JP2019121629A - Vapor growth device and vapor growth system - Google Patents

Abstract

To provide a vapor growth device capable of improving utilization efficiency of material gas.SOLUTION: A vapor growth device 1 forms a substance on a substrate S by causing chemical reaction of multiple different material gases Gn. The vapor growth device 1 includes a chamber 3, a holding part 5, and a heating part 7. The holding part 5 is placed in the chamber 3, and holds the substrate S. The heating part 7 heats the substrate S. The chamber 3 includes at least one material introduction port GPn for introducing the material gases Gn into the chamber 3. In a partial or all period when the substance is formed on a substrate S, outflow of the material gases Gn from the inside to the outside of the chamber 3 is blocked.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a vapor phase growth apparatus and a vapor phase growth system that cause chemical reactions of a plurality of different source gases to form a substance on a substrate.

  Patent Document 1 describes a nitride semiconductor crystal production apparatus. The nitride semiconductor crystal manufacturing apparatus includes a first reaction tube and a second reaction tube, and executes a first process, a second process, and a third process. The first reaction tube and the second reaction tube are connected. The first step is performed in a first zone in the first reaction tube, and the second step is performed in a second zone in the first reaction tube. The third step is carried out in the third zone in the second reaction tube. Temperature control is performed in each of the first zone, the second zone and the third zone.

  In the first step, metal gallium and chlorine gas are reacted to generate gallium monochloride gas. In the second step, gallium monochloride gas and chlorine gas are reacted to produce gallium trichloride gas. In the third step, gallium trichloride gas and ammonia gas are used as source gases, and a nitride semiconductor crystal containing gallium is grown on the substrate by vapor phase growth.

International Publication No. 2011/142402

  However, in the nitride semiconductor crystal manufacturing apparatus described in Patent Document 1, the source gas (chlorine gas, gallium monochloride gas, gallium trichloride gas, and ammonia gas) is supplied from the supply port of the reaction tube while being discharged. By discharging from the outlet, a nitride semiconductor crystal is grown while the source gas is always circulated. Therefore, since a large amount of source gas is discharged without being used, the utilization efficiency of the source gas is low.

  The present invention has been made in view of the above problems, and an object thereof is to provide a vapor phase growth apparatus and a vapor phase growth system capable of improving the utilization efficiency of a source gas.

  According to a first aspect of the present invention, a vapor deposition apparatus causes a chemical reaction of a plurality of different source gases to form a substance on a substrate. The vapor deposition apparatus includes a chamber, a holding unit, and a heating unit. A holder is disposed inside the chamber to hold the substrate. The heating unit heats the substrate. The chamber includes at least one source introduction port for introducing the source gas into the chamber. During part or all of the period in which the substance is formed on the substrate, the flow of the source gas from the inside to the outside of the chamber is blocked.

  Preferably, the vapor deposition apparatus of the present invention further comprises a byproduct exhaust part. The by-product exhaust unit preferably exhausts by-products generated by a chemical reaction of the plurality of source gases from the inside to the outside of the chamber.

  The vapor deposition apparatus of the present invention preferably further comprises a by-product detection unit. Preferably, the by-product detection unit detects the concentration of the by-product inside the chamber. The by-product exhaust unit preferably exhausts the by-product according to the concentration of the by-product.

  In the vapor phase growth apparatus according to the present invention, preferably, the source gas is replenished from the source introduction port in accordance with a reduction amount of the source gas caused by a chemical reaction inside the chamber. It is preferable that the source gas be replenished so that the mole fraction of each of the source gas is maintained constant in the chamber when the source gas is replenished.

  In the vapor phase growth apparatus of the present invention, it is preferable that a predetermined amount be determined for each of the source gases. Preferably, after the predetermined amount of the source gas is introduced into the chamber, the flow path of the source gas is shut off to stop the introduction of the source gas from the source introduction port. It is preferable that the raw material gas be replenished from the raw material introduction port in accordance with a reduction amount of the raw material gas caused by a chemical reaction inside the chamber. It is preferable that the source gas be replenished so that the mole fraction of each of the source gas is maintained constant in the chamber when the source gas is replenished.

  In the vapor phase growth apparatus of the present invention, it is preferable that a predetermined amount be determined for each of the source gases. After the predetermined amount of the raw material gas is introduced into the chamber, the raw material gas is constantly replenished from the raw material introduction port according to the amount of reduction of the raw material gas due to a chemical reaction inside the chamber. Is preferred. It is preferable that the source gas be constantly replenished so that the mole fraction of each of the source gas is maintained constant inside the chamber when the source gas is constantly replenished.

  In the vapor phase growth apparatus of the present invention, the chamber preferably includes a plurality of the material introduction ports. Each of the plurality of raw material introduction ports preferably introduces the plurality of raw material gases into the chamber.

  In the vapor phase growth apparatus of the present invention, it is preferable that the raw material introduction port introduce a mixed gas in which the plurality of raw material gases are mixed into the chamber.

  In the vapor deposition apparatus according to the present invention, preferably, the chamber further includes a carrier introduction port for introducing a carrier gas into the chamber.

  In the vapor deposition apparatus of the present invention, the chamber preferably further includes an etching introduction port for introducing an etching gas into the chamber.

  Preferably, the vapor deposition apparatus of the present invention further comprises a wall having an opening. Preferably, the wall portion is disposed between the holding portion in which the heating portion is disposed and an inner wall surface of the chamber. The opening preferably exposes the substrate.

  According to a second aspect of the present invention, a vapor deposition system includes the vapor deposition apparatus according to the first aspect, and a gas supply apparatus for supplying a gas to the vapor deposition apparatus. The gas supply device includes a raw material container, a dilution container, and an introduction unit. The source container accommodates the source gas. The dilution container mixes the raw material gas introduced from the raw material container with a carrier gas for diluting the raw material gas, and stores it as a diluted raw material gas. The introducing unit introduces the source gas and the carrier gas into the dilution container at different timings, and releases the diluted source gas from the dilution container after the source gas and the carrier gas are mixed.

  According to the present invention, the utilization efficiency of the source gas can be improved.

It is a figure showing a vapor phase growth system concerning Embodiment 1 of the present invention. FIG. 1 is a view showing a gas supply device according to a first embodiment. FIG. 2 is a view showing a part of the gas supply device according to the first embodiment. FIG. 1 is a view showing a part of a vapor phase growth system according to a first embodiment. FIG. 7 is a view showing a part of a gas supply device according to a first modification of the first embodiment. FIG. 7 is a view showing a part of a gas supply device according to a second modified example of the first embodiment. It is a figure which shows the vapor phase growth system which concerns on Embodiment 2 of this invention. FIG. 7 is a view showing a gas supply device according to a second embodiment. FIG. 7 is a view showing a part of a gas supply device according to a second embodiment. FIG. 7 is a view showing a part of a vapor phase growth system according to a second embodiment. FIG. 10 is a view showing a part of a gas supply device according to a modification of the second embodiment.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. In the drawings, the same or corresponding portions are denoted by the same reference characters and description thereof will not be repeated.

(Embodiment 1)
FIG. 1 is a view showing a vapor phase growth system 100 according to a first embodiment of the present invention. As shown in FIG. 1, the vapor deposition system 100 includes a vapor deposition apparatus 1, a gas supply apparatus 60, and a residue discharge apparatus 80. In FIG. 1, a cross section of a part of the vapor phase growth apparatus 1 is shown for the convenience of understanding. Cross sections are hatched.

  The vapor deposition apparatus 1 includes a chamber 3. Then, the vapor deposition apparatus 1 executes a chemical vapor deposition method inside the chamber 3 to grow a substance on the substrate S, and describes the substance on the substrate S (hereinafter, “target substance”). Form). That is, the vapor deposition apparatus 1 causes a chemical reaction of a plurality of different source gases Gn inside the chamber 3 to form the target substance on the substrate S. The target substance is, for example, a III-V compound semiconductor. The target substance is, for example, a solid. The source gas Gn is a gas that forms a target substance by a chemical reaction. That is, the source gas Gn is a gas that produces a target substance by a chemical reaction. In addition, when distinguishing and demonstrating the several source gas Gn, it describes as source gas G1, ..., GN (N is an integer greater than or equal to 2). For example, when N = 2, the source gas G1 is a compound containing a Group III (Group 13) element, and the source gas G2 is a compound containing a Group V (Group 15) element.

  In the vapor phase growth apparatus 1, the source gas from the inside to the outside of the chamber 3 in part or all of a period RP (hereinafter referred to as “reaction period RP”) in which the target substance is formed on the substrate S Shut off the outflow of Gn. Therefore, the chamber 3 is sealed in part or all of the reaction period RP. That is, the vapor phase growth apparatus 1 causes a plurality of different source gases Gn to stay in the chamber 3 to cause a chemical reaction, thereby forming the target substance on the substrate S.

  As a result, according to the first embodiment, as compared with the case where the source gas is circulated to form the target substance as in the manufacturing apparatus described in Patent Document 1 (hereinafter referred to as “prior art”). The utilization efficiency of the source gas Gn can be improved. The utilization efficiency of the source gas Gn is the ratio of the amount of the reaction source gas to the amount of the source gas Gn introduced into the chamber 3. The reactive raw material gas is a raw material gas Gn which causes a chemical reaction in the raw material gas Gn and contributes to the formation of the target substance. "Quantity" indicates, for example, the amount of substance (mol), mass, or volume.

  Further, in the first embodiment, the vapor phase growth apparatus 1 can be miniaturized as compared with the prior art, and hence the cost of the vapor phase growth apparatus 1 can be reduced. In the prior art, in order to circulate the source gas, a relatively long reaction tube having a plurality of zones is required, which makes it difficult to miniaturize the manufacturing apparatus.

  Further, in the first embodiment, since it is sufficient to control the temperature of the substrate S by the heating unit 7, temperature control is easily performed as compared with the case where the temperature is controlled for each zone in the reaction tube as in the prior art. it can.

  Furthermore, in the first embodiment, when a plurality of different source gases Gn are introduced and retained inside the chamber 3 to form the target substance, when the source gas Gn is introduced into the inside of the chamber 3 compared to the prior art. Is easy to control. In the prior art, since the target substance is formed by circulating the source gas in a plurality of zones in the reaction tube and performing a plurality of steps, control of causing the source gas to flow in the reaction tube is complicated.

  Furthermore, in the first embodiment, since the plurality of different source gases Gn are retained inside the chamber 3 to form the target substance, the growth rate of the target substance is affected by the structure of the chamber 3 as compared with the prior art. hard. In the prior art, since the target substance is formed by a relatively long reaction tube having a plurality of zones, the growth rate of the target substance is susceptible to the structure of the reaction tube.

  Furthermore, in the first embodiment, a plurality of different source gases Gn are introduced into and retained in the chamber 3 to form the target substance, so that the source gases are circulated to perform a plurality of steps as in the prior art. In comparison, the amount of residue and the amount of by-products can be reduced. Therefore, it is easy to process residue discharge and by-product discharge.

  The vapor deposition apparatus 1 preferably blocks the flow of the source gas Gn from the inside to the outside of the chamber 3 during the entire reaction period RP. Moreover, it is preferable that the vapor phase growth apparatus 1 shuts off the outflow of the plurality of source gases Gn from the inside to the outside of the chamber 3 in a part or all of the reaction period RP. Furthermore, it is more preferable that the vapor deposition apparatus 1 shuts off the outflow of the plurality of source gases Gn from the inside to the outside of the chamber 3 during the entire reaction period RP. The vapor deposition apparatus 1 may block the flow of a single source gas Gn among the plurality of source gases Gn.

  Specifically, in addition to the chamber 3, the vapor deposition apparatus 1 further includes the holding unit 5, the heating unit 7, the plurality of wall units 8, the temperature control unit 9, the power supply line 11, and the byproduct detection unit 13. The by-product exhaust unit 15, the cooling unit 17, the plurality of raw material introduction pipes An, the carrier introduction pipe 19, the etching introduction pipe 21, the power supply lead-out pipe 23, the residue discharge pipe 25, the by-product exhaust pipe And 27. In addition, when distinguishing and demonstrating several raw material introduction pipe | tube An, it describes as raw material introduction pipe A1, ..., AN (N is an integer greater than or equal to 2).

  The chamber 3 is a reactor and has an internal space SP. The chamber 3 has, for example, a hollow substantially cylindrical shape, but the shape of the chamber 3 is not particularly limited. The chamber 3 includes a plurality of raw material introduction ports GPn, a carrier introduction port CP, an etching introduction port EP, a residue discharge port ZP, and a byproduct exhaust port FP. The chamber 3 is formed of, for example, quartz. When the plurality of raw material introduction ports GPn are described separately, they are described as raw material introduction ports GP1, ..., GPN (N is an integer of 2 or more). Further, the chamber 3 has a pair of windows WD facing each other. The window WD is formed of a transparent member and is provided in the chamber 3 in an airtight state.

  The plurality of raw material introduction ports GPn are respectively arranged corresponding to the plurality of raw material introduction pipes An. The raw material introduction port GPn is airtightly connected to the corresponding raw material introduction pipe An. The plurality of raw material introduction pipes An respectively supply a plurality of different raw material gases Gn. Therefore, the plurality of raw material introduction ports GPn respectively introduce a plurality of different raw material gases Gn into the chamber 3.

  As a result, according to the first embodiment, the plurality of source gases Gn can be introduced into the chamber 3 from the plurality of source containers prepared respectively for the plurality of source gases Gn. In particular, since the procedure for mixing the plurality of source gases Gn into the chamber 3 in advance can be reduced, the procedure before introducing the plurality of source gases Gn into the chamber 3 can be simplified.

  Carrier introduction port CP is arranged corresponding to carrier introduction pipe 19. The carrier introduction port CP is connected to the carrier introduction pipe 19 in an airtight state. Then, the carrier introduction pipe 19 supplies the carrier gas CG. Accordingly, the carrier introduction port CP introduces the carrier gas CG into the chamber 3. The carrier gas CG is, for example, an inert gas. The inert gas is, for example, nitrogen gas. According to the first embodiment, since the carrier gas CG is introduced into the chamber 3, the plurality of source gases Gn in the chamber 3 can be uniformly mixed.

  The etching introduction port EP is disposed corresponding to the etching introduction pipe 21. The etching introduction port EP is airtightly connected to the etching introduction pipe 21. Then, the etching introduction pipe 21 supplies the etching gas EG. Therefore, the etching introduction port EP introduces the etching gas EG into the chamber 3. The etching gas EG is, for example, a halogen gas. According to the first embodiment, since the etching gas EG is introduced into the chamber 3, the inner wall of the chamber 3, the surface of the holding unit 5, the surface of the substrate S, and the surface of the target material grown on the substrate S can be cleaned. .

  The residue discharge port ZP discharges the residue ZG inside the chamber 3 to the outside of the chamber 3. The residue ZG is, for example, a gas, a liquid, and / or a solid, and is a substance remaining in the chamber 3 after the formation of the target substance on the substrate S is completed. Specifically, the residue discharge port ZP is disposed corresponding to the residue discharge pipe 25. The residue discharge port ZP is connected to the residue discharge pipe 25 in an airtight manner. Then, the residue discharge port ZP discharges the residue ZG from the inside of the chamber 3 to the outside through the residue discharge pipe 25.

