WO2012132878A1 - Vaporiseur, dispositif d'alimentation en gaz et appareil de formation de film - Google Patents

Vaporiseur, dispositif d'alimentation en gaz et appareil de formation de film Download PDF

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Publication number
WO2012132878A1
WO2012132878A1 PCT/JP2012/056416 JP2012056416W WO2012132878A1 WO 2012132878 A1 WO2012132878 A1 WO 2012132878A1 JP 2012056416 W JP2012056416 W JP 2012056416W WO 2012132878 A1 WO2012132878 A1 WO 2012132878A1
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WIPO (PCT)
Prior art keywords
gas
raw material
vaporization
nozzle
vaporizer
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PCT/JP2012/056416
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English (en)
Japanese (ja)
Inventor
成幸 大倉
純一 武井
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東京エレクトロン株式会社
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Publication of WO2012132878A1 publication Critical patent/WO2012132878A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/06—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane
    • B05B7/062—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet
    • B05B7/066—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet with an inner liquid outlet surrounded by at least one annular gas outlet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/08—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point
    • B05B7/0869—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point the liquid or other fluent material being sucked or aspirated from an outlet orifice by another fluid, e.g. a gas, coming from another outlet orifice
    • 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
    • C23C16/4481—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 evaporation using carrier gas in contact with the source material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B15/00—Details of spraying plant or spraying apparatus not otherwise provided for; Accessories
    • B05B15/50—Arrangements for cleaning; Arrangements for preventing deposits, drying-out or blockage; Arrangements for detecting improper discharge caused by the presence of foreign matter
    • B05B15/55—Arrangements for cleaning; Arrangements for preventing deposits, drying-out or blockage; Arrangements for detecting improper discharge caused by the presence of foreign matter using cleaning fluids

Definitions

  • the present invention relates to a liquid source vaporizer used when a thin film is formed on an object to be processed such as a semiconductor wafer, a gas supply apparatus using the vaporizer, and a film forming apparatus using the gas supply apparatus.
  • various processes such as a film forming process, an etching process, and an oxidation diffusion process are repeatedly performed on an object to be processed such as a semiconductor wafer.
  • film formation processing taking film formation processing as an example, with regard to film quality characteristics of thin films such as insulating films, barrier films, and wiring films used in semiconductor integrated circuits, higher integration, higher miniaturization, and higher operation speed of semiconductor integrated circuits.
  • rare metals such as hafnium (Hf) and zirconium (Zr) may be used as the material for the thin film.
  • the raw material containing such a metal is generally solid or liquid at room temperature, for example, at the time of film formation, the solid is dissolved in an organic solvent to form a liquid raw material.
  • a liquid material at room temperature is mixed with an organic solvent to adjust the concentration, etc. to form a liquid raw material, and this liquid raw material is vaporized with a carrier gas in a vaporizer to form a raw material gas. To supply.
  • the carrier gas is used as described above is that the liquid raw material as described above generally has a low vapor pressure. Therefore, the carrier gas promotes vaporization of the liquid raw material and lowers the partial pressure of the raw material in the gas. Because.
  • the types of the vaporizer include a post-mix type that sprays and mixes liquid raw material and carrier gas in the vaporization chamber, and mixes the liquid raw material and carrier gas before vaporization to mix the liquid mixture in the vaporization chamber.
  • the premix type sprayed with is mainly known.
  • the liquid raw material described above generally reacts with moisture in the carrier gas and is easily hydrolyzed and easily oxidized. Therefore, a postmix type vaporizer is mainly used to prevent the injection nozzle from being blocked. ing.
  • this post-mix type vaporizer for example, disclosed in Patent Documents 1, 2, and 3 and the like, the liquid raw material and the carrier gas are simultaneously injected from the injection nozzle portion toward the vaporization chamber in a reduced pressure state. As a result, the liquid raw material is vaporized to form the raw material gas.
  • FIG. 1 is a schematic view showing an injection nozzle portion of a conventional vaporizer.
  • an injection nozzle portion 4 having a double-pipe structure is provided at one end of the vaporization chamber 2, and a liquid raw material and a carrier gas made of Ar or the like are separately provided in the vaporization chamber 2 from the injection nozzle portion 4.
  • the raw material gas is formed by injecting the liquid raw material to vaporize the liquid raw material.
  • the inside of the vaporizing chamber 2 is in a reduced pressure atmosphere as in the film forming apparatus, and is heated as necessary.
  • the outlet side 6 of the above-mentioned injection nozzle part 4 is in a state of opening at a large obtuse angle toward the inside of the vaporizing chamber 2, and the liquid raw material and carrier gas injected from the injection nozzle part 4 immediately go outside. It can diffuse.
  • the injected carrier gas flow is entrained in the outer peripheral portion, and the material gas retention 8 as indicated by the arrow occurs in the side portion on the outlet side 6 of the injection nozzle portion 4.
