WO2010018768A1 - 金属回収方法、金属回収装置、排気系及びこれを用いた成膜装置 - Google Patents
金属回収方法、金属回収装置、排気系及びこれを用いた成膜装置 Download PDFInfo
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- WO2010018768A1 WO2010018768A1 PCT/JP2009/063810 JP2009063810W WO2010018768A1 WO 2010018768 A1 WO2010018768 A1 WO 2010018768A1 JP 2009063810 W JP2009063810 W JP 2009063810W WO 2010018768 A1 WO2010018768 A1 WO 2010018768A1
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- Prior art keywords
- gas
- metal recovery
- exhaust gas
- metal
- collection
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- B01D2258/0216—Other waste gases from CVD treatment or semi-conductor manufacturing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Definitions
- the present invention relates to a metal recovery method, a metal recovery apparatus, an exhaust system, and a film forming apparatus using the same, which recover a metal component in an unreacted source gas in an exhaust gas discharged from a film forming apparatus.
- a process of forming a desired thin film on a surface of a semiconductor wafer, an LCD substrate or the like and a process of etching the film into a desired pattern are repeatedly performed. .
- a silicon thin film, a silicon oxide thin film, and a silicon nitride thin film are reacted by reacting a predetermined processing gas (raw material gas) in a processing container during this process. Then, a metal thin film, a metal oxide thin film, a metal nitride thin film, or the like is formed on the surface of the object to be processed. At this time, an extra reaction by-product is generated simultaneously with the film formation reaction and is discharged together with the exhaust gas. Unreacted processing gas is also discharged.
- a predetermined processing gas raw material gas
- this reaction by-product or unreacted processing gas is released into the atmosphere as it is, it causes environmental pollution.
- a trap mechanism is provided in the exhaust system extending from the processing vessel, thereby capturing reaction by-products and unreacted processing gas contained in the exhaust gas. It is supposed to be removed.
- this trap mechanism when removing reaction by-products that condense (liquefy) and solidify (solidify) at room temperature, this trap mechanism is configured by providing a large number of fins in a casing having an exhaust gas inlet and an exhaust port as an example. ing. The fins are arranged along the flow direction of the exhaust gas. When the exhaust gas passes between the fins, the reaction by-products in the exhaust gas are attached to the fin surface and captured, and discarded. It is supposed to be.
- this fin is cooled by a cooling medium or the like to increase the capture efficiency (for example, JP2001-214272A).
- a scrubber device that sprays water or the like as a trap mechanism is used to recover the reaction by-products and unreacted gas components in the sprayed water by bringing the exhaust gas into contact with the sprayed water and collecting it. It has been broken.
- a cartridge-type adsorption tower which is made detachable on the premise of disposal is provided, and reaction by-products and unreacted raw material gas components are adsorbed and removed from the exhaust gas. Some have done.
- the adsorption tower having the lowered removal capacity is discarded and replaced with a new adsorption tower.
- the reason for discarding in this way is that it is relatively difficult to regenerate useful metals from the recovered reaction byproducts when the source gas contains a halogen element such as fluorine (F) or chlorine (Cl). That's why.
- exhaust gas discharged from the trap mechanism often contains harmful gas components.
- This harmful gas component was detoxified by a detoxifying device provided on the downstream side (rear stage) of the trap mechanism, and then this exhaust gas was released into the atmosphere.
- a thin film is formed by using a raw material (source gas) of an organometallic compound containing a noble metal such as silver, gold, or ruthenium. Forming is also done.
- a noble metal such as silver, gold, or ruthenium.
- Such noble metals are very expensive.
- the raw materials of the organometallic compound as described above there are raw materials that contain C, H, O, etc. in addition to metal atoms but do not contain halogen elements such as F and Cl. Therefore, the application of the collection method based on the premise of the disposal of the collected material as described above has a problem that the expensive metal is wasted and the running cost is increased. .
- a conventional trap mechanism using a scrubber device or fins must be provided with a separate detoxifying device for detoxifying exhaust gas exhausted from the trap mechanism, which increases the installation space. There was a problem such as.
- An object of the present invention is to recover metal components from exhaust gas discharged from a processing container that forms a thin film on the surface of an object to be processed and to remove exhaust gas while having a simple structure with a small space.
- An object of the present invention is to provide a metal recovery method, a metal recovery apparatus, an exhaust system, and a film forming apparatus using the same.
- the metal recovery method recovers a metal component from exhaust gas discharged from a processing vessel that forms a thin film on the surface of an object to be processed using a source gas made of an organometallic compound source.
- a metal recovery method for removing exhaust gas wherein the exhaust gas is brought into contact with a heated collecting member to thermally decompose unreacted source gas contained in the exhaust gas,
- the exhaust gas when recovering metal components from the exhaust gas discharged from the processing vessel that forms a thin film on the surface of the object to be processed using the raw material gas made of the organometallic compound, the exhaust gas is heated and exhausted.