  The byproduct exhaust port FP exhausts the byproduct FG inside the chamber 3 to the outside of the chamber 3. The by-product FG is, for example, a gas, and is a substance produced by causing a plurality of source gases Gn to undergo a chemical reaction, and is different from the target substance. The by-product FG is, for example, a gas that inhibits the growth of a target substance. The gas that inhibits the growth of the target substance is, for example, a gas that etches the substance, and is hydrogen chloride that is produced when gallium trichloride gas and ammonia gas are chemically reacted to form gallium nitride.

  Specifically, the by-product exhaust port FP is disposed corresponding to the by-product exhaust pipe 27. The by-product exhaust port FP is airtightly connected to the by-product exhaust pipe 27. Then, the by-product exhaust port FP exhausts the by-product FG from the inside of the chamber 3 to the outside through the by-product exhaust pipe 27.

  The power supply line drawing pipe 23 is connected to the chamber 3 in an airtight state. On the other hand, the power supply line 11 is connected to the heating unit 7. Then, the power supply line 11 is drawn from the inside of the chamber 3 to the outside through the power supply line drawing pipe 23.

  The holder 5 is disposed inside the chamber 3. In the first embodiment, the holding unit 5 is installed on the inner bottom surface 4 a of the chamber 3. The holding unit 5 holds the substrate S. Specifically, the holder 5 has a holding surface HS. Then, the substrate S is installed on the holding surface HS. The holding unit 5 is, for example, a susceptor. The susceptor is formed of, for example, silicon carbide. The substrate S is, for example, a seed substrate. The seed substrate is, for example, a seed crystal substrate. The substrate S is, for example, a sapphire substrate.

  The heating unit 7 is disposed inside the chamber 3. The heating unit 7 is disposed in the holding unit 5 so as to face the holding surface HS. In the first embodiment, the heating unit 7 is fixed to the holding unit 5. Then, the heating unit 7 heats the holding unit 5. That is, the heating unit 7 heats the substrate S through the holding unit 5. The heating unit 7 is, for example, a heater. The heating unit 7 may heat the holding unit 5 by induction heating.

  One end of a power supply line 11 is connected to the heating unit 7. Therefore, the power supply voltage and the power supply current are supplied from the temperature control unit 9 to the heating unit 7 through the power supply line 11. Specifically, the temperature control unit 9 includes a power supply 9a. Then, the other end of the power supply line 11 is connected to the power supply 9a. Therefore, the power supply voltage and the power supply current are supplied to the heating unit 7 from the power supply 9a.

  The temperature control unit 9 controls the heating unit 7 by controlling the power supply voltage or the power supply current supplied to the heating unit 7. Specifically, the temperature control unit 9 controls the heating unit 7 to control the temperature of the holding unit 5. More specifically, the temperature control unit 9 controls the heating unit 7 to control the temperature of the substrate S via the holding unit 5. Then, the temperature control unit 9 controls the heating unit 7 to hold the temperature of the substrate S at a predetermined temperature via the holding unit 5. The temperature control unit 9 includes a processor and a storage device. Thus, the processor controls the heating unit 7 by executing the computer program stored in the storage device.

  The vapor deposition apparatus 1 may include a temperature sensor (eg, a thermistor). The temperature sensor is fixed to the holder 5 (for example, the holding surface HS). The temperature sensor detects the temperature of the holding unit 5. The thermal conductivity of the holder 5 is high, and in the thermal equilibrium state, the temperature of the holder 5 is equal to the temperature of the substrate S. Therefore, the temperature control unit 9 receives a signal indicating the temperature of the holding unit 5 from the temperature sensor, and monitors the temperature of the substrate S. The temperature control unit 9 controls the heating unit 7 while monitoring the temperature of the substrate S to maintain the temperature of the substrate S at a predetermined temperature. The temperature sensor may directly detect the temperature of the substrate S.

  Each of the wall portions 8 is disposed between the holding portion 5 in which the heating portion 7 is disposed and the inner wall surface 4 b of the chamber 3. Each of the walls 8 has an opening 10 for exposing the substrate S. In the first embodiment, the opening 10 exposes the substrate S toward the inner top surface 4 c of the chamber 3. Each of the walls 8 has, for example, a substantially cylindrical shape. The material of the wall 8 is, for example, carbon, boron nitride, or quartz. The heights of the plurality of walls 8 with respect to the inner bottom surface 4a may be different or the same. The height of the wall 8 with respect to the inner bottom surface 4 a is preferably higher than the height of the holding portion 5 with respect to the inner bottom surface 4 a. Adjacent walls 8 are spaced apart. The wall portion 8 surrounds the side surface of the holding portion 5. Specifically, the innermost wall portion 8 a among the plurality of wall portions 8 surrounds the side surface of the holding portion 5 at an interval. The outermost wall 8 b of the plurality of walls 8 faces the inner wall 4 b of the chamber 3 at an interval. Note that the number of wall portions 8 is not limited to two, and may be three or more. Also, one wall 8 may be provided.

  According to the first embodiment, since the wall portion 8 is provided, direct transfer of heat from the heating unit 7, the holding unit 5, and the substrate S to the chamber 3 can be suppressed. As a result, it can suppress that the chamber 3 becomes high temperature, and the durability of the chamber 3 can be improved. Further, since the wall portion 8 is provided, the heat flow from the substrate S and the holding portion 5 can be suppressed, and the temperature of the substrate S can be kept constant with higher accuracy.

  The cooling unit 17 cools the chamber 3. Specifically, the cooling unit 17 cools the chamber 3 by circulating the cooling liquid WT (for example, cooling water) in the chamber 3. As a result, according to Embodiment 1, the influence of heat from the heating unit 7, the holding unit 5, and the substrate S can be reduced, and the durability of the chamber 3 can be further improved.

  The gas supply device 60 is connected to the plurality of raw material introduction pipes An. Then, the gas supply device 60 supplies the source gas Gn to the chamber 3 through the source introduction pipe An and the source introduction port GPn.

  Then, after supplying the source gas Gn of the first predetermined amount M1 (predetermined amount) to the chamber 3, the gas supply device 60 shuts off the flow path of the source gas Gn, and supplies the source gas Gn to the chamber 3 Stop. In other words, after the source gas Gn of the first predetermined amount M1 is introduced into the chamber 3, the flow path of the source gas Gn is blocked, and the introduction of the source gas Gn from the source introduction pipe An and the source introduction port GPn It is stopped.

  Therefore, according to the first embodiment, the source gas Gn can be further suppressed from flowing out of the chamber 3. As a result, the utilization efficiency of the source gas Gn can be further improved.

  The first predetermined amount M1 indicates, for example, the amount of substance (mol), mass, or volume. The first predetermined amount M1 is determined for each source gas Gn based on a chemical reaction formula when a plurality of different source gases Gn chemically react. That is, the first predetermined amount M1 is determined for each source gas Gn so that the mole fraction of each source gas Gn is maintained constant inside the chamber 3. In the present specification, a chemical reaction formula indicates a chemical reaction formula for producing a target substance.

  Therefore, according to the first embodiment, excess and deficiency of the plurality of source gases Gn can be suppressed, and an appropriate amount of source gases Gn can be introduced into the chamber 3. As a result, waste of the source gas Gn can be suppressed. The mole fraction of the source gas Gn indicates the ratio of the amount of the source gas Gn to the total amount of the plurality of source gases Gn.

  Further, the gas supply device 60 supplements the source gas Gn to the chamber 3 through the source introduction pipe An and the source introduction port GPn according to the decrease amount of the source gas Gn resulting from the chemical reaction inside the chamber 3.

  Therefore, according to the first embodiment, a situation in which the source gas Gn runs short can be avoided, so that growth defects of the target material can be suppressed.

  Further, when replenishing the source gas Gn, the gas supply device 60 supplements the source gas Gn such that the mole fraction of each of the source gas Gn is maintained constant inside the chamber 3.

  Therefore, according to the first embodiment, the excess and deficiency of the plurality of source gases Gn can be further suppressed, and an appropriate amount of the source gases Gn can be further introduced into the chamber 3. As a result, waste of the source gas Gn can be further suppressed.

  Specifically, the gas supply device 60 supplies the source gas Gn of the second predetermined amount M2 to the chamber 3 in accordance with the amount of decrease of the source gas Gn inside the chamber 3.

  The second predetermined amount M2 indicates, for example, a substance amount (mol), a mass, or a volume. The second predetermined amount M2 is preferably equal to, for example, the amount of reduction of the source gas Gn. In addition, the second predetermined amount M2 is determined for each source gas Gn based on a chemical reaction formula when a plurality of different source gases Gn chemically react. That is, the second predetermined amount M2 is determined for each source gas Gn such that the mole fraction of each source gas Gn is maintained constant inside the chamber 3.

  Then, after the source gas Gn of the second predetermined amount M2 is replenished, the gas supply device 60 shuts off the flow path of the source gas G, and enters the chamber 3 through the source introduction pipe An and the source introduction port GPn. The replenishment of the source gas Gn is stopped.

  Therefore, according to the first embodiment, the source gas Gn can be further suppressed from flowing out of the chamber 3. As a result, the utilization efficiency of the source gas Gn can be further improved.

  Note that the gas supply device 60 receives the raw material introduction pipe An and the raw material introduction pipe An in accordance with the amount of reduction of the raw material gas Gn resulting from the chemical reaction inside the chamber 3 after the raw material gas Gn of the first predetermined amount M1 is supplied. The source gas Gn may be constantly replenished through the source introduction port GPn. In this case, the source gas Gn is constantly maintained at a constant amount inside the chamber 3 by constantly replenishing the source gas Gn by an amount corresponding to the decrease of the source gas Gn. Therefore, the growth of the target substance can be controlled with high precision. Moreover, while the source gas Gn is replenished, the source gas Gn does not flow out of the chamber 3, so that the utilization efficiency of the source gas Gn can be improved.

  For example, when the amount of the raw material gas Gn in the chamber 3 becomes smaller than the threshold value Th1, the gas supply device 60 uses the raw material gas Gn as a raw material introduction port according to the amount of reduction of the raw material gas Gn in the chamber 3 You may always replenish from GPn. The threshold value Th1 is preferably set to, for example, the same value as the first predetermined amount M1. In this case, the source gas Gn can be held at the first predetermined amount M1 inside the chamber 3. As a result, the growth of the target substance can be accurately controlled.

  Also, for example, when constantly replenishing the source gas Gn, the gas supply device 60 always replenishes the source gas Gn such that the mole fraction of each of the source gas Gn is maintained constant inside the chamber 3. It is also good. In this case, excess and deficiency of the plurality of source gases Gn can be suppressed, and an appropriate amount of source gases Gn can be introduced into the chamber 3. As a result, waste of the source gas Gn can be suppressed.

  Further, the gas supply device 60 is connected to the carrier introduction pipe 19. Then, the gas supply device 60 supplies the carrier gas CG to the chamber 3 through the carrier introduction pipe 19 and the carrier introduction port CP.

  Specifically, after supplying the carrier gas CG of the third predetermined amount M3 to the chamber 3, the gas supply device 60 shuts off the flow path of the carrier gas CG, and stops the supply of the carrier gas CG to the chamber 3. Do.

  Therefore, according to the first embodiment, the source gas Gn can be prevented from flowing out of the carrier introduction pipe 19 to the outside of the chamber 3. As a result, the utilization efficiency of the source gas Gn can be further improved.

  The third predetermined amount M3 indicates, for example, a substance amount (mol), a mass, or a volume. Note that the gas supply device 60 may replenish a certain amount of carrier gas CG through the carrier introduction pipe 19 and the carrier introduction port CP according to the amount of decrease of the carrier gas CG inside the chamber 3. The fixed amount is preferably equal to, for example, the reduction amount of the carrier gas CG. Further, the gas supply device 60 may always replenish the carrier gas CG when constantly replenishing the source gas Gn.

  Further, the gas supply device 60 is connected to the etching introduction pipe 21. Then, the gas supply device 60 supplies the etching gas EG to the chamber 3 through the etching introduction pipe 21 and the etching introduction port EP.

  Specifically, after supplying the etching gas EG of the fourth predetermined amount M4 to the chamber 3, the gas supply device 60 shuts off the flow path of the etching gas EG and stops the supply of the etching gas EG to the chamber 3 Do.

  Therefore, according to the first embodiment, the source gas Gn can be suppressed from flowing out of the etching introduction pipe 21 to the outside of the chamber 3. As a result, the utilization efficiency of the source gas Gn can be further improved.

  The fourth predetermined amount M4 indicates, for example, the amount of substance (mol), mass, or volume. The gas supply device 60 may replenish a certain amount of etching gas EG through the etching introduction pipe 21 and the etching introduction port EP according to the amount of decrease of the etching gas EG inside the chamber 3. The fixed amount is preferably equal to, for example, the reduction amount of the etching gas EG. In addition, the gas supply device 60 may always replenish the etching gas EG when constantly replenishing the source gas Gn.

  The residue discharging device 80 is connected to the residue discharging pipe 25. Then, after the formation of the target substance on the substrate S is completed, the residue discharge device 80 discharges the residue ZG from the inside of the chamber 3 to the outside through the residue discharge pipe 25 and the residue discharge port ZP. As a result, according to the first embodiment, the inside of the chamber 3 can be effectively cleaned.

  Specifically, the residue discharge device 80 has one or more valves and a vacuum pump. Then, the residue discharge device 80 closes the valve and closes the residue discharge pipe 25 in the reaction period RP, and the gas from the inside of the chamber 3 to the outside (the source gas Gn, the carrier gas CG, the etching gas, and the byproducts) Block the outflow of FG). Therefore, according to the first embodiment, it is possible to suppress the source gas Gn from flowing out of the residue discharge pipe 25 to the outside of the chamber 3 in the reaction period RP. As a result, the utilization efficiency of the source gas Gn can be further improved.

  Then, after the formation of the target substance on the substrate S is completed, the residue discharge device 80 drives the vacuum pump and opens the valve to open the residue discharge pipe 25 to discharge the residue ZG. The residue discharging device 80 includes a processor and a storage device. Thus, the processor controls the valve and the vacuum pump by executing a computer program stored in the storage device.

  The by-product detection unit 13 detects the concentration of the by-product FG in the chamber 3. Specifically, the by-product detection unit 13 applies light to the gas (the source gas Gn, the carrier gas CG, the etching gas, and the by-product FG) existing in the inner space SP through one window WD of the pair of windows WD. Irradiate. Then, the by-product detection unit 13 detects the light transmitted through the gas present in the internal space SP and emitted from the other window WD. Furthermore, the by-product detection unit 13 processes and analyzes the detected light to calculate the concentration of the by-product FG. The by-product detection unit 13 includes, for example, a Fourier transform infrared spectrometer (FT-IR).

