JP6376982B2 - Degassing method and film forming apparatus for raw material tank - Google Patents

Description

  The present invention relates to a material tank degassing method and a film forming apparatus.

  In a semiconductor device or the like, for example, a metal film or a metal compound film such as a metal oxide and a metal nitride is formed to form a thin film used for a conductor or an insulator. When forming a metal film or a metal compound film, for example, as described in Patent Document 1, a metal compound raw material is used as a metal precursor. Some metal compound raw materials are solid at room temperature, for example, in the form of powder. Such powder metal compound raw materials are accommodated in a raw material tank and attached to a processing gas supply source of a film forming apparatus. . The powdered metal compound raw material is vaporized, for example, by heating the raw material tank, and sent to the processing chamber of the film forming apparatus together with the carrier gas. A semiconductor wafer is accommodated as an object to be processed in the processing chamber, and a metal film or a metal compound film is formed on the semiconductor wafer by a gas containing a metal compound raw material sent into the processing chamber.

  When the metal compound raw material in the raw material tank becomes empty, as described in Patent Document 1, the raw material tank is removed and a new raw material tank containing the metal compound raw material is attached.

JP 2012-212854 A

  By the way, when a metal compound raw material having high reactivity with the atmosphere is accommodated in the raw material tank, it is recommended that an inert gas be enclosed in the tank to be at normal pressure or slightly pressurized during transportation. This is to prevent a sudden reaction with the atmosphere when an external leak occurs.

After attaching the raw material tank in the normal pressure or slightly pressurized state to the processing gas supply mechanism of the film forming apparatus,
(1) Leak check of material tank mounting part
(2) Cycle purge of gas piping
(3) The inert gas sealed in the raw material tank is degassed.

  However, if the inert gas is suddenly evacuated from the raw material tank, the solid powder, which is a metal compound, is scattered from the raw material tank, and the secondary pipe on the secondary side of the raw material tank is contaminated and treated. There is concern about the inflow of solid powder into the room.

  The present invention relates to a gas piping on the secondary side of a raw material tank, a degassing method for a raw material tank that can suppress the inflow of particles into a processing chamber, and the like, even if the raw material tank is degassed. Provided is a film forming apparatus capable of performing a method of venting a tank.

According to a first aspect of the present invention, there is provided a method for venting a raw material tank using the metal compound raw material of a film forming apparatus for forming a film containing a metal on a surface to be processed using a metal compound raw material. A method for venting a raw material tank when degassing a contained raw material tank, wherein the film forming apparatus includes a metal source gas supply source that supplies a metal source gas to a processing chamber of the film forming apparatus, and the metal The raw material tank that contains the metal compound raw material that can be attached to and detached from the raw material gas supply source, a carrier gas supply source that supplies a carrier gas to a gas introduction part of the raw material tank, and a gas in the raw material tank A gas pipe having a pipe opening / closing valve connected between the discharge section and the processing chamber, and an exhaust valve connected between the gas discharge section of the raw material tank and the pipe opening / closing valve; Tank or When degassing, (1) the raw material tank is closed with the metal raw material gas in a state in which all of the gas inlet side on-off valve and gas outlet side on-off valve, the pipe on-off valve and the exhaust valve of the raw material tank are closed. A step of attaching to the supply source; and (2) opening the exhaust valve with the gas inlet side on / off valve, the gas outlet side on / off valve, and the pipe on / off valve closed, A step of evacuating a portion from the gas discharge part side opening / closing valve to the pipe opening / closing valve; and (3) closing the gas introduction part side opening / closing valve, the gas discharge part side opening / closing valve, and the pipe opening / closing valve, respectively. And (4) opening the gas discharge side opening / closing valve with the gas inlet side opening / closing valve, the pipe opening / closing valve, and the exhaust valve closed, respectively. Present in the raw material tank And (5) the gas inlet side opening / closing valve, the pipe opening / closing, and a step of exhausting the sealed gas to the portion of the gas pipe from the gas discharge side opening / closing valve to the pipe opening / closing valve and the exhaust valve; And closing the gas exhaust side on-off valve again with the valve and the exhaust valve closed, and repeating the steps (2) to (5), Reduce the pressure step by step.

