WO2012039107A1 - 薄膜製造方法及び薄膜製造装置 - Google Patents
薄膜製造方法及び薄膜製造装置 Download PDFInfo
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- WO2012039107A1 WO2012039107A1 PCT/JP2011/005134 JP2011005134W WO2012039107A1 WO 2012039107 A1 WO2012039107 A1 WO 2012039107A1 JP 2011005134 W JP2011005134 W JP 2011005134W WO 2012039107 A1 WO2012039107 A1 WO 2012039107A1
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- gas
- thin film
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- 239000010409 thin film Substances 0.000 title claims abstract description 141
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 72
- 239000000758 substrate Substances 0.000 claims abstract description 89
- 229910052751 metal Inorganic materials 0.000 claims abstract description 67
- 239000002184 metal Substances 0.000 claims abstract description 67
- 239000002994 raw material Substances 0.000 claims abstract description 63
- 239000013078 crystal Substances 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims description 164
- 230000001590 oxidative effect Effects 0.000 claims description 47
- 239000011261 inert gas Substances 0.000 claims description 46
- 239000000203 mixture Substances 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 8
- 230000004044 response Effects 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract 2
- 238000007254 oxidation reaction Methods 0.000 abstract 2
- 239000010408 film Substances 0.000 description 72
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 55
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 55
- 230000015572 biosynthetic process Effects 0.000 description 44
- 238000012546 transfer Methods 0.000 description 27
- 239000000243 solution Substances 0.000 description 20
- 239000002904 solvent Substances 0.000 description 15
- 239000006200 vaporizer Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 239000010936 titanium Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 238000012545 processing Methods 0.000 description 8
- 239000002344 surface layer Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000008016 vaporization Effects 0.000 description 5
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 4
- 238000005192 partition Methods 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 229910004356 Ti Raw Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- 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
- C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
-
- 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
- C23C16/409—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or lead and B representing a refractory metal, nickel, scandium or a lanthanide
-
- 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
- C23C16/56—After-treatment
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02197—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides the material having a perovskite structure, e.g. BaTiO3
-
- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L28/00—Passive two-terminal components without a potential-jump or surface barrier for integrated circuits; Details thereof; Multistep manufacturing processes therefor
- H01L28/40—Capacitors
- H01L28/55—Capacitors with a dielectric comprising a perovskite structure material
Definitions
- the present invention relates to a thin film manufacturing method and a thin film manufacturing apparatus for manufacturing a dielectric thin film such as a PZT (lead zirconate titanate) thin film.
- a dielectric thin film such as a PZT (lead zirconate titanate) thin film.
- a thin film such as lead zirconate titanate (Pb (Zr, Ti) O 3 ; PZT) having a perovskite structure is known as a ferroelectric thin film used in a ferroelectric memory (Ferroelectric Random Access Memory; FeRAM) or the like. It has been.
- a dielectric thin film is manufactured by, for example, a metal organic chemical vapor deposition (MOCVD) method.
- the MOCVD method is a method of manufacturing a dielectric thin film by reacting an organic metal raw material gas and an oxidizing gas at a high temperature.
- a self-aligned region which is a region where the composition ratio of the thin film hardly changes even when the flow rate of the source gas is changed, is used.
- Patent Document 1 describes a MOCVD method in which a mixed gas of an organic metal raw material gas, an oxidizing gas, and a dilution gas is supplied onto a heated substrate.
- a mixed gas when a mixed gas is supplied to a substrate, a highly combustible combustible gas is supplied together. As a result, excess oxygen on the substrate surface is burned and discharged during the film formation process, so that a high-quality thin film can be manufactured (see paragraphs [0011] and [0025] of Patent Document 1).
- the surface roughness of the produced dielectric thin film is small. If the surface roughness of the dielectric thin film is large, for example, a problem may occur in the manufacturing process when a ferroelectric memory having the dielectric thin film is manufactured. Moreover, for example, there is a concern that the electrical characteristics of the dielectric thin film are not sufficiently exhibited.
- an object of the present invention is to provide a thin film manufacturing method and a thin film manufacturing apparatus capable of manufacturing a dielectric thin film having a small surface roughness.
- a thin film manufacturing method includes a mixed gas containing a metal raw material gas that is a raw material for a dielectric thin film having a perovskite crystal and an oxidizing gas that reacts with the metal raw material gas.
- the supply of the metal source gas to the substrate is stopped.
- the supply of the oxidizing gas to the substrate is restricted.
