WO2017081953A1 - ハロゲン系ガスを用いる処理装置における処理方法 - Google Patents
ハロゲン系ガスを用いる処理装置における処理方法 Download PDFInfo
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- WO2017081953A1 WO2017081953A1 PCT/JP2016/079249 JP2016079249W WO2017081953A1 WO 2017081953 A1 WO2017081953 A1 WO 2017081953A1 JP 2016079249 W JP2016079249 W JP 2016079249W WO 2017081953 A1 WO2017081953 A1 WO 2017081953A1
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- Prior art keywords
- chamber
- gas
- halogen
- processing method
- based gas
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- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 52
- 150000002367 halogens Chemical class 0.000 title claims abstract description 52
- 238000012545 processing Methods 0.000 title claims abstract description 47
- 238000003672 processing method Methods 0.000 title claims description 45
- 239000007789 gas Substances 0.000 claims abstract description 156
- 238000010926 purge Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 42
- 230000008569 process Effects 0.000 claims abstract description 41
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 36
- 239000011651 chromium Substances 0.000 claims description 23
- 229910001220 stainless steel Inorganic materials 0.000 claims description 22
- 239000010935 stainless steel Substances 0.000 claims description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002161 passivation Methods 0.000 claims description 3
- -1 argon ions Chemical class 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 description 46
- 238000005260 corrosion Methods 0.000 description 30
- 230000007797 corrosion Effects 0.000 description 30
- 235000012431 wafers Nutrition 0.000 description 22
- 238000001020 plasma etching Methods 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 238000005530 etching Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 229910052801 chlorine Inorganic materials 0.000 description 8
- 238000011109 contamination Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910019923 CrOx Inorganic materials 0.000 description 7
- 230000007246 mechanism Effects 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010405 reoxidation reaction Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 229910015189 FeOx Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 1
Images
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- 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
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- 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
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- 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
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
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- 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
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- 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
- H01L21/31116—Etching inorganic layers by chemical means by dry-etching
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- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
- H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
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- H01J2237/02—Details
- H01J2237/022—Avoiding or removing foreign or contaminating particles, debris or deposits on sample or tube
Definitions
- the present invention relates to a processing method in a processing apparatus using a halogen-based gas such as an etching apparatus.
- a plasma etching process in which a predetermined pattern is formed on a predetermined layer formed on a semiconductor wafer that is an object to be processed, and etching is performed by plasma using a resist or the like as a mask.
- Such a plasma etching process is performed by introducing a corrosive etching gas into a chamber held in a vacuum of a plasma etching apparatus and turning the etching gas into plasma.
- a plasma etching apparatus needs to be regularly maintained, and the chamber is opened to the atmosphere during the maintenance.
- the reaction product in the chamber reacts with moisture in the air when it is opened to the atmosphere as it is, harmful substances are generated, so the chamber is cycle purged before the chamber is opened to the atmosphere (for example, Patent Document 1 “Prior Art”).
- the cycle purge is a process in which N 2 gas is introduced into the chamber, the pressure is increased, the reaction product is mixed, the inside of the chamber is evacuated, and N 2 gas is introduced again a plurality of times.
- the chamber is opened to the atmosphere for maintenance, and then the wafer is processed to mainly contain chromium on the wafer. Metal contamination occurs. For this reason, even after the chamber is opened to the atmosphere, N 2 purge and cycle purge are performed until the metal contamination is below the reference value, and then dummy wafer processing is performed.
- a halogen-based gas such as Cl 2 gas or HBr as an etching gas
- Such metal contamination of the wafer after opening the chamber to the atmosphere is considered to be caused by corrosion of stainless steel piping by halogen-based gas due to opening to the atmosphere, and metal contamination is below the standard value. Even if N 2 purge or cycle purge is performed until this occurs, and then dummy wafer processing is performed, it will be handled after corrosion has occurred. For this reason, it takes a long time to purge, and several tens to several hundreds of dummy wafers are required, and a total time of about half a day to about a day is required.
- an object of the present invention is to provide a treatment method capable of suppressing corrosion per se caused by a halogen-based gas generated in a treatment apparatus using a halogen-based gas.