  • the staying source gas hits the partition wall of the vaporizing chamber 2 and deposits adhere to the partition wall.
  • the carrier gas outlet at the tip of the injection nozzle portion 4 is blocked to deteriorate the vaporization performance. There was a problem.
  • the present invention has been devised to pay attention to the above problems and to effectively solve them.
  • the embodiment of the present invention uses a vaporizer capable of suppressing clogging of a carrier gas outlet at the tip of an injection nozzle for vaporizing a liquid raw material, a gas supply device using such a vaporizer, and such a gas supply device.
  • a film forming apparatus uses a vaporizer capable of suppressing clogging of a carrier gas outlet at the tip of an injection nozzle for vaporizing a liquid raw material, a gas supply device using such a vaporizer, and such a gas supply device.
  • a vaporizer includes a vaporization container having a vaporization chamber formed therein, and a first nozzle that is provided in the vaporization container and injects a liquid raw material in the center.
  • An injection nozzle unit that has a second nozzle that is concentrically arranged on the outer periphery of one nozzle and injects a carrier gas, and vaporizes the liquid source by the carrier gas to form a source gas; and the injection nozzle unit
  • a gas diffusion suppression block that forms a gas diffusion suppression region that opens toward the vaporization chamber with an opening angle extending from the tip of the liquid material toward the injection direction of the liquid raw material at an acute angle, and the vaporization of the raw material gas A raw material gas outlet for flowing out of the container.
  • the carrier gas injected from the injection nozzle section passes through the gas diffusion suppression region where the opening angle spreads at an acute angle, so that the flow velocity is maintained high without decreasing the flow velocity of the carrier gas. Is suppressed, and as a result, it is possible to prevent the outlet of the carrier gas from being blocked by the deposit.
  • a gas supply device includes a vaporization container having a vaporization chamber formed therein, and a first nozzle that is provided in the vaporization container and injects a liquid raw material in the center.
  • An injection nozzle unit that has a second nozzle that is concentrically arranged on the outer periphery of the first nozzle and injects a carrier gas, vaporizes the liquid source with the carrier gas, and forms a source gas, and the injection nozzle
  • a gas diffusion suppression block that forms a gas diffusion suppression region that opens at an acute angle toward the liquid material injection direction from the tip of the portion and opens toward the vaporization chamber; and
  • a vaporizer provided with a raw material gas outlet that flows out of the vaporization container; a liquid raw material passage connected to the injection nozzle portion of the vaporizer and having a liquid flow controller in the middle; and the injection nozzle portion Contact Comprising a carrier gas passage, and a source gas passage flush out the feed gas wherein connected to the raw material gas outlet of the vaporizing
  • a vaporization container formed, and a first nozzle that is provided in the vaporization container and injects a liquid raw material at the center, is arranged concentrically on the outer periphery of the first nozzle, and injects a carrier gas.
  • An injection nozzle portion that forms a raw material gas by vaporizing the liquid raw material with the carrier gas, and an opening angle thereof is acute from the tip of the injection nozzle portion toward the liquid raw material injection direction.
  • a gas diffusion suppression block that forms an open gas diffusion suppression region, a raw material gas outlet that allows the raw material gas to flow out of the vaporization vessel, and a vaporizer that is connected to the injection nozzle portion of the vaporizer
  • a liquid source passage having a flow controller for liquid in the middle, a carrier gas passage having a flow controller for gas being connected to the injection nozzle part, and the source gas outlet of the vaporization container of the vaporizer And a raw material gas passage through which the raw material gas flows out.
  • the following excellent operational effects can be exhibited.
  • the carrier gas injected from the injection nozzle of the vaporizer passes through the gas diffusion suppression region where the opening angle spreads sharply, the flow rate of the carrier gas is maintained high without lowering the carrier gas flow rate, and the carrier gas is retained. As a result, it is possible to prevent the carrier gas outlet from being blocked by the deposit. Therefore, deterioration of the vaporization performance of the liquid raw material can be prevented and maintained at a high level.
  • FIG. 2 is a schematic configuration diagram showing the entire film forming apparatus having the vaporizer according to the present embodiment
  • FIGS. 3A and 3B are enlarged partial cross-sections showing the nozzle unit having the spray nozzle portion of the vaporizer according to the present embodiment and the vicinity thereof.
  • 4A and 4B are views showing the state of the tip of the injection nozzle portion
  • FIG. 4A is an enlarged sectional view
  • FIG. 4B is a plan view.
  • the film forming apparatus 10 includes a gas supply apparatus 14 for supplying a raw material gas and the like formed by the vaporizer 12 according to the present embodiment, and a film forming apparatus that actually forms a thin film using the raw material gas.
  • the main body 16 is mainly provided.
  • the said film-forming apparatus main body 16 has the processing container 18 formed, for example with the aluminum alloy etc.
  • a holding unit 20 that holds, for example, a semiconductor wafer W as an object to be processed is provided.