  The by-product exhaust unit 15 is connected to the by-product exhaust pipe 27. Then, the by-product exhaust unit 15 exhausts the by-product FG from the inside of the chamber 3 to the outside through the by-product exhaust port FP and the by-product exhaust pipe 27.

  According to the first embodiment, since the by-product FG is exhausted, the growth rate of the target material can be improved. In particular, when the by-product FG has the property of inhibiting the growth of the target substance (for example, the property of etching the target substance), the growth rate of the target substance can be further improved by evacuating the by-product FG.

  Specifically, the byproduct exhaust unit 15 acquires information indicating the concentration of the byproduct FG from the byproduct detection unit 13. Then, the by-product exhaust unit 15 exhausts the by-product FG in accordance with the concentration of the by-product FG. For example, when the concentration of the by-product FG becomes higher than the threshold Th2, the by-product exhaust unit 15 exhausts the by-product FG until the concentration of the by-product FG becomes equal to or less than the threshold Th2. As a result, since the concentration of the by-product FG is maintained at or below the threshold Th2 inside the chamber 3, the growth rate of the target substance can be further improved.

  In particular, according to the first embodiment, the by-product exhaust unit 15 exhausts the by-product FG based on the concentration of the by-product FG acquired from the by-product detection unit 13, so the amount of the by-product FG increases without waste. It is possible to work only when. As a result, the power consumption of the byproduct exhaust unit 15 can be suppressed.

  More specifically, the byproduct exhaust unit 15 includes a valve unit 15a, a suction pump 15b, and a control unit 15c. The valve portion 15a includes one or more valves.

  When the concentration of the by-product FG is equal to or lower than the threshold Th2, the control unit 15c closes the valve to close the by-product exhaust pipe 27, and the gas from the inside of the chamber 3 to the outside (source gas Gn, carrier gas CG, etching gas, And the outflow of by-product FG).

  On the other hand, when the concentration of the by-product FG becomes higher than the threshold Th2, the control unit 15c drives the suction pump 15b and opens the valve to open the by-product exhaust pipe 27 to exhaust the by-product FG. Then, when the concentration of the by-product FG becomes equal to or lower than the threshold Th2, the control unit 15c closes the valve to close the by-product exhaust pipe 27, and stops the suction pump 15b. As a result, the exhaust of by-product FG is stopped.

  For example, when the concentration of the by-product FG becomes higher than the threshold Th2, the control unit 15 c drives the suction pump 15 b and opens the valve to open the by-product exhaust pipe 27, so that the gas inside the chamber 3 (source gas Gn, carrier gas CG, etching gas, and by-product FG) are exhausted. As a result, the by-product FG is exhausted together with the source gas Gn, the carrier gas CG, and the etching gas.

  In this example, the source gas Gn, the carrier gas CG, and the etching gas are exhausted from the byproduct exhaust pipe 27. Therefore, the gas supply device 60 supplements the source gas Gn to the chamber 3 according to the amount of decrease of the source gas Gn. When replenishing the source gas Gn, the gas supply device 60 supplements the source gas Gn such that the molar fraction of the source gas Gn is maintained constant inside the chamber 3. In addition, the gas supply device 60 supplements the carrier gas CG to the chamber 3 in accordance with the decrease amount of the carrier gas CG. Furthermore, the gas supply device 60 replenishes the etching gas EG to the chamber 3 according to the amount of decrease of the etching gas EG.

  In particular, also in this example, according to the first embodiment, the by-product exhaust unit 15 exhausts the by-product FG based on the concentration of the by-product FG acquired from the by-product detection unit 13. It is possible to operate. Therefore, the amount of the source gas Gn exhausted together with the byproduct FG can be suppressed. As a result, the utilization efficiency of the source gas Gn can be further improved.

  As described above with reference to FIG. 1, according to the first embodiment, each of the source gases Gn is a plurality of different source gases Gn introduced and retained inside the chamber 3 to form the target substance. A plurality of different source gases Gn can be introduced into the chamber 3 so as to have a mole fraction based on a chemical reaction formula for producing a target substance. That is, a plurality of different source gases Gn can be introduced into the chamber 3 so that the mole fraction of each source gas Gn can be maintained constant inside the chamber 3. As a result, the amount of residue can be suppressed. In the prior art, it is difficult to introduce the source gas into the reaction tube so that each molar fraction of the source gas can be kept constant because the source gas is circulated.

  The control unit 15c includes a processor and a storage device. Therefore, the processor controls the valve unit 15a and the suction pump 15b by executing a computer program stored in the storage device.

  Here, it is preferable that the gas supply device 60 supply a plurality of different dilution source gases Dn to the vapor phase growth apparatus 1 instead of the plurality of different source gases Gn. The diluted source gas Dn is a gas obtained by mixing the source gas Gn and the carrier gas CG and diluting the source gas Gn with the carrier gas CG. For example, in the plurality of diluted source gases Dn, the source gases Gn are different from each other, while the carrier gas CG is the same. In addition, when distinguishing and demonstrating the several dilution source gas Dn, it describes as dilution source gas D1, ..., DN (N is an integer greater than or equal to 2).

  Next, referring to FIG. 1, the mode of supplying diluted source gas Dn to vapor phase growth apparatus 1 instead of source gas Gn is mainly different from the mode of supplying source gas Gn to vapor phase growth apparatus 1. explain.

  That is, the plurality of source introduction pipes An respectively supply a plurality of dilution source gases Dn different from each other. Therefore, the plurality of raw material introduction ports GPn respectively introduce a plurality of dilution raw material gases Dn different from each other into the chamber 3.

  The gas supply device 60 supplies the diluted material gas Dn to the chamber 3 through the material introduction pipe An and the material introduction port GPn.

  Specifically, the gas supply device 60 supplies the diluted raw material gas Dn containing the raw material gas Gn of the first predetermined amount M1 to the chamber 3 and then shuts off the flow path of the diluted raw material gas Dn. The supply of the diluted source gas Dn is stopped. In other words, after the diluted raw material gas Dn containing the raw material gas Gn of the first predetermined amount M1 is introduced into the chamber 3, the flow path of the diluted raw material gas Dn is shut off and the raw material introduction pipe An and the raw material introduction port GPn The introduction of the diluted source gas Dn is stopped.

  Further, the gas supply device 60 supplements the diluted source gas Dn to the chamber 3 through the source introduction pipe An and the source introduction port GPn according to the decrease amount of the source gas Gn caused by the chemical reaction inside the chamber 3 . Further, when replenishing the diluted source gas Dn, the gas supply device 60 replenishes the diluted source gas Dn so that the molar fraction of the source gas Gn is maintained constant inside the chamber 3.

  Specifically, the gas supply device 60 is a diluted raw material including the raw material gas Gn of the second predetermined amount M2 through the raw material introduction pipe An and the raw material introduction port GPn according to the amount of decrease of the raw material gas Gn inside the chamber 3 The gas Dn is supplied to the chamber 3.

  Then, after the diluted source gas Dn containing the source gas Gn of the second predetermined amount M2 is replenished, the gas supply device 60 shuts off the flow path of the diluted source gas Dn, and the source introduction pipe An and the source introduction port GPn Supply of the diluted source gas Dn to the chamber 3 is stopped.

  In addition, the gas supply device 60 is supplied with the diluted source gas Dn containing the source gas Gn of the first predetermined amount M 1 according to the amount of reduction of the source gas Gn caused by the chemical reaction inside the chamber 3. The diluted material gas Dn may be constantly replenished through the material introduction pipe An and the material introduction port GPn.

  For example, when the amount of the raw material gas Gn in the chamber 3 becomes smaller than the threshold value Th1, the gas supply device 60 dilutes the raw material including the raw material gas Gn according to the amount of reduction of the raw material gas Gn in the chamber 3 The gas Dn may be constantly replenished from the raw material introduction port GPn.

  Also, for example, when constantly replenishing the diluted source gas Dn, the gas supply device 60 always replenishes the diluted source gas Dn such that the mole fraction of each of the source gas Gn is maintained constant inside the chamber 3. You may

  Furthermore, the gas supply device 60 may always replenish the carrier gas CG when constantly replenishing the diluted source gas Dn. Furthermore, the gas supply device 60 may always replenish the etching gas EG when constantly replenishing the diluted source gas Dn.

  When the byproduct exhaust unit 15 exhausts the byproduct FG together with the source gas Gn, the carrier gas CG, and the etching gas when the concentration of the byproduct FG becomes higher than the threshold Th2, the gas supply device 60 supplies the source gas Gn. The diluted source gas Dn is replenished to the chamber 3 in accordance with the decrease amount of The gas supply device 60 replenishes the dilution source gas Dn so that the molar fraction of each of the source gas Gn is maintained constant inside the chamber 3 when the dilution source gas Dn is replenished.

  Hereinafter, in the first embodiment, the gas supply device 60 supplies the diluted source gas Dn to the vapor phase growth apparatus 1 instead of the source gas Gn unless otherwise specified.

  Next, the gas supply device 60 will be described with reference to FIG. FIG. 2 is a view showing the gas supply device 60. As shown in FIG. As shown in FIG. 2, the gas supply device 60 includes a vacuum pump 61, a control unit 62, a thermostatic bath 63 (temperature control unit), a plurality of pressure adjustment units 64n, and a plurality of first flow rate control units Qn ( A plurality of flow rate control units), a second flow rate control unit 72, and a third flow rate control unit 73 are provided. Each of the pressure adjustment units 64n includes a dilution container Xn, a valve portion Yn (introduction portion), and a raw material container Zn (gas container). Then, the gas supply device 60 supplies a gas (the dilution source gas Dn, the carrier gas CG, and the etching gas EG) to the vapor deposition apparatus 1 (FIG. 1). In the present specification, the valve portion Yn is an example of the introduction portion, and the source container Zn is an example of the gas container.

  When the plurality of pressure adjustment units 64 n are described separately, they are described as pressure adjustment units 64 1,..., 64 N (N is an integer of 2 or more). When distinguishing and demonstrating the several 1st flow control part Qn, it describes as 1st flow control part Q1, ..., QN (N is an integer greater than or equal to 2). When distinguishing and explaining a plurality of dilution containers Xn, they are described as dilution containers X1, ..., XN (N is an integer of 2 or more). When distinguishing and demonstrating several valve part Yn, it describes as valve part Y1, ..., YN (N is an integer greater than or equal to 2). When distinguishing and demonstrating several raw material container Zn, it describes as raw material container Z1, ..., ZN (N is an integer greater than or equal to 2).

  The control unit 62 controls the vacuum pump 61, the thermostat 63, the plurality of valve units Yn, the plurality of first flow control units Qn, the second flow control unit 72, and the third flow control unit 73. That is, the vacuum pump 61, the constant temperature bath 63, the plurality of valve units Yn, the plurality of first flow control units Qn, the second flow control unit 72, and the third flow control unit 73 operate under the control of the control unit 62. Do. The control unit 62 includes a processor and a storage device. Therefore, the processor executes the computer program stored in the storage device, whereby the vacuum pump 61, the thermostat 63, the plurality of valve units Yn, the plurality of first flow control units Qn, the second flow control unit 72, and the second 3 Control the flow rate control unit 73.

  The constant temperature bath 63 controls the temperatures of the plurality of pressure adjustment units 64n, and holds the temperatures of the plurality of pressure adjustment units 64n at a constant temperature. The plurality of pressure adjustment units 64 n are disposed inside the thermostatic bath 63.

  The pressure adjustment unit 64n dilutes the source gas Gn with the carrier gas CG to generate a diluted source gas Dn. Then, the pressure adjustment unit 64n releases the diluted source gas Dn containing the source gas Gn. In addition, when generating the diluted source gas Dn, the pressure adjustment unit 64n adjusts the partial pressure of the carrier gas CG and the partial pressure of the source gas Gn inside the dilution container Xn.

  Specifically, the plurality of dilution containers Xn are provided corresponding to the plurality of source containers Zn, respectively. The plurality of valve portions Yn are provided corresponding to the plurality of raw material containers Zn, respectively. That is, the plurality of valve portions Yn are provided corresponding to the plurality of dilution containers Xn, respectively.

  The plurality of source containers Zn respectively store a plurality of source gases Gn (a plurality of different gases) different from each other. The source gas Gn is a non-diluted pure source gas, and has a constant pressure (vapor pressure) inside the source container Zn. Specifically, the source container Zn vaporizes the solid source to generate the source gas Gn, and stores the source gas Gn. The source container Zn may vaporize the liquid source to generate the source gas Gn and store the source gas Gn. For example, the constant temperature bath 63 controls the temperature of the source container Zn to vaporize the solid source in the source container Zn or to vaporize the liquid source in the source container Zn.

  In the present specification, the source gas Gn is an example of a gas to be supplied to the vapor phase growth apparatus 1 by the gas supply device 60. Therefore, the source container Zn contains the source gas Gn as a gas to be supplied. The vapor deposition apparatus 1 is an example of a gas supply destination by the gas supply device 60. Furthermore, unlike the gas to be supplied, the carrier gas CG transports the gas to be supplied, dilutes the gas to be supplied, or stirs the gas to be supplied, for example. .

  Each of the valve portions Yn introduces the source gas Gn and the carrier gas CG for diluting the source gas Gn into the corresponding dilution container Xn at different timings. As a result, in the dilution container Xn, a diluted source gas Dn is generated by mixing the source gas Gn and the carrier gas CG. Further, the valve unit Yn adjusts the partial pressure of the source gas Gn and the partial pressure of the carrier gas CG in the dilution container Xn. As a result, in the dilution container Xn, the total pressure p of the diluted source gas Dn is set to a predetermined total pressure value, the partial pressure pg of the source gas Gn is set to the first partial pressure value, and the partial pressure pc of the carrier gas CG is It is set to the second partial pressure value. It is p = pg + pc.

  Each of the dilution containers Xn mixes the source gas Gn introduced from the corresponding source container Zn with the carrier gas CG, and stores it as a diluted source gas Dn (dilution gas). Then, each of the valve parts Yn releases the diluted source gas Dn from the corresponding dilution container Xn after the source gas Gn and the carrier gas CG are mixed. That is, in each of the valve portions Yn, after the source gas Gn and the carrier gas CG are mixed and the partial pressure pg of the source gas Gn and the partial pressure pc of the carrier gas CG are adjusted, the diluted source gas Dn is Release from the corresponding dilution container Xn.

  In the present specification, the dilution source gas Dn is a dilution gas obtained by mixing the gas (specifically, the source gas Gn) to be supplied to the vapor phase growth apparatus 1 by the gas supply device 60 and the carrier gas CG. An example of

  The plurality of first flow rate control units Qn are provided corresponding to the plurality of valve units Yn, respectively. In addition, the plurality of first flow rate control units Qn are provided corresponding to the plurality of raw material introduction pipes An (FIG. 1).