- a detoxification process that oxidizes and detoxifies harmful gas components contained in the exhaust gas, so that a thin film is formed on the surface of the object to be processed using a space saving and simple structure recovery device.
- the metal component can be recovered from the exhaust gas discharged from the processing container forming the gas, and the exhaust gas can be removed.
- the recovered metal component can be reused without being discarded, the running cost can be reduced accordingly.
- the reuse it is not necessary to perform a complicated refining operation, and it can be easily taken out as a raw material.
- the detoxification step may be performed in the presence of an oxidizing gas.
- the collection step may be performed in the presence of an oxidizing gas.
- the temperature of the catalyst in the detoxification step may be in the range of 600 to 800 ° C.
- the temperature of the collecting member in the collecting step may be in the range of 600 to 1000 ° C.
- the catalyst may be made of one or more materials selected from the group consisting of MnO 2 , CaO, MgO, HfO 2 , and Ta 2 O 5 .
- the oxidizing gas may be composed of one or more gases selected from the group consisting of O 2 , O 3 , H 2 O, and air.
- the organometallic compound may be Ru 3 (CO) 12 and the gas discharged through the detoxification step may be CO 2 gas.
- a metal recovery apparatus recovers metal components from exhaust gas discharged from a processing vessel that forms a thin film on the surface of an object to be processed using a raw material gas made of an organic metal compound.
- a collection unit having a collection member configured to adhere; a detoxification unit having a catalyst that oxidizes and detoxifies harmful gas components contained in the exhaust gas that has passed through the collection unit; Is provided.
- the exhaust gas is heated in the metal recovery device that recovers the metal components from the exhaust gas discharged from the processing container that forms a thin film on the surface of the object to be processed using the raw material gas made of the organic metal compound.
- the collection unit and the abatement unit may be sequentially arranged in a casing along a flow direction of the exhaust gas.
- the collection unit may have a collection member heating mechanism for heating the collection member.
- the abatement unit may have a catalyst heating mechanism for heating the catalyst.
- the collection member may include a plurality of collection pieces housed in a casing.
- the collection member may have a plurality of wire meshes arranged along the flow direction of the exhaust gas.
- the collection member may include a plurality of punching plates having vent holes arranged along the flow direction of the exhaust gas.
- the metal recovery apparatus may have an oxidizing gas supply mechanism that supplies an oxidizing gas toward the collection unit.
- the metal recovery apparatus may have an oxidizing gas supply mechanism that supplies an oxidizing gas toward the abatement unit.
- the temperature of the catalyst may be in the range of 600 to 800 ° C.
- the temperature of the collecting member may be in the range of 600 to 1000 ° C.
- the catalyst may be made of one or more materials selected from the group consisting of MnO 2 , CaO, MgO, HfO 2 , and Ta 2 O 5 .
- the oxidizing gas may be composed of one or more gases selected from the group consisting of O 2 , O 3 , H 2 O, and air.
- the organometallic compound may be Ru 3 (CO) 12 and the gas discharged from the abatement unit may be CO 2 gas.
- An exhaust system is connected to a processing vessel that forms a thin film on the surface of an object to be processed using a raw material gas made of an organic metal compound, and a metal is discharged from the exhaust gas discharged from the processing vessel.
- An exhaust system that recovers components and removes exhaust gas, and is provided with an exhaust passage connected to an exhaust port of the processing container, a vacuum pump interposed in the exhaust passage, and an exhaust passage. Any of the above-described metal recovery apparatuses according to one embodiment of the present invention.
- a film forming apparatus is a film forming apparatus for performing a film forming process on an object to be processed, and a processing container that can be evacuated, and the object to be processed in the processing container.
- FIG. 1 is a configuration diagram schematically showing a film forming apparatus having a metal recovery apparatus according to an embodiment of the present invention.
- FIG. 2 is a longitudinal sectional view showing an example of the configuration inside the metal recovery apparatus.
- FIG. 3 is a flowchart for explaining the metal recovery method according to the consistent embodiment of the present invention.
- FIG. 4A is a schematic diagram for explaining a general situation in which a raw material gas is pyrolyzed and a metal component is collected.
- FIG. 4B is a schematic diagram for explaining a general situation where harmful gas is removed.
- FIG. 5A is a schematic diagram for explaining a situation where Ru 3 (CO) 12 that is a source gas is thermally decomposed and a metal component is collected.
- FIG. 5B is a schematic diagram for explaining a situation where harmful gas generated by thermally decomposing Ru 3 (CO) 12 as a raw material gas is removed.
- FIG. 6A is a diagram schematically showing a configuration of a modification of the collection unit.
- FIG. 6B is a diagram schematically showing a configuration of a modification of the collection unit.
- FIG. 1 is a schematic configuration diagram showing a film forming apparatus having a metal recovery device
- FIG. 2 is an enlarged cross-sectional configuration diagram showing an example in the metal recovery device.
