TWI682060B - Gas supply apparatus - Google Patents

Abstract

A gas supply apparatus (60) includes a material container (Zn), a thinned gas container (Xn), and a valve (Yn). The material container (Zn) accommodates a material gas (Gn). The material gas (Gn) introduced from the material container (Zn) and a carrier gas (CG) for thinning the material gas (Gn) are mixed together in the thinned gas container (Xn) to be accommodated in the thinned gas container (Xn) as a thinned material gas (Dn). The valve (Yn) is operated to allow the material gas (Gn) and the carrier gas (CG) to be introduced into the thinned gas container (Xn) at different timings. After the material gas (Gn) and the carrier gas (CG) are mixed together, the valve (Yn) is operated to allow the thinned material gas (Dn) to be released from the thinned gas container (Xn).

Description

Gas supply device

The invention relates to a gas supply device.

In the film forming apparatus described in Invention Patent Document 1, raw materials are supplied into a bubbler. Next, while the bubbler is heated by the heater, the carrier gas is flowed to the bubbler, whereby raw material gas is generated from the raw materials in the bubbler. Further, the raw gas system is supplied from the bubbler to the film forming chamber through the carrier gas. The raw material gas is an object to be supplied to the film forming chamber.

[Prior Technical Literature] [Invention Patent Literature]

[Invention Patent Document 1] Japanese Unexamined Patent Publication No. 2002-167672.

However, in the film forming apparatus described in Patent Document 1, the flow controller (Mass Flow Controller) controls the flow rate of the carrier gas while flowing the carrier gas to adjust the supply amount of the source gas. In addition, raw material gas is generated from raw materials in the bubbler, and the raw material gas is directly supplied to the film forming chamber by the bubbler. Therefore, it is difficult to adjust the supply amount of the raw material gas with high accuracy.

In view of the above problems, the present invention aims to provide a gas supply device that can adjust the supply amount of supplied gas with high accuracy.

According to an aspect of the present invention, the gas supply device includes a gas container, a dilution container, and an introduction portion. The gas container contains gas. The dilution container mixes the gas introduced from the gas container and the carrier gas that dilutes the gas, and is accommodated as a dilution gas. The introduction part introduces the gas and the carrier gas into the dilution container at different time points. The introduction part discharges the dilution gas from the dilution container after the gas and the carrier gas are mixed.

In the gas supply device of the present invention, preferably, the gas container contains a raw material gas as the gas. Preferably, the raw material gas system generates a substance gas by chemical reaction.

In the gas supply device of the present invention, preferably, a plurality of the gas containers, a plurality of the dilution containers respectively corresponding to the plurality of gas containers, and a plurality of the introductions corresponding to the plurality of dilution containers respectively unit. Preferably, the plurality of gas containers respectively contain a plurality of different gases. Preferably, each of the dilution containers mixes the gas and the carrier gas introduced from the corresponding gas container, and stores it as the dilution gas. Preferably, each of the introduction parts introduces the gas and the carrier gas into the corresponding dilution container at different time points, and after the gas and the carrier gas are mixed, the dilution gas is removed from the corresponding dilution container discharge.

In the gas supply device of the present invention, preferably, a plurality of the dilution containers corresponding to the gas container are provided. Preferably, each of the dilution containers mixes the gas and the carrier gas introduced from the gas container, and stores it as the dilution gas. Preferably, the introduction part introduces the gas and the carrier gas into the dilution container at different time points for each of the dilution containers in different time periods in which the plurality of dilution containers are allocated respectively. Preferably, the introduction part is for each of the dilution containers, and after the gas and the carrier gas are mixed, the dilution gas is discharged from the dilution container.

In the gas supply device of the present invention, preferably, a plurality of the gas containers are provided. Preferably, the plurality of gas containers respectively contain a plurality of different gases. Preferably, the dilution container mixes the plurality of gases and the carrier gas introduced from the plurality of gas containers, and stores it as the dilution gas. Preferably, the introduction part introduces the plurality of gases into the dilution container at different time points, and after the plurality of gases and the carrier gas are mixed, the dilution gas is discharged from the dilution container.

Preferably, the gas supply device of the present invention further includes a volume changing unit. Preferably, the volume changing unit changes the volume of the gas storage space of the dilution container. Preferably, the gas containing space is a space that can contain gas. Preferably, the volume changing section is arranged inside the dilution container, and the volume of the gas storage space is changed by changing the size of the volume changing section.

Preferably, the gas supply device of the present invention further includes a first temperature control unit that controls the temperature of the gas container, and a second temperature control unit that controls the temperature of the introduction unit.

Preferably, the gas supply device of the present invention further includes a flow rate control section for controlling the flow rate of the dilution gas discharged from the introduction section.

Preferably, the gas supply device of the present invention further includes a thermometer for measuring the temperature inside the dilution container, and a pressure gauge for measuring the pressure inside the dilution container.

According to the present invention, the supply amount of the supplied gas can be adjusted with high accuracy.

1‧‧‧gas growth device

3‧‧‧ chamber

4a‧‧‧Inner bottom

4b‧‧‧Inner wall

4c‧‧‧Inner top surface

5‧‧‧Maintaining Department

7‧‧‧Heating

8‧‧‧ Wall

8a‧‧‧The innermost wall

8b‧‧‧The outermost wall

9‧‧‧Temperature Control Department

9a‧‧‧Power

10‧‧‧ opening

11‧‧‧Power cord

13‧‧‧ Byproduct Detection Department

15‧‧‧ By-product exhaust department

15a‧‧‧Valve

15b‧‧‧Attract the pump

15c‧‧‧Control Department

17‧‧‧Cooling Department

19‧‧‧Carrier introduction tube

21‧‧‧Etching inlet tube

23‧‧‧Power cord outlet tube

25‧‧‧residue discharge pipe

27‧‧‧by-product exhaust pipe

60、60A‧‧‧Gas supply device

61‧‧‧Vacuum pump

62‧‧‧Control Department

63‧‧‧Constant temperature bath

63A‧‧‧The first constant temperature bath

63Bn‧‧‧The second constant temperature bath

64A, 64n, 64nA, 64nB ‧‧‧ pressure adjustment unit

72‧‧‧ 2nd Flow Control Department

73‧‧‧ Third Flow Control Department

75, 75a‧‧‧First valve unit

77, 77n‧‧‧ 2nd valve unit

80‧‧‧ Residue discharge device

90‧‧‧Volume change department

91‧‧‧Pressure Adjustment Department

92‧‧‧ gas containment space

100‧‧‧gas growth system

An, A1, A2‧‧‧ Raw material introduction tube

BG‧‧‧Drive gas

b1, b2, b3, b4, b5, b6, b7, b8, b8n

CG‧‧‧Carrier gas

CP‧‧‧Carrier inlet

Dn, D1, D2

EG‧‧‧Etching gas

EP‧‧‧Etching inlet

EX‧‧‧gas

FG‧‧‧byproduct

FP‧‧‧by-product exhaust

Gn‧‧‧ raw gas

GPn, GP1‧‧‧ Raw material inlet

HS‧‧‧Keep

MG‧‧‧gas mixture

PM1‧‧‧The first pressure gauge

PM2‧‧‧The second pressure gauge

Qn, Q1, Q2‧‧‧The first flow control unit

S‧‧‧Substrate

SP‧‧‧Internal space

TM‧‧‧thermometer

t1, t2, t3, t4, t5, t5n‧‧‧‧tube

UM‧‧‧Dilute mixed gas

WD‧‧‧Window

WT‧‧‧cooling liquid

Xn, Xmn, X1, X2‧‧‧‧Dilution container

Yn, Y1‧‧‧ valve part (introduction part)

Zn‧‧‧Raw material container

ZG‧‧‧ Residue

ZP‧‧‧Residue discharge

FIG. 1 is a schematic diagram of a vapor phase growth system according to Embodiment 1 of the present invention.

FIG. 2 is a schematic diagram of the gas supply device of Embodiment 1. FIG.

FIG. 3 is a schematic diagram of a part of the gas supply device of Embodiment 1. FIG.

FIG. 4 is a schematic diagram of a part of the gas-phase growth system of Embodiment 1. FIG.

FIG. 5 is a schematic diagram of a part of the gas supply device according to the first modification of Embodiment 1. FIG.

FIG. 6 is a schematic diagram of a part of the gas supply device according to the second modification of Embodiment 1. FIG.

7 is a schematic diagram of a vapor phase growth system according to Embodiment 2 of the present invention.

FIG. 8 is a schematic diagram of the gas supply device of Embodiment 2. FIG.

FIG. 9 is a schematic diagram of a part of the gas supply device of Embodiment 2. FIG.

FIG. 10 is a schematic diagram of a part of the gas-phase growth system of Embodiment 2. FIG.

FIG. 11 is a schematic diagram of a part of a gas supply device according to a modification of Embodiment 2. FIG.

The embodiment of the present invention will be described below with reference to the drawings. Incidentally, for the same or equivalent parts in the figure, the same reference symbols are attached without repeating the description.

(Embodiment 1)

FIG. 1 is a schematic diagram of a vapor phase growth system 100 according to Embodiment 1 of the present invention. As shown in FIG. 1, the vapor-phase growth system 100 includes a vapor-phase growth device 1, a gas supply device 60, and a residue discharge device 80. Incidentally, in FIG. 1, for easy understanding, a part of the vapor-phase growth device 1 is shown in cross section. Sections are marked with diagonal lines.

The vapor-phase growth device 1 includes a chamber 3. Next, the vapor-phase growth device 1 executes a chemical vapor-phase growth method inside the chamber 3 to grow a substance on the substrate S to form a substance on the substrate S (hereinafter referred to as “target substance”). That is, the vapor-phase growth device 1 causes a plurality of different raw material gases Gn to chemically react inside the chamber 3 and form a target substance on the substrate S. Target substance system, such as III-V compound semiconductors. Target substance system, such as solid. The raw material gas Gn is a gas that forms a target substance by chemical reaction. That is, the raw material gas Gn is a gas that generates a target substance through a chemical reaction. In addition, when distinguishing and explaining a plurality of raw material gases Gn, the raw material gases G1, ..., GN (N is an integer of 2 or more) are described. For example, when N=2, the raw material gas G1 is a compound containing a group III (Group 13) element; the raw material gas G2 is a compound containing a group V (Group 15) element.

When the vapor-phase growth device 1 forms part or all of the target substance RP (hereinafter referred to as "reaction period RP") on the substrate S, the outflow of the raw material gas Gn from the inside of the chamber 3 to the outside is blocked. Therefore, during a part or all of the reaction period RP, the chamber 3 is sealed. That is, the vapor-phase growth device 1 causes a plurality of different raw material gases Gn to stay in the chamber 3 to generate a chemical reaction, and form a target substance on the substrate S.

As a result, compared with the case where a general gas-phase growth device circulates a raw material gas to form a target substance, the use efficiency of the raw material gas Gn can be improved by the first embodiment. The utilization efficiency of the raw material gas Gn refers to the ratio of the amount of the reacted raw material gas relative to the amount of the raw material gas Gn introduced into the chamber 3. The reaction raw material gas system refers to the raw material gas Gn in which there is a raw material gas Gn that participates in generating a chemical reaction to form a target substance. "Quantity" means, for example, mass (mole), mass, or volume.

In addition, compared to a general gas-phase growth device, in Embodiment 1, the gas-phase growth device 1 can be miniaturized, thereby reducing the cost of the gas-phase growth device 1. In addition, in a general vapor-phase growth apparatus, in order to circulate the raw material gas, a long reaction tube having a plurality of regions is required, and it is difficult to miniaturize it.

Furthermore, compared to the case where the temperature of each region in the reaction tube is controlled as in a general vapor growth device, in Embodiment 1, it is sufficient to control the temperature of the substrate S by the heating section 7, so The temperature control can be easily performed.

Furthermore, compared to a general gas-phase growth device, in the first embodiment, a plurality of different raw material gases Gn are introduced and retained in the chamber 3 to form a target substance, thereby the raw material gas When Gn is introduced into the chamber 3, it is easier to control. In addition, in a general vapor phase growth device, in order to form the target substance, it is necessary to perform a plurality of steps through the plurality of areas in the reaction tube through the source gas to form the target substance, so that the control of the source gas flowing through the reaction tube becomes complex.

Furthermore, compared to a general vapor phase growth apparatus, in the first embodiment, since a plurality of different raw material gases Gn are retained in the chamber 3 to form the target substance, the growth rate of the target substance is not easy Influenced by the structure of the chamber 3. In addition, in a general vapor phase growth device, since the target substance is formed through a long reaction tube having a plurality of regions, the growth rate of the target substance is easily affected by the structure of the reaction tube.

Furthermore, compared with the case where a plurality of steps are performed by circulating a raw material gas as in a general gas phase growth device, in the first embodiment, a plurality of different raw material gases Gn are introduced and retained in the chamber The target substance is formed inside 3, whereby the amount of residue and the amount of by-products can be reduced. Therefore, the discharge processing of the residue and the exhaust processing of the by-products are made easier.

Preferably, the vapor-phase growth device 1 blocks the outflow of the raw material gas Gn from the inside of the chamber 3 to the outside during the entire reaction period. Further, preferably, the vapor phase growth device 1 is configured to block the outflow of a plurality of raw material gases Gn from the inside of the chamber 3 to the outside during a part or all of the reaction period RP. Even more preferably, the vapor-phase growth device 1 blocks the outflow of the plurality of raw material gases Gn from the inside of the chamber 3 to the outside during all the reaction periods. In addition, the gas-phase growth device 1 can also block the outflow of a single plurality of raw gas Gn among the plurality of raw gas Gn.

