Classifications

• • 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
  • C23C16/22—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
  • C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C49/00—Ketones; Ketenes; Dimeric ketenes; Ketonic chelates
  • C07C49/92—Ketonic chelates
• • 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
  • C23C16/06—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 metallic material
  • C23C16/18—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 metallic material from metallo-organic compounds

Definitions

• the present invention relates to a raw material for forming a thin film containing bis (
• a thin film containing zinc has various characteristics such as optical characteristics, electric characteristics, and catalytic activity, and is used as a member of an electronic component or an optical component.
• Examples of the method for producing the above thin film include a thermal deposition method, a sputtering method, an ion plating method, a MOD method such as a coating thermal decomposition method and a sol-gel method, and a chemical vapor deposition method. It has many advantages such as being excellent in step coverage, being suitable for mass production, and being capable of hybrid integration, so that it can be used for chemical vapor deposition (hereinafter, referred to as ALD (Atomic Layer Deposition)). The method is sometimes referred to simply as CVD).
• ALD Atomic Layer Deposition
• Patent Documents 1 to 3 report a method for producing a zinc-containing thin film using bis (pentane-2,4-dionato) zinc
• Non-Patent Document 1 discloses bis (2,2,6).
• a method for producing a zinc-containing thin film using (6,6-tetramethylheptane 3,5-dione) zinc has been reported.
• these complexes are solid, it is necessary to gasify them by sublimation in the vaporization process of the raw materials or to keep the raw materials at a high temperature above the melting point.
• Patent Document 4 discloses that a mixture of two or more kinds of 13 diketones is disclosed. A method using a liquid j8-diketonate using a compound has been reported. However, in this method, since a mixture is used, there remain problems in stability of thin film production conditions and solid deposition.
• Patent Document 1 Japanese Patent Publication No. 6-64738
• Patent Document 2 JP-A-8-3171
• Patent Document 3 Japanese Patent Application Laid-Open No. 2003-236376
• Patent Document 4 International Publication No.98Z46617 pamphlet
• Non-patent literature l Microelectron.Eng., 29 (1-4), 169-72 (1995)
• An object of the present invention is to provide a thin film-forming raw material containing a zinc compound, which is suitable for forming a zinc-containing thin film.
• the present invention has been made based on the above findings, and uses a raw material for forming a thin film containing a bis ( ⁇ -diketonato) zinc compound which is liquid at 25 ° C, and using the raw material for forming a thin film. It is intended to provide a method for producing a thin film by a chemical vapor deposition method.
• FIG. 1 is a schematic diagram showing an example of a CVD apparatus used in the method for producing a thin film of the present invention.
• FIG. 2 is a schematic diagram showing one example of a CVD apparatus used in the method for producing a thin film of the present invention.
• FIG. 3 is a schematic view showing one example of a CVD apparatus used in the method for producing a thin film of the present invention.
• the bis (j8-diketonato) zinc conjugate according to the present invention is a complex conjugate in which two j8-diketone residues are bonded to one zinc atom.
• 8—diketone residues coordinated to the zinc atom The groups may be the same or different and may have an optically active site in the ⁇ -diketone residue.
• the material for forming a thin film of the present invention contains the above bis ( ⁇ -diketonato) zinc compound as a precursor for forming a thin film, and the bis (j8-diketonato) zinc conjugate may also have strength. It may contain other components such as an organic solvent, as described below, depending on the purpose of use.
• the thin film formed from the raw material for forming a thin film of the present invention can be prepared by appropriately selecting a precursor, a reactive gas, and production conditions of other components to obtain a metal, an alloy, a sulfide, an oxide ceramic, a nitride, or the like. It is obtained as a desired type of thin film such as ceramics and glass.
• Examples of the type of thin film formed include zinc, ZnSe, zinc oxide, zinc sulfide, zinc-indium composite oxide, lithium-doped zinc oxide, zinc-doped fly, lead-zinc composite oxide, and lead-zinc oxide.
• Niobium composite oxides bismuth zinc-niobium composite oxides, and norium-zinc-tantalum composite oxides are examples of the use of these thin films, for example, transparent conductors, luminescent materials, phosphors, photocatalysts, Examples include a magnetic substance, a conductor, a high dielectric substance, a ferroelectric substance, a piezoelectric substance, a microwave dielectric substance, an optical waveguide, an optical amplifier, and an optical switch.
• the bis ( ⁇ -diketonato) zinc conjugate according to the present invention is a liquid at 25 ° C., and therefore is useful as a raw material for forming a thin film from the following viewpoints.
