WO2017150212A1 - Procédé de production de film d'oxyde d'aluminium et matériau de départ de production pour film d'oxyde d'aluminium - Google Patents

Procédé de production de film d'oxyde d'aluminium et matériau de départ de production pour film d'oxyde d'aluminium Download PDF

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WO2017150212A1
WO2017150212A1 PCT/JP2017/005852 JP2017005852W WO2017150212A1 WO 2017150212 A1 WO2017150212 A1 WO 2017150212A1 JP 2017005852 W JP2017005852 W JP 2017005852W WO 2017150212 A1 WO2017150212 A1 WO 2017150212A1
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aluminum oxide
oxide film
aluminum
producing
compound
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PCT/JP2017/005852
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Japanese (ja)
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白井　昌志
央 二瓶
貴匡 宮崎
純一 向
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宇部興産株式会社
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic System
    • C07F5/06—Aluminium compounds
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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

Definitions

  • the present invention relates to a method for producing an aluminum oxide film on a film formation target and a raw material for producing an aluminum oxide film.
  • an aluminum oxide film is known as a film useful as a gate insulating film or the like, and is widely applied in the semiconductor field. Therefore, in recent years, higher quality aluminum oxide films are being sought. For this reason, an aluminum compound (raw material for producing an aluminum oxide film) suitable for producing a high quality aluminum oxide film has been studied (see, for example, Patent Documents 1 to 3 and Non-Patent Document 3).
  • Patent Document 4 discloses an alkylaluminum dihalide compound as a polymerization catalyst.
  • Non-Patent Document 1 and Non-Patent Document 2 disclose measurement examples and synthesis examples of alkylaluminum dihalide compounds.
  • Non-Patent Document 1 Non-Patent Document 2 and Patent Document 4 have not described that the alkylaluminum dihalide compound is useful as a raw material for producing an aluminum oxide film.
  • Non-Patent Document 3 describes the production of an aluminum oxide film by a chemical vapor deposition method (hereinafter referred to as "CVD method"), but other film formation methods and film formation There were no studies on temperature etc.
  • CVD method chemical vapor deposition method
  • the alkylaluminum dihalide compound since the alkylaluminum dihalide compound is generally known to be self-combustible, it is difficult to handle and is not preferable as a raw material for producing an aluminum oxide film. Furthermore, when impurities, such as aluminum chloride and aluminum carbide, are also mixed at the time of film formation, it was not preferable in applications such as semiconductors. Therefore, the obtained aluminum oxide film needs to be chemically pure. Furthermore, in applications such as semiconductors, the thickness of the aluminum oxide film needs to be uniform.
  • the main object of the present invention is to produce a high quality aluminum oxide film by an industrially suitable method and to provide a raw material for producing an aluminum oxide film.
  • high quality indicates that the purity is high chemically and that the thickness of the obtained aluminum oxide film is uniform in the same film.
  • an aluminum compound represented by the following general formula (1) is supplied onto a film formation target heated to 300 to 550 ° C. to oxidize the aluminum oxide film. Form.
  • R represents a linear alkyl group having 1 to 6 carbon atoms
  • X represents a halogen group. Two X may be the same or different
  • the raw material for producing an aluminum oxide film according to the present invention comprises an aluminum compound represented by the following general formula (1).
  • R represents a linear alkyl group having 1 to 6 carbon atoms
  • X represents a halogen group. Two X may be the same or different
  • the present invention it is possible to provide a method for producing an aluminum oxide film capable of producing a high quality aluminum oxide film, and a raw material for producing an aluminum oxide film.
  • an aluminum compound represented by the following general formula (1) is supplied onto a film formation target heated to 300 ° C. to 550 ° C. to oxidize the aluminum oxide film. It is characterized by forming.
  • R represents a linear alkyl group having 1 to 6 carbon atoms
  • X represents a halogen group. Two X may be the same or different
  • the aluminum compound used in the method for producing an aluminum oxide film of the present invention is an alkylaluminum dihalide compound represented by the above general formula (1).
  • R in the general formula (1) is a linear alkyl group having 1 to 6 carbon atoms, preferably a linear alkyl group having 1 to 3 carbon atoms.
  • R include a methyl group, an ethyl group, an n-propyl group, an n-butyl group, an n-pentyl group and an n-hexyl group. Among them, a methyl group and an ethyl group are preferable, and an ethyl group is more preferable.
  • the n-propyl group means a linear propyl group, and the same applies to other alkyl groups.
  • X in the general formula (1) is a halogen group, and examples thereof include a chloro group, a bromo group and an iodo group. Among them, chloro group is preferable.
