel, other special steels, nickel-base alloy (below comprise alloy, all be called " metal ") in addition, can also use: the pottery that constitutes by quartz, vitrification, carbide, boride, silicide, nitride and their mixture; The such inorganic material of cermet that constitutes by these potteries and above-mentioned metal etc.; Plastics etc.In addition, can also use surperficial enterprising row metal coating (plating, fusion plating, chemical plating) and the material that forms, the material that is formed with the metal evaporation film etc. at the base material that constitutes by these materials.
In the present invention, the structure of tool feature is to have the above-mentioned secondary recrystallization layer that is provided with respect to the surface that directly is exposed to position in the plasma treatment atmosphere, parts etc.This secondary recrystallization layer at above-mentioned porous layer, be to form on the porous matter sputtered films of bismuth, for example be make the top layer part secondary of the above-mentioned porous layer that constitutes by the IIIB family metal oxide abnormal and forms layer.
Usually, at metal oxide, for example yittrium oxide (Y of IIIB family element 2O 3) situation under, crystalline texture is cube crystalline substance that belongs to regular crystal.When the powder to this yittrium oxide carries out plasma spraying, the particle of fusion is when being piled up with the substrate surface collision on one side by super chilling on one side during base material flight at a high speed, and its crystalline texture is once abnormal for also comprise the crystalline texture of the mixed crystal type of monoclinic crystal main body (monoclinic) except a cube crystalline substance (Cubic).This is the metal oxide porous layer.And, above-mentioned secondary crystallization layer be by when the spraying plating by super chilling and once abnormal and become the above-mentioned metal oxide porous layer of the mixed crystal state that comprises rhombic crystallization and tetragonal crystallization, the spraying plating processing by once more and secondary metamorphosis be behind the tetragonal crystal type layer.
Fig. 4 schematically shows Y 2O 3Sputtered films of bismuth (multiple aperture plasma membrane), the microstructure of near surface that this film is carried out the film after the electron beam treatment with irradiation and has a composite membrane of priming coat change.As can be known, the spraying plating particle that constitutes film has an independent existence respectively in the non-exposure experiment sheet shown in Fig. 4 (a), and the roughness on surface is big.On the other hand, by the electron beam treatment with irradiation shown in Fig. 4 (b), on above-mentioned sputtered films of bismuth, generate the new layer that has microstructure different.In this layer, above-mentioned spraying plating particle merges mutually and forms the layer of the few densification in space.In addition, Fig. 4 (c) expression has the example of priming coat.
In addition, below the compacted zone that generates by the electron beam irradiation, there are the many films of the distinctive pore of sputtered films of bismuth, become the layer of resistance to sudden heating excellence.
Fig. 5 is as Y 2O 3The porous layer of sputtered films of bismuth with by carrying out the XRD determining figure of the secondary recrystallization layer that the electron beam treatment with irradiation generates under the following conditions.Fig. 6 and Fig. 7 represent Y 2O 3Sputtered films of bismuth (porous layer) carries out before the electron beam treatment with irradiation and XRD figure shape afterwards.That is, Fig. 6 is the X-ray diffractogram after the longitudinal axis before handling is amplified, and Fig. 7 is the X-ray diffractogram after the longitudinal axis after handling is amplified.As can be seen from Figure 6, handle preceding Y 2O 3Sputtered films of bismuth is observed the monoclinic peak of expression especially in 30～35 ° scope, be the state of cube crystalline substance and monoclinic crystal coexistence.Relative therewith, as shown in Figure 7 as can be known, to this Y 2O 3Sputtered films of bismuth carries out the electron beam treatment with irradiation and in the secondary recrystallization layer that obtains, expression Y 2O 3The peak of particle becomes precipitous, and the decay of monoclinic peak can't be confirmed facial index (202), (3/0) etc., only is a cube crystalline substance.In addition, this XRD test uses the RINT1500X ray diffraction device of Rigaku Denki Co., Ltd's manufacturing to measure.The X-ray diffraction condition is as follows.