  • the holding means 20 is formed of a mounting table 22 made of, for example, a ceramic material or an aluminum alloy.
  • the mounting table 22 is provided with an object heating means 24 for heating the wafer W.
  • the object heating means 24 is formed by a resistance heater made of, for example, carbon wire.
  • the heating means 24 other means such as a heating lamp may be used.
  • a gate valve 26 that is opened and closed when the wafer W is loaded and unloaded and hermetically seals the processing container 18 is provided.
  • An exhaust port 28 is provided at the bottom of the processing vessel 18. The exhaust port 28 is connected to an evacuation system 34 having a pressure adjusting valve 30 and a vacuum pump 32 interposed in the middle of the exhaust passage 29 to adjust the atmosphere in the processing vessel 18 to a pressure. However, it can be vacuumed.
  • the processing vessel 18 is provided with a gas introduction means 36 for introducing a gas therein.
  • the gas introducing means 36 is composed of a shower head portion 38 provided on the ceiling portion of the processing container 18, and gas is injected into the processing container 18 from a number of gas injection holes 40 provided on the lower surface thereof. Yes.
  • a gas introduction port 42 for introducing a gas to be used is provided on the upper portion of the shower head portion 38.
  • the space inside the shower head section 38 is formed in one diffusion chamber or divided into a plurality of diffusion chambers according to the gas type used for film formation and the mixed type of the gas types, and so-called gas is premixed or post-mixed. It comes to mix.
  • gas inlets 42 as the number of the diffusion chambers are provided. In the illustrated example, only one diffusion chamber is shown for convenience.
  • the said shower head part 38 was used as the said gas introduction means 36, it is not limited to this, For example, you may make it use a simple nozzle-shaped thing.
  • a plasma generation mechanism using high-frequency power, microwave power, or the like may be provided in the processing container 18 to perform film formation using plasma.
  • the gas supply device 14 for supplying gas to the shower head unit 38 has a source gas supply system 44 and a necessary gas supply system 46 for supplying other necessary gases.
  • the necessary gas supply system 46 has a necessary gas passage 52 in which an on-off valve 48 and a gas flow rate controller 50 are interposed, and the necessary gas passage 52 is connected to the gas inlet 42 to connect to the necessary gas. Can be supplied while controlling the flow rate.
  • the required gas includes a purge gas that discharges the atmosphere in the processing vessel 18 and a reactive gas that reacts with the raw material gas, such as an oxidizing gas or a reducing gas.
  • FIG. 2 shows only one necessary gas supply system 46, but when a plurality of gas types that cannot be mixed at the time of supply is used as the necessary gas, a plurality of necessary gas supply systems 46 corresponding to the number are provided. It ’s good.
  • the purge gas N 2 soot gas is generally used, but other rare gases such as Ar and He can also be used.
  • the source gas supply system 44 includes the vaporizer 12, the liquid source passage 54 for supplying the liquid source 60 to the vaporizer 12, the carrier gas passage 56 for supplying the carrier gas to the vaporizer 12, and the vaporization. And a raw material gas passage 58 through which the raw material gas generated in the apparatus 12 flows toward the processing vessel 18.
  • the upstream end of the liquid source passage 54 is immersed in the liquid source 60 in the source storage tank 62 that stores the liquid source 60 therein, and the downstream end is the vaporizer 12.
  • the downstream end is the vaporizer 12.
  • a liquid flow controller 66 such as a liquid mass flow controller and two on-off valves 68 located on both sides of the liquid material supply direction are provided.
  • the liquid material 60 to be pumped is allowed to flow while controlling the flow rate.
  • a heater 70 for preventing the flowing liquid material 60 from solidifying is provided in the liquid material passage 54 including the liquid flow rate controller 66 and the on-off valve 68 as necessary. The raw material 60 is heated.
  • the raw material storage tank 62 is provided with a raw material heater 72 as necessary, and the liquid raw material 60 in the raw material storage tank 62 is heated to maintain a liquid state.
  • the upper space 74 in the raw material storage tank 62 is provided with a gas outlet 76A of a pressurized gas passage 76 through which an on-off valve 78 is interposed to flow pressurized gas.
  • the liquid raw material 60 in the raw material storage tank 62 is pumped into the liquid raw material passage 54 by this pressure.
  • an inert N 2 soot gas can be used in addition to a rare gas such as Ar or He.
  • the liquid raw material 60 is formed by dissolving a solid or liquid raw material containing a metal in an organic solvent.
  • the organic material may or may not be added to the liquid raw material at a temperature of about room temperature in order to adjust the concentration and viscosity.
  • an organometallic complex containing a metal such as La (lanthanum) may be used as the raw material.
  • the carrier gas passage 56 is connected to the injection nozzle portion 64.
  • a gas flow controller 80 such as a gas mass flow controller and two on-off valves 82 located on both sides of the carrier gas supply direction are provided.
  • the pressurized carrier gas is allowed to flow while controlling the flow rate.