  • two X's may be the same or different, but are preferably the same.
  • Preferred specific examples of the aluminum compound used in the method for producing an aluminum oxide film of the present invention include compounds represented by the following formulas (2) to (7). Among them, compounds represented by the following formulas (2) and (3) are preferable, and compounds represented by the following formula (3) are more preferably used.
  • Me, Et, n Pr, n Bu, n Pen, and n Hex are each methyl group, ethyl group, n- propyl group, n- butyl group, n- pentyl group, a n- hexyl group.
  • the aluminum compound is used as a raw material for producing an aluminum oxide film, and preferably used as a raw material for producing an aluminum oxide film by atomic layer deposition (hereinafter referred to as “ALD method”).
  • ALD method atomic layer deposition
  • an ALD method or a CVD method can be mentioned as a film forming method, but the ALD method is preferable in that it is easy to control the film thickness, has excellent step film property, and can form a uniform and dense film. Is preferred.
  • Chem. Mater. As described in the second paragraph on page 4845 of 2010, 22, 4844-4853, the materials used for the ALD method are much more limited than the CVD method, so search for materials that can be deposited by the ALD method. It is difficult.
  • the aluminum compound can also be deposited by ALD.
  • Deposition target examples include SiO 2 / Si, Si, TiN / Si, ZrO 2 / Si, Si 3 N 4 / SiO 2 / Si, and the like, with preference given to SiO 2 / Si.
  • the alkylaluminum dihalide compound used in the method for producing an aluminum oxide film of the present invention can be produced, for example, by a method in which trihalogenoaluminum and trialkylaluminum are reacted.
  • trihalogenoaluminum examples include trichloroaluminum, tribromoaluminum, triiodoaluminum and the like, preferably trichloroaluminum.
  • trialkylaluminum examples include trimethylaluminum, triethylaluminum, tripropylaluminum, tributylaluminum, trihexylaluminum and the like, preferably trimethylaluminum, triethylaluminum, tripropylaluminum, tributylaluminum, more preferably trimethyl.
  • the amount of the trialkylaluminum used is preferably 0.1 to 1.0 mol, more preferably 0.2 to 0.7 mol, still more preferably 0.2 to 0 mol, per 1 mol of trihalogenoaluminum. 5 moles.
  • the reaction is preferably carried out in an organic solvent, and the organic solvent used is not particularly limited as long as it does not inhibit the reaction.
  • organic solvent used is not particularly limited as long as it does not inhibit the reaction.
  • aliphatic hydrocarbons such as hexane, heptane, cyclohexane, methylcyclohexane and ethylcyclohexane; aromatic hydrocarbons such as toluene and xylene; ethers such as diethyl ether, tetrahydrofuran, dimethoxyethane and dioxane, etc. are preferable.
  • Is a mixed solvent of aliphatic hydrocarbons and aromatic hydrocarbons, or aliphatic hydrocarbons. These organic solvents may be used alone or in combination of two or more.
  • the amount of the organic solvent used is preferably 1 g to 100 g, more preferably 3 g to 50 g, still more preferably 3 g to 10 g, per 1 g of trihalogenoaluminum.
  • the reaction is performed, for example, by a method such as mixing and reacting trihalogenoaluminum, trialkylaluminum and an organic solvent.
  • the reaction temperature at that time is preferably ⁇ 100 ° C. to 100 ° C., more preferably ⁇ 80 ° C. to 40 ° C., and the reaction pressure is not particularly limited.
  • the desired product an alkylaluminum dihalide compound
  • the alkylaluminum dihalide compound is obtained by a known method such as extraction, filtration, concentration, distillation, sublimation, recrystallization, column chromatography, etc. May be isolated and purified.
  • alkylaluminum dihalide compounds and the trihalogenoaluminum compounds and trialkylaluminum compounds that are the raw materials for their production are often unstable with respect to moisture and oxygen in the atmosphere, they are under anhydrous conditions or under inert gas conditions.
  • the reaction operation of the reaction, post-treatment of the reaction solution, and the like are performed.
  • the alkyl aluminum dihalide compound is suitably used as a production raw material (production raw material) for producing an aluminum oxide film. It is preferable that the manufacturing raw material (raw material for manufacturing) for manufacturing an aluminum oxide film consists only of an alkyl aluminum dihalide compound. However, the above-mentioned production raw material (production raw material) may contain a small amount of impurities (aluminum compound etc.) other than the alkylaluminum dihalide compound within a range which does not greatly affect the quality of the formed aluminum oxide film.
  • Examples of the method of depositing the aluminum oxide film on the film formation target include the ALD method and the CVD method, but the ALD method is more preferably used.
  • the vapor of an alkylaluminum dihalide compound is supplied onto a film formation target heated with a reactive gas under normal pressure or reduced pressure, and aluminum oxide is oxidized by oxidizing the alkylaluminum dihalide compound.
  • a film may be formed.
  • the gas containing the vapor of the alkylaluminum dihalide compound (including the vaporized liquid) may be diluted with an inert gas or the like.
