KR100202532B1 - Electronic parts of electronic device and process for fabricating the same and apparatus therewith - Google Patents
Electronic parts of electronic device and process for fabricating the same and apparatus therewith Download PDFInfo
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- KR100202532B1 KR100202532B1 KR1019930702549A KR930702549A KR100202532B1 KR 100202532 B1 KR100202532 B1 KR 100202532B1 KR 1019930702549 A KR1019930702549 A KR 1019930702549A KR 930702549 A KR930702549 A KR 930702549A KR 100202532 B1 KR100202532 B1 KR 100202532B1
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- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- 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
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/60—Deposition of organic layers from vapour phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0493—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases using vacuum
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- 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
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- 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
- C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4486—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
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- 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
- C23C16/45563—Gas nozzles
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- 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
- C23C16/46—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 heating the substrate
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- 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
- C23C16/48—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 by irradiation, e.g. photolysis, radiolysis, particle radiation
- C23C16/482—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 by irradiation, e.g. photolysis, radiolysis, particle radiation using incoherent light, UV to IR, e.g. lamps
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- 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
- C23C16/52—Controlling or regulating the coating process
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- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
- C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/68—Crystals with laminate structure, e.g. "superlattices"
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- 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
- H01L28/56—Capacitors with a dielectric comprising a perovskite structure material the dielectric comprising two or more layers, e.g. comprising buffer layers, seed layers, gradient layers
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- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
- H10N30/074—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing
- H10N30/076—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing by vapour phase deposition
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- H—ELECTRICITY
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- 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
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- 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
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/105—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern by conversion of non-conductive material on or in the support into conductive material, e.g. by using an energy beam
Abstract
본 발명은 기판상에 착화합물을 빠른 속도로 증착시키는 방법 및 장치에 관한 것이다. 즉, 증착 챔버(2)내에서 기판(5)상에 화학적 화합물의 박막을 증착시키는 방법 및 장치(1)에 관한 것이다. 박막 증착 방법은 다음의 단계를 포함한다 : 바람직한 화학적 화물의 적어도 하나의 안정화 용액 및 용매를 형성시키는 단계, 증착 챔버(2) 내부에 기판(5)을 공급하는 단계, 초음파 장치(46)를 사용하여 안정화 용액의 미스트를 생산하는 단계, 미스트가 기판(5)상에 안정화 용액층을 형성하여 증착하도록 독특한 노즐 장치(8,10)를 사용해서 기판에 근접하여 증착 챔버(2) 내로 미스트를 유입시키는 단계.The present invention relates to a method and apparatus for rapidly depositing a complex on a substrate. That is, the present invention relates to a method and an apparatus 1 for depositing a thin film of a chemical compound on a substrate 5 in a deposition chamber 2. The thin film deposition method includes the following steps: forming at least one stabilization solution and a solvent of the desired chemical cargo, supplying the substrate 5 inside the deposition chamber 2, using the ultrasonic device 46 Producing a mist of the stabilization solution by introducing a mist into the deposition chamber 2 in proximity to the substrate using a unique nozzle arrangement 8, 10 so that the mist forms and deposits a stabilization solution layer on the substrate 5. Step.
Description
[발명의 명칭][Name of invention]
전자 디바이스 내의 전자 부품 제조방법 및 그 장치Method for manufacturing electronic components in electronic device, and apparatus therefor
[발명의 분야][Field of Invention]
본 발명은 전자 디바이스 내의 전자 부품 제조방법 및 그 장치에 관한 것으로, 착화합물의 고품질 박막을 기판(substrate)상에 빠른 속도로 증착시키기 위한 방법 및 이러한 방법에 효과적인 장치에 관한 것이다.TECHNICAL FIELD The present invention relates to a method for manufacturing an electronic component in an electronic device and an apparatus therefor, and to a method for rapidly depositing a high quality thin film of a complex on a substrate and to an apparatus effective for such a method.
특히, 본 발명은 비반응성의 화학 증착법(CVD) 및 안정화된 액체 화합물 소오스(source)를 이용한, 착화합물의 고품질이고 화학량적으로 보정된 박막을 빠른 속도로 증착시키기 위한 장치에 관한 것이다.In particular, the present invention relates to an apparatus for rapidly depositing high quality and stoichiometrically corrected thin films of complexes using non-reactive chemical vapor deposition (CVD) and stabilized liquid compound sources.
[관련기술의 설명][Description of Related Technology]
산화금속, 강유전체, 초전도체, 높은 유전상수를 가지는 물질, 보석등과 같은 착학합물의 박막을 증착시키는 방법은 공지되어 있다. 공지된 방법으로는 진공 증착(예를들면 E-빔(beam), 레이저 애블레이션(laser ablation) 등) ; 진공스퍼터링(sputtering) (예를들면 E-빔, D.C., R,F., 이온-빔 등) ; 분말 야금 ; 반응성의 화학 증착 ; 및 액체 도포법(예를들면 스핀-온 기술, 침지 및 분무)이 있다. 그러나, 이러한 공지된 방법들 모두는 그에 관련된 상당한 문제점을 갖는다.Methods of depositing thin films of complexes such as metal oxides, ferroelectrics, superconductors, materials with high dielectric constants, gemstones and the like are known. Known methods include vacuum deposition (eg, E-beams, laser ablation, etc.); Vacuum sputtering (eg E-beam, D.C., R, F., ion-beam, etc.); Powder metallurgy; Reactive chemical vapor deposition; And liquid application methods (eg spin-on techniques, dipping and spraying). However, all of these known methods have significant problems associated with them.
본 발명은 앞서 논의된 방법들을 포함하는, 화학적 착화합물의 박막을 증착시키기 위한 공지된 증착 기술과 관련된 많은 문계점 및 단점을 극복하기 위한 것이며, 강유전체, 초전도체, 및 산화금속과 같은 다양한 착화합물의 박막(그 두께가 몇몇 옹스트롬 내지 미크론인)을 쉽고 경제적으로 생산할 수 있는 가치있는 생산 공정을 제공함으로써 기술적인 많은 요구들을 충족시키도록 전개되어 왔다.The present invention seeks to overcome many of the problems and shortcomings associated with known deposition techniques for depositing thin films of chemical complexes, including the methods discussed above, and to provide thin films of various complexes such as ferroelectrics, superconductors, and metal oxides. It has been developed to meet many technical demands by providing a valuable production process that can produce several angstroms to microns in thickness easily and economically.
[도면의 간단한 설명][Brief Description of Drawings]
제1도는 본 발명의 제1실시 형태에 따른 CVD 장치의 개략도이고,1 is a schematic diagram of a CVD apparatus according to a first embodiment of the present invention,
제2도는 노즐 조립체 및 제1도의 실시 형태에서 사용된 배기 조립체의 확대 단면도이고,2 is an enlarged cross-sectional view of the nozzle assembly and the exhaust assembly used in the embodiment of FIG.