Specifically, the vapor-phase growth device 1 further includes a holding part 5, a heating part 7, a plurality of wall parts 8, a temperature part control part 9, a power cord 11, and a by-product detection part 13, in addition to the chamber 3 The by-product exhaust unit 15, the cooling unit 17, a plurality of raw material introduction pipes An, the carrier introduction pipe 19, the etching introduction pipe 21, the power cord extraction pipe 23, the residue discharge pipe 25, and the by-product discharge pipe 27. In addition, when distinguishing and explaining a plurality of raw material introduction pipes An, it is described as the raw material introduction pipes A1, ..., AN (N is an integer of 2 or more).

The chamber 3 is a reaction furnace 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 by-product exhaust port FP. The chamber 3 is formed of, for example, quartz. In addition, when distinguishing and explaining a plurality of raw material inlets GPn, the raw material inlets GP1, ..., GPN (N is an integer of 2 or more) are described. Furthermore, the chamber 3 has a pair of window portions WD that are opposed to each other. The window portion WD is formed of a transparent element, and is provided in the chamber 3 in an airtight state.

The plural raw material introduction ports GPn are respectively arranged corresponding to the plural raw material introduction pipes An. The raw material introduction port GPn is connected to the corresponding raw material introduction pipe An in an airtight state. Next, a plurality of raw material introduction tubes An supply a plurality of raw material gases Gn different from each other. 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 Embodiment 1, the plurality of raw material gases Gn can be introduced into the chamber 3 from the plurality of raw material containers prepared for the plurality of raw material gases Gn, respectively. In particular, the step of premixing before introducing a plurality of source gases Gn into the chamber 3 can be reduced, thereby simplifying the step before introducing the plurality of source gases Gn into the chamber 3.

The carrier introduction port CP is arranged corresponding to the carrier introduction tube 19. The carrier introduction port CP is connected to the carrier introduction tube 19 in an airtight state. Next, the carrier gas introduction tube 19 supplies the carrier gas CG. Therefore, the carrier introduction port CP introduces the carrier gas CG into the chamber 3. The carrier gas CG is, for example, an inert gas. Inert gas systems such as nitrogen. According to the first embodiment, since the carrier gas CG is introduced into the chamber 3, a plurality of raw material gases Gn in the chamber 3 can be uniformly mixed.

The etching introduction port EP is arranged corresponding to the etching introduction tube 21. The etching introduction port EP is connected to the etching introduction tube 21 in an airtight state. Next, the etching introduction tube 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 a halogen gas, for example. According to Embodiment 1, the etching gas EG is introduced into the chamber 3, whereby the inner wall of the chamber 3, the surface of the holding portion 5, the surface of the substrate S, and the target substance grown on the substrate S can be washed surface.

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, which is a substance remaining in the chamber 3 after the target substance is formed on the substrate S. Specifically, the residue discharge port ZP is arranged corresponding to the residue discharge pipe 25. The residue discharge port ZP is connected to the residue discharge pipe 25 in an airtight state. Next, 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 by-product exhaust port FP exhausts the by-product FG inside the chamber 3 to the outside of the chamber 3. The by-product FG is, for example, a gas, which is a substance generated by a chemical reaction of a plurality of raw material gases Gn, and is different from the target substance. The by-product FG is, for example, a gas that hinders the growth of the target substance. A gas system that hinders the growth of a target substance, such as a gas for etching a substance, is hydrogen chloride generated when gallium trichloride gas and ammonia gas are chemically reacted to form gallium nitride.

Specifically, the by-product exhaust port FP is arranged corresponding to the by-product exhaust pipe 27. The by-product exhaust port FP is connected to the by-product exhaust pipe 27 in an airtight state. Next, 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 lead-out tube 23 is connected to the chamber 3 in an airtight state. On the other hand, the power cord 11 is connected to the heating unit 7. Next, the power cord 11 is drawn out from the inside of the chamber 3 to the outside through the power cord extraction tube 23.

The holding portion 5 is arranged inside the chamber 3. In Embodiment 1, the holding portion 5 is provided on the inner bottom surface 4a of the chamber 3. The holding portion 5 holds the substrate S. Specifically, the holding portion 5 has a holding surface HS. Next, the substrate S is provided on the holding surface HS. The holding unit 5 is, for example, a susceptor. The bearing system is formed of, for example, silicon carbide (Silicon Carbide). The substrate S is, for example, a seed substrate. The seed substrate is, for example, a seed crystal substrate (Seed Crystal Substrate). The substrate S is, for example, a sapphire substrate (Sapphire Substrate).

The heating unit 7 is arranged inside the chamber 3. The heating unit 7 is arranged on the holding unit 5 so as to face the holding surface HS. In Embodiment 1, the heating unit 7 is fixed by the holding unit 5. Next, 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. In addition, the heating unit 7 may heat the holding unit 5 by induction heating.

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

The temperature control unit 9 controls the power supply voltage and the power supply current supplied to the heating unit 7 to control 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 and controls the temperature of the substrate S through the holding unit 5. Next, the temperature control unit 9 controls the heating unit 7 and passes through the holding unit 5 to maintain the temperature of the substrate S at a predetermined temperature. In addition, the temperature control unit 9 includes a processor and a memory device. Therefore, the processor controls the heating section 7 by executing a computer program stored in the memory device.

In addition, the vapor-phase growth device 1 may also be provided with a temperature sensor (for example, a thermistor). The temperature sensor is fixed to the holding portion 5 (for example, holding surface HS). The temperature sensor detects the temperature of the holding part 5. The holding portion 5 has high thermal conductivity, and in the thermal equilibrium state, the temperature of the holding portion 5 is equal to the temperature of the substrate S. Therefore, the temperature control unit 9 receives the signal indicating the temperature of the holding unit 5 via the temperature sensor to monitor the temperature of the substrate S. The temperature control unit 9 controls the heating unit 7 while monitoring the temperature of the substrate S so that the temperature of the substrate S is maintained at a predetermined temperature. In addition, the temperature sensor can also directly detect the temperature of the substrate S.

Each wall portion 8 is arranged between the holding portion 5 where the heating portion 7 is arranged and the inner wall surface 4b of the chamber 3. Each wall portion 8 has an opening 10 exposing the substrate S. In Embodiment 1, the opening 10 exposes the substrate S toward the inner top surface 4c of the chamber 3. Each wall portion 8 has, for example, a substantially cylindrical shape. The material of the wall portion 8 is, for example, carbon, boron nitride, or quartz. The heights of the plurality of wall portions 8 relative to the inner bottom surface 4a may be different or the same. Preferably, the height of the wall portion 8 relative to the inner bottom surface 4a is higher than the height of the holding portion 5 relative to the inner bottom surface 4a. The adjacent wall portions 8 are arranged at intervals. 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 is spaced apart to surround the side surface of the holding portion 5. Among the plurality of wall portions 8, the outermost wall portion 8 b is spaced apart and faces the inner wall surface 4 b of the chamber 3. In addition, the number of wall portions 8 is not limited to two, and may be three or more. Furthermore, one wall portion 8 may be provided.

According to Embodiment 1, since the wall portion 8 is provided, it is possible to suppress the heat from the heating portion 7, the holding portion 5, and the substrate S from being directly transmitted to the chamber 3. As a result, the temperature of the chamber 3 can be suppressed from becoming high, and the durability of the chamber 3 can be improved. Furthermore, since the wall portion 8 is provided, the outflow of heat from the substrate S and the holding portion 5 can be suppressed, whereby 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 circulates the cooling liquid WT (for example, cooling water) in the chamber 3 to cool the chamber 3. As a result, according to the first embodiment, the influence of the heat from the heating unit 7, the holding unit 5, and the substrate S can be reduced, so that the durability of the chamber 3 can be further improved.

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

Next, after supplying the first predetermined amount M1 (predetermined amount) of raw material gas Gn to the chamber 3, the gas supply device 60 blocks the flow path of the raw material gas Gn to stop the supply of the raw material gas Gn to the chamber 3. In other words, after the first predetermined amount M1 of raw material gas Gn is introduced into the chamber 3, the flow path of the raw material gas Gn is blocked, and the introduction of the raw material gas Gn from the raw material introduction pipe An and the raw material introduction port GPn is stopped.

Therefore, according to Embodiment 1, it is possible to further suppress the outflow of the raw material gas Gn from the outside of the chamber 3. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

The first predetermined amount M1 is expressed by, for example, the mass (mol), mass, or volume. The first predetermined amount M1 can be set for each of the raw material gases Gn based on the chemical reaction formulas of a plurality of different raw material gases Gn during the chemical reaction. That is, the first predetermined amount M1 can be set for each raw material gas Gn so that the molar fraction of various raw material gases Gn is kept constant inside the chamber 3. In this specification, the chemical reaction formula means a chemical reaction formula for generating a target substance.

Therefore, according to the first embodiment, the excess and deficiency of the plurality of source gases Gn are suppressed, so that the correct amount of source gases Gn can be introduced into the chamber 3. As a result, the waste of the raw material gas Gn can be suppressed. The molar fraction of the raw material gas Gn represents the ratio of the total amount of the raw material gas Gn to the raw material gas Gn.

In addition, the gas supply device 60 replenishes the raw material gas Gn to the chamber 3 through the raw material introduction pipe An and the raw material introduction port GPn according to the reduction amount of the raw material gas Gn caused by the chemical reaction inside the chamber 3.

Therefore, according to the first embodiment, the shortage of the raw material gas Gn can be avoided, thereby suppressing the growth failure of the target substance.

In addition, when supplementing the raw material gas Gn, the gas supply device 60 supplements the raw material gas Gn so that the molar fraction of various raw material gases Gn is kept constant inside the chamber 3.

Therefore, according to the first embodiment, the excesses and deficiencies of the plurality of raw material gases Gn are further suppressed, and thus the correct amount of the raw material gases Gn can be further introduced into the chamber 3. As a result, the waste of the raw material gas Gn can be further suppressed.

Specifically, the gas supply device 60 supplies the second predetermined amount M2 of raw material gas Gn to the chamber 3 according to the amount of reduction of the raw material gas Gn inside the chamber 3.

The second predetermined amount M2 is expressed by, for example, the mass (mol), mass, or volume. Preferably, the second predetermined amount M2 is equal to, for example, the decrease amount of the raw material gas Gn. In addition, the second predetermined amount M2 can be set for each raw material gas Gn based on the chemical reaction formulas of the plural raw material gases Gn during the chemical reaction. That is, the molar fraction of each raw material gas Gn is set to be constant within the chamber 3 so that the second predetermined amount M2 is set for each raw material gas Gn.

Next, after the second predetermined amount M2 of raw material gas Gn is replenished, the gas supply device 60 blocks the flow path of the raw material gas Gn to stop the raw material gas Gn from passing through the raw material introduction pipe An and the raw material introduction port GPn to the chamber 3 supplement.

Therefore, according to Embodiment 1, the outflow of the raw material gas Gn from the outside of the chamber 3 can be further suppressed. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

In addition, after the first predetermined amount M1 of raw material gas Gn is supplied, the gas supply device 60 can pass through the raw material introduction pipe An and the raw material introduction port according to the reduced amount of the raw material gas Gn caused by the chemical reaction inside the chamber 3 GPn supplements the raw gas Gn at any time. In this case, the raw material gas Gn is replenished at any time by only reducing the amount of the raw material gas Gn, so that the raw material gas Gn can maintain a certain amount in the chamber 3 at any time. Therefore, the growth of the target substance can be controlled with high accuracy. Furthermore, on the other hand, when the raw material gas Gn is replenished, since the raw material gas Gn does not flow out of the outside of the chamber 3, the utilization efficiency of the raw material 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 Th1, the gas supply device 60 can be replenished from the raw material introduction port GPn at any time according to the reduced amount of the raw material gas Gn in the chamber 3 Raw gas Gn. Preferably, the threshold Th1 is set to the same value as, for example, the first predetermined amount M1. In this case, the source gas Gn can be kept at the first predetermined amount M1 in the chamber 3. As a result, the growth of the target substance can be controlled with high precision.

In addition, for example, when the gas supply device 60 replenishes the raw material gas Gn at any time, the raw material gas Gn can be replenished at any time so that the molar fraction of various raw material gases Gn is kept constant inside the chamber 3. In this case, the excess and deficiency of the plurality of source gases Gn are suppressed, so that the correct amount of source gases Gn can be introduced into the chamber 3. As a result, the waste of the raw material gas Gn can be suppressed.

Furthermore, the gas supply device 60 is connected to the carrier introduction pipe 19. Next, the gas supply device 60 passes through the carrier introduction tube 19 and the carrier introduction port CP to supply the carrier gas CG to the chamber 3.

Specifically, the gas supply device 60 supplements the third predetermined amount M3 of carrier gas CG to the chamber 3 and then blocks the flow path of the carrier gas CG to stop the supply of the carrier gas CG to the chamber 3.

Therefore, according to Embodiment 1, it is possible to suppress the outflow of the raw material gas Gn from the carrier introduction pipe 19 to the outside of the chamber 3. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

The third predetermined amount M3 is expressed by, for example, mass (mole), mass, or volume. In addition, the gas supply device 60 can replenish a certain amount of carrier gas CG through the carrier introduction pipe 19 and the carrier introduction port CP according to the reduction amount of the carrier gas CG inside the chamber 3. Preferably, the certain amount is an amount equal to, for example, the decrease amount of the carrier gas CG. Furthermore, the gas supply device 60 can replenish the carrier gas CG at any time when the source gas Gn is replenished at any time.

Furthermore, the gas supply device 60 is connected to the etching introduction pipe 21. Next, 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 the fourth predetermined amount M4 of etching gas EG is added to the chamber 3, the gas supply device 60 blocks the flow path of the etching gas EG to stop the supply of the etching gas EG to the chamber 3.

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

The fourth predetermined amount M4 is expressed by, for example, the mass (mol), mass, or volume. In addition, the gas supply device 60 can supplement a certain amount of the etching gas EG through the etching introduction pipe 21 and the etching introduction port EP according to the reduction amount of the etching gas EG inside the chamber 3. Preferably, the certain amount is equal to the amount of reduction of the etching gas EG, for example. Furthermore, the gas supply device 60 can supplement the etching gas EG at any time when the raw gas Gn is replenished at any time.

