Mixed gas supply device

Abstract

The present invention addresses the problem of providing a mixed gas supply device capable of safely and stably supplying a mixed gas containing a film-forming material gas. Provided is a mixed gas supply device (1) for supplying a mixed gas containing at least one type of film-forming material (S) gas by adjusting the concentration of the film-forming material (S) in the mixed gas, the mixed gas supply device (1) being provided with: a raw material container (2) for accommodating the film-forming material (S); a first heater (3) for heating the raw material container (2); a carrier gas introduction path (L1) for introducing a carrier gas into the raw material container (2); a mixed gas discharge path (L2) for discharging the mixed gas from the raw material container (2); a second heater (6) for heating the mixed gas discharge path (L2); a pressure adjustment device (8) that is located on the mixed gas discharge path (L2) and that adjusts the pressure of the raw material container (2); a mixed gas metering device (9) which is positioned on the primary side or the secondary side of the pressure adjustment device (8) on the mixed gas discharge path (L2) and measures the concentration or the flow rate of the mixed gas; and one or more buffer tanks (10) positioned on the mixed gas discharge path (L2).

Description

Technical Field

[0001] The invention relates to a mixed gas supply device. Background Art

[0002] In semiconductor manufacturing processes, metal films, metal oxide films, and metal nitride films are used in many processes. For example, metal nitride films are widely used for many purposes due to their physical, chemical, electrical, and mechanical properties. Silicon nitride films (SiN) are used for gate insulating films or sidewall spacers when forming transistors. In addition, titanium nitride films (TiN), tantalum nitride films (TaN), and tungsten nitride films (WN) are used as barrier films for integrated circuit wiring, etc.

[0003] Especially in recent years, as the miniaturization of three-dimensional transistor structures such as Fin-FET (Fin Field-Effect Transistor) in cutting-edge logic devices and the further development of high integration of 3D-NAND have led to the continuous reduction in the horizontal and vertical dimensions of integrated circuits, sub-nanometer-level film thickness control and thin film formation technology with good coverage characteristics are required.

[0004] Generally, in order to form a thin film by chemical vapor deposition (CVD) or atomic layer deposition (ALD), a film-forming material such as a metal-containing compound, a nitrogen-containing compound, an oxygen-containing compound, or a carbon-containing compound needs to be vaporized and supplied. However, since the vapor pressure of the film-forming material is often low, the film-forming material needs to be vaporized and supplied to the film-forming reactor.

[0005] As a method of supplying a film-forming material to a film-forming reactor, Patent Documents 1 and 2 disclose a technique of supplying a mixed gas of film-forming material vapor (film-forming material gas) and a carrier gas by ventilating and bubbling in a raw material container using a carrier gas. In the case of bubbling supply, by keeping the temperature of the film-forming material and the pressure in the raw material container constant and controlling the carrier gas flow rate, a mixed gas of the film-forming material gas and the carrier gas can be supplied at a stable concentration.

[0006] In addition, Patent Document 3 discloses the following technology: a pipe (immersion pipe) immersed in the liquid material filled in the container and a pressurizing gas pipe are provided, and the liquid surface in the container is pressurized by introducing pressurizing gas into the pressurizing gas pipe, and the liquid material is supplied to the consumption equipment through the immersion pipe. In addition, in the case of Patent Document 3, the liquid material is usually vaporized by a vaporizer or the like after the liquid material is supplied, so that the material can be supplied to the film forming reactor at a stable flow rate.

[0007] Patent Document 1: Japanese Patent Application No. 2005-522869

[0008] Patent Document 2: Japanese Patent Application Publication No. 2015-119045

[0009] Patent Document 3: Japanese Patent Application Publication No. 2011-025104

[0010] In the technologies disclosed in Patent Documents 1 and 2, even if the temperature of the film-forming material and the pressure in the raw material container are kept constant and the carrier gas flow rate is controlled, there is a problem that the concentration of the film-forming material gas fluctuates and cannot be uniformly concentrated (set concentration) immediately after the mixed gas supply is completed. In addition, during the mixed gas supply process, the vapor pressure of the film-forming material decreases (the temperature of the film-forming material decreases) due to the heat of vaporization in the raw material container, and there is a problem that the concentration of the film-forming material gas in the mixed gas decreases (fluctuates).

[0011] In addition, regarding the concentration change of the film-forming material gas in the mixed gas caused by the above-mentioned vapor pressure change, there is a method of controlling the pressure in the raw material container. However, if the pressure in the raw material container is changed, the mixed gas flow rate will change, and the supply amount (absolute amount) of the film-forming material gas may change.

[0012] In addition, the technology disclosed in Patent Document 3 has the advantage of being able to keep the concentration of the mixed gas constant because the flow rate of the mixed gas can be controlled by the vaporizer, but the liquid material may leak from the joint of the pipeline. In the case where the liquid material is water-resistant, highly reactive, toxic, etc., even a small amount has safety issues. Summary of the invention

[0013] The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a mixed gas supply device capable of safely and stably supplying a mixed gas including a film forming material gas.

[0014] In order to solve the above-mentioned problems, the present invention has the following structures.

[0015] [1] A mixed gas supply device for supplying a mixed gas containing at least one film-forming material by adjusting the concentration of the film-forming material in the mixed gas, the mixed gas supply device comprising:

[0016] A raw material container, used for containing the film-forming material;

[0017] A first heater, used for heating the raw material container;

[0018] A carrier gas introduction path, used to introduce carrier gas into the raw material container;

[0019] A mixed gas outlet path, used for outlet of the mixed gas from the raw material container;

[0020] A second heater, used for heating the mixed gas outlet path;

[0021] A pressure regulating device, located on the mixed gas outlet path and used to regulate the pressure of the raw material container;

[0022] A mixed gas metering device, located on the primary side or the secondary side of the pressure regulating device on the mixed gas outlet path, and used to measure the concentration or flow rate of the mixed gas; and

[0023] One or more buffer tanks are located on the mixed gas outlet path.

[0024] [2] The mixed gas supply device according to [1], wherein the buffer tank includes a first buffer tank located on a secondary side of the mixed gas metering device.

[0025] [3] The mixed gas supply device according to [1] or [2], further comprising:

[0026] A mixed gas concentration adjusting device is used to adjust the concentration of the film-forming material in the mixed gas to a set value,

[0027] The mixed gas concentration adjusting device has the following functions: calculating the difference between the measured value of the concentration of the mixed gas obtained by the mixed gas metering device and the set value set in the mixed gas concentration adjusting device, and updating the pressure setting value of the pressure adjusting device based on the difference so that the measured value becomes the set value.

[0028] [4] The mixed gas supply device according to [1] or [2], further comprising:

[0029] A mixed gas concentration adjusting device, used for adjusting the concentration of the film-forming material in the mixed gas to a set value;

[0030] a carrier gas flow control device, located on the carrier gas introduction path; and

[0031] a mixed gas concentration calculation device for calculating the concentration of the film-forming material in the mixed gas based on the set value of the flow rate of the carrier gas set in the carrier gas flow control device and the measured value of the flow rate of the mixed gas measured by the mixed gas metering device,

[0032] The mixed gas concentration adjusting device has the following functions: calculating the difference between the calculated value of the concentration of the mixed gas obtained by the mixed gas concentration calculation device and the set value set in the mixed gas concentration adjusting device, and updating the pressure setting value of the pressure adjusting device based on the difference so that the calculated value becomes the set value.