제3도는 본 발명의 제1및 제2실시 형태에서 사용된 다기관 시스템의 확대 개략도이고,3 is an enlarged schematic diagram of the manifold system used in the first and second embodiments of the present invention,
제4도는 본 발명에 따른 안정화된 용액의 미스트(mist)를 형성시키는 바람직한 장치의 종단면도이고,4 is a longitudinal sectional view of a preferred device for forming a mist of a stabilized solution according to the invention,
제5a도 및5b도는 제4도의 장치의 변형을 나타낸 것이고,5a and 5b show a variant of the device of FIG. 4,
제6도는 본 발명에 따른 티탄산 납 지르코늄의 박막 형성에 사용한 안정화된 용액의 제법을 나타내는 개략적 공정도이다.6 is a schematic process diagram showing the preparation of a stabilized solution used to form a thin film of lead zirconium titanate according to the present invention.
[발명의 상세한 설명]Detailed description of the invention
본 발명의 주 양상에 따라, 우선 바람직한 화학적 화합물의 안정화된 소오스 또는 안정화된 용액을 제조하고 이 용액의 증기를 생성시켜 증착 챔버내로 흘려넣는다. 그러면 증착 챔버 내에 배치된 기판 상에 박막/층이 증착된다.According to the main aspect of the present invention, a stabilized source or stabilized solution of a preferred chemical compound is first prepared and the vapor of the solution is produced and flowed into a deposition chamber. The thin film / layer is then deposited onto the substrate disposed in the deposition chamber.
안정화된 용액으로는 적어도 공지된 액체 도포 기술에서 사용하는 것들이 모두 포함되고 특히 (용매 기제로 알콜을 포함하는) 졸-겔, (용매 기제로 n-데칸산을 사용하는) 금속유기 분해(MOD) 제제형, 용매 기제로 물을 가지는 용액, 용매기계로 카르복시산을 가지는 용액 등이 포함된다.Stabilized solutions include at least all those used in known liquid application techniques, in particular sol-gels (including alcohol as solvent base), metalorganic decomposition (MOD) using n-decanoic acid as solvent base). Formulation forms, solutions with water as solvent base, solutions with carboxylic acid as solvent machine, and the like.
본 명세서에서 사용하는 안정화된 소오스 란 용어는, 졸-겔 기술 또는 기타의 습식 화학 혼합 기술을 사용하여 공통 용매를 이끌어 낸 후 전체 화합물의 유일한 소오스로 이 공통 용매를 가지는 용액을 사용하여 각 원소의 전구체를 혼합함으로써 수득한 소오스를 나타낸다. 또한 그밖의 소오스는 화합물의 도핑이나 변형에 사용할 수 있다. 안정화된 소오스에서, 각 원소는 이미 공통 용매 또는 금속 유기 전구체를 가지는 용액 내의 화합물에 존재한다.As used herein, the term stabilized source is used to derive a common solvent using sol-gel techniques or other wet chemical mixing techniques, and then use a solution having this common solvent as the sole source of the entire compound to The source obtained by mixing precursors is shown. Other sources may also be used for doping or modifying the compound. In a stabilized source, each element is present in a compound in solution already having a common solvent or metal organic precursor.
안정학된 용액의 사용은 많은 이유로 매우 바람직하다. 첫째, 착화합물 조차도 소오스 자체가 비교적 쉽게 발생한다. 이 점에 관하여는, 앞서 논의된 대로 박막을 형성하는 공지된 액체 도포 방법에 관련하여 사용하는 다양한 졸-겔 제조 기술, MOD 제제형 기술을 설명한 많은 공고문헌이 있다. 그러한 문헌 중의 하나인, Process Optimization and Characterization of Device Worthy Sol-gel Based PZT for Ferroelectric Memories는 본 출원의 발명자 2명과 그 외의 사람들에 의해 저술되었고, FERROELECTRICS, Vol. 109에 나타나 있다. 논의된 문헌은 참고로 삽입하였다.The use of stabilized solutions is very desirable for many reasons. First, even the complex itself occurs relatively easily. In this regard, there are a number of publications describing the various sol-gel preparation techniques, MOD formulation techniques used in connection with known liquid application methods for forming thin films as discussed above. One such document, Process Optimization and Characterization of Device Worthy Sol-gel Based PZT for Ferroelectric Memories, has been authored by two inventors and others of the present application and described in FERROELECTRICS, Vol. It is shown at 109. The documents discussed are incorporated by reference.
본 발명에 사용하는 안정화된 용액은 또한 실짙적으로 독성이 약하고 앞서 논의된 CVD 방법 등에서 통상적으로 사용하는 반응물 보다 취급이 용이하므로, 이러한 안정화된 용액은 상응하는 반응물에 비해 더 적은 비용으로 취급 및 처리가 가능하다.Stabilized solutions for use in the present invention are also substantially less toxic and easier to handle than the reactants commonly used in CVD methods and the like discussed above, so such stabilized solutions are handled and treated at less cost than the corresponding reactants. Is possible.
게다가, 안정화된 소오스의 사용은 고품질 박막의 생산을 보증하는데, 이는 안정화된 소오스가 정확하게 지속적으로 생산되어 그에 함유된 바람직한 화학적 화합물이 균일하게, 화학량적으로 보정되기 때문이며, 본 발명의 증착 방법이 분자 제제형의 화학적 화합물을 불안정하게 하는 어떠한 화학 반응도 포함하지 않기 때문이다. 대신에, 안정화된 소오스의 박막은 분위기 온도(ambient temperature)에서 진공하에 증기로부터 기판상에 직접 증착시키고 이어서 건조시킨다.In addition, the use of stabilized sources ensures the production of high quality thin films because the stabilized sources are accurately and continuously produced so that the desired chemical compounds contained therein are uniformly and stoichiometrically corrected, and the deposition method of the present invention is a molecular This is because it does not contain any chemical reactions that destabilize chemical compounds of the formulation. Instead, a thin film of stabilized source is deposited directly from the vapor onto the substrate under vacuum at ambient temperature and then dried.
제1도는 본 발명의 바람직한 실시 형태에 따른 박막 증착장치를 나타내는데, 장치는 1로 표시하였다. 증착 장치(1)는 일반적으로 증착 챔버(2), 기판 지지구(4), 장벽 판(6), 노즐 조립체(8), 및 배기 조립체(10)를 포함한다.1 shows a thin film deposition apparatus according to a preferred embodiment of the present invention. The deposition apparatus 1 generally comprises a deposition chamber 2, a substrate support 4, a barrier plate 6, a nozzle assembly 8, and an exhaust assembly 10.