The residue discharge device 80 is connected to the residue discharge pipe 25. Next, the residue discharge device 80 completes the formation of the target substance on the substrate S, and then 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, by implementing aspect 1, the inside of the chamber 3 can be efficiently cleaned.

Specifically, the residue discharge device 80 has a singular or plural valves and a vacuum pump. Next, during the reaction period RP, the residue discharge device 80 closes the valve to close the residue discharge pipe 25 to block the gas (raw material gas Gn, carrier gas CG, etching gas EG, and by-product FG) from the chamber 3 Outflow from inside to outside. Therefore, according to Embodiment 1, it is possible to suppress the outflow of the raw material gas Gn in the RP from the residue discharge pipe 25 to the outside of the chamber 3 during the reaction. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

Next, after the residue discharge device 80 completes the formation of the target substance on the substrate S, when the vacuum pump is driven, the valve is opened to open the residue discharge pipe 25, and the residue ZG is discharged. In addition, the residue discharge device 80 includes a processor and a memory device. Therefore, the processor controls the valve and vacuum pump by executing the computer program stored in the memory 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 transmits the gas (raw material gas Gn, carrier gas CG, etching gas EG, etc.) existing in the internal space SP through the window part WD on one side of the pair of window parts WD. By-product FG). Next, the by-product detection section 13 detects the light emitted from the window WD on the other side through the gas existing in the internal space SP. Furthermore, the by-product detection unit 13 processes and analyzes the detected light, and calculates the concentration of the by-product FG. The by-product detection unit 13 includes, for example, a Fourier transform infrared spectrophotometer (FT-IR, Fourier ransform infrared spectrophotometer).

The by-product exhaust unit 15 is connected with a by-product exhaust pipe 27. Next, the by-product exhaust unit 15 passes through the by-product exhaust port FP and the by-product exhaust pipe 27 to discharge the by-product FG from the inside of the chamber 3 to the outside.

According to the first embodiment, the by-product FG is exhausted, thereby increasing the growth rate of the target substance. In particular, when the by-product FG has a property that hinders the growth of the target substance (for example, the property of etching the target substance), by exhausting the by-product FG, the growth rate of the target substance can be further increased.

Specifically, the by-product exhaust unit 15 obtains information indicating the concentration of by-product FG from the by-product detection unit 13. Next, the by-product exhaust unit 15 exhausts the by-product FG according to the concentration of the by-product FG. For example, when the concentration of the by-product FG becomes greater than the threshold Th2, the by-product exhaust unit 15 exhausts the by-product FG until the concentration of the by-product FG falls below the threshold Th2. As a result, since the concentration of the by-product FG in the chamber 3 is maintained below the threshold Th2, the growth rate of the target substance can be further increased.

In particular, according to Embodiment 1, since the by-product exhaust unit 15 exhausts the by-product FG based on the concentration of the by-product FG obtained by the by-product detection unit 13, it does not make meaningless The operation can only be performed when the amount of by-product FG increases. As a result, the power consumption of the by-product exhaust unit 15 can be suppressed.

More specifically, the by-product exhaust unit 15 includes a valve unit 15a, a suction pump 15b, and a control unit 15c. The valve portion 15a includes a singular or plural valves.

The control unit 15c closes the valve to close the by-product exhaust pipe 27 when the concentration of the by-product FG is below the threshold Th2 to block the gas (raw material gas Gn, carrier gas CG, etching gas EG, and by-product FG) from The inside of the chamber 3 flows out to the outside.

On the other hand, when the concentration of the by-product FG becomes greater than the threshold Th2, the control unit 15c opens the valve to open the by-product exhaust pipe 27 when the suction pump 15b is driven, and performs the by-product FG exhaust. Next, when the concentration of the by-product FG becomes equal to or less than the threshold value Th2, the control unit 15c closes the valve to close the by-product exhaust pipe 27 to stop the suction pump 15b. As a result, the exhaust of the by-product FG can be stopped.

For example, when the concentration of the by-product FG becomes greater than the threshold value Th2, the control unit 15c opens the valve to open the by-product exhaust pipe 27 when the suction pump 15b is driven, and the gas inside the chamber 3 (The raw material gas Gn, the carrier gas CG, the etching gas EG, and the by-product FG) are exhausted. As a result, the by-product FG is exhausted simultaneously with the source gas Gn, the carrier gas CG, and the etching gas EG.

In this example, the raw material gas Gn, the carrier gas CG, and the etching gas EG are exhausted by the by-product exhaust pipe 27. Here, the gas supply device 60 supplements the raw material gas Gn to the chamber 3 according to the reduction amount of the raw material gas Gn. When supplementing the raw material gas Gn, the gas supply device 60 supplements the raw material gas Gn so that the molar fraction of the raw gas Gn is kept constant inside the chamber 3. Furthermore, the gas supply device 60 replenishes the carrier gas CG to the chamber 3 according to the reduction of the carrier gas CG. Furthermore, the gas supply device 60 supplements the etching gas EG to the chamber 3 according to the reduction of the etching gas EG.

In particular, even in this example, by Embodiment 1, the by-product exhaust unit 15 exhausts the by-product FG based on the concentration of the by-product FG obtained from the by-product detection unit 13 by This may make it necessary to operate only when the amount of by-product FG increases. Therefore, the amount of the raw material gas Gn exhausted simultaneously with the by-product FG can be suppressed. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

As described above with reference to FIG. 1, according to Embodiment 1, since a plurality of different raw material gases Gn are introduced and retained in the chamber 3 to form a target substance, various raw material gases Gn can be based on In the method of generating the mole fraction of the chemical reaction formula of the target substance, a plurality of different raw material gases Gn are introduced into the chamber 3. That is, a plurality of different raw material gases Gn are introduced into the chamber 3 in such a manner that the molar fractions of the various raw material gases Gn are kept constant in the chamber 3. As a result, the amount of residue can be suppressed. In addition, in a general vapor-phase growth apparatus, in order to circulate the raw material gas, it is difficult to introduce the raw material gas into the reaction tube so that the molar fraction of each raw material gas is kept constant.

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

Here, it is preferable that the gas supply device 60 supply a plurality of different diluted raw material gases Dn instead of a plurality of different raw material gases Gn to the gas phase growth device 1. The diluted raw material gas Dn is a gas in which the raw material gas Gn and the carrier gas CG are mixed, and the raw material gas Gn is diluted by the carrier gas CG. For example, in the plurality of diluted raw material gases Dn, although the raw material gases Gn are different from each other, the carrier gas CG is the same. In addition, when distinguishing and explaining a plurality of diluted raw material gases Dn, it is described by diluted raw material gases D1, ..., DN (N is an integer of 2 or more).

Next, referring to FIG. 1, the difference between the state of supplying the diluted raw material gas Dn replacing the raw material gas Gn to the vapor phase growth device 1 and the state of supplying the raw material gas Gn to the vapor phase growth device 1 will be described. .

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

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

Specifically, after supplying the diluted raw material gas Dn containing the first predetermined amount M1 of raw material gas Gn to the chamber 3, the gas supply device 60 blocks the flow path of the diluted raw material gas Dn to stop the flow of the diluted raw material gas Dn. Supply of chamber 3. In other words, after the diluted raw material gas Dn containing the first predetermined amount of raw material gas Gn is introduced into the chamber 3, the flow path of the diluted raw material gas Dn is blocked, and the diluted raw material gas from the raw material introduction pipe An and the raw material introduction port GPn The import of Dn was stopped.

Furthermore, the gas supply device 60 replenishes the diluted raw gas Dn to the chamber 3 through the raw material introduction pipe An and the raw material introduction port GPn according to the reduction amount of the raw material gas Gn caused by the chemical reaction inside the chamber 3 . Furthermore, when supplementing the diluted raw material gas Dn, the gas supply device 60 supplements the diluted raw material gas Dn so that the molar fraction of the raw material gas Gn remains constant inside the chamber 3.

Specifically, the gas supply device 60 passes the raw material introduction pipe An and the raw material introduction port GPn according to the reduction amount of the raw material gas Gn in the chamber 3 to dilute the diluted raw material gas Dn containing the second predetermined amount of raw material gas Gn Supply to the chamber 3.

Next, the gas supply device 60 blocks the flow path of the diluted raw material gas Dn after the diluted raw material gas Dn containing the second predetermined amount of raw material gas Gn is replenished to stop the flow through the raw material introduction pipe An and the raw material introduction port GPn The chamber 3 is supplemented with diluted raw material gas Dn.

In addition, after supplying the diluted raw material gas Dn containing the first predetermined amount M1 of raw material gas Gn, the gas supply device 60 can also pass through the raw material according to the reduced amount of the raw material gas Gn caused by the chemical reaction inside the chamber 3 The introduction pipe An and the raw material introduction port GPn supplement the diluted raw material gas Dn at any time.

For example, in the gas supply device 60, when the amount of the raw material gas Gn inside the chamber 3 becomes smaller than the threshold value Th1, the raw material introduction port GPn may be used at any time according to the amount of reduction of the raw material gas Gn inside the chamber 3 The diluted raw gas Dn containing the raw gas Gn is replenished.

Furthermore, for example, when the gas supply device 60 is replenished with the diluted raw material gas Dn at any time, the diluted raw material gas Dn may be replenished at any time so that the molar fraction of the various raw material gases Gn remains constant inside the chamber 3.

Furthermore, the gas supply device 60 may supplement the carrier gas CG at any time when the diluted raw material gas Dn is replenished at any time. Furthermore, when the gas supply device 60 supplements the diluted raw material gas Dn at any time, the etching gas EG may be supplemented at any time.

In addition, when the concentration of the by-product FG becomes greater than the threshold value Th2, the by-product exhaust unit 15 exhausts the by-product FG when exhausting the source gas Gn, the carrier gas CG, and the etching gas EG. In this case, the gas supply device 60 supplements the diluted raw material gas Dn to the chamber 3 according to the amount of reduction of the raw material gas Gn. The gas supply device 60 supplements the diluted raw material gas Dn in such a manner that the molar fraction of the various raw material gases Gn is kept constant in the chamber 3 when the diluted raw material gas Dn is replenished.

In the following Embodiment 1, unless otherwise specified, the gas supply device 60 supplies the diluted raw material gas Dn instead of the raw material gas Gn to the gas phase growth device 1.

Next, the gas supply device 60 will be described with reference to FIG. 2. FIG. 2 is a schematic diagram of the gas supply device 60. As shown in FIG. 2, the gas supply device 60 includes a vacuum pump 61, a control unit 62, a thermostat 63 (temperature control unit), a plurality of pressure adjustment units 64n, and a plurality of first flow control units Qn (a plurality of flow control Part), the second flow control unit 72 and the third flow control unit 73. Each pressure adjusting unit 64n includes a dilution container Xn, a valve portion Yn (introduction portion), and a raw material container Zn (gas container). Next, the gas supply device 60 supplies gas (diluted raw material gas Dn, carrier gas CG, and etching gas EG) to the vapor phase growth device 1 (FIG. 1 ). In addition, in this specification, the valve portion Yn is an example of the introduction portion, and the raw material container Zn is an example of the gas container.

In addition, when distinguishing and describing a plurality of pressure adjustment units 64n, it is described as pressure adjustment units 641, ..., 64N (N is an integer of 2 or more). When distinguishing and explaining a plurality of first flow control units Qn, it is described as the first flow control units Q1, ..., QN (N is an integer of 2 or more). When distinguishing and explaining a plurality of dilution containers Xn, it is described as dilution containers X1, ..., XN (N is an integer of 2 or more). When distinguishing and explaining a plurality of valve parts Yn, it is described as valve parts Y1, ..., YN (N is an integer of 2 or more). When distinguishing and explaining a plurality of raw material containers Zn, it is described as raw material containers Z1, ..., ZN (N is an integer of 2 or more).

The control unit 62 controls the vacuum pump 61, the thermostat 63, the plurality of valve parts Yn, the plurality of first flow rate control parts Qn, the second flow rate control part 72, and the third flow rate control part 73. That is, the vacuum pump 61, the thermostat 63, the plurality of valve portions Yn, the plurality of first flow control portions Qn, the second flow control portion 72, and the third flow control portion 73 are controlled and operated by the control portion 62. In addition, the control unit 62 includes a processor and a memory device. Therefore, the processor controls the vacuum pump 61, the thermostat 63, the plurality of valve parts Yn, the plurality of first flow control parts Qn, the second flow control part 72 and the second by executing the computer program stored in the memory device 3Flow control unit 73.

The constant temperature bath 63 controls the temperature of the plurality of pressure adjusting units 64n, so as to maintain the temperature of the plurality of pressure adjusting units 64n at a certain temperature. A plurality of pressure adjusting units 64n are arranged inside the thermostat 63.

The pressure adjustment unit 64n generates the diluted raw material gas Dn by diluting the raw material gas Gn with the carrier gas CG. Next, the pressure adjusting unit 64n discharges the diluted raw material gas Dn containing the raw material gas Gn. Furthermore, the pressure adjusting unit 64n adjusts the partial pressure of the carrier gas CG and the partial pressure of the raw material gas Gn in the dilution container Xn when the diluted raw material gas Dn is generated.

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

The plurality of raw material containers Zn respectively contain a plurality of different raw material gases Gn (a plurality of different gas from each other). The raw material gas Gn is a pure raw material gas that has not been diluted, and has a certain pressure (vapor pressure) inside the raw material container Zn. Specifically, the raw material container Zn gasifies the solid raw material to generate the raw material gas Gn, and stores the raw material gas Gn. In addition, the raw material container Zn can also vaporize the liquid raw material to generate the raw material gas Gn and contain the raw material gas Gn. For example, the thermostat 63 controls the temperature of the raw material container Zn to vaporize the solid raw material in the raw material container Zn or the liquid raw material in the vaporized raw material container Zn.