- a halogen-based gas is supplied into the chamber while a member having an oxide film formed on the surface is connected or the inside of the chamber having the oxide film is maintained in a vacuum.
- ion sputtering may be performed simultaneously with the purging step or prior to the purging step.
- the ion sputtering treatment can be performed using argon ions obtained by generating argon gas plasma.
- a halogen-based gas is supplied into the chamber while a member having an oxide film formed on the surface is connected, or the chamber having the oxide film on the surface is kept in vacuum.
- a processing method in a processing apparatus for performing a predetermined process on an object to be processed, the step of performing the predetermined process on the object to be processed one or more times in the chamber, and then the inside of the chamber by oxygen plasma There is provided a processing method in a processing apparatus using a halogen-based gas, which includes a processing step and a step of opening the chamber to the atmosphere.
- a halogen-based gas is supplied into the chamber while a member having an oxide film formed on the surface is connected or the inside of the chamber having the oxide film on the surface is kept in vacuum.
- a processing method is provided.
- the purging at the time of idling can be performed by mixing nitrogen gas with oxygen gas. Further, after the purge at the time of idling is performed with oxygen gas for a predetermined period, the inside of the chamber may be purged with nitrogen gas for the remaining period of idling.
- an example in which the member connected to the chamber and having an oxide film formed on the surface is a gas supply pipe made of stainless steel, and the oxide film is a passive film of chromium.
- a typical example can be given.
- a typical example of the halogen gas is chlorine gas.
- the oxide film can be re-oxidized by oxygen gas, dry air, or oxygen plasma, corrosion itself by the halogen-based gas that occurs in the processing apparatus using the halogen-based gas can be suppressed.
- Stainless steel has a passive film (Cr 2 O 3 ) formed on the surface by combining chromium (Cr) contained as a component with oxygen in the air.
- This passive film is a stable substance and has high corrosion resistance against halogen-based gases.
- corrosion occurs due to reaction with halogen-based gas in an environment where moisture exists.
- chlorine (Cl) is used as the halogen
- the passive film is destroyed by hydrochloric acid generated by the reaction of water and chlorine in an environment where there is a lot of moisture when released to the atmosphere, and a large amount of chromium chloride (CrCl 3 ). When generated, it peels off or volatilizes from the surface of the stainless steel, causing particles and gas molecules to cause metal contamination.
- oxygen gas or dry air is supplied to the chamber through the gas supply pipe to purge the chamber, thereby removing halogen-based components such as chlorine in the pipe.
- the passive film can be returned to its initial healthy state, and even when it comes into contact with moisture due to release to the atmosphere, corrosion by halogen hardly occurs.
- the passive film is slightly corroded by the halogen-based gas during the treatment with the halogen-based gas in a vacuum atmosphere, but oxygen gas or oxygen is introduced into the chamber via the gas supply pipe during idling during the treatment with the halogen-based gas. It has been found that by purging the inside of the chamber by supplying dry air, the passive film can be returned to the initial healthy state and corrosion by halogen can be suppressed.
- the present invention has been made based on such knowledge.
- FIG. 1 is a sectional view showing a schematic configuration of such a processing apparatus.
- the processing apparatus 1 shown in FIG. 1 is configured as a plasma etching apparatus.
- the processing apparatus 1 includes a chamber 2 that houses a semiconductor wafer (hereinafter simply referred to as a wafer) W that is an object to be processed.
- the chamber 2 has a main body portion 2a and a lid portion 2b provided on the main body portion 2a so as to be openable and closable, and is grounded.
- the chamber 2 is made of aluminum whose inner surface is anodized (anodized).
- a mounting table 4 On the bottom wall in the main body 2a of the chamber 2, there is provided a mounting table 4 on which a wafer W is mounted via an insulating member 3 and functions as a lower electrode.
- a feeding line 5 is connected to the mounting table 4, and a matching unit 6 and a high-frequency power source 7 are connected to the feeding line 5.
- a high frequency power having a predetermined frequency is applied from the high frequency power source 7.