[0033] [5] The mixed gas supply device according to any one of [1] to [4], wherein the buffer tank includes a second buffer tank located between the pressure regulating device and the mixed gas metering device.

[0034] [6] The mixed gas supply device according to any one of [1] to [5], further comprising:

[0035] a first heater adjustment device, used to adjust the output of the first heater;

[0036] A mixed gas concentration adjusting device, used for adjusting the concentration of the film-forming material in the mixed gas to a set value;

[0037] a carrier gas flow control device, located on the carrier gas introduction path; and

[0038] a mixed gas concentration calculation device for calculating the concentration of the film-forming material in the mixed gas based on the set value of the flow rate of the carrier gas set in the carrier gas flow control device and the measured value of the flow rate of the mixed gas measured by the mixed gas metering device,

[0039] The mixed gas concentration adjusting device has the following functions: calculating the difference between the measured value of the concentration of the mixed gas obtained by the mixed gas metering device or the calculated value of the concentration of the mixed gas obtained by the mixed gas concentration calculation device and the set value set in the mixed gas concentration adjusting device, and updating the set value of the output of the first heater adjusting device based on the difference so that the measured value or the calculated value becomes the set value.

[0040] [7] The mixed gas supply device according to any one of [2] to [6], further comprising:

[0041] A carrier gas flow control device, located on the carrier gas introduction path;

[0042] a pressure gauge for measuring the pressure in the first buffer tank; and

[0043] A supply control device is used to control the carrier gas flow control device and one or more opening and closing valves located on the mixed gas outlet path,

[0044] The supply control device controls the carrier gas flow control device based on the measurement value of the pressure gauge, and controls the opening degree of each of the one or more opening and closing valves.

[0045] [8] The mixed gas supply device according to any one of [2] to [7], further comprising: a mixed gas flow rate control device located on the secondary side of the first buffer tank on the mixed gas outlet path.

[0046] [9] The mixed gas supply device according to [7] further comprises: a mixed gas flow rate control device located on the secondary side of the first buffer tank on the mixed gas outlet path.

[0047]

[10] The mixed gas supply device according to any one of [1] to [9], wherein the film-forming material is one or more compounds selected from metal-containing compounds, nitrogen-containing compounds, carbon-containing compounds and oxygen-containing compounds.

[0048]

[11] The mixed gas supply device according to

[10] , wherein the nitrogen-containing compound is a hydrazine compound.

[0049]

[12] The mixed gas supply device according to any one of [1] to

[11] further comprises: a bypass path that branches from the carrier gas introduction path and bypasses the raw material container to merge with the mixed gas outlet path.

[0050]

[13] The mixed gas supply device according to any one of [1] to

[12] further comprises: one or more exhaust paths that branch from the mixed gas outlet path and exhaust the mixed gas in the mixed gas outlet path.

[0051] The mixed gas supply device of the present invention can safely and stably supply a mixed gas containing a film-forming material gas. BRIEF DESCRIPTION OF THE DRAWINGS

[0052] Figure 1 It is a system diagram showing the structure of a first embodiment of the mixed gas supply device of the present invention.

[0053] Figure 2 It is a system diagram showing the structure of a second embodiment of the mixed gas supply device of the present invention.

[0054] Figure 3 It is a system diagram showing the structure of a third embodiment of the mixed gas supply device of the present invention.

[0055] Figure 4 It is a system diagram showing the structure of a fourth embodiment of the mixed gas supply device of the present invention.

[0056] Figure 5 It is a system diagram showing the structure of a fifth embodiment of the mixed gas supply device of the present invention.

[0057] Figure 6 It is a system diagram showing the structure of a sixth embodiment of the mixed gas supply device of the present invention.

[0058] Figure 7 It is a figure which shows the result of Example 1 of this invention.

[0059] Figure 8 It is a graph showing the results of Comparative Example 1 of the present invention.

[0060] Fig. 9 It is a figure which shows the result of Example 2 of this invention.

[0061] Fig.10 It is a figure which shows the result of Example 2 of this invention.

[0062] Fig.11 It is a figure which shows the result of Example 3 of this invention.

[0063] Fig.12 It is a figure which shows the result of Example 4 of this invention.

[0064] Fig.13 It is a graph showing the results of Comparative Example 2 of the present invention. DETAILED DESCRIPTION

[0065] Hereinafter, a mixed gas supply device as an embodiment of the present invention will be described with reference to the accompanying drawings. In the drawings used in the following description, in order to facilitate understanding of the features, the features are sometimes enlarged for convenience, and the size ratios of the various structural elements are not necessarily the same as the actual ones.

[0066] Furthermore, "to" indicating a numerical range means that the numerical values ​​described before and after it are included as the lower limit and the upper limit.

[0067] <First Embodiment>

[0068] First, a first embodiment of the mixed gas supply device according to the present invention will be described in detail with reference to the drawings. Figure 1 It is a system diagram showing the structure of the mixed gas supply device according to the first embodiment.

[0069] like Figure 1As shown, the mixed gas supply device 1 of the present embodiment includes a raw material container 2 (2A, 2B), a container heater (first heater) 3 (3A, 3B), a pipe heater (second heater) 6, a pressure regulating device 8, a mixed gas metering device 9, a first buffer tank (buffer tank) 10, a first pressure gauge 11, a second pressure gauge (pressure gauge) 12, a detector 13, a carrier gas inlet path L1 (L1A, L1B), a mixed gas outlet path L2 (L2A, L2B) and a bypass path L3 (L3A, L3B).

[0070] Furthermore, the mixed gas supply device 1 of the present embodiment may further include a container heater temperature adjustment device (first heater adjustment device) 4 , a carrier gas flow rate adjustment device 5 , and a pipe heater temperature adjustment device (second heater adjustment device) 7 .

[0071] The mixed gas supply device 1 of the present embodiment is a device for supplying a mixed gas containing at least one film forming material gas to, for example, a subsequent film forming device 100 by adjusting the concentration of the film forming material in the mixed gas.

[0072] The film forming apparatus 100 is not particularly limited as long as it can be applied to the chemical vapor deposition method. Examples of the film forming apparatus 100 include a chemical vapor deposition (CVD) apparatus and an atomic layer deposition (ALD) apparatus.

[0073] The raw material container 2 (2A, 2B) is a container (supply source) that contains the film-forming material S inside.

[0074] There may be one raw material container 2 or two or more. Hereinafter, in the mixed gas supply device 1 of the present embodiment, a case where two raw material containers 2A and 2B are used will be described as an example.

[0075] In addition, in the mixed gas supply device 1 of the present embodiment, two raw material containers 2A and 2B can be used one by one, or two raw material containers 2A and 2B can be used at the same time. Here, when the two raw material containers 2A and 2B are used one by one, the film-forming material S can be continuously supplied by switching to the other container after one container becomes empty. In addition, when the two raw material containers 2A and 2B are used at the same time, the contact area between the carrier gas and the film-forming material increases, so that the concentration of the film-forming material gas in the mixed gas can be increased. In addition, regarding the use form of the raw material container 2, an appropriate method can be appropriately selected according to the film-forming process in the film-forming device 100.