Output: 40kV
Sweep speed: 20/min
In addition, symbol 41 shown in Figure 4 is a base material, and 42 is porous layer (spraying plating granulation mass lamination), and 43 is pore (space), and 44 is granular boundary, and 45 for connecting pore, 46 secondary recrystallization layers for generating by the electron beam treatment with irradiation, and 47 is priming coat.In addition, handle by laser beam irradiation, the result who utilizes observation by light microscope to arrive sees the microstructure variation same with the electron beam shadow surface.
Like this, in the present invention, carrying out high energy radiation by the above-mentioned porous layer to the IIIB family metal oxide that mainly is made of the crystalline texture of the orthorhombic system main body after the metamorphosis once handles, arrive the volume spraying plating particle heat treated of this porous layer at least more than the fusing point, make this layer abnormal (secondary metamorphosis) once more, make its crystalline texture return to tetragonal tissue, on crystallography, make its stabilisation.
Meanwhile, in the present invention, by will be when utilizing once abnormal that spraying plating carries out, thermal deformation of accumulating in spraying plating granulation mass lamination and mechanical deformation discharge, make its proterties physically, chemically stable, and realized the densification and the smoothing of this layer together with fusion.Its result by this secondary recrystallization layer that the metal oxide of this IIIB family element constitutes, compares with the layer of direct spraying plating, and is fine and close and level and smooth.
Therefore, this secondary recrystallization layer becomes the porosity less than 5%, preferably less than 2% densification layer, and, the mean roughness (Ra) on surface is that 0.8～3.0 μ m, maximal roughness (Ry) are that 6～16 μ m, 10 mean roughness (Rz) are about 3～14 μ m, compare with above-mentioned porous layer, become visibly different layer.In addition, the control of this maximal roughness (Ry) decides from the viewpoint of anti-environmental pollution.Its reason is, the plasma ion or the electronics that are excited in etching and processing atmosphere when the surface of member inside container ream and produce under the situation of particle, its influence is often embodied by the value of the maximal roughness (Ry) on surface, and when this is worth when big, the chance that produces particle increases.
Next, the high-energy irradiation method that is used to form above-mentioned secondary recrystallization layer and carries out is described.The method that adopts among the present invention is preferably used electron beam treatment with irradiation, CO 2Laser radiations such as laser and YAG laser are handled, but are not only limited to these methods.
(1) electron beam treatment with irradiation: as the condition of this processing, in having discharged the exposure cell behind the air, import inactive gass such as Ar gas, for example, recommend to handle with illuminate condition as follows.
Irradiation atmosphere: 0～0.0005Pa (Ar gas)
Bundle irradiation power: 0.1～8kW
Processing speed: 1～30mm/s
Certainly, these conditions are not limited to above-mentioned scope, in order to obtain suitable secondary recrystallization layer illustration suitable condition, as long as can obtain regulation effect of the present invention, just be not limited only to these conditions.
The metal oxide that contains IIIB family element after the electron beam treatment with irradiation begins temperature and rises from the surface, finally arrive more than the fusing point, becomes molten condition.This melting phenomenon by increasing the electron beam irradiation power, increase the irradiation number of times and prolonging irradiation time, also can arrive film inside gradually, and therefore, the degree of depth of irradiation melting layer can be controlled by changing these illuminate conditions.In actual use, as long as fusion penetration is 1 μ m～50 μ m, just become the secondary recrystallization layer that is suitable for above-mentioned purpose of the present invention.
(2) as laser beam, can use the YAG laser that utilizes the YAG crystallization, in addition, be under the situation of gas at medium, can use CO 2Gas laser.As the treatment with irradiation of this laser beam, recommend condition shown below.