- a shower head 8 that introduces gas into the chamber 2 and functions as an upper electrode is provided inside the lid portion 2 b of the chamber 2 so as to face the mounting table 4.
- the shower head 8 has a gas diffusion space 8a for diffusing a processing gas therein, and a plurality of gas discharge holes 8b formed on the lower surface.
- the shower head 8 is grounded via the chamber 2 and constitutes a pair of parallel plate electrodes together with the mounting table 4. Therefore, by applying high frequency power from the high frequency power source 7 to the mounting table 4, a high frequency electric field is generated between the mounting table 4 and the shower head 8, and plasma is generated in the chamber 2.
- a gas inlet 9 is provided on the upper surface of the shower head 8, and a gas supply pipe 10 made of stainless steel is connected to the gas inlet 9.
- the gas supply pipe 10 is connected to a gas supply mechanism (not shown), and from the gas supply mechanism, Cl 2 gas as a halogen-based gas, which is an etching gas, and O 2 gas or dry air as a purge gas are supplied to the shower head 8. To supply. It should be noted that other components of the etching gas, dilution gas, and the like are supplied from the gas supply mechanism. Then, Cl 2 gas, which is an etching gas, is turned into plasma by the high frequency electric field, and a predetermined layer of the wafer W is etched.
- An exhaust pipe 11 is connected to the bottom of the main body 2a of the chamber 2, and an exhaust device 12 is connected to the exhaust pipe 11 and a pressure adjusting valve (not shown) is provided.
- the exhaust device 12 includes a vacuum pump such as a turbo molecular pump, and is configured so that the inside of the chamber 2 can be exhausted to be evacuated to a predetermined degree of vacuum.
- a loading / unloading port 13 for loading / unloading the wafer W is formed on the side wall of the main body 2a of the chamber 2, and a gate valve 14 for opening / closing the loading / unloading port 13 is provided. Sometimes, the wafer W is carried in and out of the chamber 2 by a transfer means (not shown).
- the gate valve 14 is opened, the wafer W is loaded from the loading / unloading port 13 by a transfer means (not shown), and the wafer W is mounted on the mounting table 4. After the transfer means is retracted from the chamber 2, the gate valve 14 is closed.
- the pressure in the chamber 2 is adjusted to a predetermined degree of vacuum by the pressure adjusting valve, and Cl 2 gas is supplied into the shower head 8 as an etching gas via the gas supply pipe 10.
- Cl 2 gas is introduced into 2 .
- a high frequency electric field is formed between the mounting table 4 and the shower head 8, and plasma of Cl 2 gas that is an etching gas is generated.
- a predetermined film of the wafer W is etched.
- FIG. 2 is a flowchart showing the processing method according to the first embodiment of the present invention.
- the plasma etching process as described above is performed once or a plurality of times by the processing apparatus 1 (step 1), and then oxygen gas (O 2 gas) or dry air (D-Air) is passed through the gas supply pipe 10.
- the chamber 2 is supplied to purge the inside of the chamber 2 (step 2), and then the chamber 2 is opened to the atmosphere (step 3). That is, after the etching process is performed, before the atmosphere is released, the chamber 2 is purged with oxygen gas (O 2 gas) or dry air instead of the conventional cycle purge.
- oxygen gas O 2 gas
- D-Air dry air
- the corrosion of the gas supply pipe 10 made of stainless steel (SUS) is caused by Cl 2 remaining on the inner surface of the pipe. If the atmosphere is opened with Cl 2 remaining on the surface, the moisture in the atmosphere and Cl 2 react with the passive film, so that corrosion progresses greatly and causes metal contamination. In contrast, in the present embodiment, moisture in the atmosphere is obtained by purging the chamber 2 by supplying oxygen gas (O 2 gas) or dry air to the chamber 2 via the gas supply pipe 10 prior to opening to the atmosphere.
- O 2 gas oxygen gas
- the Cl component adhering to the gas supply pipe 10 can be removed before contacting with the gas supply pipe 10 and the passive film can be reoxidized to return to the initial state.