  • an aluminum oxide film can be deposited by plasma CVD using the same raw material supply.
  • reactive gases examples include oxidizing gases such as oxygen and ozone; water; alcohols such as methanol, ethanol, n-propyl alcohol, isopropyl alcohol and n-butanol, etc.
  • oxidizing gases such as oxygen and ozone
  • water alcohols such as methanol, ethanol, n-propyl alcohol, isopropyl alcohol and n-butanol, etc.
  • a film it is preferably water, ozone, and more preferably water.
  • the alkylaluminum dihalide compound is oxidized by the reactive gas.
  • aluminum oxide is vapor-deposited on the film-forming object, and an aluminum oxide film is formed.
  • the reactive gas may be used as a single species or as a mixed gas.
  • the inert gas includes argon, nitrogen and helium.
  • the alkylaluminum dihalide compound In the CVD method, it is necessary to vaporize the alkylaluminum dihalide compound to form a thin film.
  • a method of vaporizing the alkylaluminum dihalide compound for example, not only a method of charging or transporting the alkylaluminum dihalide compound in the vaporizing chamber for vaporizing, but also the alkylaluminum dihalide compound can be used in an appropriate solvent (eg, hexane, cyclohexane) Aliphatic hydrocarbons such as methylcyclohexane, ethylcyclohexane, heptane and octane; aromatic hydrocarbons such as toluene, ethylbenzene and xylene; ethers such as diethyl ether, tetrahydrofuran, dimethoxyethane and dioxane)
  • solvent eg, hexane, cyclo
  • the pressure in the reaction system when depositing an aluminum oxide film using an alkylaluminum dihalide compound is preferably 1 Pa to 200 kPa, more preferably 10 Pa to 110 kPa.
  • the film formation target temperature is preferably 250 ° C. to 580 ° C., more preferably 300 ° C. to 550 ° C., still more preferably 480 ° C. to 550 ° C. More preferably, it is 500 to 550.degree. In one embodiment, it is preferably 250 ° C. to 600 ° C., more preferably 300 ° C. to 500 ° C., still more preferably 300 ° C.
  • the temperature at which the alkylaluminum dihalide compound is vaporized is preferably 30 ° C. to 250 ° C., more preferably 60 ° C. to 200 ° C.
  • the content ratio of oxygen source (for example, oxidizing gas, water vapor or alcohol vapor, or mixed gas thereof) is preferably 3 to 99% by volume, and more preferably, to the total amount of gas when depositing the aluminum oxide film. It is 5 to 98% by volume.
  • the film forming method of the present invention is an industrially suitable method, and a high quality aluminum oxide compound can be obtained.
  • a high quality aluminum oxide film can be obtained by forming a film by the film forming method using a halide compound.
  • the aluminum oxide film of the present embodiment is formed on the film formation target by supplying the aluminum compound onto the heated film formation target and oxidizing the aluminum compound.
  • the aluminum oxide film has a thickness of, for example, 1 to 100 nm, preferably 10 to 80 nm, and more preferably 20 to 60 nm.
  • the aluminum oxide film of the present embodiment can be sufficiently reduced in impurity concentration to obtain good quality.
  • the content of aluminum oxide in the aluminum oxide film is, for example, 95% by mass or more, preferably 98% by mass or more, and more preferably 99% by mass or more.
  • Such high purity aluminum oxide films having high purity and small thickness are useful in the semiconductor field.
  • one having an aluminum oxide content of 90% by mass or more is referred to as an “aluminum oxide film”.
  • the variation in thickness of the aluminum oxide film is, for example, less than 10 nm.
  • the variation in thickness of the aluminum oxide film refers to the difference (maximum value-minimum value) in the film thickness measured at an arbitrarily selected point.
  • Example A1 (Synthesis of methylaluminum dichloride (compound of formula (2))) 13.0 g (97.5 mmol) of trichloroaluminum and 50 mL of toluene were added to a 100 mL flask equipped with a stirrer, a thermometer and a dropping funnel and cooled. Into the resulting solution, 3.50 g (48.8 mmol) of trimethylaluminum was slowly dropped so that the internal temperature became 0 to 6 ° C., and the mixture was stirred at room temperature (25 ° C.) for 15 hours.
  • methylaluminum dichloride is a compound shown by the following physical-property values. 1 H-NMR (C 6 D 6 , ⁇ (ppm)); -0.45 (3 H, s)
  • Example A2 (Synthesis of Ethyl Aluminum Dichloride (Compound of Formula (3))) 7.00 g (52.5 mmol) of trichloroaluminum and 30 mL of toluene were added to a flask with an internal volume of 100 mL equipped with a stirrer, a thermometer and a dropping funnel, and cooled. To the resulting solution, 3.00 g (26.3 mmol) of triethylaluminum was dropped slowly so that the internal temperature became 0 to 6 ° C., and the mixture was stirred at room temperature (25 ° C.) for 15 hours.
  • Ethyl aluminum dichloride is a compound represented by the following physical property values. 1 H-NMR (C 6 D 6 , ⁇ (ppm)); 0.21 (2 H, q), 0.93 (3 H, t)
  • Example B1 (Production of Aluminum Oxide Film) An aluminum oxide film was formed by an ALD method using ethylaluminum dichloride (the compound of the formula (3)) synthesized in Example A2. In addition, the film thickness of the formed aluminum oxide film was measured, and the composition was analyzed. The composition was analyzed using an XPS (X-ray photoelectron spectroscopy) measuring apparatus. Next, the production of the aluminum oxide film will be described more specifically.
