WO2016147763A1 - オゾンガス発生装置およびオゾンガス発生装置の製造方法 - Google Patents
オゾンガス発生装置およびオゾンガス発生装置の製造方法 Download PDFInfo
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- WO2016147763A1 WO2016147763A1 PCT/JP2016/053935 JP2016053935W WO2016147763A1 WO 2016147763 A1 WO2016147763 A1 WO 2016147763A1 JP 2016053935 W JP2016053935 W JP 2016053935W WO 2016147763 A1 WO2016147763 A1 WO 2016147763A1
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- titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/10—Preparation of ozone
- C01B13/11—Preparation of ozone by electric discharge
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/10—Preparation of ozone
- C01B13/11—Preparation of ozone by electric discharge
- C01B13/115—Preparation of ozone by electric discharge characterised by the electrical circuits producing the electrical discharge
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/10—Dischargers used for production of ozone
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/30—Dielectrics used in the electrical dischargers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2201/00—Preparation of ozone by electrical discharge
- C01B2201/30—Dielectrics used in the electrical dischargers
- C01B2201/34—Composition of the dielectrics
Definitions
- the present invention relates to an ozone gas generator and a method for manufacturing the ozone gas generator.
- an ozone gas generator is known.
- Such an ozone gas generator is disclosed, for example, in International Publication No. WO2011 / 039971.
- the international publication WO2011 / 039971 discloses an ozone gas generator that generates high-concentration ozone gas without adding other gases such as nitrogen gas to the raw material gas.
- the ozone gas generator of International Publication WO2011 / 039971 is arranged on a pair of dielectrics arranged at a predetermined interval so as to face each other and on the outside of the pair of dielectrics.
- the functional film of the ozone gas generator is a first metal oxide of one or two metals selected from niobium, tantalum, molybdenum, and chromium, and one or two selected from titanium, tungsten, zinc, and iron.
- a second metal oxide of a type of metal is a first metal oxide of one or two metals selected from niobium, tantalum, molybdenum, and chromium, and one or two selected from titanium, tungsten, zinc, and iron.
- the ozone generation performance may vary depending on the structure of the metal oxide on the surface of the functional film. Therefore, an ozone gas generator that can generate high-concentration ozone gas more stably without adding other gases such as nitrogen gas to the source gas is desired.
- the present invention has been made to solve the above-described problems, and one object of the present invention is to increase the concentration of ozone gas without adding other gases such as nitrogen gas to the raw material gas.
- An object of the present invention is to provide an ozone gas generator that can be stably generated and a method for manufacturing the ozone gas generator.
- the functional film provided on at least one side of the opposing surfaces of the pair of dielectrics includes a crystalline compound of titanium oxide and niobium oxide. It has been found that the high-concentration ozone gas can be generated more stably without adding other gases such as nitrogen gas to the raw material gas. That is, the ozone gas generator according to the first aspect of the present invention includes a pair of electrodes arranged at a predetermined interval so as to face each other, and a pair of dielectrics provided on surfaces facing each other of the pair of electrodes. And a functional film provided on at least one side of a pair of dielectrics facing each other, the functional film including a crystalline compound of titanium oxide and niobium oxide.
- the functional film contains a crystalline compound of titanium oxide and niobium oxide, so that other gases such as nitrogen gas can be added to the source gas. Therefore, when generating ozone gas, variation in ozone generation performance can be suppressed. Thereby, high concentration ozone gas can be more stably generated, without adding other gas, such as nitrogen gas, to source gas.
- the functional film of titanium oxide and niobium oxide crystalline compound has Nb 2 O 5 in a molar number of 0.1 to 6 times that of TiO 2. It is produced by titanium oxide and niobium oxide. With this configuration, crystals such as TiNb 2 O 7 and Ti 2 Nb 10 O 29 are formed from titanium oxide and niobium oxide in which Nb 2 O 5 is 0.1 to 6 times that of TiO 2 in terms of moles. System compounds can be produced.
- the functional film further includes a solid solution of titanium oxide. If comprised in this way, high concentration ozone gas can be more stably generated by the effect
- the crystalline compound of titanium oxide and niobium oxide of the functional film includes at least one of TiNb 2 O 7 and Ti 2 Nb 10 O 29 .
- TiNb by the action of the crystal system of the compound containing at least one of the 2 O 7 and Ti 2 Nb 10 O 29, can be generated more stably a high concentration of ozone gas.
- the manufacturing method of the ozone gas generator according to the second aspect of the present invention is opposite to the step of producing a crystalline compound of titanium oxide and niobium oxide by heating titanium oxide and niobium oxide at 1000 ° C. or higher.
