JP2011208193A - Cleaning method for vacuum suction pipe - Google Patents

Abstract

The present invention relates to a cleaning method of a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure, and relates to a cleaning method that satisfactorily cleans an intake pipe that sucks gas from a processing chamber by a vacuum pump. .
An opening / closing valve 9 is provided in the vicinity of a connection port 6b with a vacuum pump 4 in an intake pipe 6 connected to a processing chamber 1, and in the vicinity of the connection port 6a with the processing chamber 1 in the intake pipe 6. By closing the device gate valve 7 provided, adjusting the opening of the on-off valve 9, supplying a specific cleaning gas made of chlorine trifluoride or the like to the intake pipe 6, and operating the vacuum pump 4 When the inside of the intake pipe 6 is kept at a predetermined pressure for cleaning, the deposited film adhering to the intake pipe 6 during the film forming process or the crystal growth process is removed well, and the apparatus is repaired or disassembled. In addition, disasters caused by harmful and dangerous deposited films were prevented.
[Selection] Figure 5

Description

  The present invention relates to a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure, and relates to a suction pipe for sucking gas by a vacuum pump from a processing chamber for film formation or crystal growth that can be reduced in pressure. Cleaning the inside of the intake pipe by cleaning the inside of the intake pipe or the inside of the intake pipe and the processing chamber by setting the pressure of the cleaning gas in the pipe and the processing chamber to a pressure suitable for cleaning. This is a technique related to a cleaning method that reduces the time required for cleaning and reduces the consumption of cleaning gas.

Conventionally, various methods have been proposed for cleaning a film forming apparatus or a crystal growing apparatus that perform processing under reduced pressure, and the pressure of the cleaning gas in the processing chamber is set higher than that during processing such as film forming, so that the processing chamber It is known to increase the etching rate (cleaning rate) in the processing chamber by cleaning (see, for example, Patent Document 1 and Patent Document 2).
Conventionally, it is also known to perform cleaning while maintaining the pressure of the cleaning gas in the processing chamber at a predetermined value suitable for cleaning (see, for example, Patent Document 3).

JP 2002-151497 A JP 2002-231712-A JP 2001-81545 A

The conventional techniques described in Patent Literature 1 to Patent Literature 3 are excellent in cleaning the processing chamber by setting the cleaning gas pressure higher than that at the time of film formation or a predetermined value. Thus, the time required for cleaning is shortened and the consumption of the cleaning gas can be reduced.
However, an intake pipe for sucking gas from the processing chamber by a vacuum pump is connected to the processing chamber, and the pressure of the cleaning gas in the processing chamber is controlled by a pressure control valve provided in the vicinity of the connection port with the processing chamber in the intake pipe. Therefore, the opening of the pressure control valve is reduced during cleaning, and the pressure of the cleaning gas in the intake pipe between the pressure control valve and the vacuum pump is lower than the pressure of the cleaning gas in the processing chamber, that is, high It becomes a vacuum state.

Therefore, in the conventional cleaning method, the pressure of the cleaning gas in the intake pipe is lower than the optimum value, and it takes a long time to clean the inside of the intake pipe. There is a problem that the time for performing the treatment is shortened and the productivity of the film forming apparatus or the crystal growing apparatus is lowered.
In addition, as the time required for cleaning is long, there is a problem that the consumption of gas required for cleaning is large.

In the conventional cleaning method, it is conceivable that the pressure in the intake pipe is set to the same pressure as in the processing chamber by providing the pressure control valve in the vicinity of the connection port with the vacuum pump in the intake pipe.
However, in this case, due to restrictions on the installation of the processing chamber and the vacuum pump, the length of the intake pipe is 4 m to 20 m and the pipe diameter is 40 mm to 250 mm. Alternatively, the pressure control valve is provided in the vicinity of the connection port with the processing chamber in the intake pipe because the gas for crystal growth is required and the responsiveness of the pressure control valve that requires high-speed and high-precision control deteriorates. It is done.

  The present invention is intended to solve the problems of such a conventional film forming apparatus or crystal growth apparatus cleaning method, and a vacuum pump is formed from a process chamber for film formation or crystal growth that can be decompressed. Cleaning the inside of the intake pipe or the intake pipe and the processing chamber by setting the pressure of the cleaning gas in the intake pipe for sucking the gas or the pressure in the intake pipe and the processing chamber to a pressure suitable for cleaning. Accordingly, an object of the present invention is to provide a cleaning method in which the time required for cleaning is shortened and the consumption of the cleaning gas is reduced.

According to a first aspect of the present invention, there is provided a film forming apparatus or a crystal growth apparatus cleaning method for performing a process under reduced pressure, wherein a film forming or crystal growth gas is provided in a process chamber for film formation or crystal growth capable of reducing pressure. And a suction pipe for sucking gas from the processing chamber by a vacuum pump, and a pressure control valve is provided in the vicinity of the connection port of the suction pipe with the processing chamber. A film-forming apparatus or a crystal growth apparatus cleaning method for performing processing under reduced pressure with the vacuum pump connected to an end side,
An opening / closing valve whose opening degree can be adjusted is provided near the connection port with the vacuum pump in the intake pipe, the pressure control valve is fully opened, and the opening degree of the opening / closing valve is adjusted,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride in the treatment chamber An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas,
By operating the vacuum pump, the processing chamber and the intake pipe are maintained at a pressure of 0.5 kPa to 80 kPa for cleaning.

According to a second aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, wherein a film deposition or crystal growth gas is provided in a process chamber for film deposition or crystal growth that can be decompressed. And a suction pipe for sucking gas from the processing chamber by a vacuum pump, and a pressure control valve is provided in the vicinity of the connection port of the suction pipe with the processing chamber. A film-forming apparatus or a crystal growth apparatus cleaning method for performing processing under reduced pressure with the vacuum pump connected to an end side,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride in the treatment chamber An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas,
Fully open the pressure control valve and adjust the number of rotations of the vacuum pump that can adjust the number of rotations, so that the processing chamber and the intake pipe are maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. It is what I did.

According to a third aspect of the present invention, there is provided a film forming apparatus or crystal growth apparatus cleaning method for performing processing under reduced pressure, wherein a film forming or crystal growth gas is provided in a film forming or crystal growth processing chamber capable of reducing pressure. And a suction pipe for sucking gas from the processing chamber by a vacuum pump, and a pressure control valve is provided in the vicinity of the connection port of the suction pipe with the processing chamber. A film-forming apparatus or a crystal growth apparatus cleaning method for performing processing under reduced pressure with the vacuum pump connected to an end side,
An open / close valve that can be opened and closed in the vicinity of the connection port with the vacuum pump in the intake pipe, the pressure control valve is fully opened, the open / close valve is closed,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride in the treatment chamber An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas By supplying a mixed gas with an inert gas to the mixed halogen compound gas,
Mixing the interhalogen compound gas alone or the mixed interhalogen compound gas or the interhalogen compound gas alone and a gas inert to the gas alone at a pressure of 0.5 kPa to 80 kPa in the processing chamber and the intake pipe Forming a sealing process for holding a gas or a mixed gas of the mixed interhalogen gas and a gas inert to the mixed interhalogen gas for a predetermined time;
Opening the on-off valve and operating the vacuum pump to the inter-halogen compound gas alone or the mixed inter-halogen compound gas or the inter-halogen compound gas alone and the gas alone sealed in the processing chamber and the intake pipe Forming an exhaust process of exhausting a mixed gas with an inert gas or a mixed gas of the mixed interhalogen compound gas and a gas inert to the mixed interhalogen compound gas;
The sealing step and the exhausting step are alternately performed a plurality of times to clean the inside of the processing chamber and the inside of the intake pipe.

