Vapor phase growth method and vapor phase growth device

Abstract

The vapor phase growth method of the embodiment is a vapor phase growth method using a vapor phase growth device, wherein the vapor phase growth device has a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, a pressure regulating valve for adjusting the pressure of the reaction chamber, and an exhaust piping including a first portion and a second portion arranged between the reaction chamber and the pressure regulating valve, wherein a silicon carbide film is formed on the surface of the first substrate by introducing a first substrate into the reaction chamber, heating the first substrate in a manner to a predetermined temperature, supplying a process gas at a predetermined flow rate and controlling the pressure regulating valve to adjust the pressure of the reaction chamber to a predetermined pressure, while simultaneously depositing a byproduct containing carbon in at least either the first portion or the second portion, the first substrate is removed from the reaction chamber, the pressure of the exhaust piping is controlled, a gas containing a fluorine-containing gas is supplied to at least a portion of the exhaust piping to remove the byproducts, and then a second substrate is introduced into the reaction chamber to form a silicon carbide film on the surface of the second substrate.

Description

Technical Field

[0001] The present invention relates to a vapor phase growth method and a vapor phase growth apparatus for cleaning using a gas containing fluorine during vapor phase growth. Background Art

[0002] In a vapor phase growth device for forming a silicon carbide film, a process gas such as a raw material gas containing silicon (Si) and carbon (C) flows into a reaction chamber to form a silicon carbide film on the surface of a substrate. Exhaust gas including process gas not consumed in the reaction chamber and gas generated by reaction of the process gas is discharged from the reaction chamber to the outside of the device via an exhaust pipe, an exhaust pump, a detoxification device, etc.

[0003] When the exhaust gas passes through the exhaust pipe from the reaction chamber, it is cooled and condensed, and liquid or solid by-products are deposited on the inner surface of the exhaust pipe. There is a problem that these by-products may cause blockage of the exhaust pipe.

[0004] If the exhaust pipe is blocked, maintenance work of the vapor phase growth device becomes necessary, and the operating rate of the vapor phase growth device decreases. In addition, among the by-products derived from the exhaust gas, there are also substances that generate harmful gases and substances that are flammable, which sometimes bring dangers during maintenance work. Therefore, a cleaning method that can effectively remove the by-products accumulated in the exhaust pipe is required.

[0005] Prior art literature

[0006] Patent Literature

[0007] Patent Document 1: Japanese Patent Application Publication No. 2013-125810 Summary of the invention

[0008] Problems to be solved by the invention

[0009] The problem to be solved by the present invention is to provide a vapor phase growth method and a vapor phase growth apparatus for effectively removing by-products accumulated in an exhaust pipe.

[0010] Means for solving problems

[0011] A vapor phase growth method according to one embodiment of the present invention is a vapor phase growth method using a vapor phase growth apparatus, the vapor phase growth apparatus comprising a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, a pressure regulating valve for regulating the pressure in the reaction chamber, and an exhaust pipe including a first portion provided between the reaction chamber and the pressure regulating valve and a second portion provided between the pressure regulating valve and the exhaust pump, wherein a silicon carbide film is formed on a surface of the first substrate by introducing a first substrate into the reaction chamber, heating the first substrate to a predetermined temperature, supplying a process gas at a predetermined flow rate and controlling the pressure regulating valve to regulate the pressure in the reaction chamber to a predetermined pressure, while a byproduct containing carbon is deposited in at least one of the first portion and the second portion, the first substrate is removed from the reaction chamber, the pressure in the exhaust pipe is controlled, a gas containing a gas containing fluorine is supplied to at least a portion of the exhaust pipe to remove the byproduct, and after the byproduct is removed, a second substrate is introduced into the reaction chamber to form a silicon carbide film on the surface of the second substrate.

[0012] A vapor phase growth apparatus according to one embodiment of the present invention comprises a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, an exhaust pipe at least provided between the reaction chamber and the exhaust pump, and a mechanism for moving the surface of byproducts accumulated in the exhaust pipe.

[0013] A vapor phase growth apparatus according to another embodiment of the present invention comprises a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, an exhaust pipe at least disposed between the reaction chamber and the exhaust pump and including a storage portion for storing the by-products, and a heater for heating the storage portion.

[0014] Effects of the Invention

[0015] According to the present invention, it is possible to provide a vapor phase growth method and a vapor phase growth apparatus for effectively removing by-products deposited in an exhaust pipe. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram of an example of a vapor phase growth apparatus according to the first embodiment.

[0017] Figure 2 It is an explanatory diagram of the vapor phase growth method according to the first embodiment.

[0018] Figure 3 It is an explanatory diagram of the action and effect of the vapor phase growth method according to the first embodiment.

[0019] Figure 4 It is an explanatory diagram of a vapor phase growth method according to a modified example of the first embodiment.

[0020] Figure 5This is a schematic diagram of an example of a vapor phase growth apparatus according to the second embodiment.

[0021] Figure 6 It is an explanatory diagram of the vapor phase growth method according to the second embodiment.

[0022] Figure 7 It is an explanatory diagram of the operation and effect of the vapor phase growth method and the vapor phase growth apparatus according to the second embodiment.

[0023] Figure 8 This is a schematic diagram of an example of a vapor phase growth apparatus according to the third embodiment.

[0024] Fig. 9 It is an explanatory diagram of the vapor phase growth method according to the third embodiment.

[0025] Fig.10 This is a schematic diagram of an example of a vapor phase growth apparatus according to a fourth embodiment.

[0026] Fig.11 This is a schematic cross-sectional view of a portion of a vapor phase growth apparatus according to a fourth embodiment.

[0027] Fig.12 It is an explanatory diagram of the vapor phase growth method according to the fourth embodiment.

[0028] Fig.13 It is an explanatory diagram of the vapor phase growth method according to the fourth embodiment.

[0029] Fig.14 This is a schematic diagram of an example of a vapor phase growth apparatus according to the fifth embodiment.

[0030] Fig.15 It is an explanatory diagram of the vapor phase growth method according to the fifth embodiment.

[0031] Fig.16 This is a schematic diagram of an example of a vapor phase growth apparatus according to the fifth embodiment.

[0032] Fig.17 It is an explanatory diagram of the vapor phase growth method according to the sixth embodiment.

[0033] Fig.18 This is a schematic diagram of an example of a vapor phase growth apparatus according to the seventh embodiment.

[0034] Fig.19 It is an explanatory diagram of the vapor phase growth method according to the seventh embodiment.

[0035] Fig. 20 This is a schematic diagram of an example of a vapor phase growth apparatus according to the eighth embodiment.

[0036] Fig.21It is an explanatory diagram of the vapor phase growth method according to the eighth embodiment. DETAILED DESCRIPTION

[0037] Hereinafter, embodiments of the present invention will be described with reference to the drawings.

[0038] In this specification, the same or similar components may be denoted by the same reference numerals.

[0039] In this specification, the gravity direction when the vapor phase growth device is set to form a film is defined as "down", and the opposite direction is defined as "up". Therefore, the so-called "down" refers to the position in the gravity direction relative to the reference, and the so-called "below" refers to the gravity direction relative to the reference. In addition, the so-called "upper" refers to the position in the opposite direction of the gravity direction relative to the reference, and the so-called "above" refers to the opposite direction of the gravity direction relative to the reference. In addition, the so-called "longitudinal direction" is the gravity direction.

[0040] In this specification, the term "process gas" is a general term for gases used to form a film, and is a concept including, for example, source gas, assist gas, doping gas, carrier gas, and mixed gases thereof.

[0041] (First embodiment)

[0042] The vapor phase growth method of the first embodiment is a vapor phase growth method using a vapor phase growth apparatus having a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, a pressure regulating valve for adjusting the pressure in the reaction chamber, and an exhaust pipe including a first portion provided between the reaction chamber and the pressure regulating valve and a second portion provided between the pressure regulating valve and the exhaust pump. The method comprises: introducing a first substrate into the reaction chamber, heating the first substrate to a predetermined temperature, supplying a process gas at a predetermined flow rate, and controlling the pressure regulating valve to adjust the pressure in the reaction chamber to a predetermined pressure, thereby forming a silicon carbide film on the surface of the first substrate, and simultaneously depositing a byproduct containing carbon in at least one of the first portion and the second portion. The first substrate is removed from the reaction chamber, the pressure in the exhaust pipe is controlled, and a gas containing a gas containing fluorine is supplied to at least a portion of the exhaust pipe to remove the byproduct. After the byproduct is removed, a second substrate is introduced into the reaction chamber, thereby forming a silicon carbide film on the surface of the second substrate.

[0043] Figure 1 1 is a schematic diagram of an example of a vapor phase growth apparatus according to the first embodiment. The vapor phase growth apparatus according to an example of the first embodiment is a vapor phase growth apparatus 100 for forming a silicon carbide film. The vapor phase growth apparatus 100 according to the first embodiment is a vertical single-wafer epitaxial silicon carbide film vapor phase growth apparatus 100 that forms a film for each wafer.