- oxygen gas (O 2 gas) When oxygen gas (O 2 gas) is used for the purge in Step 2, not only oxygen gas (O 2 gas) but also inert gas (rare gas such as N 2 gas or Ar gas) is mixed. May be. However, oxygen gas (O 2 gas) alone is more effective than using dry air or mixing an inert gas. Further, the purge in step 2 may be performed for several minutes to 30 minutes before being released to the atmosphere, and can be made shorter than the conventional cycle purge.
- the oxygen gas used for the purge in Step 2 contains moisture, the effect of reoxidation by oxygen is hindered by the action of water and Cl. For this reason, it is preferable to use a gas (oxygen gas, dry air, etc.) used for purging that does not substantially contain moisture. That is, it is preferable to remove moisture in the purge gas as much as possible.
- a gas oxygen gas, dry air, etc.
- the moisture concentration of the halogen-based gas is set to 0.5 ppm or less. Even in this embodiment, if the moisture concentration is lower than the moisture concentration of the halogen-based gas, a certain effect is obtained. In order to obtain it, the moisture concentration in the purge gas is preferably 0.5 ppm or less.
- the gas supply pipe 10 is made of stainless steel (SUS) and has a high corrosion resistance because a passive film is formed on the surface, but is a halogen-based gas in an environment containing moisture.
- SUS stainless steel
- the following reactions (1) and (2) occur between the Cl 2 gas, water (H 2 O), and the passive film (CrOx), and the passive film is corroded.
- FIG. 3 is a schematic diagram showing a reaction model example of passive film corrosion of stainless steel by Cl 2 gas.
- Cl 2 gas adheres to the passive film, it adheres to the surface of the passive film as a surface material.
- FeClx produced by reaction of Fe and Cl, and CrClx produced by the reaction of a slight amount of moisture in the chamber with Cl 2 exist.
- the corrosion inhibition model in this embodiment is as shown in FIG. That is, when a passive film (CrOx) is formed on the surface as shown in FIG. 4 (a) and Cl 2 gas adheres to the surface as shown in FIG. 4 (b), CrClx is partially formed. Arise. For this reason, before opening to the atmosphere, purging with oxygen gas (O 2 gas) or dry air as shown in FIG. 4C removes Cl components such as Cl 2 adhering to the surface. 4 (d), the passive film is reoxidized to return to the initial state. Thereby, corrosion of a passive film is suppressed.
- O 2 gas oxygen gas
- FIG. 4C dry air
- chrome oxide has a larger value on the negative side than chrome chloride and is more stable. This also confirms that Cr tends to be an oxide rather than chloride in the presence of oxygen, and that halogen corrosion due to chlorine can be suppressed by reoxidation of CrCl 3 .
- FIG. 5 is a flowchart showing a processing method according to the second embodiment of the present invention.
- the plasma etching process as described above is performed once or a plurality of times by the processing apparatus 1 (step 11), and then the gas supply pipe 10 is used instead of purging with oxygen gas or the like.
- the inner and the chamber is exposed to O 2 plasma perform the O 2 plasma treatment (step 12), then performs the air opening of the chamber 2 (step 13).
- the O 2 plasma treatment can be performed by supplying high-frequency power from the high-frequency power source 7 to the mounting table 4 while supplying oxygen gas into the chamber 2 through the gas supply pipe 10.
- the O 2 plasma may be a remote plasma is introduced into the chamber 2 through the gas supply pipe 10.
- the corrosion inhibition model of this embodiment is as shown in FIG. That is, if a Cl 2 gas adheres to the surface as shown in FIG. 6B in a state where a passive film (CrOx) is generated as shown in FIG. 6A, CrClx is partially generated. For this reason, as shown in FIG. 6C, the inside of the chamber is exposed to O 2 plasma before being released to the atmosphere, and the Cl component on the surface is removed by O radicals (O * ), as shown in FIG. 6D. As described above, the passive film is reoxidized using the oxidation effect of O radicals to return to the initial state. Since O radicals are more reactive than O 2 , higher effects can be obtained in a short time, and reoxidation can be completed in a short time of 30 seconds or less.
- FIG. 7 is a flowchart showing a processing method according to the third embodiment of the present invention.