A film forming apparatus according to a second aspect of the present invention is a film forming apparatus for forming a film containing a metal on a surface to be processed using a metal compound raw material. A processing chamber for forming a film containing the metal on the processing surface, a metal source gas supply source for supplying a metal source gas to the processing chamber, and a metal source gas supply source And a detachable raw material tank for storing the metal compound raw material, a gas inlet side on-off valve and a gas outlet side on-off valve provided in the raw material tank, and a carrier gas in the gas inlet part of the raw material tank A carrier gas supply source to be supplied, a gas pipe connecting the gas discharge part of the raw material tank and the processing chamber, and having a pipe open / close valve in the middle, between the gas discharge part of the raw material tank and the pipe open / close valve An exhaust valve connected to the An apparatus, and a controller for controlling the gas inlet side on-off valve, the gas outlet side on-off valve, the piping on-off valve, and the exhaust valve, and when degassing the raw material tank, the controller The gas inlet side on / off valve, the gas discharge side on / off valve, the piping on / off valve, and the exhaust valve are controlled so as to execute the gas tank degassing method according to the second aspect.

  According to the present invention, a gas tank degassing method capable of suppressing gas pipes on the secondary side of the raw material tank, inflow of particles into the processing chamber, and the like even when the raw material tank is degassed, and It is possible to provide a film forming apparatus capable of performing the gas tank degassing method.

Sectional drawing which shows roughly an example of the film-forming apparatus which can implement the degassing method of the raw material tank which concerns on one Embodiment of this invention Sectional view showing raw material tank and gas piping in more detail The flowchart which shows an example of the sequence of the degassing method of the raw material tank which concerns on one Embodiment of this invention Sectional drawing which shows the state in the sequence shown in FIG. 3 roughly Sectional drawing which shows the state in the sequence shown in FIG. 3 roughly Sectional drawing which shows the state in the sequence shown in FIG. 3 roughly Sectional drawing which shows the state in the sequence shown in FIG. 3 roughly Sectional drawing which shows the state in the sequence shown in FIG. 3 roughly Diagram showing the relationship between time and pressure in the raw material tank (reference example) The figure which shows the relationship between time and the pressure in a raw material tank (one embodiment) The flowchart which shows an example of the sequence of the degassing method of the raw material tank which concerns on the modification of one Embodiment of this invention Sectional drawing which shows schematically the state in the sequence shown in FIG. The figure which shows the relationship between time and the pressure in the raw material tank (modification example)

  Hereinafter, an embodiment of the present invention will be described with reference to the drawings. Note that common parts are denoted by common reference numerals throughout the drawings.

<Deposition system>
First, an example of a film forming apparatus capable of carrying out the gas tank degassing method according to an embodiment of the present invention will be described.

  FIG. 1 is a cross-sectional view schematically showing an example of a film forming apparatus capable of carrying out a material tank degassing method according to an embodiment of the present invention. FIG. 1 shows a film forming apparatus for forming a metal oxide, for example, a hafnium oxide film, on an object surface of a semiconductor wafer as an object to be processed as an example of a film forming apparatus.

  As shown in FIG. 1, a film forming apparatus 100 has a double-layered structure including an inner tube 101 having a cylindrical shape with a ceiling at the lower end and an outer tube 102 disposed concentrically outside the inner tube 101. A cylindrical processing chamber 103 is provided. The inner tube 101 and the outer tube 102 are made of, for example, quartz. The lower end of the outer tube 102 constituting the processing chamber 103 is connected to a cylindrical manifold 104 made of, for example, stainless steel via a seal member 105 such as an O-ring. Similarly, the inner tube 101 constituting the processing chamber 103 is supported on a support ring 106 attached to the inner wall of the manifold 104.

  The lower end of the manifold 104 is opened, and the vertical wafer boat 107 is inserted into the inner tube 101 through the lower end opening. The vertical wafer boat 107 has a plurality of rods 108 in which a plurality of support grooves (not shown) are formed, and a plurality of, for example, 50 to 100 target objects are processed in the support grooves. In this example, a part of the peripheral edge of the wafer 1 is supported. As a result, the wafers 1 are placed on the vertical wafer boat 107 in multiple stages in the height direction.