  • the pressure of the carrier gas is set to about 100 to 400 kPa, for example.
  • Ar gas is used, for example, but it is not limited to this, Other rare gas, such as He, and N2 soot gas can also be used.
  • the raw material gas passage 58 is provided with an on-off valve 86 in the middle thereof, the upstream side thereof is connected to the raw material gas outlet 84 of the vaporizer 12, and the downstream side thereof is connected to the gas inlet 42 of the shower head unit 38.
  • the material gas is made to flow.
  • a heater 88 for preventing the flowing raw material gas from being reliquefied is provided in the entire raw material gas passage 58 including the on-off valve 86 as necessary. Heating is performed at the following temperature.
  • a bypass passage 90 is provided by connecting the upstream side of the on-off valve 86 of the raw material gas passage 58 and the exhaust passage 29 between the pressure adjusting valve 30 and the vacuum pump 32 of the vacuum exhaust system 34.
  • the bypass passage 90 is provided with an on-off valve 92, which stabilizes the flow rate of the raw material gas or supplies the raw material gas to the processing vessel 18 when the unnecessary raw material gas is discarded.
  • the raw material gas can be discharged by flowing into the bypass passage 90.
  • the vaporizer 12 is provided with a vaporization vessel 96 having a vaporization chamber 94 formed therein, and a liquid raw material 60 and a carrier gas into the vaporization chamber 94. It has the said injection
  • FIG. 3A shows a state in which the injection nozzle portion is attached to the vaporization container 96
  • FIG. 3B shows a state in the middle of attachment to the vaporization vessel 96 of the injection nozzle portion.
  • the vaporization container 96 is formed in a substantially cylindrical shape with both ends closed, and the sealed vaporization chamber 94 is formed in the inside thereof.
  • the vaporization container 96 is provided upright in the illustrated example, and a nozzle mounting hole 102 is formed on the upstream side, that is, the ceiling portion 96a which is the upper end portion (see FIG. 3B).
  • the injection nozzle portion 64 and the gas diffusion control block 100 are integrated to form a nozzle unit 104.
  • the nozzle unit 104 is inserted into the nozzle mounting hole 102.
  • a flange portion 106 is formed at the upper end portion of the nozzle unit 104, and the nozzle unit 104 is vaporized by fixing the flange portion 106 to the upper surface of the ceiling portion 96 a of the vaporization vessel 96 with a fixing screw 108.
  • the container 96 is detachably fixed.
  • a seal member 110 made of, for example, an O-ring is interposed between the flange portion 106 and the upper surface of the ceiling portion 96a of the vaporization container 96, and the airtightness of this portion is maintained.
  • the injection nozzle section 64 has a liquid source nozzle 122 (first nozzle) for injecting the liquid source 60 at the center thereof, and is arranged concentrically on the outer peripheral side to provide a carrier gas nozzle 124 ( A second nozzle) is provided, and the carrier gas is ejected from the carrier gas nozzle 124.
  • the liquid source nozzle 122 and the carrier gas nozzle 124 are both formed into a thin tubular shape and have a double tube structure. As a result, the carrier gas flow path in the carrier gas nozzle 124 has a ring shape.
  • the liquid raw material passage 54 is connected to the upper end of the liquid raw material nozzle 122 to supply the liquid raw material 60, and the liquid raw material is discharged from the raw material discharge port 126 at the lower end. It has become.
  • the carrier gas passage 56 is connected to the upper end of the carrier gas nozzle 124 so as to supply the carrier gas, and the carrier gas is discharged from the carrier gas discharge port 128 at the lower end thereof. ing.
  • the tip (lower end) of the liquid source nozzle 122 protrudes downward within a range of a length L1 (see FIG. 4A) slightly smaller than the tip (lower end) of the carrier gas nozzle.
  • the gas diffusion suppression block 100 has an opening angle ⁇ (see FIGS. 3A and 4A) that spreads from the tip of the injection nozzle portion 64 toward the injection direction of the liquid raw material 60 at an acute angle, and the vaporization is performed.
  • a gas diffusion suppression region 130 opened toward the chamber 94 is formed inside thereof.
  • the inner peripheral surface (inner wall surface) 132 of the gas diffusion suppression block 100 that defines the gas diffusion suppression region 130 is directed from the outer periphery of the lower end of the carrier gas nozzle 124 toward the gas injection direction (downward). For example, it is formed in a divergent shape so as to spread gradually. That is, the inner peripheral surface 132 is formed in the same shape as the conical side surface, and the gas diffusion suppression region 130 is formed in the inner space.
  • the spread (opening) angle ⁇ of the gas diffusion suppression region 130 is an acute angle smaller than 90 degrees as described above, and the liquid raw material 60 and the carrier gas injected from the injection nozzle part 64 are constant. Only the distance is prevented from diffusing immediately, and during that time, a high injection speed is maintained to promote vaporization of the liquid raw material 60.