• the supply amount does not change with time due to clogging of the piping and the like, and a thin film can be manufactured with a stable deposition rate and a stable control of the thin film composition. Further, in the manufacturing process of the raw material for forming a thin film, operations such as synthesis, purification, and transfer and filling are facilitated.
• the melting point of bis (pentane-2,4 dionato) zinc is around 137 ° C
• the melting point of 2,6,6-tetramethylheptane-3,5 dionato) zinc is around 142 ° C
• that of bis (2,6 dimethylheptane 3,5 dionato) zinc is 82 ° C.
• the precursor when the precursor is a solid, when applying the precursor solution as a raw material for forming a thin film, coating unevenness or pinholes due to deposition may occur.
• the precursor when the precursor is solid, storage of the precursor solution, which is a raw material for forming a thin film, is prevented. In some cases, solids are deposited. Since the bis ( ⁇ 8-diketonato) zinc conjugate according to the present invention is a liquid at 25 ° C., these problems can be avoided, and the precursor concentration in the raw material for forming a thin film is high, and the precursor can be widely set. It becomes possible.
• the bis (j8-diketonato) zincide conjugate according to the present invention is more useful if it has high fluidity.
• the bis (j8-diketonato) zincide has a viscosity at 25 ° C of 2000 mPa's or less. Those are preferred.
• 8-diketonato) zinc conjugate according to the present invention may be increased by heating the supply line. In this case, it is advantageous to obtain a large fluidity by heating as small as possible, and specifically, a material having a viscosity of 200 mPa's or less at 50 ° C is preferable.
• the preferred bis ( ⁇ -diketonato) zinc conjugates exhibiting viscosity include, for example, bis
• a well-known general method for synthesizing a ⁇ -diketone metal complex which is not particularly limited, can be used.
• an inorganic salt such as chloride, bromide, iodide, nitrate and sulfate of zinc
• an organic acid salt such as acetate, or a hydrate thereof
• the corresponding ⁇ -diketone compound are converted to sodium hydroxide.
• alkoxides of low molecular weight alcohols such as methoxide, ethoxide, isopropoxide and butoxide of zinc, or dimethylamide, getylamide and dibutyl of zinc. It may be produced by an exchange reaction between a low molecular organic amide such as an amide and a corresponding ⁇ -diketone conjugate.
• the embodiment of the raw material for forming a thin film according to the present invention is a method for manufacturing a thin film to which the raw material for forming a thin film is applied (for example, a fire deposition method, a sputtering method, an ion plating method, a coating thermal decomposition method, or a sol-gel method).
• a fire deposition method for example, a fire deposition method, a sputtering method, an ion plating method, a coating thermal decomposition method, or a sol-gel method.
• MOD method for a chemical vapor deposition method
• CVD method including ALD method Since the bis ( ⁇ 8-diketonato) zinc conjugate according to the present invention can be easily vaporized, the thin film forming raw material of the present invention is particularly useful as a chemical vapor deposition raw material.
• the raw material for forming a thin film of the present invention is a raw material for chemical vapor deposition (CVD)
• its form is appropriately selected depending on a method such as a transport and supply method of a CVD method to be used.
• a CVD raw material is heated in a raw material container and Z or depressurized.
• Gas transport method in which a carrier gas such as argon, nitrogen, helium, etc., used as necessary, is introduced into the deposition reaction section, and raw materials for CVD are transported to the vaporization chamber in the form of a liquid or solution and vaporized.
• a liquid transport method in which a gas is heated and vaporized by Z or reduced pressure in a chamber and introduced into a deposition reaction section.
• the bis (j8-diketonato) zinc conjugate according to the present invention itself is used as a raw material for CVD
• the bis (diketonato) zinc conjugate according to the present invention itself is used.
• a solution obtained by dissolving the zinc-containing compound in an organic solvent is a raw material for CVD.
• a method of vaporizing and supplying a CVD raw material independently for each component (hereinafter, also referred to as a single source method) and a method of using a multi-component raw material.
• a method of vaporizing and supplying a mixed raw material previously mixed with a desired composition (hereinafter, also referred to as a cocktail sauce method).
• a cocktail sauce method a mixture of the bis (j8-diketonato) zinc compound according to the present invention and a metal compound as another precursor, or a mixed solution obtained by dissolving these compounds in an organic solvent is a raw material for CVD.