  The vertical wafer boat 107 is placed on the table 110 via a quartz heat insulating cylinder 109. The table 110 is supported on a rotating shaft 112 that opens and closes a lower end opening of the manifold 104 and penetrates a lid portion 111 made of, for example, stainless steel. For example, a magnetic fluid seal 113 is provided in the penetrating portion of the rotating shaft 112 and supports the rotating shaft 112 so as to be rotatable while hermetically sealing. Between the peripheral part of the lid part 111 and the lower end part of the manifold 104, for example, a seal member 114 made of an O-ring is interposed. Thereby, the sealing property in the processing chamber 103 is maintained. The rotating shaft 112 is attached to the tip of an arm 115 supported by an elevating mechanism (not shown) such as a boat elevator, for example. As a result, the vertical wafer boat 107 and the lid portion 111 are moved up and down integrally and inserted into and removed from the inner tube 101 of the processing chamber 103.

  The film forming apparatus 100 includes a processing gas supply mechanism 120 that supplies a gas used for processing in an inner tube 101, and an inert gas supply mechanism 121 that supplies an inert gas in the inner tube 101. .

The processing gas supply mechanism 120 includes an oxidizing gas supply source 122a and a metal source gas supply source 122b. The oxidizing gas supply source 122 a supplies an oxidizing gas to the processing chamber 101, and the metal source gas supply source 122 b supplies a metal source gas to the processing chamber 101. The metal source gas supply source 122b of this example includes a source tank 123 and a heater 124 that heats the source tank 123. The raw material tank 123 is a tank that can be attached to and detached from the metal raw material gas supply source 122b, that is, a replaceable tank. In the raw material tank 123, for example, hafnium chloride (HfCl ₄ ) is accommodated as a metal compound raw material in this example. HfCl ₄ is solid at room temperature, for example, powder. Carrier gas is supplied into the raw material tank 123 from a carrier gas supply source 122 c through a flow rate controller (MFC) 126 c, a pipe on-off valve 127 c, and a gas introduction part 160 of the raw material tank 123. An example of the carrier gas is nitrogen (N ₂ ) gas.

  The oxidizing gas supply source 122a is connected to the dispersion nozzle 128a via a flow rate controller (MFC) 126a and a piping on-off valve 127a.

  In addition, the raw material tank 123 of the metal raw material gas supply source 122b is connected to the dispersion nozzle 128b via a pipe opening / closing valve 127b. One end of an exhaust valve 163 that exhausts the gas pipe 162 is connected to the gas pipe 162 between the gas discharge portion 161 of the raw material tank 123 and the pipe on-off valve 127b. The other end of the exhaust valve 163 is connected to an exhaust pipe, and the exhaust pipe is connected to an exhaust device 132 described later, for example.

The inert gas supply mechanism 121 includes an inert gas supply source 122d. An example of the inert gas is nitrogen (N ₂ ) gas. The inert gas is used for purging the inner pipe 101 and the like. The inert gas supply source 122d is connected to the nozzle 128d via a flow rate controller (MFC) 126d and an on-off valve 127d.

  Each of the distribution nozzles 128a and 128b is made of, for example, a quartz tube, penetrates the side wall of the manifold 104 inward, is bent in the height direction toward the inner tube 101 inside the manifold 104, and extends vertically. A plurality of gas discharge holes 129 are formed at predetermined intervals in the vertical portions of the dispersion nozzles 128a and 128b. Thereby, each gas is discharged from the gas discharge hole 129 in the horizontal direction toward the inside of the inner tube 101 substantially uniformly. The nozzle 128d penetrates the side wall of the manifold 104 and discharges an inert gas from the tip thereof in the horizontal direction.

  An exhaust port 130 for exhausting the inside of the inner tube 101 is provided in a side wall portion of the inner tube 101 that is located on the opposite side to the dispersion nozzles 128a and 128b. The inner pipe 101 communicates with the inside of the outer pipe 102 through the exhaust port 130. The inside of the outer tube 102 communicates with a gas outlet 131 provided on the side wall of the manifold 104, and an exhaust device 132 including a vacuum pump is connected to the gas outlet 131. The exhaust device 132 exhausts the inside of the outer tube 102 and the inside of the inner tube 101 through the exhaust port 130. As a result, the processing gas used for the processing is exhausted from the inner tube 101, or the pressure in the inner tube 101 is set to a processing pressure corresponding to the processing.

  A cylindrical heating device 133 is provided on the outer periphery of the outer tube 102. The heating device 133 activates the gas supplied into the inner tube 101 and heats the wafer 1 accommodated in the inner tube 101.