- the plasma etching process as described above is performed once or a plurality of times by the processing apparatus 1 (step 21), and then a plasma of an easily ionized gas such as Ar gas is generated.
- Sputtering with Ar + ions is performed (step 22). Thereby, Cl on the surface of the gas supply pipe is removed.
- oxygen gas oxygen gas
- D-Air dry air
- the corrosion inhibition model of this embodiment is as shown in FIG. That is, when Cl 2 gas adheres to the surface as shown in FIG. 8B in a state where a passive film (CrOx) is generated as shown in FIG. 8A, CrClx is partially generated. Therefore, before opening to the atmosphere, as shown in FIG. 8C, Ar gas plasma is generated in the chamber, and the surface of the gas supply pipe is sputtered with Ar + ions to remove the Cl component on the surface. At this time, since ions reach the inside of the passive film, the passive film is in an unstable Cr state. Therefore, as shown in FIG. 8D, the passive film is reoxidized with oxygen gas (O 2 gas) or dry air to return to the initial state. Since ions such as Ar + ions have a large effect of removing the Cl component, the Cl component can be more efficiently removed.
- oxygen gas O 2 gas
- step 22 and step 23 may be performed simultaneously by supplying oxygen gas (O 2 gas) or the like into the chamber during sputtering with ions such as Ar + ions.
- oxygen gas O 2 gas
- ions such as Ar + ions.
- the passive film is slightly corroded by the Cl 2 gas, which is a halogen-based gas, during the plasma etching that is a vacuum process, but the conventional N 2 gas is used during idling during the plasma etching process.
- Cl 2 gas which is a halogen-based gas
- the conventional N 2 gas is used during idling during the plasma etching process.
- oxygen gas or dry air that is substantially free of moisture for purging, and the moisture concentration at that time is preferably 0.5 ppm or less.
- step 32 is replaced with O 2 gas by N 2 gas.
- step 33 purging with O 2 gas in step 32 is performed for a predetermined period, and then purging with N 2 gas (for the remaining idling period) Step 33) may be performed.
- a rare gas such as Ar gas may be used in place of N 2 gas as an inert gas mixed with oxygen gas (O 2 gas) during the purge in step 32.
- O 2 gas oxygen gas
- purging before opening to the atmosphere or plasma processing as in the first to third embodiments may be performed.
- FIG. 11 shows the results for chromium / iron (Cr / Fe)
- FIG. 12 shows the results for chromium chloride / chromium (CrCl 3 / Cr).
- the ratio of Cr decreases in those stored in an N 2 gas atmosphere, whereas the ratio of Cr does not decrease in those stored in a D-Air atmosphere containing oxygen.
- the ratio of chlorination of Cr is lower when stored in a D-Air atmosphere containing oxygen than when stored in an N 2 gas atmosphere. From this, it was confirmed that the corrosion of the passive film of Cr was suppressed in those stored in a D-Air atmosphere containing oxygen after exposure to Cl 2 .
- the present invention is not limited to the above-described embodiment, and can be variously modified within the scope of the idea of the present invention.
- the corrosion of the passive film of the stainless steel gas supply pipe is suppressed is shown.
- the stainless steel screw that is a member in the chamber and the stainless steel spiral tube for ensuring conductivity are shown.
- other oxide films such as aluminum oxide (Al 2 O 3 ) and yttrium oxide (Y 2 O 3 ) are not only applied to the surface of the pipe or the chamber.
- the present invention is also applicable to the case where the film is formed, and the corrosion prevention effect can be obtained in that case as well.
- plasma etching is exemplified as the process using a halogen-based gas.
- the present invention is not limited to this, and it is needless to say that the process can be applied to a process using other halogen-based gas such as a film forming process.
