JP4652785B2 - Substrate processing equipment - Google Patents

Description

  The present invention relates to a substrate processing apparatus that performs processing such as thin film generation, impurity diffusion, and etching on a substrate such as a wafer, and more particularly, a substrate that uses a gas that may ignite or explode when mixed with oxygen as a source gas. The present invention relates to a processing apparatus.

  In processing in a substrate processing apparatus, various gases and liquids are used as raw materials for substrate processing, and some raw materials are toxic, ignitable, and explosive.

  When the source gas leaks, in the case of toxic gas, a supply cylinder or supply pipe is sealed with a valve and diluted with a safe gas. In addition, fire-extinguishing gas is extinguished by water or non-combustible gas such as CO2, extinguishing by extinguishing, or suppressing ignition, and explosive gas is sealed in an explosion-proof cabinet. Processing has been done.

  However, there are gases that ignite when leaked into the atmosphere and cannot be extinguished by substances containing oxygen, such as water and carbon dioxide (CO2), such as TMA (trimethylaluminum).

  In view of such circumstances, the present invention is a substrate processing apparatus using a raw material that is ignited when leaked into the atmosphere, such as TMA, and cannot be extinguished by a substance containing oxygen, such as water or carbon dioxide (CO2). In addition, the present invention provides a substrate processing apparatus that can safely store raw materials and can quickly extinguish when ignited.

  The present invention provides a substrate processing apparatus that supplies a raw material that ignites or explodes when mixed with oxygen into a processing chamber in which a substrate is stored, and performs a desired processing on the substrate, and includes a raw material tank that stores the raw material. A storage body that is hermetically stored; a gas supply unit that is connected to the storage body and constantly supplies an inert gas to the storage body; a detection unit that detects ignition or explosion in the storage body; and the inert gas And a control means for controlling the supply amount of the substrate. The control means relates to a substrate processing apparatus for increasing the supply amount of the inert gas when the detection means detects ignition or explosion.

  According to the present invention, there is provided a substrate processing apparatus for supplying a raw material that ignites or explodes when mixed with oxygen into a processing chamber in which a substrate is stored, and performs a desired process on the substrate, the raw material storing the raw material A storage body for airtightly storing the tank; a gas supply means connected to the storage body for constantly supplying an inert gas; a detection means for detecting ignition or explosion in the storage body; Control means for controlling the supply amount of the active gas, and the control means increases the supply amount of the inert gas when the detection means detects a fire or an explosion, so that the raw material tank is sealed in the container. Since the storage body is in an inert gas atmosphere, there is no risk of ignition even if gas leaks from the raw material tank, and even if it leaks and ignites or explodes, the increased amount of inert gas increases the storage body. So that Exhibits excellent effects such as can be carried out fire extinguishing.

  The best mode for carrying out the present invention will be described below with reference to the drawings.

  First, an overall outline of a substrate processing apparatus according to the present invention will be described with reference to FIG.

  As shown in FIG. 1, the substrate processing apparatus mainly includes a substrate processing apparatus main body 1 and a source gas, and a source gas storage unit 2 that supplies the source processing gas to the substrate processing apparatus main body 1.

  A space in which the substrate processing apparatus is stored is divided into an external transfer chamber 4 and an apparatus storage chamber 5 by a partition wall 3, and an external transfer device (not shown) is provided in the external transfer chamber 4. The cleanliness is maintained higher than that of the external transfer chamber 4. In the apparatus storage chamber 5, the substrate processing apparatus main body 1 and the source gas storage unit 2 are stored, and a front portion of the substrate processing apparatus main body 1, that is, a cassette stage 9 described later is exposed to the external transfer chamber 4. ing.

  The outline of the substrate processing apparatus main body 1 will be described with reference to FIG.

  A cassette stage 9 is provided on the front side of the inside of the housing 7 as a cassette transfer means for transferring a cassette 8 as a substrate storage container with an external transfer device (not shown). The cassette elevator 11 is provided so as to be capable of traversing, and the cassette elevator 11 is provided with a cassette carrying robot 12 that can be moved up and down. The cassette elevator 11 and the cassette transport robot 12 constitute a cassette transport means. A cassette shelf 13 as a means for placing the cassette 8 is provided on the rear side of the cassette elevator 11, and a spare cassette shelf 14 is also provided above the cassette stage 9. A clean unit 15 is provided above the spare cassette shelf 14, and the clean unit 15 is configured to circulate clean air inside the housing 7.