In addition, in this specification, the raw material gas Gn is an example of the gas to be supplied to the gas-phase growth device 1 through the gas supply device 60. Therefore, the raw material container Zn contains the raw material gas Gn as the gas to be supplied. In addition, the gas-phase growth device 1 is an example of a place where the gas supplied through the gas supply device 60 is supplied. Furthermore, the carrier gas CG is different from the gas to be supplied, for example, to transport the gas to be supplied, or to dilute the gas to be supplied, or to stir the gas to be supplied.

Each valve part Yn introduces the raw material gas Gn and the carrier gas CG diluting the raw material gas Gn into the corresponding dilution container Xn at different time points. As a result, the diluted raw material gas Dn in which the raw material gas Gn and the carrier gas CG are mixed is generated in the dilution container Xn. Furthermore, the valve portion Yn adjusts the partial pressure of the raw material 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 raw material gas Dn is set to a predetermined total pressure value, the partial pressure pg of the raw gas Gn is set to the first partial pressure value, and the partial pressure pc of the carrier gas CG is set Set to the second partial pressure value. That is, p=pg+pc.

Each dilution container Xn mixes the raw material gas Gn and the carrier gas CG introduced from the corresponding raw material container Zn, and is accommodated as the diluted raw material gas Dn (dilution gas). Next, after the raw material gas Gn and the carrier gas CG are mixed, each valve portion Yn discharges the diluted raw material gas Dn from the corresponding dilution container Xn. That is, after each of the valve portions Yn is mixed with the source gas Gn and the carrier gas CG, 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 adjusted from the corresponding dilution container Xn exhausts.

In addition, in this specification, the diluted raw material gas Dn is an example of a diluted gas that mixes the gas (specifically, the raw material gas Gn) and the carrier gas CG supplied to the gas-phase growth device 1 through the gas supply device 60. .

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 respectively 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 raw material gas Dn discharged from the corresponding valve unit Yn. Next, the first flow control unit Qn passes through the corresponding raw material introduction pipe An, and supplies the diluted raw material gas Dn to the chamber 3. Specifically, the first flow control unit Qn has a laminar flow element (specifically, a porous element). The laminar flow element divides the flow channel into upstream and downstream. Next, the first flow control unit Qn uses the principle of Hagen-Poiseuille Flow to control the volume flow of the diluted raw gas Dn based on the differential pressure between the upstream and downstream of the laminar flow element or Mass Flow.

The second flow rate control unit 72 controls the flow rate of the carrier gas CG. Next, the second flow rate control unit 72 supplies the carrier gas CG to the chamber 3 through the carrier introduction tube 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. Next, 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 Embodiment 1, since the carrier gas CG is introduced into the dilution container Xn, the dilution raw material gas Dn can be increased compared to the case where only the raw material gas Gn is introduced into the dilution container Xn. The total pressure p. Therefore, compared with the case where only the raw material gas Gn is introduced into the dilution container Xn, the raw material gas Gn tends to move toward the first flow control unit Qn and the vapor phase growth device 1. That is, the total pressure p of the diluted raw material gas Dn in the dilution container Xn ensures the power to move the raw material gas Gn. On the other hand, by adjusting the amount (material mass, volume, or mass) of the raw material gas Gn introduced from the raw material container Zn to the dilution container Xn, the content of the diluted raw material gas Dn contained in the dilution container Xn can be adjusted with high accuracy The amount of raw material gas Gn (material mass, volume, or mass).

As a result, in comparison with the film forming apparatus described in Invention Patent Document 1 (hereinafter referred to as "prior art"), the flow rate of the carrier gas is controlled while flowing the carrier gas to adjust the supply amount of the source gas Next, the amount (material mass, volume amount, or mass) of the raw material gas Gn that moves along with the carrier gas CG toward the first flow control unit Qn and the vapor phase growth device 1 can be adjusted with high accuracy, that is, the raw material gas Gn Of supply. Furthermore, compared with the case where the raw material gas is directly supplied from the bubbler to the gas supply location as in the prior art, the diluted raw material gas Dn is discharged from the dilution container Xn, whereby the supply of the raw material gas Gn can be adjusted with high accuracy the amount. Since the supply amount of the raw material gas Gn can be adjusted with high precision, the vapor-phase growth device 1 can form a target substance of good quality (for example, a target substance with few defects and high purity).

Furthermore, according to Embodiment 1, the total pressure p of the diluted raw material gas Dn in the dilution container Xn is used to ensure the power to move the raw material gas Gn, and the diluted raw material gas containing the raw material gas Gn is discharged from the diluted container Xn Dn. Therefore, compared with the prior art, the supply amount of the raw material gas Gn is less susceptible to temperature, and temperature management is easier. Furthermore, since the supply amount of the raw material gas Gn is not easily affected by temperature, the supply amount of the raw material 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 addition, in the prior art, since the carrier gas is flowed to the bubbler to generate the raw material gas, and the raw material gas is directly supplied to the gas supply location through the carrier gas, the flow rate of the raw material gas is determined by the temperature in the bubbler (raw material The vapor pressure), the pressure in the bubbler and the flow rate of the carrier gas are determined. Therefore, the flow rate of the raw material gas is easily affected by temperature. As a result, if the temperature in the bubbler is not precisely controlled, the flow rate of the raw material gas cannot be controlled with high accuracy. That is, temperature management becomes difficult. Furthermore, in the prior art, when the temperature in the bubbler is precisely controlled, a temperature control device (for example, an electronic thermostat) for controlling the temperature of the bubbler becomes expensive, which increases the cost. Furthermore, since the power consumed by such a temperature control device may become larger, there is a possibility of increasing maintenance costs. In contrast, in the first embodiment, the maintenance cost can be suppressed from increasing. Furthermore, the internal shape of such a temperature control device may be limited to a special shape, so the shape of the bubbler disposed inside the temperature control device may be limited. On the other hand, in the first embodiment, the shape of the raw material container Zn can be suppressed from being restricted, so that the raw material container Zn of any shape can be used.

Furthermore, according to Embodiment 1, the total pressure p of the diluted raw material gas Dn in the dilution container Xn ensures the power to move the raw material gas Gn, and the diluted raw material gas Dn containing the raw material gas Gn is discharged from the dilution container Xn . Therefore, compared with the prior art, a small amount of raw material gas Gn can be easily supplied.

In addition, in the prior art, since the flow rate of the raw material gas is determined by the temperature in the bubbler (the vapor pressure of the raw material), the pressure in the bubbler, and the flow rate of the carrier gas, when a small amount of raw material gas is supplied, The flow rate of the carrier gas must be reduced, or the temperature in the bubbler must be reduced. However, if the flow rate of the carrier gas is reduced, continuous bubbles cannot be generated and intermittent bubbles are generated, so there is a possibility that the supply amount of the raw material gas becomes unstable. On the other hand, in Embodiment 1, since the diluted raw material gas Dn containing the raw material gas Gn is discharged from the dilution container Xn, the supply amount of the raw material gas Gn is stabilized. Furthermore, in the prior art, when the temperature in the bubbler was to be reduced, the supply of a small amount of raw material gas would depend on the cooling capacity of a temperature control device (such as an electronic thermostat), so there was a supply of a small amount of raw material gas. Limit possibilities. On the other hand, according to Embodiment 1, since the total pressure p of the diluted raw material gas Dn in the dilution container Xn ensures the force to move the raw material gas Gn, a small amount of raw material gas Gn can be easily supplied.

Furthermore, according to Embodiment 1, by adjusting the amount of carrier gas CG introduced into the dilution container Xn, the total pressure p of the diluted raw material gas Dn can be adjusted. That is, the power to move the raw material gas Gn can be adjusted.

Furthermore, according to Embodiment 1, by adjusting the partial pressure pg of the raw gas Gn in the dilution container Xn, the amount (material mass, volume, or mass) of the raw gas Gn contained in the diluted raw gas Dn can be adjusted . As a result, the amount (material mass, volume amount, or mass) of the raw material gas Gn that moves together with the carrier gas CG toward the first flow rate control unit Qn and the vapor phase growth device 1 can be adjusted with higher accuracy.

Furthermore, according to Embodiment 1, since a plurality of dilution containers Xn are provided, the amount of raw gas Gn introduced into the dilution container Xn can be adjusted for each dilution container Xn. Therefore, the various raw material gases Gn can be introduced into each dilution container Xn so as to have a molar fraction based on the chemical reaction formula for generating the target substance. That is, when the raw material gas Gn is supplied to the vapor phase growth device 1, the mole fraction of the raw material gas Gn can be easily adjusted. In this case, for example, the carrier gas CG is introduced into each dilution container Xn in such a manner that the total pressure p of the dilution raw material gas Dn in the plurality of dilution containers Xn becomes substantially the same as each other.

Furthermore, according to Embodiment 1, since a plurality of dilution containers Xn are provided, the total pressure p of the diluted raw material gas Dn can be adjusted for each dilution container Xn. Therefore, each raw material gas Gn has a molar fraction based on the chemical reaction formula for generating the target substance, so that the raw material gas Gn can be directed from each dilution container Xn toward the first flow control unit Qn and the vapor phase growth device 1 mobile. That is, when the raw material gas Gn is supplied to the vapor phase growth device 1, the mole fraction of the raw material gas Gn can be easily adjusted. In this case, for example, the total pressure p of the diluted raw material gas Dn in each dilution container Xn is determined on the basis of the mole fraction of each raw material gas Gn based on the chemical reaction formula for generating the target substance. Next, the carrier gas CG is introduced into each dilution container Xn so as to become the determined total pressure p.

Furthermore, according to the first embodiment, by using the pressure (vapor pressure) of the raw material gas Gn inside the raw material container Zn, the raw material gas Gn can be moved from the raw material container Zn to the dilution container Xn. Therefore, it is possible to suppress installation of an active device that moves the raw material gas Gn from the raw material 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, by implementing aspect 1, the step of premixing before introducing a plurality of raw material gases Gn into the chamber 3 can be reduced, thereby simplifying the step before introducing the plurality of raw material gases Gn into the chamber 3.

Furthermore, in Embodiment 1, the first flow rate control unit Qn uses the total pressure p of the diluted raw material gas Dn to easily supply the diluted raw material gas Dn to the gas phase growth device 1.

In addition, the first flow rate control unit Qn may also control the flow rate of the raw material gas Gn discharged from the raw material container Zn by the corresponding valve unit Yn. Next, the first flow rate control unit Qn may supply the raw material gas Gn to the chamber 3 through the corresponding raw material introduction pipe An. Specifically, the first flow control unit Qn may also use the principle of Hagen-Baiyi so-called flow to control the volume flow or mass flow of the raw material gas Gn based on the differential pressure between the upstream and downstream of the laminar flow element.

Next, the pressure adjusting unit 64n will be described with reference to FIG. 3. FIG. 3 is a schematic diagram of the pressure adjusting unit 64n. As shown in FIG. 3, each pressure adjusting unit 64n further includes a thermometer TM, a first pressure gauge PM1 (pressure gauge), and a second pressure gauge PM2. Thermometer TM measures the temperature inside the dilution container Xn. The first pressure gauge PM1 measures the pressure inside the dilution container Xn. The second pressure gauge PM2 measures pressure. The second pressure gauge PM2 can measure, for example, a pressure lower 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 tube t5. The valves b1 to b8 are, for example, stop valves.

The tube t1 is connected to the dilution container Xn and the valve b4. The pipe t2 connects the valves b3 to b7 to each other. The pipe t3 connects the valves b1 to b3 to each other. The tube t4 is connected to the valve b7 and the valve b8. The tube t5 is connected to the valve b8 and the raw material container Zn. In addition, the valve b8 may be directly connected to the raw material container Zn. The valve b4 may also be directly connected to the dilution container Xn.

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

[Vacuum suction and flushing]

Step 1: Start the vacuum pump 61.

Step 2: Open valve b2, valve b3, valve b4 and valve b7.

Step 3: Open the valve b6, and close the valve b3. The second pressure gauge PM2 measures the pressure inside the dilution container Xn. The operator confirms the degree of vacuum inside the dilution container Xn with the second pressure gauge PM2.

Step 4: Close the valves b2 and b6, and open the valves b1 and b3. Next, the carrier gas CG is introduced from the valve b1 to the dilution container Xn. As a result, the inside of the dilution container Xn can be washed (purge) with the carrier gas CG.

Next, the valve portion Yn is returned to the initial state, and the initial state and the second to fourth steps are repeated. As a result, the inside of the container Xn can be diluted (Cycle Purge) by carrier gas CG. By repeatedly washing the inside of the dilution container Xn, the mass (or concentration) of the residual gas inside the dilution container Xn can be reduced. After repeating the initial state and the second to fourth steps, the valve portion Yn is returned to the initial state, and then the second and third steps are performed.

[Introduction of Raw Gas Gn to Dilution Container Xn]

Step 5: Close valve b2, valve b6, and valve b7, and open valve b8.

Step 6: Repeat the opening and closing of the valve b7 to introduce the raw material gas Gn from the raw material container Zn into the dilution container Xn. When the raw material gas Gn is introduced into the dilution container Xn, the opening time and the closing time of the valve b7 are adjusted, and the pressure pg of the raw material gas Gn inside the dilution container Xn is set to the first partial pressure value. The pressure pg is expressed by formula (1). "V" represents the volume inside the dilution container Xn; "ng" represents the mass of the raw material gas Gn (mole); "R" represents the gas constant; "T" represents the temperature inside the dilution container Xn.

pg×V=ng×R×T...(1)

Since the volume V and the temperature T are known, and the pressure pg can be measured by the first pressure gauge PM1, the mass of the raw material gas Gn inside the dilution container Xn can be calculated based on equation (1).

According to Embodiment 1, 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, the temperature of the dilution container Xn and the partial pressure pg of the raw gas Gn can be controlled at The desired value. As a result, the raw material gas Gn of the desired physical mass can be introduced into the dilution container Xn.