  Control of each part of the film forming apparatus 100 is performed by a process controller 150 including, for example, a microprocessor (computer). Connected to the process controller 150 is a user interface 151 including a touch panel on which an operator inputs commands to manage the film forming apparatus 100, a display that visualizes and displays the operating status of the film forming apparatus 100, and the like. ing.

  A storage unit 152 is connected to the process controller 150. The storage unit 152 causes a control program for realizing various processes executed by the film forming apparatus 100 under the control of the process controller 150 and causes each component of the film forming apparatus 100 to execute processes according to processing conditions. This program, that is, a recipe is stored. The recipe is stored in a storage medium in the storage unit 152, for example. The storage medium may be a hard disk or a semiconductor memory, or a portable medium such as a CD-ROM, DVD, or flash memory. Moreover, you may make it transmit a recipe suitably from another apparatus via a dedicated line, for example. The recipe is read from the storage unit 152 according to an instruction from the user interface 151 as necessary, and the process controller 150 executes processing according to the read recipe, whereby the film forming apparatus 100 is Under the control of the process controller 150, a metal oxide film, for example, a hafnium oxide film, is formed on the processing surface of the wafer 1.

  The raw material tank degassing method according to an embodiment of the present invention is performed, for example, on a film forming apparatus 100 as shown in FIG. Hereinafter, a method for venting a raw material tank according to an embodiment of the present invention will be described.

<Degassing method for raw material tank>
2 is a cross-sectional view showing the raw material tank and the gas pipe in more detail, FIG. 3 is a flowchart showing an example of the sequence of the raw material tank degassing method according to one embodiment of the present invention, and FIGS. 4A to 4E are FIG. It is sectional drawing which shows the state in the sequence shown schematically.

  A broken line frame A shown in FIG. 2 indicates a portion of the raw material tank 123 that can be attached to and detached from the metal raw material gas supply source 122b. A gas introduction pipe 201 is provided in the gas introduction section 160 of the raw material tank 123, and a gas introduction section side opening / closing valve 202 for opening and closing the gas introduction pipe 201 is provided in the middle of the gas introduction pipe 201. The gas introduction unit 160 is connected to the raw material tank 123 via an introduction pipe 201 and a gas introduction unit side opening / closing valve 202.

  The gas discharge part 161 of the raw material tank 123 has the same configuration, and the gas discharge part 161 is connected to the gas discharge pipe 204 and a gas discharge part side opening / closing valve 205 provided in the middle of the gas discharge pipe 204. It is connected to the raw material tank 123. A valve 206 that short-circuits the gas introduction unit 160 and the gas discharge unit 161 is a bypass valve.

  A heater 207 for heating the gas pipe 162 is provided around the gas pipe 162. The other points are the same as the configuration shown in FIG.

  When performing the degassing from such a raw material tank 123, it carries out as follows in this embodiment.

  First, as shown in Step 1 of FIG. 3 and FIG. 4A, the gas inlet side on-off valve 202, the gas outlet side on-off valve 205, the pipe on-off valve 127b, and the exhaust valve 163 are all closed. In this state, the raw material tank 123 is attached to the metal raw material gas supply source 122b.

  In addition, after attaching the raw material tank 123 to the metal raw material gas supply source 122b, a leak check may be performed on an attachment portion between the raw material tank 123 and the metal raw material gas supply source 122b.

  Next, as shown in Step 2 of FIG. 3 and FIG. 4B, the exhaust valve 163 is opened while the gas inlet side on-off valve 202, the gas outlet side on-off valve 205, and the pipe on-off valve 127b are closed. . Thereby, the part from the gas discharge part side on-off valve 205 to the pipe on-off valve 127b in the gas pipe 162 is exhausted.

  In addition, before performing step 2, you may make it heat the gas piping 162 previously using the heater 207. FIG. By heating the gas pipe 162, even if the metal compound raw material stored in the raw material tank 123 is mixed into the gas pipe 162, the mixed metal compound raw material is vaporized in the gas pipe 162. Can do. In order to obtain such advantages, the heating temperature of the gas pipe 162 using the heater 207 is preferably set to a temperature equal to or higher than the sublimation point of the metal compound raw material. In addition, after performing step 2, a cycle purge may be performed. As an example of the cycle purge, for example, the bypass valve 206 is opened and the carrier gas is supplied to the gas pipe 162. Next, after the bypass valve 206 is closed again, the exhaust valve 163 is opened and the gas pipe 162 is exhausted. Such an operation may be repeated.