- a thin film manufacturing apparatus includes a chamber, a supply mechanism, and a gas supply control unit.
- a heated substrate is disposed in the chamber.
- the supply mechanism supplies, to the heated substrate in the chamber, a mixed gas including a metal raw material gas that is a raw material for a dielectric thin film having a perovskite crystal and an oxidizing gas that reacts with the metal raw material gas. Is to do.
- the gas supply control means stops the supply of the metal source gas to the substrate and then regulates the supply of the oxidizing gas to the substrate.
- a thin film manufacturing method provides a mixed gas containing a gas of a metal raw material that is a raw material of a dielectric thin film having a perovskite crystal and an oxidizing gas that reacts with the metal raw material gas in a chamber.
- the supply of the metal source gas to the substrate is stopped.
- the supply of the oxidizing gas to the substrate is restricted.
- this thin film manufacturing method it is possible to suppress the reaction between the surplus atoms that do not constitute the perovskite crystal and the oxidizing gas after the supply of the metal source gas to the substrate is stopped. Thereby, extra atoms are not taken into the surface layer of the dielectric thin film as an oxide, for example, and a dielectric thin film having a small surface roughness can be manufactured.
- the regulation step may stop or reduce the supply of the oxidizing gas.
- the thin film manufacturing method may further include supplying an inert gas into the chamber in response to the stop or decrease of the supply of the oxidizing gas.
- an inert gas is supplied into the chamber in response to the stop and reduction of the supply of the oxidizing gas.
- This inert gas makes it possible to adjust the pressure in the chamber, for example. Thereby, when a dielectric thin film is sequentially formed on a plurality of substrates, the film forming process can be efficiently performed.
- the step of supplying the mixed gas may supply the mixed gas containing an inert gas.
- the step of supplying the inert gas in response to the stop or reduction of the supply of the oxidizing gas may supply the inert gas contained in the mixed gas.
- an inert gas is included in the mixed gas used for manufacturing the dielectric thin film.
- This inert gas is supplied into the chamber in response to the supply and stop of the oxidizing gas. This eliminates the need for a new mechanism for supplying the inert gas, and allows the inert gas to be easily supplied.
- the step of supplying the mixed gas may supply the mixed gas via a supply path that connects the chamber and a mixer that mixes the metal source gas, the oxidizing gas, and the inert gas.
- the step of supplying the inert gas may supply the inert gas through the supply path through which the mixed gas has passed.
- an inert gas is supplied into the chamber through a supply path through which the mixed gas passes. This can prevent the mixed gas from accumulating in the supply path. As a result, the dielectric thin film can be stably formed on the substrate.
- the dielectric thin film may be PZT (Pb (Zr, Ti) O 3 ).
- the metal raw material may include Pb (dpm) 2 , Pb (divm) 2 , or a material partially including at least one of them.
- the substrate may be heated to 600 ° C. or higher.
- a thin film manufacturing apparatus includes a chamber, a supply mechanism, and a gas supply control unit.
- a heated substrate is disposed in the chamber.
- the supply mechanism supplies, to the heated substrate in the chamber, a mixed gas including a metal raw material gas that is a raw material for a dielectric thin film having a perovskite crystal and an oxidizing gas that reacts with the metal raw material gas. Is to do.
- the gas supply control means stops the supply of the metal source gas to the substrate and then regulates the supply of the oxidizing gas to the substrate.
- FIG. 1 is a schematic diagram illustrating a configuration example of a thin film manufacturing apparatus according to an embodiment of the present invention. With the thin film manufacturing apparatus of this embodiment, it is possible to manufacture a ferroelectric PZT thin film using the MOCVD method.
- the thin film manufacturing apparatus 100 includes a raw material supply unit 10 that supplies an organic solvent solution of an organic metal, and a vaporizer 20 that generates the raw material gas by vaporizing the solution. Further, the thin film manufacturing apparatus 100 includes a mixer 30 that generates a mixed gas by mixing a raw material gas, an oxidizing gas that reacts with the raw material gas, and an inert gas, and a mixer 30 and a supply line 33 as a supply path. And a film formation chamber 50 to be connected.
- a supply mechanism is comprised by the raw material supply part 10, the vaporizer 20, the mixer 30, and each line and each valve provided in these.
- the raw material supply unit 10 includes tanks A, B, C, and D that are filled with an organic metal raw material solution and a solvent, and a He (helium) supply line 11 that is supplied to each of the tanks A to D.