According to a fourth aspect of the present invention, there is provided a film-forming apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, wherein a film-forming or crystal-growing gas is provided in a film-forming or crystal-growing processing chamber capable of reducing pressure A supply passage for supplying gas and an intake pipe for sucking gas from the processing chamber by a vacuum pump, and a device gate valve and a pressure control valve are provided in the vicinity of the connection port of the intake pipe with the processing chamber, A method of cleaning a film forming apparatus or a crystal growing apparatus for performing processing under reduced pressure, wherein the vacuum pump is connected to the other end of the intake pipe,
An opening / closing valve capable of adjusting the opening degree is provided near the connection port with the vacuum pump in the intake pipe, the device gate valve is closed, and the opening degree of the opening / closing valve is adjusted,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride for the intake pipe An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas and operating the vacuum pump, the inside of the intake pipe is maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. Is.

According to a fifth aspect of the present invention, there is provided a film deposition apparatus or crystal growth apparatus cleaning method for performing a treatment under reduced pressure, wherein a film deposition or crystal growth gas is provided in a process chamber for film deposition or crystal growth that can be decompressed. A supply passage for supplying gas and an intake pipe for sucking gas from the processing chamber by a vacuum pump, and a device gate valve and a pressure control valve are provided in the vicinity of the connection port of the intake pipe with the processing chamber, A method of cleaning a film forming apparatus or a crystal growing apparatus for performing processing under reduced pressure, wherein the vacuum pump is connected to the other end of the intake pipe,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride for the intake pipe An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas,
By closing the device gate valve and adjusting the number of rotations of the vacuum pump that can adjust the number of rotations, the suction pipe is maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. .

According to a sixth aspect of the present invention, there is provided a film deposition apparatus or crystal growth apparatus cleaning method for performing a treatment under reduced pressure, wherein a film deposition or crystal growth gas is provided in a process chamber for film deposition or crystal growth that can be decompressed. A supply passage for supplying gas and an intake pipe for sucking gas from the processing chamber by a vacuum pump, and a device gate valve and a pressure control valve are provided in the vicinity of the connection port of the intake pipe with the processing chamber, A method of cleaning a film forming apparatus or a crystal growing apparatus for performing processing under reduced pressure, wherein the vacuum pump is connected to the other end of the intake pipe,
An open / close valve that can be opened and closed in the vicinity of the connection port with the vacuum pump in the intake pipe, and closes the device gate valve and the open / close valve,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride for the intake pipe An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas By supplying a mixed gas with an inert gas to the mixed halogen compound gas,
The interhalogen compound gas alone or the mixed interhalogen compound gas or the mixed gas of the interhalogen compound gas alone and a gas inert to the gas alone or the mixture at a pressure of 0.5 kPa to 80 kPa in the intake pipe Forming a sealing step for holding a state in which a mixed gas of an interhalogen compound gas and a gas inert to the mixed interhalogen gas is sealed for a predetermined time;
The interhalogen compound gas alone or the mixed interhalogen compound gas or the interhalogen compound gas alone and the gas inert to the gas alone, which opens the on-off valve and operates the vacuum pump and is sealed in the intake pipe. Or an exhaust process for exhausting a mixed gas of a mixed gas of the mixed interhalogen compound gas and a gas inert to the mixed interhalogen compound gas,
The inside of the intake pipe is cleaned by alternately performing the sealing step and the exhausting step a plurality of times.

    According to a seventh aspect of the present invention, there is provided a method for cleaning a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, in addition to the configuration of the present invention according to the third or sixth aspect, The end point of the cleaning is detected by comparing the value or the calculated value with the set value.

  The film forming apparatus or crystal growth apparatus cleaning method for processing under reduced pressure according to the present invention according to claim 8 monitors the intensity of the emission spectrum in addition to the configuration of the present invention according to claim 1, 2, 4 or 5. A monitoring chamber is provided, a monitoring vacuum pump is connected to the monitoring chamber, and a part of the exhaust gas at the outlet of the vacuum pump connected to the other end of the intake pipe is led to the monitoring chamber via a mass flow controller, and the monitoring is performed. The exhaust gas introduced into the chamber is converted into plasma by a plasma generator, the intensity of the emission spectrum is monitored, and the end point of cleaning is detected.

According to a ninth aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, wherein a film deposition or crystal growth gas is provided in a process chamber for film deposition or crystal growth that can be decompressed. And a suction pipe for sucking gas from the processing chamber by a vacuum pump, and a pressure control valve is provided in the vicinity of the connection port of the suction pipe with the processing chamber. A film forming apparatus or a crystal growth apparatus cleaning method for performing processing under reduced pressure with a vacuum pump connected to an end side,
An opening / closing valve whose opening degree can be adjusted is provided near the connection port of the vacuum pump in the intake pipe, the pressure control valve is fully opened, and the opening degree of the opening / closing valve is adjusted,
To the processing chamber, as a cleaning gas, the following mixed gas described in (1), (3), (4) or (5) or any single gas described in (2) below is supplied,
(1) fluorine,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(2) Nitrogen trifluoride simple substance or chlorine trifluoride simple substance
(3) nitrogen trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(4) chlorine trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(5) A mixed gas of dicarbon tetrafluoride, tricarbon octafluoride, sulfur hexafluoride or carbonyl fluoride and oxygen gas. Further, the cleaning gas is converted into plasma inside or outside the processing chamber by a plasma generator. At the same time, by operating the vacuum pump, the processing chamber and the intake pipe are maintained at a pressure of 50 Pa to 1.1 kPa for cleaning.

According to a tenth aspect of the present invention, there is provided a film forming apparatus or a crystal growth apparatus cleaning method for performing a process under reduced pressure, wherein a film forming or crystal growth gas is provided in a processing chamber for film formation or crystal growth capable of reducing pressure And a supply pipe for exhausting gas from the processing chamber by a vacuum pump, and a device partition valve and a pressure control valve are provided in the vicinity of the connection port of the processing chamber in the intake pipe. A method of cleaning a film forming apparatus or a crystal growing apparatus that performs processing under reduced pressure with a vacuum pump connected to the other end of the piping
An opening / closing valve whose opening degree can be adjusted is provided near the connection port of the vacuum pump in the intake pipe, the device gate valve is closed, and the opening degree of the opening / closing valve is adjusted,
To the intake pipe, as a cleaning gas, supply any one of the mixed gas described in the following (1), (3), (4) or (5) or any single gas described in the following (2),
(1) fluorine,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(2) Nitrogen trifluoride simple substance or chlorine trifluoride simple substance
(3) nitrogen trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(4) chlorine trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(5) A mixed gas of dicarbon tetrafluoride, tricarbon octafluoride, sulfur hexafluoride or carbonyl fluoride, and oxygen gas. Further, the cleaning gas is removed from the intake pipe or outside the intake pipe by a plasma generator. The inside of the intake pipe is maintained at a pressure of 50 Pa to 1.1 kPa and cleaned by turning into a plasma and operating the vacuum pump.

According to the first aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, with a vacuum pump in an intake pipe connected to a process chamber for film formation or crystal growth capable of being decompressed. An opening / closing valve whose opening degree can be adjusted is provided in the vicinity of the connection port, a pressure control valve provided in the vicinity of the connection port with the processing chamber in the intake pipe is fully opened, the opening degree of the opening / closing valve is adjusted, and the processing chamber In addition to supplying a specific cleaning gas made of chlorine trifluoride, etc., and operating the vacuum pump, the processing chamber and the intake pipe are maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. Therefore, it is possible to satisfactorily remove the deposited film adhering to the processing chamber and the intake pipe during the film forming process or the crystal growth process, shortening the time required for cleaning, and cleaning gas. It is possible to reduce the consumption of.
In particular, since the deposited film adhering to the intake pipe can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It is.

  According to a second aspect of the present invention, there is provided a cleaning method for a film forming apparatus or a crystal growth apparatus for performing a process under reduced pressure, wherein a specific chamber made of chlorine trifluoride or the like is provided in a processing chamber for film formation or crystal growth capable of reducing pressure. While supplying gas, the pressure control valve provided in the vicinity of the connection port with the process chamber in the intake pipe connected to the process chamber is fully opened, and the vacuum pump provided in the intake pipe connected to the process chamber Since the rotation speed is adjustable and the rotation speed of the vacuum pump is adjusted, the processing chamber and the intake pipe are maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. Thus, the same effects as those of the present invention can be obtained.