- Ru 3 (CO) 12 that is a carbonyl-based organometallic compound is used as a raw material for an organometallic compound
- CO carbon monoxide
- a film forming apparatus 2 includes a film forming apparatus main body 4 that actually performs a film forming process on a semiconductor wafer W as an object to be processed, and the film forming apparatus main body 4.
- the material gas supply system 6 for supplying the film forming material gas and the exhaust system 8 for exhausting the exhaust gas from the film forming apparatus main body 4 are mainly configured.
- the film forming apparatus main body 4 has a cylindrical processing container 10 made of, for example, an aluminum alloy.
- a holding mechanism 12 that holds a semiconductor wafer W as an object to be processed is provided.
- the holding mechanism 12 includes a disk-shaped mounting table 16 erected from a container bottom by a support column 14, and the wafer W is mounted on the mounting table 16.
- the mounting table 16 is made of a ceramic material such as AlN (aluminum nitride).
- a heating mechanism 18 made of, for example, tungsten wire is provided in the mounting table 16 so as to heat the wafer W.
- the heating mechanism 18 is not limited to a tungsten wire or the like, and for example, a heating lamp may be used.
- An exhaust port 20 is provided at the bottom of the processing container 10, and the exhaust system 8 is connected to the exhaust port 20 so that the atmosphere in the processing container 10 can be evacuated.
- the exhaust system 8 will be described later.
- An opening 22 for carrying in and out the wafer W is formed on the side wall of the processing container 10, and the opening 22 is provided with a gate valve 24 for opening and closing the opening.
- a gas introduction mechanism 28 including, for example, a shower head 26 is provided on the ceiling portion of the processing container 10 so that necessary gas is supplied into the processing container 10 from a gas ejection hole 30 provided on the lower surface. It has become.
- the gas inlet 26A of the shower head 26 has the source gas supply system 6 and other necessary gas, the gas supply system is connected.
- the raw material gas and other gases may be mixed in the shower head 26, or may be separately introduced into the shower head 26 and mixed separately in the processing vessel 10.
- the shower head 26 is used as the gas introduction mechanism 28, but a simple nozzle or the like may be used instead.
- the source gas supply system 6 has a source tank 32 for storing a solid source or a liquid source.
- the raw material tank 32 contains, for example, a solid raw material 34 that is a raw material of the organometallic compound.
- Ru 3 (CO) 12 is used as described above.
- the solid material 34 generally has a characteristic that vapor pressure is very low and evaporation is difficult.
- a liquid raw material in which a raw material gas is formed by bubbling or the like may be used.
- One end is connected to the gas outlet 36 provided in the ceiling portion of the raw material tank 32, and the other end is connected to the gas inlet 26A of the shower head 26 of the film forming apparatus body 4 to provide a raw material passage 38.
- the raw material gas generated in the raw material tank 32 can be supplied.
- An opening / closing valve 40 is interposed in a portion of the raw material passage 38 close to the raw material tank 32.
- a carrier gas pipe 42 for supplying a carrier gas to the raw material tank 32 is connected to the lower surface side of the raw material tank 32.
- a flow rate controller 44 such as a mass flow controller and a carrier gas on / off valve 46 are sequentially provided in the middle of the carrier gas pipe 42 to supply the carrier gas while controlling the flow rate to heat the solid material 34. By doing so, the solid raw material 34 is vaporized to form a raw material gas.
- a porous plate 48 is installed in the vicinity of the side where the carrier gas pipe 42 is installed to hold the solid raw material 34 on the porous plate 48, and the carrier gas pipe.
- the carrier gas supplied from 42 is uniformly supplied into the raw material tank 32 through the holes formed in the porous plate 48.
- CO (carbon monoxide) gas is used as the carrier gas.
- the raw material tank 32 is provided with a tank heating mechanism 50 for heating the raw material tank 32 so as to cover the entire tank, thereby promoting the vaporization of the solid raw material 34.
- the heating temperature of the solid raw material 34 is a temperature lower than the decomposition temperature.
- a bypass pipe 52 is provided so as to connect the upstream side of the carrier gas pipe 42 with respect to the carrier gas on-off valve 46 and the downstream side of the on-off valve 40 of the raw material passage 38.
- the bypass pipe 52 is provided with a bypass opening / closing valve 54 so that the carrier gas can flow by bypassing the raw material tank 32 as necessary.
- the raw material passage 38 is provided with a heating mechanism (not shown) such as a tape heater, which is heated to prevent the raw material gas from solidifying.
- the exhaust system 8 has an exhaust passage 60 connected to the exhaust port 20 of the processing container 10, and the atmosphere in the processing container 10 is exhausted along the exhaust passage 60. Specifically, a pressure regulating valve 62, a vacuum pump 64, and a metal recovery device 66 are sequentially provided in the exhaust passage 60 from the upstream side toward the downstream side.
- the pressure adjusting valve 62 is constituted by a butterfly valve, for example, and has a function of adjusting the pressure in the processing vessel 10.
- the vacuum pump 64 is, for example, a combination of a turbo molecular pump and a dry pump, and can evacuate the atmosphere in the processing vessel 10.