• organic solvent used for the above-mentioned raw material for CVD known general organic solvents which are not particularly limited can be used.
• organic solvent include alcohols such as methanol, ethanol, 2-propanol, and n-butanol; acetates such as ethyl acetate, butyl acetate, and methoxyethyl acetate; ethylene glycol monomethyl ether and ethylene glycol monoethylene.
• Ether alcohols such as aethenole, ethylene glycol monobutynole ether, diethylene glycol monomethyl ether; ethers such as tetrahydrofuran, tetrahydropyran, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, dibutyl ether; methyl butyl Ketone, methyl isobutyl ketone, ethyl butyl ketone, dipropyl ketone, diisobutyl ketone, methyl amyl ketone, Ketones such as chlorohexanone and methylcyclohexanone; hydrocarbons such as hexane, cyclohexane, methylcyclohexane, dimethylcyclohexane, ethylcyclohexane, heptane, octane, toluene and xylene; 1 cyanopropane, 1
• the total amount of the bis ( ⁇ -diketonato) zinc compound and the other precursor in the organic solvent is from 0.01 to 2.0 moles, particularly from 0.05 to 0.5%. / Let's get to the point! / ,.
• precursors used together with the bis ( ⁇ -diketonato) zinc compound according to the present invention in the case of a multi-component CVD method are not particularly limited and may be used as a raw material for CVD.
• a known general precursor can be used.
• Examples of the other precursor include one or more kinds of organic coordination compounds selected from alcohol compounds, glycol compounds, ⁇ -diketone compounds, cyclopentadiene compounds, and organic amine compounds. Examples thereof include compounds with metals, alkyl metal compounds, and aryl metal compounds.
• the metal species of the precursor include, for example, magnesium, calcium, strontium, norium, titanium, zirconium, hafdium, vanadium, niobium, tantalum, manganese, iron, ruthenium, cobalt, rhodium, iridium, nickel, ⁇ Radium, platinum, copper, silver, gold, gallium, indium, germanium, tin, lead, antimony, bismuth, silicon, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium pium, gadolinium, terbium, Examples include dysprosium, holmium, erbium, thulium, and ytterbium.
• Examples of the alcohol conjugate used as the organic ligand include methanol, ethanol, propanol, isopropanol, butanol, 2-butanol, isobutanol, tert-butanol, amyl alcohol, isoamyl alcohol, Alkyl alcohols such as tertiary amyl alcohol; 2-methoxyethanol, 2-ethoxyethanol, 2-butoxyethanol, 2- (2-methoxyethoxy) ethanol, 2-methoxy-1-methylethanol, 2-methoxy-1,1 -Dimethylethanol, 2-ethoxy 1,1-dimethylethanol, 2-isopropoxy 1,1-dimethylethanol, 2-butoxy-1,1-dimethylethanol, 2- (2-methoxyethoxy) 1,1-dimethylethanol , 2-Propoxy-1, 1-Jetylethanol, 2 Second Butoki Ether alcohols such as 1,1-dimethylethylethanol and 3-methoxy-1,1-dimethylpropanol; dial
• glycolide conjugate used as the organic ligand examples include 1,2 ethanediol, 1,2 propanediol, 1,3 propanediol, 2,4 hexanediol, and 2,2 dimethyl diol.
• Examples of the above j8-diketone conjugate used as an organic ligand include acetylacetone, hexane 2,4 dione, 5-methylhexane 2,4 dione, heptane 2,4-dione, 2 Methylheptane 3,5 dione, 5 methylheptane 2,4 dione, 6 methylheptane 2,4 dione, 2,2 dimethylheptane 3,5 dione, 2,6—dimethylheptane-1,3,5 dione, 2,2,6 Trimethylheptane-1,3,5 dione, 2,2,6,6-tetramethylheptane-1,3,5 dione, octane-1,2,4 dione, 2,2,6—Trimethyloctane 3,5 dione, 2,6 dimethyloctane Alkyl-substituted j8-diketones such as 3,5 dione, 2,9 dimethylnonane 4,6 dione 2-methyl-6-ethyldecane 3,5 dione, 2,
• Examples of the above cyclopentadiene compound used as the organic ligand include cyclopentadiene, methylcyclopentadiene, ethylcyclopentadiene, provylcyclopentadiene, isopropylcyclopentadiene, butylcyclopentadiene, Sec-butyl Clopentadiene, isobutylcyclopentadiene, tertiary butylcyclopentadiene, dimethylcyclopentadiene, tetramethylcyclopentadiene and the like can be mentioned.