증착 챔버(2)는 본체(12), 증착 챔버 내부의 둘러싸인 공간으로 규정되는 본체를 보호하는 덮개(14)를 포함하며, 이 증착 챔버(2)는 일반적으로 16에 나타낸 것과 같은 적절한 진공 소오스(도시되지 않음)와 연결된다. 덮개(14)는 18에 나타낸 것과 같은 힌지를 사용하여 본체(12)와 바람직하게 연결시킨다.The deposition chamber 2 includes a body 14, a cover 14 which protects the body defined by the enclosed space inside the deposition chamber, which is generally a suitable vacuum source as shown in FIG. Not shown). The lid 14 is preferably connected to the body 12 using a hinge as shown in 18.
기판 지지구(4)는 회전 축(20) 상에서 바람직하게 지탱되며 차례로 모터(도시되지 않음)에 연결되어 증착 공정시 회전할 수 있게 된다. 22에 나타낸 것은 23에 나타낸 DC/RF 이송관통기를 사용하여 기판 지지구(4)와 장벽 판(6)사이에 DC 또는 AC(RF) 바이어스를 발생시킬 수 있도록, 증착 장치(1)의 받침대로부터 기판(5) 및 기판 지지구(4)를 전기적으로 절연시키는 절연 접속기이다. 이러한 DC바이어스는 예를들어 박막을 기판(5) 상에 증착시킬 때 이 박막의 필드-폴링(field-poling)에 사용할 수 있다. 효과적인 DC 바이어스를 위해 전기적 소오스(도시되지 않음)는 장벽 판(5) 및 기판 지지구(4)를 가로질러 작동적으로 연결될 것이다.The substrate support 4 is preferably supported on the rotation axis 20 and in turn connected to a motor (not shown) so that it can rotate during the deposition process. Shown in FIG. 22 is from the pedestal of deposition apparatus 1 so that a DC or AC (RF) bias can be generated between the substrate support 4 and the barrier plate 6 using the DC / RF transfer through shown in 23. It is an insulated connector which electrically insulates the board | substrate 5 and the board | substrate support tool 4. Such a DC bias can be used for field-poling of the thin film, for example when depositing the thin film on the substrate 5. An electrical source (not shown) will be operatively connected across the barrier plate 5 and substrate support 4 for effective DC bias.
장벽 판(6)은 스테인레스 스틸과 같은 전기적 전도 물질로 제조하며, 이에 평행한 기판(5)을 완전히 덮을만한 충분히 큰 크기로 제조하여 노즐 조립체(8)에 의하여 분사되는 증기 소오스 또는 미스트가 장벽 판(6) 및 기판(5) 전면의 기판 지지구(4) 사이에 흐르도록 한다. 도시한 바와 같이, 장벽 판(5)은 축(24)에 의해 덮개(14)와 연결되어 덮개가 열릴때 마다 기판(5)으로부터 멀리 이동하게 된다. 축(24)의 길이는 조절이 가능하여 기판 지지구(4) 및 장벽 판(6)사이의 공간이 소오스 물질, 유동률 등에 의해 조절될 수 있도록 한다. 예를들면, 그 공간은 2-50mm 범위 내에서 조절이 가능하다.The barrier plate 6 is made of an electrically conductive material such as stainless steel, and is made large enough to completely cover the substrate 5 parallel thereto so that the vapor source or mist sprayed by the nozzle assembly 8 is free of the barrier plate. It flows between 6 and the board | substrate support 4 of the board | substrate 5 front surface. As shown, the barrier plate 5 is connected to the cover 14 by a shaft 24 so that it moves away from the substrate 5 each time the cover is opened. The length of the shaft 24 is adjustable such that the space between the substrate support 4 and the barrier plate 6 can be adjusted by source material, flow rate, or the like. For example, the space can be adjusted within the range of 2-50 mm.
특별히 노즐 조립체(8) 및 배기 조립체(10)는 제2도에 도시하였다. 도시한 바와 같이, 노즐 조립체(8)는 제3도와 관련하여 아래에서 논의되는 바와 같이 다기관 조립체(40)로부터 증기 소오스를 받아들이는 투입관(26)과 아치형의 노즐 관(28)을 포함하는데, 이 노즐 관(28)은 증착 챔버(2)의 내부로 향해 있으며 표면을 따라 일정한 간격으로 배치된 제거 가능한 나사(30)와 함께 다수의 작은 구멍(29)을 갖는다. 나사(30)는 기판(5) 전면의 증기 소오스의 흐름을 조절하기 위해 안정화된 소오스, 유동률 등에 따라 선택적으로 제거 할 수 있다. 32에 나타낸 것은 노즐 관(28)의 말단 캡이다. 배기 조립체(10)의 구조는 파이프(34)가 진공-배기 소오스(도시되지 않음)에 이른다는 것을 제외하면 실질적으로 노즐 조립체(8)의 구조와 동일하다. 도시된 바와 같이, 노즐 조립체(8)의 아치형 노즐 관(28)과 배기 조립제(10)의 상응하는 아치형관(33)은 기판(5) 주위에서 서로 대향되어 있고, 기판(5)중심부의 맞은편에서 서로 일정한 간격으로 배치된다.In particular, the nozzle assembly 8 and the exhaust assembly 10 are shown in FIG. As shown, the nozzle assembly 8 includes an input tube 26 and an arcuate nozzle tube 28 that receive a vapor source from the manifold assembly 40 as discussed below in connection with FIG. This nozzle tube 28 is directed into the deposition chamber 2 and has a number of small holes 29 with removable screws 30 arranged at regular intervals along the surface. The screw 30 may be selectively removed according to the stabilized source, flow rate, etc. to control the flow of the vapor source on the front surface of the substrate 5. Shown at 32 is the end cap of the nozzle tube 28. The structure of the exhaust assembly 10 is substantially the same as that of the nozzle assembly 8 except that the pipe 34 reaches a vacuum-exhaust source (not shown). As shown, the arcuate nozzle tube 28 of the nozzle assembly 8 and the corresponding arcuate tube 33 of the exhaust assembly 10 are opposed to each other around the substrate 5 and the center of the substrate 5 is formed. They are arranged at opposite intervals from each other.
이러한 구조를 통하여, 두 아치형 관내의 개구(29, 31)의 위치를 조절함으로써, 기판(5) 전면의 증기 소오스 또는 미스트의 흐름을 다양한 소오스, 다양한 유동률 등으로 제어할 수 있게되어 기판(5) 상에 균일한 박막의 증착이 이루어진다.Through this structure, by adjusting the positions of the openings 29 and 31 in the two arcuate tubes, it is possible to control the flow of the vapor source or the mist in front of the substrate 5 with various sources, various flow rates, and the like. A uniform thin film is deposited on the phase.
