WO2007063987A1 - Procede de traitement/lavage avec des mousses de plasma dans de l’eau ultra-pure et appareil correspondant - Google Patents
Procede de traitement/lavage avec des mousses de plasma dans de l’eau ultra-pure et appareil correspondant Download PDFInfo
- Publication number
- WO2007063987A1 WO2007063987A1 PCT/JP2006/324099 JP2006324099W WO2007063987A1 WO 2007063987 A1 WO2007063987 A1 WO 2007063987A1 JP 2006324099 W JP2006324099 W JP 2006324099W WO 2007063987 A1 WO2007063987 A1 WO 2007063987A1
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- WIPO (PCT)
- Prior art keywords
- bubbles
- plasma
- processing
- ultrapure water
- extinction
- Prior art date
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Classifications
-
- 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
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- 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
- H01L21/67—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
- H01L21/67017—Apparatus for fluid treatment
- H01L21/67028—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like
- H01L21/6704—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing
- H01L21/67057—Apparatus for fluid treatment for cleaning followed by drying, rinsing, stripping, blasting or the like for wet cleaning or washing with the semiconductor substrates being dipped in baths or vessels
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/2475—Generating plasma using acoustic pressure discharges
Definitions
- the present invention relates to a processing / cleaning method and apparatus using ultrapure water plasma bubbles, and more specifically, the surface of a substrate such as metal or semiconductor can be processed or cleaned in an ultraclean environment.
- the present invention relates to a processing and cleaning method and apparatus using ultra pure water plasma bubbles.
- Patent Documents 1 and 2 irradiate ultrasonic waves in the liquid, or generate fine bubbles by using heating or decompression.
- a method of generating plasma in bubbles by continuously irradiating electromagnetic waves inside is proposed.
- a method of forming a silicon carbide film on the substrate surface by generating plasma in a liquid containing hydrocarbons to form a diamond film on the surface of the substrate or generating plasma in a liquid containing silicon. Is also proposed!
- Patent Document 3 as a processing method using only ultrapure water, only ultrapure water is used except for a small amount of inevitable impurities, and this is subjected to a hydroxyl group increasing treatment for increasing the ion product.
- An ultrapure material that is processed to remove or form an oxide film by chemical elution reaction or acid reaction with hydroxyl groups or hydroxyl ions, when the workpiece is immersed in ultrapure water with increased hydroxyl ion concentration.
- a processing method using hydroxyl groups in water has been proposed.
- Patent Document 4 discloses that a workpiece and a high-pressure nozzle are disposed at a predetermined interval in a machining tank that also has the power of ultrapure water, and a machining surface of the workpiece.
- An ion exchange material or a catalyst material for increasing hydroxide ions is provided around the tip of the high pressure nozzle facing the A voltage is applied with the high pressure nozzle as the cathode and the work piece as the anode to generate a high-speed shear flow of ultra pure water sprayed from the high pressure nozzle near the surface of the work piece.
- Ultrapure water that supplies the processed hydroxide ions to the surface of the workpiece and removes the workpiece or forms an oxide film by chemical dissolution reaction or oxidation reaction with hydroxide ions.
- a method of adding hydroxide ions in the interior has been proposed.
- Patent Document 1 Japanese Patent No. 3624238
- Patent Document 2 Japanese Patent No. 3624239
- Patent Document 3 Japanese Patent Laid-Open No. 10-58236
- Patent Document 4 Japanese Patent No. 3316461
- the present invention intends to solve the problem by generating plasma in ultrapure water and using the plasma to treat the surface of the object to be processed in an ultraclean environment. Processed
- the object is to provide a completely new processing / cleaning method and apparatus using ultra-pure water plasma bubbles that can be cleaned.
- the present invention provides ultra-pure water without impurities as micron or nano-sized plasma bubbles using liquid plasma as a means for processing metal or semiconductor objects to be processed with high precision.
- Ultra precision machining is performed by contacting the workpiece using the flow of water.
- the processing accuracy surface roughness of the workpiece after processing
- the processing accuracy depends on the size of the ultrapure water plasma bubbles. Therefore, if nano-sized ultrapure water plasma bubbles are used, nano-sized ultra-precision processing is possible.