- the raw material supply unit 10 also has a carrier gas supply line 12 for transporting the metal raw material solution and solvent extruded by the pressure of He supplied to each of the tanks A to D.
- N 2 nitrogen
- the present invention is not limited to this, and other inert gases may be used.
- the gas supplied to each of the tanks A to D is not limited to He, and other inert gas may be used.
- the tanks A to D are filled with a Pb raw material solution, a Zr raw material solution, a Ti raw material solution, and an organic solvent, respectively.
- a raw material solution of Pb, Zr, and Ti a solution in which each metal raw material is dissolved at a concentration of 0.25 mol / L in an n-butyl acetate solution is used.
- Pb (dpm) 2 bisdipivaloylmethanate
- Zr (dmhd) 4 tetrakis (2,6) dimethyl (3,5) heptanedionate is used as the Zr raw material.
- Zirconium is used.
- Ti (iPrO) 2 (dpm) 2 ((bisisopropoxide) (bisdipivaloylmethanate)) titanium is used as the Ti raw material.
- n-butyl acetate is used as Pb (dpm) 2 is also referred to as Pb (thd) 2 (bis (2,2,6,6) tetramethyl (3,5) heptanedionate) lead.
- Each metal raw material dissolved in the solvent is not limited to the above.
- Pb raw material Pb (divm) 2 (bisdiisobutyryl methanate) lead or the like, or a material partially including both or at least one of Pb (dpm) 2 and Pb (divm) 2 may be used.
- Zr raw material Zr (thd) 4 (tetrakis (2,2,6,6) tetramethyl (3,5) heptanedionate) zirconium or the like, or a material partially containing these may be used.
- Ti (MMP) 4 tetrakis (1) methoxy (2) methyl (2) propoxy
- toluene tetrahydrofurone (THF)
- cyclohexane ethylcyclohexane
- methylcyclohexane or the like may be used instead of the above-described n-butyl acetate as the solvent for dissolving each metal raw material and the solvent charged in the tank D.
- the vaporizer 20 is connected to the raw material supply unit 10 via the supply line 12, and the metal raw material solution and solvent droplets are conveyed from the raw material supply unit 10 to the vaporizer 20.
- the vaporizer 20 has a heating means (not shown), and the conveyed metal raw material solution and solvent are vaporized by heating. Thereby, metal source gas is produced
- a method of applying gas or ultrasonic waves to the droplets of the metal raw material solution and the solvent, a method of introducing droplets that have been refined in advance through a fine nozzle, etc. may be used in combination. Good.
- the vaporizer 20 is provided with a Run line 21 connected to the mixer 30 and a Vent line 22 connected to the vacuum exhaust system 40.
- the Run line 21 is provided with a valve V 1
- the Vent line 22 is provided with a valve V 2 .
- the mixer 30 produces
- O 2 oxygen
- N 2 is supplied from the inert gas supply unit 32.
- nitrous oxide or ozone may be supplied as the oxidizing gas.
- argon etc. may be supplied as an inert gas.
- the film forming chamber 50 includes a chamber 51 connected to the supply line 33 and a stage 52 disposed in the chamber 51.
- a shower nozzle 53 is provided on the ceiling surface of the chamber 51, and a supply line 33 is connected to the shower nozzle 53.
- the stage 52 and the shower nozzle 53 are arranged at positions facing each other. Further, in the chamber 51, components such as an adhesion prevention plate (not shown) are disposed in a cleaned state.
- a substrate S on which a PZT thin film is formed is placed on the stage 52.
- the stage 52 has a heating means (not shown) such as a heater, and can heat the substrate S placed thereon.
- a heating means such as a heater
- the substrate S placed on the stage 52 a substrate in which Ir is deposited by sputtering on an 8-inch Si substrate on which a 100 nm SiO 2 oxide film is formed is used.
- the size and material of the substrate are not limited.
- the chamber 51 is connected via a pressure regulating valve 41 to a vacuum exhaust system 40 equipped with, for example, a dry pump or a turbo molecular pump.
- a pressure regulating valve 41 to a vacuum exhaust system 40 equipped with, for example, a dry pump or a turbo molecular pump.
- Each device including each line from the vaporizer 20 to the film formation chamber 50, each valve, the mixer 30 and the like is in a high temperature state of, for example, 200 ° C. or higher by a heating means (not shown) so that the vaporized metal source gas is not liquefied. To be kept.