제1도 및 2도에서, 기판 지지구(4), 장벽 판(6), 노즐조립체(8) 및 배기 조립체(10)는 기판(5)의 표면을 둘러싸는 비교적 작은 증착 공동(cavity)을 규정지으며, 증기 소오스는 실질적으로 증착 공정을 통하여 포함된다.In FIGS. 1 and 2, the substrate support 4, the barrier plate 6, the nozzle assembly 8, and the exhaust assembly 10 form a relatively small deposition cavity surrounding the surface of the substrate 5. As defined, the vapor source is substantially included through the deposition process.
기판 지지구(4), 장벽 판(6), 노즐 조립체(8) 및 배기 조립체(10)의 바람직한 형태가 나타나 있지만, 이러한 구조가 변형된 형태도 본 발명의 범주 내에서 사용할 수 있다. 예를들면, 아치형 노즐 관(28) 및 배기관은 V-형 관 또는 U-형 관과 같은 다른 구조의 관으로 대용할 수 있으며, 또는 다수의 분리 노즐 및 분리배기구로 대용할 수 있다.While the preferred forms of the substrate support 4, barrier plate 6, nozzle assembly 8 and exhaust assembly 10 are shown, variations of this structure may be used within the scope of the present invention. For example, the arcuate nozzle tube 28 and the exhaust pipe may be substituted for other structures such as V-shaped pipes or U-shaped pipes, or may be substituted for a plurality of separate nozzles and separate exhaust pipes.
제3도에는, 본 발명에 따른 다기관 조립체(40)를 나타내었다. 다기관 조립체(40)는 증기 소오스를 노즐조립체(8)로 공급하는데에 사용하며, 일반적으로 혼합 챔버(42), 각각의 밸브(48)를 통하여 상응하는 소오스 발생기(46)와 연결된 다수의 유입구(44), 혼합 챔버(42)로부터 노즐 조립체(8)로의 유량을 조절하는 밸브(50) 및 배기밸브(52)를 포함한다. 그 용도를 보면, 하나 또는 그 이상의 소오스 발생기(46)는 하나 또는 그 이상의 다양한 증기 소오스 또는 미스트를 발생시켜서, 밸브(48) 및 유입구(44)를 통하여 혼합 챔버(42)로 흐르게 한다. 혼합 챔버(42)로 흘러들어 간 증기 소오스는 균일한 증기 소오스 또는 미스트를 형성하도록 혼합되어 밸브(50)의 조절에 의한 적절한 유동률로 증착 챔버(2)로 이동한다. 안정화된 액체 소오스의 증착 막을 건조시키거나, 필요시 증착 챔버 내부의 불순물을 제거하기 위하여 증착 챔버(2) 내부의 기체를 배출할 수 있도록 밸브(50)는 선택적으로 잠글 수 있다. 유사하게, 배기 밸브(52)의 출구는 진공 소오스(도시되지 않음)에 연결되어 있으므로 필요시 하나 이상의 소오스 발생기(46)와 혼합 챔버 내부의 불순물을 제거하기 위하여 뱉브(50)은 잠그고, 밸브(52)와 하나 이상의 밸브(48)은 열어서 혼합 챔버(42) 내부의 기체를 배출할 수 있다.3 shows a manifold assembly 40 according to the present invention. The manifold assembly 40 is used to supply the vapor source to the nozzle assembly 8 and generally includes a plurality of inlets connected to the corresponding source generator 46 through the mixing chamber 42, each valve 48. 44, a valve 50 and an exhaust valve 52 that regulate the flow rate from the mixing chamber 42 to the nozzle assembly 8. In its use, one or more source generators 46 generate one or more various vapor sources or mists, which flow through the valve 48 and inlet 44 into the mixing chamber 42. The vapor source flowing into the mixing chamber 42 is mixed to form a uniform vapor source or mist and is transferred to the deposition chamber 2 at an appropriate flow rate by adjustment of the valve 50. The valve 50 may be selectively locked to allow the gas inside the deposition chamber 2 to be evacuated to dry the deposited film of the stabilized liquid source or to remove impurities within the deposition chamber if necessary. Similarly, the outlet of the exhaust valve 52 is connected to a vacuum source (not shown), so that if necessary, the spit 50 is locked to remove impurities in the one or more source generators 46 and the mixing chamber, and the valve ( 52 and one or more valves 48 may be opened to vent gas within the mixing chamber 42.
미스트는 분위기 온도 또는 실온보다 약간 높은 온도에서 다기관 조립제(40)로부터 노즐 조립체(8)로 흐르게 하는 것이 바람직하다.It is desirable for the mist to flow from the manifold assembly 40 to the nozzle assembly 8 at an ambient temperature or slightly above room temperature.
제4도에는, 본 발명에 따른 바람직한 소오스 발생기(46)가 나타나있다. 소오스 발생기(46)는 밀폐된 용기(54), 용기(54) 바닥의 유체와 밀착된 초음파 변환기(55), 용기(56)가 진공 상태로 유지되는 동안 졸-겔 또는 MOD 제제형과 같은 안정화된 액체 소오스를 용기(54)내로 유입시키는 밸브(58), 및 용기(54)를 통하여 운반 기체를 통과시키는 유입구(60)와 출구(62)를 포함한다. 용도를 보면, 안정화된 액체 소오스(64)는 밸브(58)틀 통하여 수준-검출 수단(도시되지 않음)에 의해 측정한 바와 같은 적절한 수준까지 용기(54)로 유입될 것이고, 초음파 변환기(56)는 안정화된 액체 소오스의 미스트(66)를 발생시키도록 활성화되며, 적절한 운반 기체는 유입구(60), 출구(62)를 거쳐 미스트(66)를 통과하여 습식화 또는 포화되고, 습식운반 기체는 앞에서 논의한대로 출구(62)에서 다기관 조립체(40)로 이동한다. 운반 기체는 보통 아르곤이나 헬륨과 같은 비활성 기체이지만 적절한 상황에서는 반응성있는 기체도 포함된다. 밸브(58)는 용기(54)내의 적절한 수준으로 안정화된 액체 소오스(64)를 유지하기 위해 필요시 선택적으로 작동될 것이다.4, a preferred source generator 46 according to the present invention is shown. The source generator 46 is stabilized, such as a sol-gel or MOD formulation, while the closed vessel 54, the ultrasonic transducer 55 in close contact with the fluid at the bottom of the vessel 54, and the vessel 56 are kept in vacuum. A valve 58 for introducing the prepared liquid source into the vessel 54, and an inlet 60 and an outlet 62 for passing the carrier gas through the vessel 54. In use, the stabilized liquid source 64 will enter the vessel 54 through the valve 58 to an appropriate level as measured by level-detecting means (not shown), and the ultrasonic transducer 56 Is activated to generate a mist 66 of stabilized liquid source, a suitable carrier gas is wetted or saturated through mist 66 via inlet 60, outlet 62, and the wet carrier gas is Move from outlet 62 to manifold assembly 40 as discussed. The carrier gas is usually an inert gas such as argon or helium, but also includes reactive gases under appropriate circumstances. The valve 58 will optionally be operated as needed to maintain the stabilized liquid source 64 in the vessel 54.