  • the front end side (lower end side) of the inner peripheral surface 132 is a curved surface 132A that is shaped into a curved surface so as to gradually spread outward with a predetermined curvature, and continues to the inner peripheral surface of the vaporization vessel 96 as it is. It has become.
  • the inner peripheral surface of the upper end portion (ceiling portion 96a) of the vaporization container 96 is a curved surface 96A that is formed in a curved shape so as to go downward.
  • the opening angle ⁇ is preferably set within a range of 5 to 60 degrees.
  • the opening angle ⁇ is preferably set to 60 degrees or less as described above. If the opening angle ⁇ is smaller than 5 degrees, the carrier gas injection resistance becomes too large, and conversely, vaporization of the liquid raw material 60 is suppressed, so that the opening angle ⁇ is as described above. It is preferable to set it to 5 degrees or more. In the illustrated example, the opening angle ⁇ is set to 40 degrees, for example.
  • the length L2 of the gas diffusion suppression region 130 (see FIG. 3A), that is, the length in the gas injection direction is set within a range of 2 to 15 mm. If the length L2 is shorter than 2 mm, the gas diffusion suppression region 130 does not work and the vaporization performance cannot be improved. In addition, if the length L2 is longer than 15 mm, in this case, as a result of excessively suppressing the diffusion of the carrier gas, vaporization of the liquid source 60 is suppressed, and droplets of the liquid source 60 adhere to the inner peripheral surface 132. This is not preferable.
  • a plurality of, for example, three spacer protrusions 134 are provided between the inner peripheral edge of the tip of the carrier gas nozzle 124 and the outer periphery of the liquid source nozzle 122 as shown in FIG.
  • the ring-shaped flow passage cross-sectional area of the carrier gas nozzle 124 is set to be uniform with no deviation along the circumferential direction.
  • the inner diameter D1 (see FIG. 4A) of the liquid material nozzle 122 is in the range of about 100 to 1000 ⁇ m, for example, and is set to 250 ⁇ m in the illustrated example.
  • the width W1 (see FIG. 4A) of the ring-shaped flow path of the carrier gas nozzle 124 is, for example, in the range of 20 to 200 ⁇ m, and is set to 60 ⁇ m, for example, in the illustrated example.
  • the diameter of the vaporizing chamber 94 is set within a range of 20 to 80 mm, for example, and the capacity thereof is set within a range of about 300 to 1000 cc, for example.
  • a metal such as an aluminum alloy or stainless steel, or a heat resistant resin can be used as the constituent materials of the vaporization vessel 96, the gas diffusion suppression block 100, and the injection nozzle portion 64.
  • the source gas outlet 84 (see FIG. 2) for discharging the source gas formed in the vaporization chamber 94 to the downstream side is provided on the side wall slightly above the bottom of the vaporization chamber 94 in the vaporization vessel 96.
  • a raw material gas passage 58 of the raw material gas supply system 44 is connected to the raw material gas outlet 84.
  • a heating means 136 (see FIGS. 2 and 3A) is provided on the outer peripheral side of the vaporization vessel 96, and the vaporization vessel 96 is heated to promote vaporization of the liquid raw material 60. .
  • the heating temperature of the vaporization vessel 96 is, for example, in the range of about 150 to 300 ° C., although it depends on the type of liquid raw material used.
  • the overall operation control of the film forming apparatus 10 configured as described above is controlled by an apparatus control unit 140 (see FIG. 2) made of, for example, a computer, and the computer program for performing this operation is Are stored in the storage medium 142 (see FIG. 2).
  • the storage medium 142 includes, for example, a flexible disk, a CD (Compact Disk), a hard disk, a flash memory, a DVD (Digital Versatile Disk), or the like.
  • supply of each gas is started, stopped, flow rate is controlled, process temperature and process pressure are controlled, and the like.
  • the operation of the film forming apparatus 10 formed as described above will be described.
  • the raw material gas supply system 44 of the gas supply device 14 the liquid raw material 60 stored in the raw material storage tank 62 is pumped by the pressurized gas toward the liquid raw material passage 54, and the flow rate is controlled by the liquid flow rate controller 66. While being supplied, the gas is supplied to the spray nozzle portion 64 of the vaporizer 12. On the other hand, the pressurized carrier gas is supplied to the injection nozzle unit 64 while the flow rate is controlled by the gas flow rate controller 80.
  • the liquid raw material 60 supplied to the injection nozzle section 64 is injected from the raw material discharge port 126 at the tip of the liquid raw material nozzle 122 and passes through the gas diffusion suppression region 130 formed at the center of the gas diffusion suppression block 100. Through the vaporizing chamber 94. At the same time, the carrier gas supplied to the injection nozzle section 64 is injected from the carrier gas discharge port 128 at the tip of the carrier gas nozzle 124, and the gas diffusion suppression region 130 formed at the center of the gas diffusion suppression block 100. Is introduced into the vaporizing chamber 94.
  • the jetted liquid raw material 60 is vaporized in the vaporization chamber 94 by the carrier gas to form the raw material gas.