Laser power: 0.1～10kW
Laser beam area: 0.01～2500mm 2
Processing speed: 5～1000mm/s
Layer after above-mentioned electron beam treatment with irradiation and laser beam irradiation are handled as mentioned above, through high temperature metamorphosis, is separated out secondary recrystallization when cooling, become crystal type stable on physical chemistry, and therefore, the modification of film is carried out with other unit of crystallization stage.For example, the Y that utilizes the atmosphere plasma metallikon to form 2O 3Film as mentioned above, is the iris main body under the spraying plating state, and after the electron beam irradiation, major part becomes a cube crystalline substance.
Below, the feature of the secondary recrystallization layer that the metal oxide of the periodic table of elements IIIB family element after being handled by high energy radiation is constituted is summarized.
A. handle the secondary recrystallization layer that generates by high energy radiation, be make the porous layer that constitutes by metal oxide etc. as the once abnormal layer of lower floor further take place secondary abnormal and forms layer, perhaps the oxide particle with this lower floor is heated to more than the fusing point, therefore at least a portion pore is eliminated, thus densification.
B. handle the secondary recrystallization layer that generates by high energy radiation, be to make under the situation of the abnormal layer that obtains of the porous layer generation secondary that constitutes by metal oxide of lower floor especially at it, especially under it be situation with the sputtered films of bismuth of metallikon formation, not melt granules during spraying plating is fusion fully also, and the surface becomes mirror status, is therefore eliminated by the thrust of plasma etching easily.
C. according to the effect of above-mentioned a, b, above-mentioned porous layer is to handle the secondary recrystallization layer that generates by high energy radiation, and therefore, the perforation pore is blocked, the corrosive gas of invading inside (base material) by these perforation pores has not had, corrosion resistance improves, and, because densification, so, for the plasma etching effect, will give play to strong resistance, will give play to excellent corrosion resistance and anti-plasma corrosivity for a long time.
D. above-mentioned secondary recrystallization layer is crystallization stable on physical chemistry, so modification can realize with level of crystallization.And at this moment, the thermal deformation that imports during spraying plating also is released simultaneously, becomes stable layer.
E. the thickness of handling the secondary recrystallization layer generates by high energy radiation is preferably the thickness about surperficial 1～50 μ m of distance.Its reason is, when less than 1 μ m, do not have the effect of film forming, and on the other hand, under the situation of thickness greater than 50 μ m, it is big that the burden that high energy radiation is handled becomes, and the effect of film forming is saturated.
In addition, the porous layer of lower floor exists as the layer of resistance to sudden heating excellence, this layer have and the upper strata between bear the feature of cushioning effect.That is, has the effect that thermal shock that effect that the thermal shock that applies by the compact substance secondary crystallization layer that makes to the upper strata relaxes is subjected to film integral body relaxes.In this meaning, under the situation that has this porous layer that constitutes by sputtered films of bismuth, the composite membrane that forms at top laminate secondary recrystallization layer in lower floor, produce synergy by this two-layer composite action, the durability of film improves.
In addition, as mentioned above, when carrying out etching with high beta plasma output, the parts in the chamber etc. become big with the potential difference of plasma, cover the Y on the parts etc. 2O 3Be corroded Deng sputtered films of bismuth, thus the particle of the corrosion product of Sheng Chenging fall and the surface attached to handled object on, cause that device is bad.; in plasma processing apparatus of the present invention, the corrosion resistance of the film that forms on the surface of parts etc. improves, thus; even become under the situation about 550V increasing the potential difference of plasma output, also can suppress the generation of particle until parts etc. and plasma.In addition, the potential difference of above-mentioned parts etc. and plasma is utilized and is controlled to the electric power that mounting table 5 applies from the high frequency electric source 7 of Fig. 1, is preferably below the 550V, more preferably below the above 550V of 120V.