[0076] The film-forming material S is a liquid or solid material at room temperature and pressure and is used in thin film forming processes such as CVD or ALD. The film-forming material S is one or more compounds selected from metal-containing compounds, nitrogen-containing compounds, carbon-containing compounds and oxygen-containing compounds.

[0077] (Containing metal compounds)

[0078] The metal-containing compound is not particularly limited, and examples include compounds containing one or more metal elements selected from silicon (Si), titanium (Ti), tantalum (Ta), aluminum (Al), gallium (Ga), vanadium (V), iron (Fe), zirconium (Zr), niobium (Nb), tungsten (W), molybdenum (Mo), indium (In), hafnium (Hf), cobalt (Co) and ruthenium (Ru).

[0079] Among the metal-containing compounds, if it is a halogenated metal compound, it is preferably a compound selected from TiCl4, Si2Cl6 (HCDS: hexachlorodisilane), SiCl4, SiHCl3, SiH2Cl2, SiH3Cl, SiI4, SiHI3, SiH2I2, SiH3I, TaCl5, AlCl3, GaCl3, ZrCl4, HfCl4, MoO2Cl2, MoCl5, WF6, WCl6 and WCl5.

[0080] In addition, among the metal-containing compounds, if it is an organic metal compound, it is preferably a compound selected from TDMAT (tetrakisdimethylaminotitanium), 3DMAS (tridimethylaminosilane), BDEAS (bisdiethylaminosilane), BTBAS (bis-tert-butylaminosilane), DIPAS (diisopropylaminosilane), PDMAT (pentadimethylaminotantalum), TMA (trimethylaluminum), TMG (trimethylgallium), hafnium-containing compounds, zirconium-containing compounds, cobalt-containing compounds and ruthenium-containing compounds.

[0081] (Nitrogen-containing compounds)

[0082] The nitrogen-containing compound is not particularly limited, and examples thereof include amine compounds, hydrazine compounds, and ammonia.

[0083] The amine compound is preferably a compound selected from methylamine, dimethylamine, ethylamine, diethylamine and tert-butylamine.

[0084] The hydrazine compound is not particularly limited, and examples thereof include hydrazine (N2H4), monomethylhydrazine, dimethylhydrazine, tert-butylhydrazine, phenylhydrazine, propylhydrazine, etc. As the hydrazine compound, any one of them may be selected and used, or two or more thereof may be mixed and used.

[0085] Generally, it is known that hydrazine compounds react violently in order to be used as spacecraft propellants or rocket engine fuels. In addition, hydrazine and monomethylhydrazine are highly toxic, and their allowable concentration (TLV-TWA) is 0.01ppm, which is much lower than the allowable concentrations of ammonia (allowable concentration: 25ppm), phosphine (allowable concentration: 0.3ppm) and monosilane (allowable concentration: 5ppm) used in semiconductor manufacturing processes. In the NFPA (National Fire Protection Association), which is a standard for indicating the danger of chemicals, hydrazine is 4-4-4 (Health-Flammability-Instability) and monomethylhydrazine is 4-3-2, which also shows the above properties of hydrazine compounds, so it is required to give full consideration to safety when handling. Therefore, the raw material container 2 is preferably a sealed container.

[0086] (Carbon compounds)

[0087] The carbon-containing compound is not particularly limited, and an organic solvent may be mentioned. As the organic solvent, one or more compounds selected from hydrocarbon compounds, alcohol compounds, ether compounds, diol compounds, and ketone compounds may be used.

[0088] (oxygenated compounds)

[0089] The oxygen-containing compound is not particularly limited, and examples thereof include water (H2O) and hydrogen peroxide (H2O2).

[0090] Furthermore, the film-forming material S may be a material obtained by mixing two or more liquids, or may be a material obtained by dissolving a solid in a liquid.

[0091] In addition, the gas of the film-forming material refers to the gas in a vaporized state of the film-forming material.

[0092] The container heaters 3 (3A, 3B) are located around the raw material containers 2 (2A, 2B) and are used to heat the raw material containers 2 (2A, 2B) respectively so that the film forming material S in the raw material containers 2 (2A, 2B) is within a specified temperature range.

[0093] The container heater 3 (3A, 3B) is not particularly limited as long as it can heat the raw material container 2 (2A, 2B). Examples of the container heater 3 (3A, 3B) include a breeze heater, a mantle heater, a water bath, an oil bath, and the like. Among them, when heating the film-forming material S in the container, it is preferable to use a water bath or an oil bath from the viewpoint of heat uniformity and safety.

[0094] The container heater temperature adjustment device 4 is not particularly limited as long as it can adjust (control) the output of the container heater 3 (3A, 3B). In addition, the container heater temperature adjustment device 4 only needs to have a function of adjusting (controlling) the output of the container heater 3 (3A, 3B), and may be integrated with the container heater 3 (3A, 3B).

[0095] From the perspective of safety and stable supply of the film-forming material S, the temperature at which the raw material container 2 (2A, 2B) is heated by the container heater 3 (3A, 3B) and the container heater temperature adjustment device 4 is preferably set to a temperature that does not cause decomposition of the film-forming material S. Specifically, the temperature is preferably set in the range of room temperature (20°C) to 200°C, and more preferably in the range of 30°C to 60°C.

[0096] The carrier gas introduction path L1 is a flow path for introducing a carrier gas into the raw material container 2. The base end of the carrier gas introduction path L1 is connected to a carrier gas supply source not shown. The front end of the carrier gas introduction path L1 in the gas flow direction is connected to the raw material container 2. In the present embodiment, the front end of the carrier gas introduction path L1 branches into a path L1A and a path L1B, the path L1A is connected to the raw material container 2A, and the path L1B is connected to the raw material container 2B. Thus, according to the mixed gas supply device 1 of the present embodiment, the carrier gas can be introduced into the raw material containers 2A and 2B respectively via the carrier gas introduction path L1.

[0097] The carrier gas is not particularly limited and can be appropriately selected according to the type of film-forming material S. As the carrier gas, rare gases such as helium (He), nitrogen (N2), argon (Ar), hydrogen (H2) and ammonia (NH3) can be listed. As the carrier gas, one of them can be selected for use, or two or more can be mixed for use.

[0098] The carrier gas flow control device 5 is located on the carrier gas introduction path L1. The carrier gas flow control device 5 controls the flow rate of the carrier gas supplied to the carrier gas introduction path L1. The carrier gas flow control device 5 is not particularly limited as long as it can control the flow rate. As examples of the carrier gas flow control device 5, a mass flow controller (MFC) or a pressure regulator with a controllable opening can be cited.

[0099] The flow rate of the carrier gas supplied to the carrier gas introduction path L1 is not particularly limited and can be appropriately selected. The carrier gas flow rate control range of the carrier gas flow rate control device 5 is preferably 10 to 10000 sccm.