  According to a third aspect of the present invention, there is provided a cleaning method for a film forming apparatus or a crystal growing apparatus for performing a process under reduced pressure, with a vacuum pump in an intake pipe connected to a film forming or crystal growing processing chamber capable of reducing pressure. An on-off valve that can be opened and closed in the vicinity of the connection port is provided, the pressure control valve provided in the vicinity of the connection port with the processing chamber in the intake pipe is fully opened, the on-off valve is closed, and chlorine trifluoride is provided in the processing chamber. Forming a sealing step for holding a state in which the specific cleaning gas is sealed at a pressure of 0.5 kPa to 80 kPa for a predetermined time by supplying a specific cleaning gas composed of Opening the on-off valve and operating the vacuum pump to form an exhaust process for exhausting the specific cleaning gas sealed in the processing chamber and the intake pipe, the sealing process and the exhaust Extent and the from is obtained so as to clean the processing chamber and in the intake pipe performed a plurality of times alternately, it is possible to obtain the same benefits as those of the present invention according to claim 1.

  According to a fourth aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, with a vacuum pump in an intake pipe connected to a process chamber for film formation or crystal growth capable of decompression. An opening / closing valve capable of adjusting the opening degree is provided in the vicinity of the connection port, the device gate valve provided in the vicinity of the connection port with the processing chamber in the intake pipe is closed, the opening degree of the opening / closing valve is adjusted, and the intake pipe is provided. While supplying a specific cleaning gas such as chlorine trifluoride and operating the vacuum pump, the inside of the intake pipe is kept at a pressure of 0.5 kPa to 80 kPa for cleaning. Alternatively, the deposited film adhering to the intake pipe during the crystal growth process can be removed satisfactorily, and when the film forming apparatus or the crystal growing apparatus is repaired or disassembled, disasters caused by harmful or dangerous deposited films can be prevented. Can be further possible to decrease the time required for the cleaning, it is possible to reduce the consumption of the cleaning gas.

  According to a fifth aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure. A specific cleaning gas is supplied, and the device gate valve provided in the vicinity of the connection port with the processing chamber in the intake piping connected to the processing chamber is closed, and provided in the intake piping connected to the processing chamber. Since the rotation speed of the vacuum pump is configured to be adjustable and the rotation speed of the vacuum pump is adjusted, the inside of the intake pipe is maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. The same effect as that of the present invention according to No. 4 can be achieved.

  According to a sixth aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, with a vacuum pump in an intake pipe connected to a process chamber for film formation or crystal growth capable of decompression. An open / close valve that can be opened and closed in the vicinity of the connection port is provided, and a device gate valve provided in the vicinity of the connection port with the processing chamber in the intake pipe is closed, and the open / close valve is closed, and chlorine trifluoride is used in the intake pipe. By supplying a specific cleaning gas, forming a sealing step for holding the specific cleaning gas sealed in the intake pipe at a pressure of 0.5 kPa to 80 kPa for a predetermined time, opening the on-off valve and An exhaust process for operating the vacuum pump to exhaust the specific cleaning gas sealed in the intake pipe is formed, and the sealing process and the exhaust process are alternately performed a plurality of times to perform the intake process. Since is obtained so as to clean the pipe, it is possible to obtain the same benefits as those of the present invention according to claim 4.

    In addition to the effect of the present invention according to claim 3 or 6, the cleaning method for a film forming apparatus or crystal growth apparatus for performing processing under reduced pressure according to the present invention according to claim 7 detects and detects the sealing pressure in the sealing process. The end point of the cleaning is detected by comparing the value or the calculated value with the set value, so that the cleaning after performing various processes in the film forming or crystal growth processing chamber. However, it is possible to accurately detect the end point of cleaning according to the condition of the processing chamber and the intake pipe or the state of the deposited film adhering to the intake pipe, and it is possible to eliminate excessive or insufficient cleaning.

  In addition to the effect of the present invention according to claim 1, 4, or 5, the film forming apparatus or crystal growth apparatus cleaning method for processing under reduced pressure according to the present invention according to claim 8 monitors the intensity of the emission spectrum. A monitoring chamber is provided, a monitoring vacuum pump is connected to the monitoring chamber, and a part of the exhaust gas at the outlet of the vacuum pump connected to the other end of the intake pipe is led to the monitoring chamber via a mass flow controller, and the monitoring is performed. Since the exhaust gas introduced into the chamber is converted into plasma by a plasma generator and the emission spectrum intensity is monitored and the end point of cleaning is detected, various treatments are performed in the processing chamber for film formation or crystal growth. Even after cleaning, it is possible to detect an accurate cleaning end point according to the state of the deposited film attached to the processing chamber and the intake pipe or the intake pipe, It is possible to eliminate the excess and deficiency of cleaning.

According to a ninth aspect of the present invention, there is provided a film deposition apparatus or a crystal growth apparatus cleaning method for performing a treatment under reduced pressure, with a vacuum pump in an intake pipe connected to a process chamber for film formation or crystal growth capable of being decompressed. An opening / closing valve whose opening degree can be adjusted is provided in the vicinity of the connection port, a pressure control valve provided in the vicinity of the connection port with the processing chamber in the intake pipe is fully opened, the opening degree of the opening / closing valve is adjusted, and the processing chamber Supplying a cleaning gas composed of a specific fluorine-based gas, etc., and further converting the cleaning gas into plasma outside the processing chamber or outside the processing chamber by a plasma generator and operating the vacuum pump, Since the inside of the intake pipe is maintained at a pressure of 50 Pa to 1.1 kPa for cleaning, the inside of the process chamber and the intake pipe are used during the film forming process or the crystal growth process. The adhered deposited film can be satisfactorily removed, thereby shortening the time required for cleaning, it is possible to reduce the consumption of the cleaning gas.
In particular, since the deposited film adhering to the intake pipe can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It is.

  According to a tenth aspect of the present invention, there is provided a cleaning method for a film forming apparatus or a crystal growing apparatus for performing processing under reduced pressure, with a vacuum pump in an intake pipe connected to a processing chamber for film forming or crystal growing capable of reducing pressure. An opening / closing valve capable of adjusting the opening degree is provided in the vicinity of the connection port, the device gate valve provided in the vicinity of the connection port with the processing chamber in the intake pipe is closed, the opening degree of the opening / closing valve is adjusted, and the intake pipe is provided. Supplying a cleaning gas composed of a specific fluorine-based gas, etc., and further converting the cleaning gas into plasma inside or outside the intake pipe by a plasma generator and operating the vacuum pump, thereby Was maintained at a pressure of 50 Pa to 1.1 kPa for cleaning, so that the deposited film adhering to the intake pipe during the film formation process or crystal growth process can be removed well. When repairing or disassembling the film deposition device or crystal growth device, it is possible to prevent disasters caused by harmful and dangerous deposited films, and further reduce the time required for cleaning and the consumption of cleaning gas. Can be reduced.

Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning 1st embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning 2nd embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning 3rd embodiment of this invention Explanatory drawing which shows the pressure change in the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning 3rd embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning 4th embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning the 5th embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus which performs a process under reduced pressure, or the crystal growth apparatus which concerns on the 6th embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus which performs a process under pressure reduction, or the crystal growth apparatus which concerns on 7th embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus or crystal growth apparatus which processes under reduced pressure concerning 8th Embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus which performs a process under reduced pressure, or the crystal growth apparatus which concerns on 9th embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus which performs a process under reduced pressure, or a crystal growth apparatus based on 10th Embodiment of this invention Explanatory drawing which shows the outline of the cleaning method of the film-forming apparatus which performs a process under reduced pressure, or a crystal growth apparatus based on 11th Embodiment of this invention

DESCRIPTION OF EMBODIMENTS Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
A cleaning method of a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to the first embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.