- the metal recovery device 66 exposes the exhaust gas flowing in the exhaust passage 60 to a high temperature, decomposes the unreacted raw material gas contained in the exhaust gas, recovers the metal component, and further in the exhaust gas Oxidizes harmful components and eliminates them.
- the unreacted source gas that is, Ru 3 (CO) 12 gas is recovered. This configuration will be described later.
- an opening / closing valve 68 is provided in each of the exhaust passage 60 upstream of the metal recovery device 66 and the exhaust passage 60 downstream of the metal recovery device 66. During maintenance of the metal recovery device 66, the metal recovery device 66 can be shut off from the exhaust passage 60 side by closing the on-off valve 68.
- the metal recovery device 66 has an outer shell formed by a casing 70 formed into a cylindrical shape by, for example, stainless steel.
- a gas inlet 72 is formed in the upper part of the housing 70 and a gas outlet 74 is formed in the lower part.
- the gas inlet 72 is hermetically connected to one side of the exhaust passage 60 via a seal member 76 such as an O-ring by a flange portion 72A formed here.
- the gas outlet 74 is hermetically connected to the other side of the exhaust passage 60 through a seal member 78 such as an O-ring by a flange portion 74A formed here.
- the exhaust gas is exposed to a high temperature, and the unreacted source gas contained in the exhaust gas is thermally decomposed to capture the metal components contained in the source gas.
- a collection unit 80 that collects and a detoxification unit 82 that oxidizes and removes harmful gas components contained in the exhaust gas that has passed through the collection unit 80 are arranged in order along the flow direction of the exhaust gas. Has been.
- the collection unit 80 has a collection member 84 for adhering the metal component generated by the thermal decomposition.
- the collection member 84 has a plurality (a large number) of collection pieces 86 formed in a spherical shape, a lump shape, or a block shape.
- the collection piece 86 is accommodated in a cylindrical casing 88 so that it can be taken out.
- the casing 88 is made of, for example, stainless steel.
- a large number of ventilation holes 90 and 92 for passing exhaust gas are formed in the ceiling and bottom of the casing 88, respectively, so that the exhaust gas can pass through the casing 88.
- a collecting member heating mechanism 94 made of, for example, a tungsten heater is provided on the outer periphery of the casing 88 to heat the collecting member 84, and the collecting piece 86 is moved to a predetermined temperature, for example, 600. It can be heated to temperatures in the range of ⁇ 1000 ° C.
- the diameter of the collection piece 86 may be set to 10 mm or more.
- a ceramic piece made of silicon piece, aluminum nitride, alumina, or the like can be used in addition to a metal piece such as stainless steel.
- the abatement unit 82 disposed downstream of the collection unit 80 is a catalyst that oxidizes and removes harmful gas components contained in the exhaust gas flowing through the collection unit 80. 100.
- the catalyst 100 has a spherical shape, a block shape, or a block shape.
- the catalyst 100 is accommodated in a cylindrical casing 102 so that it can be taken out.
- the casing 102 is made of, for example, stainless steel.
- a large number of vent holes 104 and 106 for allowing exhaust gas to pass therethrough are formed in the ceiling and bottom of the casing 102, respectively, and the exhaust gas that has passed through the collection unit 80 passes through the casing 102. You can pass through.
- a catalyst heating mechanism 108 made of, for example, a tungsten heater is provided on the outer periphery of the casing 102 to heat the catalyst 100.
- the catalyst 100 is kept at a predetermined temperature, for example, within a range of 600 to 800 ° C. It can be heated to a temperature of
- the diameter thereof is preferably set to 5 mm or more.
- the catalyst 100 can be used MnO 2, CaO, MgO, HfO 2, Ta 2 O 5 or the like.
- the casing 70 is connected to an oxidizing gas supply mechanism 110 for supplying oxidizing gas into the casing 70.
- the oxidizing gas supply mechanism 110 includes a shower head 112 formed in a circular ring shape provided at a ceiling portion in the casing 70, that is, an uppermost stream portion in the casing 70 of the exhaust gas flow. Have.
- the shower head 112 is connected to a gas flow path 116 provided with an on-off valve 114 in the middle.
- the flow rate-controlled oxidizing gas is supplied from the plurality of gas injection holes 112 ⁇ / b> A formed in the shower head 112 toward substantially the entire upstream side of the collection unit 80.
- the oxidizing gas supplied from the shower head 112 flows not only into the collection unit 80 but also into the abatement unit 82 located downstream thereof.
- the shower head 112 of the oxidizing gas supply mechanism 110 is installed between the collection unit 80 and the abatement unit 82.
- This oxidizing gas O 2 can be used.
- the structure of the oxidizing gas supply mechanism 110 is not limited to the above structure.
- a passage heater 120 such as a tape heater is provided in the exhaust passage 60 from the exhaust port 20 of the processing vessel 10 to the metal recovery device 66 and each member interposed in the middle thereof.