  A processing furnace 16 is provided above the rear portion of the casing 7, and a boat elevator 17 is provided as a lifting means below the processing furnace 16, and the boat elevator 17 lifts and lowers a boat 18 as a substrate holder. The boat 18 is loaded into and withdrawn from the processing furnace 16, and the boat 18 holds wafers 19 as substrates to be processed in a horizontal posture in multiple stages.

  A seal cap 22 serving as a lid is attached to the tip of the lift arm 21 attached to the boat elevator 17 to support the boat 18 vertically.

  A transfer elevator 23 is provided between the boat elevator 17 and the cassette shelf 13, and a wafer transfer machine 24 as a substrate transfer means is attached to the transfer elevator 23. Next to the boat elevator 17, there is provided a furnace port shutter 25 as a shielding member having an opening / closing mechanism and closing the furnace port of the processing furnace 16.

  The cassette 8 loaded with the wafer 19 is loaded into the cassette stage 9 from an external transfer device (not shown) in a vertical posture, and 90 ° on the cassette stage 9 so that the wafer 19 is in a horizontal posture. It is rotated. Further, the cassette 8 is transported from the cassette stage 9 to the cassette shelf 13 or the spare cassette shelf 14 by the cooperation of the raising / lowering operation, traversing operation of the cassette elevator 11, advance / retreat operation of the cassette transport robot 12, and rotation operation. Is done.

  The cassette shelf 13 has a transfer shelf 26 in which the cassette 8 to be transferred by the wafer transfer machine 24 is stored. The cassette 8 to be transferred is the cooperation of the cassette elevator 11 and the cassette transport robot 12. It is transferred to the transfer shelf 26 by operation.

  When the cassette 8 is transferred to the transfer shelf 26, the cassette 8 is lowered from the transfer shelf 26 by the cooperation of the advance / retreat operation, the rotation operation of the wafer transfer device 24, and the lifting / lowering operation of the transfer elevator 23. The wafer 19 is transferred to the boat 18.

  When a predetermined number of wafers 19 are transferred to the boat 18, the boat 18 is loaded into the processing furnace 16 by the boat elevator 17, and the processing furnace 16 is airtightly closed by the seal cap 22. In the processing furnace 16, the wafer 19 is heated and a raw material gas is supplied into the processing furnace 16 to process the wafer 19.

  When the processing on the wafer 19 is completed, the wafer 19 is transferred from the boat 18 to the cassette 8 of the transfer shelf 26 by the reverse procedure of the above-described operation, and the cassette 8 is transferred to the cassette elevator 11 and the cassette elevator 11. The cassette is transferred from the transfer shelf 26 to the cassette stage 9 by the cassette transfer robot 12 and is carried out of the casing 7 by an external transfer device (not shown). The furnace port shutter 25 closes the furnace port of the processing furnace 16 when the boat 18 is in the lowered state, and prevents outside air from entering the processing furnace 16.

  Transfer operations of the cassette elevator 11, the cassette transfer robot 12, the transfer elevator 23, the wafer transfer machine 24, and the like are controlled by a transfer control unit 27.

  Next, the source gas storage unit 2 will be described with reference to FIG.

  The source gas storage unit 2 is installed in the vicinity of the substrate processing apparatus main body 1.

  A housing 31 that is a raw material tank housing body of the raw material gas storage unit 2 has an airtight structure, and a receiving base 32 is provided inside the housing 31, and the raw material tank 30 is installed in the receiving base 32. . The raw material tank 30 stores a compressed raw material gas or a liquefied raw material gas, and the cradle 32 has a basin-like concave shape, and a leak detector 33 is provided at a required position inside the cradle 32. Is provided.

  A raw material gas distribution pipe 34 is connected to the raw material tank 30, the raw material gas distribution pipe 34 is connected to a gas supply / discharge section 35 of the substrate processing apparatus main body 1, and an open / close valve 40 is connected to the raw material gas distribution pipe 34. Is provided.