- the thin film manufacturing apparatus 100 has a control unit (not shown) as a gas supply control means for controlling each valve and each apparatus described above.
- the control unit includes, for example, a main memory including a CPU (Central Processing Unit), a ROM (Read Only Memory), a RAM (Random Access Memory), and the like.
- the operation of the thin film manufacturing apparatus 100 is controlled by outputting a control signal from the control unit to each device or the like via, for example, wired or wireless.
- FIG. 2 is a schematic diagram illustrating a configuration example of a multi-chamber film forming apparatus including the thin film manufacturing apparatus 100 according to the present embodiment.
- the multi-chamber type film forming apparatus 200 includes a transfer chamber 201 in which a transfer robot (not shown) capable of transferring the substrate S is provided, and two stocker chambers 202 each capable of mounting one lot of 25 substrates. Have.
- the multi-chamber film forming apparatus 200 includes the two thin film manufacturing apparatuses 100, and the two film forming chambers 50 are disposed around the transfer chamber 201.
- the film formation chamber 50 and the stocker chamber 202 are connected to the transfer chamber 201 via a partition valve 203, respectively. Note that the number of stocker chambers 202 is not limited to two, and more stocker chambers or one stocker chamber may be arranged around the transfer chamber 201.
- the vacuum evacuation system 204 is also connected to the transfer chamber 201 and the stocker chamber 202, respectively.
- each chamber can be independently evacuated to a vacuum atmosphere.
- the inside of the transfer chamber 201, the film formation chamber 50, and the stocker chamber 202 may be exhausted by using one vacuum exhaust system together.
- the evacuation system functions as the evacuation system 40 shown in FIG.
- a gas source 205 is connected to the transfer chamber 201, and the inside of the transfer chamber 201 can be adjusted to a predetermined pressure by a regulated gas such as an inert gas introduced from the gas source 205. Adjustment of the internal pressure of the transfer chamber 201 is performed by an automatic pressure adjustment valve (not shown) provided in the transfer chamber 201.
- the stocker chamber 202 is connected to an atmospheric substrate transfer system 206 via a partition valve 203.
- the atmospheric substrate transfer system 206 is provided with a transfer robot (not shown) that transfers a substrate S that has not been subjected to film formation or has been subjected to film formation between the plurality of wafer cassettes 207 and the stocker chamber 202.
- a predetermined number of substrates S are transferred from the 25 wafer cassette 207 to the stocker chamber 202 by a transfer robot provided in the atmospheric substrate transfer system 206.
- the stocker chamber 202 into which the substrate S is loaded is evacuated.
- the partition valve 203 between the evacuated stocker chamber 202 and the transfer chamber 201 is opened, and both the transfer chamber 201 and the stocker chamber 202 are evacuated.
- An adjustment gas such as N 2 is supplied to the transfer chamber 201 by the gas source 205, for example, 1200 sccm, and the internal pressure of the transfer chamber 201 is adjusted.
- the internal pressure of the film formation chamber 50 is set to about 2 Torr as the film formation pressure condition.
- the internal pressure of the transfer chamber 201 is adjusted to a pressure substantially equal to the internal pressure of the film forming chamber 50 or a pressure about 5% higher than that.
- the internal pressure in the film forming chamber 50 is adjusted by N 2 supplied from the inert gas supply unit 32 shown in FIG.
- the film formation pressure conditions may be set as appropriate.
- two stocker chambers 202 are arranged. Therefore, when all the substrates S are placed in one stocker chamber 202, the substrate S is mounted in the other stocker chamber 202. be able to.
- the second stocker chamber 202 is evacuated when the film formation process of the substrate S loaded in the first stocker chamber 202 is completed. The substrate S is again carried to the film forming chamber 50.
- the nozzle flash of the vaporizer 20 with the solvent pushed out from the tank D and carried by the carrier gas starts, and the metal raw material solution and the solvent can be vaporized in about 3 minutes.
- the valve V 2 of the Vent line 22 is opened, and the solvent vaporized gas and the carrier gas are discarded to the Vent line 22.
- the substrate S is heated by the heating means provided on the stage 52.
- the temperature of the substrate settles at a predetermined temperature in about 3 minutes.
- the substrate S is heated so that the temperature of the substrate S is 600 ° C. or higher.
- the temperature of the substrate S to be heated may be set as appropriate.
- the vaporization of the vaporizer 20 is switched from the vaporization of the solvent to the vaporization of the metal raw material solution mainly controlled by the flow rate for film formation (the Vent line 22 is opened). keeping).