  • this raw material gas is discarded to the evacuation system 34 through a bypass passage 90 that is branched from the middle of the raw material gas passage 58.
  • the raw material gas is opened and closed.
  • the open / close state of the valves 86 and 92 is switched to flow into the source gas passage 58 and supplied to the shower head unit 38 provided in the film forming apparatus main body 16.
  • the shower head unit 38 is also supplied with necessary gas from another necessary gas supply system 46.
  • the raw material gas and the necessary gas are introduced from the shower head portion 38 into the processing vessel 18 that has been previously in a reduced-pressure atmosphere, and the raw material gas reacts with the necessary gas or is thermally decomposed on the mounting table 22.
  • a thin film is deposited on the surface of the semiconductor wafer W held on the substrate.
  • the wafer W is maintained at a predetermined process temperature by the workpiece heating means 24.
  • the atmosphere in the processing vessel 18 is evacuated by the evacuation system 34 and maintained at a predetermined process pressure. In this way, the film forming process is continuously performed.
  • the flow rate of the liquid material 60 is, for example, in the range of about 0.05 to 1 sccm
  • the flow rate of the carrier gas is, for example, in the range of about 50 to 1000 sccm.
  • the carrier gas and the liquid raw material injected from the injection nozzle section 4 are immediately on the outlet side where the cross-sectional area is expanded at an obtuse angle. Since the gas is diffused, the carrier gas flow rate immediately decreases and the vaporization performance of the liquid raw material deteriorates, or the carrier gas stays and deposits adhere to the outlet side of the carrier gas, and the outflow area of the carrier gas is increased. There were problems such as narrowing or blocking the outlet side.
  • the gas diffusion suppression block 100 is provided in the injection nozzle portion 64, and the opening angle ⁇ toward the injection direction forward of the tip portion of the injection nozzle portion 64 in the injection direction. Since the gas diffusion suppression region 130 that spreads at an acute angle is formed, the flow rate of the injected carrier gas is not immediately reduced, but the high flow rate is maintained and the liquid raw material 60 is effectively vaporized. Vaporization performance can be improved. That is, the carrier gas injected from the carrier gas discharge port 128 of the carrier gas nozzle 124 has a gas diffusion suppression region in which the opening angle ⁇ is set to an acute angle, specifically, a narrow range of 5 to 60 degrees. Since it is injected into 130, the diffusion of the carrier gas is suppressed and the injection speed is maintained in a high state, and the vaporization of the liquid raw material injected at this time can be promoted.
  • the opening angle ⁇ is set to be narrow, it is possible to suppress the occurrence of retention of carrier gas as occurred in the conventional vaporizer shown in FIG. It is possible to prevent deposits such as unnecessary thin films from being generated on the inner peripheral surface 132 of the suppression block 100, and an unnecessary thin film adheres to the carrier gas discharge port 128 at the tip of the carrier gas nozzle 124 to reduce the flow path area. It is possible to prevent it from being narrowed or blocked.
  • the opening angle ⁇ is preferably set within a range of 5 to 60 degrees in order to efficiently generate the above-described effects.
  • the length of the gas diffusion suppression region 130 is preferably set within a range of 2 to 15 mm in order to efficiently generate the above-described effects.
  • the liquid material 60 flows out from the material discharge port 126 through the surface of the liquid material nozzle 122 so as to ooze out toward the carrier gas discharge port 128, and tends to block the carrier gas discharge port 128 as a deposit.
  • the raw material discharge port 126 protrudes from the carrier gas discharge port 128 by a length L1
  • the cross-sectional area of the carrier gas channel at the same horizontal level as the raw material discharge port 126 is substantially equal. Therefore, it is possible to prevent the outlet of the carrier gas from being blocked.
  • the opening angle ⁇ is 40 degrees
  • the width W1 of the carrier gas discharge port 128 is 60 ⁇ m
  • the protruding length L1 of the raw material discharge port 126 is 1 mm, the same as the raw material discharge port 126
  • the width W2 of the carrier gas flow path in the horizontal level in the cross-sectional direction is widened to 640 ⁇ m, and this portion can be prevented from being blocked by the widened portion.
  • the protrusion length L1 is preferably set within a range of 0 to 5 mm. If the protrusion length L1 is greater than 5 mm, the flow rate of the carrier gas in the region where the raw material discharge port 126 is located is lowered, and accordingly, the vaporization performance is lowered accordingly.
  • the carrier gas injected from the injection nozzle portion 64 of the vaporizer 12 passes through the gas diffusion suppression region 130 in which the opening angle ⁇ spreads at an acute angle, so the flow rate of the carrier gas decreases. Therefore, it is possible to prevent the carrier gas from staying and to prevent the carrier gas outlet from being clogged with deposits. Therefore, deterioration of the vaporization performance of the liquid raw material 60 can be prevented and high vaporization performance can be maintained.