- the present invention generates plasma bubbles by continuously and intensively irradiating ultrapure water with at least high-frequency electromagnetic waves, and the plasma bubbles or after the plasma is extinguished.
- Table of objects to be treated with bubbles or active radicals after bubbles disappeared in ultrapure water A processing / cleaning method using ultrapure water plasma bubbles, characterized in that it is supplied to the surface for processing or cleaning (claim 1).
- the present invention generates fine bubbles by irradiating ultrasonic waves in ultrapure water, and continuously and intensively irradiates high-frequency electromagnetic waves toward the bubbles to generate plasma in the bubbles.
- Processing with ultrapure water plasma bubbles that supply or process the plasma bubbles, or bubbles after plasma extinguishing or active radicals after bubble extinction are supplied to the surface of the object to be processed placed in ultrapure water.
- a cleaning method is provided (claim 2).
- the flow of ultrapure water is used as means for supplying the plasma bubbles, or the bubbles after the extinction of the plasma or the active radicals after the extinction of the bubbles to the surface of the object to be processed (Claim 3).
- the means for supplying the plasma bubbles, or the bubbles after the extinction of the plasma or the active radicals after the extinction of the bubbles to the surface of the object to be processed is an injection nozzle of ultra pure water, which is disposed in the ultra pure water.
- Ultrapure water is jetted from the jet nozzle toward the plasma bubbles to generate a flow of ultrapure water, and plasma bubbles or bubbles after the extinction of plasma or active radicals after the extinction of the bubbles are generated on the surface of the object to be processed.
- the present invention holds an object to be processed and an electromagnetic wave probe that generates plasma bubbles by continuously and intensively irradiating high-frequency electromagnetic waves in ultrapure water disposed in a processing chamber.
- An ultrapure water provided with a plasma bubble supply means for supplying the plasma bubbles or bubbles after the extinction of the plasma or active radicals after the extinction of the bubbles to the surface of the object to be processed held by the holder.
- a processing / cleaning device using plasma bubbles was constructed (claim 5).
- the present invention provides an ultrasonic generation horn that generates fine bubbles by irradiating ultrasonic waves in ultrapure water disposed in a processing chamber, and continuously and intensively irradiates high-frequency electromagnetic waves.
- An electromagnetic wave probe for generating plasma bubbles by irradiation and a holder for holding an object to be processed are arranged, and the plasma bubbles, bubbles after extinction of plasma or active radicals after extinction of bubbles are held in the holder.
- a processing / cleaning apparatus using ultrapure water plasma bubbles provided with plasma bubble supply means for supplying to the surface of the processed material was constructed (claim 6).
- a pressure adjusting means for adjusting the pressure in the processing chamber is provided. (Claim 7) It is preferable that a gas supply means for supplying gas into the processing chamber (Claim 8) is further supplied to the surface of the object to be processed and used for processing the surface. It is also preferable to provide plasma bubble discharging means for removing plasma bubbles, bubbles after plasma extinction or active radicals after bubble extinction (claim 9).
- the processing / cleaning method and apparatus using the ultrapure water plasma foam according to the present invention as described above are processed since clean ultrapure water used for cleaning in the final process is used in all conventional methods. There is no surface contamination. Therefore, the cleaning process using ultrapure water at the final stage, which was necessary in the conventional method, is not necessary. In addition, no harmful substances as etching agents are required, which is necessary in the conventional method, and it is not necessary to discard the solution or gas after processing. It can be said that the present invention is an environmentally friendly and efficient method.
- FIG. 1 shows a conceptual diagram of a processing / cleaning method using ultrapure water plasma bubbles according to the present invention.
- fine bubbles are locally generated in ultra pure water, and high frequency electromagnetic waves are continuously and intensively irradiated to the bubbles.
- irradiation with ultrasonic waves is the simplest and most efficient, but other means by local heating or reduced pressure can also be used.
- bubbles are generated only by concentrated irradiation of high-frequency electromagnetic waves.
- the plasma bubbles generated in this way are supplied to the surface of the object to be processed disposed in ultrapure water, and the surface is covered by the interaction with the plasma.
- Reference numeral 1 in FIG. 1 is an electromagnetic wave generator that generates high-frequency electromagnetic waves
- 2 is an electromagnetic wave probe that is electromagnetically connected to the electromagnetic wave generator 1 to irradiate high-frequency electromagnetic waves into ultrapure water.