제4도에 나타난 바람직한 소오스 발생기(46)는 냉동과 같은 복잡함 없이 증착 쳄버(2)내로 효과적인 주입이 가능한 증기 소오스를 발생해 내기 때문에 매우 유익하다.The preferred source generator 46 shown in FIG. 4 is very beneficial because it produces a vapor source that can be effectively injected into the deposition chamber 2 without the complexity of refrigeration.
제5a도에는 제4도에 나타난 소오스 발생기(46)의 변형된 형태인 소오스 발생기(46')가 나타나있는데, 이에 따라 초음파 변환기(56)는 안정화된 액체 소오스(64)와 접촉하지 않는다. 대신, 안정화된 액체 소오스(54)는 밀폐 용기(54')내에 포함되고 초음파 변환기(56)는 개방 용기(68)의 바닥 벽에 고정되며, 물이나 기타 액체와 같은 작용 매체(70)는 변환기 전면의 개방 용기(58)에 배치된다. 그리고, 밀폐 용기(54')는 작용 매체(70)의 상부면에서 일정한 거리를 두고 배열되어 초음파 변환기(56)에 의해 생성된 작용 매체의 미스트 기둥(72)이 밀폐 용기의 바닥벽과 접촉하게 된다. 그에 의하여 밀폐 용기(54') 내에 안정화된 액체(64)의 미스트(66)가 생성되고 이것은 제4도와 관련하여 앞에서 논의한 바와 동일한 방식으로 다기관 조립체(40)에 흘러간다. 제5도에 나타난 변형된 소오스발생기(46')는 제4도에 나타낸 소오스 발생기(46)의 잇점을 모두 가지고 있을 뿐 아니라 초음파 변환기(56)가 바람직한 박막을 형성하는데 사용하는 안정화된 액체에 오염되지 않는다는 부가적인 잇점까지 가진다.5A shows a source generator 46 'which is a modified form of the source generator 46 shown in FIG. 4, so that the ultrasound transducer 56 is not in contact with the stabilized liquid source 64. FIG. Instead, a stabilized liquid source 54 is contained within the closed vessel 54 'and the ultrasonic transducer 56 is fixed to the bottom wall of the open vessel 68, and the working medium 70, such as water or other liquid, It is arranged in the open container 58 of the front surface. And, the sealed container 54 'is arranged at a constant distance from the upper surface of the working medium 70 so that the mist pillar 72 of the working medium produced by the ultrasonic transducer 56 contacts the bottom wall of the closed container. do. This produces a mist 66 of stabilized liquid 64 in a sealed container 54 'that flows to the manifold assembly 40 in the same manner as discussed above in connection with FIG. The modified source generator 46 'shown in FIG. 5 not only has all the advantages of the source generator 46 shown in FIG. 4 but also contaminates the stabilized liquid that the ultrasonic transducer 56 uses to form the desired thin film. It has the additional advantage of not being.
제5b도에는 제4도의 미스트 발생 장치가 변형된 또다른 형태의 미스트 발생 장치가 나타나 있다. 제5b도의 변형은, 초음파 변환기(56)가 용기의 바닥 벽에 밀착되어 있기 보다 오히려 안정화된 액체 소오스 상부의 발생기(46)에 달려있다는 점 외에는 제4도의 형태와 거의 유사하다.5b shows another type of mist generating device in which the mist generating device of FIG. 4 is modified. The modification of FIG. 5B is almost similar to that of FIG. 4 except that the ultrasonic transducer 56 rests on the generator 46 on top of the stabilized liquid source rather than on the bottom wall of the vessel.
제4도, 5a도 및 5b도에 나타난 소오스 발생기(46)(46')(46)가 본 발명에 따른 바람직한 형태이기는 하지만, 기타의 소오스 발생기도 본 발명에 따라 사용이 가능하다. 예를들면, 안정화된 액체 소오스는 밀폐 용기내에 공급이 가능하여 적절한 운반 기체가 안정화된 액체를 통해 기포를 발생한 후 혼합 챔버(42)로 흘러 들어갈 수 있다 ; 또는 밀폐 용기 내에서 안정학된 액체 소오스의 미스트를 발생시키는데 분무 노즐을 사용할 수 있고, 적절한 운반 기체가 제 4도에 나타난 유입구(50), 출구(52)와 유사한 유입구, 출구를 지닌 혼합 챔버(42) 내로 미스트를 통하여 흩러들어 갈 수 있다.Although the source generators 46, 46 ', 46 shown in FIGS. 4, 5a and 5b are preferred forms according to the present invention, other source generators may also be used in accordance with the present invention. For example, a stabilized liquid source may be supplied in a closed container such that an appropriate carrier gas may bubble through the stabilized liquid and flow into the mixing chamber 42; Or a spray nozzle may be used to generate a mist of stabilized liquid source in a closed vessel, and a suitable chamber containing a mixing chamber having an inlet 50, an inlet similar to outlet 52, and an outlet as shown in FIG. 42) I can scatter through the mist.
YMnO3의 졸-겔 합성예를 다음에 나타내었다. 1 그램의 이소프로폭시화 이트륨 Y[OCH(CH3)2]3를 8 ml 의 2-메톡시에탄올과 혼합하였다. 이소프로폭시화 이트륨은 용액 상태로 되지 않았으나 염산을 대략 25방울( 1㎖를 조금 초과한 양) 가하여 용액 상태로 만들 수 있었다. 0.25그램의 아세트산 망간 Mn(OOCCH3)2·H2O 를 5 ㎖ 2-메톡시에탄올과 혼합하였다. 아세트산 망간은 2-메톡시에탄올에 용해되지 않았으나 염산을 대략 10방울 가하여 용액 상태로 만들 수 있었다.A sol-gel synthesis example of YMnO 3 is shown next. 1 gram of isopropoxylated yttrium Y [OCH (CH 3 ) 2 ] 3 was mixed with 8 ml of 2-methoxyethanol. Yttrium isopropoxylate was not in solution but could be brought into solution by adding approximately 25 drops of hydrochloric acid (a little more than 1 ml). 0.25 grams of manganese acetate Mn (OOCCH 3 ) 2 .H 2 O was mixed with 5 mL 2-methoxyethanol. Manganese acetate was not dissolved in 2-methoxyethanol but could be brought into solution by adding approximately 10 drops of hydrochloric acid.