  The first flow rate control unit Qn controls the flow rate of the diluted source gas Dn released by the corresponding valve unit Yn. Then, the first flow rate control unit Qn supplies the diluted material gas Dn to the chamber 3 through the corresponding material introduction pipe An. Specifically, the first flow rate control unit Qn has a laminar flow element (specifically, a porous member). The laminar flow element divides the flow path into the upstream side and the downstream side. Then, the first flow rate control unit Qn controls the volumetric flow rate or the mass flow rate of the diluted source gas Dn based on the differential pressure between the upstream side and the downstream side of the laminar flow element by using the Hagen-Poiseil principle. .

  The second flow rate control unit 72 controls the flow rate of the carrier gas CG. Then, the second flow rate control unit 72 supplies the carrier gas CG to the chamber 3 through the carrier introduction pipe 19 (FIG. 1). The configuration of the second flow control unit 72 is the same as the configuration of the first flow control unit Qn.

  The third flow rate control unit 73 controls the flow rate of the etching gas EG. Then, the third flow rate control unit 73 supplies the etching gas EG to the chamber 3 through the etching introduction pipe 21 (FIG. 1). The configuration of the third flow control unit 73 is the same as the configuration of the first flow control unit Qn.

  As described above with reference to FIG. 2, according to the first embodiment, since the carrier gas CG is introduced into the dilution container Xn, compared with the case where only the source gas Gn is introduced into the dilution container Xn. The total pressure p of the diluted source gas Dn can be increased. Therefore, the source gas Gn easily moves toward the first flow rate control unit Qn and the vapor phase growth apparatus 1 as compared with the case where only the source gas Gn is introduced into the dilution container Xn. That is, the force to move the source gas Gn is secured by the total pressure p of the dilution source gas Dn in the dilution container Xn. On the other hand, by adjusting the amount (quantity of substance, volume, or mass) of the source gas Gn introduced from the source container Zn into the dilution container Xn, the amount of source gas Gn included in the dilution source gas Dn in the dilution container Xn It is possible to precisely adjust the amount of substance, volume or mass).

  As a result, compared to the case where the flow rate of the carrier gas is controlled to flow the carrier gas and the supply amount of the source gas is adjusted, as in a general film forming apparatus, the first flow rate control unit Qn and the vapor phase growth apparatus The amount (quantity of substance, volume, or mass) of the source gas Gn to be moved together with the carrier gas CG toward 1, the supply amount of the source gas Gn can be accurately adjusted. Further, in order to discharge the diluted source gas Dn from the dilution container Xn, the supply amount of the source gas Gn is more accurate than in the case where the source gas is directly supplied from the bubbler to the gas supply destination like a general film forming apparatus. It can be adjusted well. Since the supply amount of the source gas Gn can be accurately adjusted, the vapor deposition apparatus 1 can form a target substance with high quality (for example, a target substance with few defects and high purity).

  Further, according to the first embodiment, the force to move the source gas Gn is secured by the total pressure p of the dilution source gas Dn in the dilution container Xn, and the dilution source gas Dn containing the source gas Gn is used as the dilution container Xn. Released from Therefore, compared to a general film forming apparatus, the supply amount of the source gas Gn is less affected by the temperature, and the temperature management is easy. Further, since the supply amount of the source gas Gn is not easily influenced by the temperature, the supply amount of the source gas Gn can be adjusted with higher accuracy. Furthermore, since the temperature management is easy, the cost of the gas supply device 60 can be reduced.

  In a general film forming apparatus, the carrier gas is supplied to the bubbler to generate the source gas, and the source gas is directly supplied to the gas supply destination by the carrier gas. Pressure), the pressure in the bubbler, and the flow rate of the carrier gas. Therefore, the flow rate of the source gas is susceptible to the temperature. As a result, the flow rate of the source gas can not be accurately controlled unless the temperature in the bubbler is precisely controlled. That is, temperature control is difficult. Further, in a general film forming apparatus, when the internal temperature of the bubbler is precisely controlled, a temperature control device (for example, an electronic thermostat) for controlling the temperature of the bubbler becomes expensive and the cost increases. In addition, the power consumption of such a temperature control device may be relatively large, and the maintenance cost may increase. On the other hand, in the first embodiment, the increase in the maintenance cost can be suppressed. Furthermore, the internal shape of such a temperature control device may be limited to a special shape, and the shape of the bubbler disposed inside the temperature control device may be limited. On the other hand, in the first embodiment, the restriction of the shape of the raw material container Zn can be suppressed, and the raw material container Zn of any shape can be adopted.

  Further, according to the first embodiment, the force to move the source gas Gn is secured by the total pressure p of the dilution source gas Dn in the dilution container Xn, and the dilution source gas Dn containing the source gas Gn is used as the dilution container Xn. Released from Therefore, a small amount of the source gas Gn can be easily supplied as compared with a general film forming apparatus.

  In a general film forming apparatus, the flow rate of the source gas is determined by the temperature inside the bubbler (the vapor pressure of the source), the pressure inside the bubbler, and the flow rate of the carrier gas. It is necessary to reduce the flow rate of the carrier gas or to lower the temperature in the bubbler. However, if the flow rate of the carrier gas is reduced, continuous bubble generation can not be realized, intermittent bubble generation may occur, and the supply amount of the source gas may become unstable. On the other hand, in the first embodiment, since the diluted source gas Dn including the source gas Gn is released from the dilution container Xn, the supply amount of the source gas Gn is stable. In a general film forming apparatus, when lowering the temperature inside the bubbler, the supply of a small amount of source gas depends on the cooling capacity of a temperature control device (for example, an electronic thermostat), and the supply of a small amount of source gas Limits can occur. On the other hand, according to the first embodiment, since the force for moving the source gas Gn is secured by the total pressure p of the diluted source gas Dn in the dilution container Xn, a small amount of the source gas Gn can be easily supplied. .

  Further, according to the first embodiment, the total pressure p of the diluted source gas Dn can be adjusted by adjusting the amount of introduction of the carrier gas CG into the dilution container Xn. That is, the force of moving the source gas Gn can be adjusted.

  Furthermore, according to Embodiment 1, the amount (quantity of substance, volume or mass) of the source gas Gn contained in the diluted source gas Dn can be adjusted by adjusting the partial pressure pg of the source gas Gn in the dilution container Xn. It can be adjusted. As a result, it is possible to more precisely adjust the amount (the amount of substance, the amount of volume, or the mass) of the source gas Gn moved together with the carrier gas CG toward the first flow rate control unit Qn and the vapor deposition apparatus 1.

  Furthermore, according to the first embodiment, since the plurality of dilution containers Xn are provided, the amount of the source gas Gn to be introduced into the dilution container Xn can be adjusted for each dilution container Xn. Therefore, the source gas Gn can be introduced into each of the dilution containers Xn such that each of the source gases Gn has a mole fraction based on a chemical reaction formula for producing the target substance. That is, when the source gas Gn is supplied to the vapor phase growth apparatus 1, the mole fraction of the source gas Gn can be easily adjusted. In this case, for example, in the plurality of dilution containers Xn, the carrier gas CG is introduced into each of the dilution containers Xn such that the total pressures p of the dilution source gas Dn are substantially the same.

  Furthermore, according to the first embodiment, since the plurality of dilution containers Xn are provided, the total pressure p of the dilution source gas Dn can be adjusted for each of the dilution containers Xn. Therefore, from each of the dilution containers Xn to the first flow rate control unit Qn and the vapor phase growth apparatus 1 so that each of the source gases Gn has a mole fraction based on a chemical reaction formula for producing the target substance. The source gas Gn can be moved. That is, when the source gas Gn is supplied to the vapor phase growth apparatus 1, the mole fraction of the source gas Gn can be easily adjusted. In this case, for example, the total pressure p of the diluted source gas Dn in each dilution container Xn is determined based on the molar fraction of each source gas Gn based on the chemical reaction formula for generating the target substance. Then, the carrier gas CG is introduced into each of the dilution containers Xn so as to reach the determined total pressure p.

  Furthermore, according to the first embodiment, the source gas Gn can be moved from the source container Zn to the dilution container Xn using the pressure (vapor pressure) of the source gas Gn inside the source container Zn. Therefore, it is possible to suppress the provision of an active device for moving the source gas Gn from the source container Zn to the dilution container Xn. As a result, the gas supply device 60 can be simplified, and the cost of the gas supply device 60 can be reduced.

  Furthermore, according to the first embodiment, since the procedure for mixing the plurality of source gases Gn into the chamber 3 in advance can be reduced, the procedure before introducing the plurality of source gases Gn into the chamber 3 can be simplified.

  Furthermore, according to the first embodiment, the first flow rate control unit Qn can easily supply the diluted source gas Dn to the vapor phase growth apparatus 1 using the total pressure p of the diluted source gas Dn.

  The first flow rate control unit Qn can also control the flow rate of the source gas Gn released from the source container Zn by the corresponding valve Yn. Then, the first flow rate control unit Qn can also supply the source gas Gn to the chamber 3 through the corresponding source introduction pipe An. Specifically, the first flow rate control unit Qn uses the Hagen Poiseil principle, and based on the differential pressure between the upstream side and the downstream side of the laminar flow element, the volume flow rate or mass flow rate of the source gas Gn is calculated. It can also be controlled.

  Next, with reference to FIG. 3, the pressure adjustment unit 64 n will be described. FIG. 3 is a diagram showing the pressure adjustment unit 64n. As shown in FIG. 3, each of the pressure adjustment units 64n further includes a thermometer TM, a first pressure gauge PM1 (pressure gauge), and a second pressure gauge PM2. The thermometer TM measures the temperature inside the dilution container Xn. The first pressure gauge PM1 measures the pressure in the dilution container Xn. The second pressure gauge PM2 measures the pressure. The second pressure gauge PM2 can measure, for example, a lower pressure than the first pressure gauge PM1.

  The valve portion Yn includes a first valve unit 75 and a second valve unit 77. The first valve unit 75 includes valves b1 to b7 and tubes t1 to t4. The second valve unit 77 includes a valve b8 and a pipe t5. The valves b1 to b8 are, for example, stop valves.

  The pipe t1 connects the dilution container Xn and the valve b4. The pipe t2 interconnects the valve b3 to the valve b7. The pipe t3 mutually connects the valve b1 to the valve b3. The pipe t4 connects the valve b7 and the valve b8. The pipe t5 connects the valve t8 and the raw material container Zn. The valve t8 may be directly connected to the raw material container Zn. The valve b4 and the dilution container Xn may be directly connected.

  Continuing to refer to FIG. 3, the control procedure of the valve portion Yn will be described. The control procedure includes first to sixteenth procedures. In the initial state of the valve portion Yn, the valves b1 to b8 are closed.

[Vacuum evacuation and purge]
First procedure: The vacuum pump 61 is started.

  Second procedure: Open the valves b2, b3, b4 and b7.

  Third procedure: Open the valve b6 and close the valve b3. The second pressure gauge PM2 measures the pressure in the dilution container Xn. The operator confirms the degree of vacuum inside the dilution container Xn by the second pressure gauge PM2.

  Fourth procedure: Close the valves b2 and b6 and open the valves b1 and b3. Then, the carrier gas CG is introduced into the dilution container Xn from the valve b1. As a result, the inside of the dilution container Xn is cleaned by the carrier gas CG (purge).

  Then, the valve portion Yn is returned to the initial state, and the initial state and the second to fourth procedures are repeated. As a result, the inside of the dilution container Xn is repeatedly cleaned by the carrier gas CG (cycle purge). By repeatedly washing the inside of the dilution container Xn, the amount of substance (or concentration) of the residual gas inside the dilution container Xn can be reduced. After repeating the initial state and the second to fourth procedures, the valve portion Yn is returned to the initial state, and the second and third procedures are executed again.

[Introduction of raw material gas Gn into dilution container Xn]
Fifth procedure: Close the valves b2, b6 and b7 and open the valve b8.

  Sixth procedure: The opening and closing of the valve b7 is repeated to introduce the source gas Gn from the source container Zn into the dilution container Xn. When the source gas Gn is introduced into the dilution container Xn, the pressure pg of the source gas Gn inside the dilution container Xn is set to the first partial pressure value by adjusting the opening time and closing time of the valve b7. The pressure pg is expressed by equation (1). “V” indicates the internal volume of the dilution container Xn, “ng” indicates the amount of substance (moles) of the raw material gas Gn, “R” indicates the gas constant, and “T” indicates the temperature inside the dilution container Xn Indicates

  pg × V = ng × R × T (1)

  The volume V and the temperature T are known, and the pressure pg can be measured by the first pressure gauge PM1, so the amount of substance of the source gas Gn inside the dilution container Xn can be calculated based on the equation (1).

  According to the first embodiment, the temperature of the dilution container Xn and the partial pressure of the raw material gas Gn are monitored by monitoring the temperature of the dilution container Xn with the thermometer TM and monitoring the pressure of the dilution container Xn with the first pressure gauge PM1. We can control pg to the desired value. As a result, it is possible to introduce a desired amount of material gas Gn into the dilution container Xn.

  When the pressure pg of the source gas Gn is low, the valve pg may be opened to measure the pressure pg by the second pressure gauge PM2.

  Seventh procedure: When the pressure pg of the source gas Gn reaches the first partial pressure value, the valve b7 is closed.

[Introduction of carrier gas CG into dilution vessel Xn]
Eighth procedure: Close the valves b4 and b8 and open the valves b2, b3 and b7.

  Ninth procedure: Open the valve b6. The second pressure gauge PM2 measures the pressure in the tubes t2, t3 and t4. The operator confirms the degree of vacuum inside the tubes t2, t3 and t4 by the second pressure gauge PM2.

  Tenth procedure: Close the valves b2 and b6 and open the valve b1.

  Eleventh procedure: The carrier gas CG is introduced into the dilution container Xn by repeating the opening and closing of the valve b4. When the carrier gas CG is introduced into the dilution container Xn, the opening time and closing time of the valve b4 are adjusted to set the total pressure p of the diluted material gas Dn inside the dilution container Xn to a predetermined total pressure value. . The total pressure p is expressed by equation (2). “V” indicates the internal volume of the dilution container Xn, “n” indicates the amount of substance (moles) of the diluted raw material gas Dn, “R” indicates the gas constant, and “T” indicates the inside of the dilution container Xn Indicates the temperature. Specifically, “n” is the sum of the substance mass (mol) of the carrier gas CG and the substance mass (mol) of the source gas Gn inside the dilution container Xn.

  p × V = n × R × T (2)

  The volume V and the temperature T are known, and the total pressure p can be measured by the first pressure gauge PM1, so the substance mass n of the dilution source gas Dn inside the dilution container Xn can be calculated based on the equation (2) . Furthermore, since the substance mass ng of the source gas Gn is known, the substance mass nc of the carrier gas CG can be calculated based on the equation (3).

  n = ng + nc ... (3)

  According to the first embodiment, the temperature of the dilution container Xn is monitored by the thermometer TM, and the pressure of the dilution container Xn is monitored by the first pressure gauge PM1, the temperature of the dilution container Xn and the total amount of the diluted source gas Dn. The pressure p can be controlled to a desired value. As a result, it is possible to introduce a carrier gas CG having a desired amount of substance into the dilution container Xn.