- the exhaust gas flowing in the exhaust passage 60 is heated to about 110 ° C., for example, depending on the raw material used, and unreacted source gas in the unreacted exhaust gas is condensed (solidified) on the way. ) To prevent.
- the overall operation of the film forming apparatus 2 configured as described above, for example, control of start of gas supply, stop of gas supply, process temperature, process pressure, supply of oxidizing gas in the metal recovery device 66, etc. For example, it is performed by the control device 122 formed of a computer.
- a computer-readable program necessary for this control is stored in a storage medium 124.
- a storage medium 124 a flexible disk, a CD (Compact Disc), a CD-ROM, a hard disk, a flash memory, a DVD, or the like is used. Can do.
- an auxiliary trap mechanism for auxiliaryly collecting a part of the unreacted raw material gas may be installed upstream of the metal recovery device 66.
- FIG. 3 is a process diagram for explaining a metal recovery method
- FIGS. 4A and 4B are schematic diagrams showing a general situation in which a raw material gas is thermally decomposed to collect metal components and remove harmful gases
- FIG. 5A is a schematic diagram showing a situation where Ru 3 (CO) 12 which is a raw material gas is thermally decomposed to collect metal components and remove harmful gases.
- the vacuum pump 64 of the exhaust system 8 is continuously driven to evacuate the processing container 10 to a predetermined pressure.
- the semiconductor wafer W on the mounting table 16 is maintained at a predetermined temperature by the heating mechanism 18.
- the side wall of the processing vessel 10 and the shower head 26 are also maintained at predetermined temperatures by a vessel-side heating mechanism (not shown).
- the entire raw material gas supply system 6 is heated to a predetermined temperature in advance by a tank heating mechanism 50 or a passage heating mechanism (not shown).
- the carrier gas (CO) whose flow rate is controlled is supplied into the raw material tank 32 via the carrier gas pipe 42.
- the solid material 34 stored in the inside is heated and vaporized, thereby generating a material gas.
- the generated raw material gas flows in the raw material passage 38 toward the downstream side together with the carrier gas.
- This source gas is introduced from the shower head 26 of the film forming apparatus body 4 into the processing container 10 in a reduced pressure atmosphere.
- a Ru metal thin film is formed on the wafer W by, for example, CVD (Chemical Vapor Deposition).
- the process pressure can be set to about 0.1 Torr (13.3 Pa)
- the wafer temperature can be set to about 200 to 250 ° C.
- the temperature of the sidewall of the processing vessel 10 can be set to about 75 to 80 ° C.
- Ru 3 (CO) 12 which is a solid raw material 34 is a raw material which has a very low vapor pressure and hardly evaporates (vaporizes), and contributes very little to the film forming reaction, and is about 90% of the raw material.
- the gas flows down through the exhaust passage 60 of the exhaust system 8 together with the carrier gas CO in an unreacted state.
- the reaction at this time is represented by the following chemical formula, and CO (carbon monoxide), which is the same gas type as the carrier gas, is generated by the reaction.
- the exhaust gas flowing down the exhaust passage 60 passes through the pressure regulating valve 62, the vacuum pump 64, and the metal recovery device 66 in order, and is then diffused into the atmosphere.
- the metal component of the unreacted raw material gas is recovered in the metal recovery device 66, only the CO gas remains as the exhaust gas. Therefore, the CO gas is further oxidized in the metal recovery device 66. It becomes CO 2 and is released into the atmosphere.
- step S1 the exhaust gas is exposed to a high temperature, and the unreacted source gas contained in the exhaust gas is thermally decomposed to collect the metal component contained in the source gas into the collecting member 84.
- step S2 an abatement process for oxidizing and detoxifying harmful gas components contained in the exhaust gas by bringing the exhaust gas having passed through the collecting process into contact with the catalyst 100 ) And are performed.
- the exhaust gas flowing in the exhaust passage 60 is introduced into the housing 70 from the gas inlet 72 provided in the ceiling portion of the metal recovery device 66 and flows into the collection unit 80, and then into the casing 88. It flows toward the downstream side in contact with the surfaces of a large number of collecting pieces 86 constituting the collecting member 84 accommodated in the container.
- the collection piece 86 is heated by the collection member heating mechanism 94 to a predetermined temperature, that is, within a range of 600 to 1000 ° C. which is a temperature at which unreacted source gas can be thermally decomposed.
- the source gas, that is, Ru 3 (CO) 12 is thermally decomposed into “Ru” and “CO”. And among these, "Ru" which is a metal component adheres to the surface of the collection piece 86 made into the said high temperature state, and is collected.
- FIGS. 4A and 5A The situation at this time is schematically shown in FIGS. 4A and 5A.
- a source gas in which a ligand 132 is bonded to a metal atom 130 is exposed to a high temperature. Then, it is thermally decomposed and separated into the metal atom 130 and the ligand 132, and the metal atom 130 adheres to the surface of the high temperature collection piece 86.