그 후 이트륨 및 망간 용액을 실온에서 함께 혼합하니 연황색의 용액이 얻어졌다. 결과로 얻어진 YMnO3용액은 실리콘 웨이펴 상에서 방사시킬 때 막을 형성하지 않았다. 가수 분해를 위해 H2O 를 가했으나 막-형성 특질을 개선시키지는 않았다. 그러나, 이소프로폭시화 티타늄(겔 형성제) 약 25방울을 이트륨/망간 용액에 가하니 용액이 얻어졌고(이 용액은 약 3시간 동안 맑은 상태를 유지하였다.) 실리콘 웨이퍼 상에서 방사시킬 때 우수한 막을 형성하였다.The yttrium and manganese solutions were then mixed together at room temperature to give a pale yellow solution. The resulting YMnO 3 solution did not form a film when spun on a silicon wafer. H 2 O was added for hydrolysis but did not improve the film-forming properties. However, about 25 drops of titanium isopropoxylated (gel former) was added to the yttrium / manganese solution to give a solution (which remained clear for about 3 hours) and produced a good film when spinning on a silicon wafer. Formed.
제6도는, 제 1-5도의 장치를 사용하여 증착시키기 위한 티탄산 납 지르코늄(이하 'PZT' 라 기술한다)의 안정화된 액체용액의 제법을 나타낸 전형적인 공정도를 보이고 있다. P1-P3단계에서, 통상적인 각 전구체의 용매로 2-메톡시에탄올을 사용하여 이소프로폭시화 티타늄, n-프로폭시화 지르코늄 및 아세트산 납의 안정화된 액체 전구체들을 각기 형성한다. P4단계에서는 이소프로폭시화 티타늄 및 n-프로폭시화 지르코늄의 안정화된 용액을 혼합하고, P5단계에서 이 혼합물을 아세트산 납 전구체의 안정화된 용액 및 증착시킬 박막에 바람직한 도펀트나 첨가제와 함께 혼합한다. P6단계에서 P5의 최종 혼합물을 여과시켜 P7에 나타낸 바와 같은 모액을 형성시킨다. 다음의 표 1 은 P1- P7단계를 더욱 상세히 분석한 것이다.FIG. 6 shows a typical process diagram showing the preparation of a stabilized liquid solution of lead zirconium titanate (hereinafter referred to as 'PZT') for deposition using the apparatus of FIGS. 1-5. In the P 1 -P 3 steps, stabilized liquid precursors of titanium isopropoxylated, zirconium zirconium and lead acetate are each formed using 2-methoxyethanol as the solvent of each conventional precursor. In the step P 4 iso propoxylated mixed with the titanium and zirconium n- propoxylated preferred dopant or additive to the mixture in mixing the stabilizing solution, and the step P 5 in a stabilized solution and to deposit thin films of a precursor of lead acetate do. In step P 6 the final mixture of P 5 is filtered to form a mother liquor as shown in P 7 . Table 1 below is a more detailed analysis of the P 1 -P 7 steps.
[표 1]TABLE 1
졸-겔 PZT 용액 공정도Sol-Gel PZT Solution Flowchart
100 화학양론100 stoichiometry
110 Pb : Pb(Ac)2·3H2O 94.7 그램 = Pb 0.25 몰110 Pb: Pb (Ac) 2 3 H 2 O 94.7 grams = Pb 0.25 mol
120 Zr : n-프로폭시화 Zr 46.8 그램 (30 중량% 프로판올) = Zr 0.10몰120 Zr: 46.8 grams (30 wt% propanol) of n-propoxylated Zr = 0.10 mol of Zr
130 Ti : 이소프로폭시화 Ti 42.6 그램 = Ti 0.15 몰130 Ti: 42.6 grams of isopropoxylated Ti = 0.15 mol of Ti
140 10 : 1 몰비 (2-메톡시에탄올 : 금속의 몰비)140 10: 1 molar ratio (2-methoxyethanol: molar ratio of metal)
200 납 전구체200 lead precursor
210 Pb(Ac)2ㆍ3H2O 94.73 그램을 2-메톡시에탄올 197 ml에 첨가한다.94.73 grams of 210 Pb (Ac) 2 .3H 2 O are added to 197 ml of 2-methoxyethanol.
220 이 용액을 114℃ 온도까지 증류시킨다.220 The solution is distilled to 114 ° C.
230 최종 증류액의 양 : 107 mlVolume of 230 final distillate: 107 ml
300 지르코늄 전구체300 zirconium precursor
310 프로판올 내의 n-프로폭시화 Zr 46.8 그램을 2-메톡시에탄올 79 ml 에 첨가한다.46.8 grams of n-propoxylated Zr in 310 propanol are added to 79 ml of 2-methoxyethanol.
320 이 용액을 113℃ 온도까지 증류시킨다.320 The solution is distilled to 113 ° C.
330 최종 증류액의 양 : 79 ml330 Amount of final distillate: 79 ml
400 티타늄 전구체400 titanium precursor
410 이소프로폭시화 Ti 42.62 그램을 2-메톡시에탄올 118 ml 에 첨가한다.42.62 grams of 410 isopropoxylated Ti are added to 118 ml of 2-methoxyethanol.
420 이 용액을 114℃ 온도까지 증류시킨다.420 The solution is distilled to 114 ° C.
430 최종 증류액의 양 : 76 mlAmount of 430 final distillate: 76 ml
500 전구체 혼합500 precursor mix
510 Ti 전구체를 Zr 전구체에 가한 후 교반한다.510 Ti precursor is added to the Zr precursor and then stirred.
520 TiZr 용액을 Pb 용액에 가한 후 1/2 시간 동안 교반한다.520 TiZr solution is added to the Pb solution and stirred for 1/2 hour.
530 PZT 모액의 양 : 250 mlVolume of 530 PZT Stock Solution: 250 ml
540 PZT 모액을 적당한 크기의 시린지(syringe) 여과기에서 여과시킨다.The 540 PZT mother liquor is filtered in a syringe filter of the appropriate size.
550 용액의 몰농도 = 1.0 M (PZT 몰수/용액 1)Molarity of solution 550 = 1.0 M (PZT moles / solution 1)
P8단계에서 P7의 모액을 아세트산 및 H2O 또는 기타 적절한 물질로 가수분해한다. 그러나, P7에서 P9로 연장된 점선에 나타난 바와 같이 이 가수분해 단계는 생략할 수도 있다. P1에서 P8까지의 단계는 통상적인 스핀-온 박막 형성 절차에 사용하는 졸-겔을 형성하는데 이용하는 통상의 단계들이다.In step P 8 the mother liquor of P 7 is hydrolyzed with acetic acid and H 2 O or other suitable substance. However, this hydrolysis step may be omitted, as indicated by the dashed line extending from P 7 to P 9 . The steps from P 1 to P 8 are the conventional steps used to form the sol-gel for use in conventional spin-on thin film formation procedures.