  Further, the partial pressure pc of the carrier gas CG can be calculated from the equation (4). “Pg” indicates the pressure of the source gas Gn inside the dilution container Xn, that is, the partial pressure of the source gas Gn.

  p = pg + pc (4)

  Based on the total pressure p, the partial pressure pg, and the partial pressure pc, or the substance mass n, the substance mass ng, and the substance mass nc, the mole fraction of the source gas Gn and the mole fraction of the carrier gas CG can be calculated.

  Twelfth procedure: When the total pressure p of the diluted raw material gas Dn reaches a predetermined total pressure value, the valve b4 is closed. That is, when the partial pressure pc of the carrier gas CG reaches the second partial pressure value, the valve b4 is closed.

[Supply of diluted source gas Dn to vapor phase growth apparatus 1]
Thirteenth procedure: The valve b5 may be opened. As a result, the flow path from the valve b5 to the first flow rate control unit Qn is cleaned (purge) by the carrier gas CG.

  Fourteenth Procedure: Close the valves b1, b5 and b7 and open the valve b2.

  15th procedure: Open valve b6. The second pressure gauge PM2 measures the pressure in the tubes t2 and t3. The operator confirms the degree of vacuum inside the tubes t2 and t3 by the second pressure gauge PM2. When the flow path volume of the tubes t2 and t3 is smaller than the volume of the dilution container Xn, the fifteenth procedure is unnecessary.

  Sixteenth procedure: Close the valves b2, b3 and b6 and open the valves b4 and b5. As a result, the diluted material gas Dn is released from the dilution container Xn toward the first flow rate control unit Qn (FIG. 2).

Next, an example of forming gallium nitride (GaN) as a target substance on the substrate S will be described with reference to FIG. FIG. 4 is a diagram showing a part of the vapor phase growth system 100. As shown in FIG. As shown in FIG. 4, the dilution source gas D1 is accommodated in the dilution container X1. The diluted source gas D1 contains gallium trichloride (GaCl ₃ ) as the source gas G1 and nitrogen (N ₂ ) as the carrier gas CG. Further, the dilution source gas D2 is accommodated in the dilution container X2. The diluted source gas D2 contains ammonia (NH ₃ ) as the source gas G2 and nitrogen (N ₂ ) as the carrier gas CG. Further, nitrogen (N ₂ ) as the carrier gas CG is supplied to the second flow rate control unit 72. The third flow rate control unit 73 is supplied with chlorine (Cl ₂ ) as the etching gas EG.

  In the initial state, the first flow rate control unit Q1 closes the raw material introduction pipe A1, the first flow rate control unit Q2 closes the raw material introduction pipe A2, and the second flow rate control unit 72 closes the carrier introduction pipe 19, The third flow control unit 73 closes the etching introduction pipe 21, the residue discharge device 80 closes the residue discharge pipe 25, and the by-product exhaust unit 15 closes the by-product exhaust pipe 27.

  The first flow control unit Q1, the first flow control unit Q2, the second flow control unit 72, and the third flow control unit 73 are respectively a raw material introduction pipe A1, a raw material introduction pipe A2, a carrier introduction pipe 19 and an etching introduction pipe 21 and open. As a result, the diluted source gas D1 is introduced into the chamber 3 from the dilution container X1, the diluted source gas D2 is introduced into the chamber 3 from the dilution container X2, and the carrier gas CG and the etching gas EG are introduced into the chamber 3.

  In the chamber 3, gallium trichloride (G1) and ammonia (G2) react chemically according to the reaction formula (r1). As a result, gallium nitride (GaN) as a target substance is grown on the substrate S.

GaCl ₃ + NH ₃ → GaN + ₃ HCl (r 1)

  Since there is no outflow path of gallium trichloride (G1) and ammonia (G2) in the chamber 3, the outflow of gallium trichloride (G1) and ammonia (G2) from the chamber 3 is suppressed. Therefore, the utilization efficiency of gallium trichloride (G1) and ammonia (G2) can be improved.

  On the other hand, the by-product exhaust unit 15 exhausts hydrogen chloride (HCl) as the by-product FG. Therefore, the growth rate of gallium nitride can be improved. In addition, after the formation of gallium nitride on the substrate S is completed, the residue discharge device 80 discharges the residue ZG inside the chamber 3 and cleans the inside of the chamber 3.

(First modification)
Next, with reference to FIG. 5, a pressure adjustment unit 64nA according to a first modification of the first embodiment of the present invention will be described. FIG. 5 is a diagram showing the pressure adjustment unit 64nA. As shown in FIG. 5, the pressure adjustment unit 64nA according to the first modification differs from the pressure adjustment unit 64n shown in FIG. 3 in that the pressure adjustment unit 64nA has a dilution container Xn whose volume can be changed. Otherwise, the configuration of the pressure adjustment unit 64nA is similar to the configuration of the pressure adjustment unit 64n. The differences between the first modification and the first embodiment will be mainly described below.

  Each of the pressure adjustment units 64 nA includes a volume change unit 90 and a pressure adjustment unit 91. The dilution container Xn has a gas storage space 92. The gas containing space 92 is a space capable of containing a gas.

  The volume changer 90 is disposed inside the dilution container Xn. Then, the volume changing unit 90 changes the volume of the volume changing unit 90 to change the volume of the gas storage space 92. As a result, the pressure inside the dilution container Xn is changed according to the volume of the gas storage space 92.

  Specifically, the pressure adjustment unit 91 adjusts the pressure inside the volume change unit 90 to change the volume of the volume change unit 90. For example, the pressure adjustment unit 91 sends the driving gas BG into the volume change unit 90, and drives the volume change unit 90 so that the volume of the volume change unit 90 is increased. In this case, the pressure inside the dilution container Xn rises. For example, the pressure adjustment unit 91 discharges the gas EX from the inside of the volume change unit 90, and drives the volume change unit 90 so that the volume of the volume change unit 90 decreases. In this case, the pressure inside the dilution container Xn drops. In addition, since the volume change unit 90 is separated inside the dilution container Xn, the driving gas BG and the dilution source gas Dn are not in contact with each other.

  The volume changer 90 is, for example, a bellows. The volume changer 90 includes, for example, a bottomed cylindrical member and a piston inserted into the bottomed cylindrical member. The pressure adjustment unit 91 is, for example, an electropneumatic converter.

  As described above with reference to FIG. 5, according to the first modification of the first embodiment, the volume changing unit 90 can adjust the pressure inside the dilution container Xn to a desired value. That is, even after the carrier gas CG and the source gas Gn are introduced into the dilution container Xn, the total pressure p of the diluted source gas Dn can be adjusted to a desired value. In addition, even before the source gas Gn is introduced into the dilution container Xn before the carrier gas CG is introduced into the dilution container Xn, the pressure of the source gas Gn in the dilution container Xn, that is, the partial pressure pg is adjusted to a desired value it can.

  The pressure adjustment unit 91 may also receive information indicating the pressure of the gas accommodation space 92 from the first pressure gauge PM1. Therefore, the pressure adjustment unit 91 can also change the volume of the volume change unit 90 based on the pressure of the gas storage space 92. As a result, feedback control is performed, and the pressure of the gas storage space 92 can be adjusted with high accuracy. That is, the total pressure p of the diluted source gas Dn can be adjusted with high accuracy. In addition, the partial pressure pg of the source gas Gn can be adjusted with high accuracy.

  In the first modification, the gas supply device 60 includes a pressure adjustment unit 64nA shown in FIG. 5 instead of the pressure adjustment unit 64n shown in FIG. That is, in the first modification, the gas supply device 60 includes a plurality of pressure adjustment units 64nA instead of the plurality of pressure adjustment units 64n. When the plurality of pressure adjustment units 64nA are distinguished, they can be expressed as pressure adjustment units 641A, ..., 64NA (N is an integer of 2 or more).

(2nd modification)
Next, with reference to FIG. 6, a pressure adjustment unit 64nB according to a second modified example of the first embodiment of the present invention will be described. FIG. 6 is a diagram showing the pressure adjustment unit 64nB. As shown in FIG. 6, the pressure adjustment unit 64nB according to the second modification has a plurality of dilution containers Xmn for one raw material container Zn, and thus the pressure adjustment unit 64n shown in FIG. It is different. Otherwise, the configuration of the pressure adjustment unit 64nB is similar to the configuration of the pressure adjustment unit 64n. The differences between the second modification and the first embodiment will be mainly described below.

  Each of the pressure adjustment units 64nB includes a plurality of dilution containers Xmn corresponding to one raw material container Zn in place of the dilution container Xn shown in FIG. 3, and the thermometer TM and the first pressure for each dilution container Xmn A total of PM1 (pressure gauge) is provided. Further, each of the pressure adjustment units 64nB includes a first valve unit 75a instead of the first valve unit 75 shown in FIG. The first valve unit 75a includes a plurality of valves b4 corresponding to the plurality of dilution containers Xmn instead of the valve b4 shown in FIG. In addition, the first valve unit 75a includes a plurality of pipes t1 corresponding to the plurality of dilution containers Xmn instead of the pipe t1 shown in FIG. In addition, when distinguishing and demonstrating the several dilution container Xmn, it describes as dilution container X1n, ..., XMn (M is an integer greater than or equal to 2).

  Each dilution vessel Xmn is connected to a corresponding valve b4 by a corresponding tube t1. The pipe t2 mutually connects the valve b3, the plurality of valves b4, the valve b5, the valve b6 and the valve b7. Each of the dilution containers Xmn mixes the source gas Gn introduced from the source container Zn with the carrier gas CG, and stores it as a diluted source gas Dn.

  The control procedure of the valve portion Yn (introduction portion) is the same as the control procedure of the valve portion Yn described with reference to FIG.

  However, the valve unit Yn introduces the source gas Gn and the carrier gas CG into the dilution container Xmn at different timings for each of the dilution containers Xmn in different time zones assigned to the plurality of dilution containers Xmn. For example, when the source gas Gn and the carrier gas CG are introduced into the dilution container X1n, only the valve b4 corresponding to the dilution container X1n is opened, and the valve b4 corresponding to each of the dilution container X2n to the dilution container XMn is closed. Be

  In addition, the valve portion Yn discharges the diluted source gas Dn from the dilution container Xmn after the source gas Gn and the carrier gas CG are mixed for each dilution container Xmn. For example, when releasing the diluted source gas Dn from the dilution container X1n, only the valve b4 corresponding to the dilution container X1n is opened, and the valve b4 corresponding to each of the dilution container X2n to the dilution container XMn is closed.

  As described above with reference to FIG. 6, according to the second modification of the first embodiment, a plurality of dilution containers Xmn are provided for each pressure adjustment unit 64nB. Then, the same source gas Gn is introduced into the plurality of dilution containers Xmn. Therefore, for example, when the concentration of the source gas Gn stored in a plurality of dilution containers Xmn is the same, a certain dilution container Xmn can be used as a reserve for the dilution container Xmn in use. In addition, for example, when the concentrations of the source gases Gn stored in the plurality of dilution containers Xmn are different, it is possible to discharge diluted source gases Dn having different concentrations from one pressure adjustment unit 64nB.

  In the second modification, the gas supply device 60 includes a pressure adjustment unit 64nB shown in FIG. 6 instead of the pressure adjustment unit 64n shown in FIG. That is, in the second modification, the gas supply device 60 includes a plurality of pressure adjustment units 64nB instead of the plurality of pressure adjustment units 64n. When the plurality of pressure adjustment units 64nB are distinguished, they can be expressed as pressure adjustment units 641B, ..., 64NB (N is an integer of 2 or more). When the dilution containers Xmn are distinguished for each pressure adjustment unit 64nB, they can be expressed as dilution containers Xm1,..., XmN (N is an integer of 2 or more) corresponding to the pressure adjustment units 641B,.

Second Embodiment
A vapor deposition system 100 according to a second embodiment of the present invention will be described with reference to FIGS. 7 to 11. The second embodiment is different from the first embodiment in which the vapor deposition apparatus 1 individually introduces a plurality of source gases Gn in that the vapor deposition apparatus 1 introduces a mixed gas MG obtained by mixing a plurality of source gases Gn. The differences between the second embodiment and the first embodiment will be mainly described below.

  FIG. 7 is a view showing a vapor deposition system 100 according to a second embodiment of the present invention. As shown in FIG. 7, the vapor phase growth system 100 includes a gas supply device 60A in place of the gas supply device 60 shown in FIG. 1. Moreover, the vapor phase growth system 100 is provided with a single raw material introduction pipe A1. The raw material introduction pipe A1 supplies the mixed gas MG. The mixed gas MG is a gas in which a plurality of different source gases Gn are mixed. In the mixed gas MG before being introduced into the chamber 3, the plurality of source gases Gn do not cause a chemical reaction.

  The vapor phase growth apparatus 1 is provided with a single raw material introduction port GP1 corresponding to a single raw material introduction pipe A1. Therefore, the raw material introduction port GP1 introduces the mixed gas MG into the chamber 3 through the raw material introduction pipe A1.

  Then, the vapor phase growth apparatus 1 blocks the outflow of the source gas Gn from the inside to the outside of the chamber 3 in a part or all of the reaction period RP. Therefore, the chamber 3 is sealed in part or all of the reaction period RP. That is, the vapor deposition apparatus 1 causes the mixed gas MG (that is, a plurality of different source gases Gn) to stay in the chamber 3 to cause a chemical reaction, and forms the target substance on the substrate S.

  As a result, according to the second embodiment, the utilization efficiency of the source gas Gn contained in the mixed gas MG can be improved as compared to the case where the target gas is formed by circulating the mixed gas. In addition, according to the second embodiment, due to the same configuration as the first embodiment, the same effect as the first embodiment is obtained.

  Further, according to the second embodiment, the single raw material introduction port GP1 introduces the mixed gas MG into the chamber 3 through the single raw material introduction pipe A1. That is, a plurality of different source gases Gn are introduced into the chamber 3 from a single source introduction port GP1. Therefore, the configuration of the chamber 3 can be simplified as compared with the case where the plurality of source gases Gn are introduced from each of the plurality of source introduction ports GPn. As a result, the cost of the vapor phase growth apparatus 1 can be reduced. Further, since the single raw material introduction pipe A1 is provided, the configuration of the vapor phase growth system 100 can be simplified as compared with the case where a plurality of raw material introduction pipes An are provided. As a result, the cost of the vapor deposition system 100 can be reduced.

  With continued reference to FIG. 7, the gas supply device 60A will be described. The gas supply device 60A supplies the mixed gas MG to the chamber 3 through the raw material inlet pipe A1 and the raw material inlet port GP1.

  Specifically, after supplying the mixed gas MG of the fifth predetermined amount M5 to the chamber 3, the gas supply device 60A shuts off the flow path of the mixed gas MG and stops the supply of the mixed gas MG to the chamber 3 Do. In other words, after the mixed gas MG of the fifth predetermined amount M5 is introduced into the chamber 3, the flow path of the mixed gas MG is blocked, and the introduction of the mixed gas MG from the raw material inlet pipe A1 and the raw material inlet port GP1 is It is stopped.