[0044] The vapor phase growth apparatus 100 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, and a pressure control unit 28. The reaction chamber 10 includes a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24.

[0045] The reaction chamber 10 is made of, for example, stainless steel. The reaction chamber 10 has a cylindrical wall. A silicon carbide film is formed on the surface of a wafer W in the reaction chamber 10. The wafer W is an example of a substrate.

[0046] The gas supply port 10a is provided at the upper portion of the reaction chamber 10. The process gas is supplied into the reaction chamber 10 from the gas supply port 10a.

[0047] The process gas is, for example, a mixed gas containing a source gas of silicon (Si), a source gas of carbon (C), a doping gas of n-type impurities, and a carrier gas. The source gas of silicon is, for example, silane (SiH4). The source gas of carbon is, for example, propane (C3H8). The doping gas of n-type impurities is, for example, nitrogen. The carrier gas is, for example, hydrogen or argon. Furthermore, an auxiliary gas may be added for the purpose of achieving a high film formation rate by suppressing the clustering of silicon in the gas phase. The auxiliary gas is a gas containing chlorine, such as hydrogen chloride gas (HCl).

[0048] The wafer W can be placed on the susceptor 10b. The susceptor 10b may be provided with an opening at the center. The susceptor 10b is an example of a holder.

[0049] The heater 10c is provided below the susceptor 10b. The heater 10c heats the wafer W held on the susceptor 10b from below. The heater 10c is, for example, a resistance heater.

[0050] The gas exhaust port 10d is provided at the lower part of the reaction chamber 10. The exhaust gas is exhausted from the gas exhaust port 10d. The exhaust gas includes the process gas that is not consumed in the reaction chamber 10 and the gas generated by the reaction of the process gas.

[0051] Exhaust gas Figure 1As shown by the white arrow in FIG. 1 , the exhaust gas is exhausted to the outside of the vapor phase growth apparatus 100 via the first exhaust pipe 18, the pressure regulating valve 12, the second exhaust pipe 20, the exhaust pump 14, the third exhaust pipe 22, the detoxification device 16, and the fourth exhaust pipe 24. The exhaust gas is further exhausted to the outside of the building where the vapor phase growth apparatus 100 is installed, for example, via the exhaust duct 30. The outside of the exhaust duct 30 is at atmospheric pressure.

[0052] The first exhaust pipe 18 is provided between the reaction chamber 10 and the pressure regulating valve 12. The second exhaust pipe 20 is provided between the pressure regulating valve 12 and the exhaust pump 14. The third exhaust pipe 22 is provided between the exhaust pump 14 and the detoxification device 16. The fourth exhaust pipe 24 is provided between the detoxification device 16 and the exhaust duct 30.

[0053] Hereinafter, the pressure in the reaction chamber 10 is referred to as the 0th pressure P0, the pressure in the first exhaust pipe 18 is referred to as the first pressure P1, the pressure in the second exhaust pipe 20 is referred to as the second pressure P2, the pressure in the third exhaust pipe 22 is referred to as the third pressure P3, and the pressure in the fourth exhaust pipe 24 is referred to as the fourth pressure P4.

[0054] The exhaust pump 14 exhausts gas from the reaction chamber 10. The exhaust pump 14 reduces the pressure in the reaction chamber 10. The exhaust pump 14 is, for example, a vacuum pump.

[0055] The pressure regulating valve 12 regulates the pressure in the reaction chamber 10 to a desired pressure. The pressure regulating valve 12 regulates the first pressure P1 in the first exhaust pipe 18. The pressure regulating valve 12 is, for example, a throttle valve. The pressure regulating valve 12 may also be, for example, a butterfly valve.

[0056] The pressure control unit 28 controls, for example, the pressure regulating valve 12. For example, the opening of the pressure regulating valve 12 changes according to a command from the pressure control unit 28, thereby controlling the pressure in the reaction chamber 10 or the first pressure P1 in the first exhaust pipe 18.

[0057] The pressure P0 and the first pressure P1 of the reaction chamber 10 are measured by, for example, a pressure gauge (not shown). The pressure control unit 28 determines the opening of the pressure regulating valve 12 so that the pressure P0 or the first pressure P1 of the reaction chamber 10 becomes a desired pressure based on, for example, the measured result of the pressure P0 or the first pressure P1 of the reaction chamber 10. The pressure control unit 28 issues a command to the pressure regulating valve 12 so that the opening of the pressure regulating valve 12 becomes the determined opening.

[0058] The second pressure P2 is measured by, for example, a pressure gauge (not shown). For example, based on at least one of the measured pressure P0, the first pressure P1, and the second pressure P2 of the reaction chamber 10, the exhaust speed of the exhaust pump 14 is determined so that at least one of the pressure P0, the first pressure P1, and the second pressure P2 of the reaction chamber 10 becomes a desired pressure. The exhaust speed of the pump is controlled, for example, by the rotation speed of the rotor in the pump.

[0059] The detoxification device 16 is provided between the exhaust pump 14 and the exhaust pipe 30. The detoxification device 16 is, for example, a combustion-type detoxification device, or may be a dry-type (adsorption-type) detoxification device.

[0060] The detoxification device 16 renders the exhaust gas exhausted from the reaction chamber 10 harmless. The detoxified exhaust gas is exhausted to the outside of the vapor phase growth apparatus 100.

[0061] The cleaning gas supply pipe 26 is connected to the first exhaust pipe 18. The cleaning gas supply pipe 26 supplies the cleaning gas to the first exhaust pipe 18. The cleaning gas removes byproducts accumulated in the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22 when film formation in the reaction chamber 10 is not performed.

[0062] At this time, a purge gas such as nitrogen or argon is flowed from the gas supply port 10a into the reaction chamber 10 to prevent the cleaning gas from flowing into the reaction chamber 10. This is because even if the temperature of the pipe rises to about 180°C due to the exothermic reaction caused by the cleaning of the byproducts, the exhaust pipe mainly formed of metal will not be etched, but there are components such as the susceptor 10b and the heater 10c in the reaction chamber 10 that are easily etched by cleaning.

[0063] The cleaning gas may also be supplied from the gas supply port 10a to the first exhaust pipe 18 through the reaction chamber 10 when film formation is not being performed in the reaction chamber 10. In this case, in addition to the by-products accumulated in the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22, the by-products accumulated in the reaction chamber 10 are also removed. In this case, in order to prevent the susceptor 10b or the heater 10c in the reaction chamber 10, which are easily etched by cleaning, from being etched, it is necessary to control the flow rate of the etching gas, etc., so as to prevent the temperature in the reaction chamber 10 from rising to, for example, 100°C or more.

[0064] The cleaning gas includes a gas containing fluorine. The cleaning gas includes, for example, chlorine trifluoride (ClF3) gas and fluorine (F2). The cleaning gas may be, for example, a single gas of chlorine trifluoride gas or a mixed gas with other gases. The cleaning gas may be, for example, a mixed gas of chlorine trifluoride gas and nitrogen gas, or a mixed gas of chlorine trifluoride gas and argon gas.

[0065] The exhaust duct 30 is provided outside the vapor phase growth apparatus 100. The exhaust duct 30 is connected to the fourth exhaust pipe 24. Through the exhaust duct 30, the third pressure P3 in the third exhaust pipe 22 and the fourth pressure P4 in the fourth exhaust pipe 24 are maintained at atmospheric pressure or negative pressure relative to the atmospheric pressure.

[0066] Next, the vapor phase growth method according to the first embodiment will be described, taking the case of forming a silicon carbide film on a wafer W by epitaxial growth as an example.

[0067] It should be noted that the vapor phase growth method according to the first embodiment is a vapor phase growth method for cleaning by-products generated during the formation of a silicon carbide film.

[0068] First, a wafer W (first substrate) is loaded into the reaction chamber 10 and placed on the susceptor 10b. The wafer W is heated by the heater 10c. The wafer W is heated to a predetermined temperature. The wafer W is heated to 1600°C, for example.

[0069] A process gas at a predetermined flow rate is supplied from the gas supply port 10a to the reaction chamber 10. The process gas is, for example, a mixed gas of silane (SiH4), propane (C3H8), nitrogen, and hydrogen. Hydrogen chloride gas (HCl) may also be added.

[0070] While supplying the process gas into the reaction chamber 10, the pressure in the reaction chamber 10 is kept low using the exhaust pump 14. The reaction chamber 10 is set to a reduced pressure state. The pressure in the reaction chamber 10 is adjusted to a predetermined pressure such as 200 Torr using the pressure regulating valve 12.

[0071] The silicon carbide film is formed on the surface of the wafer W by epitaxial growth.

[0072] In the growth of silicon carbide film, the exhaust gas is as follows Figure 1 As shown by the white arrow in FIG. 1 , the exhaust gas is exhausted to the outside of the vapor phase growth apparatus 100 via the first exhaust pipe 18, the pressure regulating valve 12, the second exhaust pipe 20, the exhaust pump 14, the third exhaust pipe 22, the detoxification device 16, and the fourth exhaust pipe 24. The exhaust gas is further exhausted to the outside of the building where the vapor phase growth apparatus 100 is installed, for example, via the exhaust duct 30.