- the ligand includes any one or more of carbon (C), oxygen (O), and hydrogen (H), preferably any two or more, and fluorine or chlorine. Halogen elements such as are not included.
- Ru 3 (CO) 12 is used as a raw material and CO (carbon monoxide) is used as a carrier gas, so that Ru is separated as a metal component, and The ligand is desorbed to generate CO, and the carrier gas, CO, remains as it is.
- CO carbon monoxide
- the exhaust gas from which the metal component is collected in the collection unit 80 passes through the collection unit 80 and is then subjected to downstream detoxification in a state containing “CO” which is a harmful component. It flows into the unit 82.
- the exhaust gas flows in the abatement unit 82 while being in contact with a catalyst made of, for example, MnO 2 or CaO heated to a high temperature, for example, 600 to 800 ° C. by the catalyst heating mechanism 108.
- O 2 gas is introduced as an oxidizing gas into the casing 70 from the oxidizing gas supply mechanism 110 provided on the ceiling of the casing 70, so that the O 2 gas is mixed in the exhaust gas. Yes. Therefore, the toxic gas, CO, is promoted by the catalytic action of the catalyst 100 in a high temperature state, and the oxidation reaction with the O 2 gas is promoted to be detoxified as CO 2 .
- the ligand 132 containing C, O, and H is oxidized with O 2 gas to be detoxified as CO 2 , H 2 O, and O 2 .
- the CO component is oxidized to CO 2 and detoxified.
- the exhaust gas contains only gas components that are safe to the human body even if released into the atmosphere, such as CO 2 , H 2 O, O 2, etc. Therefore, this metal recovery device 66 The exhaust gas exhausted from the air is released into the atmosphere as it is.
- the metal component adhering to the collection piece 86 is recovered and reused by periodically exchanging the collection unit 80. Moreover, since there is nothing adhering to the catalyst 100 of the abatement unit 80, this catalyst 100 is repeatedly used semipermanently.
- a processing container for forming a thin film on the surface of an object to be processed for example, a semiconductor wafer W, using a source gas of an organometallic compound, for example, a source gas made of Ru 3 (CO) 12.
- a source gas of an organometallic compound for example, a source gas made of Ru 3 (CO) 12.
- the exhaust gas is brought into contact with a heated collecting member to thermally decompose the unreacted source gas contained in the exhaust gas into the source gas.
- a collecting step for adhering the contained metal component to the collecting member, and contacting exhaust gas that has passed through the collecting step with the catalyst 100 oxidizes and removes harmful gas components contained in the exhaust gas.
- a decontamination process so that metal components can be circulated from the exhaust gas discharged from the processing vessel that forms a thin film on the surface of the object to be processed, while using a space-saving and simple metal recovery device. And, and, it is possible to detoxify the exhaust gas.
- the recovered metal component is reused without being discarded, the running cost can be reduced accordingly.
- the reuse it is not necessary to perform a complicated refining operation, and it can be easily taken out as a raw material.
- a metal recovery apparatus that recovers metal components from exhaust gas discharged from a processing vessel that forms a thin film on the surface of the object to be processed using a raw material gas made of an organometallic compound
- the exhaust gas is exposed to a high temperature.
- FIG. 6A and 6B are diagrams schematically showing a configuration of a modification of the collection unit.
- constituent parts that can be configured identically to the constituent parts shown in FIG.
- FIG. 6A shows a modification of the collection unit 80, in which a plurality of punching plates 140 are used as the collection member 84.
- a plurality of (many) vent holes 140A are formed over the entire surface.
- the punching plates 140 are arranged at a predetermined pitch along the exhaust gas flow direction.
- the punching plates 140 adjacent to each other in the vertical direction are arranged such that the vent holes 140A are displaced in the horizontal direction or the front-rear direction in the horizontal plane so that the exhaust gas does not flow linearly. Efficiently contacts the surface of the punching plate 140.
- a collecting member heating mechanism 94 is provided on a side portion of each punching plate 140 so that the punching plate 140 can be heated.
- a material of the punching plate 140 for example, stainless steel, ceramic or the like can be used. Also according to the first modification, it is possible to obtain the same effects as the effects described in the above-described embodiment, and it is possible to attach and collect metal components in the exhaust gas.
- FIG. 6B shows another modification of the collection unit 80, in which a plurality of wire nets 146 are used as the collection member 84.
- the plurality of wire meshes 146 are arranged at a predetermined pitch along the flow direction of the exhaust gas.
- a collecting member heating mechanism 94 is provided on the side portion of each wire mesh 146 so that the wire mesh 146 can be heated.
- a material of the wire mesh 146 for example, stainless steel, tungsten, or the like can be used. Also according to the second modified example, the same effect as the effect described in the above embodiment can be obtained, and the metal component in the exhaust gas can be attached and collected.
- the case where MnO 2 or CaO is used as the catalyst 100 has been described as an example.
- the present invention is not limited thereto, and examples of the catalyst 100 include MnO 2 , CaO, MgO, HfO 2 , One or more materials selected from the group consisting of Ta 2 O 5 can be used.