  Therefore, according to the second embodiment, the source gas Gn can be further suppressed from flowing out of the chamber 3. As a result, the utilization efficiency of the source gas Gn can be further improved.

  The fifth predetermined amount M5 indicates, for example, the amount of substance (mol), mass, or volume. The fifth predetermined amount M5 is the sum of a plurality of first predetermined amounts M1 determined for each of the plurality of source gases Gn. The first predetermined amount M1 is the same as the first predetermined amount M1 of the first embodiment.

  Therefore, according to the second embodiment, the excess and deficiency of the mixed gas MG can be suppressed, and an appropriate amount of the mixed gas MG can be introduced into the chamber 3. As a result, waste of the mixed gas MG can be suppressed.

  Further, the gas supply device 60A supplements the mixed gas MG to the chamber 3 through the raw material introduction pipe A1 and the raw material introduction port GP1 according to the decrease amount of the mixed gas MG resulting from the chemical reaction inside the chamber 3.

  Therefore, according to the second embodiment, a situation in which the source gas Gn runs short in the chamber 3 can be avoided, so that growth defects of the target material can be suppressed.

  In addition, when replenishing the mixed gas MG, the gas supply device 60A replenishes the mixed gas MG such that the mole fraction of each of the source gases Gn is maintained constant inside the chamber 3.

  Therefore, according to the second embodiment, excess and deficiency of the source gas Gn can be suppressed, and an appropriate amount of the source gas Gn can be introduced into the chamber 3. As a result, waste of the source gas Gn can be suppressed.

  Specifically, the gas supply device 60A supplies the mixed gas MG of the sixth predetermined amount M6 to the chamber 3 according to the amount of reduction of the mixed gas MG inside the chamber 3.

  The sixth predetermined amount M6 indicates, for example, a substance amount (mol), a mass, or a volume. The sixth predetermined amount M6 is the sum of a plurality of second predetermined amounts M2 determined for each of the plurality of source gases Gn. The second predetermined amount M2 is the same as the second predetermined amount M2 of the first embodiment. The sixth predetermined amount M6 is preferably equal to, for example, the reduction amount of the mixed gas MG.

  Then, after the mixed gas MG of the sixth predetermined amount M6 is replenished, the gas supply device 60A cuts off the flow path of the mixed gas MG, and enters the chamber 3 through the raw material introduction pipe A1 and the raw material introduction port GP1. The replenishment of the mixed gas MG is stopped.

  Therefore, according to the second embodiment, the source gas Gn can be further suppressed from flowing out of the chamber 3. As a result, the utilization efficiency of the source gas Gn can be further improved.

  Note that, after the mixed gas MG of the fifth predetermined amount M5 is supplied, the gas supply device 60A responds to the amount of reduction of the mixed gas MG due to the chemical reaction inside the chamber 3, according to the raw material introduction pipe A1 and The mixed gas MG may be constantly replenished through the raw material introduction port GP1. In this case, the mixed gas MG is constantly maintained at a constant amount inside the chamber 3 by constantly replenishing the mixed gas MG by an amount corresponding to the decrease of the mixed gas MG. Therefore, the growth of the target substance can be controlled with high precision. Moreover, while the mixed gas MG is replenished, the mixed gas MG does not flow out of the chamber 3, so that the utilization efficiency of the mixed gas MG can be improved.

  For example, when the amount of the mixed gas MG in the chamber 3 becomes smaller than the threshold value Th3, the gas supply device 60A uses the mixed gas MG as a raw material introduction port according to the amount of reduction of the mixed gas MG in the chamber 3. You may always replenish from GP1. The threshold value Th3 is preferably set to, for example, the same value as the fifth predetermined amount M5. In this case, the mixed gas MG can be held at the fifth predetermined amount M5 in the chamber 3. As a result, the growth of the target substance can be accurately controlled.

  Also, for example, when constantly replenishing the mixed gas MG, the gas supply device 60A constantly replenishes the mixed gas MG so that the mole fraction of each of the source gases Gn is maintained constant inside the chamber 3. It is also good. In this case, excess or deficiency of the source gas Gn in the chamber 3 is suppressed, and an appropriate amount of the source gas Gn can be introduced into the chamber 3. As a result, waste of the source gas Gn can be suppressed.

  The gas supply device 60A may always replenish the carrier gas CG when constantly replenishing the mixed gas MG. The gas supply device 60A may always replenish the etching gas EG when constantly replenishing the mixed gas MG.

  When the by-product exhaust unit 15 exhausts the by-product FG together with the source gas Gn, the carrier gas CG, and the etching gas when the concentration of the by-product FG becomes larger than the threshold Th2, the gas supply device 60A generates the source gas The mixed gas MG is replenished to the chamber 3 according to the decrease amount of Gn. When replenishing the mixed gas MG, the gas supply device 60A replenishes the mixed gas MG such that the molar fraction of the source gas Gn is maintained constant inside the chamber 3.

  Here, it is preferable that the gas supply device 60A supply the diluted mixed gas UM to the vapor phase growth apparatus 1 instead of the mixed gas MG. The diluted mixed gas UM is a gas obtained by mixing the mixed gas MG and the carrier gas CG and diluting the mixed gas MG with the carrier gas CG.

  Next, referring to FIG. 7, the mode in which diluted mixed gas UM is supplied to vapor phase growth apparatus 1 instead of mixed gas MG mainly differs from the mode in which mixed gas MG is supplied in vapor phase growth apparatus 1. explain.

  The raw material inlet pipe A1 supplies a diluted mixed gas UM. Therefore, the raw material introduction port GP1 introduces the diluted mixed gas UM into the chamber 3 through the raw material introduction pipe A1. That is, the gas supply device 60A supplies the diluted mixed gas UM to the chamber 3 through the raw material inlet pipe A1 and the raw material inlet port GP1.

  Specifically, the gas supply device 60A supplies the diluted mixed gas UM containing the mixed gas MG of the fifth predetermined amount M5 to the chamber 3, and then shuts off the flow path of the diluted mixed gas UM to the chamber 3. Stop the supply of diluted mixed gas UM. In other words, after the diluted mixed gas UM containing the mixed gas MG of the fifth predetermined amount M5 is introduced into the chamber 3, the flow path of the diluted mixed gas UM is blocked, and from the raw material inlet pipe A1 and the raw material inlet port GP1. The introduction of the diluted mixed gas UM is stopped.

  Further, the gas supply device 60A supplements the diluted mixed gas UM to the chamber 3 through the raw material introduction pipe A1 and the raw material introduction port GP1 according to the amount of reduction of the mixed gas MG resulting from the chemical reaction inside the chamber 3. . In addition, when replenishing the diluted mixed gas UM, the gas supply device 60A replenishes the diluted mixed gas UM such that the molar fraction of the source gas Gn is maintained constant inside the chamber 3.

  Specifically, the gas supply device 60A performs the dilution mixing including the mixed gas MG of the sixth predetermined amount M6 through the raw material inlet pipe A1 and the raw material inlet port GP1 according to the amount of reduction of the mixed gas MG inside the chamber 3. The gas UM is supplied to the chamber 3.

  Then, after the diluted mixed gas UM containing the mixed gas MG of the sixth predetermined amount M6 is replenished, the gas supply device 60A cuts off the flow path of the diluted mixed gas UM, and the raw material inlet pipe A1 and the raw material inlet port GP1. Stop the replenishment of the diluted mixed gas UM to the chamber 3.

  Note that, after the diluted mixed gas UM including the mixed gas MG of the fifth predetermined amount M5 is supplied to the gas supply device 60A, the reduced amount of mixed gas MG resulting from the chemical reaction in the chamber 3 is supplied. The diluted mixed gas UM may be constantly replenished through the raw material introduction pipe A1 and the raw material introduction port GP1.

  For example, when the amount of the mixed gas MG in the chamber 3 becomes smaller than the threshold value Th3, the gas supply device 60A performs dilution and mixing including the mixed gas MG according to the amount of reduction of the mixed gas MG in the chamber 3. The gas UM may be constantly replenished from the raw material introduction port GP1.

  Also, for example, when constantly replenishing the diluted mixed gas UM, the gas supply device 60A constantly replenishes the diluted mixed gas UM such that the mole fraction of each of the source gases Gn is maintained constant inside the chamber 3. You may

  The gas supply device 60A may always replenish the carrier gas CG when constantly replenishing the diluted mixed gas UM. In addition, the gas supply device 60A may always replenish the etching gas EG when constantly replenishing the diluted mixed gas UM.

  When the by-product exhaust unit 15 exhausts the by-product FG together with the source gas Gn, the carrier gas CG, and the etching gas when the concentration of the by-product FG becomes larger than the threshold Th2, the gas supply device 60A generates the source gas The diluted mixed gas UM is refilled into the chamber 3 according to the amount of decrease of Gn. When replenishing the diluted mixed gas UM, the gas supply device 60A replenishes the diluted mixed gas UM so that the molar fraction of the source gas Gn is maintained constant inside the chamber 3.

  Hereinafter, in the second embodiment, the gas supply device 60A supplies the diluted mixed gas UM to the vapor phase growth apparatus 1, instead of the mixed gas MG, unless otherwise specified.

  Next, the gas supply device 60A will be described with reference to FIG. FIG. 7 is a view showing a gas supply device 60A. As shown in FIG. 7, the gas supply device 60A includes a vacuum pump 61, a control unit 62, a thermostatic bath 63 (temperature control unit), a pressure adjustment unit 64A, and a first flow control unit Q1 (flow control unit). , A second flow rate control unit 72, and a third flow rate control unit 73. The pressure adjustment unit 64A includes a dilution container X1, a valve unit Y1 (introduction part), and a plurality of raw material containers Zn (a plurality of gas containers). Then, the gas supply device 60A supplies the gas to the vapor deposition apparatus 1 (FIG. 7). In the present specification, the valve portion Y1 is an example of the introduction portion, and the raw material container Zn is an example of the gas container.

  The control unit 62 controls the vacuum pump 61, the thermostat 63, the valve unit Y1, the first flow control unit Q1, the second flow control unit 72, and the third flow control unit 73. That is, the vacuum pump 61, the thermostat 63, the valve Y1, the first flow control unit Q1, the second flow control unit 72, and the third flow control unit 73 operate under the control of the control unit 62. The control unit 62 includes a processor and a storage device. Therefore, the processor executes the computer program stored in the storage device, whereby the vacuum pump 61, the thermostat 63, the valve Y1, the first flow control unit Q1, the second flow control unit 72, and the third flow control unit Control 73

  The constant temperature bath 63 controls the temperature of the pressure adjustment unit 64A, and maintains the temperature of the pressure adjustment unit 64A at a constant temperature. The pressure adjustment unit 64 </ b> A is disposed inside the thermostatic bath 63.

  The pressure adjustment unit 64A dilutes the mixed gas MG obtained by mixing a plurality of source gases Gn with the carrier gas CG to generate a diluted mixed gas UM. Then, the pressure adjustment unit 64A discharges the diluted mixed gas UM containing the mixed gas MG. In addition, when generating the diluted mixed gas UM, the pressure adjusting unit 64A adjusts the partial pressure of the carrier gas CG and the partial pressure of each of the source gas Gn inside the dilution container X1.

  Specifically, the plurality of source containers Zn respectively store a plurality of source gases Gn (a plurality of gases different from each other) different from each other. The source gas Gn is a non-diluted pure source gas, and has a constant pressure (vapor pressure) inside the source container Zn.

  The valve portion Y1 introduces a plurality of different source gases Gn at different timings from the plurality of source containers Zn to the dilution container X1, and also differs in the carrier gas CG for diluting the plurality of source gases Gn from the plurality of source gases Gn It is introduced into the dilution container X1 at the timing. As a result, in the dilution container X1, a diluted mixed gas UM in which the plurality of source gases Gn and the carrier gas CG are mixed is generated.

  For example, the valve unit Y1 introduces a plurality of different source gases Gn from the plurality of source containers Zn into the dilution container X1 at different timings. As a result, mixed gas MG obtained by mixing a plurality of source gases Gn is accommodated in dilution container X1. Then, the valve unit Y1 introduces the carrier gas CG into the dilution container X1 at a timing different from that of the plurality of source gases Gn. As a result, in the dilution container X1, a diluted mixed gas UM in which the mixed gas MG and the carrier gas CG are mixed is generated.

  In addition, the valve unit Y1 adjusts the partial pressure of each source gas Gn and the partial pressure of the carrier gas CG in the dilution container X1. As a result, in the dilution container X1, the total pressure p of the diluted mixed gas UM is set to a predetermined total pressure value, the partial pressure pgn of the source gas Gn is set to a first partial pressure value, and the partial pressure pc of the carrier gas CG is It is set to the second partial pressure value. The first partial pressure value is determined for each source gas Gn based on a chemical reaction formula when a plurality of different source gases Gn chemically react. In the case where the plurality of partial pressures pgn are described separately, they are described as partial pressure pg1,..., PgN (N is an integer of 2 or more). Therefore, p = pg1 +, ..., + pgN + pc.

  The dilution container X1 mixes the plurality of source gases Gn respectively introduced from the plurality of source containers Zn and the carrier gas CG, and stores the mixture as a diluted mixed gas UM (dilution gas). Then, after the plurality of raw material gases Gn and the carrier gas CG are mixed, the valve unit Y1 releases the diluted mixed gas UM from the dilution container X1. That is, after the plurality of source gases Gn and the carrier gas CG are mixed, and the partial pressure pgn of each source gas Gn and the partial pressure pc of the carrier gas CG are adjusted, the valve portion Y1 is a diluted mixed gas UM. Are discharged from the dilution container X1.

  In the present specification, the diluted mixed gas UM is a diluted gas obtained by mixing the gas (specifically, the mixed gas MG) to be supplied to the vapor phase growth apparatus 1 by the gas supply device 60A and the carrier gas CG. An example of

  The first flow rate control unit Q1 is provided corresponding to the valve unit Y1. Further, the first flow rate control unit Q1 is provided corresponding to the raw material introduction pipe A1 (FIG. 7).

  The first flow rate control unit Q1 controls the flow rate of the diluted mixed gas UM released by the valve unit Y1. Then, the first flow rate control unit Q1 supplies the diluted mixed gas UM to the chamber 3 through the raw material introduction pipe A1. Specifically, the first flow rate control unit Q1 utilizes the Hagen Poiseil principle, and based on the differential pressure between the upstream side and the downstream side of the laminar flow element, the volumetric flow rate or mass flow rate of the diluted mixed gas UM Control.

  As described above with reference to FIG. 8, according to the second embodiment, since the carrier gas CG is introduced into the dilution container X1, as compared with the case where only the mixed gas MG is introduced into the dilution container X1. The total pressure p of the diluted mixed gas UM can be increased. Therefore, compared with the case where only the mixed gas MG is introduced into the dilution container X1, the mixed gas MG moves easily toward the first flow rate control unit Q1 and the vapor phase growth apparatus 1. That is, the force to move the mixed gas MG (that is, the source gas Gn) is secured by the total pressure p of the diluted mixed gas UM in the dilution container X1. On the other hand, each raw material gas Gn is included in the diluted mixed gas UM in the dilution container X1 by adjusting the amount (quantity, volume or mass) of the raw material gas Gn to be introduced into the dilution container X1 from the raw material container Zn. The amount of the source gas Gn (quantity of substance, volume, or mass) can be adjusted with high accuracy.