P9단계에서, P7의 모액 또는 P8의 가수분해 용액을 본 발명의 증착 공정에 사용하도록 변성시킨다.In step P 9 , the mother liquor of P 7 or the hydrolysis solution of P 8 is modified for use in the deposition process of the present invention.
이러한 P9단계는 기본적으로 졸-겔 내 바람직한 화학적 화합물, 또는 기타의 안정화된 소오스 농도를 조절하는 과정을 포함하므로 증착 챔버(2) 내로 흐르는 증기 소오스(미스트) 몇 방울이 기판(5)상에 증착되고 전개되어 기판(5)의 상부면 전체에서 졸-겔의 균일한 막을 형성할 것이다. 바꾸어 말하면, 증기 소오스의 상당한 양이 건조되어서 기판(5)상에 작은 크기의 입자들을 분리 생성하여, 결국 매우 다공성의/또는 미립자인 박막을 형성하는 바람직하지 않은 결과가 일어나기 전에, 졸-겔 막이 완전히 기판(5)상에 증착되도록 졸-겔 농도를 조절할 것이다. 졸-겔 또는 기타 안정화된 액체 소오스 내 화학적 화합물의 적절한 농도를 결정하는 과정에서는 증착 챔버(2)내에서 유지되는 진공 수준 뿐 아니라 특히 안정화된 액체 소오스에서 사용되는 화학적 화합물 및 용매를 고려하는 것이 필요하다. 예를들면, 앞서 논의된 PZT 졸-겔에서 사용하는 2-메톡시에탄올과 같이 비교적 끓는점이 높은 용매는, 메탄올과 같이 비교적 끓는점이 낮은 용매보다 건조가 느리다 ; 반면 높은 진공 수준은 다른 안정화된 액체 소오스보다 건조가 빠르다.This P 9 step basically involves adjusting the desired chemical compound, or other stabilized source concentration, in the sol-gel so that a few drops of vapor source (mist) flowing into the deposition chamber 2 are deposited on the substrate 5. And develop to form a uniform film of the sol-gel throughout the upper surface of the substrate 5. In other words, before a significant amount of vapor source is dried to separate and produce small sized particles on the substrate 5, which eventually results in the formation of a very porous and / or particulate thin film, the sol-gel membrane The sol-gel concentration will be adjusted to completely deposit on the substrate 5. Determining the appropriate concentration of chemical compounds in the sol-gel or other stabilized liquid source requires consideration of the chemical compounds and solvents used, particularly in the stabilized liquid source, as well as the vacuum level maintained in the deposition chamber 2. Do. For example, a relatively high boiling solvent, such as 2-methoxyethanol used in the PZT sol-gel discussed above, is slower to dry than a relatively low boiling solvent such as methanol; High vacuum levels, on the other hand, dry faster than other stabilized liquid sources.
앞서 논의된 바와 같은 방식으로 제조한 졸-겔로부터의 PZT 증착 및 570-575 Torr의 진공에서 작동하는 증착 챔버(2)의 경우, P7의 모액 또는 P8의 가수분해 용액은 P9단계에서 10-15펴센트(부피 펴센트)의 메탄올을 첨가함으로써 변성될 것이다. 바꾸어 말해서, 일반적인 졸-겔은 기판(5)상에 증착한 충분히 유동적인 증기 소오스 방울이 전개되어 앞서 논의한 바와같이 연속적이고 균일한 막을 형성하도록 충분히 희석된다.Previously prepared in a manner as discussed sol-case of the deposition chamber (2) operating in the PZT deposition and 570-575 Torr of vacuum from the gel, the hydrolysis solution in the mother liquor or P 7 P 8 P 9 a are in phase It will be denatured by adding 10-15 docent (volume docent) of methanol. In other words, a typical sol-gel is sufficiently diluted so that a sufficiently fluid vapor source droplet deposited on the substrate 5 develops to form a continuous and uniform film as discussed above.
메탄올은 본 발명에 따른 PZT 의 졸-겔에 대한 바람직한 희석제이나, 기타의 희석제 (2-메톡시에탄올을 포함하여)도 PZT의 졸-겔을 희석시키는데 사용할 수 있으며, 그 밖의 다양한 희석제도 본 발명에 따라 사용되는 안정학된 액체 소오스 및 졸-겔과 함께 사용할 수 있다.Methanol is the preferred diluent for the sol-gel of PZT according to the invention, but other diluents (including 2-methoxyethanol) can also be used to dilute the sol-gel of PZT. It can be used with the stabilized liquid source and sol-gel used according to the invention.
P10단계에서는 P9의 변성 용액을 제4도 또는 5도에 도시한 것과 같은 소오스 발생기(46)를 사용하여 증발시키고, 다기관 조립체(40)를 통하여 증착 장치(1)로 흐르게 한 후 기판(5) 상에 증착시켜서 졸-겔의 박막을 형성시킨다. 증착된 박막의 두께는 통상적인 수단(도시되지 않음)에 의해 연속적으로 모니터된다.In step P 10 , the denatured solution of P 9 is evaporated using a source generator 46 as shown in FIG. 4 or 5, flowed through the manifold assembly 40 to the deposition apparatus 1, and then the substrate ( 5) Deposit on to form a thin film of sol-gel. The thickness of the deposited thin film is continuously monitored by conventional means (not shown).
건조 단계 P11에서는, 졸-겔로부터 용매를 제거하기 위하여 졸-겔 또는 기타 안정학된 액체 소오스의 박막을 증착시킨 기판(5)을 진공 상에 놓게되고, 따라서 기판(5)상에는 바람직한 화학적 화합물의 박막이 남겨진다. 반면 P12단계에서는, 화합물의 박막이, 필요하다면, 어닐링 될 것이다. 건조단계 P11에서, 졸-겔 박막과 건조는 가열 수단을 사용하거나 증착 박막을 가열시킴으로써 수행된다. 더 나아가, 강유전체와 같은 다수의 복합 박합과 함께 건조시킨 박막을, 상기 박막이 바람직한 방식으로 작용하기 전에, 어닐링시켜 활성화 하는 것이 필요하다. 건조 및 어닐링 단계 P11ㆍP12는 적절한 가열 수단을 사용하는 증착 챔버(2)내에서 효과적일 것이며, 증착 챔버(2) 외부의 다른 장치에서도 수행될 수 있다.In drying step P 11 , a substrate 5 on which a thin film of sol-gel or other stabilized liquid source is deposited is placed in a vacuum to remove the solvent from the sol-gel, and thus on the substrate 5 a desired chemical compound. The thin film of is left. Whereas in the P 12 step, a thin film of the compound, if necessary, will be annealed. In drying step P 11 , the sol-gel thin film and the drying are performed by using a heating means or by heating the deposited thin film. Furthermore, it is necessary to anneal and activate the thin film dried together with a plurality of composite laminates, such as ferroelectrics, before the thin film can function in a preferred manner. The drying and annealing steps P 11 .P 12 will be effective in the deposition chamber 2 using suitable heating means, and may be performed in other apparatus outside the deposition chamber 2.