In addition, when the pressure pg of the raw material gas Gn is low, the valve b6 may be opened, and the pressure pg may be measured by the second pressure gauge PM2.

Step 7: When the pressure pg of the source gas Gn becomes the first partial pressure value, the valve b7 is closed.

[Introduction of Carrier Gas CG to Dilution Container Xn]

Step 8: Close the valves b4 and b8, and open the valves b2, b3 and b7.

Step 9: Open the valve b6. The second pressure gauge PM2 measures the pressure inside the tube t2, the tube t3, and the tube t4. The operator confirms the degree of vacuum inside the tube t2, the tube t3, and the tube t4 with the second pressure gauge PM2.

Step 10: Close valve b2 and valve b6, and open valve b1.

Step 11: Repeat the opening and closing of the valve b4, and introduce the carrier gas CG into the dilution container Xn. When the carrier gas CG is introduced into the dilution container Xn, the opening time and the closing time of the valve b4 are adjusted, and the total pressure p of the diluted raw material gas Dn inside the dilution container Xn is set to a predetermined total pressure value. The total pressure p is expressed by formula (2). "V" represents the volume inside the dilution container Xn; "n" represents the mass of the diluted raw material gas Dn (mole); "R" represents the gas constant; "T" represents the temperature inside the dilution container Xn . Specifically, "n" is the sum of the material mass (mole) of the carrier gas CG inside the dilution container Xn and the material mass (mole) of the raw material gas Gn.

p×V=n×R×T...(2)

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

n=ng+nc...(3)

According to Embodiment 1, 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, the temperature of the dilution container Xn and the total pressure p of the diluted raw material gas Dn can be controlled At the desired value. As a result, the carrier gas CG of the desired physical mass can be introduced into the dilution container Xn.

Furthermore, the partial pressure pc of the carrier gas CG can be calculated from equation (4). "Pg" means the pressure of the raw material gas Gn inside the dilution container Xn, that is, the partial pressure of the raw material gas Gn.

p=pg+pc...(4)

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

Step 12: When the total pressure p of the diluted raw material gas Dn becomes a predetermined total pressure value, the valve b4 is closed. That is, when the partial pressure pc of the carrier gas CG becomes the second partial pressure value, the valve b4 is closed.

[Supply of Dilution Raw Gas Dn to Gas Phase Growth Apparatus 1]

Step 13: You can also open the valve b5. As a result, the flow path up to the first flow control unit Qn can be purged (purge) by the carrier gas CG.

Step 14: Close valve b1, valve b5, and valve b7, and open valve b2.

Step 15: Open the valve b6. The second pressure gauge PM2 measures the pressure inside the tubes t2 and t3. The operator confirms the degree of vacuum inside the tube t2 and the tube t3 with the second pressure gauge PM2. In addition, when the volume of the flow channels of the tubes t2 and t3 is smaller than the volume of the dilution container Xn, the fifteenth step is unnecessary.

Step 16: Close the valves b2, b3 and b6, and open the valves b4 and b5. As a result, the diluted raw material gas Dn is discharged from the dilution container Xn toward the first flow 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. 4. FIG. 4 is a schematic diagram of a part of the vapor phase growth system 100. As shown in FIG. 4, the dilution raw material gas D1 is contained in the dilution container X1. The diluted raw material gas D1 contains gallium trichloride (GaCl ₃ ) as the raw material gas G1 and nitrogen gas (N ₂ ) as the carrier gas CG. In addition, the dilution raw material gas D2 is accommodated in the dilution container X2. The diluted raw material gas D2 contains ammonia gas (NH ₃ ) as the raw material gas G2 and nitrogen gas (N ₂ ) as the carrier gas CG. In addition, nitrogen gas (N ₂ ) as the carrier gas CG is supplied to the second flow rate control unit 72. Chlorine gas (Cl ₂ ) as the etching gas EG is supplied to the third flow rate control unit 73.

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

The first flow control section Q1, the first flow control section Q2, the second flow control section 72, and the third flow control section 73 open the raw material introduction pipe A1, the raw material introduction pipe A2, the carrier introduction pipe 19, and the etching introduction pipe 21, respectively. As a result, the dilution raw material gas D1 is introduced into the chamber 3 from the dilution container X1; the dilution raw material 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 interior of the chamber 3, according to the reaction formula (r1), the gallium trichloride (G1) system and the ammonia gas (G2) produce a chemical reaction. As a result, gallium nitride (GaN) as a target substance is generated on the substrate S.

GaCl ₃ +NH ₃ →GaN+3HCl...(r1)

In the chamber 3, since there is no outflow channel of gallium trichloride (G1) and ammonia gas (G2), the outflow of gallium trichloride (G1) and ammonia gas (G2) from the chamber 3 is suppressed. Therefore, the utilization efficiency of gallium trichloride (G1) and ammonia gas (G2) can be improved.

On the other hand, the by-product exhaust unit 15 exhausts hydrogen chloride (HCl) as a by-product FG. Therefore, the generation speed of gallium nitride can be increased. Furthermore, after the residue discharge device 80 completes the formation of gallium nitride on the substrate S, the residue ZG inside the chamber 3 is discharged to clean the inside of the chamber 3.

(First modification)

Next, the pressure adjusting unit 64nA according to the first modification of Embodiment 1 of the present invention will be described with reference to FIG. 5. FIG. 5 is a schematic diagram of the pressure adjusting unit 64nA. As shown in FIG. 5, the pressure adjusting unit 64nA of the first modification has a variable volume of the dilution container Xn, and therefore is different from the pressure adjusting unit 64n shown in FIG. In other respects, the structure of the pressure adjusting unit 64nA is the same as the structure of the pressure adjusting unit 64n. The following mainly describes the differences between the first modification and Embodiment 1.

Each pressure adjusting unit 64 nA includes a volume changing unit 90 and a pressure adjusting unit 91. The dilution container Xn has a gas storage space 92. The gas storage space 92 is a space that can store gas.

The volume changing unit 90 is arranged inside the dilution container Xn. Next, the volume changing unit 90 changes the volume of the gas storage space 92 by changing the volume of the volume changing unit 90. As a result, the pressure inside the dilution container Xn changes according to the volume of the gas storage space 92.

Specifically, the pressure adjusting unit 91 adjusts the pressure inside the volume changing unit 90 to change the volume of the volume changing unit 90. For example, the pressure adjusting unit 91 sends the driving gas BG into the volume changing unit 90 and drives the volume changing unit 90 so as to expand the volume of the volume changing unit 90. In this case, the pressure inside the dilution container Xn will increase. For example, the pressure adjusting unit 91 discharges the gas EX from inside the volume changing unit 90 and drives the volume changing unit 90 so as to reduce the volume of the volume changing unit 90. In this case, the pressure inside the dilution container Xn will be reduced. In addition, since the volume changing unit 90 is separated from the inside of the dilution container Xn, it does not come into contact with the driving gas BG and the diluted raw material gas Dn.

The volume changing unit 90 is, for example, a bellows. The volume changing unit 90 includes, for example, a bottomed cylindrical element and a piston (Piston) into which the bottomed cylindrical element is inserted. The pressure adjustment unit 91 is, for example, an electro-pneumatic converter (Electropneumatic Converter).

As described above with reference to FIG. 5, in the first modification of Embodiment 1, the pressure inside the dilution container Xn can be adjusted to a desired value by the volume changing unit 90. That is, even after the carrier gas CG and the raw material gas Gn are introduced into the dilution container Xn, the total pressure p of the diluted raw material gas Dn can be adjusted to a desired value. Furthermore, before the carrier gas CG is introduced into the dilution container Xn, even after the raw material gas Gn is introduced into the dilution container Xn, the pressure of the raw material gas Gn in the dilution container Xn, that is, the partial pressure pg can be adjusted to the desired Value.

In addition, the pressure adjustment unit 91 may also receive information indicating the pressure of the gas storage space 92 from the first pressure gauge PM1. Therefore, the pressure adjusting unit 91 may change the volume of the volume changing unit 90 based on the pressure of the gas storage space 92. As a result, the feedback control (Feedback) is executed, so that the pressure of the gas storage space 92 can be adjusted with high accuracy. That is, the total pressure p of the diluted raw material gas Dn can be adjusted with high accuracy. Furthermore, the partial pressure pg of the source gas Gn can be adjusted with high accuracy.

In addition, in the first modification, the gas supply device 60 includes the pressure adjustment unit 64nA shown in FIG. 5 instead of the pressure adjustment unit 64n shown in FIG. 3. 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. In addition, when distinguishing a plurality of pressure adjusting units 64nA, it can be expressed as pressure adjusting units 641A, ..., 64NA (N is an integer of 2 or more).

(Second modification)

Next, the pressure adjusting unit 64nB according to the second modification of Embodiment 1 of the present invention will be described with reference to FIG. 6. FIG. 6 is a schematic diagram of the pressure adjusting unit 64nB. As shown in FIG. 6, the pressure adjusting unit 64nB of the second modification has a plurality of dilution containers Xmn with respect to one raw material container Zn, and therefore is different from the pressure adjusting unit 64n shown in FIG. 3. Otherwise, the structure of the pressure adjusting unit 64nB is the same as the structure of the pressure adjusting unit 64n. The following mainly describes the differences between the second modification and Embodiment 1.

Each pressure adjusting unit 64nB is provided with a plurality of dilution containers Xmn corresponding to one raw material container Zn instead of the dilution container Xn shown in FIG. 3, and each dilution container Xmn is provided with a thermometer TM and a first pressure gauge PM1 (pressure gauge). In addition, each pressure adjusting unit 64nB includes a first valve unit 75a instead of the first valve unit 75 shown in FIG. 3. 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. 3. Furthermore, the first valve unit 75a is provided with a plurality of tubes t1 corresponding to the plurality of dilution containers Xmn, respectively, instead of the tube t1 shown in FIG. 3. In addition, when distinguishing and explaining a plurality of dilution containers Xmn, it is described as dilution containers X1n, ..., XMn (M is an integer of 2 or more).

Each dilution container Xmn is connected to the corresponding valve b4 via the corresponding tube t1. The pipe t2 is connected to the valve b3, the plurality of valves b4, the valve b5, the valve b6, and the valve b7. Each dilution container Xmn mixes the raw material gas Gn and the carrier gas CG introduced from the raw material container Zn, and is accommodated as the diluted raw material 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. 3.

However, the valve portion Yn introduces the raw material gas Gn and the carrier gas CG into the dilution container Xmn at different time points for each dilution container Xmn during different time periods in which the plurality of dilution containers Xmn are allocated respectively. 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 valves b4 corresponding to the dilution container X2n to the dilution container XMn are closed.

Furthermore, for each dilution container Xmn, after the source gas Gn and the carrier gas CG are mixed, the valve portion Yn discharges the dilution source gas Dn from the dilution container Xmn. For example, when the dilution raw material gas Dn is discharged from the dilution container X1n, only the valve b4 corresponding to the dilution container X1n is opened, and the valves b4 corresponding to the dilution container X2n to the dilution container XMn are closed.

As described above with reference to FIG. 6, by the second modification of Embodiment 1, each pressure adjusting unit 64 nB is provided with a plurality of dilution containers Xmn. Next, the same raw material gas Gn is introduced into a plurality of dilution containers Xmn. Therefore, for example, when the concentration of the raw material gas Gn contained in the plurality of dilution containers Xmn is the same, a certain dilution container Xmn can be used as a spare container of the dilution container Xmn in use. Furthermore, for example, when the concentrations of the raw material gases Gn contained in the plurality of dilution containers Xmn are different, the diluted raw material gases Dn having different concentrations can be discharged from one pressure adjustment unit 64nB.

In addition, in the second modification, the gas supply device 60 includes the pressure adjustment unit 64nB shown in FIG. 6 instead of the pressure adjustment unit 64n shown in FIG. 3. 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. In addition, when distinguishing a plurality of pressure adjustment units 64nB, it can be expressed as pressure adjustment units 641B, ..., 64NB (N is an integer of 2 or more). Furthermore, when distinguishing the dilution container Xmn for each pressure adjustment unit 64nB, it can be expressed as the dilution containers Xm1, ..., XmN (N is an integer of 2 or more) relative to the pressure adjustment units 641B, ..., 64NB, respectively .

(Example 2)

7 to FIG. 11 for a gas-phase growth system 100 according to Embodiment 2 of the present invention. In the second embodiment, since the gas-phase growth device 1 introduces the mixed gas MG in which a plurality of raw material gases Gn are mixed, it is different from the first embodiment 1 in which the plurality of raw material gases Gn are individually introduced into the gas-phase growth device 1. The following mainly describes the differences between Embodiment 2 and Embodiment 1.

FIG. 7 is a schematic diagram of a vapor phase growth system 100 according to Embodiment 2 of the present invention. As shown in FIG. 7, the gas-phase growth system 100 includes a gas supply device 60A instead of the gas supply device 60 shown in FIG. 1. Furthermore, the vapor-phase growth system 100 is equipped with a single number of raw material introduction pipes 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 raw material gases Gn are mixed. In the mixed gas MG before being introduced into the chamber 3, a plurality of raw material gases Gn do not cause a chemical reaction.

The vapor-phase growth apparatus 1 is provided with the singular raw material inlet GP1 corresponding to the singular raw material introduction pipe A1. Therefore, the raw material introduction port GP1 passes through the raw material introduction pipe A1 to introduce the mixed gas MG into the chamber 3.

Next, the vapor-phase growth device 1 blocks the outflow of the raw material gas Gn from the inside of the chamber 3 to the outside during a part or all of the reaction period RP. Therefore, in a part or all of the reaction period RP, the chamber 3 is sealed. That is, the vapor-phase growth device 1 causes the mixed gas MG (that is, a plurality of different raw material gases Gn) to stay in the chamber 3 to generate a chemical reaction, and form a target substance on the substrate S.