- reference numeral 3 is an ultrasonic generator that generates ultrasonic waves
- 4 is an ultrasonic generator that is acoustically connected to the ultrasonic generator 3 to irradiate ultrasonic waves into ultrapure water. It is. Then, the ultrasonic generation horn 4 force ultrasonic wave is irradiated locally to make fine Bubbles are generated, and high-frequency electromagnetic waves are continuously emitted from the electromagnetic probe 2 toward the bubbles to generate plasma in the bubbles.
- gas such as water corresponding to the saturated vapor pressure of ultrapure water or oxygen dissolved in the ultrapure water is confined, and high-frequency electromagnetic wave irradiation is performed. It turns into plasma. It is confirmed that OH radicals, H atoms, and O atoms are generated in the plasma bubbles 5 generated here. Even if the plasma in the bubbles disappears, the active radicals are present in the bubbles or in the liquid depending on the lifetime, so that the force proceeds.
- the processing method of the present invention can be said to be an extremely efficient and rational processing method.
- the frequency of the electromagnetic wave generated by the electromagnetic wave generating device 1 is most easily absorbed by water molecules. 2. It is necessary to avoid 45 GHz, and in this embodiment, the range of 3 MHz to 1 GHz is used. In addition, the higher the frequency of the ultrasonic wave generated by the ultrasonic generator 3, the smaller the bubble size, but it is practically in the range of 10 kHz to 30 MHz. By the way, 20 kHz ultrasonic waves generate / z m size bubbles, and tens of MHz ultrasonic waves generate nm size bubbles. The smaller the bubbles, the higher the processing accuracy and the higher the processing speed.
- the plasma bubbles 5 generated in this way, or the bubbles after the extinction of the plasma or the active radicals after the extinction of the bubbles are supplied to the surface 7 of the object 6 to be processed.
- the flow of ultrapure water is used. Specifically, an injection nozzle 8 of ultrapure water is disposed in ultrapure water toward the region where the plasma bubbles 5 are generated, and the superposition of the plasma bubbles 5 from the injection nozzle 8 toward the plasma bubbles 5 is performed.
- the pure water is jetted to generate the flow of ultra pure water, and the plasma bubbles 5 or the bubbles after the extinction of the plasma or the active radicals after the extinction of the bubbles are supplied to the surface 7 of the workpiece 6 together with the ultra pure water.
- the plasma bubbles 5 that have reached the surface 7 of the workpiece 6 are supplied by supplying OH radicals, H atoms, and O atoms to the surface 7 and changing the surface atoms into volatile or water-soluble substances to be removed. .
- an appropriate plasma bubble discharging means that collects them by the bubble collecting means and discharges them outside the process area may be provided. I like it.
- FIG. 2 shows a conceptual diagram of the processing apparatus of the first embodiment of the present invention.
- a processing chamber 10 that can be sealed is filled with ultrapure water 11, and a flat plate-like object is formed at the lower end of a holder 12 that extends into the ultrapure water 11 from the upper surface side of the cache chamber 10.
- the surface 13 of the workpiece 13 is held to be horizontal, and the tip of the electromagnetic wave probe 15 raised from the lower surface side of the cabinet 10 is disposed immediately below the surface 14 of the workpiece 13;
- a port 17 communicating with the gas phase portion 16 in the processing chamber 10 is provided in the upper portion of the processing chamber 10.
- the inside of the processing chamber 10 can be depressurized by exhausting from the port 17, and conversely, the inside of the cache chamber 10 can be pressurized by pumping gas from the port 17. .
- reference numeral 18 indicates a plasma generation region, and 19 indicates a plasma bubble.
- the processing conditions are:
- Electromagnetic frequency 27. 12MHz
- Fig. 3 shows the result of measuring the processed surface of the Si wafer with a phase shift interference microscope. It can be seen that the Si wafer has an area of about 4 mm in diameter that is covered to a maximum depth of about 400 nm! .
- the processing speed of Si Wha is about 130nmZ. This processing speed is sufficiently high compared with plasma etching!
- Fig. 4 shows the result of measuring the processed surface of the Au vapor-deposited wafer with a stylus roughness meter.