[0100] The mixed gas outlet path L2 is a flow channel for outlet of a mixed gas from the raw material container 2, the mixed gas containing at least one gas of a film-forming material S. The base end of the mixed gas outlet path L2 is connected to the raw material container 2. In the present embodiment, the base end of the mixed gas outlet path L2 branches into a path L2A and a path L2B, the path L2A is connected to the raw material container 2A, and the path L2B is connected to the raw material container 2B. In addition, the front end of the mixed gas outlet path L2 is connected to the above-mentioned film-forming device 100. Therefore, according to the mixed gas supply device 1 of the present embodiment, after the mixed gas is respectively outlet from the raw material containers 2A and 2B to the mixed gas outlet path L2, the mixed gas can be supplied to the subsequent film-forming device 100.

[0101] In the mixed gas supply device 1 of the present embodiment, since the carrier gas inlet path L1 and the mixed gas outlet path L2 are connected to the raw material container 2, the carrier gas can be introduced into the raw material container 2 (2A, 2B) from the carrier gas inlet path L1, and the gas (gas) of the film forming material S accompanied by the carrier gas can be exported as a mixed gas to the mixed gas outlet path L2.

[0102] When the carrier gas is introduced into the raw material container 2 , the carrier gas may be supplied by bubbling, or the carrier gas may be supplied into the gas phase (that is, the vapor of the film-forming material S) in the container.

[0103] The mixed gas contains at least one gas of the film-forming material S as a main component. The mixed gas may contain a carrier gas. Among them, the main components of the mixed gas are preferably a nitrogen-containing compound and a carrier gas or a metal-containing compound and a carrier gas from the viewpoint of low vapor pressure and difficulty in concentration control.

[0104] The pipe heater (second heater) 6 is configured to cover the surface of the pipe constituting the paths L1A, L1B and the mixed gas outlet path L2 (L2A, L2B) branching off after the carrier gas flow control device 5 on the carrier gas inlet path L1, and heat the carrier gas inlet path L1 and the mixed gas outlet path L2.

[0105] The duct heater temperature adjustment device (second heater adjustment device) 7 is not particularly limited as long as it can adjust (control) the output of the duct heater 6. In addition, the duct heater temperature adjustment device 7 only needs to have a function of adjusting (controlling) the output of the duct heater 6, and may be integrated with the duct heater 6.

[0106] The temperature of the pipe constituting the flow path of the carrier gas and the mixed gas needs to be set to a temperature that does not cause the gas of the film-forming material S to reliquefy and resolidify, and is therefore preferably higher than the temperature of the raw material container 2. As a result, the film-forming material S can be prevented from reliquefying in the mixed gas outlet path L2, and the mixed gas containing the gas of the film-forming material S can be safely and stably circulated in the mixed gas outlet path L2.

[0107] The bypass path L3 is a flow path branched from the carrier gas introduction path L1 and bypassing the raw material container 2 without passing through the raw material container 2 to merge with the mixed gas outlet path L2. In the mixed gas supply device 1 of the present embodiment, the bypass path L3A branches from the carrier gas introduction path L1A and bypasses the raw material container 2A without passing through the raw material container 2A to merge with the mixed gas outlet path L2A. Similarly, the bypass path L3B branches from the carrier gas introduction path L1B and bypasses the raw material container 2B without passing through the raw material container 2B to merge with the mixed gas outlet path L2B.

[0108] By selecting the bypass path L3 (L3A, L3B) as the flow path, the carrier gas flowing in the carrier gas introduction path L1 can be supplied to the mixed gas outlet path L2 on the secondary side of the raw material container 2 without being introduced into the raw material container 2. In addition, when removing the gas (residual gas) containing the film-forming material S remaining in the mixed gas outlet path L2, the carrier gas can be supplied through the bypass path L3 (L3A, L3B), thereby effectively purging and removing the residual gas.

[0109] In the mixed gas supply device 1 of the present embodiment, preferably, one or more on-off valves are provided on each path, and any flow path can be formed according to the purpose by appropriately selecting the open and closed state of the on-off valves.

[0110] The first pressure gauge 11 is located on the mixed gas outlet path L2 and is used to measure the pressure in the raw material container 2 (2A, 2B). By detecting the pressure in the raw material container 2, the remaining amount of the film forming material S can be determined and abnormalities in the container can be discovered.

[0111] The pressure regulating device 8 is located on the mixed gas outlet path L2 and is used to regulate the pressure of the raw material container 2 (2A, 2B). The pressure regulating device 8 is not particularly limited as long as it can regulate the pressure in the raw material container 2 based on the pressure in the raw material container 2. Examples of the pressure regulating device 8 include a back pressure valve (BPR), an automatic pressure regulator, a piezoelectric valve, and a pressure control system.

[0112] In addition, the pressure regulating device 8 may be a device in which a pressure gauge and a pressure regulating valve are integrated, or may be a device in which a pressure gauge and a pressure regulating valve are separate.

[0113] When the pressure regulating device 8 is a device in which a pressure gauge and a pressure regulating valve are separated, for example, a first pressure gauge 11 for measuring the pressure in the raw material container 2 and a pressure regulating valve (an on-off valve with adjustable opening, a butterfly valve, etc.) are used and linked together to regulate the pressure in the raw material container 2.

[0114] The mixed gas metering device 9 is a device located on the secondary side of the pressure regulating device 8 on the mixed gas outlet path L2 and used to measure the concentration or flow rate of the mixed gas flowing in the mixed gas outlet path L2. The mixed gas metering device 9 is not particularly limited, and is preferably selected from a gas concentration meter capable of measuring the concentration of the film-forming material S in the mixed gas and a flow meter capable of measuring the flow rate of the mixed gas.

[0115] As a gas concentration meter which can be used as the mixed gas measuring device 9, for example, FT-IR, ND-IR, an ultrasonic gas concentration meter, a gas concentration sensor, and a laser gas concentration meter can be cited.

[0116] As flow meters that can be used as the mixed gas metering device 9, for example, a mass flow meter (MFM) and a flow sensor can be cited. When a flow meter is used as the mixed gas metering device 9, the flow rate and the mixing ratio (mixed gas concentration) of the gas of the film forming material S in the mixed gas can be calculated based on the flow value of the carrier gas controlled by the carrier gas flow control device 5 and the measured value of the flow meter.

[0117] The first buffer tank 10 is a container that is located on the secondary side of the mixed gas measuring device 9 in the mixed gas outlet path L2 and temporarily stores the mixed gas flowing in the mixed gas outlet path L2.

[0118] Since the first buffer tank 10 is located on the secondary side of the mixed gas measuring device 9 in the mixed gas outlet path L2, the effect of making the mixed gas concentration uniform is produced.

[0119] The first buffer tank 10 is not particularly limited as long as it is a sealed container capable of storing the mixed gas. In addition, the capacity of the first buffer tank 10 is not particularly limited, and a capacity of 1 to 100 L can be applied, and a capacity of 10 to 50 L is preferred.

[0120] Since the mixed gas supply device 1 of this embodiment is a structure in which the first buffer tank 10 is located on the mixed gas outlet path L2 through a branch path, when performing maintenance such as replacement or cleaning of the first buffer tank 10, operations can be performed without mixing atmospheric components into the mixed gas outlet path L2.

[0121] In addition, in the mixed gas supply device 1 of the present embodiment, the structure in which the first buffer tank 10 is located on the mixed gas outlet path L2 through the branch path is described as an example, but the present invention is not limited to this. For example, the first buffer tank 10 may be provided on the mixed gas outlet path L2 without the branch path.