As a result, according to Embodiment 2, the utilization efficiency of the raw material gas Gn contained in the mixed gas MG can be improved compared to when the mixed gas is circulated to form the target substance. In addition, according to the second embodiment, since it has the same structure as the first embodiment, it has the same effect as the first embodiment.

In addition, in the second embodiment, the singular raw material introduction ports GP1 pass through the singular raw material introduction tubes A1 to introduce the mixed gas MG into the chamber 3. That is, a plurality of different raw material gases Gn are introduced into the chamber 3 from a single raw material introduction port GP1. Therefore, the structure of the chamber 3 can be simplified compared to the case where a plurality of raw material gases Gn are introduced from the plurality of raw material introduction ports GPn, respectively. As a result, the cost of the vapor phase growth device 1 can be reduced. Furthermore, compared with the case where a plurality of raw material introduction pipes An are provided, since a single plurality of raw material introduction pipes A1 are provided, the structure of the vapor phase growth system 100 can be simplified. As a result, the cost of the vapor-phase growth system 100 can be reduced.

Continuing to refer 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 introduction pipe A1 and the raw material introduction port GP1.

Specifically, after supplying the fifth predetermined amount M5 of the mixed gas MG to the chamber 3, the gas supply device 60A blocks the flow path of the mixed gas MG to stop the supply of the mixed gas MG to the chamber 3. 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 introduction pipe A1 and the raw material introduction port GP1 is stopped.

Therefore, according to Embodiment 2, the outflow of the raw material gas Gn to the outside of the chamber 3 can be further suppressed. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

The fifth predetermined amount M5 represents, for example, the mass (mol), mass, or volume. The fifth predetermined amount M5 is the total of the plurality of first predetermined amounts M1 set for the plurality of raw material gases Gn, respectively. The first predetermined amount M1 is the same as the first predetermined amount M1 of Embodiment 1.

Therefore, according to Embodiment 2, the excess and deficiency of the mixed gas MG are suppressed, so that the correct amount of the mixed gas MG can be introduced into the chamber 3. As a result, the waste of the mixed gas MG can be suppressed.

Furthermore, the gas supply device 60A replenishes 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 reduction amount of the mixed gas MG caused by the chemical reaction inside the chamber 3.

Therefore, according to Embodiment 2, the shortage of the raw material gas Gn in the chamber 3 can be avoided, and the growth failure of the target substance can be suppressed.

In addition, when supplementing the mixed gas MG, the gas supply device 60A supplements the mixed gas MG in such a manner that the molar fraction of various raw material gases Gn is kept constant inside the chamber 3.

Therefore, according to Embodiment 2, the excess and deficiency of the raw material gas Gn are suppressed, so that the correct amount of the raw material gas Gn can be introduced into the chamber 3. As a result, the waste of the raw material gas Gn can be suppressed.

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

The sixth predetermined amount M6 represents, for example, the mass (mol), mass, or volume. The sixth predetermined amount M6 is the total of the plurality of second predetermined amounts M2 set for the plurality of raw material gases Gn, respectively. The second predetermined amount M2 is the same as the second predetermined amount M2 of Embodiment 1. Preferably, the sixth predetermined amount M6 is equal to, for example, the decrease amount of the mixed gas MG.

Next, after the sixth predetermined amount M6 of mixed gas MG is replenished, the gas supply device 60A blocks the flow path of the mixed gas MG to stop the mixed gas MG passing through the raw material introduction pipe A1 and the raw material introduction port GP1 to the chamber 3 Supplement.

Therefore, according to Embodiment 2, it is possible to further suppress the outflow of the raw material gas Gn from the outside of the chamber 3. As a result, the utilization efficiency of the raw material gas Gn can be further improved.

In addition, the gas supply device 60A may also pass through the raw material introduction pipe A1 and the raw material introduction port after the fifth predetermined amount of mixed gas MG M5 is supplied, according to the amount of reduction of the mixed gas MG caused by the chemical reaction inside the chamber 3 GP1, and replenish the mixed gas MG at any time. In this case, since the mixed gas MG is replenished at any time based only on the reduced amount of the mixed gas MG, the mixed gas MG is kept within the chamber 3 by a certain amount at any time. Therefore, the growth of the target substance can be controlled with high accuracy. In addition, on the other hand, when the mixed gas MG is replenished, the mixed gas MG does not flow out to the outside of the chamber 3, thereby improving the utilization efficiency of the mixed gas MG.

For example, in the gas supply device 60A, when the amount of the mixed gas MG in the chamber 3 becomes smaller than the threshold value Th3, the raw material introduction port GP1 can be used at any time according to the decrease in the mixed gas MG in the chamber 3 Supplement the mixed gas MG. Preferably, the threshold Th3 is set to the same value as, for example, the fifth predetermined amount M5. In this case, the mixed gas MG can be maintained at the fifth predetermined amount M5 inside the chamber 3. As a result, the growth of the target substance can be controlled with high accuracy.

Furthermore, for example, when the gas supply device 60A replenishes the mixed gas MG at any time, the mixed gas MG can be replenished at any time so that the molar fraction of various raw material gases Gn is kept constant inside the chamber 3. In this case, the excess and deficiency of the raw material gas Gn in the chamber 3 are suppressed, so that the correct amount of the raw material gas Gn can be introduced into the chamber 3. As a result, the waste of the raw material gas Gn can be suppressed.

In addition, the gas supply device 60A may replenish the carrier gas CG at any time when the mixed gas MG is replenished at any time. Furthermore, the gas supply device 60A may supplement the etching gas EG at any time when the mixed gas MG is replenished at any time.

In addition, the by-product exhaust section 15 is a system where the source gas Gn, the carrier gas CG, and the etching gas EG are exhausted together with the by-product FG when the concentration of the by-product FG becomes greater than the threshold Th2. The device 60A supplements the mixed gas MG to the chamber 3 according to the amount of reduction of the raw material gas Gn. The gas supply device 60A replenishes the mixed gas MG so that the molar fractions of various raw material gases Gn remain constant inside the chamber 3 when the mixed gas MG is replenished.

Preferably, here, the gas supply device 60A supplies the diluted mixed gas UM instead of the mixed gas MG to the gas-phase growth device 1. 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, with reference to FIG. 7, the difference between the state of supplying the diluted mixed gas UM instead of the mixed gas MG to the gas-phase growth device 1 and the state of supplying the mixed gas MG to the gas-phase growth device 1 will be described.

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

Specifically, after supplying the diluted mixed gas UM containing the mixed gas MG of the fifth predetermined amount M5 to the chamber 3, the gas supply device 60A blocks the flow path of the diluted mixed gas UM to stop the supply of the diluted gas to the chamber 3 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 the diluted mixed gas from the raw material introduction pipe A1 and the raw material introduction port GP1 The UM import system was stopped.

In addition, the gas supply device 60A replenishes the diluted gas mixture UM to the chamber 3 through the raw material introduction pipe A1 and the raw material introduction port GP1 according to the reduction amount of the mixed gas MG caused by the chemical reaction inside the chamber 3. In addition, when supplementing the diluted mixed gas UM, the gas supply device 60A supplements the diluted mixed gas UM so that the molar fraction of the raw material gas Gn remains constant inside the chamber 3.

Specifically, the gas supply device 60A passes through the raw material introduction pipe A1 and the raw material introduction port GP1 in accordance with the reduced amount of the mixed gas MG in the chamber 3 to dilute the mixed gas UM containing the sixth predetermined amount M6 of the mixed gas MG Supply to the chamber 3.

Next, after the diluted gas mixture UM containing the mixed gas MG of the sixth predetermined amount M6 is replenished, the gas supply device 60A blocks the flow path of the diluted gas mixture UM to stop passing through the raw material introduction pipe A1 and the raw material introduction port GP1 toward the chamber Chamber 3 is supplemented with diluted mixed gas UM.

In addition, the gas supply device 60A may also pass through the raw material according to the reduced amount of the mixed gas MG caused by the chemical reaction in the chamber 3 after the diluted mixed gas UM containing the mixed gas MG of the fifth predetermined amount M5 is supplied. The introduction pipe A1 and the raw material introduction port GP1 supplement the diluted mixed gas UM at any time.

For example, in the gas supply device 60A, when the amount of the mixed gas MG in the chamber 3 becomes smaller than the threshold value Th3, the raw material introduction port GP1 can be used at any time according to the decrease in the mixed gas MG in the chamber 3 The diluted mixed gas UM containing the mixed gas MG is replenished.

In addition, for example, when the gas supply device 60A replenishes the diluted mixed gas UM at any time, the diluted mixed gas UM can be replenished at any time so that the molar fractions of various raw material gases Gn remain constant inside the chamber 3.

In addition, the gas supply device 60A may replenish the carrier gas CG at any time when the diluted mixed gas UM is replenished at any time. Furthermore, the gas supply device 60A may also supplement the etching gas EG at any time when the diluted mixed gas UM is supplemented at any time.

In addition, the by-product exhaust section 15 is a system where the source gas Gn, the carrier gas CG, and the etching gas EG are exhausted together with the by-product FG when the concentration of the by-product FG becomes greater than the threshold Th2. The device 60A replenishes the diluted mixed gas UM to the chamber 3 according to the reduction amount of the raw material gas Gn. The gas supply device 60A supplements the diluted mixed gas UM so that the molar fraction of the raw material gas Gn remains constant inside the chamber 3 when the diluted mixed gas UM is replenished.

Unless otherwise specified, in Embodiment 2, the gas supply device 60A supplies the diluted gas mixture UM instead of the gas mixture MG to the gas phase growth device 1.

Next, the gas supply device 60A will be described with reference to FIG. 8. 8 is a schematic diagram of the gas supply device 60A. As shown in FIG. 8, the gas supply device 60A includes a vacuum pump 61, a control unit 62, a thermostat 63 (temperature control unit), a pressure adjustment unit 64A, a first flow control unit Q1 (flow control unit), and a second flow rate The control unit 72 and the third flow control unit 73. The pressure adjusting unit 64A includes a dilution container X1, a valve portion Y1 (introduction portion), and a plurality of raw material containers Zn (a plurality of gas containers). Next, the gas supply device 60A supplies gas to the vapor phase growth device 1 (FIG. 7). In addition, in this 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 thermostatic bath 63, the valve section Y1, the first flow control section Q1, the second flow control section 72, and the third flow control section 73 are controlled and operated by the control section 62. In addition, the control unit 62 includes a processor and a memory device. Therefore, the processor controls the vacuum pump 61, the thermostat 63, the valve section Y1, the first flow control section Q1, the second flow control section 72 and the third flow control section by executing the computer program stored in the memory device 73.

The thermostat 63 controls the temperature of the pressure adjusting unit 64A, so that the temperature of the pressure adjusting unit 64A is maintained at a certain temperature. The pressure adjusting unit 64A is arranged inside the thermostat 63.

The pressure adjustment unit 64A generates a diluted mixed gas UM by diluting the mixed gas MG in which a plurality of raw material gases Gn are mixed by the carrier gas CG. Next, the pressure adjusting unit 64A discharges the diluted mixed gas UM containing the mixed gas MG. Furthermore, the pressure adjusting unit 64A adjusts the partial pressure of the carrier gas CG and the partial pressures of various raw material gases Gn in the dilution container X1 when the diluted mixed gas UM is generated.

Specifically, the plurality of raw material containers Zn respectively contain a plurality of different raw material gases Gn (a plurality of different gas). The raw material gas Gn is a pure raw material gas that has not been diluted, and has a certain pressure (vapor pressure) inside the raw material container Zn.

The valve portion Y1 introduces a plurality of raw material gases Gn from a plurality of raw material containers Zn into a dilution container X1 at different time points, and uses a carrier gas for diluting the plurality of raw material gas Gn at a time point different from the plurality of raw material gas Gn CG is introduced into the dilution container X1. As a result, a dilution mixed gas UM in which a plurality of source gas Gn and carrier gas CG are mixed is generated in the dilution container X1.

For example, the valve portion Y1 introduces a plurality of different raw material gases Gn from the plurality of raw material containers Zn into the dilution container X1 at different time points. As a result, the mixed gas MG in which a plurality of raw material gases Gn are mixed is accommodated in the dilution container X1. Next, the valve portion Y1 introduces the carrier gas CG into the dilution container X1 at a time point different from the plurality of raw material gases Gn. As a result, the diluted mixed gas UM in which the mixed gas MG and the carrier gas CG are mixed is generated in the dilution container X1.

In addition, the valve portion Y1 adjusts the partial pressure of each raw material 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 raw material gas Gn is set to the first partial pressure value, and the partial pressure pc of the carrier gas CG is set Set to the second partial pressure value. The first partial pressure value is set for each raw material gas Gn based on the chemical reaction formula when a plurality of different raw material gases Gn generate a chemical reaction. In addition, when distinguishing and explaining a plurality of partial pressures pgn, it is described as partial pressures pg1, ..., pgN (N is an integer of 2 or more). Therefore, that is, p=pg1+, ..., +pgN+pc,.

The dilution container X1 mixes a plurality of raw material gas Gn and a carrier gas CG introduced from the plurality of raw material containers Zn, and stores it as a dilution mixed gas UM (dilution gas). Next, after the plurality of source gas Gn and carrier gas CG are mixed, the valve portion Y1 discharges the diluted mixed gas UM from the dilution container X1. That is, the valve portion Y1 is to mix the plurality of raw gas Gn and the carrier gas CG, and adjust the partial pressure pgn of the various raw gas Gn and the partial pressure pc of the carrier gas CG, and then to dilute the mixed gas UM from the dilution container X1 emission.

In addition, in this specification, the diluted mixed gas UM is an example of a diluted gas in which the gas (specifically, the mixed gas MG) supplied to the gas-phase growth device 1 passing through the gas supply device 60A and the carrier gas CG are mixed .

The first flow control unit Q1 may be provided corresponding to the valve unit Y1. Furthermore, the first flow control unit Q1 may be provided corresponding to the raw material introduction pipe A1 (FIG. 7 ).

