EP3684485A1 - Appareil et procédé de génération de vapeur et de dépôt de film - Google Patents

Appareil et procédé de génération de vapeur et de dépôt de film

Info

Publication number
EP3684485A1
EP3684485A1 EP18869624.9A EP18869624A EP3684485A1 EP 3684485 A1 EP3684485 A1 EP 3684485A1 EP 18869624 A EP18869624 A EP 18869624A EP 3684485 A1 EP3684485 A1 EP 3684485A1
Authority
EP
European Patent Office
Prior art keywords
gas
flow
heat exchanger
housing
metal housing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP18869624.9A
Other languages
German (de)
English (en)
Other versions
EP3684485A4 (fr
Inventor
Thuc M. Dinh
Yamin Ma
Benjamin Y.H. Liu
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MSP Corp
Original Assignee
MSP Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US15/790,906 external-priority patent/US10287679B2/en
Application filed by MSP Corp filed Critical MSP Corp
Publication of EP3684485A1 publication Critical patent/EP3684485A1/fr
Publication of EP3684485A4 publication Critical patent/EP3684485A4/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0011—Heating features
    • B01D1/0017—Use of electrical or wave energy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01B—BOILING; BOILING APPARATUS ; EVAPORATION; EVAPORATION APPARATUS
    • B01B1/00—Boiling; Boiling apparatus for physical or chemical purposes ; Evaporation in general
    • B01B1/005—Evaporation for physical or chemical purposes; Evaporation apparatus therefor, e.g. evaporation of liquids for gas phase reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/06—Evaporators with vertical tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/14—Evaporating with heated gases or vapours or liquids in contact with the liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/26—Multiple-effect evaporating
    • 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
    • C23C16/448—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