  A fire extinguishing gas supply line 36 serving as a fire extinguishing gas supply means is provided inside the casing 31, and a fire extinguishing gas supply pipe 37 of the fire extinguishing gas supply line 36 is opened at a required position inside the casing 31. The casing 31 is connected to an exhaust device (not shown) via an exhaust line 38, and the exhaust line 38 is provided with a flow rate adjusting valve, for example, a damper 39 for adjusting the exhaust flow rate.

  The fire extinguishing gas supply line 36 communicates with a fire extinguishing gas source (not shown) outside the housing 31 via a regulator (pressure regulator) 41. The fire extinguishing gas source supplies a gas that does not react with the raw material gas, for example, an inert gas such as nitrogen gas.

  The fire extinguishing gas supply pipe 37 is provided with a gas flow meter 42 and a main opening / closing valve 43, and a bypass pipe 44 communicating with the upstream side of the gas flow meter 42 and the downstream side of the main opening / closing valve 43 is provided. The tube 44 is provided with a sub open / close valve 45.

  A gas leak detector 46, an infrared sensor 47, a smoke detector 48, a temperature sensor 49, and a pressure gauge 51 are provided at appropriate positions inside the casing 31, for example, on the ceiling surface of the casing 31. The detection results of the leak detector 33, the gas leak detector 46, the infrared sensor 47, the smoke detector 48, the temperature sensor 49, and the pressure gauge 51 are sent to the source gas storage control unit 52, and the source gas storage control is performed. The unit 52 controls the regulator 41 and the gas flow meter 42 based on the detection result, or controls the opening and closing of the main on-off valve 43 and the auxiliary on-off valve 45.

  The fire-extinguishing gas supply line 36 is only required to have the fire-extinguishing gas supply pipe 37 open to the housing 31, and the gas flow meter 42, the main on-off valve 43, the bypass pipe 44, and the auxiliary on-off valve 45. Etc. may be provided outside the casing 31. Further, the ignition and explosion detection means of the leak detector 33 and the gas leak detector 46, the infrared sensor 47, the smoke detector 48, the temperature sensor 49, etc. are appropriately selected according to the type of gas to be detected. It is sufficient that at least one is provided.

  In the steady state, the main on-off valve 43 is opened, the inert gas is constantly supplied from the fire extinguishing gas supply line 36, the supply amount is adjusted by the regulator 41 and the gas flow meter 42, and the The pressure inside the casing 31 is adjusted by adjusting the exhaust amount of the damper 39, and the pressure detected by the pressure gauge 51 is adjusted to be 1 kPa or less, that is, a negative pressure as a gauge pressure.

  Therefore, the inside of the casing 31 is a reduced pressure atmosphere in which the source gas is in a non-reactive state, and even if the source gas leaks, the ignition and explosion are suppressed, and the leaked gas is prevented by setting the reduced pressure atmosphere. The casing 31 does not leak outside.

  When the raw material gas leaks, ignites or explodes, the gas leak detector 46 detects the gas leak, the infrared sensor 47 detects the infrared rays emitted from the flame, and the smoke detector 48 detects the smoke at the time of ignition. The temperature sensor 49 detects an increase in temperature due to ignition, detects that an ignition or explosion has occurred, and the detection result is sent to the source gas storage control unit 52. The source gas storage control unit 52 ignites or explodes when a detection signal is sent from at least one of the gas leak detector 46, the infrared sensor 47, the smoke detector 48, and the temperature sensor 49. A buzzer is sounded, a warning light is turned on to notify the occurrence of ignition or explosion, and the auxiliary on-off valve 45 and the damper 39 are fully opened to supply a large amount of inert gas to extinguish the fire. .

  The casing 31 has a hermetically sealed structure, and by filling the casing 31 with a large amount of inert gas, it is possible to quickly extinguish the fire and prevent it from spreading outside the casing 31.

  Next, a substrate processing apparatus for forming an Al2 O3 film by an ALD (Atomic Layer Deposition) method using a source gas, for example, TMA, which is an object of the present invention will be described.

  As a substrate processing apparatus for forming such an Al2 O3 film, there has been proposed a vertical batch type apparatus for forming a film while holding a plurality of substrates in multiple layers.