[0122] The second pressure gauge 12 (pressure gauge) is used to measure the pressure in the first buffer tank 10. The second pressure gauge 12 is preferably provided near the first buffer tank 10. Thus, the pressure abnormality in the first buffer tank 10 can be detected immediately, and a safety device (not shown) can be activated.

[0123] The detector 13 constitutes a part of the safety mechanism in the mixed gas supply device 1 of this embodiment. As the detector 13, a gas leak detector, a liquid leak detector, etc. can be listed. By linking the detector 13 with a safety device not shown in the figure, a structure can be set to automatically cut off the supply of each gas in an emergency such as a leak or a liquid leak.

[0124] In the mixed gas supply device 1 of the present embodiment, signals can be sent and received between the pressure regulating device 8 and the mixed gas metering device 9 by wired or wireless means. Therefore, in the mixed gas supply device 1 of the present embodiment, while the mixed ratio of the carrier gas and the gas of the film-forming material S in the mixed gas is monitored by the mixed gas metering device 9, the pressure in the raw material container 2 (2A, 2B) is manually or automatically controlled by the pressure regulating device 8, thereby adjusting the concentration of the gas of the film-forming material S in the mixed gas to a desired value.

[0125] Specifically, when the concentration value actually measured by the mixed gas metering device 9 is less than the concentration (set value) set in the pressure regulating device 8, or when the concentration value actually measured decreases with the supply of the mixed gas, a control signal for updating the pressure set value is sent from the mixed gas metering device 9 to the pressure regulating device 8. As a result, the opening of the pressure regulating device 8 can be instantly adjusted in the opening direction, and the mixed gas of the set concentration can be supplied with good responsiveness.

[0126] When the pressure in the raw material container 2 is manually controlled, the set value of the pressure in the raw material container 2 is updated by manually operating the pressure regulating device 8 so that the concentration actually measured by the mixed gas measuring device 9 becomes the set concentration.

[0127] Unlike manual control, automatic control is preferred because it is possible to adjust the pressure in the raw material container 2 instantly.

[0128] Therefore, according to the mixed gas supply device 1 of this embodiment, a mixed gas containing at least one film forming material S can be supplied as a part of the raw material gas to, for example, the subsequent film forming device 100 by adjusting the concentration of the film forming material S in the mixed gas.

[0129] In addition, according to the mixed gas supply device 1 of the present embodiment, since the first buffer tank 10 is provided on the mixed gas outlet path L2, the mixed gas flowing in the mixed gas outlet path L2 can be temporarily stored in the first buffer tank 10 and then supplied to the secondary side. In this way, since the mixed gas is supplied through the first buffer tank 10, the pressure fluctuation generated during the supply process can be suppressed, and the concentration and flow rate of the mixed gas can be stabilized.

[0130] <Second Embodiment>

[0131] Figure 2 It is a system diagram showing the structure of a second embodiment of the mixed gas supply device of the present invention.

[0132] like Figure 2 As shown, the difference between the mixed gas supply device 21 of the second embodiment and the mixed gas supply device 1 is that the structure of the mixed gas supply device 1 is provided with a second buffer tank 14, a mixed gas flow control device 15, a vacuum pump 16 and exhaust paths L4A, L4B, and the other structures are the same. Therefore, in the mixed gas supply device 21 of this embodiment, the same reference numerals are used for the same structures as the mixed gas supply device 1, and their descriptions are omitted.

[0133] The second buffer tank 14 is a container that is located between the pressure regulating device 8 and the mixed gas measuring device 9 on the mixed gas outlet path L2 and temporarily stores the mixed gas flowing in the mixed gas outlet path L2 .

[0134] By locating the second buffer tank 14 between the pressure regulating device 8 and the mixed gas measuring device 9 on the mixed gas outlet path L2 , it is possible to suppress pressure fluctuations and flow rate fluctuations in the mixed gas measuring device 9 .

[0135] The second buffer tank 14 is not particularly limited as long as it is a sealed container capable of storing the mixed gas. The capacity of the second buffer tank 14 is not particularly limited, and a capacity of 1 to 100 L is applicable, and a capacity of 1 to 20 L is preferably applicable.

[0136] Since the mixed gas supply device 21 of this embodiment is a structure in which the second buffer tank 14 is located on the mixed gas outlet path L2 through a branch path, when performing maintenance such as replacement or cleaning of the second buffer tank 14, operations can be performed without mixing atmospheric components into the mixed gas outlet path L2.

[0137] In addition, in the mixed gas supply device 21 of the present embodiment, the second buffer tank 14 is described as an example in which the second buffer tank 14 is located on the mixed gas outlet path L2 via a branch path, but the present invention is not limited thereto. For example, the second buffer tank 14 may be provided on the mixed gas outlet path L2 without a branch path.

[0138] The mixed gas flow rate control device 15 is located on the secondary side of the first buffer tank 10 in the mixed gas outlet path L2 and controls the flow rate of the mixed gas adjusted to a set concentration.

[0139] According to the mixed gas supply device 21 of this embodiment, since a mixed gas flow control device 15 is provided on the mixed gas outlet path L2, even if pressure changes occur on the upstream side of the mixed gas flow control device 15 for concentration control or pressure changes occur in the reactor of the film forming device 100 on the downstream side of the mixed gas flow control device 15, the mixed gas can be supplied at a flow rate that is stable relative to the set value.

[0140] Furthermore, according to the mixed gas supply device 21 of this embodiment, since the first buffer tank 10 is located upstream (primary side) of the mixed gas flow control device 15, it is possible to effectively suppress rapid pressure fluctuations that occur when the pressure in the raw material container 2 is controlled by the pressure regulating device 8.

[0141] The exhaust paths L4A and L4B are flow paths branching from the mixed gas outlet path L2 and exhausting the mixed gas in the mixed gas outlet path L2. In addition, by providing vacuum pumps 16 on the exhaust paths L4A and L4B, the mixed gas in the mixed gas outlet path L2 can be vacuum-exhausted.

[0142] According to the mixed gas supply device 21 of this embodiment, since the primary side of the pressure regulating device 8 on the mixed gas outlet path L2 is provided with an exhaust path L4A, the mixed gas containing the film-forming material S remaining in the mixed gas outlet path L2 can be effectively purged and removed by repeating the process of pressurizing with a carrier gas and the process of vacuum exhaust before replacing the raw material container 2.

[0143] Furthermore, according to the mixed gas supply device 21 of the present embodiment, since the exhaust path L4B is provided on the secondary side of the mixed gas measuring device 9 in the mixed gas outlet path L2, the mixed gas remaining on the secondary side of the mixed gas measuring device 9 can be purged and removed efficiently.

[0144] As a purging method, a method of continuously flowing a carrier gas may be applied instead of repeating the above-mentioned cyclic purging method.

[0145] The vacuum pump 16 is not particularly limited, and examples thereof include a dry vacuum pump, a diaphragm pump, a turbomolecular pump, a scroll pump, a rotary oil pump, and a vacuum generator.