• Examples of the above-mentioned organic amine conjugate used as an organic ligand include methylamine, ethylamine, propylamine, isopropylamine, butylamine, sec-butylamine, disanbutylamine, isobutylamine, dimethylamine, getylamine, diamine.
• Examples thereof include propylamine, diisopropylamine, ethylmethylamine, propylmethylamine, and isopropylmethylamine.
• Examples of the alkyl group of the above alkyl metal compound include methyl, ethyl, propyl, isopropyl, butyl, sec-butyl, tert-butyl, isobutyl, pentyl, tert-pentyl, and isopentyl.
• examples of the aryl group of the above aryl metal compound include, but are not limited to, ethyl, methyl, dimethyl, and ethyl.
• the thin film forming raw material of the present invention is required, if necessary, in order to impart stability to the bis (
• a nuclear reagent may be contained.
• the nucleophilic reagent include ethylene glycol ethers such as glyme, diglyme, triglyme and tetraglyme, 18 crown-6, dicyclohexyl-18-crown-6, 24 crown-18, and dicyclohexyl-24 crown-1.
• crown ethers such as dibenzo-24 crown-18, ethylenediamine, ⁇ , ⁇ '-tetramethylethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, 1,1,4,7 7
• Polyamines such as pentamethylmethylethylenetriamine, 1,1,4,7,10,10hexamethyltriethylenetetramine, cyclic polyamines such as cyclam and cyclen, methyl acetoacetate, methyl acetoacetate, acetoacetic acid 2 -Ketoesters such as methoxyethyl or acetylaceto J8-diketones such as 2,4-hexanedione, 2,4-heptanediene, 3,5-heptandiene, dipivaloylmethane, etc., and their nucleophilicity as a stabilizer
• the amount of the reagent to be used is generally 0.1 mol to 10 mol, preferably 1
• the method for producing a thin film of the present invention uses the raw material for forming a thin film of the present invention as a raw material for CVD, and comprises a vapor containing a zinc compound obtained by vaporizing the raw material for forming a thin film of the present invention.
• the vapor of other precursors used as needed and the reactive gas used as needed are introduced on the substrate, and then the precursor is decomposed and Z or chemically reacted on the substrate. This is based on the CVD method in which a thin film is grown and deposited on a substrate.
• the method of deposition, the manufacturing conditions, the manufacturing equipment, and the like well-known general conditions and methods without any particular restrictions can be used.
• Examples of the reactive gas used as necessary include oxygen, ozone, nitrogen dioxide, nitric oxide, water vapor, hydrogen peroxide, formic acid, acetic acid, and anhydrous acetic acid as oxidizing gases.
• Hydrogen is mentioned as the reducing compound, and organic amine compounds such as monoalkylamine, dialkylamine, trialkylamine, alkylenediamine, etc. Hydrazine, ammonia and the like.
• Examples of the transport and supply method include the gas transport method, the liquid transport method, the single source method, and the cocktail sauce method.
• the above-mentioned deposition methods include thermal CVD in which a source gas or a source gas and a reactive gas are reacted only by heat to deposit a thin film, plasma CVD using heat and plasma, heat and light.
• ALD Atomic Layer Deposition
• ALD Atomic Layer Deposition which separates the deposition reaction of photo-CVD using heat, light, plasma and light plasma CVD, and the deposition reaction of CVD into elementary processes and performs step-wise deposition at the molecular level.
• Examples of the manufacturing conditions include a reaction temperature (substrate temperature), a reaction pressure, and a deposition rate.
• the reaction temperature is preferably 160 ° C. or higher, which is a temperature at which the bis ( ⁇ 8-diketonato) zinc conjugate according to the present invention sufficiently reacts, and more preferably 250 to 800 ° C.
• the reaction pressure is preferably from atmospheric pressure to 10 Pa to 2000 Pa in the case of thermal CVD or photo CVD, in the case of using plasma, which is preferably at atmospheric pressure to 10 MPa.
• the deposition rate can be controlled by the supply conditions of the raw materials (vaporization temperature, vaporization pressure), reaction temperature, and reaction pressure.
• the 0.5 to 5000 nmZ component is preferable, and the 1 to: More preferred.
• ALD it is controlled by the number of cycles so that a desired film thickness is obtained.
• a reflow step may be provided.
• the temperature in this case is usually 500 to 1200 ° C, preferably 600 to 800 ° C.