Embodiment
(embodiment 1)
On the surface of the chamber inner wall parts (aluminum baffle plate) of plasma processing apparatus shown in Figure 1, spraying plating is as the Y of the example of IIIB family metal oxide 2O 3(purity is more than the 95mass%) obtains being formed with the parts (comparative example B) of film; At spraying plating Y 2O 3Form after the film,, make its secondary metamorphosis, form parts (example A) with secondary crystallization layer to its surface irradiation electron beam.In each chamber, alternately repeat importing and contain F gas and contain CH gas, carry out plasma treatment, make above-mentioned Y 2O 3After the sputtered films of bismuth fragilityization, by controlling to amount as the High frequency power that is applied by the mounting table of the semiconductor wafer of plasma treatment body, the potential difference of chamber wall current potential and plasma is changed at 200V～300V, measure the generation of the dust (particle) on the semiconductor wafer under each potential difference.It is the results are shown in Fig. 2.
The result, in comparative example B, increase along with potential difference, except the dust that causes by semiconductor wafer, also produced the dust that causes by film (yttrium), and in example A, though observed the dust that causes by semiconductor wafer, but can't see the dust that generation is caused by film component (yttrium) fully, or only produce dust seldom.
(embodiment 2)
For the limiting value of the potential difference of investigating container for plasma treatment inwall parts (lower isolator of aluminum, baffle plate, deposit shield) and plasma (scope that can suppress the generation of the dust that film (yttrium) causes), prepare out similarly to Example 1: spraying plating Y on the surface of container handling inwall parts 2O 3And be formed with the parts (comparative example B) of film; With at spraying plating Y 2O 3And after the formation film, again its surface is carried out the electron beam treatment with irradiation and made its secondary metamorphosis, thereby be formed with the parts (example A) of secondary crystallization layer.In each container handling, alternately repeat to import and contain F gas and contain CH gas and carry out plasma treatment, make Y 2O 3After the film fragilityization, the amount of the High frequency power that applies to lower electrode by control changes the parts etc. and the potential difference of plasma, measures the generation of the dust on the semiconductor wafer under each potential difference.It is the results are shown in Fig. 3.
As a result, in comparative example B, along with the increase of potential difference, the dust that is caused by yttrium and its increase pro rata, and in example A, even when 550V, also do not have to find the generation of the dust that caused by yttrium.Therefore, as can be known: utilize plasma processing apparatus of the present invention,, also can suppress the generation of the dust that causes by yttrium even potential difference is increased under the situation of maximum 550V.
Utilizability on the industry
Technology of the present invention, the member, the section that much less use in the general semiconductor processing Parts etc., the plasma processing apparatus that can be used as the nearest processing that more requires precise height is used The process for treating surface of parts. The present invention be particularly suitable for as use separately respectively contain F gas or Contain the device of CH gas or in alternately reusing the harsh atmosphere of these gases, advance The deposit shield, baffle plate, focusing ring of the semiconductor processing of row plasma treatment, The members such as upper and lower insulator ring, shading ring, bellows cover, electrode, solid inductor, The process for treating surface of parts etc. In addition, the present invention can also be used as the liquid crystal device manufacturing installation Process for treating surface with parts.

Claims (21)

1. a plasma processing apparatus is characterized in that, comprising:
Accommodate the chamber that utilizes the handled object that the etch processes gaseous plasma processes; With
Being exposed to position that plasma generates atmosphere, being arranged on member or parts in this chamber of this chamber itself,
On surface more than in described position, described member or described parts any, be provided with composite bed, this composite bed comprises the secondary recrystallization layer of porous layer that is made of metal oxide and this metal oxide that forms on this porous layer,
Described etch processes is the processing that alternate repetition importing fluoro-gas and gas containing hydrocarbon carry out.
2. plasma processing apparatus according to claim 1 is characterized in that:
Below described porous layer, has the priming coat that constitutes by metal, alloy, pottery or cermet.
3. plasma processing apparatus according to claim 1 is characterized in that:
Described fluoro-gas is for being selected from C xF yGas, CHF are that gas, HF are that gas, SF are gas and these gas and O 2Mist in the gas more than a kind.