Reference numeral 1 denotes a process chamber for film formation or crystal growth that can be depressurized. Connected to the process chamber 1 is a supply path 2 for a cleaning gas and an intake pipe 6 for sucking gas from the process chamber 1 by a vacuum pump 4. Has been.
The cleaning gas supply path 2 is provided with a mass flow controller 2a and an on-off valve 2b.

An apparatus gate valve 7 and a pressure control valve 8 are provided in the vicinity of the connection port 6a with the processing chamber 1 in the intake pipe 6, the vacuum pump 4 is connected to the other end side of the intake pipe 6, and the intake pipe In the vicinity of the connection port 6b with the vacuum pump 4 in FIG.
An exhaust gas passage 10 is provided on the exhaust side of the vacuum pump 4, and the exhaust gas passage 10 is provided with a treatment device for adsorbing or decomposing harmful or dangerous gas in the exhaust gas as necessary.

When the film formation is performed as a film formation process chamber, the process chamber 1 is not shown, but for example, an amorphous silicon film as a material of a polysilicon thin film for a liquid crystal display is formed on a glass substrate by plasma CVD. In addition, an amorphous silicon film or a microcrystal silicon film for a thin film solar cell is formed on a glass substrate by plasma CVD, and a film forming gas and a diluting gas necessary for forming a thin film are processed in the processing chamber. 1 is used to form a film.
In addition, when the crystal growth is performed as a processing chamber for crystal growth, the processing chamber 1 is not shown, but for example, a bulk silicon solar cell is formed by a crystal growth method such as molecular beam epitaxy (Molecular Beam Epitaxy). A crystal thin film is formed.

The processing for film formation or crystal growth in the processing chamber 1 has been put into practical use and is not related to the technical features of the present invention, so illustration and description thereof are omitted.
When the film formation process or the crystal growth process is continued for a predetermined number of times in the processing chamber 1, powder, film formation, or crystal growth for chipping of amorphous silicon or microcrystal silicon is placed in the processing chamber 1 and the intake pipe 6. Deposited films of amorphous silicon, silicon nitride, silicon oxide, silicon oxynitride, and other materials, and molybdenum, tantalum, tungsten, arsenic, boron, phosphorus, germanium, antimony, etc., are produced, resulting in thin films of products. In order to maintain the quality, it is necessary to perform regular cleaning.

In the cleaning method according to the first embodiment, the device gate valve 7 is opened, the pressure control valve 8 is fully opened, the on-off valve 2b interposed in the supply path 2 is opened, and the mass flow controller 2a is set to a predetermined value. The opening of the on-off valve 9 is adjusted so that the pressure in the intake pipe 6 becomes a predetermined pressure suitable for cleaning, and chlorine trifluoride as a cleaning gas is supplied to the processing chamber 1 in the supply path. 2 and the vacuum pump 4 is operated to clean the inside of the processing chamber 1 and the intake pipe 6 while maintaining a predetermined pressure, for example, 5 kPa.
The predetermined pressure suitable for chlorine trifluoride cleaning is determined from the temperature at the time of chlorine trifluoride cleaning, the type of deposited film, and the like.

Then, by performing the above cleaning method, the deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 during the film forming process or the crystal growth process can be removed well, and the time required for cleaning is shortened. Therefore, the consumption of cleaning gas can be reduced.
In particular, since the deposited film adhering in the intake pipe 6 can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It can be done.

In the first embodiment described above, chlorine trifluoride alone was used as the cleaning gas, but a mixed gas of chlorine trifluoride and nitrogen gas inert to chlorine trifluoride was used as the cleaning gas. In this case, a supply path provided with a mass flow controller for nitrogen gas and an on-off valve is provided in parallel with the supply path 2, and the mixed gas is supplied to the processing chamber 1 by merging. The predetermined pressure in the processing chamber 1 and the intake pipe 6 at the time is increased according to the mixing ratio of nitrogen gas.
The cleaning gas can be chlorine fluoride, chlorine trifluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride instead of chlorine trifluoride alone or a mixed gas of chlorine trifluoride and nitrogen gas. , An interhalogen compound gas selected from the group consisting of iodine pentafluoride and iodine heptafluoride may be used alone, or chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, It may be a mixed interhalogen gas containing two or more interhalogen gas selected from the group consisting of bromine monochloride, iodine pentafluoride and iodine heptafluoride, and the interhalogen gas and the gas And a mixed gas of the mixed interhalogen compound gas and a gas inert to the mixed interhalogen compound gas.

In these cases, the opening degree of the on-off valve 9 is adjusted so that the predetermined pressure in the processing chamber 1 and the intake pipe 6 is in the range of 0.5 kPa to 80 kPa according to the properties of the cleaning gas.
Also, as a cleaning gas, a mixed gas of the interhalogen compound gas alone and a gas inert to the gas alone or a mixture of the mixed interhalogen compound gas and a gas inert to the mixed halogen compound gas In the case of a gas, the mixing ratio of the interhalogen compound gas and the inert gas is determined according to the amount, thickness, composition, etc. of the deposited film adhering to the inner wall of the processing chamber 1 and the inner surface of the intake pipe 6. To do.

It should be noted that the opening of the on-off valve 9 that can be adjusted during cleaning may be adjusted by an opening controller so that the pressure in the intake pipe 6 is detected and a predetermined pressure is obtained. When the same film forming process or the same crystal growth process is performed in the processing chamber 1, the cleaning may be performed at a preset opening degree.
As for the end of cleaning, a cleaning time is set, and when the set time elapses, the cleaning may be ended, or a known cleaning end means may be adopted.

Next, a cleaning method of a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to the second embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
Hereinafter, a cleaning method similar to that of the first embodiment will be described with the same reference numerals in FIG.

In the first embodiment, an opening / closing valve 9 is provided in the intake pipe 6 near the connection port 6b to the vacuum pump 4, and the opening degree of the opening / closing valve 9 can be adjusted during cleaning. In the second embodiment, the vacuum pump 5 capable of adjusting the rotational speed is provided on the other end side of the intake pipe 6 without providing the on-off valve. The pressure of the vacuum pump 5 is adjusted by a pressure detector 5a for detecting the pressure in the intake pipe 6 and a pressure control device 5b.
In the cleaning method according to the second embodiment, the device gate valve 7 is opened, the pressure control valve 8 is fully opened, the on-off valve 2b provided in the supply path 2 is opened, and the mass flow controller 2a is set in a predetermined manner. The value is set, and chlorine trifluoride as a cleaning gas is supplied to the processing chamber 1 from the supply path 2 and the rotation speed of the vacuum pump 5 is adjusted, whereby the inside of the processing chamber 1 and the intake air are adjusted. The inside of the pipe 6 is cleaned at a predetermined pressure, for example, 5 kPa.

By performing the cleaning method according to the second embodiment described above, the deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 during the film formation process or the crystal growth process is removed as in the first embodiment. It can be removed satisfactorily, shortening the time required for cleaning, and reducing the consumption of the cleaning gas.
In particular, since the deposited film adhering in the intake pipe 6 can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It can be done.

  As for the end of cleaning, similar to the first embodiment, a cleaning time may be set, and the cleaning may be ended when the set time has elapsed. A known cleaning end means is employed. May be.

Next, referring to the schematic explanatory view of FIG. 3 and the explanatory view showing the pressure change of FIG. 4 for the cleaning method of the film forming apparatus or the crystal growth apparatus for performing the treatment under reduced pressure according to the third embodiment of the present invention. While explaining.
Hereinafter, a cleaning method similar to that of the first embodiment will be described with the same reference numerals in FIG.

