WO2005087975A1 - 有機金属化学気相堆積装置用原料気化器 - Google Patents
有機金属化学気相堆積装置用原料気化器 Download PDFInfo
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- WO2005087975A1 WO2005087975A1 PCT/JP2005/003877 JP2005003877W WO2005087975A1 WO 2005087975 A1 WO2005087975 A1 WO 2005087975A1 JP 2005003877 W JP2005003877 W JP 2005003877W WO 2005087975 A1 WO2005087975 A1 WO 2005087975A1
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- WIPO (PCT)
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- raw material
- vaporizer
- orifice
- chemical vapor
- vapor deposition
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Classifications
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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
- 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
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4485—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation without using carrier gas in contact with the source material
Definitions
- the present invention relates to a material degasser for a metalorganic chemical vapor deposition apparatus capable of performing liquid-filled equilibrium vaporization, and performs continuous supply and stable vaporization of the raw material during film formation by the apparatus. It relates to a vaporizer that can be used.
- Source gases obtained by vaporizing various organometallic compounds using a vaporizer are transported into a reaction chamber using a carrier gas to be decomposed, and the decomposed products are deposited on a substrate disposed in the reaction chamber.
- the metal organic chemical vapor deposition (MOCV D) method is used for (i) excellent step coverage, (ii) a dense film can be obtained, and (iii) large-area wafers. And (iv) the process can be performed at low temperature.Therefore, it is widely used in this field as a film forming method suitable for high integration and mass production. ing.
- a sublimation gas obtained by heating a solid material contained in a container is transferred into a reaction chamber using a carrier gas by a simple solid sublimation method, Solid sublimation method in which the raw material is supported on porous ceramic balls to suppress the change in the amount of vaporization due to the change in surface area, and liquid publishing in which a carrier gas is passed through a heated liquid raw material to transport the raw material gas corresponding to the vapor pressure
- a method and a liquid supply method for supplying a raw material in a liquid state into a gasifier are known!
- More specific simple solid sublimation methods include: (i) after an organic alkaline earth metal complex is completely melted, the melt is cooled and solidified in a raw material container, and then the complex is cooled. Or the melt is poured into a cylindrical container so that the thickness in the longitudinal axis direction is substantially constant, and then the carrier gas is not allowed to flow in the longitudinal direction.
- a method of vaporizing the complex at a temperature lower than its melting point see Patent Document 1
- (ii) bis (cyclopentagel) ruthenium having an average particle size of 0.03-5. See Patent Document 2.
- the simple solid sublimation method is not suitable for industrial use because the raw material cannot be continuously filled because the amount of vaporization is not stable due to the change in the surface area of the raw material due to sublimation.
- the supported solid sublimation method is also unsuitable for industry because it is difficult to continuously fill the raw materials.
- the liquid supply method is expected to be applied to industrialization in order to transport the raw material in a liquid state.
- this method involves (i) feeding the raw material liquid into a vaporizer heated to a high temperature.
- the raw material may be decomposed due to direct injection, and particles may be generated because the raw material is transported in a misted state.
- a large amount of solvent gas may be deposited on the substrate together with the raw material. Not only carbon is taken into the film as impurities because it is transported to the membrane, but the burden on the exhaust system increases and maintenance costs increase.
- Tetrahydrofuran (THF) which is frequently used as a solvent, has high erosion ! This can cause catastrophic damage to Northton O-rings and increase maintenance costs, and (iv) generally high carrier gas flow rates make the use of expensive raw materials inefficient and increase product costs There is a problem.
- Patent Document 1 JP-A-11-193462
- Patent Document 2 Japanese Patent Application Laid-Open No. 2003-160865
- the present invention relates to the above-mentioned problems of the liquid supply method in the metal organic chemical vapor deposition method, in particular, because the surface area of the raw material changes with the sublimation of the solid raw material and the temperature of the raw material changes.
- a thin film cannot be formed with good reproducibility
- a problem that the thin film forming apparatus has to be stopped in order to add a solid raw material a problem that an operation rate of the apparatus is reduced, and many problems.
- the metal-organic chemical vapor phase enables continuous filling and stable vaporization of raw materials by eliminating the problem that the composition of the formed thin film fluctuates due to changes in the flow rate of liquid over time. Provide raw material vaporizer for deposition equipment It was done for.
- a raw material vaporizer for a metal organic chemical vapor deposition apparatus in a raw material vaporizer for a metal organic chemical vapor deposition apparatus, the vapor pressure of a solid raw material present in the vaporizer is kept substantially constant.