  4 is a schematic longitudinal sectional view of the vertical substrate processing furnace 55 of the substrate processing apparatus, FIG. 5 is a schematic longitudinal sectional view of the vertical substrate processing furnace 55, and FIG. 6 is the vertical substrate processing furnace 55. 7 is an explanatory view of a merging type gas supply nozzle of the vertical substrate processing furnace 55, FIG. 7 (A) is a schematic view, and FIG. 7 (B) is FIG. 7 (A). 8) is a partially enlarged view of part A, FIG. 8 is an explanatory view of a separation type gas supply nozzle, FIG. 8 (A) is a schematic view, and FIG. 8 (B) is B in FIG. 8 (A). It is the elements on larger scale of a part.

  A reaction tube 57 is provided inside the heater 56 as a heating means as a reaction vessel for processing the wafer 19 as a substrate to be processed. A manifold 58 made of, for example, stainless steel is concentrically formed at the lower end of the reaction tube 57. Further, it is airtightly provided through a seal member 59, for example, an O-ring. The lower end opening of the manifold 58 is hermetically closed by, for example, an O-ring 61 by a seal cap 22 that is a lid, and the heater 56, the reaction tube 57, the manifold 58, and the seal cap 22 are sealed. Thus, the vertical substrate processing furnace 55 is formed, and the processing chamber 62 is defined by the reaction tube 57, the manifold 58, and the seal cap 22. The reaction tube 57 is supported by the heater base 63 through the manifold 58.

  A boat 18 as a substrate holder is erected on the seal cap 22 via a quartz cap 64, and the quartz cap 64 serves as a holding body of the boat 18. The boat 18 holds a plurality of batch-processed wafers 19 in a horizontal posture in multiple stages in the axial direction. The heater 56 heats the wafer 19 loaded in the reaction tube 57 to a predetermined temperature.

  Three gas supply pipes 65, 66, and 67 for supplying a plurality of types of gas, here three types of gas, are provided to the reaction tube 57. The gas supply pipes 65, 66, and 67 are provided so as to penetrate the lower portion of the manifold 58 in an airtight manner, and the gas supply pipe 65 and the gas supply pipe 66 are formed in a single hole in the reaction tube 57. A merged gas supply nozzle 69 described later is formed by the two gas supply pipes 65, 66 and the multi-hole nozzle 68. The gas supply pipe 67 communicates with another porous nozzle 71 independently, and the single gas supply pipe 67 and the porous nozzle 71 form a separation type gas supply nozzle 72 described later. In the reaction tube 57, two gas supply nozzles, that is, the merge type gas supply nozzle 69 and the separation type gas supply nozzle 72 are provided.

  The upper part of the merging type gas supply nozzle 69 extends in a region above the decomposition temperature of TMA supplied from the gas supply pipe 66 in the reaction pipe 57. Further, the portion of the gas supply pipe 66 that joins the gas supply pipe 65 in the reaction pipe 57 is an area below the decomposition temperature of TMA, which is higher than the temperature of the wafer 19 and the vicinity of the wafer 19. It is a low temperature region.

  Here, from the first gas supply pipe 65, the reaction pipe 57 is passed through the merging type gas supply nozzle 69 through the first mass flow controller 73 which is a flow rate control means and the first valve 74 which is an on-off valve. The second gas supply pipe 66 is supplied with a second mass flow controller 75 which is a flow rate control means, a second valve 76 which is an on-off valve, a TMA container 30, and an on-off valve. A reaction gas (TMA) is supplied to the reaction tube 57 through a third valve 77 and the combined gas supply nozzle 69. A heater 78 is provided in the gas supply pipe 66 from the TMA container 30 to the manifold 58, and the gas supply pipe 66 is maintained at 50 to 60 ° C.

  From the third gas supply pipe 67, the third mass flow controller 79 which is a flow control means, a fifth valve 81 which is an on-off valve, a TEMAH container 82, and a sixth valve 91 which is an on-off valve, A reaction gas (tetrakis (N-ethyl-N-methylamino) hafnium: TEMAH) is supplied to the reaction tube 57 through the separation type gas supply nozzle 72. A heater 83 is provided in the gas supply pipe 67 from the TEMAH container 82 to the manifold 58, and the gas supply pipe 67 is maintained at 130 ° C.