- O 2 gas is used as the oxidizing gas.
- the present invention is not limited to this, and is selected from the group consisting of O 2 , O 3 , H 2 O, and air (mixed gas of oxygen and nitrogen). One or more gases can be used.
- the case where Ru 3 (CO) 12 is used as the raw material of the organometallic compound has been described as an example.
- the present invention is not limited to this, and the raw material of the organometallic compound does not include a halogen element.
- Each of the above raw materials contains a ligand containing, for example, C, O, and H in addition to the metal component.
- a halogen element such as fluorine or chlorine is contained in the raw material because a complicated purification process (work) is required.
- a metal that is easily oxidized may be recovered as a metal oxide, such as Mn or Ta, in this case, as shown in FIG.
- a reducing gas may be used in addition to the raw material gas for forming the metal film. In this case, H 2 gas or the like is used as the reducing gas, and this H 2 gas is also described above. To be abolished.
- 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 present invention can also be applied to glass substrates, ceramic substrates, and the like used in display devices.
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Abstract
Description
Ru3(CO)12↑ ⇔ Ru3(CO)12-x↑+XCO↑
Ru3(CO)12-x↑+Q → 3Ru+(12-X)CO↑
Ru3(CO)12↑+Q → 3Ru+12CO↑
ここで”⇔”は可逆的であることを示し、”↑”はガス状態であることを示し、”↑”が付いていないものは固体状態であることを示し、”Q”は熱量が加わることを示している。
次に、上記捕集ユニット80の変形例について説明する。先の図2に示す金属回収装置66の捕集ユニット80では、捕集部材84として多数の例えば球体状の捕集片86を用いたが、これに限定されず、以下に説明するような構造としてもよい。図6Aおよび図6Bは捕集ユニットの変形例の構成を概略的に示す図である。尚、図6Aおよび図6B中において、図2に示す構成部分と同一に構成され得る構成部分については同一参照符号を付して、その説明を省略する。
Claims (26)
- 有機金属化合物の原料よりなる原料ガスを用いて被処理体の表面に薄膜を形成する処理容器より排出される排気ガス中から、金属成分を回収して排気ガスを除害する金属回収方法であって、
前記排気ガスを加熱された捕集部材に接触させることにより該排気ガス中に含まれる未反応の前記原料ガスを熱分解させ、前記原料ガス中に含まれている金属成分を前記捕集部材に付着させる捕集工程と、
前記捕集工程を経た前記排気ガスを触媒に接触させることにより前記排気ガス中に含まれる有害なガス成分を酸化して除害する除害工程と、を有することを特徴とする金属回収方法。 - 前記除害工程は、酸化ガスの存在下で行われることを特徴とする請求項1記載の金属回収方法。
- 前記捕集工程は、酸化ガスの存在下で行われることを特徴とする請求項1記載の金属回収方法。
- 前記除害工程の前記触媒の温度は600~800℃の範囲内であることを特徴とする請求項1記載の金属回収方法。
- 前記捕集工程の前記捕集部材の温度は600~1000℃の範囲内であることを特徴とする請求項1記載の金属回収方法。
- 前記触媒は、MnO2、CaO、MgO、HfO2、Ta2O5よりなる群から選択される1以上の材料よりなることを特徴とする請求項1記載の金属回収方法。
- 前記酸化ガスは、O2、O3、H2O、空気よりなる群から選択される1以上のガスよりなることを特徴とする請求項1記載の金属回収方法。