[0146] According to the mixed gas supply device 21 of this embodiment, like the above-mentioned mixed gas supply device 1, while monitoring the mixing ratio of the carrier gas and the gas of the film-forming material S in the mixed gas through the mixed gas metering device 9, the pressure in the raw material container 2 (2A, 2B) is controlled by the pressure regulating device 8, so that the mixed gas adjusted to a specified gas concentration can be stably supplied to the subsequent film-forming device 100 as a part of the raw material gas.

[0147] In addition, according to the mixed gas supply device 21 of this embodiment, since the first buffer tank 10 and the second buffer tank 14 are provided on the mixed gas outlet path L2, and the mixed gas is supplied through the first buffer tank 10 and the second buffer tank 14, the pressure fluctuation occurring during the supply process can be suppressed, and the concentration and flow rate of the mixed gas can be stabilized.

[0148] In addition, according to the mixed gas supply device 21 of this embodiment, since one or more exhaust paths L4A and L4B are provided on the mixed gas outlet path L2, the mixed gas remaining in the mixed gas outlet path L2 can be purged before replacing the raw material container 2 or before opening the pipeline during maintenance. Thus, the raw material container 2 can be replaced and maintained safely.

[0149] In addition, according to the mixed gas supply device 21 of the present embodiment, since the mixed gas flow rate control device 15 is provided on the mixed gas outlet path L2, the mixed gas can be supplied at a flow rate that is stable relative to the set value even if pressure fluctuations occur on the upstream side of the mixed gas flow rate control device 15 for concentration control or pressure fluctuations occur in the reactor of the film forming device 100 on the downstream side of the mixed gas flow rate control device 15. Thus, the mixed gas can be supplied at a stable flow rate to the film forming device 100 located on the secondary side of the mixed gas supply device 21.

[0150] <Third Embodiment>

[0151] Figure 3 It is a system diagram showing the structure of a third embodiment of the mixed gas supply device of the present invention.

[0152] like Figure 3As shown, the difference between the mixed gas supply device 31 of the third embodiment and the mixed gas supply device 21 is that in the structure of the mixed gas supply device 21, the mixed gas metering device 9 is a mixed gas concentration analysis device 9A, and a mixed gas concentration adjustment device 17 is provided instead of the second buffer tank 14, and the other structures are the same. Therefore, in the mixed gas supply device 31 of this embodiment, the same reference numerals are used for the same structures as the mixed gas supply device 21, and their descriptions are omitted.

[0153] The mixed gas concentration adjusting device 17 is a control device that adjusts the concentration of the film forming material S in the mixed gas to a set value.

[0154] The mixed gas concentration adjusting device 17 can send and receive signals with the pressure adjusting device 8 and the mixed gas concentration analyzing device 9A by wire or wireless means. Specifically, the mixed gas concentration adjusting device 17 receives the measured value of the concentration from the mixed gas concentration analyzing device 9A and sends a control signal to the pressure adjusting device 8.

[0155] In addition, the mixed gas concentration adjusting device 17 can set the concentration of the film forming material S in the mixed gas to a set value. The set value can be directly input to the mixed gas concentration adjusting device 17 by an operator, or a signal can be sent by wire or wirelessly.

[0156] In addition, the mixed gas concentration adjusting device 17 has the following function: that is, calculating the difference between the measured value of the mixed gas concentration obtained by the mixed gas concentration analysis device 9A and the set value set in the mixed gas concentration adjusting device 17, and updating the pressure setting value of the pressure regulating device 8 based on the obtained difference, so that the measured value (actual measured value) becomes the set value.

[0157] Specifically, when the measured value of the concentration actually measured by the mixed gas concentration analysis device 9A is less than the concentration (set value) set in the mixed gas concentration adjustment device 17, or when the measured value of the concentration actually measured decreases as the mixed gas is supplied, a control signal for updating the pressure set value is sent from the mixed gas concentration adjustment device 17 to the pressure adjustment device 8. As a result, the opening of the pressure adjustment device 8 can be instantly adjusted in the opening direction, and the mixed gas of the set concentration can be supplied with good responsiveness.

[0158] When the measured value of the concentration actually measured increases, a control signal for updating the pressure setting value is also sent from the mixed gas concentration adjusting device 17 to the pressure adjusting device 8. Thus, the opening of the pressure adjusting device 8 can be instantly adjusted in the closing direction, and the mixed gas of the set concentration can be supplied with good responsiveness.

[0159] According to the mixed gas supply device 31 of the present embodiment, it is possible to obtain the same effects as those of the mixed gas supply devices 1 and 21 described above.

[0160] In addition, according to the mixed gas supply device 31 of the present embodiment, since it is provided with a mixed gas concentration regulating device 17 capable of sending and receiving signals between the pressure regulating device 8 and the mixed gas concentration analysis device 9A, even if the concentration changes at the initial stage of the mixed gas supply or the vapor pressure changes due to the decrease in the material temperature during the continuous supply process, the mixed gas of the concentration (set value) set in the mixed gas concentration regulating device 17 can be stably supplied.

[0161] <Fourth Embodiment>

[0162] Figure 4 It is a system diagram showing the structure of a fourth embodiment of the mixed gas supply device according to the present invention.

[0163] like Figure 4 As shown, the difference between the mixed gas supply device 41 of the fourth embodiment and the mixed gas supply device 21 is that in the structure of the mixed gas supply device 21, the mixed gas metering device 9 is a mixed gas flow meter 9B, and is provided with a mixed gas concentration adjustment device 17 and a mixed gas concentration calculation device 18, and the other structures are the same. Therefore, in the mixed gas supply device 41 of this embodiment, the same reference numerals are used for the same structures as the mixed gas supply device 21, and their descriptions are omitted.

[0164] The mixed gas concentration calculation device 18 is a calculation device for calculating the concentration of the film forming material S in the mixed gas. The mixed gas concentration calculation device 18 can send and receive signals with the carrier gas flow control device 5, the mixed gas flow meter 9B and the mixed gas concentration adjustment device 17 in a wired or wireless manner.

[0165] Specifically, the mixed gas concentration calculation device 18 receives the set value of the carrier gas flow rate set in the carrier gas flow control device 5 and the flow rate measurement value (actual measurement value) of the mixed gas measured by the mixed gas flow meter 9B, and calculates and calculates the concentration of the film-forming material S in the mixed gas based on them. And, the mixed gas concentration calculation device 18 sends the concentration (calculated value) obtained by the above calculation to the mixed gas concentration adjustment device 17.

[0166] The mixed gas concentration adjusting device 17 is a control device that adjusts the concentration of the film forming material S in the mixed gas to a set value.

[0167] The mixed gas concentration adjusting device 17 can send and receive signals with the pressure adjusting device 8 and the mixed gas concentration calculating device 18 in a wired or wireless manner. Specifically, the mixed gas concentration adjusting device 17 receives the calculated value of the concentration from the mixed gas concentration calculating device 18 and sends a control signal to the pressure adjusting device 8.

[0168] In addition, the mixed gas concentration adjusting device 17 can set the concentration of the film forming material S in the mixed gas to a set value. The set value can be directly input to the mixed gas concentration adjusting device 17 by an operator, or a signal can be sent by wire or wirelessly.