  An inert gas line 84 for supplying an inert gas such as nitrogen gas is connected to the gas supply pipe 66 on the downstream side of the third valve 77 through an open / close valve 85. In addition, an inert gas line 86 is connected to the gas supply pipe 65 on the downstream side of the first valve 74 via an open / close valve 87. An inert gas line 88 that supplies an inert gas such as nitrogen gas is connected to the gas supply pipe 67 on the downstream side of the sixth valve 91 via an open / close valve 89.

  The reaction tube 57 is connected to a vacuum pump 94, which is an exhaust means, through a fourth valve 93 by a gas exhaust tube 92, and is evacuated. The fourth valve 93 is a pressure adjusting valve that can open and close the valve to stop evacuation and evacuation in the reaction tube 57, and further adjust the valve opening to adjust the pressure.

  The confluence type gas supply nozzle 69 and the separation type gas supply nozzle 72 extend from the lower part of the reaction tube 57 to the upper part along the holding direction of the wafer 19. The multi-hole nozzle 68 of the merging type gas supply nozzle 69 is provided with gas supply holes 95 which are supply holes for supplying a plurality of gases, and the gas is also supplied to the multi-hole nozzle 71 of the separation type gas supply nozzle 72. A gas supply hole 96 is provided as a supply hole.

  A boat 18 holding a predetermined number of wafers 19 is supported by a boat elevator 17 (see FIG. 2) through the quartz cap 64 in the center of the reaction tube 57, and the boat 18 is supported by the boat elevator 17. The reaction tube 57 is charged and withdrawn. Further, in order to improve the uniformity of processing, a boat rotating mechanism 97 that is a rotating means for rotating the boat 18 is provided in the lift arm 21 so that the boat 18 is rotated by the boat rotating mechanism 97. It has become.

  The controller 98 which is a control means includes the first, second and third mass flow controllers 73, 75, 79, first to sixth valves 74, 76, 77, 93, 81, 91, and open / close valves 85, 87. 89, heater 56, vacuum pump 94, boat rotation mechanism 97, and boat elevator 17 are connected to the first, second, and third mass flow controllers 73, 75, and 79, and the first, second, 2, opening and closing operation of the third valve 74, 76, 77, fifth and sixth valves 81, 91, opening and closing valves 85, 87, 89, opening and closing of the fourth valve 93 and pressure adjusting operation, the heater 56 Are adjusted, the vacuum pump 94 is started and stopped, the rotation speed of the boat rotating mechanism 97 is adjusted, and the lifting operation of the boat elevator 17 is controlled.

  Next, a case where an Al2 O3 film is formed using TMA and O3 gas and a case where an HfO2 film is formed using TEMAH and O3 gas will be described.

  First, a procedure for forming an Al2 O3 film will be described.

  A wafer 19 to be deposited is loaded into the boat 18 and loaded into the reaction tube 57. After charging, the following three steps are executed sequentially.

[Step 1]
In step 1, O3 gas is flowed. First, both the first valve 74 and the fourth valve 93 are opened, and the O 3 gas whose flow rate is adjusted by the first mass flow controller 73 from the gas supply pipe 65 is supplied to the gas of the merging type gas supply nozzle 69. The gas exhaust pipe 92 is exhausted while being supplied to the reaction pipe 57 from the supply hole 95. When the O3 gas is allowed to flow, the pressure in the reaction tube 57 is adjusted to 10 to 100 Pa by adjusting the fourth valve 93 appropriately. The supply flow rate of O3 gas controlled by the first mass flow controller 73 is 1000 to 10000 sccm. The time for exposing the wafer 19 to O3 gas is 2 to 120 seconds. The temperature of the heater 56 at this time is set so that the temperature of the wafer 19 is 77 to 450 ° C.

  At the same time, the on-off valves 85 and 89 are opened from the inert gas line 84 connected in the middle of the gas supply pipe 66 and the inert gas line 88 connected in the middle of the gas supply pipe 67 to be inactive. By flowing the gas, it is possible to prevent the O3 gas from flowing into the TMA side and the TEMAH side.