In the first embodiment, an opening / closing valve 9 is provided in the intake pipe 6 near the connection port 6b to the vacuum pump 4, and the opening degree of the opening / closing valve 9 can be adjusted during cleaning. In the third embodiment, the opening / closing valve 9a is replaced with the opening / closing valve 9a, and the opening / closing valve 9a is provided. An enclosed pressure detector 11 for detecting pressure and an end point detecting device 11a for detecting the end point of cleaning are provided.
In the cleaning method according to the third embodiment, the device gate valve 7 is opened, the pressure control valve 8 is fully opened, the on-off valve 9a is closed, and the cleaning gas is supplied to the processing chamber 1 By supplying from 2, the cleaning gas is sealed so that the inside of the processing chamber 1 and the intake pipe 6 are at a predetermined pressure, and then the on-off valve 2b of the supply path 2 is closed to finish the sealing of the cleaning gas. Then, an enclosing process for holding the encapsulated state for a predetermined time is formed, and the opening / closing valve 9a is opened and the vacuum pump 4 is operated to exhaust the cleaning gas enclosed in the processing chamber 1 and the intake pipe 6 The inside of the processing chamber 1 and the inside of the intake pipe 6 are cleaned by alternately performing the sealing step and the exhausting step a plurality of times.

Thus, by performing the sealing step and the exhausting step alternately a plurality of times to clean the inside of the processing chamber 1 and the inside of the intake pipe 6, as in the first embodiment, The deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 during the crystal growth process can be removed satisfactorily, and the time required for cleaning can be shortened and the consumption of the cleaning gas can be reduced.
In particular, since the deposited film adhering in the intake pipe 6 can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It can be done.

Further, in the third embodiment, as described below, the end point of the cleaning is accurately detected so that the cleaning without excess or deficiency can be performed.
FIG. 4 shows changes in pressure in the intake pipe 6 and the processing chamber 1 in the sealing process and the exhaust process, with the time T on the horizontal axis and the pressure P on the vertical axis.

In FIG. 4, P1 to P20 indicate the sealing process, E1 to E20 indicate the exhaust process, and in the sealing process of P1 to P6, if cleaning gas is sealed, it accumulates in the processing chamber 1 and the intake pipe 6. This shows that the deposited film reacts with the cleaning gas to generate a reactive compound gas and the pressure rises, indicating that the cleaning of the deposited film is not completed.
Then, the absence of the pressure increase after the sealing indicates that the cleaning is completed, and in the sealing process after P10, the cleaning is completed.

Therefore, the end point detection device 11a detects the end point of cleaning by comparing the detected value obtained by detecting the pressure in the intake pipe 6 with the sealed pressure detector 11 or the calculated value thereof with a set value.
For example, the end point detection device 11a compares a detection value obtained by detecting the pressure in the intake pipe 6 with the enclosed pressure detector 11 with a set value that is a detection value detected in a state where no deposited film is present, The end point of cleaning can be detected by differentiating the change or comparing the previous detection value with the current detection value.

The cleaning may be terminated immediately after the end point of cleaning is detected, or the cleaning may be terminated by performing several sealing steps and exhausting steps after the end point of cleaning is detected in order to ensure complete cleaning. .
In the third embodiment described above, the end point of cleaning is detected. However, the detection of the end point of cleaning can be omitted. In this case, the end of cleaning includes the sealing step and the exhausting step. The number of repetitions may be set in advance to end the cleaning.

Next, a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to a fourth embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
Hereinafter, the same cleaning method as in the first embodiment will be described with the same reference numerals in FIG.

In the first embodiment, the cleaning gas supply path 2 is connected to the processing chamber 1. In the fourth embodiment, the cleaning pipe is provided in the vicinity of the connection port 6 a with the processing chamber 1 in the intake pipe 6. The cleaning gas supply path 3 is connected to the intake pipe 6 between the device gate valve 7 and the pressure control valve 8, and the mass flow controller 3 a and the opening / closing valve 3 b are interposed in the supply path 3.
In the cleaning method according to the fourth embodiment, the device gate valve 7 is closed, the pressure control valve 8 is fully opened, the on-off valve 3b provided in the supply path 3 is opened, and the mass flow controller 3a is set in a predetermined manner. The opening / closing valve 9 is set to a value, and the opening of the on-off valve 9 is adjusted so that the pressure in the intake pipe 6 becomes a predetermined pressure suitable for cleaning, and the cleaning gas is supplied to the intake pipe 6 from the supply path 3. At the same time, by operating the vacuum pump 4, the inside of the intake pipe 6 is maintained at a predetermined pressure for cleaning.

Thus, by performing the cleaning method according to the fourth embodiment, it is possible to satisfactorily remove the deposited film adhering to the intake pipe 6 during the film forming process or the crystal growth process, and the film forming apparatus or the crystal When repairing or disassembling growth equipment, it is possible to prevent disasters caused by harmful and dangerous deposited films, and further reduce the time required for cleaning and the consumption of cleaning gas. .
In the fourth embodiment, the cleaning of the processing chamber 1 is not intended. However, the cleaning of the processing chamber 1 is performed manually.

Cleaning the inside of the processing chamber 1 by hand is a product in which a trace amount of an interhalogen compound remains in the processing chamber 1 among products in which film formation or crystal growth is performed in the processing chamber 1 Because there is.
As in the first embodiment, the cleaning may be ended by setting a cleaning time, and when the set time has elapsed, the cleaning may be ended by employing a known cleaning end means. Also good.

Next, a cleaning method of a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to a fifth embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
Hereinafter, a cleaning method similar to that of the second embodiment will be described with the same reference numerals in FIG.

In the second embodiment, the cleaning gas supply path 2 is connected to the processing chamber 1. In the fifth embodiment, the cleaning pipe is provided in the vicinity of the connection port 6 a with the processing chamber 1 in the intake pipe 6. The cleaning gas supply path 3 is connected to the intake pipe 6 between the device gate valve 7 and the pressure control valve 8, and the mass flow controller 3 a and the opening / closing valve 3 b are interposed in the supply path 3.
In the cleaning method according to the fifth embodiment, the device gate valve 7 is closed, the pressure control valve 8 is fully opened, the on-off valve 3b provided in the supply path 3 is opened, and the mass flow controller 3a is set in a predetermined manner. The value is set, and cleaning gas is supplied to the intake pipe 6 from the supply path 3, and the inside of the intake pipe 6 is maintained at a predetermined pressure for cleaning by adjusting the rotation speed of the vacuum pump 5. .

In this way, by performing the cleaning method according to the fifth embodiment, similarly to the fourth embodiment, the deposited film adhering to the intake pipe 6 during the film formation process or the crystal growth process can be satisfactorily removed. When repairing or disassembling the film formation apparatus or crystal growth apparatus, it is possible to prevent disasters caused by harmful and dangerous deposited films, and further reduce the time required for cleaning and reduce the amount of cleaning gas. Consumption can be reduced.
Note that the cleaning of the processing chamber 1 is performed manually separately as in the fourth embodiment.

  As for the end of cleaning, as in the second embodiment, a cleaning time may be set, and the cleaning may be ended when the set time has elapsed. A known cleaning end means is employed. May be.

Next, a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to the sixth embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
Hereinafter, a cleaning method similar to that of the third embodiment will be described with the same reference numerals in FIG.

In the third embodiment, the cleaning gas supply path 2 is connected to the processing chamber 1. However, in the sixth embodiment, the cleaning pipe is provided in the vicinity of the connection port 6 a with the processing chamber 1 in the intake pipe 6. The cleaning gas supply path 3 is connected to the intake pipe 6 between the device gate valve 7 and the pressure control valve 8, and the mass flow controller 3 a and the opening / closing valve 3 b are interposed in the supply path 3.
In the cleaning method according to the sixth embodiment, the device gate valve 7 is closed, the pressure control valve 8 is fully opened, the on-off valve 9a is closed, and the cleaning gas is supplied to the intake pipe 6. 3, the intake pipe 6 is filled with a cleaning gas at a predetermined pressure, and then the on-off valve 3 b of the supply passage 3 is closed to finish the sealing of the cleaning gas, and the sealed state is maintained for a predetermined time. Forming the sealing step, opening the on-off valve 9a, and operating the vacuum pump 4 to exhaust the cleaning gas sealed in the intake pipe 6 to form the sealing step and the exhausting step. The inside of the intake pipe 6 is cleaned by alternately performing a plurality of times.