Definitions

  • the process of creating a vapor from a liquid can be accomplished by heating the liquid to a sufficiently high temperature to cause the liquid to undergo a phase change and become a vapor.
  • To generate vapor at a sufficiently high rate it is necessary to supply an adequate amount of heating energy to the liquid in a relatively short time. This can be accomplished by increasing the operating temperature of the vapor generating apparatus or providing a larger heat transfer surface so that heat can be conducted more easily into the liquid.
  • precursor chemicals are available in liquid form for vapor generation and for subsequent thin film deposition on a substrate by a vapor phase process.
  • Processes such as chemical vapor deposition (CVD), plasma-enhanced chemical vapor deposition (PECVDP), metal-organic CVD (MOCVD), atmosphere pressure chemical vapor deposition (APCVD) and atomic layer deposition (ALD) are well known to those skilled in the art of semiconductor device fabrication.
  • Some precursor chemicals such as metal-organic compounds can decompose at high temperatures to form undesirable by-products to cause process or equipment contamination. For such applications, the heating temperature must be kept low to avoid thermal decomposition and by-product formation.
  • the present disclosure is directed to a method of vapor generation that allows for a more compact vaporizer design, while reducing the maximum temperature to which the liquid and vapor are exposed to.
  • the method includes flowing a mixture of gas and liquid droplets for vaporization through at least one heat exchanger having a plurality of surfaces for heat transfer to the gas, the increased surface area in the heat exchanger directing the gas and liquid mixture through a tortious flow path to further increase heat transfer and vaporization.
  • the method may further include directing the mixture to a second heat exchanger to further vaporize any remaining liquid droplets in the gas.
  • One or both heat exchangers may be configured with a tortious flow path comprising a plurality of tubular flow passageways.
  • the apparatus may be smaller and more compact in size, but able to maintain a high capacity for vaporization of liquid droplets in a gas.
  • An increased heat transfer surface area in the apparatus allows for increased vaporization at a lower maximum temperature of the apparatus.
  • the apparatus incorporates at least one heat exchanger having an increased surface area of heated flow paths for thermal transfer from a heating element to the gas comprising the liquid droplets.
  • the apparatus is configured to vaporize the liquid droplets to form a vapor and comprises at least a first and preferably a second heat exchanger, the first heat exchanger in fluid communication with the second heat exchanger.
  • the first heat exchanger is a primary heat exchanger comprising a housing having an inlet and an outlet allowing a gas carrying suspended liquid droplets to enter and flow through the first heat exchanger.
  • This gas and liquid droplet mixture is flown through the first heat exchanger and the liquid droplets may be vaporized by a tortious flow path, in that the flow direction of the gas alternates in flow direction at least once in the first heat exchanger.
  • the flow path may comprise a plurality of metal tubes within the first heat exchanger.
  • the primary heat exchanger may then be in fluid communication with a second heat exchanger, also referred to as a secondary heat exchanger.
  • the secondary heat exchanger may have a construction substantially similar to the construction of the first heat exchanger and is configured to receive the gas and liquid mixture having at least some liquid droplets that were not vaporized after the gas and liquid mixture flows through the primary heat exchanger, and to further vaporize the gas and liquid mixture.
  • One or both of the heat exchangers may comprise tubular flow passageways configured to provide a tortious flow path for vaporization.
  • FIG. 1A is a vertical sectional view of a vapor generating apparatus.
  • FIG. IB is a horizontal sectional view along the line B - B of the vapor generating apparatus of the embodiment illustrated in FIG. 1A.
  • FIG. 2 is an enlarged view of the structure according to the embodiment illustrated in FIG. 1A.
  • FIG. 3A is a sectional view of an embodiment of the vapor generation apparatus.
  • FIG. 3B is a sectional view of an embodiment of the vapor generation apparatus along the line C - C in FIG. 3A.
  • FIG. 3C is a sectional view of an embodiment of the vapor generation apparatus along the line D - D in FIG. 3A.
  • FIG. 4 is a cross-sectional view of an embodiment of a vapor generating apparatus.
  • FIG. 1A A vertical sectional view of the vapor generating apparatus is illustrated in FIG. 1A, and FIG. IB is a horizontal sectional view of the same apparatus along line B-B of FIG.IA.
  • FIG. 1A A vertical sectional view of the vapor generating apparatus is illustrated in FIG. 1A
  • FIG. IB is a horizontal sectional view of the same apparatus along line B-B of FIG.IA.
  • Like reference characters will be used for like elements throughout the figures.
  • the vapor generating apparatus is generally illustrated at 100.
  • the apparatus 100 includes a metal housing 110, and an electric heater 120 surrounding the metal housing 110 and in good thermal contact with the metal housing 110.
  • an atomizer 140 Located above the vapor generating apparatus is an atomizer 140. Liquid to be vaporized is introduced into the liquid inlet 120 of the atomizer 140 along with a carrier gas, which flows into a gas inlet 150 of the atomizer 140, to form a droplet aerosol comprised of small liquid droplets suspended in the carrier gas. The droplet aerosol then flows out of the atomizer 140 through an outlet 160 and into a space 170 in the vapor generating apparatus 100 for heating and vaporization.
  • the atomizer 140 Under normal operating conditions, the atomizer 140 is located in a cleanroom. Both the precursor liquid and the carrier gas flowing into the atomizer 140, as well as the droplet aerosol flowing out of the atomizer 140, are both held at substantially the same temperature as the ambient air temperature (generally "room temperature"). The droplet aerosol then flows down a multitude of tubular gas flow passageways. One of the gas flow passage ways is illustrated by circular hole 180 in FIG. IB. As the aerosol flows down the tubular gas flow passage ways, heat is transferred from heated metal surfaces by convection into the droplet aerosol, causing the suspended droplets in the aerosol to vaporize and form a vapor.