- a step of providing a pair of electrodes disposed at a predetermined interval, a step of providing a pair of dielectrics on the surfaces of the pair of electrodes facing each other, and at least one side of the surfaces of the pair of dielectrics facing each other And a step of providing a functional film containing a crystalline compound of titanium oxide and niobium oxide.
- the ozone generation performance it is possible to manufacture an ozone gas generator capable of suppressing the variation of the above. Thereby, the ozone gas generator which can generate high concentration ozone gas more stably can be manufactured, without adding other gas, such as nitrogen gas, to source gas.
- the step of generating a crystalline compound of titanium oxide and niobium oxide includes the step of mixing titanium oxide and niobium oxide, and the mixed titanium oxide and oxide.
- the method includes a step of heating niobium at 1000 ° C. or higher to produce a crystalline compound, and a step of pulverizing the produced compound. If comprised in this way, the crystalline compound of a titanium oxide and niobium oxide can be easily produced
- the step of providing the functional film is a step of applying the generated titanium oxide and niobium oxide crystal-based compound and a solid solution of titanium oxide to a dielectric. including. If constituted in this way, an ozone gas generating device capable of generating high-concentration ozone gas more stably by the action of both a titanium oxide and niobium oxide crystalline compound and a solid solution of titanium oxide is manufactured. can do.
- high-concentration ozone gas can be generated more stably without adding other gases such as nitrogen gas to the source gas.
- FIG. 3 is a diagram illustrating a phase diagram of TiO 2 —Nb 2 O 5 . It is the figure which showed the manufacturing process of the ozone gas production
- the ozone gas generator 100 is configured to generate ozone used in a semiconductor manufacturing process. That is, the ozone gas generator 100 uses high-purity oxygen gas (for example, an oxygen concentration of 99.9% or more) to suppress the concentration of impurities (substances other than ozone and oxygen) in the generated ozone gas. It is configured as follows. As shown in FIG. 1, the ozone gas generation apparatus 100 includes an ozone gas generation unit 1, a power source 2, and a control unit 3.
- high-purity oxygen gas for example, an oxygen concentration of 99.9% or more
- the ozone gas generation unit 1 is configured to be supplied with high-purity oxygen gas (O 2 ) as a raw material and generate high-concentration ozone gas (O 3 ). Note that no other gas such as nitrogen is added to the high-purity oxygen gas of the raw material.
- the ozone gas generator 1 includes a discharge cell 10. As shown in FIG. 2, the discharge cell 10 includes a pair of electrodes 11, a pair of dielectric bodies 12, and a pair of functional films 13.
- the ozone gas generation unit 1 is provided with a plurality of discharge cells 10 (not shown).
- the plurality of discharge cells 10 have the same configuration.
- the discharge cell 10 is configured to perform silent discharge when applied by the power source 2. Between each of the plurality of discharge cells 10, a flow path through which cooling water passes is provided.
- the pair of electrodes 11 are respectively arranged outside the pair of dielectrics 12 and are configured to generate a discharge between the pair of dielectrics 12. That is, the power source 2 is connected to the pair of electrodes 11.
- the pair of electrodes 11 is supplied with high-frequency high-voltage power from the power source 2.
- the pair of electrodes 11 are each formed in a film shape. Further, the pair of electrodes 11 are disposed so as to face each other.
- the pair of dielectrics 12 are arranged at a predetermined interval so as to face each other.
- Each of the pair of dielectrics 12 is made of alumina (ceramic).
- the pair of dielectrics 12 are each formed in a plate shape.
- Each of the pair of dielectrics 12 has a larger area than the electrodes 11 and is disposed so as to cover the inner surfaces (opposite surfaces) of the pair of electrodes 11.
- the dielectric 12 has a plate thickness of about 0.05 mm or more and about 1 mm or less, for example. In order to obtain stable performance, the dielectric 12 preferably has a plate thickness of about 0.1 mm or more and about 0.3 mm or less.
- the pair of dielectrics 12 are disposed, for example, with an interval of about 30 ⁇ m or more and about 100 ⁇ m or less. Further, the raw material oxygen gas is supplied to the gap between the pair of dielectrics 12.
- the pair of functional films 13 are provided on the surfaces of the pair of dielectric bodies 12 facing each other. That is, the functional film 13 is disposed so as to be in contact with the gap (discharged space) between the pair of dielectrics 12.
- the dielectric 12 includes a crystalline compound of titanium oxide and niobium oxide.