  • FIG. 5 is a graph showing the relationship between the integrated amount (gram) of the flow rate of the liquid raw material and the supply pressure of the carrier gas in the comparative experiment.
  • FIG. 5 (b) and (c) also show schematic diagrams of the injection nozzle portions of Comparative Examples 1 and 2.
  • the comparative example 1 is formed in the same shape as the injection nozzle unit 4 shown in FIG. 1, the outlet side 6 of the injection nozzle unit 4 extends at an obtuse angle, and the tip side of the injection nozzle unit 4 is in the vaporization chamber 2. Protrusions are provided.
  • the comparative example 2 is formed in the same shape as the injection nozzle unit 4 shown in FIG. 1, the outlet side 6 of the injection nozzle unit 4 extends at an obtuse angle, and the tip side of the injection nozzle unit 4 is in the vaporization chamber 2. It is accommodated in a recess 7 provided in the ceiling.
  • the opening angle ⁇ is set to 40 degrees
  • the protruding length L1 of the raw material discharge port 126 is set to 1 mm
  • the length L2 of the gas diffusion suppression region 130 is set to 8 mm.
  • the carrier gas was always set to flow at 1000 sccm, and the required minimum supply pressure of the carrier gas at that time and the integrated amount of the weight (flow rate) of the flowing liquid material were plotted.
  • the total amount of liquid raw materials was increased to 250 g, and thereafter, it was assumed that the obtained characteristics changed linearly, and overall characteristics were obtained.
  • Characteristic A indicates comparative example 1
  • characteristic B indicates comparative example 2
  • characteristic C indicates the vaporizer 12 of the present embodiment.
  • Characteristics A and B are inclined upward as the integrated amount of liquid raw material increases, and the carrier gas supply pressure gradually increases. This is because deposits adhere to the carrier gas discharge port and gradually close the discharge port as the operation time becomes longer, so that the carrier gas supply pressure must be increased.
  • the slope is larger than that of the characteristic B of Comparative Example 2, and it can be seen that more deposits are attached.
  • the slope of the straight line is almost zero, and the carrier gas discharge port 128 is hardly blocked by deposits, and maintenance is performed. It can be seen that it is not necessary and exhibits good characteristics.
  • the water repellent coating film is formed on the surface of the tip of the liquid material nozzle 122, the surface of the tip of the carrier gas nozzle 124, and the inner peripheral surface 132 of the gas diffusion suppression block 100. It may be. Accordingly, it is possible to prevent the liquid raw material 60 from seeping out and thermally decomposing on these surface portions due to long-term use and depositing deposits and blocking the carrier gas discharge port 128.
  • FIG. 6 is an enlarged partial cross-sectional view showing the tip of the injection nozzle portion of the vaporizer according to the first modification and the vicinity thereof.
  • the same components as those shown in FIGS. 3A and 3B and FIGS. 4A and 4B are denoted by the same reference numerals, and the description thereof is omitted.
  • a water-repellent coating film is formed on at least one of the surface of the tip portion of the injection nozzle portion 64 and the inner peripheral surface 132 of the gas diffusion suppression block 100.
  • the water repellent coating is applied to the surface of the tip of the liquid material nozzle 122, the surface of the tip of the carrier gas nozzle 124, and the inner peripheral surface 132 of the gas diffusion suppression block 100, respectively.
  • Films 144A, 144B, and 144C are formed.
  • a water-repellent coating film 144 A is formed on the outer peripheral surface of the nozzle and the end surface of the material discharge port 126.
  • a water-repellent coating film 144 B is formed on the inner peripheral surface of the nozzle and the end surface of the carrier gas discharge port 128.
  • a water repellent coating film 144C is formed over the entire inner peripheral surface 132. In this case, it is preferable to cover at least 10 mm or more of the tip portion of the spray nozzle portion 64 with the water-repellent coating films 144A and 144B.
  • water-repellent coating films 144A to 144C for example, a Teflon (registered trademark) film, a SiO2 film or the like can be used, and the thickness thereof may be, for example, about 0.1 to 3 ⁇ m.
  • the liquid raw material 60 does not ooze out along the surface of the tip of the injection nozzle portion 64, and the gas diffusion suppression block 100 has a It does not bleed along the peripheral surface 132.
  • the gas diffusion suppression block 100 has a It does not bleed along the peripheral surface 132.
  • FIG. 7 is an enlarged partial cross-sectional view showing the spray nozzle portion and its vicinity of the vaporizer according to the second modification.
  • the same components as those shown in FIGS. 3A and 3B are denoted by the same reference numerals, and the description thereof is omitted.
  • the gas diffusion suppression block 100 and the vaporization vessel 96 are integrated. Specifically, the gas diffusion suppression block 100 and the vaporization container 96 are integrally formed. Only the injection nozzle portion 64 can be inserted into and removed from the nozzle mounting hole 150 formed in the gas diffusion suppression block 100, and the flange portion 106 provided in the injection nozzle portion 64 is fixed with the fixing screw 108 to suppress the gas diffusion.