- 前記有機金属化合物は、Ru3(CO)12、TEMAT(テトラキスエチルメチルアミノチタニウム)、TAIMATA、Cu(EDMDD)2、Ru3(CO)12、W(CO)6、TaCl5、TMA(トリメチルアルミニウム)、TBTDET(ターシャリーブチルイミド-トリ-ジエチルアミドタンタル)、PET(ペンタエトキシタンタル)、TMS(テトラメチルシラン)、TEH(テトラキスエトキシハフニウム)、Cp2Mn[=Mn(C5H5)2]、(MeCp)2Mn[=Mn(CH3C5H4)2]、(EtCp)2Mn[=Mn(C2H5C5H4)2]、(i-PrCp)2Mn[=Mn(C3H7C5H4)2]、MeCpMn(CO)3[=(CH3C5H4)Mn(CO)3]、(t-BuCp)2Mn[=Mn(C4H9C5H4)2]、CH3Mn(CO)5、Mn(DPM)3[=Mn(C11H19O2)3]、Mn(DMPD)(EtCp)[=Mn(C7H11C2H5C5H4)]、Mn(acac)2[=Mn(C5H7O2)2]、Mn(DPM)2[=Mn(C11H19O2)2]、Mn(acac)3[=Mn(C5H7O2)3]よりなる群から選択されるハロゲン元素を含まない1以上の材料よりなることを特徴とする請求項1記載の金属回収方法。
- 前記有機金属化合物はRu3(CO)12であり、前記除害工程を経て排出されるガスはCO2ガスであることを特徴とする請求項1記載の金属回収方法。
- 有機金属化合物の原料よりなる原料ガスを用いて被処理体の表面に薄膜を形成する処理容器から排出される排気ガス中から、金属成分を回収して排気ガスを除害する金属回収装置であって、
前記排気ガスを加熱して該排気ガス中に含まれる未反応の前記原料ガスを熱分解させて前記原料ガス中に含まれている金属成分を付着させるように構成された捕集部材を有する捕集ユニットと、
前記捕集ユニットを通過した前記排気ガス中に含まれる有害なガス成分を酸化して除害する触媒を有する除害ユニットと、を備えたことを特徴とする金属回収装置。 - 前記捕集ユニットと前記除害ユニットとは筐体内に、前記排気ガスの流れ方向に沿って順に配列されていることを特徴とする請求項10記載の金属回収装置。
- 前記捕集ユニットは、前記捕集部材を加熱する捕集部材加熱機構を有することを特徴とする請求項10記載の金属回収装置。
- 前記除害ユニットは、前記触媒を加熱する触媒加熱機構を有することを特徴とする請求項10記載の金属回収装置。
- 前記捕集部材は、ケーシング内に収容された複数の捕集片と、を有することを特徴とする請求項10記載の金属回収装置。
- 前記捕集部材は、前記排気ガスの流れ方向に沿って配列された複数の金網を有することを特徴とする請求項10記載の金属回収装置。
- 前記捕集部材は、前記排気ガスの流れ方向に沿って配列された、通気孔を有する複数のパンチング板を有することを特徴とする請求項10記載の金属回収装置。
- 前記捕集ユニットに向けて酸化ガスを供給する酸化ガス供給機構を有することを特徴とする請求項10記載の金属回収装置。
- 前記除害ユニットに向けて酸化ガスを供給する酸化ガス供給機構を有することを特徴とする請求項10記載の金属回収装置。
- 前記触媒の温度は、600~800℃の範囲内であることを特徴とする請求項10記載の金属回収装置。
- 前記捕集部材の温度は、600~1000℃の範囲内であることを特徴とする請求項10記載の金属回収装置。
- 前記触媒は、MnO2、CaO、MgO、HfO2、Ta2O5よりなる群から選択される1以上の材料よりなることを特徴とする請求項10記載の金属回収装置。
- 前記酸化ガスは、O2、O3、H2O、空気よりなる群から選択される1以上のガスよりなることを特徴とする請求項10記載の金属回収装置。
- 前記有機金属化合物は、Ru3(CO)12、TEMAT(テトラキスエチルメチルアミノチタニウム)、TAIMATA、Cu(EDMDD)2、Ru3(CO)12、W(CO)6、TaCl5、TMA(トリメチルアルミニウム)、TBTDET(ターシャリーブチルイミド-トリ-ジエチルアミドタンタル)、PET(ペンタエトキシタンタル)、TMS(テトラメチルシラン)、TEH(テトラキスエトキシハフニウム)、Cp2Mn[=Mn(C5H5)2]、(MeCp)2Mn[=Mn(CH3C5H4)2]、(EtCp)2Mn[=Mn(C2H5C5H4)2]、(i-PrCp)2Mn[=Mn(C3H7C5H4)2]、MeCpMn(CO)3[=(CH3C5H4)Mn(CO)3]、(t-BuCp)2Mn[=Mn(C4H9C5H4)2]、CH3Mn(CO)5、Mn(DPM)3[=Mn(C11H19O2)3]、Mn(DMPD)(EtCp)[=Mn(C7H11C2H5C5H4)]、Mn(acac)2[=Mn(C5H7O2)2]、Mn(DPM)2[=Mn(C11H19O2)2]、Mn(acac)3[=Mn(C5H7O2)3]よりなる群から選択されるハロゲン元素を含まない1以上の材料よりなることを特徴とする請求項10記載の金属回収装置。
- 前記有機金属化合物はRu3(CO)12であり、前記除害ユニットから排出されるガスはCO2ガスであることを特徴とする請求項10記載の金属回収装置。
- 有機金属化合物の原料よりなる原料ガスを用いて被処理体の表面に薄膜を形成する処理容器に接続し、前記処理容器から排出される排気ガス中から金属成分を回収して排気ガスを除害する排気系であって、
前記処理容器の排気口に接続された排気通路と、
前記排気通路に介設された真空ポンプと、
前記排気通路に介設された請求項10記載の金属回収装置と、を備えたことを特徴とする排気系。 - 被処理体に対して成膜処理を施すための成膜装置において、
真空排気が可能になされた処理容器と、
前記処理容器内で前記被処理体を保持する保持機構と、
前記被処理体を加熱する加熱機構と、
前記処理容器内へガスを導入するガス導入機構と、
前記ガス導入機構に接続された原料ガスの供給系と、
前記処理容器に接続された請求項25に記載の排気系と、を備えたことを特徴とする成膜装置。
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