  At this time, the gases flowing in the reaction tube 57 are only inert gases such as O3, N2 and Ar, and TMA and TEMAH do not exist. Therefore, O3 does not cause a gas phase reaction, but reacts with the underlying film on the wafer 19.

[Step 2]
In step 2, the first valve 74 is closed to stop the supply of O3 gas. Further, the fourth valve 93 is kept open, and the reaction tube 57 is evacuated to 20 Pa or less by the vacuum pump 94 to remove residual O3 gas from the reaction tube 57. At this time, if an inert gas such as N2 is supplied from the gas supply pipe 65, the gas supply pipe 66, and the gas supply pipe 67 to the reaction pipe 57, the effect of eliminating residual O3 gas is further enhanced.

[Step 3]
In step 3, TMA gas is flowed. TMA is a liquid at normal temperature, and in order to supply it to the reaction tube 57, a method of supplying it after heating and vaporizing, an inert gas such as nitrogen or a rare gas called a carrier gas is introduced into the TMA container 30. There is a method of supplying the vaporized component together with the carrier gas to the reaction tube 57, and the latter case will be described as an example.

  The second valve 76, the third valve 77, and the fourth valve 93 are both opened, and the carrier gas whose flow rate is adjusted by the second mass flow controller 75 from the gas supply pipe 66 is the TMA container 30. The gas exhaust pipe 92 is exhausted while being supplied from the gas supply hole 95 of the merged type gas supply nozzle 69 to the reaction pipe 57 as a mixed gas of TMA and carrier gas.

  When flowing TMA gas, the pressure in the reaction tube 57 is adjusted to 10 to 900 Pa by adjusting the fourth valve 93 appropriately. The supply flow rate of the carrier gas controlled by the second mass flow controller 75 is 10,000 sccm or less. The time for supplying the TMA gas is set to 1 to 4 seconds. Thereafter, the time for exposure to the increased pressure atmosphere for adsorption onto the wafer 19 may be set to 0 to 4 seconds. At this time, the temperature of the wafer 19 is 77 to 450 ° C. as in the case of supplying the O 3 gas. By supplying the TMA gas, O3 and TMA on the base film react with each other to form an Al2 O3 film on the wafer 19.

  At the same time, if the inert gas is flowed from the inert gas line 86 and the inert gas line 88 by opening the on-off valves 87 and 89, it is possible to prevent the TMA gas from flowing into the O3 side and the TEMAH side. it can.

  After the film formation, the third valve 77 is closed, the fourth valve 93 is opened, and the reaction tube 57 is evacuated to exhaust the residual gas after contributing to the remaining TMA film formation. At this time, an inert gas such as N2 is supplied from the inert gas lines 86, 84, 88 to the reaction tube 57 through the gas supply pipe 65, the gas supply pipe 66, and the gas supply pipe 67, respectively. When supplied, the effect of eliminating residual gas after contributing to the film formation of TMA is further enhanced.

  Steps 1 to 3 are defined as one cycle, and this cycle is repeated a plurality of times to form an Al2 O3 film having a predetermined thickness on the wafer 19.

  In [Step 2], the inside of the reaction tube 57 is evacuated to remove the O3 gas and then the TMA gas is flown, so that they do not react on the way to the wafer 19. The supplied TMA gas can effectively react only with O3 adsorbed on the wafer 19.

  Next, the procedure for forming the HfO2 film will be described.

[Step 4]
In step 4, O3 gas is flowed in the same manner as the formation of the Al2 O3 film. First, both the first valve 74 and the fourth valve 93 are opened, and the O3 gas whose flow rate is adjusted by the first mass flow controller 73 from the gas supply pipe 65 is supplied to the gas supply hole of the merge type gas supply nozzle 69. The gas exhaust pipe 92 is exhausted while being supplied from 95 to the reaction pipe 57.

  When flowing O3 gas, the pressure in the reaction tube 57 is adjusted to 10 to 100 Pa by adjusting the fourth valve 93 appropriately. The supply flow rate of O3 gas controlled by the first mass flow controller 73 is 1000 to 10000 sccm. The time for exposing the wafer 19 to O3 gas is 2 to 120 seconds. The temperature of the heater 56 at this time is set so that the temperature of the wafer 19 is 77 to 450 ° C.