[0073] The exhaust gas includes process gas that is not consumed in the reaction chamber 10 and gas generated by the reaction of the process gas. The exhaust gas is cooled and condensed when passing through the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22 from the reaction chamber 10, so that liquid or solid byproducts are deposited on the inner surfaces of the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22.

[0074] A silicon carbide film is formed on the surface of the wafer W, and a byproduct containing carbon is deposited at least on the upstream side or the downstream side of the pressure regulating valve 12. A silicon carbide film is formed on the surface of the wafer W, and a byproduct containing carbon is deposited in at least one of the first exhaust pipe 18 and the second exhaust pipe 20.

[0075] The byproducts include, for example, polymer compounds containing silicon (Si) and hydrogen (H). In addition, chlorine (Cl) is sometimes contained. The polymer compounds containing silicon (Si) and hydrogen (H) are highly flammable substances. Furthermore, when chlorine (Cl) is contained, it is called oily silane, which is also a highly flammable substance.

[0076] After the silicon carbide film is formed on the surface of the wafer W, the wafer W is carried out to the outside of the reaction chamber 10 .

[0077] Figure 2 It is an explanatory diagram of the vapor phase growth method according to the first embodiment.

[0078] After the wafer W is carried out to the outside of the reaction chamber 10, a dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, a cleaning gas is supplied to the first exhaust pipe 18 from the cleaning gas supply pipe 26, and a purge gas is supplied to the first exhaust pipe 18 from the gas supply port 10a through the reaction chamber 10. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen, and its flow rate is, for example, 500 sccm for nitrogen and 100 sccm for chlorine trifluoride. In addition, the purge gas is, for example, nitrogen or argon, and its flow rate is, for example, 500 sccm.

[0079] While supplying the cleaning gas, the pressure in the reaction chamber 10, the first exhaust pipe 18, and the second exhaust pipe 20 is kept low using the exhaust pump 14. The reaction chamber 10, the first exhaust pipe 18, and the second exhaust pipe 20 are set to a reduced pressure state. The pressure in the reaction chamber 10 is, for example, 100 Torr, the first pressure P1 in the first exhaust pipe 18 is, for example, 10 Torr, and the second pressure P2 in the second exhaust pipe 20 is, for example, 1.0 Torr.

[0080] Alternatively, after the wafer W is carried out of the reaction chamber 10, a dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, a cleaning gas is supplied from the gas supply port 10a to the first exhaust pipe 18 via the reaction chamber 10. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen. The flow rate is, for example, 1 slm for nitrogen and 100 sccm for chlorine trifluoride.

[0081] While supplying the cleaning gas, the pressure in the reaction chamber 10, the first exhaust pipe 18, and the second exhaust pipe 20 is kept low using the exhaust pump 14. The reaction chamber 10, the first exhaust pipe 18, and the second exhaust pipe 20 are set to a reduced pressure state. The pressure in the reaction chamber 10 is, for example, 100 Torr, the first pressure P1 in the first exhaust pipe 18 is, for example, 50 Torr, and the second pressure P2 in the second exhaust pipe 20 is, for example, 1.5 Torr.

[0082] In addition, the pressure in the third exhaust pipe 22 and the fourth exhaust pipe 24 is maintained at atmospheric pressure or lower than atmospheric pressure by exhausting the exhaust pipe 30. The pressure in the third exhaust pipe 22 and the fourth exhaust pipe 24 is at atmospheric pressure or negative pressure relative to atmospheric pressure. The third pressure P3 in the third exhaust pipe 22 is, for example, 95% or more of atmospheric pressure.

[0083] Clean gas such as Figure 2 As shown by the black arrow in FIG. 1 , the clean gas is exhausted to the outside of the vapor phase growth apparatus 100 via the first exhaust pipe 18, the pressure regulating valve 12, the second exhaust pipe 20, the exhaust pump 14, the third exhaust pipe 22, the detoxification device 16, and the fourth exhaust pipe 24. The clean gas is further exhausted via the exhaust duct 30 to, for example, the outside of the building where the vapor phase growth apparatus 100 is installed.

[0084] When the pressure in the reaction chamber 10 is set to the 0th pressure P0, the pressure in the first exhaust pipe 18 is set to the first pressure P1, the pressure in the second exhaust pipe 20 is set to the second pressure P2, the pressure in the third exhaust pipe 22 is set to the third pressure P3, the pressure in the fourth exhaust pipe 24 is set to the fourth pressure P4, and the atmospheric pressure is set to the atmospheric pressure AP, the following relationship is maintained during cleaning using a cleaning gas.

[0085] P0>P1>P2

[0086] Furthermore, the first pressure P1 is controlled to be, for example, 10 Torr to 50 Torr, and the second pressure P2 is controlled to be, for example, 1 Torr to 5 Torr. These pressures are controlled by adjusting the opening of the pressure regulating valve 12 according to a command from the pressure control unit 28 .

[0087] At this time, for example, a pressure gauge (not shown) is used to measure the pressure P0 and the first pressure P1 of the reaction chamber 10. Based on the measured pressure P0 and the first pressure P1 of the reaction chamber 10, the opening of the pressure regulating valve 12 is adjusted.

[0088] The pressure control unit 28 determines the opening of the pressure regulating valve 12 so that the pressure P0 and the first pressure P1 of the reaction chamber 10 become desired pressures, based on the measured results of the pressure P0 and the first pressure P1 of the reaction chamber 10. The pressure control unit 28 issues a command to the pressure regulating valve 12 so that the opening of the pressure regulating valve 12 becomes the determined opening.

[0089] In addition, for example, a pressure gauge (not shown) is used to measure the pressure P0, the first pressure P1, and the second pressure P2 of the reaction chamber 10. Based on the measured pressure P0 and the first pressure P1 of the reaction chamber 10, the exhaust speed of the exhaust pump 14 is adjusted.

[0090] The exhaust speed of the exhaust pump 14 is based on the measured results of, for example, the pressure P0, the first pressure P1 and the second pressure P2 of the reaction chamber 10, and determines the rotation speed of, for example, the rotor in the exhaust pump so that the 0th pressure P0, the first pressure P1 and the second pressure P2 of the reaction chamber 10 become the specified pressures.

[0091] In addition, for example, the third pressure P3 is controlled to be 95% or more of the atmospheric pressure. By adjusting the exhaust volume in the exhaust duct 30, the third pressure P3 is controlled to be 95% or more of the atmospheric pressure AP.

[0092] The cleaning gas removes byproducts accumulated in the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22. When the cleaning gas is flowed in the reaction chamber 10, the byproducts in the reaction chamber 10 are also removed.

[0093] During the supply of the clean gas, the walls of the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22 generate heat due to the reaction between the clean gas and the byproducts, but the temperature thereof is maintained at, for example, 180° C. or less. During the supply of the clean gas, the walls of the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22 are not necessarily actively heated from the outside.

[0094] After the byproducts accumulated in the first exhaust pipe 18 , the second exhaust pipe 20 , and the third exhaust pipe 22 are removed by the cleaning gas, a wafer W (second substrate) is loaded into the reaction chamber 10 , and a silicon carbide film is formed on the surface of the wafer W.

[0095] Next, the operation and effects of the vapor phase growth method according to the first embodiment will be described.

[0096] In a vapor phase growth device for forming a silicon carbide film, a process gas such as a raw material gas containing silicon (Si) and carbon (C) flows into a reaction chamber to form a silicon carbide film on the surface of a substrate. Exhaust gas including process gas not consumed in the reaction chamber and gas generated by reaction of the process gas is discharged from the reaction chamber to the outside of the device via an exhaust pipe, an exhaust pump, a detoxification device, etc.

[0097] When the exhaust gas passes through the exhaust pipe from the reaction chamber, it is cooled and condensed, causing liquid and solid by-products to accumulate on the inner surface of the exhaust pipe. There is a problem that these by-products may cause blockage of the exhaust pipe.

[0098] If the exhaust pipe is blocked, maintenance work of the vapor phase growth device becomes necessary, and the operating rate of the vapor phase growth device decreases. In addition, among the by-products derived from the exhaust gas, there are also substances that generate harmful gases and flammable substances, which sometimes bring dangers during maintenance work. Therefore, a cleaning method that can effectively remove the by-products accumulated in the exhaust pipe is required.

[0099] For example, when epitaxially growing a silicon film on the surface of a substrate, a gas containing silane (SiH4) is sometimes used as a process gas. In this case, it is known that a highly flammable substance containing silicon (Si) and hydrogen (H), namely a polymer compound, is deposited as a byproduct in the exhaust pipe of the vapor phase growth device. Furthermore, it is known that when chlorine (Cl) is contained as a process gas, a polymer compound containing silicon (Si), hydrogen (H), and chlorine (Cl) is deposited as a byproduct. Furthermore, a polymer compound containing chlorine (Cl) is called an oily silane, which is also a highly flammable substance.