In this way, by performing the sealing step and the exhausting step alternately a plurality of times to clean the inside of the intake pipe 6, as in the fourth embodiment, the intake pipe is used during the film forming process or the crystal growth process. 6 can be removed satisfactorily, and when repairing or disassembling the film forming apparatus or crystal growth apparatus, it is possible to prevent disasters caused by harmful and dangerous deposited films, and further cleaning. In addition to shortening the time required for the cleaning, the consumption of the cleaning gas can be reduced.
Note that the cleaning of the processing chamber 1 is performed manually separately as in the fourth embodiment.

In the sixth embodiment, the end point of the cleaning is accurately detected so that the cleaning without excess or deficiency can be performed. This point is the same as the third embodiment. Therefore, explanation is omitted.
Furthermore, in the above sixth embodiment, the end point of cleaning is detected, but detection of the end point of cleaning can be omitted. In this case, the end of cleaning is the same as in the third embodiment. Similarly, the number of times of repeating the sealing step and the exhausting step may be set in advance to end the cleaning.

Next, a cleaning method for a film forming apparatus or a crystal growing apparatus that performs processing under reduced pressure according to a seventh embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
In the seventh embodiment, an exhaust gas branch path 12 is attached to the exhaust gas path 10 in the first embodiment to detect the end point of cleaning.

Hereinafter, differences from the first embodiment will be described.
In FIG. 8, an exhaust gas branch 12 is branched and connected to the exhaust gas path 10, and a monitoring chamber 13 for monitoring the intensity of the emission spectrum is provided at the end of the exhaust gas branch 12.
A monitoring vacuum pump 13a is connected to the monitoring chamber 13, and a part of the exhaust gas in the exhaust gas passage 10 is guided from the exhaust gas branching passage 12 to the monitoring chamber 13 via the mass flow controller 12a.

The exhaust gas introduced into the monitoring chamber 13 is provided with a high frequency power source 14a and electrodes 14b and 14c, and is converted into plasma by the plasma generator 14 so that the emission spectrum intensity is monitored by the emission spectrum intensity monitoring apparatus 15. .
As the cleaning progresses, the emission spectrum intensity monitoring device 15 reduces the reaction product gas of the deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 to reduce the intensity of the emission spectrum. The end point of cleaning is detected by comparing with the set value.

The outlet of the monitoring vacuum pump 13a is joined to the exhaust gas passage 10 by the exhaust gas joint passage 12b.
In the cleaning method according to the seventh embodiment, the monitoring chamber 13 for monitoring the intensity of the emission spectrum is provided in the first embodiment, the monitoring vacuum pump 13a is connected to the monitoring chamber 13, and the intake air is sucked. A part of the exhaust gas at the outlet of the vacuum pump 4 connected to the other end of the pipe 6 is guided to the monitoring chamber 13 via the mass flow controller 12a, and the exhaust gas guided to the monitoring chamber 13 is converted into plasma by the plasma generator 14. Since the intensity of the emission spectrum is monitored by the intensity monitoring device 15 and the end point of cleaning is detected, the processing chamber 1 and the intake pipe 6 according to the first embodiment can be cleaned while being cleaned. In the process chamber 1 for film formation or crystal growth, even in the cleaning after performing various processes, it adheres to the inside of the process chamber 1 and the intake pipe 6. Could be detected the end point of accurate cleaning according to the situation of the deposited film, it is possible to eliminate the excess or shortage of the cleaning.

The cleaning may be terminated immediately after the end point of the cleaning is detected by the intensity monitoring device 15, or the cleaning may be terminated after the cleaning is performed for a certain time after the end point of the cleaning is detected in order to ensure complete cleaning. .
In the seventh embodiment described above, the cleaning end point detection mechanism is attached to the exhaust gas passage 10 in the first embodiment, but the second embodiment, the fourth embodiment, or the fifth embodiment. A cleaning end point detection mechanism may be attached to the exhaust gas passage 10 in the embodiment.
In this case, in the second embodiment, the fourth embodiment, or the fifth embodiment, the cleaning is performed after various processes are performed in the processing chamber 1 for film formation or crystal growth. However, it is possible to accurately detect the end point of cleaning in accordance with the situation of the deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 or the intake pipe 6, thereby eliminating excessive or insufficient cleaning. It can be done.

Next, a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to an eighth embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
In the eighth embodiment, the cleaning gas is converted into plasma using the cleaning gas plasma generator 16 in the processing chamber 1 in the first embodiment, and the cleaning gas is also cleaned. This is different from the first embodiment.

Hereinafter, differences from the first embodiment will be described.
In FIG. 9, a plasma generator 16 composed of an upper electrode 16 a and a lower electrode 16 b connected to a high frequency power supply 16 a is disposed in the processing chamber 1, and the cleaning gas supplied from the supply path 2 to the processing chamber 1 is plasma. It tries to become.

In the cleaning method according to the eighth embodiment, the device gate valve 7 is opened, the pressure control valve 8 is fully opened, the on-off valve 2b interposed in the supply path 2 is opened, and the mass flow controller 2a is set to a predetermined value. The opening of the on-off valve 9 is adjusted so that the pressure in the intake pipe 6 becomes a predetermined pressure suitable for cleaning, and nitrogen trifluoride as a cleaning gas is supplied to the processing chamber 1 in the supply path. 2 and the vacuum pump 4 is operated to clean the inside of the processing chamber 1 and the intake pipe 6 while maintaining a predetermined pressure, for example, 300 Pa.
Then, by performing the above cleaning method, the deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 during the film forming process or the crystal growth process can be removed well, and the time required for cleaning is shortened. Therefore, the consumption of cleaning gas can be reduced.

In particular, since the deposited film adhering in the intake pipe 6 can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It can be done.
In the above eighth embodiment, nitrogen trifluoride alone was used as the cleaning gas, but a mixed gas containing nitrogen trifluoride and at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas May be used as a cleaning gas. In this case, a supply path provided with a mass flow controller and an on-off valve for each gas is provided in parallel with the supply path 2, and the mixed gas is supplied to the processing chamber 1 by merging. The predetermined pressure in the processing chamber 1 and the intake pipe 6 at the time of cleaning is set to a pressure suitable for plasma formation.

Further, as the cleaning gas, instead of the nitrogen trifluoride alone or the mixed gas with nitrogen trifluoride, any one of the mixed gas described in the following (1), (3) or (4) or the following (2 ) May be used as a simple substance gas.
(1) fluorine,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(2) Chlorine trifluoride simple substance
(3) chlorine trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(4) Gas mixture of dicarbon tetrafluoride, tricarbon octafluoride, sulfur hexafluoride or carbonyl fluoride and oxygen gas

In these cases, the opening degree of the on-off valve 9 is adjusted so that the predetermined pressure in the processing chamber 1 and the intake pipe 6 is in the range of 50 Pa to 1.1 kPa according to the properties of the cleaning gas.
It should be noted that the opening of the on-off valve 9 that can be adjusted during cleaning may be adjusted by an opening controller so that the pressure in the intake pipe 6 is detected and a predetermined pressure is obtained. When the same film forming process or the same crystal growth process is performed in the processing chamber 1, the cleaning may be performed at a preset opening degree.

  As for the end of cleaning, a known cleaning end means such as monitoring of the emission spectrum intensity, setting of the cleaning time, detection of the opening degree of the on-off valve 9 and the like can be employed.

Next, a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to the ninth embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
In the ninth embodiment, the cleaning gas is changed to plasma in the processing chamber 1 in the eighth embodiment, and the cleaning gas is changed to plasma in the cleaning gas supply passage 3.

Hereinafter, differences from the eighth embodiment will be described.
In FIG. 10, a plasma generator 17 composed of an upper electrode 17 c and a lower electrode 17 d connected to a high-frequency power source 17 b is formed in a plasma generation chamber 17 a interposed in a cleaning gas supply path 2. The cleaning gas supplied to the chamber 1 is turned into plasma.