  As a result, compared to the case where the flow rate of the carrier gas is controlled to flow the carrier gas and the supply amount of the source gas is adjusted, as in a general film forming apparatus, the first flow rate control unit Q1 and the vapor phase growth apparatus The amount (quantity of substance, volume, or mass) of the source gas Gn to be moved together with the carrier gas CG toward 1, the supply amount of the source gas Gn can be accurately adjusted. Further, in order to discharge the diluted mixed gas UM from the dilution container X1, the supply amount of the source gas Gn is more accurate than in the case where the source gas is directly supplied from the bubbler to the gas supply destination like a general film forming apparatus. It can be adjusted well. Since the supply amount of the source gas Gn can be accurately adjusted, the vapor deposition apparatus 1 can form a target substance with high quality (for example, a target substance with few defects and high purity).

  Further, according to Embodiment 2, the force for moving the source gas Gn is secured by the total pressure p of the diluted mixed gas UM in the dilution container X1, and the diluted mixed gas UM containing the source gas Gn is diluted in the dilution container X1. Released from Therefore, as in the first embodiment, the supply amount of the source gas Gn is not easily influenced by the temperature, and the temperature management is easy. Further, in the second embodiment, for the same reason as the first embodiment, the supply amount of the source gas Gn can be adjusted with higher accuracy, and the cost of the gas supply device 60A can be reduced. Furthermore, in the second embodiment, for the same reason as the first embodiment, an increase in the maintenance cost can be suppressed, and the limitation of the shape of the raw material container Zn can be suppressed.

  Furthermore, according to Embodiment 2, as in Embodiment 1, a small amount of mixed gas MG (that is, a small amount of source gas Gn) can be easily supplied. Further, in the second embodiment, since the diluted mixed gas UM containing the source gas Gn is released from the dilution container X1, the supply amount of the source gas Gn is stable as in the first embodiment.

  Further, according to the second embodiment, the total pressure p of the diluted mixed gas UM can be adjusted by adjusting the amount of introduction of the carrier gas CG into the dilution container Xn. That is, the force of moving the mixed gas MG (that is, the source gas Gn) can be adjusted.

  Furthermore, according to the second embodiment, by adjusting the partial pressure pgn of the source gas Gn in the dilution container X1, the amount (quantity, volume or mass) of the source gas Gn contained in the diluted mixed gas UM can be determined. It can be adjusted. As a result, the amount (quantity of substance, volume, or mass) of the source gas Gn to be moved together with the carrier gas CG toward the first flow rate control unit Q1 and the vapor deposition apparatus 1 can be adjusted more accurately.

  Furthermore, according to the second embodiment, since the plurality of source containers Zn are provided, the amount of source gas Gn to be introduced into the dilution container X1 can be adjusted for each source container Zn. Therefore, the source gas Gn can be introduced into the dilution container X1 such that each of the source gases Gn has a molar fraction based on a chemical reaction formula for producing the target substance. That is, when the source gas Gn is supplied to the vapor phase growth apparatus 1, the mole fraction of the source gas Gn can be easily adjusted.

  Furthermore, according to Embodiment 2, a plurality of source gases Gn from a plurality of source containers Zn are mixed in one dilution container X1, and carrier gas CG is introduced to further dilute the mixed gas in one dilution container X1. UM is generated. Therefore, the configuration of the gas supply device 60A can be simplified as compared to the case where the plurality of dilution containers Xn are provided for the plurality of raw material containers Zn. For example, the number of dilution containers Xn and the number of valve portions Yn can be reduced.

  Furthermore, according to Embodiment 2, the pressure (vapor pressure) of the source gas Gn inside the source container Zn can be used to move the source gas Gn from the source container Zn to the dilution container X1. Therefore, it is possible to suppress the installation of an active device for moving the source gas Gn from the source container Zn to the dilution container X1. As a result, the gas supply device 60A can be simplified, and the cost of the gas supply device 60A can be reduced.

  Furthermore, according to the second embodiment, the first flow rate control unit Q1 can easily supply the diluted mixed gas UM to the vapor phase growth apparatus 1 using the total pressure p of the diluted mixed gas UM.

  The dilution container X1 can also accommodate the mixed gas MG by introducing a plurality of source gases Gn from a plurality of source containers Zn without introducing the carrier gas CG. In this case, the first flow rate control unit Q1 can also control the flow rate of the mixed gas MG released by the valve unit Y1. Then, the first flow rate control unit Q1 can also supply the mixed gas MG to the chamber 3 through the raw material introduction pipe A1. Specifically, the first flow rate control unit Q1 utilizes the Hagen Poiseil principle, and based on the differential pressure between the upstream side and the downstream side of the laminar flow element, the volumetric flow rate or mass flow rate of the mixed gas MG is It can also be controlled.

  Next, with reference to FIG. 9, the pressure adjustment unit 64A will be described. FIG. 9 is a view showing a pressure adjustment unit 64A. As shown in FIG. 9, the pressure adjusting unit 64A further includes a thermometer TM, a first pressure gauge PM1 (pressure gauge), a second pressure gauge PM2, a tube t1 to a tube t4 and a plurality of tubes t5n. .

  The valve portion Y1 includes a first valve unit 75 and a plurality of second valve units 77n. The first valve unit 75 includes valves b1 to b7 and tubes t1 to t4. The second valve unit 77n includes a valve b8n and a pipe t5n. The valves b1 to b7 and the valve b8 n are, for example, stop valves. The plurality of second valve units 77 n are provided corresponding to the plurality of source containers Zn, respectively.

  The pipe t1 connects the dilution container X1 and the valve b4. The pipe t2 interconnects the valve b3 to the valve b7. The pipe t3 mutually connects the valve b1 to the valve b3. The pipe t4 mutually connects the valve b7 and the plurality of valves b8n. The pipe t5n connects the valve t8n and the raw material container Zn. The valve t8 n may be directly connected to the raw material container Zn. The valve b4 and the dilution container X1 may be directly connected.

  In addition, when distinguishing and demonstrating several 2nd valve unit 77n, it describes as 2nd valve unit 771, ..., 77N (N is an integer greater than or equal to 2). When the plurality of valves t8 n are described separately, they are described as valves t81,..., T8 N (N is an integer of 2 or more). When the plurality of tubes t5n are described separately, they are described as tubes t51,..., T5N (N is an integer of 2 or more).

  Continuing to refer to FIG. 9, the control procedure of the valve portion Y1 will be described. The control procedure includes first to twenty-second procedures. In the initial state of the valve portion Y1, the valves b1 to b7 and the valve b8 n are closed. Hereinafter, for the convenience of understanding, a control procedure of the valve portion Y1 when the two raw material containers Zn and the two second valve units 77n are provided will be described.

[Vacuum evacuation and purge]
The first to fourth procedures are the same as the first to fourth procedures of the first embodiment.

[Introduction of raw material gas G1 into dilution container X1]
Fifth procedure: Close the valves b2, b6 and b7 and open the valve b81.

  Sixth procedure: The opening and closing of the valve b7 is repeated to introduce the source gas G1 from the source container Z1 into the dilution container X1. When introducing the source gas G1 into the dilution container X1, the opening time and closing time of the valve b7 are adjusted, and the pressure pg1 of the source gas G1 inside the dilution container X1 is set to the first partial pressure value. The pressure pg1 is expressed by equation (5). “V” indicates the internal volume of the dilution vessel X1, “ng1” indicates the amount of substance (moles) of the source gas G1, “R” indicates the gas constant, and “T” indicates the temperature inside the dilution vessel X1 Indicates

  pg1 × V = ng1 × R × T (5)

  The volume V and the temperature T are known, and the pressure pg1 can be measured by the first pressure gauge PM1. Therefore, the amount of substance of the source gas G1 inside the dilution container X1 can be calculated based on the equation (5).

  According to the second embodiment, the temperature of the dilution container X1 and the partial pressure of the raw material gas G1 are monitored by monitoring the temperature of the dilution container X1 with a thermometer TM and monitoring the pressure of the dilution container X1 with a first pressure gauge PM1. It is possible to control pg1 to a desired value. As a result, it is possible to introduce a desired amount of the raw material gas G1 into the dilution container X1.

  When the pressure pg1 of the source gas G1 is low, the valve b6 may be opened and the pressure pg1 may be measured by the second pressure gauge PM2.

  Seventh procedure: When the pressure pg1 of the raw material gas G1 reaches the first partial pressure value, the valve b7 is closed.

  Eighth procedure: Close the valves b4 and b81 and open the valves b2, b3 and b7.

  Ninth procedure: Open the valve b6. The second pressure gauge PM2 measures the pressure in the tubes t2, t3 and t4. The operator confirms the degree of vacuum inside the tubes t2, t3 and t4 by the second pressure gauge PM2.

[Introduction of raw material gas G2 into dilution container X1]
Tenth procedure: Close the valves b2, b3, b6 and b7 and open the valve b82.

  Eleventh procedure: Open the valve b4.

  Twelfth procedure: The source gas G2 is introduced from the source container Z2 into the dilution container X1 by repeating opening and closing of the valve b7. When the source gas G2 is introduced into the dilution container X1, the opening time and closing time of the valve b7 are adjusted to set the total pressure pm of the mixed gas MG inside the dilution container X1 to the first total pressure value. . The total pressure pm is expressed by equation (6). “Pg1” indicates the pressure of the source gas G1 in the dilution container X1, that is, the partial pressure of the source gas G1, and “pg2” indicates the partial pressure of the source gas G2 in the dilution container X1.

  pm = pg1 + pg2 (6)

  Since the total pressure pm and the partial pressure pg1 have been measured, the partial pressure pg2 of the source gas G2 can be calculated based on the equation (6).

  Further, the total pressure pm is expressed by equation (7). “V” indicates the internal volume of the dilution container X1, “ng1” indicates the amount of substance (mol) of the source gas G1, “ng2” indicates the amount of substance (mol) of the source gas G2, and “R” indicates The gas constant is indicated, and "T" indicates the temperature inside the dilution vessel X1.

  pm × V = (ng1 + ng2) × R × T (7)

  Since the volume V and the temperature T are known, the total pressure pm can be measured by the first pressure gauge PM1, and the substance mass ng1 can be calculated based on the equation (5), the substance of the raw material gas G2 inside the dilution container X1 The amount ng2 can be calculated based on the equation (7).

  According to the second embodiment, the temperature of the dilution container X1 and the partial pressure of the raw material gas G2 are monitored by monitoring the temperature of the dilution container X1 with the thermometer TM and monitoring the pressure of the dilution container X1 with the first pressure gauge PM1. It is possible to control pg2 to a desired value. As a result, it is possible to introduce a desired amount of material gas G2 into the dilution container X1.

  If the pressure pg2 of the source gas G2 is low, the valve b6 may be opened to measure the total pressure pm by the second pressure gauge PM2.

  Thirteenth Procedure: When the total pressure pm of the mixed gas MG reaches the first total pressure value, the valve b7 is closed. That is, when the partial pressure pg2 of the source gas G2 becomes the first partial pressure value, the valve b7 is closed. The first partial pressure value is determined individually for the source gas G1 and the source gas G2.

[Introduction of carrier gas CG into dilution vessel X1]
Fourteenth Procedure: Close the valves b4 and b82 and open the valves b2, b3 and b7.

  15th procedure: Open valve b6. The second pressure gauge PM2 measures the pressure in the tubes t2, t3 and t4. The operator confirms the degree of vacuum inside the tubes t2, t3 and t4 by the second pressure gauge PM2.

  Sixteenth procedure: Close the valves b2 and b6 and open the valve b1.

  Seventeenth Procedure: The carrier gas CG is introduced into the dilution container X1 by repeating opening and closing of the valve b4. When the carrier gas CG is introduced into the dilution container X1, the opening time and closing time of the valve b4 are adjusted to adjust the total pressure p of the diluted mixed gas UM inside the dilution container X1 to the second total pressure value (that is, , Predetermined total pressure value). The total pressure p is expressed by equation (8). "V" indicates the internal volume of the dilution vessel X1, "n" indicates the amount of substance (moles) of the diluted mixed gas UM, "R" indicates the gas constant, and "T" indicates the interior of the dilution vessel X1 Indicates the temperature. Specifically, “n” is the sum of the substance mass (mol) of the carrier gas CG inside the dilution vessel X1, the substance mass (mol) of the source gas G1, and the substance mass (mol) of the source gas G2 is there.

  p × V = n × R × T (8)

  The volume V and the temperature T are known, and the total pressure p can be measured by the first pressure gauge PM1, so the substance mass n of the diluted mixed gas UM inside the dilution container X1 can be calculated based on the equation (8) . Further, since the substance mass ng1 of the source gas G1 and the substance mass ng2 of the source gas G2 are known, the substance mass nc of the carrier gas CG can be calculated based on the equation (9).

  n = ng 1 + ng 2 + nc (9)

  According to the second embodiment, by monitoring the temperature of the dilution container X1 with a thermometer TM and monitoring the pressure of the dilution container X1 with a first pressure gauge PM1, the temperature of the dilution container X1 and all of the diluted mixed gas UM are monitored. The pressure p can be controlled to a desired value.

  Also, the partial pressure pc of the carrier gas CG can be calculated from the equation (10). “Pg1” indicates the pressure of the source gas G1 inside the dilution container X1, that is, the partial pressure of the source gas G1, “pg2” indicates the pressure of the source gas G2 inside the dilution container X1, that is, the source The partial pressure of gas G2 is shown.

  p = pg1 + pg2 + pc (10)

  The molar fraction of the source gas G1, the source gas G2 based on the total pressure p, partial pressure pg1, partial pressure pg2, and partial pressure pc, or substance mass n, substance mass ng1, substance mass ng2, and substance mass nc And the molar fraction of the carrier gas CG can be calculated.

  Eighteenth procedure: When the total pressure p of the diluted mixed gas UM reaches the second total pressure value, the valve b4 is closed. That is, when the partial pressure pc of the carrier gas CG becomes the second predetermined value, the valve b4 is closed.

[Supply of diluted source gas Dn to vapor phase growth apparatus 1]
Nineteenth procedure: The valve b5 may be opened. As a result, the flow path from the valve b5 to the first flow rate control unit Q1 is cleaned (purge) by the carrier gas CG.

  Twentieth procedure: Close the valves b1, b5 and b7 and open the valve b2.

  Step 21: Open the valve b6. The second pressure gauge PM2 measures the pressure in the tubes t2 and t3. The operator confirms the degree of vacuum inside the tubes t2 and t3 by the second pressure gauge PM2. When the flow path volume of the tubes t2 and t3 is smaller than the volume of the dilution container X1, the fifteenth procedure is unnecessary.

  Twenty-second procedure: Close the valves b2, b3 and b6 and open the valves b4 and b5. As a result, the diluted mixed gas UM is discharged from the dilution container X1 toward the first flow rate control unit Q1 (FIG. 8).