The first flow control unit Q1 controls the flow rate of the diluted mixed gas UM discharged from the valve unit Y1. Next, the first flow control unit Q1 supplies the diluted mixed gas UM to the chamber 3 through the raw material introduction pipe A1. Specifically, the first flow control unit Q1 controls the volume flow or mass flow of the diluted mixed gas UM based on the differential pressure between the upstream and downstream of the laminar flow element using the principle of Hagen-Baiyi flow.

As described above with reference to FIG. 8, according to Embodiment 2, since the carrier gas CG is introduced into the dilution container X1, the dilution mixed gas UM can be increased compared to the case where only the mixed gas MG is introduced into the dilution container X1. The total pressure p. Therefore, compared with the case where only the mixed gas MG is introduced into the dilution container X1, the mixed gas MG tends to move toward the first flow control unit Q1 and the vapor-phase growth device 1. That is, the total pressure p of the diluted mixed gas UM in the dilution container X1 ensures the power to move the mixed gas MG (that is, the raw material gas Gn). On the other hand, by adjusting the amount (material mass, volume, or mass) of the raw material gas Gn introduced from the raw material container Zn to the dilution container X1, the dilution in the dilution container X1 can be adjusted with high precision for each raw material gas Gn The amount (material mass, volume, or mass) of the raw gas Gn contained in the mixed gas UM.

As a result, compared to the case where the carrier gas flow rate is controlled while the carrier gas is being flown to adjust the supply amount of the raw material gas as in the prior art, the first flow rate control along with the carrier gas CG can be adjusted with high accuracy The amount (material mass, volume amount, or mass) of the raw material gas Gn moved by the part Q1 and the vapor-phase growth device 1, that is, the supply amount of the raw material gas Gn. Furthermore, compared with the case where the raw material gas is directly supplied from the bubbler to the gas supply point as in the prior art, the diluted mixed gas UM is discharged from the dilution container X1, whereby the raw gas Gn can be adjusted with high accuracy Supply amount. Since the supply amount of the raw material gas Gn can be adjusted with high precision, the vapor-phase growth device 1 can form a target substance of good quality (for example, a target substance with few defects and high purity).

Furthermore, according to Embodiment 2, the total pressure p of the diluted mixed gas UM in the dilution container X1 ensures the power to move the raw gas Gn, and the diluted mixed gas containing the raw gas Gn is discharged from the diluted container X1 UM. Therefore, as in the first embodiment, the supply amount of the raw material gas Gn is not easily affected by temperature, so temperature management is easy. In addition, in the second embodiment, for the same reason as the first embodiment, the supply amount of the raw material gas Gn can be adjusted with higher accuracy; further, the cost of the gas supply device 60A can be reduced. Furthermore, in the second embodiment, for the same reason as the first embodiment, it is possible to suppress the increase in maintenance cost; further, it is possible to suppress the shape of the raw material container Zn from being restricted.

Furthermore, according to the second embodiment, as in the first embodiment, a small amount of mixed gas MG (that is, a small amount of raw material gas Gn) can be easily supplied. In addition, in the second embodiment, since the dilution mixed gas UM containing the raw material gas Gn is discharged from the dilution container X1, the supply amount of the raw material gas Gn is stabilized in the same manner as in the first embodiment.

Furthermore, according to Embodiment 2, by adjusting the introduction amount of the carrier gas CG introduced into the dilution container X1, the total pressure p of the diluted mixed gas UM can be adjusted. That is, the power of the mobile mixed gas MG (that is, the raw material gas Gn) can be adjusted.

Furthermore, according to Embodiment 2, by adjusting the partial pressure pgn of the raw gas Gn in the dilution container X1, the amount (material mass, volume, or mass) of the raw gas Gn contained in the diluted mixed gas UM can be adjusted . As a result, the amount (material mass, volume amount, or mass) of the raw material gas Gn that moves along with the carrier gas CG toward the first flow control unit Q1 and the vapor phase growth device 1 can be adjusted with higher accuracy.

Furthermore, according to Embodiment 2, since a plurality of raw material containers Zn are provided, the amount of raw material gas Gn introduced into the dilution container X1 can be adjusted for each raw material container Zn. Therefore, the various raw material gases Gn can be introduced into the dilution container X1 so as to have a molar fraction based on the chemical reaction formula for generating the target substance. That is, when the raw material gas Gn is supplied to the vapor phase growth device 1, the mole fraction of the raw material gas Gn can be easily adjusted.

Furthermore, according to Embodiment 2, by mixing a plurality of raw material gases Gn from a plurality of raw material containers Zn in one dilution container X1 and further introducing a carrier gas CG, it is generated in one dilution container X1 There is diluted mixed gas UM. Therefore, the structure of the gas supply device 60A can be simplified compared to the case where a plurality of dilution containers Xn are provided respectively corresponding to 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, by using the pressure (vapor pressure) of the raw material gas Gn inside the raw material container Zn, the raw material gas Gn can be moved from the raw material container Zn to the dilution container X1. Therefore, the active device provided to move the raw material gas Gn from the raw material container Zn to the dilution container X1 can be suppressed. 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 Embodiment 2, the first flow rate control unit Q1 uses the total pressure p of the diluted mixed gas UM to easily supply the diluted mixed gas UM to the gas-phase growth device 1.

In addition, the dilution container X1 may not introduce the carrier gas CG, but may respectively introduce a plurality of raw material gases Gn from the plurality of raw material containers Zn and accommodate the mixed gas MG. In this case, the first flow rate control unit Q1 may control the flow rate of the mixed gas MG discharged from the valve unit Y1. Next, the first flow control unit Q1 may supply the mixed gas MG to the chamber 3 through the raw material introduction pipe A1. Specifically, the first flow control unit Q1 may also use the principle of Hagen-Baiyi flow to control the volume flow or mass flow of the mixed gas MG based on the differential pressure between the upstream and downstream of the laminar flow element.

Next, the pressure adjustment unit 64A will be described with reference to FIG. 9. 9 is a schematic diagram of the pressure adjusting unit 64A. As shown in FIG. 9, the pressure adjustment unit 64A further includes a thermometer TM, a first pressure gauge PM1 (pressure gauge), a second pressure gauge PM2, tubes t1 to 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 tube t5n. The valves b1 to b7 and the valve b8n are, for example, stop valves. The plurality of second valve units 77n are respectively provided corresponding to the plurality of raw material containers Zn.

The tube t1 is connected to the dilution container X1 and the valve b4. The pipe t2 connects the valves b3 to b7 to each other. The pipe t3 connects the valves b1 to b3 to each other. The tube t4 connects the valve b7 and the plurality of valves b8n to each other. The tube t5n is connected to the valve b8n and the raw material container Zn. In addition, the valve b8n may also be directly connected to the raw material container Zn. The valve b4 may also be directly connected to the dilution container X1.

In addition, when distinguishing and explaining a plurality of second valve units 77n, it is described as the second valve units 771, ..., 77N (N is an integer of 2 or more). When distinguishing and explaining a plurality of valves b8n, they are described as valves b81, ..., b8N (N is an integer of 2 or more). When distinguishing and explaining a plurality of tubes t5n, it is described as tubes t51, ..., t5N (N is an integer of 2 or more).

The control procedure of the valve portion Y1 will be described with continued reference to FIG. 9. The control step includes the first step to the 22nd step. In the initial state of the valve portion Y1, the valves b1 to b7 and the valve b8n are closed. For ease of understanding, the following will describe the operation procedure of the valve portion Y1 when two raw material containers Zn and two second valve units 77n are provided.

[Vacuum suction and flushing]

The first step to the fourth step are the same as the first step to the fourth step of Embodiment 1.

[Introduction of Raw Gas G1 to Dilution Container X1]

Step 5: Close valve b2, valve b6, and valve b7, and open valve b81.

Step 6: Repeat the opening and closing of the valve b7 to introduce the raw material gas G1 from the raw material container Z1 into the dilution container X1. When the raw material gas G1 is introduced into the dilution container X1, the opening time and the closing time of the valve b7 are adjusted, and the pressure pg1 of the raw material gas G1 inside the dilution container X1 is set to the first partial pressure value. The pressure pg1 is expressed by formula (5). "V" represents the volume inside the dilution container X1; "ng1" represents the mass of the raw material gas G1 (mole); "R" represents the gas constant; "T" represents the temperature inside the dilution container X1.

pg1×V=ng1×R×T...(5)

Since the volume V and the temperature T are known, and the pressure pg1 can be measured by the first pressure gauge PM1, the mass of the raw material gas G1 inside the dilution container X1 can be calculated based on equation (5).

According to Embodiment 2, by monitoring the temperature of the dilution container X1 with a thermometer TM and monitoring the pressure of the dilution container X1 through the first pressure gauge PM1, the temperature of the dilution container X1 and the partial pressure pg1 of the raw gas G1 can be controlled at The desired value. As a result, the raw material gas G1 of the desired physical mass can be introduced into the dilution container X1.

In addition, when the pressure pg1 of the raw material gas G1 is low, the valve b6 may be opened, and the pressure pg1 may be measured by the second pressure gauge PM2.

Step 7: When the pressure pg1 of the raw material gas G1 becomes the first partial pressure value, the valve b7 is closed.

Step 8: Close the valves b4 and b81, and open the valves b2, b3 and b7.

Step 9: Open the valve b6. The second pressure gauge PM2 measures the pressure inside the tube t2, the tube t3, and the tube t4. The operator confirms the degree of vacuum inside the tube t2, the tube t3, and the tube t4 with the second pressure gauge PM2.

[Introduction of Raw Gas G2 to Dilution Vessel X1]

Step 10: Close valve b2, valve b3, valve b6, and valve b7, and open valve b82.

Step 11: Open the valve b4.

Step 12: Repeat the opening and closing of the valve b7 to introduce the raw material gas G2 from the raw material container Z2 into the dilution container X1. When the raw material gas G2 is introduced into the dilution container X1, the opening time and the closing time of the valve b7 are adjusted, and the total pressure pm of the mixed gas MG inside the dilution container X1 is set to the first total pressure value. The total pressure pm is expressed by equation (6). "Pg1" indicates the pressure of the raw material gas G1 in the dilution container X1, that is, the partial pressure of the raw gas G1; "pg2" indicates the partial pressure of the raw material 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 raw material gas G2 can be calculated based on equation (6).

Furthermore, the total pressure pm is expressed by equation (7). "V" means the volume inside the dilution container X1; "ng1" means the mass of the raw material gas G1 (mole); "ng2" means the mass of the raw material gas G2 (mole); "R" means the Gas constant; "T" means the temperature inside the dilution container X1.

pm×V=(ng1+ng2)×R×T...(7)

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

According to Embodiment 2, by monitoring the temperature of the dilution container X1 through the thermometer TM and monitoring the pressure of the dilution container X1 through the first pressure gauge PM1, the temperature of the dilution container X1 and the partial pressure pg2 of the raw gas G2 can be controlled at The desired value. As a result, the raw material gas G2 of the desired physical mass can be introduced into the dilution container X1.

In addition, when the pressure pg2 of the raw material gas G2 is low, the valve b6 may be opened, and the total pressure pm may be measured by the second pressure gauge PM2.

Step 13: When the total pressure pm of the mixed gas MG becomes the first total pressure value, the valve b7 is closed. That is, when the partial pressure pg2 of the raw material gas G2 becomes the first partial pressure value, the valve b7 is closed. In addition, the first partial pressure value is set individually for the raw material gas G1 and the raw material gas G2.

[Introduction of Carrier Gas CG to Dilution Container X1]

Step 14: Close valve b4 and valve b82, and open valve b2, valve b3 and valve b7.

Step 15: Open the valve b6. The second pressure gauge PM2 measures the pressure inside the tube t2, the tube t3, and the tube t4. The operator confirms the degree of vacuum inside the tube t2, the tube t3, and the tube t4 with the second pressure gauge PM2.

Step 16: Close valve b2 and valve b6, and open valve b1.

Step 17: Repeat the opening and closing of the valve b4, and introduce the carrier gas CG into the dilution container X1. When the carrier gas CG is introduced into the dilution container X1, the opening time and the closing time of the valve b4 are adjusted, and the total pressure p of the diluted mixed gas UM inside the dilution container X1 is set to the second total pressure value (that is, the predetermined total pressure value ). The total pressure p is expressed by formula (8). "V" represents the volume inside the dilution container X1; "n" represents the mass of the diluted mixed gas UM (mole); "R" represents the gas constant; "T" represents the temperature inside the dilution container X1 . Specifically, "n" is the sum of the material mass (mole) of the carrier gas CG inside the dilution container X1, the material mass (mole) of the raw material gas G1 and the material mass (mole) of the raw material gas G2.

p×V=n×R×T...(8)

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

n=ng1+ng2+nc...(9)

According to Embodiment 2, by monitoring the temperature of the dilution container X1 through the thermometer TM and monitoring the pressure of the dilution container X1 through the first pressure gauge PM1, the temperature of the dilution container X1 and the total pressure p of the diluted mixed gas UM can be controlled At the desired value.

Furthermore, the partial pressure pc of the carrier gas CG can be calculated from equation (10). "Pg1" means the pressure of the raw material gas G1 inside the dilution container X1, that is, the partial pressure of the raw gas G1; "pg2" means the pressure of the raw material gas G2 inside the dilution container X1, that is, the fraction of the raw gas G2 Pressure.

p=pg1+pg2+pc...(10)

Based on the total pressure p, partial pressure pg1, partial pressure pg2 and partial pressure pc, or the mass n, mass ng1, mass ng2 and mass nc, the mole fraction of the raw gas G1 and the raw gas G2 can be calculated Molar fraction of the carrier gas and the carrier gas CG.

Step 18: 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 reaches the second predetermined value, the valve b4 is closed.