  At the same time, when the opening and closing valves 89 and 85 are opened from the inert gas line 88 and the inert gas line 84 to allow the inert gas to flow, O3 gas is prevented from flowing into the TEMAH side and the TMA side. it can.

  At this time, the gases flowing in the reaction tube 57 are only inert gases such as O3, N2, and Ar, and there is no TEMAH or TMA. Therefore, O3 does not cause a gas phase reaction, but reacts with the underlying film on the wafer 19.

[Step 5]
In step 5, the first valve 74 is closed to stop the supply of O3 gas. Further, the fourth valve 93 is kept open, and the reaction tube 57 is evacuated to 20 Pa or less by the vacuum pump 94, and residual O3 gas is removed from the reaction tube 57. At this time, an inert gas such as N2 is supplied from the inert gas lines 86, 84, 88 to the reaction tube 57 through the gas supply pipe 65, the gas supply pipe 66, and the gas supply pipe 67, respectively. Then, the effect of eliminating residual O3 gas is further enhanced.

[Step 6]
In step 6, TEMAH gas is flowed. Since TEMAH is a liquid at room temperature like TMA, there are a method of supplying the reaction tube 57 after heating and vaporizing, and a method of supplying the reaction tube 57 together with a carrier gas.

  FIG. 9 shows a configuration in which an inert gas such as nitrogen or a rare gas called a carrier gas is passed through the TEMAH vessel 82 and the vaporized portion is supplied to the reaction tube 57 together with the carrier gas. However, a method for supplying TEMAH will be described using the vaporizer unit 100 shown in FIG. As an example, a description will be given of a method in which the vaporizer unit 100 is used to heat and vaporize TEMAH and supply it to the reaction tube 57 together with a carrier gas.

  First, the valve 102 and the valve 103 provided in the carrier gas supply pipe 101 are opened, and the flow rate is adjusted by the mass flow controller 104.

  Next, the valve 106, the valve 107 and the valve 108 provided in the TEMAH supply pipe 105 are opened, and the flow rate is adjusted by the liquid flow meter 109 and the control valve 111 in the vaporizer unit 100. Next, when introducing into the reaction tube 57, the valve 112 is closed, the valve 103 is opened, and a mixed gas of TEMAH gas and carrier gas is supplied from the separation type gas supply nozzle 72.

  When flowing the TEMAH gas, the mass flow controller 104 is adjusted appropriately, the flow rate is further adjusted by the liquid flow meter 109 and the control valve 111 in the vaporizer unit 100, and the internal pressure of the reaction tube 57 is set to 10 to 100 Pa. And The supply amounts of the mass flow controller 104 and the liquid flow meter 109 are 100 to 1000 sccm and 0.01 to 0.2 g / min, respectively. The time for supplying the TEMAH gas may be set to 1 to 600 seconds. At this time, the temperature of the wafer 19 is 150 to 78 [deg.] C. as in the case of supplying the O3 gas. By supplying the TEMAH gas, O3 and TEMAH on the base film react with each other to form an HfO2 film on the wafer 19.

  At the same time, when the inert gas is flowed from the inert gas line 86 and the inert gas line 84 by opening the on-off valves 87 and 85, it is possible to prevent the TEMAH gas from flowing into the O3 side and the TMA side. it can.

  After film formation, the valve 91 is closed, the fourth valve 93 is opened, the reaction tube 57 is evacuated, and the residual gas after contributing to the film formation of the remaining TEMAH is exhausted. Further, when an inert gas such as N2 is supplied from the inert gas lines 86, 84, 88 to the gas supply pipe 65, the gas supply pipe 66, and the gas supply pipe 67, respectively, the reaction pipe 57 is further supplied. The effect of removing the residual gas after contributing to the film formation from the reaction tube 57 is enhanced.

  The above steps 4 to 6 are defined as one cycle, and a HfO2 film having a predetermined thickness is formed on the wafer 19 by repeating this cycle a plurality of times.

  In [Step 5], the inside of the reaction tube 57 is evacuated to remove the O3 gas, and then the TEMAH gas is flown, so that they do not react on the way to the wafer 19. The supplied TEMAH can effectively react only with O3 adsorbed on the wafer 19.