• a precursor of another component, a reactive gas and production conditions are appropriately selected for the thin film produced by the method for producing a thin film of the present invention using the raw material for forming a thin film of the present invention.
• a desired type of thin film such as a metal, an alloy, a sulfide, an oxide ceramic, a nitride ceramic, and a glass can be obtained.
• the types of thin film to be produced for example, zinc, ZnS e, zinc oxide, zinc sulfide, zinc one indium composite Sani ⁇ , Li added oxide zinc, zinc added ferrite, lead - zinc oxide, lead - Zinc-niobium composite oxide, bismuth-zinc-niobium composite oxide, barium-zinc-tantalum composite oxide, and the use of these thin films include, for example, transparent conductors, luminescent materials, Examples include a fluorescent substance, a photocatalyst, a magnetic substance, a conductor, a high dielectric substance, a ferroelectric substance, a piezoelectric substance, a microwave dielectric substance, an optical waveguide, an optical amplifier, and an optical switch.
• a reaction flask purged with dry argon was charged with 1.0 mol of octane-2,4-dione, 1.0 mol of sodium hydroxide, and lOOOOg of methanol dried to a water content of less than 5 ppm, and 600 g of methanol and nitric acid were added thereto.
• a solution of as little as 0.5 molar force of zinc hexahydrate was dropped at 25 ° C. After stirring at 25 ° C for 5 hours, the solid phase was separated by filtration, and the residue obtained by distilling off the solvent was subjected to reduced pressure distillation.
• a yellow liquid of 53 g (yield 30%) was obtained with a fractional force at a tower top temperature of 128 ° C and a pressure of 20 Pa.
• the resulting yellow liquid was identified as the desired product, bis (octane 2,4 dionato) zinc.
• the analysis results of the obtained yellow liquid are shown below.
• Viscosity measurement (falling ball method using an automatic microviscometer AMVn (manufactured by Anton Paar GmbH))
• Carbon 65.1% by mass (theoretical value 65.2%), Hydrogen: 9.0% by mass (theoretical value 9.8%), Zinc: 13.7% by mass (theoretical value 12.7%)
• Viscosity measurement (falling ball method using an automatic microviscometer AMVn (manufactured by Anton Paar GmbH)) Viscosity at 25 ° C: 1022 mPa's, Viscosity at 50 ° C: 118 mPa's
• a zinc oxide thin film was manufactured on a silicon wafer under the following manufacturing conditions.
• the film thickness and film composition of the manufactured thin film were confirmed by X-ray fluorescence. The results are shown below.
• Zinc Raw material for CVD bis (octane 2, 4 dionato) zinc [raw material temperature: 180 ° C, pressure: 666 Pa, carrier gas: argon 150 sccm], oxidizing gas: oxygen 150 sccm, reaction pressure 666 Pa, reaction temperature (base temperature) : T “t” 550 ° C, deposition time: 20 minutes
• Film thickness 84 mm; film composition; zinc oxide
• a bismuth dumbbell niobium composite oxide thin film was manufactured on a silicon wafer under the following manufacturing conditions.
• the thickness and composition of the manufactured thin film were confirmed by X-ray fluorescence. The results are shown below.
• Bismuth raw material for CVD Triphenyl bismuth [raw material temperature; 130 ° C, pressure: 666 Pa, carrier gas; argon 150 sccm], zinc raw material for CVD: bis (2,2 dimethyl-6-ethyldecane 3,5 dionato) zinc [raw material temperature 160 ° C, pressure; 666 Pa, carrier gas; argon 50 sccm], niobium CVD raw material: penta (ethoxy) niobium [raw material temperature: 120 ° C, pressure: 666 Pa, carrier gas: argon 100 sccm], oxidizing gas: Oxygen 150sccm, reaction pressure 50, reaction temperature (base temperature): 550 ° C, deposition time: 20 minutes
• Vaporization chamber temperature 230 ° C
• raw material flow rate 50sccm
• oxygen gas flow rate 350sccm
• reaction pressure 666Pa
• reaction time 10 minutes
• substrate temperature 550 ° C
• carrier gas argon 150sccm (result)
• PbZZnZNb 1.0 / 0.30 / 0.67
• the present invention it is possible to provide a raw material for forming a thin film suitable for forming a zinc-containing thin film.
• a raw material for forming a thin film By using the raw material for forming a thin film, it is possible to supply raw material gas and to transport the raw material in-line. It is possible to manufacture a thin film with stable film forming speed and thin film composition control without problems.

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