- the crystalline compound of titanium oxide and niobium oxide in the functional film 13 is produced by titanium oxide and niobium oxide in which Nb 2 O 5 is about 0.1 to 6 times that of TiO 2 in terms of moles.
- the crystalline compound of titanium oxide and niobium oxide in the functional film 13 is generated by titanium oxide and niobium oxide in which Nb 2 O 5 is greater than about 1 time and less than about 2.5 times that of TiO 2 in terms of moles.
- the functional film 13 further includes a solid solution of titanium oxide.
- TiO 2 and Nb 2 O about 85.7% mol% of Nb 2 O 5 is more than about 9% of a mixture of 5 or less (When Nb 2 O 5 in mole number is about 0.1 to 6 times that of TiO 2 ), by firing (heating), at least of TiNb 2 O 7 and Ti 2 Nb 10 O 29 One is generated. Specifically, when the mole percentage of Nb 2 O 5 is about 9% or more and less than about 50%, a solid solution of TiNb 2 O 7 and TiO 2 is generated.
- Nb 2 O 5 in moles to about greater than the molar percent to about 50 percent of Nb 2 O 5 of about 2.5 times or more and less than about 1 times the TiO 2 (a mixture of TiO 2 and Nb 2 O 5
- TiO 2 a mixture of TiO 2 and Nb 2 O 5
- the power source 2 is configured to supply AC power to the pair of electrodes 11 of the ozone gas generation unit 1.
- the power supply 2 is configured to supply high-frequency power resonated by an LC circuit or the like.
- the control unit 3 is configured to control each unit of the ozone gas generator 100.
- the control unit 3 controls the power supply 2 to control the power supplied to the ozone gas generation unit 1.
- a predetermined proportion of titanium oxide (TiO 2 ) and niobium oxide (Nb 2 O 5 ) are mixed. Specifically, particulate TiO 2 and Nb 2 O 5 , a binder such as ethanol, and zirconia balls for mixing and pulverization are placed in a mill and mixed.
- the mixed titanium oxide (TiO 2 ) and niobium oxide (Nb 2 O 5 ) are fired (heated). Specifically, a mixture of particulate TiO 2 and Nb 2 O 5 is fired at a temperature of 1000 ° C. or higher in a furnace. Particulate TiO 2 and Nb 2 O 5 are fired under atmospheric pressure. Further, the particulate TiO 2 and Nb 2 O 5 are fired at a temperature of 1000 ° C. or higher and a temperature at which the particles do not dissolve (for example, about 1400 ° C.) or lower. Preferably, the baking is performed at a temperature of 1300 ° C. or higher and not melting (for example, about 1400 ° C.) or lower. As a result, a crystalline compound of titanium oxide and niobium oxide (at least one of TiNb 2 O 7 and Ti 2 Nb 10 O 29 ) is generated.
- the fired titanium oxide and niobium oxide crystalline compounds are cooled.
- the cooled titanium oxide and niobium oxide crystalline compounds are pulverized. Specifically, a crystalline compound of titanium oxide and niobium oxide, a binder such as ethanol, and zirconia balls for mixing and pulverization are put in a mill and pulverized. The crystalline compound of titanium oxide and niobium oxide is pulverized until the particle size is smaller than the particle size that can pass through a screen printing mesh used in a subsequent coating step. For example, a crystalline compound of titanium oxide and niobium oxide is pulverized until the particle size becomes 1000 nm or less.
- a crystalline compound of titanium oxide and niobium oxide, a solid solution (ss) of titanium oxide (TiO 2 ), glass and oil are mixed to form a paste.
- the paste containing a crystalline compound of titanium oxide and niobium oxide is adjusted to a viscosity capable of screen printing in a subsequent coating step. Specifically, the viscosity of the paste is adjusted by adjusting the amount of oil to be mixed. Thereby, the material of the functional film 13 is generated.
- the pasted functional film 13 material containing a crystalline compound of titanium oxide and niobium oxide and a solid solution of titanium oxide is applied to the dielectric 12 by screen printing.
- the functional film 13 is applied with a thickness of about 10 ⁇ m, for example.
- step S7 the applied paste is fired (heated) to fix the functional film 13 to the dielectric 12. Specifically, firing is performed for a predetermined time at a temperature at which the glass in the paste melts (for example, about 850 ° C.). Thereafter, the functional film 13 is fixed on the dielectric 12 by cooling.
- the pair of dielectrics 12 each having the functional film 13 formed thereon are joined at a predetermined interval.
- a pair of electrodes 11 that generate discharge between the pair of dielectrics 12 are provided on the outer sides of the pair of dielectrics 12.