In the cleaning method according to the ninth embodiment, the device gate valve 7 is opened, the pressure control valve 8 is fully opened, the on-off valve 2b interposed in the supply path 2 is opened, and the mass flow controller 2a is set to a predetermined value. The opening of the on-off valve 9 is adjusted so that the pressure in the intake pipe 6 becomes a predetermined pressure suitable for cleaning, and nitrogen trifluoride as a cleaning gas is generated in the processing chamber 1 by generating the plasma. Since it is converted into plasma by the apparatus 17 and supplied from the supply path 2 and the vacuum pump 4 is operated, the inside of the processing chamber 1 and the intake pipe 6 are maintained at a predetermined pressure, for example, 300 Pa for cleaning. is there.
By performing the above cleaning method, it is possible to satisfactorily remove the deposited film adhering to the inside of the processing chamber 1 and the intake pipe 6 during the film forming process or the crystal growth process, as in the eighth embodiment. In addition, the time required for cleaning can be shortened and the consumption of the cleaning gas can be reduced.

In particular, since the deposited film adhering in the intake pipe 6 can be removed well, it is possible to prevent disasters caused by harmful and dangerous deposited films when repairing or disassembling the film forming apparatus or the crystal growing apparatus. It can be done.
As for the end of cleaning, as in the eighth embodiment, a known cleaning end means such as monitoring of the emission spectrum intensity, setting of the cleaning time, detection of the opening degree of the on-off valve 9 and the like may be employed. it can.

Next, a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to the tenth embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
In the tenth embodiment, a cleaning gas remote plasma generator 18 is provided in the cleaning gas supply path 3 in the fourth embodiment to convert the cleaning gas into plasma and clean it.

Hereinafter, a cleaning method similar to that of the fourth embodiment will be described with the same reference numerals in FIG.
In the tenth embodiment, a plasma generation chamber 18a is provided in the cleaning gas supply path 2 connected to the intake pipe 6, and an upper electrode 18c and a lower electrode 18d connected to a high-frequency power source 18b in the plasma generation chamber 18a. The plasma generator 18 is configured to form the cleaning gas supplied from the supply path 2 to the intake pipe 6 into plasma.

In the cleaning method according to the tenth embodiment, the device gate valve 7 is closed, the pressure control valve 8 is fully opened, the on-off valve 2b interposed in the supply path 2 is opened, and the mass flow controller 2a is set to a predetermined value. The opening of the on-off valve 9 is adjusted so that the pressure in the intake pipe 6 becomes a predetermined pressure suitable for cleaning, and nitrogen trifluoride as a cleaning gas is converted into plasma by the plasma generator 18, While supplying from the supply path 2 and operating the vacuum pump 4, the inside of the intake pipe 6 is maintained at a predetermined pressure, for example, 300 Pa, and cleaned.
By performing the above cleaning method, it is possible to satisfactorily remove the deposited film adhering to the intake pipe 6 during the film forming process or the crystal growth process, as in the fourth embodiment. Or, when repairing or disassembling the crystal growth apparatus, it is possible to prevent disasters caused by harmful and dangerous deposited films, and further reduce the time required for cleaning and the consumption of cleaning gas. It is.

In the tenth embodiment, the cleaning of the processing chamber 1 is not intended, but the cleaning of the processing chamber 1 is performed manually.
As for the end of cleaning, as in the ninth embodiment, a known cleaning end means, for example, monitoring of the emission spectrum intensity, setting of the cleaning time, detection of the opening degree of the on-off valve 9, etc. may be employed. it can.

Next, a cleaning method for a film forming apparatus or a crystal growth apparatus that performs processing under reduced pressure according to the eleventh embodiment of the present invention will be described with reference to a schematic explanatory diagram of FIG.
In the eleventh embodiment, instead of the cleaning gas remote plasma generator 18 provided in the supply passage 3 in the tenth embodiment, a cleaning gas plasma generator 19 is provided in the intake pipe 6 for cleaning. The gas is turned into plasma.

Hereinafter, a cleaning method similar to that of the tenth embodiment will be described with the same reference numerals in FIG.
In the eleventh embodiment, an electrode pipe 19b connected to a high frequency power supply 19a is provided in the intake pipe 6, and the high frequency power supply 19a is connected to the intake pipe 6 made of stainless steel to form an electrode pipe 19c. The cleaning gas for cleaning the inside of the intake pipe 6 is turned into plasma by discharging it to 19c (the intake pipe 6).

In the cleaning method according to the eleventh embodiment, the device gate valve 7 is closed, the pressure control valve 8 is fully opened, the on-off valve 3b provided in the supply path 3 is opened, and the mass flow controller 3a is set to a predetermined value. Then, the opening degree of the on-off valve 9 is adjusted so that the pressure in the intake pipe 6 becomes a predetermined pressure suitable for cleaning, and nitrogen trifluoride as a cleaning gas is supplied from the supply path 3 to the intake pipe 6. At the same time, the plasma generator 19 is turned into plasma and the vacuum pump 4 is operated to keep the intake pipe 6 at a predetermined pressure, for example, 300 Pa, for cleaning.
By performing the above cleaning method, it is possible to satisfactorily remove the deposited film adhering to the intake pipe 6 during the film forming process or the crystal growth process, as in the tenth embodiment, and the film forming apparatus. Or, when repairing or disassembling the crystal growth apparatus, it is possible to prevent disasters caused by harmful and dangerous deposited films, and further reduce the time required for cleaning and the consumption of cleaning gas. It is.

In the eleventh embodiment, the cleaning of the processing chamber 1 is not intended, but the cleaning of the processing chamber 1 is performed manually.
As for the end of cleaning, as in the tenth embodiment, a known cleaning end means, for example, monitoring of the emission spectrum intensity, setting of the cleaning time, detection of the opening degree of the on-off valve 9 or the like may be employed. it can.

  In the first to eleventh embodiments described above, the mass flow controllers 2a and 3a and the on-off valves 2b and 3b are provided in the cleaning gas supply paths 1 and 3. The supply amount of the cleaning gas may be adjusted and the supply path may be closed by a valve.

DESCRIPTION OF SYMBOLS 1 Processing chamber 2, 3 Supply path of cleaning gas 4, 5 Vacuum pump 6 Intake piping 6a Connection port with processing chamber in intake piping 6b Connection port with vacuum pump in intake piping 7 Device gate valve 8 Pressure control valve 9 Opening Adjustable on / off valve 9a Openable / closable valve 10 Exhaust gas passage 12a Mass flow controller 13 Monitoring room 13a Monitoring vacuum pump 14, 15, 16, 17, 18, 19 Plasma generator

Claims (10)