[Supply of Dilution Raw Gas Dn to Gas Phase Growth Apparatus 1]

Step 19: The valve b5 can also be opened. As a result, the flow path from the valve b5 up to the first flow control unit Q1 can be washed (rinsed) by the carrier gas CG.

Step 20: Close valve b1, valve b5, and valve b7, and open valve b2.

Step 21: Open the valve b6. The second pressure gauge PM2 measures the pressure inside the tubes t2 and t3. The operator confirms the degree of vacuum inside the tube t2 and the tube t3 with the second pressure gauge PM2. In addition, when the volume of the flow channels of the tubes t2 and t3 is smaller than the volume of the dilution container X1, step 15 is not required.

Step 22: Close valve b2, valve b3, and valve b6, and open valve b4, valve b5. As a result, the diluted mixed gas UM is discharged from the dilution container X1 toward the first flow control unit Q1 (FIG. 8 ).

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

In the initial state, the first flow control section Q1 closes the raw material introduction pipe A1; the second flow control section 72 closes the carrier introduction pipe 19; the third flow control section 73 closes the etching introduction pipe 21; the residue discharge device 80 series The residue discharge pipe 25 is closed; the by-product exhaust section 15 closes the by-product exhaust pipe 27.

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

In the embodiment 2 described with reference to FIG. 10, in the same manner as the embodiment 1 described with reference to FIG. 4, gallium nitride (GaN) as a target substance grows on the substrate S. Next, as in the first embodiment, the utilization efficiency of gallium trichloride (G1) and ammonia gas (G2) can be improved. In addition, as in the first embodiment, the growth rate of gallium nitride can be increased. Furthermore, as in Embodiment 1, the residue ZG inside the chamber 3 can be exhausted to clean the inside of the chamber 3.

(Modification)

Next, a gas supply device 60A according to a modification of Embodiment 2 of the present invention will be described with reference to FIG. 11. In a modified example, the temperature control of the dilution container X1 and the first valve unit 75 and the temperature control of the raw material container Zn and the second valve unit 77n can be performed separately, and at this point, it is the implementation example 2 that the temperature control cannot be performed separately different. The following mainly describes the differences between the modified example and Embodiment 2.

FIG. 11 is a schematic view of a part of the gas supply device 60A. As shown in FIG. 11, the gas supply device 60A of the modified example includes a first constant temperature bath 63A (first temperature control unit) and a plurality of second constant temperature baths 63Bn (second temperature control unit) instead of the constant temperature shown in FIG. 9槽63。 Groove 63. In addition, when distinguishing and explaining a plurality of second constant temperature baths 63Bn, it is described as the second constant temperature baths 63B1, ..., 63BN (N is an integer of 2 or more).

The first thermostat 63A system controls the temperature of the dilution container X1 and the temperature of the first valve unit 75, and maintains the temperature of the dilution container X1 and the temperature of the first valve unit 75 at a constant temperature (for example, the first temperature). The first thermostat 63A is independent of the second thermostat 63Bn and controls the temperature of the dilution container X1 and the first valve unit 75. The dilution container X1 and the first valve unit 75 are arranged inside the first thermostat 63A.

Preferably, the first constant temperature bath 63A keeps the temperature of the dilution container X1 and the first valve unit 75 higher than the temperature at which the vapor pressure equivalent to the partial pressure of the raw material gas Gn inside the dilution container X1 can be obtained. temperature. This is to suppress the liquefaction or solidification of the raw material 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 arranged inside the corresponding second constant temperature bath 63Bn.

The second thermostat 63Bn system 1 controls the temperature of the corresponding raw material container Zn and the corresponding temperature of the second valve unit 77n, and maintains the temperature of the corresponding raw material container Zn and the temperature of the corresponding second valve unit 77n At a certain temperature (for example, the second temperature). Each second constant temperature bath 63Bn is independent and controls the temperature of the corresponding raw material container Zn and the corresponding second valve unit 77n. Furthermore, each second thermostat 63Bn is independent of the first thermostat 63A, and controls the temperature of the corresponding raw material container Zn and the corresponding second valve unit 77n.

As described above with reference to FIG. 11, according to the modification of Embodiment 2, since the second thermostat 63Bn and the first thermostat 63A are provided separately, they do not depend on the temperature of the dilution container X1 and the first valve unit 75. This can control the temperature of the raw material container Zn. Therefore, the pressure (vapor pressure) of the raw material gas Gn in the raw material container Zn can be adjusted to a desired value. For example, the second constant temperature 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 raw material gas Gn inside the raw material container Zn can be increased.

If the pressure (vapor pressure) of the raw material gas Gn inside the raw material container Zn can be adjusted to a desired value, the pressure range of the raw material 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 increased, so that the conditions when the target substance is formed on the substrate S can be expanded. Furthermore, since the sufficient total pressure p of the diluted mixed gas UM in the diluted container X1 can be ensured, the diluted mixed gas UM can be stably supplied to the first flow control unit Q1.

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

In addition, a plurality of raw material containers Zn and a plurality of second valve units 77n may be arranged inside one second constant temperature bath 63B1. Next, the temperature of the plurality of raw material containers Zn and the plurality of second valve units 77n may be collectively controlled by the second constant temperature bath 63B1.

The above has described the embodiment of the present invention with reference to the drawings. However, the present invention is not limited to the above-mentioned embodiments, and various embodiments (for example, (1) to (4) below) can be implemented without departing from the gist thereof. Furthermore, various inventions can be formed by appropriately combining a plurality of constituent elements described in the above-described embodiment. For example, several constituent elements may be deleted from all constituent elements shown in the embodiment. In order to make the drawings easy to understand, the respective constituent elements are schematically shown in the main body, and the number of each constituent element shown in the drawings may be different from the actual one due to the drawing. In addition, each component shown in the above embodiment is only an example and is not intended to be particularly limited. Various changes can be made within a range that does not substantially deviate from the effect of the present invention.

(1) The volume change section 90 and the pressure adjustment section 91 described with reference to FIG. 5 may be provided in the pressure adjustment unit 64nB described with reference to FIG. 6, or the pressure adjustment unit 64A described with reference to FIGS. 9 and 11 . Furthermore, 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. Further, the first thermostatic bath 63A and the second thermostatic bath 63B1 described with reference to FIG. 11 may be replaced by the thermostatic bath 63 described with reference to FIGS. 3, 5 and 6 and provided with reference to FIGS. 3, 5 and 6. The gas supply device 60 illustrated in FIG. 6. In other respects, the first modification of the first embodiment, the first modification of the first embodiment, the second modification of the first embodiment, the second embodiment and the second modification of the second embodiment can be combined as appropriate.

(2) In the vapor-phase growth device 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. In addition, the target substance may be a thin film or a bulk material (Bulk), which is not particularly limited. Furthermore, the type of raw material gas Gn is not particularly limited. Furthermore, the by-product exhaust unit 15 may also discharge liquid or solid by-products.

In addition, 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 portion 8 and the cooling portion 17 may not be provided. The positions of the raw material introduction port GPn, the carrier introduction port CP, the etching introduction port EP, the residue discharge port ZP, and the by-product exhaust port FP are not particularly limited. The position of the holding portion 5 is not particularly limited. In addition, although the thermostat 63, the first thermostat 63A, and the second thermostat 63Bn are cited as an example of the temperature control unit, the temperature control unit is not limited thereto, and may be a heater, for example.

(3) In the gas-phase growth device described with reference to FIGS. 1 to 11, the capacities of the plurality of dilution containers Xn may be the same or different. Furthermore, the capacity of the plurality of raw material containers Zn may be the same or different. Furthermore, in the vapor-phase growth device 1 described with reference to FIG. 6, the capacities of the plurality of dilution containers Xmn may be the same or different. Furthermore, the concentration of the raw material gas Gn contained in the plurality of dilution containers Xmn may be the same or different. Therefore, in the valve portion Yn, the concentration of the raw material gas Gn contained in the plurality of dilution containers Xmn may be the same, and the raw material gas Gn and the carrier gas CG may be introduced into each dilution container Xmn. In addition, in the valve portion Yn, the concentration of the raw material gas Gn contained in the plurality of dilution containers Xmn may be different, and the raw material gas Gn and the carrier gas CG may be introduced into each dilution container Xmn. In addition, 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) Where the gas supplied through 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 not limited to the gas-phase growth device 1, On the other hand, the gas supply device 60 and the gas supply device 60A may supply the gas to be supplied to an arbitrary gas supply point (for example, device or substance). In addition, the type of the raw material gas Gn is not particularly limited, and various gases can be supplied instead of the raw material gas Gn. In addition, the first flow rate control unit Qn, the second flow rate control unit 72, and the third flow rate control unit 73 may be regarded as the structure of the vapor phase growth device 1.

For example, the gas supply device 60 and the gas supply device 60A can supply gas to various analysis instruments (such as a trace analysis instrument). For example, the gas supply device 60 and the gas supply device 60A can be used in the field of chemical biology or the medical field. For example, the gas supply device 60 and the gas supply device 60A may supply gas to a bioreactor (Bioreactor), or may supply gas to a cell culture device, or may supply gas to a microreactor.

Furthermore, in the gas supply device 60 described with reference to FIGS. 2, 3, 5 and 6, singular pressure adjustment units 64 n, singular pressure adjustment units 64 nA, and singular pressures may be provided. The adjustment unit 64nB may be provided with an singular first flow control unit Qn. In the gas supply device 60A described with reference to FIGS. 8, 9 and 11, a single number of raw material containers Zn may be provided, and a single second number of constant temperature baths 63Bn may be provided.

[Industry availability]

The present invention relates to a gas supply device that has industrial applicability.

60‧‧‧Gas supply device

61‧‧‧Vacuum pump

62‧‧‧Control Department

63‧‧‧Constant temperature bath

64n‧‧‧Pressure adjustment unit

72‧‧‧ 2nd Flow Control Department

73‧‧‧ Third Flow Control Department

CG‧‧‧Carrier gas

EG‧‧‧Etching gas

Dn‧‧‧Dilution raw material gas

Gn‧‧‧ raw gas

Qn‧‧‧First Flow Control Department

Xn‧‧‧Dilution container

Yn‧‧‧Valve (introduction)

Zn‧‧‧Raw material container

Claims (11)

A gas supply device is provided with: a gas container, which contains a gas; a dilution container, which mixes the gas introduced from the gas container and a carrier gas that dilutes the gas, and stores it as a dilution gas; The gas and the carrier gas are introduced into the dilution container at different time points; and a pressure gauge is used to measure the pressure inside the dilution container; wherein, the introduction part is based on the measurement result of the pressure gauge to The total pressure of the dilution gas inside is set to a predetermined total pressure value, and the total pressure of the dilution gas inside the dilution container is used to ensure the power to move the gas; where the gas and the carrier gas are mixed, And after setting the total pressure of the dilution gas to the predetermined total pressure value, the dilution gas is discharged from the dilution container. The gas supply device according to claim 1, wherein the gas container contains a raw material gas as the gas, and the raw gas system generates a substance gas by chemical reaction. The gas supply device as described in claim 1 or 2 includes: a plurality of the gas containers; a plurality of the dilution containers corresponding to the plurality of gas containers; and a plurality of the introduction parts corresponding to the respective A plurality of dilution containers; wherein the plurality of gas containers respectively contain a plurality of the gases different from each other; wherein each of the dilution containers mixes the gas and the carrier gas introduced from the corresponding gas container and serves as the Diluted gas and contain; Each of the introduction parts introduces the gas and the carrier gas into the corresponding dilution container at different time points; wherein, after the gas and the carrier gas are mixed, the dilution gas is discharged from the corresponding dilution container . The gas supply device described in claim 1 or 2 includes: a plurality of the dilution containers corresponding to the gas container; wherein each of the dilution containers mixes the gas and the carrier gas introduced from the gas container, And contained as the dilution gas; wherein, the introduction part introduces the gas and the carrier gas at different time points for each of the dilution containers in different time periods in which the plurality of dilution containers are allocated respectively The dilution container; wherein, for each of the dilution containers, after the gas and the carrier gas are mixed, the dilution gas is discharged from the dilution container. The gas supply device described in claim 1 or 2 includes: a plurality of the gas containers; wherein the plurality of gas containers respectively contain a plurality of the gases different from each other; wherein the dilution container is mixed from the plurality The plurality of gases and the carrier gas introduced into the gas container, and accommodated as the dilution gas; wherein, the introduction part introduces the plurality of gases into the dilution container at different time points; wherein, in the plurality of gases After the carrier gas is mixed, the dilution gas is discharged from the dilution container. The gas supply device described in claim 1 or 2 further includes: The volume changing unit changes the volume of the gas storage space of the dilution container; wherein the gas storage space is a space that can contain gas; wherein the volume changing unit is arranged inside the dilution container and changes by changing the volume The size of the part changes the volume of the gas storage space. The gas supply device according to claim 1 or 2 further includes: a first temperature control unit that controls the temperature of the dilution container; and a second temperature control unit that controls the temperature of the gas container. The gas supply device described in claim 1 or 2 further includes a flow rate control unit for controlling the flow rate of the dilution gas discharged from the introduction unit. The gas supply device according to claim 1 or 2 further includes: a thermometer for measuring the temperature inside the dilution container. The gas supply device according to claim 1 or 2, wherein: the introduction part includes a tube for passing the carrier gas, the gas, and the dilution gas at different points in time; wherein, the tube is connected to the vacuum pump; Wherein, the introduction part: after the exhaust of the vacuum pump, introduces the gas from the gas container through the tube to the dilution container; after the exhaust of the vacuum pump, passes the tube The carrier gas is introduced into the dilution container; and after the exhaust of the vacuum pump, the dilution gas is released from the dilution container through the tube. The gas supply device according to claim 1 or 2, wherein: the introduction part supplies the dilution gas from the dilution container to the chamber of the vapor growth device; when the vapor growth device forms a part of the substance on the substrate or During all the time, the outflow of the gas from the inside of the chamber to the outside is blocked.

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