- a gap forming rib is disposed on the first surface of the dielectric 12 (alumina substrate) on which the functional film 13 is provided.
- the electrode 11 is provided on the second surface of the dielectric 12 opposite to the functional film 12.
- the 1st surfaces (surface by the side of the functional film 12) of the dielectric material 12 are joined by a joining member via a rib.
- the joining member includes, for example, glass.
- firing is performed for a predetermined time at a temperature at which the glass melts (for example, about 850 ° C.).
- a temperature at which the glass melts for example, about 850 ° C.
- it cools and several pairs of dielectrics 12 are joined.
- the several discharge cell 10 is assembled.
- the flow path which lets a cooling water pass between each of the some discharge cells 10 is provided, and the ozone gas production
- ozone gas is generated without adding other gases such as nitrogen gas to the source gas. Moreover, the variation in ozone generation performance can be suppressed. Thereby, high concentration ozone gas can be more stably generated, without adding other gas, such as nitrogen gas, to source gas.
- the crystalline compound of titanium oxide and niobium oxide of the functional film 13 has a Nb 2 O 5 molar ratio of about 0.1 to about 6 times that of TiO 2. It is produced by titanium oxide and niobium oxide. Thereby, from titanium oxide and niobium oxide in which Nb 2 O 5 is about 0.1 to 6 times that of TiO 2 in terms of moles, a crystal system such as TiNb 2 O 7 and Ti 2 Nb 10 O 29 can be obtained. Compounds can be produced.
- the functional film 13 includes a solid solution of titanium oxide.
- high concentration ozone gas can be more stably generated by the action of both the titanium oxide and niobium oxide crystalline compounds and the solid solution of titanium oxide.
- the crystalline compound of titanium oxide and niobium oxide of the functional film 13 includes at least one of TiNb 2 O 7 and Ti 2 Nb 10 O 29 .
- high-concentration ozone gas can be generated more stably by the action of a crystalline compound containing at least one of TiNb 2 O 7 and Ti 2 Nb 10 O 29 .
- the functional film according to the comparative example has a variation in ozone generation performance.
- a functional film may be provided on at least one side of the pair of dielectrics.
- the ozone gas generator may generate ozone gas by discharge other than silent discharge.
- the ozone gas generator may be configured to generate ozone gas by creeping discharge.
- the functional film is formed by applying the functional film material to the dielectric by screen printing.
- the present invention is not limited to this.
- the functional film may be formed on the dielectric by sputtering. Further, the functional film may be formed by applying a functional film material to the dielectric by a method other than screen printing.
- the dielectric is made of alumina.
- the present invention is not limited to this.
- the dielectric may be formed of a ceramic other than alumina or may be formed of a material other than ceramic.
- the ozone gas generator may be provided with one discharge cell.
- the ozone gas generator of the present invention may be used by being incorporated in an apparatus such as an ozone water production apparatus.
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Abstract
Description
図1を参照して、本発明の一実施形態によるオゾンガス発生装置100の構成について説明する。
図4を参照して、オゾンガス発生装置100(オゾンガス生成部1)の製造方法について説明する。