P13단계에서, 화학적 화합물의 박막층이 형성된 기판은 그 위에 상부 전극을 증착시키는 식으로 그 이상의 공정이 이루어진다. 앞에서 제 1-5도와 관련하여 논의되었던 본 발명의 제 1 실시 형태의 장치는, 조절된 환경에서 매우 복잡한 다원소 막을 쉽게 생산할 수 있는 최상의 진공, CVD 및 습식 화학 (졸-겔, MOD, 등) 기술들이 효과적으로 결합하였기에 잇점이 많다. 몇가지 잇점으로는 증착시킨 박막의 화학양론을 지속적으로 신중하게 조절할 수 있는 능력, 안정화된 액체 소오스의 생산 및 취급의 용이성, (증착 공정이 진공 하에서 진행되기 때문에) 증착시킨 막을 오염원으로부터 분리하여 유지시키는 능력, 기판의 표면을 완전히 피복할 만한 매우 얇고 균일한 막 형성 능력 등이 포함된다.In step P 13, the substrate is a thin film layer of a chemical compound formed is made of a further step in a way to deposit an upper electrode thereon. The apparatus of the first embodiment of the present invention, discussed above in connection with FIGS. 1-5, provides the best vacuum, CVD and wet chemistry (sol-gel, MOD, etc.) that can easily produce very complex multi-element films in a controlled environment. There are many benefits to the effective combination of technologies. Some advantages include the ability to continuously and carefully control the stoichiometry of the deposited thin film, ease of production and handling of stabilized liquid sources, and keeping the deposited film away from the source (since the deposition process is under vacuum). Ability, a very thin and uniform film-forming ability to completely cover the surface of the substrate, and the like.
제1도에 나타난 증착 장치(1)의 구조에는 가열 수단이 부족하기 매문에, 본 발명에 따른 증착 공정은 실온/분위기 온도에서 이루어지는 것이 바람직하다.Since the structure of the deposition apparatus 1 shown in FIG. 1 lacks a heating means, the deposition process according to the present invention is preferably carried out at room temperature / atmosphere temperature.
제4도 및 5도에 관련하여 앞서 논의한 대로, 본 발명의 양상은 안정화된 화합물 소오스가 증착 챔버내로 유입되기 전에 이 소오스를 원자화 되도록 초음파로 교란시키는 것이다. 특히 안정화된 소오스에 있어서는, 증기가 다기관 조립체 및/또는 증착 챔버내로 유입될 때 가열시키는 것이 바람직할 것이다.As discussed above in connection with FIGS. 4 and 5, an aspect of the present invention is to ultrasonically disturb the source to atomize before the stabilized compound source enters the deposition chamber. In particular stabilized sources, it will be desirable to heat the steam as it enters the manifold assembly and / or deposition chamber.
본 발명의 또다른 양상은 용매 교환 기술을 포함한다. 많은 경우에 화합물 X는 단지 하나의 특정한 용매에만 용해될 것이다. 유사하게, 화합물 Y는 X가 용해된 용매와는 양립할 수 없는 다른 용매에 용해될 것이다. 본 발명에 있어서, 용매 교환 기술은 졸-겔 또는 X 및 Y 화합물을 가지는 안정화된 액체를 생산하기 위하여 공통 용매에서 수행된다.Another aspect of the invention involves solvent exchange techniques. In many cases Compound X will only dissolve in one particular solvent. Similarly, compound Y will be dissolved in another solvent which is incompatible with the solvent in which X is dissolved. In the present invention, solvent exchange techniques are performed in a common solvent to produce sol-gels or stabilized liquids having X and Y compounds.
본 발명은 강유전체, 초-전도체, 높은 유전 상수를 가지는 물질, 보석 등과 같은 착화합물의 박막을 증착시키는데에 이롭다.The present invention is beneficial for depositing thin films of complexes such as ferroelectrics, super-conductors, materials with high dielectric constants, gemstones and the like.
이상으로 본 발명의 바람직한 실시 형태로 간주되는 것들이 서술되었지만, 본 발명의 기본적인 특성을 벗어나지 않는 기타의 특정한 형태로 실시될 수도 있다. 따라서, 본 실시형태는 모든 양상에 있어서 예시적으로 나타냈으며 제한적으로 나타내지 않았다. 본 발명의 범주는 다음에 첨부하는 특허 청구의 범위로 나타난다.Although what has been described as a preferred embodiment of the present invention has been described above, it may be embodied in other specific forms without departing from the basic features of the present invention. Accordingly, the present embodiment has been shown by way of example in all aspects and not by way of limitation. It is intended that the scope of the invention be defined by the claims appended hereto.
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US66042891A | 1991-02-25 | 1991-02-25 | |
US660,428 | 1991-02-25 | ||
PCT/US1992/001380 WO1992015112A1 (en) | 1991-02-25 | 1992-02-21 | Methods and apparatus for material deposition |
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US5456945A (en) * | 1988-12-27 | 1995-10-10 | Symetrix Corporation | Method and apparatus for material deposition |
FR2897281B1 (en) * | 2006-02-14 | 2009-01-23 | Saint Louis Inst | PROCESS FOR THE MANUFACTURE BY NANOCRYSTALLIZATION OF ENERGETIC OR INERT COMPOUNDS |
WO2011060444A2 (en) | 2009-11-16 | 2011-05-19 | Fei Company | Gas delivery for beam processing systems |
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US3473959A (en) * | 1964-08-10 | 1969-10-21 | Licentia Gmbh | Method for coating semiconductors and apparatus |
US3880112A (en) * | 1971-10-20 | 1975-04-29 | Commissariat Energie Atomique | Device for the preparation of thin films |
US4290384A (en) * | 1979-10-18 | 1981-09-22 | The Perkin-Elmer Corporation | Coating apparatus |
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US4689247A (en) * | 1986-05-15 | 1987-08-25 | Ametek, Inc. | Process and apparatus for forming thin films |
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US5041229A (en) * | 1988-12-21 | 1991-08-20 | Board Of Regents, The University Of Texas System | Aerosol jet etching |
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