Next, with reference to FIG. 10, an example of forming gallium nitride (GaN) as a target substance on the substrate S will be described. FIG. 10 shows a part of the vapor phase growth system 100. As shown in FIG. As shown in FIG. 10, the diluted mixed gas UM is accommodated in the dilution container X1. The diluted mixed gas contains gallium trichloride (GaCl ₃ ) as the source gas G1, ammonia (NH ₃ ) as the source gas G2, and nitrogen (N ₂ ) as the carrier gas CG. Further, nitrogen (N ₂ ) as the carrier gas CG is supplied to the second flow rate control unit 72. The third flow rate control unit 73 is supplied with chlorine (Cl ₂ ) as the etching gas EG.

  In the initial state, the first flow rate control unit Q1 closes the raw material introduction pipe A1, the second flow rate control unit 72 closes the carrier introduction pipe 19, and the third flow rate control unit 73 closes the etching introduction pipe 21. The substance discharge device 80 closes the residue discharge pipe 25, and the byproduct exhaust part 15 closes the byproduct exhaust pipe 27.

  The first flow control unit Q1, the second flow control unit 72, and the third flow control unit 73 respectively open the raw material introduction pipe A1, the carrier introduction pipe 19, and the etching introduction pipe 21. As a result, the diluted mixed gas UM is introduced into the chamber 3 from the dilution container X1, and the carrier gas CG and the etching gas EG are introduced into the chamber 3.

  In the second embodiment described with reference to FIG. 10, gallium nitride (GaN) as a target substance is grown on the substrate S, as in the first embodiment described with reference to FIG. Then, as in the first embodiment, the utilization efficiency of gallium trichloride (G1) and ammonia (G2) can be improved. Further, as in the first embodiment, the growth rate of gallium nitride can be improved. Furthermore, as in the first embodiment, the residue ZG in the chamber 3 can be evacuated to clean the inside of the chamber 3.

(Modification)
Next, a gas supply device 60A according to a modification of the second embodiment of the present invention will be described with reference to FIG. The modification differs from Embodiment 2 in that the dilution container X1 and the first valve unit 75, the temperature control, and the temperature control of the raw material container Zn and the second valve unit 77n can be individually performed. The differences between the modification example and the second embodiment will be mainly described below.

  FIG. 11 is a view showing a part of the gas supply device 60A. As shown in FIG. 11, the gas supply device 60A according to the modification is replaced by a first thermostat 63A (a first temperature control unit) and a plurality of second thermostats 63Bn (a first thermostat) instead of the thermostat 63 shown in FIG. And a second temperature control unit). In addition, when distinguishing and demonstrating several 2nd thermostatic bath 63 Bn, it describes as 2nd thermostatic bath 63 B1, ..., 63 BN (N is an integer greater than or equal to 2).

  The first constant temperature bath 63A collectively controls the temperature of the dilution container X1 and the temperature of the first valve unit 75, and keeps the temperature of the dilution container X1 and the temperature of the first valve unit 75 constant (for example, a first temperature) Hold on. The first constant temperature bath 63A controls the temperatures of the dilution container X1 and the first valve unit 75 independently of the second constant temperature bath 63Bn. The dilution container X1 and the first valve unit 75 are disposed inside the first thermostatic bath 63A.

  The first constant temperature bath 63A preferably holds the temperatures of the dilution container X1 and the first valve unit 75 at a temperature higher than a temperature at which a vapor pressure corresponding to the partial pressure of the source gas Gn inside the dilution container X1 is obtained. . This is to suppress the liquefaction or solidification of the source gas Gn.

  The plurality of second constant temperature baths 63Bn are provided corresponding to the plurality of raw material containers Zn, respectively. That is, the plurality of second constant temperature baths 63Bn are provided corresponding to the plurality of second valve units 77n, respectively. The raw material container Zn and the second valve unit 77n are disposed inside the corresponding second thermostatic bath 63Bn.

  The second constant temperature bath 63Bn collectively controls the temperature of the corresponding raw material container Zn and the corresponding second valve unit 77n, and keeps the temperature of the corresponding raw material container Zn and the temperature of the corresponding second valve unit 77n constant. Hold at a temperature (eg, a second temperature). Each of the second thermostatic baths 63Bn independently controls the temperature of the corresponding raw material container Zn and the corresponding second valve unit 77n. Further, each of the second constant temperature baths 63Bn controls the temperature of the corresponding raw material container Zn and the corresponding second valve unit 77n independently of the first constant temperature bath 63A.

  As described above with reference to FIG. 11, according to the modification of the second embodiment, since the second constant-temperature tank 63Bn is provided separately from the first constant-temperature tank 63A, the dilution container X1 and the first valve are provided. The temperature of the source container Zn can be controlled independently of the temperature of the unit 75. Therefore, the pressure (vapor pressure) of the source gas Gn inside the source container Zn can be adjusted to a desired value. For example, the second thermostatic bath 63Bn sets the temperature of the raw material container Zn to a temperature higher than the temperature of the dilution container X1. As a result, the pressure (vapor pressure) of the source gas Gn inside the source container Zn can be increased.

  When the pressure (vapor pressure) of the source gas Gn inside the source container Zn can be adjusted to a desired value, the pressure range of the source gas Gn in the dilution container X1 can be expanded. As a result, the degree of freedom of the supply amount of the diluted mixed gas UM can be improved, and the conditions for forming the target substance on the substrate S can be expanded. In addition, a sufficient total pressure p of the diluted mixed gas UM in the dilution container X1 can be secured, and the diluted mixed gas UM can be stably supplied to the first flow rate control unit Q1.

  Further, according to the modification, since the plurality of second constant temperature baths 63Bn are provided, the temperature of the raw material container Z can be controlled for each raw material container Zn. Therefore, the pressure (vapor pressure) of the source gas Gn in the source container Zn can be adjusted to a desired value for each source container Zn.

  Note that the plurality of raw material containers Zn and the plurality of second valve units 77n may be disposed inside one second thermostatic bath 63B1. Then, the second constant temperature bath 63B1 may control the temperatures of the plurality of raw material containers Zn and the plurality of second valve units 77n collectively.

  The embodiments of the present invention have been described above with reference to the drawings. However, this invention is not limited to said embodiment, It is possible to implement in a various aspect in the range which does not deviate from the summary (for example, following (1)-(4)). In addition, various inventions can be formed by appropriately combining the plurality of components disclosed in the above-described embodiments. For example, some components may be deleted from all the components shown in the embodiment. The drawings schematically show the respective components mainly for the purpose of easy understanding, and the number of the respective components illustrated may be different from the actual for the convenience of drawing preparation. In addition, each component shown in the above-described embodiment is an example, is not particularly limited, and various modifications can be made without substantially departing from the effects of the present invention.

  (1) The volume changing unit 90 and the pressure adjusting unit 91 described with reference to FIG. 5 may be provided in the pressure adjusting unit 64nB described with reference to FIG. 6, or with reference to FIGS. It may be provided in the pressure adjustment unit 64A described. Further, the plurality of dilution containers Xmn and the plurality of valves b4 described with reference to FIG. 6 may be provided in the pressure adjustment unit 64A described with reference to FIGS. 9 and 11. Furthermore, the first thermostatic bath 63A and the second thermostatic bath 63B1 described with reference to FIG. 11 are replaced with the thermostatic bath 63 described with reference to FIG. 3, FIG. 5 and FIG. And the gas supply device 60 described with reference to FIG. In addition, the first embodiment, the first variation of the first embodiment, the second variation of the first embodiment, the second embodiment, and the variations of the second embodiment can be combined as appropriate.

  (2) In the vapor phase growth apparatus 1 described with reference to FIGS. 1 to 11, the target substance formed on the substrate S may be an inorganic compound or an organic compound, and is not particularly limited. Also, the target substance may be a thin film or a bulk, and is not particularly limited. Furthermore, the type of source gas Gn is not particularly limited. In addition, the by-product exhaust unit 15 can also discharge liquid or solid by-products.

  The by-product detection unit 13 and the by-product exhaust unit 15 may not be provided. The etching gas EG may not be introduced into the chamber 3 from the etching introduction port EP. The carrier gas CG may not be introduced into the chamber 3 from the carrier introduction port CP. The wall 8 and the cooling unit 17 may not be provided. The positions of the material introduction port GPn, the carrier introduction port CP, the etching introduction port EP, the residue discharge port ZP, and the byproduct exhaust port FP are not particularly limited. The position of the holding portion 5 is not particularly limited. Moreover, although the thermostat 63, the 1st thermostat 63A, and the 2nd thermostat 63Bn were mentioned as an example of a temperature control part, a temperature control part is not limited to these, For example, a heater may be sufficient.

  (3) In the vapor phase growth apparatus 1 described with reference to FIGS. 1 to 11, the capacities of the plurality of dilution vessels Xn may be the same or different. Further, the capacities of the plurality of raw material containers Zn may be the same or different. Further, in the vapor phase growth apparatus 1 described with reference to FIG. 6, the volumes of the plurality of dilution vessels Xmn may be the same or different. Further, the concentrations of the source gases Gn stored in the plurality of dilution containers Xmn may be the same or different. Therefore, the valve unit Yn may introduce the source gas Gn and the carrier gas CG for each dilution container Xmn so that the concentrations of the source gas Gn stored in the plurality of dilution containers Xmn are the same. Further, the valve portion Yn may introduce the source gas Gn and the carrier gas CG for each dilution container Xmn so that the concentrations of the source gas Gn stored in the plurality of dilution containers Xmn are different. The carrier gas CG introduced into the dilution container Xn, the dilution container Xmn, or the dilution container X1 may be different from the carrier gas CG introduced into the chamber 3 from the carrier introduction port CP.

  (4) The gas supply destination by the gas supply device 60 and the gas supply device 60A described with reference to FIGS. 2, 3, 5, 6, 8, 9, and 11 is the vapor phase growth device 1 The gas supply device 60 and the gas supply device 60A may supply, for example, a gas to be supplied to any gas supply destination (for example, a device or a substance). Further, the type of the source gas Gn is not particularly limited either, and various gases can be supplied instead of the source gas Gn. The first flow rate control unit Qn, the second flow rate control unit 72, and the third flow rate control unit 73 can also be understood as the configuration of the vapor deposition apparatus 1.

  For example, the gas supply device 60 and the gas supply device 60A can supply gas to various analysis devices (for example, micro analysis devices). For example, the gas supply device 60 and the gas supply device 60A can be used in the chemical biology field or the medical field. For example, the gas supply device 60 and the gas supply device 60A can supply gas to the bioreactor, supply gas to the cell culture device, and supply gas to the microreactor.

  In the gas supply device 60 described with reference to FIGS. 2, 3, 5, and 6, a single pressure adjustment unit 64n may be provided, or a single pressure adjustment unit 64nA may be provided. A single pressure adjustment unit 64nB may be provided, or a single first flow control unit Qn may be provided. In the gas supply device 60A described with reference to FIGS. 8, 9 and 11, a single source container Zn may be provided, or a single second thermostatic bath 63Bn may be provided.

  The present invention relates to a vapor deposition apparatus and a vapor deposition system, and has industrial applicability.

DESCRIPTION OF SYMBOLS 1 vapor phase growth apparatus 3 chamber 5 holding part 7 heating part 10 opening 13 by-product detection part 15 by-product exhaust part 60, 60A gas supply apparatus Xn, Xmn, X1 dilution container Yn, Y1 valve part (introduction part)
Zn material container GPn, GP1 material introduction port CP carrier introduction port EP etching introduction port

Claims (12)

A vapor phase growth apparatus for causing a chemical reaction of a plurality of different source gases to form a substance on a substrate,
With the chamber,
A holding unit disposed inside the chamber and holding the substrate;
And a heating unit for heating the substrate.
The chamber includes at least one source introduction port for introducing the source gas into the chamber,
A vapor phase growth apparatus in which the flow of the source gas from the inside to the outside of the chamber is blocked during part or all of a period in which the substance is formed on the substrate.   The vapor deposition apparatus according to claim 1, further comprising a byproduct exhaust unit that exhausts byproducts generated by causing the plurality of source gases to chemically react from the inside of the chamber to the outside. It further comprises a by-product detection unit that detects the concentration of the by-product inside the chamber,
The vapor deposition apparatus according to claim 2, wherein the byproduct exhaust unit exhausts the byproduct in accordance with the concentration of the byproduct. The source gas is replenished from the source introduction port according to the amount of decrease of the source gas due to a chemical reaction inside the chamber.
The raw material gas is replenished so that the mole fraction of each raw material gas is maintained constant inside the chamber when the raw material gas is replenished. The vapor phase growth apparatus according to any one of the preceding claims. A predetermined amount is determined for each of the source gases,
After the predetermined amount of the source gas is introduced into the chamber, the flow path of the source gas is shut off, and the introduction of the source gas from the source introduction port is stopped.
The source gas is replenished from the source introduction port according to the amount of decrease of the source gas due to a chemical reaction inside the chamber.
The raw material gas is replenished so that the mole fraction of each raw material gas is maintained constant inside the chamber when the raw material gas is replenished. The vapor phase growth apparatus according to any one of the preceding claims. A predetermined amount is determined for each of the source gases,
After the predetermined amount of the raw material gas is introduced into the chamber, the raw material gas is constantly replenished from the raw material introduction port according to the amount of reduction of the raw material gas due to a chemical reaction inside the chamber. ,
The raw material gas is constantly replenished so that the molar fraction of each of the raw material gas is maintained constant inside the chamber when the raw material gas is constantly replenished. The vapor phase growth apparatus according to any one of the above. The chamber includes a plurality of the raw material introduction ports,
The vapor deposition apparatus according to any one of claims 1 to 6, wherein the plurality of source introduction ports introduce the plurality of source gases into the chamber, respectively.   The vapor deposition apparatus according to any one of claims 1 to 6, wherein the source introduction port introduces a mixed gas obtained by mixing the plurality of source gases into the chamber.   The vapor phase growth apparatus according to any one of claims 1 to 8, wherein the chamber further includes a carrier introduction port for introducing a carrier gas into the chamber.   The vapor deposition apparatus according to any one of claims 1 to 9, wherein the chamber further includes an etching introduction port for introducing an etching gas into the chamber. Further comprising a wall having an opening,
The wall portion is disposed between the holding portion in which the heating portion is disposed and an inner wall surface of the chamber.
The vapor phase growth apparatus according to any one of claims 1 to 10, wherein the opening exposes the substrate. The vapor phase growth apparatus according to any one of claims 1 to 11,
And a gas supply device for supplying a gas to the vapor phase growth apparatus.
The gas supply device
A raw material container for containing the raw material gas;
A dilution container for mixing the source gas introduced from the source container and a carrier gas for diluting the source gas, and storing the mixture as a dilution source gas;
And an introduction unit for introducing the source gas and the carrier gas into the dilution container at different timings and releasing the diluted source gas from the dilution container after the source gas and the carrier gas are mixed. , Vapor phase growth system.

Images