[0100] High molecular weight compounds containing silicon (Si), hydrogen (H), and chlorine (Cl) can be removed by chlorine trifluoride (ClF3) gas.

[0101] For example, when epitaxially growing a silicon carbide film on the surface of a substrate, a gas containing silane (SiH4) and chlorine (Cl) is sometimes used as a process gas. In this case, as in the case of the silicon film, a polymer compound containing silicon (Si) and hydrogen (H) is accumulated as a by-product in the exhaust piping of the vapor phase growth device. In addition, the process gas sometimes further contains chlorine (Cl). In this case, a polymer compound containing silicon (Si), hydrogen (H), and chlorine (Cl) is accumulated as a by-product in the exhaust piping of the vapor phase growth device.

[0102] Figure 3 It is an explanatory diagram of the action and effect of the vapor phase growth method according to the first embodiment.

[0103] The inventors compared the byproducts of epitaxially growing a silicon film with the byproducts of epitaxially growing a silicon carbide film, and found that the silicon carbide film contained a large amount of low molecular weight compounds with a mass number of 200 or less. It was also found that the low molecular weight compounds contained carbon. It is believed that the carbon is derived from the carbon source gas of the silicon carbide film, such as propane (C3H8).

[0104] Low molecular weight compounds containing carbon include, for example, CH4, C2H6, C3H8, CH3Cl, CH2Cl2, CHCl3, CCl4, C2H5Cl, C2H4Cl2, C2H3Cl3, C2H2Cl4, C2HCl5, C2Cl6, C2H4Cl, C2H3Cl, C2H2Cl, C2HCl, C3H7Cl, C3H6Cl, C3H5Cl, C3H4Cl, C3H3Cl, C3H2Cl, C3HCl, C3H, C3Cl, etc.

[0105] Furthermore, the inventors investigated the accumulation sites of byproducts when epitaxially growing a silicon carbide film, and found that Figure 3 As shown in FIG. 1 , a large amount of byproducts 40 are accumulated near the pressure regulating valve 12 in the first exhaust pipe 18 on the upstream side of the pressure regulating valve 12, near the pressure regulating valve 12 in the second exhaust pipe 20 on the downstream side of the pressure regulating valve 12, and in the third exhaust pipe 22 on the downstream side of the exhaust pump 14. For example, when a silicon film is epitaxially grown, the accumulation site of the byproducts is mainly a site in the first exhaust pipe 18 on the upstream side of the pressure regulating valve 12 that is away from the reaction chamber 10 and where the temperature does not rise during film formation.

[0106] When epitaxially growing a silicon carbide film, unlike when epitaxially growing a silicon film, the exhaust gas discharged from the reaction chamber contains carbon, which is an atom lighter than silicon. Therefore, the saturated vapor pressure of the exhaust gas increases, and even if it flows from the reaction chamber to the exhaust pipe at a high temperature, it is not easily liquefied or solidified. The difference in the accumulation position of the by-product is believed to be caused by the above difference.

[0107] The second pressure P2 in the second exhaust pipe 20 becomes lower than the first pressure P1 in the first exhaust pipe 18 because the flow path of the gas is narrowed by passing through the pressure regulating valve 12. Therefore, when the exhaust gas passes through the pressure regulating valve 12, the temperature drops at once due to adiabatic expansion. Therefore, it is considered that byproducts are formed on the downstream side of the pressure regulating valve 12.

[0108] It is believed that the by-products are generated near the pressure regulating valve 12 in the first exhaust pipe 18 on the upstream side of the pressure regulating valve 12 and near the pressure regulating valve 12 in the second exhaust pipe 20 on the downstream side of the pressure regulating valve 12 because the by-products generated in the pressure regulating valve 12 flow toward the upstream and downstream sides of the pressure regulating valve 12.

[0109] In the vapor phase growth method of the first embodiment, when supplying the cleaning gas, the first pressure P1 of the first exhaust pipe 18 on the upstream side of the pressure regulating valve 12 is controlled to be 1 Torr or more and 700 Torr or less.

[0110] That is, the first pressure P1 is maintained at a high pressure. By maintaining the first pressure P1 at a high pressure, the reaction between the clean gas and the byproduct 40 is promoted. Therefore, the byproduct 40 in the first exhaust pipe 18 on the upstream side of the pressure regulating valve 12 can be effectively removed.

[0111] From the viewpoint of effectively removing by-products in the first exhaust pipe 18 on the upstream side of the pressure regulating valve 12 , the first pressure P1 is preferably 10 Torr or more.

[0112] In the vapor phase growth method of the first embodiment, when supplying the cleaning gas, the second pressure P2 of the second exhaust pipe 20 on the downstream side of the pressure regulating valve 12 is controlled to be 0.1 Torr or more and 100 Torr or less.

[0113] That is, the second pressure P2 is maintained at a high pressure. By maintaining the second pressure P2 at a high pressure, the reaction between the clean gas and the byproduct 40 is promoted. Therefore, the byproduct 40 in the second exhaust pipe 20 on the downstream side of the pressure regulating valve 12 can be effectively removed.

[0114] From the viewpoint of effectively removing by-products in the second exhaust pipe 20 on the downstream side of the pressure regulating valve 12 , the pressure is preferably 1 Torr or more.

[0115] From the viewpoint of effectively removing by-products in the second exhaust pipe 20 on the downstream side of the pressure regulating valve 12, the second pressure P2 is preferably controlled to be 1% or more of the first pressure P1, more preferably to be 5% or more, and even more preferably to be 10% or more.

[0116] In addition, it is clarified that in the case of epitaxially growing a silicon carbide film, Figure 3 As shown in FIG. 1 , a considerable amount of byproducts 40 are also accumulated in the third exhaust pipe 22 between the exhaust pump 14 and the detoxification device 16. It is considered that the byproducts are seen in the third exhaust pipe 22 on the downstream side of the exhaust pump 14 because the exhaust gas is compressed inside the exhaust pump 16, and the byproducts are polymerized and polymerized, becoming easy to liquefy or solidify. In the vapor growth method of the first embodiment, for example, when supplying the cleaning gas, the third pressure P3 in the third exhaust pipe 22 is controlled to be 95% or more of the atmospheric pressure.

[0117] That is, the third pressure P3 is maintained at a relatively high pressure. By maintaining the third pressure P3 at a relatively high pressure, the reaction between the clean gas and the by-products is promoted. Therefore, the by-products 40 in the third exhaust pipe 22 can be effectively removed.

[0118] From the viewpoint of effectively removing by-products in the third exhaust pipe 22, the third pressure P3 in the third exhaust pipe 22 is preferably 98% or more of the atmospheric pressure, and more preferably 99% or more.

[0119] When supplying the cleaning gas, it is preferred to monitor the 0th pressure P0, the first pressure P1, and the second pressure P2 of the reaction chamber, and feed back the monitoring results to the opening of the pressure regulating valve 12 and the exhaust speed of the exhaust pump 14. The second pressure P2 is stable, and the by-products in the third exhaust pipe 22 can be stably removed.

[0120] During the supply of the clean gas, the temperature of the walls of the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22 is preferably maintained at or below 180° C. In addition, during the supply of the clean gas, the walls of the first exhaust pipe 18, the second exhaust pipe 20, and the third exhaust pipe 22 are preferably not heated from the outside.

[0121] Compared with high molecular weight compounds such as silicon (Si), hydrogen (H), and chlorine (Cl), low molecular weight compounds containing carbon have higher reactivity with gases containing fluorine, and generate more heat during the reaction. Therefore, compared with reaction byproducts such as high molecular weight compounds containing only silicon (Si), hydrogen (H), and chlorine (Cl), reaction byproducts containing low molecular weight compounds containing carbon can be removed at a low temperature, and cleaning can be performed effectively even if external heating is not necessarily performed.

[0122] The inventors investigated the gases exhausted during the cleaning process using chlorine trifluoride (ClF3) gas, and found that in addition to SiF4, SiF3, Cl2, Si2F6, and Si2F5 contained in the case of cleaning a reaction byproduct containing only a polymer compound containing silicon (Si), hydrogen (H), and chlorine (Cl), it also contained gases containing C, namely CF4, CF3Cl, CF2Cl2, CFCl3, CCl4, CHF3, CHF2Cl, CHFCl2, C2H5F, C2H4F2, C2H3F3, C2H2F4, C2H3F2, C2H2F, C2H2F3, C2H2F2, C2H2F, C3H7F, C3H6F2, C3H5F3, C3H5F, C3H5F2, C3H4F, C3H4F2, C4H9F, C4H8F2, C4H7F3, C4H6F4, C4H5F5, C4H8F, C4H7F2, C4H6F3, C4H5F4, C4H4F5, C4H7F, C4H6F2, C4H5F3, C4H4F4, C4H3F5, C4H6F, C4H5F2, C4H4F3, C5H3F2, C5H3F6, etc. These compounds are compounds generated as a result of the inclusion of a compound containing carbon (C) in the by-product 40. By generating such a compound containing both carbon and fluorine (F) during cleaning, the amount of heat generated by the chemical reaction during cleaning is increased, and effective cleaning can be performed even without heating from outside the pipe.