  Next, as shown in Step 3 of FIG. 3 and FIG. 4C, the exhaust valve 163 is again turned on with the gas inlet side on / off valve 202, the gas outlet side on / off valve 205, and the pipe on / off valve 127b closed. close up.

  Next, as shown in Step 4 of FIG. 3 and FIG. 4D, the gas discharge side on-off valve 205 is opened while the gas introduction side on-off valve 202, the pipe on-off valve 127b, and the exhaust valve 163 are closed. . As a result, the sealed gas existing in the raw material tank 123 is exhausted to a portion of the gas pipe 162 from the gas discharge side open / close valve 205 to the pipe open / close valve 127b and the exhaust valve 163.

  Next, as shown in Step 5 of FIG. 3 and FIG. 4E, the gas exhaust side opening / closing valve 205 is again opened with the gas introduction side opening / closing valve 202, the piping on / off valve 127b, and the exhaust valve 163 closed. close up.

  Next, as shown in step 6 of FIG. 3, it is determined whether or not the number of execution times of the sequence from step 2 to step 5 is a set number. If it is determined that the set number has not been reached (No), the process returns to step 2 again, and the sequence from step 2 to step 5 is repeated. On the other hand, if it is determined that the set number of times has been reached (Yes), for example, the exhaust valve 163 is opened, and the portion from the gas discharge side opening / closing valve 205 to the piping opening / closing valve 127b of the gas pipe 162 is removed. After exhausting, the degassing of the raw material tank 123 is terminated.

  In this example, the set value is set in advance, and in step 6, it is determined whether or not the number of executions of the sequence from step 2 to step 5 has reached the set value. It is also possible to determine whether or not to repeat the sequence from step 2 to step 5 according to the pressure inside the tank 123. For example, when it is determined that the internal pressure of the raw material tank 123 has been reduced to a pressure at which dust rolling up is suppressed in the raw material tank 123, the degassing method of the raw material tank 123 may be terminated. .

  In this case, the internal pressure of the raw material tank 123 may be monitored directly from the internal pressure of the raw material tank 123, or the pressure in the pipe downstream from the exhaust valve 163 is monitored, The internal pressure may be known indirectly.

  However, when directly monitoring the internal pressure of the raw material tank 123, a pressure gauge must be attached to the raw material tank 123. However, when monitoring the pressure in the piping after the exhaust valve 163, There is no need to attach a pressure gauge to the tank 123. For this reason, the existing equipment can be used as it is, and in carrying out the degassing method according to the present embodiment, it is possible to obtain an advantage that an increase in cost due to the hardware configuration can be suppressed.

  5A and 5B are diagrams showing the relationship between time and pressure in the raw material tank. 5A shows a reference example, and FIG. 5B shows an example of one embodiment.

  As shown in FIG. 5A, when the inert gas sealed in the raw material tank 123 is extracted, conventionally, the raw material tank 123 is evacuated and the inert gas is extracted all at once. For this reason, the pressure in the raw material tank 123 falls at a stretch in a short time. However, since the raw material tank 123 is suddenly evacuated, the solid powder as the metal compound is scattered from the raw material tank 123, for example, dust is rolled up, and the gas pipe 162 on the secondary side of the raw material tank 123 is generated. , And inflow of the solid powder into the processing chamber 101 is a concern.

  In this regard, in the raw material tank degassing method according to one embodiment, as shown in FIG. 5B, the pressure in the raw material tank 123 is gradually reduced. This utilizes the volume of the gas pipe 162 connecting the raw material tank 123 and the processing chamber 101, and exhausts the sealed gas sealed in the raw material tank 123 into the gas pipe 162 by the volume of the gas pipe 162. This is because the process (step 4 in FIG. 3) is repeated. That is, the pressure in the raw material tank 123 can be decreased step by step in accordance with the volume of the gas pipe 162. In the present embodiment, the volume of the gas pipe 162 refers to the volume of the portion of the gas pipe 162 from the gas discharge side open / close valve 205 to the pipe open / close valve 127b (more strictly, from the gas pipe 162 to the exhaust valve 163). The volume of the pipe up to is also added).