4. plasma processing apparatus according to claim 1 is characterized in that:
Described gas containing hydrocarbon is for being selected from C xH yGas, contain H gas and C xH yGas and O 2Mist in the gas more than a kind.
5. plasma processing apparatus according to claim 1 is characterized in that:
Described metal oxide is the metal oxide that contains IIIB family element.
6. plasma processing apparatus according to claim 1 and 2 is characterized in that:
Described secondary recrystallization layer forms its secondary metamorphosis by the once abnormal metal oxide that contains in the porous layer being carried out the high energy radiation processing.
7. plasma processing apparatus according to claim 1 and 2 is characterized in that:
Described secondary recrystallization layer for the porous layer that contains the orthorhombic system crystallization by high energy radiation handle carry out secondary abnormal become behind the tetragonal system tissue layer.
8. plasma processing apparatus according to claim 6 is characterized in that:
Described high energy radiation is treated to the electron beam treatment with irradiation or laser beam irradiation is handled.
9. plasma processing apparatus according to claim 7 is characterized in that:
Described high energy radiation is treated to the electron beam treatment with irradiation or laser beam irradiation is handled.
10. plasma processing apparatus according to claim 1 is characterized in that:
The surface of the position that is exposed to plasma atmosphere, member or the parts of described chamber itself and described plasma have the following potential difference of the above 550V of 120V.
11. plasma processing apparatus according to claim 10 is characterized in that:
The High frequency power that the mounting table of described potential difference by the handled object in being arranged on described chamber applies is controlled.
12. a method of plasma processing, it is to utilize the plasma of etch processes gas to the plasma treatment that the surface that is housed in the handled object in the chamber processes, and it is characterized in that, comprising:
At first, at the position that is exposed to plasma atmosphere of described chamber itself, be arranged on the surface of member in this chamber or parts, cover the operation that forms composite bed in advance, this composite bed comprises the secondary recrystallization layer of porous layer that is made of metal oxide and the described metal oxide that forms on this porous layer;
After importing comprises first gas of fluoro-gas in this chamber, it is excited, produce the operation of first plasma; With
Then, after importing comprises second gas of appropriate hydrocarbon gas in this chamber, it is excited, produce second plasma, the operation of handling.
13. method of plasma processing according to claim 12 is characterized in that:
Described fluoro-gas is for being selected from C xF yGas, CHF are that gas, HF are that gas, SF are gas and these gas and O 2Mist in the gas more than a kind.
14. method of plasma processing according to claim 12 is characterized in that:
Described gas containing hydrocarbon is for being selected from C xH yGas, contain H gas and C xH yGas and O 2Mist in the gas more than a kind.
15. method of plasma processing according to claim 12 is characterized in that:
Described metal oxide is the metal oxide that contains IIIB family element.
16. method of plasma processing according to claim 12 is characterized in that:
Described secondary recrystallization layer forms its secondary metamorphosis by the once abnormal metal oxide that contains in the porous layer being carried out the high energy radiation processing.
17. method of plasma processing according to claim 12 is characterized in that:
Described secondary recrystallization layer for the porous layer that contains the orthorhombic system crystallization by high energy radiation handle carry out secondary abnormal become behind the tetragonal system tissue layer.
18. method of plasma processing according to claim 16 is characterized in that:
Described high energy radiation is treated to the electron beam treatment with irradiation or laser beam irradiation is handled.
19. method of plasma processing according to claim 17 is characterized in that:
Described high energy radiation is treated to the electron beam treatment with irradiation or laser beam irradiation is handled.
20. method of plasma processing according to claim 12 is characterized in that:
The surface of the position that is exposed to plasma atmosphere, member or parts in the described chamber and described plasma have the following potential difference of the above 550V of 120V.
21. method of plasma processing according to claim 20 is characterized in that:
The High frequency power that the mounting table of described potential difference by the handled object in being arranged on described chamber applies is controlled.
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