- the Au vapor-deposited wafer is covered with a region with a diameter of about 2 mm up to a maximum depth of about 250 nm. You can see that The processing speed of Au evaporated wafer is about 80nmZ.
- Au is a very stable material, and it is a remarkable point that it is processed. Since Au has a very high redox potential and is known to ionize when reacted with a substance, it is thought that a strong acid-acidic substance is produced during the Karoe process.
- FIG. 5 shows a conceptual diagram of a machining apparatus according to the second embodiment of the present invention.
- this processing apparatus B the inside of the processing chamber 20 is filled with ultrapure water 21, a supply port 22 of ultrapure water is provided on one side wall of the cache chamber 20, and a discharge port 23 is provided on the opposite side wall.
- the ultrapure water is caused to flow by being discharged from the discharge port 23 while continuously supplying ultrapure water from the supply port 22.
- the electromagnetic probe 24 is raised from the lower surface side of the casing chamber 20 and the tip thereof is directed to the flowing portion of the ultrapure water, and the ultrasonic horn 25 is directed from the upper surface side to the flowing portion of the ultrapure water.
- the ultrasonic horn 25 is directed from the upper surface side to the flowing portion of the ultrapure water.
- the plasma bubbles 27 generated in the plasma generation region 26 are supplied to the surface 30 of the workpiece 29 held by the holder 28 installed on the downstream side as the ultrapure water flows.
- the surface 30 of the workpiece 29 is inclined with respect to the flow direction of the ultrapure water so as not to hinder the flow.
- the discharge port 23 serves as a plasma bubble discharge means for discharging unnecessary plasma bubbles 27 and substances removed from the surface 30 by the cache.
- (l) Au evaporated wafer This is one type of depositing 0: 10011111 on p-type 3 001) wafer and depositing Au on it about lOOnm.
- the processing conditions are:
- Liquid ultrapure water
- Liquid flow rate in the processing chamber 9.3LZ
- Incident high frequency electromagnetic wave Frequency 27.12MHz, input power: 350W, reflected power: 15W, incident ultrasonic wave: 21.7kHz, input power 15W,
- Figs. 7 (a), (b), and (c) show the results of measuring the processed surface with a stylus roughness meter when the processing time is 2 minutes, 4 minutes, and 10 minutes, respectively. .
- a schematic diagram of the processed sample is shown on the left side of each measurement result, and the measurement position on the stylus roughness meter is indicated by an arrow.
- Figure 7 (a) is processed to a depth of several tens of nm
- Figure 7 (b) is processed to a depth of about 50 nm
- Figure 7 (c) is a depth of about lOOnm (complete removal of the Au plating layer). Shown that it has been catered to.
- FIG. 8 shows an emission spectrum (pressure 2 OOhPa) of plasma in liquid generated using the above-mentioned cache apparatus A
- FIG. 9 shows that generated in the atmosphere using the processing apparatus B.
- the light emission spectrum is shown.
- the pressure is 200 hPa
- OH It is predicted that back bonds will break when dical and H atoms act on Si.
- O atoms are observed and few H atoms. Since O atoms are connected to acids, there is a possibility that Si processing does not proceed.
- the activated species generated by controlling the atmosphere can be selected to change the processing characteristics.
- FIG. 1 is a conceptual diagram for explaining the processing principle of the present invention.
- FIG. 2 is a conceptual cross-sectional view of the processing apparatus of the first embodiment.
- FIG. 3 is a graph showing a result of measuring a processed surface of a Si wafer covered with the processing apparatus of FIG. 2 using a phase shift interference microscope.
- FIG. 4 is a graph showing the results of measuring the processed surface of an Au-deposited wafer processed by the processing apparatus of FIG. 2 using a stylus roughness meter.
- FIG. 5 is a conceptual cross-sectional view of a processing apparatus according to a second embodiment.
- FIG. 6 is an observation result of a processed surface of an Au vapor-deposited wafer that is covered using the processing apparatus of FIG.
- FIG. 7 is a graph showing the results of measuring the machined surface with a stylus roughness meter when machining time is 2 minutes, 4 minutes, and 10 minutes.
- FIG. 8 is a graph showing an emission spectrum (pressure 200 h Pa) of in-liquid plasma generated using the processing apparatus of FIG. 2.