- the valve V 2 of the Vent line 22 is closed and the valve V 1 of the Run line 21 is opened.
- the vaporized gas mainly composed of the metal raw material solution vaporized by the vaporizer 20 is supplied to the mixer 30.
- the vaporized gas supplied from the vaporizer 20 and the oxidizing gas O 2 and the inert gas N 2 are mixed at a predetermined mixing ratio (mol ratio).
- the mixing ratio is appropriately set, for example, in order to obtain the desired crystal orientation of the PZT thin film to be formed.
- the mixed gas generated by the mixer 30 is supplied into the chamber 51 of the film forming chamber 50 through the supply line 33. Then, a mixed gas is supplied to the heated substrate S, and a PZT thin film having a perovskite crystal is formed on the substrate S.
- a PZT thin film of about 70 nm is formed at a film formation rate of about 15 nm / min. Accordingly, the time required for film formation is about 300 seconds.
- the thickness of the PZT thin film to be deposited, the deposition rate, and the time spent for deposition are not limited to these.
- valve V 1 of the Run line 21 is closed and the valve V 2 of the Vent line 22 is opened. Accordingly, the supply of the vaporized gas of the metal raw material solution to the substrate S in the chamber 51 is stopped, and the vaporized gas is discarded to the Vent line 22.
- the supply of O 2 from the oxidizing gas supply unit 31 connected to the mixer 30 is regulated.
- the regulation here means stopping of the supply of O 2 to the substrate S.
- N 2 of a predetermined amount is supplied from the inert gas supply unit 32, the mixed gas is N 2 through a supply line 33 passing through is supplied into the chamber 51.
- the amount of N 2 at this time may be maintained at a flow rate before the supply of O 2 from the oxidizing gas supply unit 31 is stopped, or may be appropriately adjusted after the supply of O 2 is stopped.
- the amount of N 2 may be set so that the internal pressure in the chamber 51 is a pressure that satisfies the film formation pressure condition (about 2 Torr).
- the substrate S is unloaded after about 60 seconds, but this is not limitative.
- the substrate S may be unloaded after 30 seconds to 120 seconds have elapsed.
- the time until the substrate S is unloaded may be set as appropriate based on, for example, the processing time of the film forming process and the possibility of alteration of the substrate.
- the mixed gas remaining in the film formation chamber 50 is sufficiently exhausted before the substrate S is unloaded. Can do. Thereby, for example, when the substrate S is unloaded, it is possible to prevent the remaining mixed gas from flowing into the transfer chamber 201 and generating particles or the like.
- FIG. 3 shows the Pb composition ratio film (Pb / (Zr + Ti)) and the Zr composition ratio film in the manufactured PZT thin film with respect to the flow rate ratio Gas (Pb / (Zr + Ti)) of the Pb source gas supplied to the substrate S. It is a graph showing (Zr / (Zr + Ti)).
- the graph of FIG. 3 shows a graph of a PZT thin film manufactured by the thin film manufacturing apparatus 100 according to the present embodiment and a graph of a PZT thin film manufactured by a thin film manufacturing method given as a comparative example.
- the PZT thin film according to this embodiment is manufactured by supplying N 2 into the chamber 51 after film formation, that is, after stopping the supply of the metal source gas to the film formation chamber 50.
- the PZT thin film mentioned as a comparative example is manufactured by supplying O 2 into the chamber 51 after the supply of the metal source gas to the film forming chamber 50 is stopped.
- a PZT thin film which is a dielectric thin film having a perovskite crystal
- an amorphous region, a self-aligned region, and a PbO precipitation region appear in order from the one with the smaller flow rate of the Pb source gas.
- the amorphous region is a region where the Pb composition is less than the stoichiometric ratio and a crystalline PZT thin film cannot be obtained.
- the self-aligned region is a change in the Pb composition ratio in the thin film even when the flow rate of the Pb source gas is changed. It is a small area.
- the PbO precipitation region is a region where the PbO crystal is precipitated and the Pb composition in the thin film is rapidly increased. In the graph shown in FIG. 3, the measurement results in the self-aligned region among the three regions are shown.
- the region where the value of the Pb flow ratio is about 1.15 to about 1.5 is defined as the region within the self-alignment region.
- the self-alignment region varies based on film formation conditions such as internal pressure and temperature in the film formation chamber 50, for example. Therefore, when the PZT thin film is manufactured, the Pb flow rate ratio included in the self-aligned region is appropriately set based on each film forming condition.