  According to such a method for venting a raw material tank according to an embodiment, the pressure in the raw material tank 123 is gradually reduced by an amount corresponding to the volume of the gas pipe 162. Thereby, when degassing the raw material tank 123, it is possible to suppress a rapid pressure drop in the raw material tank 123. Therefore, scattering of solid powder, which is a metal compound, from the raw material tank 123 due to a rapid pressure drop, for example, dust dust, can be suppressed, the gas pipe 162 on the secondary side of the raw material tank 123, and processing A raw material tank degassing method capable of suppressing the inflow of solid powder into the chamber 101 and the film forming apparatus 100 capable of performing the degassing method of the raw material tank 123 can be obtained. .

  In such a degassing method according to an embodiment, the metal compound raw material stored in the raw material tank 123 is highly reactive with the atmosphere, and an inert gas is sealed in the raw material tank 123. Is particularly effective.

  Further, the contained metal compound raw material is particularly effective when it is accommodated in the raw material tank 123 in a solid state, particularly in a powder state.

<Modification>
Next, a modification of the gas tank degassing method according to an embodiment will be described.

  FIG. 6 is a flowchart showing an example of a sequence of a raw material tank degassing method according to a modification of the embodiment of the present invention, FIG. 7 is a sectional view schematically showing a state in the sequence shown in FIG. 6, and FIG. It is a figure which shows the relationship between time and the pressure in a raw material tank.

  In one embodiment described with reference to FIG. 3, after repeating steps 2 to 5, the degassing of the raw material tank 123 is completed. However, the filled gas remaining in the raw material tank 123 may be directly exhausted after the repetition of Step 2 to Step 5 is completed.

  Specifically, as shown in step 7 of FIG. 6 and FIG. 7, after it is determined in step 6 that the set number of times has been reached (Yes), the gas inlet side on-off valve 202 and the pipe on-off valve 127 b are closed. The gas discharge part side opening / closing valve 205 and the exhaust valve 163 are each opened with the state kept. Thereby, the raw material tank 123 is connected to the exhaust pipe, and the sealed gas remaining in the raw material tank 123 is exhausted to the exhaust pipe through the exhaust valve 163.

  In such a modification, the pressure in the raw material tank 123 rapidly decreases at the position of step 7 shown in FIG. However, even if the pressure in the raw material tank 123 suddenly decreases, for example, if the pressure in the raw material tank 123 is reduced to a pressure at which the dust in the raw material tank 123 is suppressed, any trouble is caused. Absent.

  In this way, after the pressure in the raw material tank 123 has been reduced to a pressure at which dust is prevented from rising in the raw material tank 123, the raw material tank 123 can be directly evacuated.

  According to such a modification, it is possible to further shorten the degassing sequence of the raw material tank 123 as compared with the embodiment. As a result, according to this modification, it is possible to reduce the time required for a series of steps from attaching and detaching the raw material tank 123 to degassing, reducing the stop time of the film forming apparatus 100, and The advantage that the throughput can be improved can be obtained.

  As mentioned above, although this invention was demonstrated by one Embodiment and the modification, this invention is not restricted to the said one Embodiment and a modification, It can implement in various deformation | transformation in the range which does not deviate from the meaning. Is possible.

For example, in the above embodiment, HfCl ₄ is exemplified as the metal compound raw material stored in the raw material tank 123, but examples of the metal compound raw material include the following in addition to HfCl ₄ .
AlCl ₃

  In the above embodiment, as the film forming apparatus for carrying out the present invention, the batch-type film forming apparatus 100 that loads a plurality of wafers 1 and performs film formation at once is exemplified. Not only the type but also a single-wafer type film forming apparatus that forms a film for each wafer 1 can be used.

  Further, the object to be processed is not limited to the wafer 1, and the present invention can be applied to other substrates such as an LCD glass substrate. In addition, the present invention can be variously modified without departing from the gist thereof.