- the vaporizer is characterized by having an orifice having such a large hole diameter.
- a raw material vaporizer for a metal organic chemical vapor deposition apparatus (i) a filling port for filling a liquid raw material, An orifice having a pore diameter large enough to keep the vapor pressure of the solid raw material in the vaporizer substantially constant when the solid raw material remaining after removing the contained solvent is vaporized; and
- the vaporizer having a heater "is provided.
- a method for supplying a source gas for an organometallic chemical vapor deposition apparatus wherein the orifice is provided in a vaporizer and is present in the vaporizer.
- the raw material gas is supplied to an organometallic chemical vapor deposition system through an orifice having a pore size large enough to keep the vapor pressure of the raw material substantially constant.
- a gas supply method is provided.
- a method for supplying a source gas for a metal organic chemical vapor deposition apparatus having the following steps (i) to (V):
- the vapor pressure of the raw material in the vaporizer is substantially one. Since the raw material is kept at a constant level, there is no problem that the vaporization amount of the raw material is not stable due to the change of the raw material surface area due to the sublimation of the raw material, and the solid raw material is prepared in a liquid state using a solvent. Since it can be filled into the vaporizer through piping later, it is possible to continuously supply raw materials that are important for application to industrialization. Further, when the vaporizer is used, it is sufficient that a predetermined amount or more of the liquid raw material is introduced into the vaporizer, and the vaporization amount of the raw material can be appropriately adjusted by the temperature in the vaporizer.
- the lead zirconate titanate thin film which has been difficult to produce, can be industrially produced by the method.
- FIG. 1 is a schematic configuration diagram showing one embodiment of an organometallic chemical vapor deposition apparatus equipped with a vaporizer according to the present invention.
- FIG. 2 is a schematic configuration diagram showing an operation procedure of the vaporizer according to the present invention shown in FIG. 1.
- FIG. 3 is a TiO thin film on a substrate measured in an example of the present invention. Film thickness and source gas
- FIG. 1 is a schematic configuration diagram showing one embodiment of an organometallic chemical vapor deposition apparatus equipped with a vaporizer according to the present invention.
- FIG. 2 is a schematic configuration diagram showing an operation procedure of the vaporizer according to the present invention shown in FIG.
- the vapor pressure of the solid raw material 10 existing in the vaporizer 9 is substantially constant.
- the vaporizer 9 "provided with an orifice 8 having a hole diameter large enough to be held by the vaporizer 9".
- the vapor pressure of the solid raw material 10 present in the vaporizer 9 is kept substantially constant
- the vapor pressure PmmHg of the solid raw material 10 specified by the set temperature of the vaporizer 9 is equal to the vapor pressure PmmHg.
- the difference from the vapor pressure P'mmHg of the solid raw material 10 measured in the vessel 9 is maintained within a range of about 0 to 0.5 mmHg, preferably about 0 to 0.2 mmHg, particularly preferably about 0 to 0.05 mmHg. Means to be done.
- the diameter of the spores of the sifidus 8 arranged in the vaporizer 9 should be about 50-5000 ⁇ m, preferably ⁇ 100- It is set at 3000 ⁇ m, particularly preferably about 500-1500 ⁇ m. If the hole diameter of the orifice 8 is smaller than about 50 ⁇ m, the film forming speed of the thin film deposited on the substrate 2 becomes practically insufficient, and if the hole diameter of the orifice 8 is larger than about 5000 m, the vaporizer 9 It becomes impossible to keep the vapor pressure of the solid raw material 10 constant.
- a plurality of orifices may be provided in consideration of the volume of the vaporizer 9, the hole diameter of the orifice 8, the film forming speed, the vapor pressure of the solid raw material 10, and the like.
- the orifice 8 provided in the vaporizer 9 is compared with the amount of the raw material gas generated by vaporization inside the vaporizer 9. Since the amount of raw material gas supplied to the reaction chamber 3 through the reactor is almost negligible, the inside of the vaporizer 9 is always kept in an equilibrium state, and the amount of vaporized solid raw material 10 depends on the surface area of the raw material. Since it is substantially determined by the vapor pressure of the raw material without being performed, the supply of the raw material gas to the reaction chamber 3 is performed stably for a long time.