- the Zr composition ratio of the manufactured PZT thin film has almost no difference between the PZT thin film according to the present embodiment and the PZT thin film according to the comparative example. That is, almost no change was observed in the Zr composition ratio of the PZT thin film regardless of whether the gas supplied into the chamber 51 after film formation was N 2 or O 2 .
- the Zr composition ratio of the PZT thin film can be set as appropriate based on the Zr flow ratio in the raw material supply unit 10 shown in FIG.
- the Zr composition ratio may be set so that the manufactured PZT thin film has desired characteristics.
- the PZT thin film according to the comparative example has a larger value than the PZT thin film according to the present embodiment. That is, the Pb composition in the self-aligned region is increased in the manufacturing method according to this embodiment in which the gas supplied after film formation is N 2 , compared to the manufacturing method of the comparative example in which O 2 is supplied after film formation. Can be suppressed.
- a PZT crystal In the self-aligned region, a PZT crystal is ideally obtained, and extra atoms that do not constitute a perovskite crystal are eliminated. However, in actuality, excess Pb atoms remain, for example, at the crystal grain boundaries and the surface of the PZT thin film. In some cases, Pb adheres to the components in the chamber 51.
- FIG. 4 shows a photograph of each surface layer of the PZT thin film manufactured by the thin film manufacturing apparatus 100 according to this embodiment and a PZT thin film manufactured by the manufacturing method according to the comparative example, and each measured value for the surface layer.
- FIG. FIG. 4A shows a PZT thin film according to this embodiment
- FIG. 4B shows a PZT thin film according to a comparative example.
- Each photograph was taken with an atomic force microscope.
- Each PZT thin film shown in FIGS. 4 (A) and 4 (B) is manufactured when the flow rate ratio of the Pb source gas is 1.15.
- the measured value Ra is the average surface roughness
- the measured value Rms is the root mean square roughness.
- the measured value PV is peak-to-valley.
- the supply of O 2 to the substrate S is stopped after the supply of the metal source gas to the substrate S is stopped. Therefore, it is possible to suppress the reaction between extra Pb atoms that do not constitute the perovskite crystal after the film formation and O 2 . Thereby, extra Pb atoms are not taken into the surface layer of the PZT thin film, for example, as oxide PbO, and a PZT thin film having a small surface roughness can be manufactured.
- N 2 is supplied as an inert gas into the chamber 51 in response to the stop of the supply of O 2 after film formation.
- the internal pressure in the chamber 51 is set to the film formation pressure. It is possible to adjust the pressure to satisfy the condition. Thereby, for example, when a PZT thin film is sequentially formed on a plurality of substrates S of about 300 sheets, the film forming process can be advanced efficiently.
- an inert gas supply unit 32 is connected to the mixer 30, and N is an inert gas in the mixed gas for manufacturing the PZT thin film. 2 included.
- This N 2 is supplied into the chamber 51 in response to the stop of the supply of O 2 . This eliminates the need for a new mechanism for supplying the inert gas into the chamber 51 after the film formation, and allows the inert gas to be easily supplied after the film formation.
- the mixed gas is supplied through the supply line 33 that connects the mixer 30 and the chamber 51, and N 2 is supplied through the supply line 33 through which the mixed gas passes after film formation. Supplied. Therefore, after the supply of the metal source gas is stopped, N 2 is supplied into the chamber 51 so as to extrude the mixed gas containing the metal source gas. Thereby, it is possible to prevent the metal source gas from accumulating in the supply line 33. As a result, for example, it can be prevented that the metal source gas (mixed gas) accumulated in the supply line is supplied into the chamber 51 during the supply of N 2 after the film formation, and the substrate S can be stably supplied. A PZT thin film can be formed.
- FIG. 5 is a schematic diagram showing a modification of the thin film manufacturing apparatus 100 shown in FIG.
- the inert gas supply unit 332 is not connected to the mixer 330, but is separately connected to the shower nozzle 353 of the chamber 351.
- the metal source gas and the oxidizing gas are mixed by the mixer 330, and the mixed gas is supplied to the substrate S.
- a PZT thin film is formed on the substrate S.
- the supply of the mixed gas (metal source gas and oxidizing gas) from the mixer 330 is stopped, and the inert gas is supplied from the inert gas supply unit 332 into the chamber.
- the inert gas supply unit 332 may be connected to the chamber 351 separately from the mixer 330.