- FIG. 9 is a graph showing an emission spectrum generated in the open atmosphere using the processing apparatus of FIG.
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Abstract
Le problème à résoudre dans le cadre de la présente invention consiste à proposer un procédé assez nouveau de traitement/lavage d’un matériau avec des mousses de plasma dans de l’eau ultra-pure, lequel permet le traitement ou le lavage de la surface du matériau dans des environnements ultra-propres en utilisant le plasma produit dans de l’eau ultra-pure ; et un appareil correspondant. La solution proposée est la suivante : un matériau (6) à traiter est placé dans de l'eau ultra-pure. L'eau ultra-pure est irradiée par des ondes ultrasoniques de façon à produire de fines bulles d'air et, en même temps, est également irradiée par une onde électromagnétique à haute fréquence de manière continue se concentrant sur les bulles d'air de façon à produire de ce fait un plasma dans les bulles d'air. La surface (7) sur le matériau (6) peut être traitée ou lavée par l’intermédiaire des bulles d'air (5) ayant le plasma produit dans celles-ci, des bulles d'air produites après la rupture du plasma, ou des radicaux actifs produits après la rupture des bulles d'air sur la surface.
Priority Applications (1)
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JP2007548022A JPWO2007063987A1 (ja) | 2005-12-02 | 2006-12-01 | 超純水プラズマ泡による加工・洗浄方法及びその装置 |
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JP2005348734 | 2005-12-02 | ||
JP2005-348734 | 2005-12-02 |
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PCT/JP2006/324099 WO2007063987A1 (fr) | 2005-12-02 | 2006-12-01 | Procede de traitement/lavage avec des mousses de plasma dans de l’eau ultra-pure et appareil correspondant |
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Cited By (10)
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JP2009016433A (ja) * | 2007-07-02 | 2009-01-22 | Noritsu Koki Co Ltd | レジスト除去装置 |
WO2012011332A1 (fr) * | 2010-07-21 | 2012-01-26 | パナソニック株式会社 | Dispositif générateur de plasma et procédé de production de radical, dispositif de lavage et de nettoyage, et petit appareil électrique l'utilisant |
JP2012527757A (ja) * | 2009-05-18 | 2012-11-08 | アンスティテュ ポリテク二ック ドゥ グルノーブル | ガスの存在下で材料をエッチングする方法 |
JP2013234894A (ja) * | 2012-05-08 | 2013-11-21 | Mitsubishi Heavy Ind Ltd | 除染方法及び除染装置 |
US9339572B2 (en) | 2013-03-15 | 2016-05-17 | EP Technologies LLC | Methods and solutions for killing or deactivating spores |
JP2016107165A (ja) * | 2014-12-02 | 2016-06-20 | 富士機械製造株式会社 | 洗浄方法、および洗浄装置 |
WO2017055002A1 (fr) * | 2015-09-30 | 2017-04-06 | Siemens Aktiengesellschaft | Procédé de nettoyage de turbines à vapeur au moyen de vapeur humide activée |
US10692704B2 (en) | 2016-11-10 | 2020-06-23 | Gojo Industries Inc. | Methods and systems for generating plasma activated liquid |
US10897894B2 (en) | 2015-08-31 | 2021-01-26 | Gojo Industries, Inc. | Methods of and system for generating antimicrobial wipes |
US11123446B2 (en) | 2015-07-28 | 2021-09-21 | Gojo Industries, Inc. | Scrubbing device for cleaning, sanitizing or disinfecting |
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JP2009016433A (ja) * | 2007-07-02 | 2009-01-22 | Noritsu Koki Co Ltd | レジスト除去装置 |
JP2012527757A (ja) * | 2009-05-18 | 2012-11-08 | アンスティテュ ポリテク二ック ドゥ グルノーブル | ガスの存在下で材料をエッチングする方法 |
WO2012011332A1 (fr) * | 2010-07-21 | 2012-01-26 | パナソニック株式会社 | Dispositif générateur de plasma et procédé de production de radical, dispositif de lavage et de nettoyage, et petit appareil électrique l'utilisant |
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JP2013234894A (ja) * | 2012-05-08 | 2013-11-21 | Mitsubishi Heavy Ind Ltd | 除染方法及び除染装置 |
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