A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A method for cleaning a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, wherein a pressure control valve is provided in the vicinity of a connection port of the intake pipe with the processing chamber, and the vacuum pump is connected to the other end of the intake pipe. Because
An opening / closing valve whose opening degree can be adjusted is provided near the connection port with the vacuum pump in the intake pipe, the pressure control valve is fully opened, and the opening degree of the opening / closing valve is adjusted,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride in the treatment chamber An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas,
Cleaning the film forming apparatus or the crystal growing apparatus for performing processing under reduced pressure, by operating the vacuum pump and cleaning the processing chamber and the intake pipe while maintaining a pressure of 0.5 kPa to 80 kPa. Method. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A method for cleaning a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, wherein a pressure control valve is provided in the vicinity of a connection port of the intake pipe with the processing chamber, and the vacuum pump is connected to the other end of the intake pipe. Because
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride in the treatment chamber An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas,
Fully open the pressure control valve and adjust the number of rotations of the vacuum pump that can adjust the number of rotations, so that the processing chamber and the intake pipe are maintained at a pressure of 0.5 kPa to 80 kPa for cleaning. A cleaning method for a film forming apparatus or a crystal growing apparatus for performing processing under reduced pressure. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A method for cleaning a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, wherein a pressure control valve is provided in the vicinity of a connection port of the intake pipe with the processing chamber, and the vacuum pump is connected to the other end of the intake pipe. Because
An open / close valve that can be opened and closed in the vicinity of the connection port with the vacuum pump in the intake pipe, the pressure control valve is fully opened, the open / close valve is closed,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride in the treatment chamber An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas By supplying a mixed gas with an inert gas to the mixed halogen compound gas,
Mixing the interhalogen compound gas alone or the mixed interhalogen compound gas or the interhalogen compound gas alone and a gas inert to the gas alone at a pressure of 0.5 kPa to 80 kPa in the processing chamber and the intake pipe Forming a sealing process for holding a gas or a mixed gas of the mixed interhalogen gas and a gas inert to the mixed interhalogen gas for a predetermined time;
Opening the on-off valve and operating the vacuum pump to the inter-halogen compound gas alone or the mixed inter-halogen compound gas or the inter-halogen compound gas alone and the gas alone sealed in the processing chamber and the intake pipe Forming an exhaust process of exhausting a mixed gas with an inert gas or a mixed gas of the mixed interhalogen compound gas and a gas inert to the mixed interhalogen compound gas;
A cleaning method for a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, wherein the sealing step and the exhausting step are alternately performed a plurality of times to clean the inside of the processing chamber and the inside of the intake pipe. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A film forming apparatus or a crystal growth for performing processing under reduced pressure, in which an apparatus gate valve and a pressure control valve are provided in the vicinity of the connection port with the processing chamber in the intake pipe, and the vacuum pump is connected to the other end of the intake pipe An apparatus cleaning method comprising:
An opening / closing valve capable of adjusting the opening degree is provided near the connection port with the vacuum pump in the intake pipe, the device gate valve is closed, and the opening degree of the opening / closing valve is adjusted,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride for the intake pipe An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas A mixed gas with an inert gas is supplied to the mixed interhalogen gas, and the vacuum pump is operated to keep the intake pipe at a pressure of 0.5 kPa to 80 kPa for cleaning. A method for cleaning a film forming apparatus or a crystal growing apparatus that performs the processing under reduced pressure. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A film forming apparatus or a crystal growth for performing processing under reduced pressure, in which an apparatus gate valve and a pressure control valve are provided in the vicinity of the connection port with the processing chamber in the intake pipe, and the vacuum pump is connected to the other end of the intake pipe An apparatus cleaning method comprising:
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride for the intake pipe An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas While supplying a mixed gas with an inert gas to the mixed halogen compound gas,
By closing the device gate valve, fully opening the pressure control valve, and adjusting the rotation speed of the vacuum pump configured to be able to adjust the rotation speed, the pressure inside the intake pipe is maintained at a pressure of 0.5 kPa to 80 kPa. A method for cleaning a film forming apparatus or a crystal growing apparatus for performing processing under reduced pressure. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A film forming apparatus or a crystal growth for performing processing under reduced pressure, in which an apparatus gate valve and a pressure control valve are provided in the vicinity of the connection port with the processing chamber in the intake pipe, and the vacuum pump is connected to the other end of the intake pipe An apparatus cleaning method comprising:
An open / close valve that can be opened and closed in the vicinity of the connection port with the vacuum pump in the intake pipe, and closes the device gate valve and the open / close valve,
Halogen selected from the group consisting of chlorine fluoride, chlorine trifluoride, chlorine pentafluoride, bromine trifluoride, bromine pentafluoride, bromine monochloride, iodine pentafluoride and iodine heptafluoride for the intake pipe An intermetallic gas or a mixed interhalogen gas containing two or more interhalogen gases, or a mixed gas of the interhalogen gas and a gas inert to the gas, or the mixed interhalogen gas and the gas By supplying a mixed gas with an inert gas to the mixed halogen compound gas,
The interhalogen compound gas alone or the mixed interhalogen compound gas or the mixed gas of the interhalogen compound gas alone and a gas inert to the gas alone or the mixture at a pressure of 0.5 kPa to 80 kPa in the intake pipe Forming a sealing step for holding a state in which a mixed gas of an interhalogen compound gas and a gas inert to the mixed interhalogen gas is sealed for a predetermined time;
The interhalogen compound gas alone or the mixed interhalogen compound gas or the interhalogen compound gas alone and the gas inert to the gas alone, which opens the on-off valve and operates the vacuum pump and is sealed in the intake pipe. Or an exhaust process for exhausting a mixed gas of a mixed gas of the mixed interhalogen compound gas and a gas inert to the mixed interhalogen compound gas,
A cleaning method for a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, wherein the inside of the intake pipe is cleaned by alternately performing the sealing step and the exhausting step a plurality of times. The processing is performed under reduced pressure according to claim 3 or 6, wherein an end point of cleaning is detected by detecting a sealing pressure in the sealing step and comparing the detected value or a calculated value thereof with a set value. Cleaning method for film forming apparatus or crystal growing apparatus. A monitoring room for monitoring the intensity of the emission spectrum is provided, a monitoring vacuum pump is connected to the monitoring room, and a part of the exhaust gas at the outlet of the vacuum pump connected to the other end of the intake pipe is monitored via the mass flow controller. 6. The cleaning end point is detected by converting the exhaust gas guided to the chamber into plasma by a plasma generator and monitoring the intensity of the emission spectrum. A method for cleaning a film forming apparatus or a crystal growing apparatus that performs processing under reduced pressure. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for sucking gas from the processing chamber by a vacuum pump are connected, A cleaning method for a film forming apparatus or a crystal growth apparatus for performing processing under reduced pressure, in which a pressure control valve is provided in the vicinity of a connection port of the intake pipe with the processing chamber, and a vacuum pump is connected to the other end of the intake pipe. There,
An opening / closing valve whose opening degree can be adjusted is provided near the connection port of the vacuum pump in the intake pipe, the pressure control valve is fully opened, and the opening degree of the opening / closing valve is adjusted,
To the processing chamber, as a cleaning gas, the following mixed gas described in (1), (3), (4) or (5) or any single gas described in (2) below is supplied,
(1) fluorine,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(2) Nitrogen trifluoride simple substance or chlorine trifluoride simple substance
(3) nitrogen trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(4) chlorine trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(5) A mixed gas of dicarbon tetrafluoride, tricarbon octafluoride, sulfur hexafluoride or carbonyl fluoride and oxygen gas. Further, the cleaning gas is converted into plasma inside or outside the processing chamber by a plasma generator. In addition, by operating the vacuum pump, the processing chamber and the intake pipe are cleaned while being maintained at a pressure of 50 Pa to 1.1 kPa. Cleaning method. A supply path for supplying a gas for film formation or crystal growth to a processing chamber for film formation or crystal growth capable of depressurization and an intake pipe for exhausting gas from the processing chamber by a vacuum pump are connected, An apparatus gate valve and a pressure control valve are provided near the connection port of the processing chamber in the intake pipe, and a vacuum pump is connected to the other end side of the intake pipe. A cleaning method,
An opening / closing valve whose opening degree can be adjusted is provided near the connection port of the vacuum pump in the intake pipe, the device gate valve is closed, and the opening degree of the opening / closing valve is adjusted,
To the intake pipe, as a cleaning gas, supply any one of the mixed gas described in the following (1), (3), (4) or (5) or any single gas described in the following (2),
(1) fluorine,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(2) Nitrogen trifluoride simple substance or chlorine trifluoride simple substance
(3) nitrogen trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(4) chlorine trifluoride,
A mixed gas containing at least one gas selected from the group consisting of helium, argon, xenon and nitrogen gas
(5) A mixed gas of dicarbon tetrafluoride, tricarbon octafluoride, sulfur hexafluoride or carbonyl fluoride, and oxygen gas. Further, the cleaning gas is removed from the intake pipe or outside the intake pipe by a plasma generator. Cleaning the film-forming apparatus or the crystal-growing apparatus for performing processing under reduced pressure, wherein the inside of the intake pipe is maintained at a pressure of 50 Pa to 1.1 kPa by turning into a plasma and operating the vacuum pump Method.

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