- the inert gas need not be supplied. Even in this case, if the supply of the oxidizing gas is stopped after the supply of the metal source gas is stopped, unnecessary Pb atoms react with the oxidizing gas after the film formation, and the oxide PbO is taken into the surface layer of the PZT thin film. Can be prevented.
- the inert gas is not supplied after the film formation, the inside of the film formation chamber is once pulled after the film formation, and the substrate is transferred from the transfer chamber in this state.
- the mixer may not be provided, and the metal source gas, the oxidizing gas supply unit, and the inert gas supply unit may be separately connected to the chamber.
- a mixed gas of the metal source gas, the oxidizing gas, and the inert gas is generated in the chamber.
- the supply of the oxidizing gas and the inert gas may be controlled as described above.
- the supply of the oxidizing gas was stopped after the supply of the metal source gas to the substrate was stopped.
- the supply of oxidizing gas may be reduced after film formation. That is, the regulation of the supply of the oxidizing gas may include both stop and reduction of the supply of the oxidizing gas.
- the PZT thin film is manufactured by the thin film manufacturing apparatus 100.
- the present invention is applicable even when a thin film other than a PZT thin film is manufactured as a dielectric thin film having a perovskite crystal.
- a dielectric thin film for example, lanthanum-doped lead zirconate titanate ((Pb, La) (Zr, Ti) O 3 ; PLZT), strontium bistrontate tantalate (SrBi 2 , Ta 2 , O 9 ; SBT) ) Etc.
- a multi-chamber film forming apparatus 200 is exemplified as an apparatus including the thin film manufacturing apparatus 100 according to the embodiment of the present invention.
- the thin film manufacturing apparatus 100 of this embodiment may be provided in a substrate processing apparatus including a plurality of processing apparatuses such as an etching processing apparatus and a cleaning processing apparatus.
- a substrate processing apparatus for example, there is a cluster tool type or in-line type substrate processing apparatus.
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Abstract
Description
前記基板への前記金属原料ガスの供給が停止される。
前記金属原料ガスの供給の停止後、前記基板への前記酸化ガスの供給が規制される。
前記チャンバには、加熱された基板が配置される。
前記供給機構は、ペロブスカイト型結晶を有する誘電体薄膜の原料となる金属原料のガスと、前記金属原料ガスと反応する酸化ガスとを含む混合ガスを、前記チャンバ内の前記加熱された基板に供給するためのものである。
前記ガス供給制御手段は、前記基板への前記金属原料ガスの供給を停止させ、その後前記基板への前記酸化ガスの供給を規制する。
前記基板への前記金属原料ガスの供給が停止される。
前記金属原料ガスの供給の停止後、前記基板への前記酸化ガスの供給が規制される。
前記チャンバには、加熱された基板が配置される。
前記供給機構は、ペロブスカイト型結晶を有する誘電体薄膜の原料となる金属原料のガスと、前記金属原料ガスと反応する酸化ガスとを含む混合ガスを、前記チャンバ内の前記加熱された基板に供給するためのものである。
前記ガス供給制御手段は、前記基板への前記金属原料ガスの供給を停止させ、その後前記基板への前記酸化ガスの供給を規制する。