  • the upper surface of the block 100, that is, the upper surface of the vaporization container 96 is detachably fastened and fixed.
  • the opening angle ⁇ of the gas diffusion suppression region 130 is set to 40 degrees and the cross-section of the gas diffusion suppression region 130 is linear, but the embodiment of the present invention is not limited to this.
  • the opening angle ⁇ of the diffusion suppressing region 130 is in the range of 5 to 60 degrees, the opening angle ⁇ gradually increases as it goes in the gas injection direction, and the inner peripheral surface 132 gradually expands outward in a trumpet shape. You may form in.
  • the liquid raw material 60 used for film formation is formed by dissolving an organic metal material in, for example, an organic solvent.
  • organic solvent include toluene, octane. , Decane, dodecane and the like can be used.
  • the metal contained in the organometallic material has been described by taking the case of La as an example.
  • the present invention is not limited to this, and the organometallic material may be La, Hf, Zr, Sr, Ni, Co.
  • Pt can include one or more metals selected from the group consisting of Pt.
  • the present invention is not limited to this type of metal, and the embodiment of the present invention can be applied to the case of using a raw material containing another metal.
  • the semiconductor wafer includes a silicon substrate and a compound semiconductor substrate such as GaAs, SiC, GaN, and the like, and is not limited to these substrates.
  • the embodiments of the present invention can also be applied to glass substrates, ceramic substrates, and the like used in display devices.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

Un vaporiseur comprend : un récipient de vaporisation dans lequel il est formé une chambre de vaporisation ; une partie à buses de pulvérisation comprenant une première buse, située dans le récipient de vaporisation, qui pulvérise une matière première liquide en son centre, ainsi qu'une seconde buse qui est disposée de manière concentrique autour de la périphérie extérieure de la première buse, qui pulvérise un gaz porteur et forme un gaz de source en vaporisant la matière première liquide au moyen du gaz porteur ; un bloc de suppression de diffusion de gaz qui définit une région de suppression de diffusion de gaz dont un angle d'ouverture s'évase à un angle précis à partir de la pointe de la partie à buses de pulvérisation dans la direction dans laquelle la matière première liquide est pulvérisée et qui est ouverte vers la chambre de vaporisation ; et une sortie de gaz de source par laquelle le gaz de source sort du récipient de vaporisation.
PCT/JP2012/056416 2011-03-28 2012-03-13 Vaporiseur, dispositif d'alimentation en gaz et appareil de formation de film WO2012132878A1 (fr)

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JP2011070661A JP2012204791A (ja) 2011-03-28 2011-03-28 気化装置、ガス供給装置及びこれを用いた成膜装置
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US20150345046A1 (en) * 2012-12-27 2015-12-03 Showa Denko K.K. Film-forming device
WO2014103727A1 (fr) * 2012-12-27 2014-07-03 昭和電工株式会社 DISPOSITIF DE FORMATION DE FILM DE SiC ET PROCÉDÉ DE PRODUCTION DE FILM DE SiC
JP6087621B2 (ja) * 2012-12-27 2017-03-01 昭和電工株式会社 成膜装置
WO2017094469A1 (fr) * 2015-11-30 2017-06-08 株式会社アルバック Appareil d'évacuation de vapeur et procédé de formation de film
JP7402801B2 (ja) * 2018-08-24 2023-12-21 株式会社堀場エステック 気化器、液体材料気化装置、及び気化方法
JP7417191B2 (ja) * 2020-01-30 2024-01-18 セイコーエプソン株式会社 液体噴射装置

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JP2004211183A (ja) * 2003-01-07 2004-07-29 Shimadzu Corp 気化器
JP2004335564A (ja) * 2003-05-01 2004-11-25 Japan Pionics Co Ltd 気化器
JP2005026599A (ja) * 2003-07-01 2005-01-27 Lintec Co Ltd 液体気化供給器及びこれを用いた液体気化供給装置
JP2005228889A (ja) * 2004-02-12 2005-08-25 Tokyo Electron Ltd 成膜装置
JP2009054655A (ja) * 2007-08-23 2009-03-12 Tokyo Electron Ltd 気化器、気化器を用いた原料ガス供給システム及びこれを用いた成膜装置

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
JP2004211183A (ja) * 2003-01-07 2004-07-29 Shimadzu Corp 気化器
JP2004335564A (ja) * 2003-05-01 2004-11-25 Japan Pionics Co Ltd 気化器
JP2005026599A (ja) * 2003-07-01 2005-01-27 Lintec Co Ltd 液体気化供給器及びこれを用いた液体気化供給装置
JP2005228889A (ja) * 2004-02-12 2005-08-25 Tokyo Electron Ltd 成膜装置
JP2009054655A (ja) * 2007-08-23 2009-03-12 Tokyo Electron Ltd 気化器、気化器を用いた原料ガス供給システム及びこれを用いた成膜装置

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