- a raw material vaporizer 9 for a metal organic chemical vapor deposition apparatus wherein (i) a filling port 14 for filling a liquid raw material 13, When the solid raw material 10 remaining after the solvent contained in the liquid raw material 13 is removed is vaporized, the pore size is set so that the vapor pressure of the solid raw material 10 in the vaporizer 9 is kept substantially constant.
- Orifice 8 having an orifice 8 and (iii) a heater 7 for heating.
- a filling port 14 provided in the vaporizer 9 is connected to a pipe 11 communicating with a liquid source, and the liquid source 13 is filled into the vaporizer 9 through the filling port 14.
- the diameter of the filling port 14 is not particularly limited, in the case of a commonly used vaporizer 9 (volume: about 10-lOOcc), it is usually about 18 mm, preferably about 2-6 mm, and particularly preferably about 2-6 mm. 3-4 mm. If desired, a plurality of filling ports may be provided depending on the volume of the vaporizer 9 to be used, the size of the diameter of the filling port 14, the continuous use time of the vaporizer 9, and the like.
- the liquid raw material 13 introduced into the vaporizer 9 through the filling port 14 is subjected to a heating treatment by a heating heater 7 arranged at the bottom of the vaporizer 9, whereby the liquid raw material 13 is heated.
- the solvent contained in the feed 13 is removed by evaporation, and the solid raw material 10 remains at the bottom of the vaporizer 9. .
- the remaining solid raw material 10 is heated to an appropriate temperature using a heater 7 and vaporized to generate a raw material gas inside the vaporizer 9.
- the vaporizer 9 includes an orifice 8 having a hole diameter large enough to keep the vapor pressure of the solid raw material in the vaporizer substantially constant when the residual solid raw material 10 is vaporized. Will be arranged. Regarding the configuration of the orifice 8, the above description in the case of the vaporizer according to the first aspect of the present invention is applied as it is.
- a filling port 14 for filling the liquid raw material 13 and (ii) a vaporization of the solid raw material 10 remaining after removing the solvent contained in the liquid raw material 13,
- the inside of the vaporizer 9 is kept in a normal equilibrium state, and the force of vaporization of the solid raw material 10 is not affected by the surface area of the raw material and the like.
- the pressure of the source gas to the reaction chamber 3 Performed time Niwata connexion stably.
- a method for supplying a source gas for an organometallic chemical vapor deposition apparatus wherein the orifice 8 disposed in the vaporizer 9, Wherein the source gas is supplied to an organometallic chemical vapor deposition system through an orifice 8 having a pore size large enough to keep the vapor pressure of the source present at a substantially constant level.
- a source gas supply method is provided.
- the organometallic chemical vapor deposition apparatus of the embodiment shown in FIG. 1 comprises (i) a reaction chamber 3 containing a substrate 2 and a substrate heater 1, (ii) an exhaust system including a vacuum pump 5 ′, and (iii) Supply source of argon gas as carrier gas, carrier gas supply system including flow controller 16 and preheater 4, and (iv) supply source of oxygen gas as reaction gas, flow controller 16 'and preheater 4' And a reaction gas supply system.
- the carrier gas, the reaction gas, and the raw material gas before reaching the substrate 2 are kept warm by the warming heater 12 attached to the lower region of the reaction chamber 3.
- a vaporizer 9 is connected to a lower region of the reaction chamber 3 in which the heat retaining heater 12 is mounted, and the lower region and the vaporizer are communicated via an orifice 8 provided in the vaporizer.
- the orifice 8 has such a diameter as to keep the vapor pressure of the solid raw material present in the vaporizer substantially constant.
- the above description in the case of the vaporizer according to the first aspect of the present invention is applied as it is.
- the gas is generated by vaporization inside the vaporizer 9.
- the amount of the source gas supplied to the reaction chamber 3 through the orifice 8 provided in the vaporizer 9 is almost negligible compared to the amount of the source gas to be vaporized.
- a method for supplying a source gas for an organometallic chemical vapor deposition apparatus having the following step (i)-(V):
- the liquid raw material 13 is prepared by dissolving, dispersing, suspending, or dissolving a solid raw material 10 which is a raw material of a thin film deposited on the substrate 2 installed inside the reaction chamber 3 in a solvent. It is prepared by emulsification, but the liquid raw material 13 is most preferably a solution.
- the concentration of the liquid raw material 13 is not particularly limited as long as it can be appropriately selected according to the type of the solid raw material 10, the type of the solvent, the filling efficiency of the raw material, and the like, but is usually about 0.1 to 5 molZ1, Preferably it is about 0.2-2 mol Zl, particularly preferably about 0.5-Imol Zl.