[0123] Figure 4 1 is an explanatory diagram of a vapor phase growth method according to a modification of the first embodiment. In the modification, a vapor phase growth apparatus having a cleaning gas supply pipe 32 connected to a third exhaust pipe 22 is used.

[0124] like Figure 4 As shown in FIG. 1 , a clean gas supply pipe 32 is provided relative to the third exhaust pipe 22, and a clean gas ( Figure 4 As a result, byproducts in the third exhaust pipe 22 between the exhaust pump 14 and the detoxification device 16 can also be effectively removed.

[0125] As described above, according to the vapor phase growth method of the first embodiment and the modified example, by-products deposited in the exhaust pipe during formation of the silicon carbide film can be effectively removed.

[0126] (Second embodiment)

[0127] The vapor phase growth method of the second embodiment is different from the vapor phase growth method of the first embodiment in that the surface of the byproduct is mobilized when the byproduct is removed. The vapor phase growth method of the second embodiment mobilizes the surface of the byproduct by vibrating the first part when the byproduct is removed. The vapor phase growth method of the second embodiment rapidly vibrates the pipe by knocking the first part from the outside to give an impact to the first part when the byproduct is removed. The first part is mobilized by giving an impact to the first part.

[0128] The vapor growth apparatus of the second embodiment includes a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, an exhaust pipe at least provided between the reaction chamber and the exhaust pump, and a mechanism for moving the surface of by-products accumulated in the exhaust pipe. The vapor growth apparatus of the second embodiment is different from the vapor growth apparatus of the first embodiment in that it includes a mechanism for moving the surface of by-products accumulated in the exhaust pipe. The mechanism for moving the surface of by-products accumulated in the exhaust pipe is a vibration excitation device for vibrating the exhaust pipe by knocking. The mechanism for moving the surface of by-products accumulated in the exhaust pipe is a vibration excitation device for moving the exhaust pipe by knocking.

[0129] Hereinafter, description of the contents overlapping with those of the first embodiment will be partially omitted.

[0130] Figure 5 Schematic diagram of an example of a vapor phase growth apparatus according to the second embodiment. The vapor phase growth apparatus according to an example of the second embodiment is a vapor phase growth apparatus 200 for forming a silicon carbide film. The vapor phase growth apparatus 200 according to the second embodiment is a vertical single-wafer epitaxial silicon carbide film vapor phase growth apparatus 200 that performs film formation for each wafer.

[0131] The vapor phase growth apparatus 200 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, a pressure control unit 28, and an excitation device 42. The reaction chamber 10 includes a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24.

[0132] The vibrator 42 has a function of externally striking the first exhaust pipe 18. The vibrator 42 strikes the first exhaust pipe 18 at a predetermined cycle and a predetermined load, for example. The vibrator 42 strikes the first exhaust pipe 18 from the outside using a hammer 42a included in the vibrator 42.

[0133] Figure 6 It is an explanatory diagram of the vapor phase growth method according to the second embodiment.

[0134] In the vapor phase growth method of the second embodiment, similarly to the vapor phase growth method of the first embodiment, after the wafer W is carried out of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied from the cleaning gas supply pipe 26 to the first exhaust pipe 18, and the purge gas is supplied from the gas supply port 10a through the reaction chamber 10 to the first exhaust pipe 18. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0135] In the vapor phase growth method of the second embodiment, while supplying the cleaning gas, the first exhaust pipe 18 is externally struck using the vibrator 42. The first exhaust pipe 18 is struck by the hammer 42a of the vibrator 42, for example, at a predetermined cycle and a predetermined load.

[0136] The first exhaust pipe 18 is moved by striking the first exhaust pipe 18 from the outside using the vibration device 42 while supplying the clean gas. By striking the first exhaust pipe 18 from the outside, for example, the first exhaust pipe 18 vibrates.

[0137] By striking the first exhaust pipe 18 from the outside using the vibration device 42, the surface of the byproduct 40 accumulated in the first exhaust pipe 18 moves. By striking the first exhaust pipe 18 from the outside using the vibration device 42, for example, the surface of the byproduct 40 vibrates.

[0138] In the vapor phase growth method of the second embodiment, the surface of the byproduct 40 accumulated in the first exhaust pipe 18 is moved by knocking the first exhaust pipe 18 from the outside using the vibration device 42 while supplying the cleaning gas. The reaction between the cleaning gas and the byproduct 40 is promoted by the surface movement of the byproduct 40 accumulated in the first exhaust pipe 18. Therefore, the byproduct 40 accumulated in the first exhaust pipe 18 can be effectively removed.

[0139] Figure 7 It is an explanatory diagram of the operation and effect of the vapor phase growth method and the vapor phase growth apparatus according to the second embodiment. Figure 7 FIG. 1 shows a time change in the exhaust pipe temperature in a state where a cleaning gas is supplied to the exhaust pipe of the vapor phase growth apparatus 200 .

[0140] like Figure 7 As shown in , when the supply of the clean gas to the exhaust pipe starts, the temperature of the exhaust pipe rises. The rise in the temperature of the exhaust pipe is caused by the generation of reaction heat between the clean gas and the by-products.

[0141] The temperature of the exhaust pipe rises and then falls. If the exhaust pipe is tapped, the temperature of the exhaust pipe rises again. If the temperature of the exhaust pipe falls again and the exhaust pipe is tapped again, the temperature of the exhaust pipe rises again.

[0142] Figure 7 The temperature change of the exhaust pipe observed in the process is described as follows. If the clean gas is supplied to the exhaust pipe, the clean gas reacts with the surface of the by-product, and the removal of the by-product begins. If the reaction between the clean gas and the surface of the by-product progresses, a film that hinders the reaction between the clean gas and the by-product is formed on the surface of the by-product. If a film is formed on the surface of the by-product, the reaction is suppressed and the generation of reaction heat is suppressed, and the temperature of the exhaust pipe decreases.

[0143] The film formed on the surface of the by-product is considered to be a substance having a carbon-carbon bond. The inventors have clarified the presence of a substance having a carbon-carbon bond in the residue of the by-product after cleaning through Raman spectroscopic analysis of the residue.

[0144] By knocking the exhaust pipe, the surface of the byproduct is activated. By knocking the exhaust pipe, the film on the surface of the byproduct is activated. The film on the surface of the byproduct is activated, and the film is cut off, and the byproduct is exposed between the films. The exposed byproduct reacts with the clean gas, and the temperature of the exhaust pipe rises.

[0145] If a film is formed again on the surface of the byproduct, the temperature of the exhaust pipe turns to decrease again. After that, each time the exhaust pipe is struck, the film is cut off, the byproduct is exposed between the films, and the exposed byproduct reacts with the clean gas, causing the temperature of the exhaust pipe to rise.

[0146] In the vapor phase growth method of the second embodiment, while supplying the cleaning gas, the first exhaust pipe 18 is knocked from the outside using the vibration device 42. By knocking the first exhaust pipe 18 from the outside, the first exhaust pipe 18 moves. By the movement of the first exhaust pipe 18, the surface of the by-product 40 accumulated in the first exhaust pipe 18 moves. By the surface movement of the by-product 40, even if a film is formed on the surface of the by-product, it is immediately cut off. Therefore, the reaction between the cleaning gas and the by-product 40 is promoted. Therefore, the by-product 40 can be effectively removed. It should be noted that as a method of applying vibration to the exhaust pipe, a method of knocking from the outside using a vibration device is described, but the vibration device is not particularly limited as long as vibration is applied. The vibration device can be any device that quickly moves the exhaust pipe by shaking or vibrating the exhaust pipe.

[0147] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the second embodiment, by-products deposited in the exhaust pipe during formation of the silicon carbide film can be effectively removed.

[0148] (Third embodiment)

[0149] The vapor phase growth method of the third embodiment is different from the vapor phase growth method of the second embodiment in that the storage portion provided in the first portion is knocked from the outside to vibrate the first portion when removing the by-products. In addition, the vapor phase growth apparatus of the third embodiment is different from the vapor phase growth apparatus of the second embodiment in that the exhaust pipe includes the storage portion and the vibration device knocks the storage portion.

[0150] Hereinafter, description of the contents overlapping with those of the second embodiment will be partially omitted.

[0151] Figure 8 1 is a schematic diagram of an example of a vapor phase growth apparatus according to Embodiment 3. The vapor phase growth apparatus according to an example of Embodiment 3 is a vapor phase growth apparatus 300 for forming a silicon carbide film.

[0152] The vapor phase growth device 300 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, a pressure control unit 28, and an excitation device 42. The reaction chamber 10 has a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24. The first exhaust pipe 18 includes a storage unit 18a.

[0153] The storage portion 18 a has a function of storing by-products accumulated in the first exhaust pipe 18 during the formation of the silicon carbide film.