  • XPS X-ray photoelectron spectroscopy
  • An aluminum oxide film was formed on the substrate by the ALD method using ethylaluminum dichloride synthesized in Example A2 as the aluminum compound, that is, the compound represented by the above formula (3).
  • the formation of the aluminum oxide film was performed using the apparatus shown in FIG.
  • the apparatus shown in FIG. 1 includes a vaporizer 1 (ample made of SUS) that vaporizes an aluminum compound 2, a vaporizer 6 (ample made of SUS) that vaporizes water 7 and supplies water vapor that is a reactive gas, and a substrate 15 And a heater 11 for heating the substrate 15, and a reactor 11 for reacting the aluminum compound 2 with water vapor to form an aluminum oxide film on the substrate 15.
  • a vacuum pump is connected to the reactor 11 via a flow path.
  • the flow path is provided with a pressure gauge 13, a pressure control valve 12, and a trap 16. By this, the pressure in the reactor 11 is adjusted to a predetermined range.
  • the gas derived from the reactor 11 is exhausted to the atmosphere via the trap 16 and a vacuum pump.
  • the aluminum compound 2 and the water 7 synthesized in Example A2 were accommodated in the vaporizer 1 and the vaporizer 6 provided with the heater 3 and the constant temperature bath 8, respectively.
  • the vaporizer 1 was supplied with argon gas whose flow rate was adjusted by the mass flow controller 4 and which was preheated by the preheater 5. As a result, argon gas containing the aluminum compound 2 was introduced into the reactor 11 from the vaporizer 1.
  • water vapor adjusted to a constant temperature by the constant temperature bath 8 and vaporized from the vaporizer 6 was introduced into the reactor 11.
  • the argon gas containing the aluminum compound 2 from the vaporizer 1 and the water vapor from the vaporizer 6 were alternately introduced into the reactor 11.
  • the amounts of introduced argon gas and water vapor containing the aluminum compound 2 were adjusted by the valve 17 and the valve 18, respectively.
  • the argon gas and the water vapor containing the aluminum compound 2 were respectively flow-regulated by the mass flow controller 9 and entrained in the dilution argon gas preheated by the preheater 10 and introduced into the reactor 11.
  • the aluminum compound 2 and the water 7 were alternately supplied to the reactor 11 to form an aluminum oxide film 20 on the substrate 15 heated to a predetermined temperature by the heater 14.
  • the operating conditions of the apparatus of FIG. 1 were as follows.
  • An aluminum oxide film 20 was formed on the substrate 15 under the conditions described above.
  • the thickness of the formed aluminum oxide film 20 was measured using a reflection spectrophotometer. Further, the composition of the aluminum oxide film 20 was analyzed using an XPS (X-ray photoelectron spectroscopy) measurement apparatus. The results of thickness and composition analysis were as shown in Table 1.
  • the thickness of the aluminum oxide film 20 was measured at five places arbitrarily selected, and the maximum value and the minimum value were obtained.
  • maximum value-minimum value ⁇ 10 nm the arithmetic mean value is shown in the table.
  • the maximum value-minimum value ⁇ 10 nm the maximum value and the minimum value were shown.
  • Examples B2 to B6, Comparative Examples 1 to 2 (Production of Aluminum Oxide Film) An aluminum oxide film 20 was formed on the substrate 15 in the same manner as in Example B1, except that the temperature of the substrate 15 was changed as shown in Table 1. The analysis results of the thickness and composition of the formed aluminum oxide film 20 are as shown in Table 1.
  • All of the aluminum oxide films of Examples B1 to B6 had no variation in thickness and were excellent in uniformity of thickness. Further, it was confirmed that when the temperature of the substrate 15 is in the range of 300 to 550 ° C., the composition of the formed film is uniform, and the thickness of the aluminum oxide film does not change much. From this, it was confirmed that an aluminum oxide film can be stably formed by using the ethylaluminum dichloride synthesized in Example A2. The content of aluminum oxide in the aluminum oxide films of Examples B1 to B6 was 99% by mass or more, and the content of aluminum carbide was 1% by mass or less.
  • the aluminum compound represented by the formula (3) did not ignite spontaneously.
  • the aluminum compound of the present invention since the aluminum thin film is formed under the above conditions, the aluminum compound of the present invention has good reactivity with at least one of the thermally decomposable gas and the reactive gas, and contains the aluminum compound of the present invention It has also been found that the vapor is excellent in the adsorptivity to the substrate surface. Furthermore, as long as the temperature of the substrate is set to 300 ° C. to 550 ° C., the composition of the formed film is only aluminum oxide and no halogen atoms remain, so according to the manufacturing method of the present invention, the quality is improved. It turned out that a good aluminum oxide film can be manufactured.
  • a high quality aluminum oxide film can be manufactured by an industrially suitable method. Moreover, the manufacturing raw material suitably used for the said manufacturing method can be provided.