  As described above, when the Al2 O3 film is formed, the gas supply pipe 65 and the gas supply pipe 66 are merged in the reaction tube 57, whereby TMA and O3 are combined in the merge type gas supply nozzle 69. However, by alternately adsorbing and reacting, the deposited film can be made of Al2 O3, and when TMA and O3 are supplied by separate nozzles, an Al film that can become a foreign matter generation source is generated in the TMA nozzle. The problem can be eliminated. Since the Al2 O3 film has better adhesion than the Al film and is difficult to peel off, it is unlikely to become a source of foreign matter.

  When the HfO2 film is formed, the gas supply pipe 65 and the gas supply pipe 66 merge in the reaction pipe 57 and communicate with the single porous nozzle 68. Supplying O3 gas and supplying the TEMAH gas from the separation type gas supply nozzle 72 in which the gas supply pipe 67 alone communicates with the single porous nozzle 71, so that the combined type gas is supplied when the TEMAH gas is supplied. Inert gas purging to prevent backflow and entry required when using a nozzle can be avoided, and a rise in pressure in the nozzle due to purging, which becomes a problem when using a merged type gas nozzle with TEMAH gas supply, can be eliminated. it can. In addition, generation of particles due to reliquefaction of TEMAH accompanying the increase in pressure can be prevented.

  In this embodiment, the Al2 O3 film and the HfO2 film are formed in the same processing chamber. However, in the processing chamber for the purpose of forming only the HfO2 film, the TEMAH gas is supplied. It is possible to form a film with a configuration of two types, a type gas supply nozzle and a separation type gas supply nozzle that supplies O3 gas.

It is a whole explanatory view showing an embodiment of the invention. 1 is a perspective view showing a substrate processing apparatus according to an embodiment of the present invention. It is a schematic explanatory drawing which shows the principal part of embodiment of this invention. It is a schematic longitudinal cross-sectional view of the vertical substrate processing furnace of the substrate processing apparatus which concerns on embodiment of this invention. It is a schematic longitudinal cross-sectional view of the vertical substrate processing furnace of the substrate processing apparatus which concerns on embodiment of this invention. 1 is a schematic cross-sectional view of a vertical substrate processing furnace of a substrate processing apparatus according to an embodiment of the present invention. 7A and 7B are explanatory views of a merging type gas supply nozzle of the vertical substrate processing furnace, in which FIG. 7A is a schematic view and FIG. 7B is a partially enlarged view of a portion A in FIG. 7A. It is explanatory drawing of the separation type gas supply nozzle of the said vertical substrate processing furnace, FIG. 8 (A) is a schematic diagram, FIG.8 (B) is the elements on larger scale of the B section of FIG. 8 (A). . It is explanatory drawing which shows the supply method of the TEMAH gas to the vertical substrate processing furnace which concerns on embodiment of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Substrate processing apparatus main body 2 Raw material gas storage part 30 Raw material tank 31 Case 32 Receptacle 33 Leak detector 36 Fire extinguishing gas supply line 37 Fire extinguishing gas supply pipe 39 Damper 42 Gas flow meter 43 Main on-off valve 45 Sub on-off valve 46 Gas Leakage detector 47 Infrared sensor 48 Smoke detector 49 Temperature sensor 51 Pressure gauge 52 Source gas storage controller

Claims (1)

A substrate processing apparatus that supplies a raw material that ignites or explodes when mixed with oxygen into a processing chamber in which a substrate is stored, and performs a desired processing on the substrate, and stores a raw material tank that stores the raw material in an airtight manner. A storage body, a gas supply means connected to the storage body and constantly supplying an inert gas to the storage body, a detection means for detecting ignition or explosion in the storage body, and a supply amount of the inert gas. Control means for controlling,
The gas supply means has a first on-off valve, and in a steady state, the first on-off valve is opened, and a first gas supply line that constantly supplies the inert gas to the storage body;
A second gas supply line having a second on-off valve , wherein when the detection means detects an ignition or explosion, the control means opens the second on-off valve and supplies an inert gas to the housing body; the substrate processing apparatus according to claim Rukoto to Yusuke.

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