[0154] The vibrator 42 has a function of externally striking the reservoir 18a of the first exhaust pipe 18. The vibrator 42 strikes the reservoir 18a at a predetermined cycle and a predetermined load, for example. The vibrator 42 strikes the reservoir 18a from the outside using a hammer 42a of the vibrator 42.

[0155] Fig. 9 It is an explanatory diagram of the vapor phase growth method according to the third embodiment.

[0156] In the vapor phase growth method of the third embodiment, similarly to the vapor phase growth method of the second embodiment, after the wafer W is carried out of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied to the first exhaust pipe 18 from the cleaning gas supply pipe 26, and the purge gas is supplied to the first exhaust pipe 18 from the gas supply port 10a through the reaction chamber 10. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0157] In the vapor phase growth method of the third embodiment, while supplying the cleaning gas, the reservoir 18a of the first exhaust pipe 18 is externally struck using the vibrator 42. The hammer 42a of the vibrator 42 strikes the reservoir 18a at a predetermined cycle and a predetermined load.

[0158] The reservoir 18a is moved by knocking the reservoir 18a from the outside using the vibration device 42 while supplying the clean gas. For example, the reservoir 18a is vibrated by knocking the reservoir 18a from the outside. For example, the reservoir 18a is moved by knocking the reservoir 18a from the outside.

[0159] The surface of the byproduct 40 accumulated in the reservoir 18a moves by striking the reservoir 18a from the outside using the vibration device 42 while supplying the clean gas. For example, the surface of the byproduct 40 accumulated in the reservoir 18a vibrates.

[0160] In the vapor phase growth method of the third embodiment, the surface of the byproduct 40 accumulated in the reservoir 18a is moved by knocking the reservoir 18a from the outside using the vibration device 42 while supplying the cleaning gas. Due to the surface movement of the byproduct 40, even if a film that inhibits the reaction between the cleaning gas and the byproduct 40 is formed on the surface of the byproduct 40, it is immediately blocked. Therefore, the reaction between the cleaning gas and the byproduct 40 is promoted. Therefore, the byproduct 40 can be effectively removed.

[0161] In order to improve the efficiency of accumulating the by-product 40, it is preferred that Figure 8 As shown in , the first exhaust pipe 18 is provided with an inclination toward the storage portion 18a. In order to improve the efficiency of storing the byproduct 40, it is preferable to provide a cooler (not shown) in the first exhaust pipe 18 near the storage portion 18a.

[0162] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the third embodiment, by-products deposited in the exhaust pipe during formation of the silicon carbide film can be effectively removed.

[0163] (Fourth embodiment)

[0164] The vapor phase growth method of the fourth embodiment is different from the vapor phase growth method of the third embodiment in that the first portion is shaken when removing the by-products. In addition, the vapor phase growth apparatus of the fourth embodiment is different from the vapor phase growth apparatus of the third embodiment in that the mechanism for moving the surface of the by-products accumulated in the exhaust pipe is a shaking device for shaking the exhaust pipe.

[0165] Hereinafter, description of the contents overlapping with the third embodiment will be partially omitted.

[0166] Fig.10 1 is a schematic diagram of an example of a vapor phase growth apparatus according to Embodiment 4. The vapor phase growth apparatus according to an example of Embodiment 4 is a vapor phase growth apparatus 400 for forming a silicon carbide film.

[0167] The vapor phase growth device 400 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, a pressure control unit 28, and a shaking device 44. The reaction chamber 10 has a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24. The first exhaust pipe 18 includes a storage unit 18a.

[0168] The storage portion 18 a has a function of storing by-products accumulated in the first exhaust pipe 18 during the formation of the silicon carbide film.

[0169] The shaking device 44 has a function of shaking the storage portion 18 a of the first exhaust pipe 18 .

[0170] Fig.11 This is a schematic cross-sectional view of a portion of a vapor phase growth apparatus according to a fourth embodiment. Fig.11 It is a schematic cross-sectional view of the first exhaust pipe 18 . Fig.11 (a) Yes Fig.10 AA' cross-section diagram. Fig.11 (b) Yes Fig.10 BB' cross section.

[0171] The oscillating device 44 uses, for example, a bidirectional rotary motor capable of switching the rotation direction as a driving source, and can oscillate the reservoir 18 a in the circumferential direction of the first exhaust pipe 18 .

[0172] Fig.12 , Fig.13 It is an explanatory diagram of the vapor phase growth method according to the fourth embodiment. Fig.13It is a schematic cross-sectional view of the first exhaust pipe 18 . Fig.13 yes Fig.12 AA' cross-section diagram.

[0173] In the vapor phase growth method of the fourth embodiment, similarly to the vapor phase growth method of the third embodiment, after the wafer W is carried out of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied from the cleaning gas supply pipe 26 to the first exhaust pipe 18, and the purge gas is supplied from the gas supply port 10a through the reaction chamber 10 to the first exhaust pipe 18. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0174] In the vapor phase growth method of the fourth embodiment, the reservoir 18a of the first exhaust pipe 18 is shaken by the shaking device 44 while supplying the cleaning gas. Fig.13 As shown in (b), the reservoir 18a is shaken in the circumferential direction of the first exhaust pipe 18 using the shaking device 44.

[0175] By shaking the storage part 18a using the shaking device 44, the surface of the byproduct 40 accumulated in the storage part 18a is mobilized. Due to the surface mobility of the byproduct 40 accumulated in the storage part 18a, even if a film that inhibits the reaction between the cleaning gas and the byproduct 40 is formed on the surface of the byproduct 40, it is immediately blocked. Therefore, the reaction between the cleaning gas and the byproduct 40 is promoted. Therefore, the byproduct 40 can be effectively removed.

[0176] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the fourth embodiment, by-products deposited in the exhaust pipe during the formation of the silicon carbide film can be effectively removed.

[0177] (Fifth embodiment)

[0178] The vapor phase growth method of the fifth embodiment is different from the vapor phase growth method of the third embodiment in that the surface of the by-products is mobilized by stirring the by-products when removing the by-products. In addition, the vapor phase growth apparatus of the fifth embodiment is different from the vapor phase growth apparatus of the third embodiment in that the mechanism for mobilizing the surface of the by-products accumulated in the exhaust pipe is a stirring device for stirring the by-products.

[0179] Hereinafter, description of the contents overlapping with the third embodiment will be partially omitted.

[0180] Fig.14 1 is a schematic diagram of an example of a vapor phase growth apparatus according to Embodiment 5. The vapor phase growth apparatus according to an example of Embodiment 5 is a vapor phase growth apparatus 500 for forming a silicon carbide film.

[0181] The vapor phase growth apparatus 500 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, a pressure control unit 28, and a stirring device 46. The reaction chamber 10 includes a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24. The first exhaust pipe 18 includes a storage unit 18a.

[0182] The storage portion 18 a has a function of storing by-products accumulated in the first exhaust pipe 18 during the formation of the silicon carbide film.

[0183] The stirring device 46 has a function of stirring the by-products accumulated in the storage portion 18a of the first exhaust pipe 18. The stirring device 46 is an electromagnetic stirrer having a stirring element 46a and a driving portion 46b.

[0184] The stirring element 46a includes a magnetic bar. The driving unit 46b includes a magnet and a motor for rotating the magnet. The stirring element 46a rotates due to the rotation of the magnet of the driving unit 46b.

[0185] Fig.15 It is an explanatory diagram of the vapor phase growth method according to the fifth embodiment.

[0186] In the vapor phase growth method of the fifth embodiment, similarly to the vapor phase growth method of the third embodiment, after the wafer W is carried out of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied from the cleaning gas supply pipe 26 to the first exhaust pipe 18, and the purge gas is supplied from the gas supply port 10a through the reaction chamber 10 to the first exhaust pipe 18. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0187] In the vapor phase growth method of the fifth embodiment, while supplying the cleaning gas, the byproduct 40 accumulated in the reservoir 18a is stirred using the stirring device 46. The stirring element 46a rotates due to the rotation of the magnet of the driving unit 46b, thereby stirring the byproduct 40 accumulated in the reservoir 18a.

[0188] In the vapor phase growth method of the fifth embodiment, the byproduct 40 accumulated in the reservoir 18a is stirred while supplying the cleaning gas, so that the surface of the byproduct 40 is mobilized. Due to the surface mobility of the byproduct 40 accumulated in the reservoir 18a, even if a film that inhibits the reaction between the cleaning gas and the byproduct 40 is formed on the surface of the byproduct 40, it is immediately blocked. Therefore, the reaction between the cleaning gas and the byproduct 40 is promoted. Therefore, the byproduct 40 can be effectively removed.

[0189] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the fifth embodiment, by-products deposited in the exhaust pipe during the formation of the silicon carbide film can be effectively removed.

[0190] (Sixth embodiment)

[0191] The vapor phase growth apparatus of the sixth embodiment is different from the vapor phase growth apparatus of the fifth embodiment in that the configuration of a stirring device is different.

[0192] Hereinafter, description of contents overlapping with the fifth embodiment will be partially omitted.