Abstract

La présente invention concerne un procédé de production d'un film d'oxyde d'aluminium, selon lequel un film d'oxyde d'aluminium est formé en fournissant un composé d'aluminium ayant une structure spécifique sur un objet de formation de film, qui a été chauffé à 300-550 °C, ce qui permet ainsi d'oxyder le composé d'aluminium.
PCT/JP2017/005852 2016-03-01 2017-02-17 Procédé de production de film d'oxyde d'aluminium et matériau de départ de production pour film d'oxyde d'aluminium WO2017150212A1 (fr)

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JP2018503028A JPWO2017150212A1 (ja) 2016-03-01 2017-02-17 酸化アルミニウム膜の製造方法及び酸化アルミニウム膜の製造原料

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JP2016-038497 2016-03-01
JP2016038497 2016-03-01

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003059016A (ja) * 2001-05-11 2003-02-28 Asm Microchemistry Oy 磁気ヘッドのための薄膜を堆積する方法
JP2003526218A (ja) * 2000-03-07 2003-09-02 エーエスエム アメリカ インコーポレイテッド 傾斜薄膜
JP2005011904A (ja) * 2003-06-17 2005-01-13 Tokyo Electron Ltd 成膜方法
JP2014022631A (ja) * 2012-07-20 2014-02-03 Nippon Telegr & Teleph Corp <Ntt> 半導体装置およびその製造方法
JP2015012179A (ja) * 2013-06-28 2015-01-19 住友電気工業株式会社 気相成長方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003526218A (ja) * 2000-03-07 2003-09-02 エーエスエム アメリカ インコーポレイテッド 傾斜薄膜
JP2003059016A (ja) * 2001-05-11 2003-02-28 Asm Microchemistry Oy 磁気ヘッドのための薄膜を堆積する方法
JP2005011904A (ja) * 2003-06-17 2005-01-13 Tokyo Electron Ltd 成膜方法
JP2014022631A (ja) * 2012-07-20 2014-02-03 Nippon Telegr & Teleph Corp <Ntt> 半導体装置およびその製造方法
JP2015012179A (ja) * 2013-06-28 2015-01-19 住友電気工業株式会社 気相成長方法

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