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Abstract
Description
を有する、ハロゲン系ガスを用いる処理装置における処理方法が提供される。
ステンレス鋼は、成分として含有するクロム(Cr)が空気中の酸素と結合することにより、表面に不動態膜(Cr2O3)が形成されている。この不動態膜は安定な物質であり、ハロゲン系ガスに対しても高い耐食性を有している。しかし、水分が存在する環境下ではハロゲン系ガスと反応して腐食が生じることが判明した。例えば、ハロゲンとして塩素(Cl)を用いた場合、大気開放した際の水分が多い環境では、水と塩素が反応して生じた塩酸によって不動態膜が破壊され、塩化クロム(CrCl3)が多く生成されて、ステンレス鋼の表面から剥離または揮発し、パーティクルやガス分子となってメタル汚染を引き起こす。
最初に、本発明の実施形態の処理方法に用いることができる処理装置の一例について説明する。図1はそのような処理装置の概略構成を示す断面図である。
このようなプラズマエッチングを複数枚のウエハについて繰り返して行うと、チャンバ2内や排気装置12等には反応生成物が付着するため、定期的にチャンバ2を大気開放し蓋部2bを開けてチャンバ2内等をメンテナンスする。
本実施形態に係る処理方法は、このような問題を解決するものである。
上述したように、ガス供給配管10はステンレス鋼(SUS)製であり、表面に不動態膜が形成されているため高い耐食性を有しているが、水分を含む環境下ではハロゲン系ガスであるCl2ガスと水(H2O)と不動態膜(CrOx)との間では、一例として以下の(1)式および(2)式の反応が生じ、不動態膜が腐食される。
Cl2+H2O ⇔ HCl+HClO ・・・(1)
CrOx+HCl ⇔ CrClx+H2O ・・・(2)
すなわち、塩素ガス(Cl2)と水(H2O)とが反応して塩酸(HCl)が生じ、塩酸が不動態膜(CrOx)と反応して塩化クロム(CrClx)を生成する。
次に、本発明の第2の実施形態に係る処理方法について説明する。
図5は、本発明の第2の実施形態に係る処理方法を示すフロー図である。本実施形態では、第1の実施形態と同様、処理装置1により上記のようなプラズマエッチング処理を1回または複数回行い(ステップ11)、その後酸素ガス等でパージする代わりに、ガス供給配管10内およびチャンバ内をO2プラズマに曝してO2プラズマ処理を行い(ステップ12)、その後チャンバ2の大気開放を行う(ステップ13)。O2プラズマ処理は、ガス供給配管10を介してチャンバ2内に酸素ガスを供給しつつ、高周波電源7から載置台4に高周波電力を供給することにより行うことができる。他の機構でO2プラズマを生成した後、O2プラズマをガス供給配管10を介してチャンバ2内に導入するリモートプラズマであってもよい。
次に、本発明の第3の実施形態に係る処理方法について説明する。
図7は、本発明の第3の実施形態に係る処理方法を示すフロー図である。本実施形態では、第1の実施形態と同様、処理装置1により上記のようなプラズマエッチング処理を1回または複数回行い(ステップ21)、その後、イオン化しやすいガス例えばArガスのプラズマを生成し、Ar+イオンによるスパッタ処理を行う(ステップ22)。これによりガス供給配管表面のClを取り除く。この場合、Clを除去した後は不動態膜が不安定なCrの状態となるため、その後、酸素ガス(O2ガス)またはドライエア(D-Air)をガス供給配管10を介してチャンバ2内に供給してチャンバ2内をパージする(ステップ23)。これにより不動態膜を再酸化させる。その後、チャンバ2の大気開放を行う(ステップ24)。
次に、本発明の第4の実施形態に係る処理方法について説明する。
本実施形態においては、図9に示すように、チャンバ2内で上述したプラズマエッチング処理(ステップ31)を複数回繰り返し行うに際し、一回のプラズマエッチング処理が終了後、次のウエハのプラズマエッチングの間のアイドリングの際に、ガス供給配管10を介してチャンバ2内に酸素ガス(O2ガス)またはドライエア(D-Air)を供給し、チャンバ内をパージする(ステップ32)。これを大気開放までの一連の処理の間、常時続ける。
ここではステンレス鋼(SUS)の試験片を複数準備し、これらを塩素ガス(Cl2ガス)に曝した後、一部を窒素ガス(N2ガス)雰囲気で、残部を水分が0.5ppm以下の実質的に水分が存在しない状態に管理したドライエア(D-Air)雰囲気で72時間保管した。