- the solvent used for preparing the liquid raw material 13 from the solid raw material may be appropriately selected in consideration of the solubility of the solid raw material and the cost and toxicity of the solvent, and is not particularly limited. Illustrative are: tetrahydrofuran, butyl acetate, ethylcyclohexane, toluene, xylene and tetraethylheptanedione.
- two or more such solvents may be used in combination.
- the liquid raw material 13 prepared as described above is introduced into a vaporizer 9 having an orifice 8 having a hole diameter large enough to keep the vapor pressure of the solid raw material 10 substantially constant.
- the mixture is introduced through a pipe 11 connected to the gasifier 9, and then the solvent contained in the liquid raw material 13 is evaporated from the vaporizer 9 in the next step.
- valve 6 communicating with the liquid material introduction pipe 11 is opened, and the valve 6 'communicating with the pipe 11 and the vacuum pump 5 is closed.
- the pressure inside the reaction chamber (film formation chamber) 3 is set to be higher than the pressure inside the vaporizer 9, so that the solvent from the vaporizer 9 to the reaction chamber 3 Gas intrusion can be suppressed.
- a method for supplying a source gas for an organometallic chemical vapor deposition apparatus is described.
- the configuration of the orifice 8 the above description in the case of the vaporizer according to the first aspect of the present invention is applied as it is.
- the solid raw material 10 remaining in the vaporizer 9 is heated and sublimated to generate a raw material gas in the vaporizer.
- the source gas is then supplied to the metal organic chemical vapor deposition system through the orifice 8.
- the film forming conditions are set as follows. That is, the temperature of the substrate 2 is set to a predetermined temperature (for example, 500 ° C.) using the substrate heater 1, and the pressure inside the reaction chamber 3 is set to a predetermined pressure (eg, 275 Pa), and the flow rate of argon as a carrier gas of the raw material gas generated by sublimation of the solid raw material 10 is adjusted to a predetermined flow rate (for example, 14 scc Zm) using the flow rate regulator 16, and the reaction gas as the reaction gas is adjusted.
- a predetermined temperature for example, 500 ° C.
- a predetermined pressure eg, 275 Pa
- the flow rate of argon as a carrier gas of the raw material gas generated by sublimation of the solid raw material 10 is adjusted to a predetermined flow rate (for example, 14 scc Zm) using the flow rate regulator 16, and the reaction gas as the reaction gas is adjusted.
- the flow rate of the oxygen gas is adjusted to a predetermined flow rate (for example, 100 scc / m) using the flow rate regulator 16 ′, and the temperature inside the gasifier 9 is specified using the heating heater 7. Temperature (eg, 150 ° C, 155 ° C or 160 ° C). Under such film forming conditions, a desired thin film (for example, a TiO thin film) is formed on the substrate 2.
- the amount of the source gas generated by vaporization inside the vaporizer 9 is reduced. Since the amount of raw material gas supplied to the reaction chamber 3 through the orifice 8 provided is almost negligible, the inside of the vaporizer 9 is always kept in an equilibrium state, and the amount of vaporized solid raw material 10 is Since it is almost determined by the vapor pressure of the raw material without being influenced by the surface area of the raw material, the supply of the raw material gas to the reaction chamber 3 is performed stably for a long time.
- the solid raw material after converting the solid raw material into a liquid state using a solvent, the solid raw material is connected to the inside of the vaporizer 9 through a pipe 11 of external force without opening the vaporizer 9. Before or after film formation, only the solvent in the liquid raw material 13 is evaporated and removed, so that a raw material gas is always generated in the vaporizer 9 as well as a fresh solid raw material power. Is continuously supplied to the metal organic chemical vapor deposition system through the orifice 8.
- a TiO thin film was prepared using the metal organic chemical vapor deposition apparatus shown in FIG.
- Titanium isopropoxide Sibi Varo yl methane (2. 66 g) was a raw material solution was prepared by dissolving in tetrahydrofuran (10 ml) (raw material concentration: 0. 5mol / l) 0 also compost the TiO thin film
- a silicon wafer was used as the substrate 2 for stacking.
- This raw material solution was introduced into the vaporizer 9 through the pipe 11.
- the raw material solution was heated at 80 ° C. for 15 minutes using the heater 7 while evacuating the gasifier using the vacuum pump 5 to remove tetrahydrofuran from the vaporizer by evaporation.