  • the resulting gas/vapor mixture then flows out of the vaporization apparatus through the downstream flow passageways for additional heating and vaporization.
  • the gas flow passageways shown as round holes 180 in FIG. IB are considered as the first, primary heating stage for droplet vaporization. Any un- vaporized droplets can then be vaporized in a second heating stage described further below.
  • droplet vaporization in gas flow passage ways 180 may be incomplete.
  • the droplet aerosol then enters into space 200 and into a metal structure 220 for further heating and vaporization.
  • the metal structure 220 thus becomes a second vaporization stage for the un-vaporized liquid droplets in this two stage heating and vaporization process.
  • FIG. 2 Illustrated at FIG. 2 is an enlarged vertical sectional view of the metal structure 220.
  • the metal structure may be generally cylindrical in shape.
  • a base flange 270 is in good thermal contact with a vertical cylindrical wall 230 which is attached to an inner vertical cylindrical wall 250 and in good thermal contact with the cylindrical wall 250.
  • a cup shaped cylinder wall 240 is also attached to the vertical cylindrical wall 230 by contact (not shown in this vertical sectional view). All elements of the metal structure 220, including the vertical walls 230, 240, and 250 are in good thermal contact with each other allowing heat to flow easily by conduction from the outer wall 230 into inner walls 240 and 250.
  • the walls 230, 240 and 250 may be cylindrical or tubular in nature and may be referred to as tubes or cylinders throughout this disclosure.
  • the gas would first flow in a generally downward direction through the tube 250 as indicated by arrow 225 then upwardly through the annular space between tubes 240 and 250 as indicated by arrow 235.
  • the gas then flows in a downward direction between tubes 230 and 240 as indicated by arrow 245 before exiting the metal structure 220 through outlet 250.
  • the gas flow between vertical cylinders 230, 240, and 250 creates a tortuous flow path which greatly increases the surface area of contact between the heated metal tubes and the gas flowing along the walls of the tubes.
  • the vaporization apparatus illustrated in FIG.1A and FIG. IB may be used in a semiconductor device lab for fabricating integrated circuit device chips.
  • a preferred material of construction is stainless steel.
  • Stainless steel is generally used because of its resistance to corrosion and ability to provide a contaminant free surface as preferred for the application.
  • Stainless steel is thermally conductive, however, compared to other metals, stainless steel is a relatively poor thermal conductor. Table 1 shows the thermal conductivity of stainless steel in comparison to other metals. The flow of heat from the electric heater 120 to the tortuous flow passage will be slower when less thermally conductive materials are used, resulting in an increased response time of the vaporization apparatus.
  • a second electric heater 232 is provided.
  • the second heater 232 may be located near the center of the vaporization apparatus 100. The flow of heat from the second electric heater 232 to all parts of the vaporization apparatus 100 located near the center of the vaporization apparatus 100 will be improved, thus reducing overall response time of the apparatus.
  • FIG. 3A Illustrated in FIG. 3A is a vertical sectional view of an additional embodiment
  • the heat exchanger is heated by an electric heater (not shown) similar to electric heater 120 illustrated in FIG. 1A.
  • the droplet aerosol enters the heat exchanger through inlet hole 310 into empty space 320 in the direction of downward arrow 315.
  • the droplet aerosol flow then undergoes a change in flow direction and flows upward as depicted by group of arrows 325.
  • This droplet aerosol then flows into tubular flow passageways, one of which is identified at 330 in FIG. 3B, along the direction of arrows 345.
  • the droplet aerosol then flows through the multitude of tubular flow passageways for heating the gas and vaporizing the droplets contained therein.
  • the primary heat exchanger may still contain un-vaporized droplets suspended in the gas.
  • This droplet aerosol then flows into space 340 and subsequently through secondary heat exchanger 350.
  • the aerosol then flows through gas flow passageways 360 in the secondary heat exchanger in order to vaporize the remaining un-vaporized droplets suspended in the gas.
  • the gas and vapor mixture then flows out of the secondary heat exchanger through exit 370.
  • FIG. 4 As illustrated in FIG. 4, the concepts of vapor generation described above with respect to FIGS. 1 and 3 have been combined.
  • the embodiment illustrated in FIG. 4 further increases the vaporization capacity of the apparatus.
  • an orifice 400 is provided at or near a center well 402.
  • the orifice 400 for example is provided at the bottom of the center well 402 and aids in balancing the load of two sections of the heat exchanger.
  • the orifice connects a heat exchanger to a multitude of tubular passageways for increasing the flow path and thus the vaporization capacity of the apparatus.
  • a vapor generating apparatus 460 is a housing comprising a vapor generation apparatus 420 (similarly described and illustrated in FIGS. 1A and IB) that is fluidly connected at the orifice 400 to heat exchanger 410, such as a metal heat exchanger, for heating and vaporizing the droplet aerosol (similarly described and illustrated in FIGS. 3A, 3B, and 3C).
  • heat exchanger 410 such as a metal heat exchanger
  • the droplet aerosol enters the heat exchanger 410 through an opening and into an empty space in the direction of downward arrow 430.
  • the droplet aerosol flow then undergoes a change in flow direction and flows upward as depicted by arrows 432.
  • This droplet aerosol then flows into tubular flow passageways, along the direction of arrows 434.
  • the droplet aerosol then flows through orifice 400 in the direction of downward arrow 440 and into the vapor generation apparatus including a multitude of tubular flow passageways for heating the gas and vaporizing the droplets contained therein.
  • the droplet aerosol flow then undergoes a change in flow direction and flows upward as depicted by arrows 442.
  • This droplet aerosol then flows into tubular flow passageways, along the direction of arrows 444 and into the multitude of tubular flow passageways before exiting in the direction of arrow 450 via outlet 452.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)