[0169] In addition, the mixed gas concentration adjusting device 17 has the following function: that is, calculating the difference between the concentration calculated value of the mixed gas obtained by the mixed gas concentration calculation device 18 and the set value set in the mixed gas concentration adjusting device 17, and updating the pressure setting value of the pressure adjusting device 8 based on the obtained difference so that the calculated value becomes the set value.

[0170] Specifically, when the measured value of the concentration calculated by the mixed gas concentration calculation device 18 is insufficient relative to the concentration (set value) set in the mixed gas concentration adjustment device 17, or when the measured value of the calculated concentration decreases with the supply of the mixed gas, a control signal for updating the pressure set value is sent from the mixed gas concentration adjustment device 17 to the pressure adjustment device 8. As a result, the opening of the pressure adjustment device 8 can be instantly adjusted in the opening direction, and the mixed gas of the set concentration can be supplied with good responsiveness.

[0171] When the calculated concentration value increases, a control signal for updating the pressure setting value is also sent from the mixed gas concentration adjusting device 18 to the pressure adjusting device 8. Thus, the opening of the pressure adjusting device 8 can be instantly adjusted in the closing direction, and the mixed gas of the set concentration can be supplied with good responsiveness.

[0172] According to the mixed gas supply device 41 of the present embodiment, it is possible to obtain the same effects as those of the mixed gas supply devices 1 and 21 described above.

[0173] In addition, according to the mixed gas supply device 41 of the present embodiment, since it is provided with a mixed gas concentration regulating device 17 capable of sending and receiving signals between the pressure regulating device 8 and the mixed gas concentration calculation device 18, even if the concentration changes at the initial stage of the mixed gas supply or the vapor pressure changes due to a drop in the material temperature during continuous supply, a mixed gas of the concentration (set value) set in the mixed gas concentration regulating device 17 can be stably supplied.

[0174] In addition, according to the mixed gas supply device 41 of this embodiment, since a second buffer tank 14 is provided between the pressure regulating device 8 and the mixed gas flow meter 9B, it is possible to suppress flow rate fluctuations or pressure fluctuations that occur when the pressure in the raw material container 2 is controlled by the pressure regulating device 8, and stably supply a mixed gas of the required concentration.

[0175] <Fifth Embodiment>

[0176] Figure 5 It is a system diagram showing the structure of a fifth embodiment of the mixed gas supply device according to the present invention.

[0177] like Figure 5 As shown, the difference between the mixed gas supply device 51 of the fifth embodiment and the mixed gas supply device 41 is that, in the structure of the mixed gas supply device 41, the mixed gas concentration adjustment device 17 sends a control signal to the container heater temperature adjustment device 4 instead of the pressure adjustment device 8, and the other structures are the same. Therefore, in the mixed gas supply device 51 of this embodiment, the same reference numerals are used for the same structures as the mixed gas supply device 41, and their descriptions are omitted.

[0178] The mixed gas concentration adjusting device 17 is a control device that adjusts the concentration of the film forming material S in the mixed gas to a set value.

[0179] The mixed gas concentration adjusting device 17 can send and receive signals with the container heater temperature adjusting device 4 and the mixed gas concentration calculating device 18 in a wired or wireless manner. Specifically, the mixed gas concentration adjusting device 17 receives the calculated value of the concentration from the mixed gas concentration calculating device 18 and sends a control signal to the container heater temperature adjusting device 4.

[0180] In addition, the mixed gas concentration adjusting device 17 can set the concentration of the film forming material S in the mixed gas to a set value. The set value can be directly input to the mixed gas concentration adjusting device 17 by an operator, or a signal can be sent by wire or wirelessly.

[0181] In addition, the mixed gas concentration adjusting device 17 has the following function: that is, calculating the difference between the calculated value of the mixed gas concentration obtained by the mixed gas concentration calculation device 18 and the set value set in the mixed gas concentration adjusting device 17, and updating the set value of the output of the container heater temperature adjusting device 4 based on the obtained difference so that the calculated value becomes the set value.

[0182] Specifically, when the calculated value of the mixed gas concentration obtained by the mixed gas concentration calculation device 18 is insufficient relative to the concentration (set value) set in the mixed gas concentration adjustment device 17, or when the calculated value of the mixed gas concentration decreases with the supply of the mixed gas, a control signal for updating the set value of the output is sent from the mixed gas concentration adjustment device 17 to the container heater temperature adjustment device 4. Here, the higher the temperature of the raw material container 2, the higher the vapor pressure of the film forming material S, so that the gas concentration of the film forming material S in the mixed gas can be increased. Therefore, by controlling the output of the container heater 3 (3A, 3B) to increase its output, it is possible to adjust in the direction of heating the raw material container 2 (2A, 2B), and supply the mixed gas of the set concentration with good responsiveness.

[0183] According to the mixed gas supply device 51 of this embodiment, since it includes the mixed gas concentration adjustment device 17 capable of transmitting and receiving signals between the container heater temperature adjustment device 4 and the mixed gas concentration calculation device 18, the same effects as those of the mixed gas supply device 41 can be obtained.

[0184] (Variation of the Fifth Embodiment)

[0185] The modification of the fifth embodiment is different from the mixed gas supply device 51 in that, in the structure of the mixed gas supply device 51, the mixed gas metering device 9B is replaced by the mixed gas concentration analysis device 9A, and the mixed gas concentration calculation device 18 is omitted, and the other structures are the same.

[0186] The mixed gas concentration adjusting device 17 can send and receive signals with the container heater temperature adjusting device 4 and the mixed gas concentration analyzing device 9A by wired or wireless means. Specifically, the mixed gas concentration adjusting device 17 receives the measured value of the concentration from the mixed gas concentration analyzing device 9A and sends a control signal to the container heater temperature adjusting device 4.

[0187] In addition, the mixed gas concentration adjusting device 17 has the following function: that is, calculating the difference between the measured value of the mixed gas concentration obtained by the mixed gas concentration analysis device 9A and the set value set in the mixed gas concentration adjusting device 17, and updating the set value of the output of the container heater temperature adjusting device 4 based on the obtained difference, so that the measured value (actual measured value) becomes the set value.

[0188] Specifically, when the measured value of the mixed gas concentration obtained by the mixed gas concentration analysis device 9A is insufficient for the concentration (set value) set in the mixed gas concentration adjustment device 17, or when the measured value of the mixed gas concentration decreases as the mixed gas is supplied, a control signal for updating the output set value is sent from the mixed gas concentration adjustment device 17 to the container heater temperature adjustment device 4.

[0189] Here, the higher the temperature of the raw material container 2, the higher the vapor pressure of the film-forming material S, thereby increasing the gas concentration of the film-forming material S in the mixed gas. Therefore, by controlling the output of the container heater 3 (3A, 3B) to increase its output, it is possible to adjust in the direction of heating the raw material container 2 (2A, 2B), and supply a mixed gas of a set concentration with good responsiveness.

[0190] According to the modified example of the mixed gas supply device 51 of this embodiment, since it is provided with the mixed gas concentration adjustment device 17 capable of transmitting and receiving signals between the container heater temperature adjustment device 4 and the mixed gas concentration analysis device 9A, the same effect as the mixed gas supply device 51 can be obtained.

[0191] <Sixth Implementation Method>

[0192] Figure 6 It is a system diagram showing the structure of a sixth embodiment of the mixed gas supply device according to the present invention.