- the operation procedure in this case was performed according to the procedure described above with reference to FIG. Next, the temperature of the substrate 2 was set to 500 ° C using the substrate heater 1, the pressure inside the reaction chamber 3 was adjusted to 275 Pa using the vacuum pump 5 ', and the raw material generated by sublimation of the solid raw material 10
- the flow rate of argon as a carrier gas of gas was adjusted to 14 scccZm using a flow regulator 16, and the flow rate of oxygen gas as a reaction gas was adjusted to 100 scccZm using a flow regulator 16 ′.
- the temperature inside the dagger 9 was set to 150 ° C., 155 ° C. or 160 ° C. using the heater 7 for heating.
- a TiO thin film is formed on a substrate, and the thickness of the TiO thin film is changed.
- FIG. 3 shows that the rate of deposition of the source gas on the substrate can be controlled by appropriately selecting the temperature of the vaporizer 9.
- the operation rate of the production process is a very important requirement in terms of product cost and the like.
- the material vaporizer for the metal organic chemical vapor deposition apparatus according to the present invention, it is necessary to ensure the stable vaporization of the important material for producing a uniform thin film, and to increase the operation rate of the apparatus. Continuous or sequential supply of critical raw materials The salary becomes possible. Therefore, by incorporating the vaporizer according to the present invention into the mass production process of the thin film by the metalorganic chemical vapor deposition method, the operation rate of the mass production process is greatly increased, and this is combined with the stable vaporization of the raw material. As a result, it is possible to provide uniform thin-film products at low cost.
- the raw material vaporizer for the metal organic chemical vapor deposition apparatus can be generally applied to the production of a thin film by the metal organic chemical vapor deposition method.
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JP2004-070656 | 2004-03-12 | ||
JP2004070656A JP4595356B2 (ja) | 2004-03-12 | 2004-03-12 | 有機金属化学気相堆積装置用原料気化器 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114402093A (zh) * | 2019-09-24 | 2022-04-26 | 东京毅力科创株式会社 | 原料供给装置和原料供给方法 |
CN114402092A (zh) * | 2019-09-24 | 2022-04-26 | 东京毅力科创株式会社 | 原料供给装置和原料供给方法 |
CN116018426A (zh) * | 2020-09-15 | 2023-04-25 | 东京毅力科创株式会社 | 原料供给装置和原料供给方法 |
Families Citing this family (4)
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JP5273936B2 (ja) * | 2007-04-02 | 2013-08-28 | 株式会社日立国際電気 | 基板処理装置および半導体装置の製造方法 |
JP5461786B2 (ja) | 2008-04-01 | 2014-04-02 | 株式会社フジキン | 気化器を備えたガス供給装置 |
US20230151486A1 (en) * | 2020-03-17 | 2023-05-18 | Tokyo Electron Limited | Raw material supply system |
JP2022007656A (ja) * | 2020-06-26 | 2022-01-13 | 東京エレクトロン株式会社 | 洗浄方法、洗浄機構、および原料供給システム |
Citations (2)
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JPH10298768A (ja) * | 1997-01-24 | 1998-11-10 | Applied Materials Inc | チタン層を堆積するための、高温、高堆積率の方法及び装置 |
JP2003332243A (ja) * | 2002-05-13 | 2003-11-21 | Japan Pionics Co Ltd | 気化器及び気化供給装置 |
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JP2003282556A (ja) * | 2002-03-25 | 2003-10-03 | Canon Inc | 固体有機金属原料供給装置および供給方法 |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH10298768A (ja) * | 1997-01-24 | 1998-11-10 | Applied Materials Inc | チタン層を堆積するための、高温、高堆積率の方法及び装置 |
JP2003332243A (ja) * | 2002-05-13 | 2003-11-21 | Japan Pionics Co Ltd | 気化器及び気化供給装置 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114402093A (zh) * | 2019-09-24 | 2022-04-26 | 东京毅力科创株式会社 | 原料供给装置和原料供给方法 |
CN114402092A (zh) * | 2019-09-24 | 2022-04-26 | 东京毅力科创株式会社 | 原料供给装置和原料供给方法 |
US11965242B2 (en) | 2019-09-24 | 2024-04-23 | Tokyo Electron Limited | Raw material supply apparatus and raw material supply method |
CN116018426A (zh) * | 2020-09-15 | 2023-04-25 | 东京毅力科创株式会社 | 原料供给装置和原料供给方法 |
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JP2005256107A (ja) | 2005-09-22 |
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