本実施形態では、以下のような効果を得ることができる。
次に、図5を参照して、本実施形態によるオゾンガス発生装置100の機能膜13の評価を行った実験結果について説明する。
なお、今回開示された実施形態および実施例は、すべての点で例示であって制限的なものではないと考えられるべきである。本発明の範囲は、上記した実施形態および実施例の説明ではなく特許請求の範囲によって示され、さらに特許請求の範囲と均等の意味および範囲内でのすべての変更(変形例)が含まれる。
12 誘電体
13 機能膜
100 オゾンガス発生装置
Claims (7)
- 互いに対向するように所定の間隔を隔てて配置された一対の電極と、
前記一対の電極の互いに対向する面にそれぞれ設けられた一対の誘電体と、
前記一対の誘電体の互いに対向する面の少なくとも一方側に設けられた機能膜とを備え、
前記機能膜は、酸化チタンおよび酸化ニオブの結晶系の化合物を含む、オゾンガス発生装置。 - 前記機能膜の酸化チタンおよび酸化ニオブの結晶系の化合物は、モル数においてNb2O5がTiO2の0.1倍以上6倍以下となる酸化チタンおよび酸化ニオブにより生成されている、請求項1に記載のオゾンガス発生装置。
- 前記機能膜は、酸化チタンの固溶体をさらに含む、請求項1または2に記載のオゾンガス発生装置。
- 前記機能膜の酸化チタンおよび酸化ニオブの結晶系の化合物は、TiNb2O7およびTi2Nb10O29のうち少なくとも一方を含む、請求項1~3のいずれか1項に記載のオゾンガス発生装置。
- 酸化チタンおよび酸化ニオブを1000℃以上で加熱することにより酸化チタンおよび酸化ニオブの結晶系の化合物を生成する工程と、
互いに対向するように所定の間隔を隔てて配置された一対の電極を設ける工程と、
前記一対の電極の互いに対向する面にそれぞれ一対の誘電体を設ける工程と、
前記一対の誘電体の互いに対向する面の少なくとも一方側に酸化チタンおよび酸化ニオブの結晶系の化合物を含む機能膜を設ける工程とを備える、オゾンガス発生装置の製造方法。 - 酸化チタンおよび酸化ニオブの結晶系の化合物を生成する工程は、酸化チタンおよび酸化ニオブを混合する工程と、混合した酸化チタンおよび酸化ニオブを1000℃以上で加熱して結晶系の化合物を生成する工程と、生成した化合物を粉砕する工程とを含む、請求項5に記載のオゾンガス発生装置の製造方法。
- 前記機能膜を設ける工程は、生成した酸化チタンおよび酸化ニオブの結晶系の化合物と、酸化チタンの固溶体とを前記誘電体に塗布する工程を含む、請求項5または6に記載のオゾンガス発生装置の製造方法。
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Application Number | Priority Date | Filing Date | Title |
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EP16764594.4A EP3272706B1 (en) | 2015-03-18 | 2016-02-10 | Ozone gas generator and method for manufacturing ozone gas generator |
KR1020177020512A KR101921915B1 (ko) | 2015-03-18 | 2016-02-10 | 오존 가스 발생 장치 및 오존 가스 발생 장치의 제조 방법 |
CN201680007700.0A CN107428529B (zh) | 2015-03-18 | 2016-02-10 | 臭氧气体产生装置及臭氧气体产生装置的制造方法 |
US15/546,848 US20180022607A1 (en) | 2015-03-18 | 2016-02-10 | Ozone Gas Generator and Method for Manufacturing Ozone Gas Generator |
FIEP16764594.4T FI3272706T3 (fi) | 2015-03-18 | 2016-02-10 | Otsonikaasugeneraattori ja menetelmä otsonikaasugeneraattorin valmistamiseksi |
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JPH1160207A (ja) * | 1997-08-20 | 1999-03-02 | Toshiba Corp | オゾン発生装置 |
JP2005320223A (ja) * | 2004-04-08 | 2005-11-17 | Mitsubishi Electric Corp | オゾン発生装置 |
WO2011039971A1 (ja) * | 2009-10-02 | 2011-04-07 | 住友精密工業株式会社 | オゾンガス発生装置及びその製造方法 |
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TW200528390A (en) * | 2004-02-25 | 2005-09-01 | Toshiba Mitsubishi Elec Inc | Apparatus and method of producing ozone gas |
JP5638746B2 (ja) * | 2008-08-20 | 2014-12-10 | 堺化学工業株式会社 | 有機物を熱分解するための触媒と方法と、そのような触媒を製造する方法 |
JP2011150908A (ja) * | 2010-01-22 | 2011-08-04 | Panasonic Corp | プラズマディスプレイパネルおよびプラズマディスプレイ装置 |
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Patent Citations (3)
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JPH1160207A (ja) * | 1997-08-20 | 1999-03-02 | Toshiba Corp | オゾン発生装置 |
JP2005320223A (ja) * | 2004-04-08 | 2005-11-17 | Mitsubishi Electric Corp | オゾン発生装置 |
WO2011039971A1 (ja) * | 2009-10-02 | 2011-04-07 | 住友精密工業株式会社 | オゾンガス発生装置及びその製造方法 |
Non-Patent Citations (1)
Title |
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CN107428529B (zh) | 2020-09-25 |
EP3272706B1 (en) | 2022-12-07 |
KR20170100592A (ko) | 2017-09-04 |
EP3272706A4 (en) | 2018-08-29 |
TW201637996A (zh) | 2016-11-01 |
TWI682893B (zh) | 2020-01-21 |
JP6534544B2 (ja) | 2019-06-26 |
KR101921915B1 (ko) | 2018-11-26 |
US20180022607A1 (en) | 2018-01-25 |
JP2016172676A (ja) | 2016-09-29 |
EP3272706A1 (en) | 2018-01-24 |
FI3272706T3 (fi) | 2023-03-23 |
CN107428529A (zh) | 2017-12-01 |
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