DESCRIPTION OF SYMBOLS 1 ... Wafer, 100 ... Film-forming apparatus, 122b ... Metal raw material gas supply source, 122c ... Carrier gas supply source, 123 ... Raw material tank, 125 ... Metal compound raw material, 127b ... Pipe on-off valve, 160 ... Gas introduction part, 161 ... Gas exhaust part 162 ... Gas pipe, 163 ... Exhaust valve, 202 ... Gas introduction part side on-off valve, 205 ... Gas exhaust part side on-off valve

Claims (9)

Degassing method of a raw material tank when performing degassing from a raw material tank containing the metal compound raw material in a film forming apparatus for forming a film containing a metal on a surface to be processed of the object to be processed using the metal compound raw material Because
The film forming apparatus includes:
A metal source gas supply source for supplying a metal source gas to the processing chamber of the film forming apparatus;
The raw material tank for storing the metal compound raw material, which can be attached to and detached from the metal raw material gas supply source,
A carrier gas supply source for supplying a carrier gas to the gas introduction part of the raw material tank;
A gas pipe connecting the gas discharge part of the raw material tank and the processing chamber, and having a pipe on-off valve in the middle;
An exhaust valve connected between the gas discharge part of the raw material tank and the piping on-off valve;
When degassing from the raw material tank,
(1) A step of attaching the raw material tank to the metal raw material gas supply source in a state in which all of the gas inlet side on-off valve and the gas outlet side on-off valve, the pipe on-off valve and the exhaust valve of the raw material tank are closed. ,
(2) Open the exhaust valve while keeping the gas inlet side on / off valve, the gas outlet side on / off valve, and the pipe on / off valve closed, and the gas outlet side on / off of the gas pipe Exhausting a portion from the valve to the piping on-off valve;
(3) a step of closing the exhaust valve again with the gas inlet side opening / closing valve, the gas discharge side opening / closing valve, and the pipe opening / closing valve closed,
(4) With the gas inlet side on / off valve, the pipe on / off valve, and the exhaust valve closed, the gas outlet side on / off valve is opened, and the sealed gas present in the raw material tank is Exhausting the gas pipe from the gas discharge part side opening / closing valve to the pipe opening / closing valve and the exhaust valve;
(5) a step of closing the gas discharge side opening / closing valve again with the gas introduction side opening / closing valve, the pipe opening / closing valve, and the exhaust valve closed, and
With
A method for venting a raw material tank, wherein the pressure in the raw material tank is gradually reduced while repeating the steps (2) to (5). After repeating the steps (2) to (5) a set number of times or until the pressure in the raw material tank drops to a set pressure,
While the gas introduction part side opening / closing valve and the pipe opening / closing valve are closed, the gas discharge part side opening / closing valve and the exhaust valve are opened, and the sealed gas remaining in the raw material tank is supplied to the exhaust valve. degassing method of the raw material tank according to claim 1, characterized in that the exhaust in the exhaust pipe via the. The method of venting a raw material tank according to claim 1 or 2, wherein the raw material tank contains the metal compound raw material in a solid state .   The method for venting a raw material tank according to claim 3, wherein the solid state is powder. 5. The gas in the raw material tank according to claim 4 , wherein the number of repetitions is set to the number of times that the pressure in the raw material tank is reduced to a pressure at which dust rising is suppressed in the raw material tank. Unplugging method. The metal compound raw material reacts with the atmosphere ,
The method for venting a raw material tank according to any one of claims 1 to 5 , wherein an inert gas is enclosed in the raw material tank as an enclosed gas. Wherein (1) after the step, the raw material tank according to claims 1, characterized in that the leak check for the mounting portion and the metal raw material gas supply source and the raw material tank to one of claims 6 Degassing method. The material tank degassing method according to any one of claims 1 to 7 , wherein the gas pipe is heated before the step (2). A film forming apparatus for forming a film containing a metal on a surface to be processed using a metal compound raw material,
A processing chamber for performing a film forming process for forming a film containing the metal on a surface to be processed of the object to be processed;
A metal source gas supply source for supplying a metal source gas to the processing chamber;
A raw material tank for housing the metal compound raw material, which can be attached to and detached from the metal raw material gas supply source;
A gas inlet side on / off valve and a gas outlet side on / off valve provided in the raw material tank;
A carrier gas supply source for supplying a carrier gas to the gas introduction part of the raw material tank;
A gas pipe connecting the gas discharge part of the raw material tank and the processing chamber, and having a pipe on-off valve in the middle;
An exhaust valve connected between the gas discharge part of the raw material tank and the piping on-off valve;
The film forming apparatus, and the gas inlet on-off valve to perform a degassing process of the raw material tank, the gas discharge portion side valve, the pipe on-off valve, and the Turkey controller controls the exhaust valve, With
When performing degassing from the material tank, the controller, the film-forming apparatus according to claim according to any one of claims 1 to 8.

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