図1は、本発明の一実施形態に係る薄膜製造装置の構成例を示す模式的な図である。本実施形態の薄膜製造装置により、MOCVD法を利用した強誘電体PZTの薄膜の製造が可能となる。
図2は、本実施形態に係る薄膜製造装置100を含む多室型成膜装置の構成例を示す模式的な図である。多室型成膜装置200は、基板Sを搬送することが可能な図示しない搬送ロボットが設けられる搬送室201と、1ロット25枚の基板をそれぞれ搭載することができる2つのストッカー室202とを有する。また多室型成膜装置200は2つの上記薄膜製造装置100を有しており、搬送室201の周囲に2つの上記成膜室50がそれぞれ配置される。成膜室50及びストッカー室202は、仕切りバルブ203を介して搬送室201にそれぞれ接続される。なおストッカー室202の数は2つに限られず、より多くのストッカー室あるいは1つのストッカー室が搬送室201の周囲に配置されてもよい。
図1に示すHeの供給ライン11から各タンクA~DにHeが供給されると、各タンクA~Dの内部圧力が上昇し、各タンクA~Dに充填されていた有機金属の原料溶液及び溶媒がキャリアガス(N2)の供給ライン12に押し出される。押し出された金属原料溶液及び溶媒の液滴は、それぞれの流量が液体流量制御器等で制御されて、キャリアガスにより気化器20に運搬される。
10…原料供給部
11、12、33…供給ライン
12…供給ライン
20…気化器
21…Runライン
22…Ventライン
30、330…混合器
31…酸化ガス供給部
32、332…不活性ガス供給部
51、351…チャンバ
100、300…薄膜製造装置
Claims (7)
- ペロブスカイト型結晶を有する誘電体薄膜の原料となる金属原料のガスと、前記金属原料ガスと反応する酸化ガスとを含む混合ガスを、チャンバ内の加熱された基板に供給し、
前記基板への前記金属原料ガスの供給を停止させ、
前記金属原料ガスの供給の停止後、前記基板への前記酸化ガスの供給を規制する
薄膜製造方法。 - 請求項1に記載の薄膜製造方法であって、
前記規制工程は、前記酸化ガスの供給を停止又は減少させ、
前記薄膜製造方法は、前記酸化ガスの供給の停止又は減少に応じて、不活性ガスを前記チャンバ内に供給することをさらに具備する
薄膜製造方法。 - 請求項2に記載の薄膜製造方法であって、
前記混合ガスを供給する工程は、不活性ガスを含む前記混合ガスを供給し、
前記酸化ガスの供給の停止又は減少に応じて不活性ガスを供給する工程は、前記混合ガスに含まれる前記不活性ガスを供給する
薄膜製造方法。 - 請求項3に記載の薄膜製造方法であって、
前記混合ガスを供給する工程は、前記金属原料ガス、前記酸化ガス、及び前記不活性ガスを混合する混合器と前記チャンバとを接続する供給経路を介して、前記混合ガスを供給し、
前記不活性ガスを供給する工程は、前記混合ガスが通った前記供給経路を介して前記不活性ガスを供給する
薄膜製造方法。 - 請求項1~4のうちいずれか1項に記載の薄膜製造方法であって、
前記誘電体薄膜は、PZT(Pb(Zr,Ti)O3)であり、
前記金属原料は、Pb(dpm)2、Pb(dibm)2、又はこれらのうち少なくとも一方を一部に有する材料を含む
薄膜製造方法。 - 請求項1~5のうちいずれか1項に記載の薄膜製造方法であって、
前記基板は、600℃以上に加熱されている薄膜製造方法。 - 加熱された基板が配置されるチャンバと、
ペロブスカイト型結晶を有する誘電体薄膜の原料となる金属原料のガスと、前記金属原料ガスと反応する酸化ガスとを含む混合ガスを、前記チャンバ内の前記加熱された基板に供給するための供給機構と、
前記基板への前記金属原料ガスの供給を停止させ、その後前記基板への前記酸化ガスの供給を規制するガス供給制御手段と
を具備する薄膜製造装置。
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JP2012534919A JP5719849B2 (ja) | 2010-09-21 | 2011-09-13 | 薄膜製造方法 |
CN2011800450686A CN103119696A (zh) | 2010-09-21 | 2011-09-13 | 薄膜制造方法和薄膜制造装置 |
EP11826558.6A EP2620975A4 (en) | 2010-09-21 | 2011-09-13 | METHOD AND DEVICE FOR MANUFACTURING THIN FILMS |
US13/825,091 US20130216710A1 (en) | 2010-09-21 | 2011-09-13 | Thin film forming method and thin film forming apparatus |
KR1020137005578A KR101408431B1 (ko) | 2010-09-21 | 2011-09-13 | 박막 제조 방법 및 박막 제조 장치 |
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JP2014150191A (ja) * | 2013-02-01 | 2014-08-21 | Ulvac Japan Ltd | Pzt膜の製造方法及び成膜装置 |
JP2015065277A (ja) * | 2013-09-25 | 2015-04-09 | 株式会社アルバック | Pzt薄膜製造方法 |
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EP2620975A1 (en) | 2013-07-31 |
JP5719849B2 (ja) | 2015-05-20 |
TWI561666B (en) | 2016-12-11 |
TW201213593A (en) | 2012-04-01 |
EP2620975A4 (en) | 2014-07-23 |
KR101408431B1 (ko) | 2014-06-17 |
US20130216710A1 (en) | 2013-08-22 |
JPWO2012039107A1 (ja) | 2014-02-03 |
CN103119696A (zh) | 2013-05-22 |
KR20130032914A (ko) | 2013-04-02 |
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