[0193] Fig.16 1 is a schematic diagram of an example of a vapor phase growth apparatus according to Embodiment 6. The vapor phase growth apparatus according to an example of Embodiment 6 is a vapor phase growth apparatus 600 for forming a silicon carbide film.

[0194] The stirring device 46 has a function of stirring the by-products accumulated in the storage portion 18a of the first exhaust pipe 18. The stirring device 46 has a stirring element 46a, a driving portion 46b, and a rotating shaft 46c.

[0195] The stirring element 46a is fixed to the rotating shaft 46c. The driving unit 46b has a motor for rotating the rotating shaft 46c. The stirring element 46a rotates when the rotating shaft 46c is rotated by the driving unit 46b.

[0196] Fig.17 It is an explanatory diagram of the vapor phase growth method according to the sixth embodiment.

[0197] In the vapor phase growth method of the sixth embodiment, similarly to the vapor phase growth method of the fifth embodiment, after the wafer W is carried out of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied from the cleaning gas supply pipe 26 to the first exhaust pipe 18, and the purge gas is supplied from the gas supply port 10a through the reaction chamber 10 to the first exhaust pipe 18. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0198] In the vapor phase growth method of the sixth embodiment, the byproduct 40 accumulated in the reservoir 18a is stirred by the stirring device 46 while supplying the cleaning gas. The stirring element 46a is rotated by the driving unit 46b, thereby stirring the byproduct 40 accumulated in the reservoir 18a.

[0199] In the vapor phase growth method of the sixth embodiment, the byproduct 40 accumulated in the reservoir 18a is stirred while supplying the cleaning gas, so that the surface of the byproduct 40 is mobilized. Due to the surface mobility of the byproduct 40 accumulated in the reservoir 18a, even if a film that inhibits the reaction between the cleaning gas and the byproduct 40 is formed on the surface of the byproduct 40, it is immediately blocked. Therefore, the reaction between the cleaning gas and the byproduct 40 is promoted. Therefore, the byproduct 40 can be effectively removed.

[0200] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the sixth embodiment, by-products deposited in the exhaust pipe during formation of the silicon carbide film can be effectively removed.

[0201] (Seventh Implementation Method)

[0202] The vapor phase growth method of the seventh embodiment is different from the vapor phase growth method of the third embodiment in that the storage portion is heated when removing the by-products.

[0203] In addition, the vapor phase growth apparatus of the seventh embodiment includes a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, an exhaust pipe provided between the reaction chamber and the exhaust pump and including a storage portion for storing by-products, and a heater for heating the storage portion.

[0204] Hereinafter, description of the contents overlapping with the third embodiment will be partially omitted.

[0205] Fig.18 1 is a schematic diagram of an example of a vapor phase growth apparatus according to Embodiment 7. The vapor phase growth apparatus according to an example of Embodiment 7 is a vapor phase growth apparatus 700 for forming a silicon carbide film.

[0206] The vapor phase growth device 700 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, a pressure control unit 28, a heater 48, a first cooler 50a, and a second cooler 50b. The reaction chamber 10 has a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24. The first exhaust pipe 18 includes a storage unit 18a.

[0207] The storage portion 18 a has a function of storing by-products accumulated in the first exhaust pipe 18 during the formation of the silicon carbide film.

[0208] The heater 48 is provided, for example, so as to surround the storage portion 18a. The heater 48 has a function of heating the storage portion 18a. The heater 48 can heat the storage portion 18a to a temperature of, for example, 150° C. or higher and 300° C. or lower. The temperature of the storage portion 18a can be measured, for example, by a thermometer provided outside the storage portion 18a.

[0209] The first cooler 50a is provided in the first exhaust pipe 18 on the side of the reaction chamber 10 of the storage part 18a. The second cooler 50b is provided in the first exhaust pipe 18 on the side of the exhaust pump 14 of the storage part 18a.

[0210] The first cooler 50a and the second cooler 50b have a function of cooling the first exhaust pipe 18 on the upstream side and the downstream side of the storage portion 18a. The first cooler 50a and the second cooler 50b are, for example, water-cooled coolers.

[0211] Fig.19 It is an explanatory diagram of the vapor phase growth method according to the seventh embodiment.

[0212] In the vapor phase growth method of the seventh embodiment, similarly to the vapor phase growth method of the third embodiment, after the wafer W is carried out of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied to the first exhaust pipe 18 from the cleaning gas supply pipe 26, and the purge gas is supplied to the first exhaust pipe 18 from the gas supply port 10a through the reaction chamber 10. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0213] While supplying the cleaning gas, the storage portion 18a is heated by the heater 48. By heating the storage portion 18a, the byproduct 40 accumulated in the storage portion 18a is heated.

[0214] In addition, while supplying the clean gas, the first exhaust pipe 18 on the upstream side and the downstream side of the storage portion 18 a is cooled using the first cooler 50 a and the second cooler 50 b .

[0215] In the vapor phase growth method of the seventh embodiment, the reaction between the cleaning gas and the byproduct 40 is promoted by heating the byproduct 40 while supplying the cleaning gas. Therefore, the byproduct 40 can be effectively removed. In particular, when a substance having a carbon-carbon bond is generated, it is difficult to remove it at a low temperature, and raising the temperature is effective in removing the byproduct 40.

[0216] In the vapor growth method of the seventh embodiment, the first exhaust pipe 18 on the upstream and downstream sides of the storage portion 18a is cooled using the first cooler 50a and the second cooler 50b while supplying the cleaning gas. By cooling the storage portion 18a, which has reached a high temperature due to heating by the heater 48, components with low heat resistance such as those provided in the exhaust pipe can be protected.

[0217] From the viewpoint of promoting the reaction between the clean gas and the byproduct 40, the temperature of the storage portion 18a is preferably set to 150°C or higher, more preferably 200°C or higher, and further preferably 250°C or higher. From the viewpoint of protecting components with low heat resistance, the temperature of the storage portion 18a is preferably set to 300°C or lower.

[0218] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the seventh embodiment, by-products deposited in the exhaust pipe during formation of the silicon carbide film can be effectively removed.

[0219] (Eighth Implementation Method)

[0220] The vapor phase growth method of the eighth embodiment is different from the vapor phase growth method of the second embodiment in that the storage unit is removed after the by-products are removed and before the second substrate is loaded into the reaction chamber, and the by-products remaining in the storage unit are removed using a chemical solution.

[0221] Furthermore, the vapor phase growth apparatus of the eighth embodiment is different from the vapor phase growth apparatus of the second embodiment in that the storage portion can be removed from the first portion.

[0222] Hereinafter, description of the contents overlapping with those of the second embodiment will be partially omitted.

[0223] Fig. 20 1 is a schematic diagram of an example of a vapor phase growth apparatus according to Embodiment 8. The vapor phase growth apparatus according to an example of Embodiment 8 is a vapor phase growth apparatus 800 for forming a silicon carbide film.

[0224] The vapor phase growth apparatus 800 includes a reaction chamber 10, a pressure regulating valve 12, an exhaust pump 14, a detoxification device 16, a first exhaust pipe 18 (first part), a second exhaust pipe 20 (second part), a third exhaust pipe 22 (third part), a fourth exhaust pipe 24, a cleaning gas supply pipe 26, and a pressure control unit 28. The reaction chamber 10 includes a gas supply port 10a, a susceptor 10b, a heater 10c, and a gas exhaust port 10d. An exhaust pipe 30 is connected to the fourth exhaust pipe 24. The exhaust pipe includes the first exhaust pipe 18, the second exhaust pipe 20, the third exhaust pipe 22, and the fourth exhaust pipe 24. The first exhaust pipe 18 includes a storage unit 18a.

[0225] The storage portion 18a has a function of storing byproducts accumulated in the first exhaust pipe 18 during the formation of the silicon carbide film. The storage portion 18a can be removed from the first exhaust pipe 18.

[0226] Fig.21 It is an explanatory diagram of the vapor phase growth method according to the eighth embodiment.

[0227] In the vapor phase growth method of the eighth embodiment, similarly to the vapor phase growth method of the second embodiment, after the wafer W (first substrate) is carried out to the outside of the reaction chamber 10, the dummy wafer DW is carried into the reaction chamber 10 and placed on the susceptor 10b. Next, the cleaning gas is supplied to the first exhaust pipe 18 from the cleaning gas supply pipe 26, and the purge gas is supplied to the first exhaust pipe 18 from the gas supply port 10a through the reaction chamber 10. The cleaning gas is, for example, chlorine trifluoride (ClF3) gas diluted with nitrogen.

[0228] After the byproducts 40 are removed by supplying the cleaning gas, the reservoir 18a is removed from the first exhaust pipe 18 before the wafer W (second substrate) is loaded into the reaction chamber 10. Then, the byproducts 40 remaining in the reservoir 18a are removed using a chemical solution.

[0229] The chemical liquid is, for example, an acidic solution, such as hydrofluoric acid or nitric acid.