Abstract

L'invention concerne un appareil et un procédé pour générer une vapeur avec une conception de vaporisateur compacte et exposer le mélange de gaz et de liquide pour une vaporisation à une température maximale réduite. Un écoulement de gouttelettes de gaz et de liquide à travers un boîtier métallique (110) configuré pour chauffer l'écoulement de mélange de gouttelettes de gaz et de liquide pour la vaporisation consiste à diriger le mélange de gouttelettes de gaz et de liquide à travers une entrée (120) du boîtier métallique et l'écoulement du gaz à travers un chemin d'écoulement laminaire défini par une pluralité de passages d'écoulement tubulaires (180) disposés autour d'un axe central pour une vaporisation. Le chemin d'écoulement est dirigé à travers un échangeur de chaleur (410) comprenant un ou plusieurs changements dans la direction du chemin d'écoulement avant de s'écouler dans le chemin d'écoulement supplémentaire décrit ci-dessus. Des gouttelettes de liquide résiduel peuvent être encore vaporisées en s'écoulant à travers un second boîtier métallique configuré pour chauffer le mélange de gouttelettes de gaz et de liquide pour une vaporisation et ayant une construction similaire au premier boîtier métallique et fournir un second chemin d'écoulement forcé.
EP18869624.9A 2017-10-23 2018-10-23 Appareil et procédé de génération de vapeur et de dépôt de film Withdrawn EP3684485A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US15/790,906 US10287679B2 (en) 2015-05-11 2017-10-23 Apparatus and method for vapor generation and film deposition
PCT/US2018/057083 WO2019083987A1 (fr) 2017-10-23 2018-10-23 Appareil et procédé de génération de vapeur et de dépôt de film

Publications (2)

Publication Number Publication Date
EP3684485A1 true EP3684485A1 (fr) 2020-07-29
EP3684485A4 EP3684485A4 (fr) 2020-11-04

Family

ID=66246659

Family Applications (1)

Application Number Title Priority Date Filing Date
EP18869624.9A Withdrawn EP3684485A4 (fr) 2017-10-23 2018-10-23 Appareil et procédé de génération de vapeur et de dépôt de film

Country Status (4)

Country Link
EP (1) EP3684485A4 (fr)
KR (1) KR102610173B1 (fr)
CN (1) CN111447982B (fr)
WO (1) WO2019083987A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114743900A (zh) * 2022-04-25 2022-07-12 北京北方华创微电子装备有限公司 汽化系统以及半导体工艺设备
WO2025251252A1 (fr) * 2024-06-06 2025-12-11 阿尔法原子有限公司 Vaporisateur pour dépôt chimique en phase vapeur

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CH238036A (de) * 1942-03-09 1945-06-15 Sulzer Ag Röhrenkühler.
CH240037A (de) * 1943-10-16 1945-11-30 Sulzer Ag Verfahren zur Regelung von Gaserhitzern und Einrichtung zur Ausführung des Verfahrens.
US5955037A (en) * 1996-12-31 1999-09-21 Atmi Ecosys Corporation Effluent gas stream treatment system having utility for oxidation treatment of semiconductor manufacturing effluent gases
JP3470055B2 (ja) * 1999-01-22 2003-11-25 株式会社渡邊商行 Ｍｏｃｖｄ用気化器及び原料溶液の気化方法
US6776809B2 (en) * 2000-06-08 2004-08-17 Toyota Jidosha Kabushiki Kaisha Fuel reforming apparatus
KR20050014796A (ko) * 2002-03-20 2005-02-07 알베르트 파리토비치 사이푸트디노프 혼합 유체의 분리를 위한 콤팩트한 정류 장치 및 이러한혼합 유체의 분리를 위한 정류 방법
US20050147749A1 (en) * 2004-01-05 2005-07-07 Msp Corporation High-performance vaporizer for liquid-precursor and multi-liquid-precursor vaporization in semiconductor thin film deposition
AU2009225950B2 (en) * 2008-03-20 2013-01-24 Creative Water Technology Ltd Fluid fractionation process and apparatus
KR101639577B1 (ko) * 2008-04-14 2016-07-14 헴로크세미컨덕터코포레이션 재료를 증착하기 위한 제조 장치와 이에 사용하기 위한 전극
KR101502415B1 (ko) * 2008-09-12 2015-03-13 엠 에스피 코포레이션 액체 전구물질 분무 방법 및 장치
KR101879805B1 (ko) * 2012-01-20 2018-08-17 삼성디스플레이 주식회사 박막 증착 장치 및 방법
JP5885564B2 (ja) * 2012-03-30 2016-03-15 株式会社ブイテックス 気化装置
CN104492103B (zh) * 2014-11-28 2016-05-25 武汉钧安制药有限公司 制备浓缩液用的蓄流单元
US9797593B2 (en) * 2015-05-11 2017-10-24 Msp Corporation Apparatus and method for vapor generation and film deposition
CN206167953U (zh) * 2016-10-28 2017-05-17 武汉友谊食品工程有限公司 一种用于油脂混合油溶剂蒸发的蒸发冷凝器

Also Published As

Publication number Publication date
EP3684485A4 (fr) 2020-11-04
WO2019083987A1 (fr) 2019-05-02
KR20200070363A (ko) 2020-06-17
CN111447982B (zh) 2022-09-13
CN111447982A (zh) 2020-07-24
KR102610173B1 (ko) 2023-12-04

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