なお、本発明は上記実施形態に限定されることなく本発明の思想の範囲内で種々変形可能である。例えば、上記実施形態では、ステンレス鋼製のガス供給配管の不動態膜の腐食を抑制する例を示したが、チャンバ内部材であるステンレス鋼製ネジや導電性確保のためのステンレス鋼製スパイラルチューブにも効果があり、さらにステンレス鋼の不動態膜のみならず、配管やチャンバ内の表面等に酸化アルミニウム(Al2O3)、酸化イットリウム(Y2O3)等の他の酸化物の膜が形成されている場合にも適用可能であり、その場合にも同様に腐食防止効果を得ることができる。
2;チャンバ
2a;本体部
2b;蓋部
4;載置台
7;高周波電源
8;シャワーヘッド
9;ガス導入口
10;ガス供給配管
11;排気管
12;排気装置
W;半導体ウエハ(被処理体)
Claims (13)
- 表面に酸化膜が形成された部材が接続され、または表面に酸化膜を有するチャンバ内を真空に保持しつつ、前記チャンバ内にハロゲン系ガスを供給して被処理体に所定の処理を行う処理装置における処理方法であって、
前記チャンバ内で被処理体に対する前記所定の処理を1回または複数回行う工程と、
その後、前記チャンバに酸素ガスまたはドライエアを供給して前記チャンバをパージする工程と、
その後、前記チャンバを大気開放する工程と
を有する、ハロゲン系ガスを用いる処理装置における処理方法。 - 前記パージする工程と同時に、または前記パージする工程に先立って、イオンスパッタ処理を行う、請求項1に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記イオンスパッタ処理は、アルゴンガスのプラズマを生成して得られたアルゴンイオンを用いて行う、請求項2に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記チャンバに接続された前記表面に酸化膜が形成された部材は、ステンレス鋼製のガス供給配管であり、前記酸化膜はクロムの不動態膜である、請求項1に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記ハロゲン系ガスは、塩素ガスである、請求項1に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 表面に酸化膜が形成された部材が接続され、または表面に酸化膜を有するチャンバ内を真空に保持しつつ、前記チャンバ内にハロゲン系ガスを供給して被処理体に所定の処理を行う処理装置における処理方法であって、
前記チャンバ内で被処理体に対する前記所定の処理を1回または複数回行う工程と、
その後、前記チャンバ内を酸素プラズマにより処理する工程と、
その後、前記チャンバを大気開放する工程と
を有する、ハロゲン系ガスを用いる処理装置における処理方法。 - 前記チャンバに接続された前記表面に酸化膜が形成された部材は、ステンレス鋼製のガス供給配管であり、前記酸化膜はクロムの不動態膜である、請求項6に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記ハロゲン系ガスは、塩素ガスである、請求項6に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 表面に酸化膜が形成された部材が接続され、または表面に酸化膜を有するチャンバ内を真空に保持しつつ、前記チャンバ内にハロゲン系ガスを供給して被処理体に所定の処理を行う処理装置における処理方法であって、
前記チャンバ内で被処理体に対して前記所定の処理を、前記チャンバを真空に保持したまま複数回行う工程と、
前記複数回の前記所定の処理の間にアイドリングを行う工程と
を有し、
前記アイドリングの際に、前記チャンバに酸素ガスまたはドライエアを供給し、前記チャンバをパージする、ハロゲン系ガスを用いる処理装置における処理方法。 - 前記アイドリングの際の前記パージは、酸素ガスに窒素ガスを混合して行う、請求項9に記載の、ハロゲン系ガスを用いる処理装置における処理方法
- 前記アイドリングの際の前記パージを酸素ガスにより所定期間行った後、前記アイドリングの残りの期間に、前記チャンバ内を窒素ガスによりパージする、請求項9に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記チャンバに接続された前記表面に酸化膜が形成された部材は、ステンレス鋼製のガス供給配管であり、前記酸化膜はクロムの不動態膜である、請求項9に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
- 前記ハロゲン系ガスは、塩素ガスである、請求項9に記載の、ハロゲン系ガスを用いる処理装置における処理方法。
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