[0230] Thereafter, the storage portion 18 a is installed in the first exhaust pipe 18 , and the wafer W (second substrate) is loaded into the reaction chamber 10 .

[0231] In the vapor phase growth method of the eighth embodiment, by using a chemical solution to remove the byproduct 40 remaining in the reservoir 18a, the byproduct 40 can be effectively removed. In particular, when a substance having a carbon-carbon bond is generated, it is difficult to remove it with a cleaning gas, and it is effective to remove it with a chemical solution.

[0232] As described above, according to the vapor phase growth method and the vapor phase growth apparatus of the eighth embodiment, by-products deposited in the exhaust pipe during formation of the silicon carbide film can be effectively removed.

[0233] In the first to eighth embodiments and variations, a vertical single-wafer epitaxial device that forms a film on each wafer is used as an example for description, but the vapor phase growth device is not limited to a single-wafer epitaxial device. For example, a planetary CVD device that simultaneously forms a film on a plurality of rotating and revolving wafers, a horizontal epitaxial device, etc. can also be applied to the present invention.

[0234] In the first to eighth embodiments and modifications, the case where a source gas of silicon (Si) and a source gas of carbon (C) are mixed and supplied to the reaction chamber 10 from one gas supply port 10a during the formation of a silicon carbide film is described as an example, but for example, the source gas of silicon (Si) and the source gas of carbon (C) may be supplied to the reaction chamber 10 from different gas supply ports 10a.

[0235] The cleaning of the vapor phase growth apparatus in the first to eighth embodiments and the modified examples does not need to be performed every time a silicon carbide film is formed. For example, the vapor phase growth apparatus may be cleaned after silicon carbide films are formed on a plurality of substrates.

[0236] In the second to fourth embodiments, the form in which the first exhaust pipe 18 (first part) is vibrated is used as an example for explanation, but it can also be set to a form in which the second exhaust pipe 20 (second part) is vibrated, or a form in which both the first exhaust pipe 18 (first part) and the second exhaust pipe 20 (second part) are vibrated.

[0237] In the second to eighth embodiments, the first exhaust pipe 18 (first part) is described as an example in which the storage portion 18a is included. However, it may also be configured such that the second exhaust pipe 20 (second part) includes a storage portion, or both the first exhaust pipe 18 (first part) and the second exhaust pipe 20 (second part) include a storage portion.

[0238] In the first to eighth embodiments and variations, descriptions of parts of the present invention that do not require direct description, such as device configurations or growth methods, are omitted, but necessary device configurations or growth methods, etc. can be appropriately selected and used. In addition, all vapor phase growth methods and vapor phase growth devices that have the elements of the present invention and can be appropriately designed and modified by those skilled in the art are included in the scope of the present invention. The scope of the present invention is defined by the scope of the claims and their equivalents.

[0239] Explanation of symbols

[0240] 10. Reaction Chamber

[0241] 10a Gas supply port

[0242] 10b Base

[0243] 10c Heater

[0244] 10d Gas exhaust port

[0245] 12 Pressure regulating valve

[0246] 14 Exhaust pump

[0247] 16 Pest control device

[0248] 18 1st exhaust pipe (Part 1)

[0249] 18a Storage

[0250] 20 2nd exhaust pipe (Part 2)

[0251] 22 3rd exhaust pipe (Part 3)

[0252] 24 4th exhaust pipe

[0253] 26 Clean gas supply pipe

[0254] 28 Pressure Control Department

[0255] 30 Exhaust duct

[0256] 40 Byproducts

[0257] 42 Vibration device

[0258] 42a Hammering part

[0259] 44 Shaking device

[0260] 46. ​​Stirring device

[0261] 46a Stirring bar

[0262] 46b Drive unit

[0263] 46c Rotation axis

[0264] 48 Heater

[0265] 50a 1st cooler

[0266] 50b Second cooler

[0267] 100 Vapor Growth Device

[0268] 200 Vapor Growth Device

[0269] 300 Vapor Growth Device

[0270] 400 Vapor Growth Device

[0271] 500 Vapor Growth Device

[0272] 600 Vapor Growth Device

[0273] 700 Vapor Growth Device

[0274] 800 Vapor Growth Device

[0275] AP atmospheric pressure

[0276] P0 Pressure in the reaction chamber

[0277] P1 1st pressure

[0278] P2 2nd pressure

[0279] P3 3rd Pressure

[0280] P4 4th Pressure

[0281] W wafer (first substrate, second substrate)

[0282] DW Fake Wafer

Claims

1. A vapor phase growth method using a vapor phase growth apparatus, the vapor phase growth apparatus comprising a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, a pressure regulating valve for adjusting the pressure in the reaction chamber, and an exhaust pipe including a first portion provided between the reaction chamber and the pressure regulating valve and a second portion provided between the pressure regulating valve and the exhaust pump, A silicon carbide film is formed on the surface of the first substrate by placing the first substrate into the reaction chamber, heating the first substrate to a predetermined temperature, supplying a process gas at a predetermined flow rate, and controlling the pressure regulating valve to adjust the pressure in the reaction chamber to a predetermined pressure, thereby depositing a byproduct containing carbon on at least the second portion. carrying the first substrate out of the reaction chamber, The pressure in the second portion is controlled to be 0.1 Torr or more and 100 Torr or less, and a gas including a fluorine-containing gas is supplied to at least the second portion to remove the by-product. After removing the byproducts, a second substrate is placed in the reaction chamber, and a silicon carbide film is formed on a surface of the second substrate. When removing the byproducts, the surface of the byproducts is mobilized so that the film formed on the surface of the byproducts is cut off and the byproducts are exposed.

2. The vapor phase growth method according to claim 1, wherein: The fluorine-containing gas is chlorine trifluoride.

3. The vapor phase growth method according to claim 1, wherein: The exhaust pipe has a harm removal device and a third portion disposed between the exhaust pump and the harm removal device. When the gas including the fluorine-containing gas is supplied, the pressure in the third portion is controlled so as to be 95% or more of the atmospheric pressure and to be a negative pressure with respect to the atmospheric pressure.

4. The vapor phase growth method according to claim 1, wherein: When the gas including the fluorine-containing gas is supplied, the opening degree of the pressure regulating valve is adjusted based on the pressure in the first portion.

5. The vapor phase growth method according to claim 1, wherein: The process gas contains chlorine.

6. The vapor phase growth method according to claim 1, wherein: By vibrating at least one of the first part and the second part, the surface of the byproduct is mobilized.

7. The vapor phase growth method according to claim 6, wherein: By applying an impact from the outside to at least one of the first portion and the second portion, at least the second portion is vibrated.

8. The vapor phase growth method according to claim 1, wherein: By stirring the by-product, the surface of the by-product is activated.

9. The vapor phase growth method according to claim 1, wherein: At least one of the first part and the second part includes a storage portion for storing the by-product, and the storage portion is heated when removing the by-product.

10. The vapor phase growth method according to claim 9, wherein: At least one of the first part and the second part is heated to 150° C. or higher.

11. The vapor phase growth method according to claim 9, wherein: The exhaust pipe on the reaction chamber side of the storage section and the exhaust pipe on the exhaust pump side of the storage section are cooled.

12. The vapor phase growth method according to claim 1, wherein: At least one of the first part and the second part includes a storage portion for storing the by-product. After the by-products are removed and before the second substrate is loaded into the reaction chamber, the reservoir is removed, and the by-products remaining in the reservoir are removed using a chemical solution.

13. A vapor phase growth method, which is a vapor phase growth method using a vapor phase growth device, the vapor phase growth device comprising a reaction chamber, an exhaust pump for exhausting gas from the reaction chamber, a harm removal device for removing harm from the gas exhausted from the exhaust pump, a pressure regulating valve for adjusting the pressure in the reaction chamber, and an exhaust pipe including a first portion provided between the reaction chamber and the pressure regulating valve, a second portion provided between the pressure regulating valve and the exhaust pump, and a third portion provided between the exhaust pump and the harm removal device, A silicon carbide film is formed on the surface of the first substrate by placing the first substrate into the reaction chamber, heating the first substrate to a predetermined temperature, supplying a process gas at a predetermined flow rate, and controlling the pressure regulating valve to adjust the pressure in the reaction chamber to a predetermined pressure, thereby depositing a byproduct containing carbon on at least the third portion. carrying the first substrate out of the reaction chamber, The pressure in the third portion is controlled to be 95% or more of the atmospheric pressure and negative pressure relative to the atmospheric pressure, and a gas containing a fluorine-containing gas is supplied to at least the third portion to remove the by-product. After removing the byproducts, a second substrate is placed in the reaction chamber, and a silicon carbide film is formed on a surface of the second substrate. When removing the byproducts, the surface of the byproducts is mobilized so that the film formed on the surface of the byproducts is cut off and the byproducts are exposed.

14. The vapor phase growth method according to claim 13, wherein: The vapor phase growth device further comprises a cleaning gas supply pipe connected to the third part, The gas including the fluorine-containing gas is supplied to the third portion from the cleaning gas supply pipe.

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