[0193] like Figure 6 As shown, the difference between the mixed gas supply device 61 of the sixth embodiment and the mixed gas supply device 21 is that the mixed gas supply device 21 is provided with a supply control device 19, and the other structures are the same. Therefore, in the mixed gas supply device 61 of this embodiment, the same reference numerals are used for the same structures as the mixed gas supply device 21, and their descriptions are omitted.

[0194] The supply control device 19 controls the carrier gas flow rate control device 5 and the opening degree of one or more on-off valves located in the mixed gas outlet path L2.

[0195] The supply control device 19 can send and receive signals with the carrier gas flow control device 5, one or more on-off valves located on the mixed gas outlet path L2, and the second pressure gauge (pressure gauge) 12 in a wired or wireless manner. Specifically, the supply control device 19 receives the measured value of the pressure in the first buffer tank 10 from the second pressure gauge 12, and sends a control signal to the carrier gas flow control device 5 and one or more on-off valves.

[0196] Specifically, the supply control device 19 controls the set value of the carrier gas flow rate of the carrier gas flow control device 5 (or supply stop) and the opening of one or more on-off valves based on the measurement value of the second pressure gauge 12, thereby controlling the measurement value of the second pressure gauge 12 (i.e., the pressure in the first buffer tank 10) to a required value.

[0197] When the pressure of the first buffer tank 10 is insufficient relative to the set pressure value, a control signal for starting the supply of the carrier gas flow control device 5 and a control signal for "opening" one or more on-off valves located on the mixed gas outlet path L2 are sent from the second pressure gauge 12. In this way, by instantaneously controlling the supply stop of the carrier gas flow control device 5 and the opening (opening and closing) of one or more on-off valves based on the measurement value of the second pressure gauge 12, the pressure in the first buffer tank 10 can be controlled to reach a desired value.

[0198] However, in the mixed gas supply device 61 of this embodiment, the flow rate of the mixed gas may greatly vary in the mixed gas outlet path L2 due to pressure fluctuations generated to control the concentration of the mixed gas or pressure fluctuations generated in the reactor of the film forming apparatus 100 .

[0199] Therefore, by providing the mixed gas flow control device 15 in the mixed gas outlet path L2, even if pressure fluctuations occur on either the upstream side or the downstream side of the mixed gas flow control device 15, the mixed gas can be supplied at a flow rate stable with respect to the set value.

[0200] That is, by controlling the pressure on the upstream side of the mixed gas flow control device 15 in the mixed gas outlet path L2 to be within a predetermined range, the mixed gas flowing through the mixed gas outlet path L2 can be controlled to a stable flow rate.

[0201] In particular, when the first buffer tank 10 is provided upstream of the mixed gas flow control device 15 on the mixed gas outlet path L2, the influence of a sudden pressure change occurring when the pressure in the raw material container 2 is controlled by the pressure regulating device 8 can be suppressed, which is more preferable.

[0202] According to the mixed gas supply device 61 of the present embodiment, since it is provided with a supply control device 19 linked with the carrier gas flow control device 5, one or more opening and closing valves located on the mixed gas outlet path L2, and a second pressure gauge (pressure gauge) 12, and the pressure in the first buffer tank 10 on the upstream side of the mixed gas flow control device 15 is controlled within a prescribed range, the flow rate of the mixed gas flowing in the mixed gas outlet path L2 can be controlled to a stable flow rate.

[0203] As described above, according to the mixed gas supply devices 1 , 21 , 31 , 41 , 51 , and 61 of the first to sixth embodiments, the mixed gas of the gas containing the film forming material S can be supplied safely and stably.

[0204] Furthermore, when the mixed gas supply devices 1 , 21 , 31 , 41 , 51 , and 61 according to the first to sixth embodiments are used, the concentration of H 2 O contained in the mixed gas is preferably 0.1 ppm or less.

[0205] When the water concentration in the mixed gas is high, the mixed gas supply device 1 , 21 , 31 , 41 , 51 , 61 may be provided with a purifier including an adsorbent, a separation membrane, and the like.

[0206] In addition, the technical scope of the present invention is not limited to the above-mentioned embodiment, and various changes can be made without departing from the gist of the present invention.

[0207] Example

[0208] Hereinafter, the present invention will be described in more detail using examples, but the present invention is not limited to these examples.

[0209] (Example 1)

[0210] use Figure 1 The mixed gas supply device 1 shown was used as a mixed gas supply device, and a mixed gas supply test was conducted. The test conditions were as follows.

[0211] Carrier gas: Nitrogen (N2)

[0212] Carrier gas flow rate: 3000sccm

[0213] Film-forming material S: Hydrazine (N2H4)

[0214] Concentration of film-forming material S in the mixed gas (mixed gas concentration): 5% by volume

[0215] ·Pressure in the container: The pressure regulating device 8 is controlled based on the concentration measurement value of the mixed gas measuring device 9 .

[0216] The results are shown in Figure 7 .exist Figure 7 In the figure, the X-axis represents the supply time (min), the first Y-axis represents the concentration (volume %) of the mixed gas, namely, N2H4 gas, and the second Y-axis represents the pressure in the container (kPa).

[0217] like Figure 7 As shown, by providing the first buffer tank 10 and adjusting the pressure in the raw material container 2 by the pressure regulating device 8, the mixed gas can be stably supplied at a concentration of 5 volume %.

[0218] (Comparative Example 1)

[0219] Use from Figure 1 A mixed gas supply test was conducted using the mixed gas supply device 1 shown above with the first buffer tank 10 omitted. The test conditions are as follows.

[0220] Carrier gas: Nitrogen (N2)

[0221] Carrier gas flow rate: 1000sccm

[0222] Film-forming material S: Hydrazine (N2H4)

[0223] Concentration of film-forming material S in the mixed gas (mixed gas concentration): 5% by volume

[0224] ·Pressure in container: 30kPa

[0225] The results are shown in Figure 8 .exist Figure 8 In the figure, the X-axis represents the supply time (min), and the Y-axis represents the concentration (volume %) of the mixed gas, namely, N2H4 gas.

[0226] like Figure 8 As shown, in Comparative Example 1 in which the first buffer tank 10 is not provided and the pressure in the raw material container 2 is not adjusted, the mixed gas cannot be stably supplied at a concentration of 5 volume %.

[0227] Specifically, the concentration of the film forming material S gas in the mixed gas varies greatly and is not constant immediately after the supply is completed. This is because the film forming material S gas corresponding to the vapor pressure accumulated in the raw material container 2 is discharged together with the carrier gas and the concentration immediately after the supply is completed becomes high.

[0228] When the mixed gas is supplied for a long time, the gas concentration of the film forming material S in the mixed gas decreases. This is because the vapor pressure of hydrazine decreases in the raw material container 2 due to the heat of vaporization during the supply of the mixed gas.

[0229] (Example 2)

[0230] use Figure 3 The mixed gas supply device 31 shown was used as the mixed gas supply device, and a mixed gas supply test was conducted. The test conditions were as follows.

[0231] Carrier gas: Nitrogen (N2)

[0232] Carrier gas flow rate: 3000sccm

[0233] Film-forming material S: Hydrazine (N2H4)

[0234] Concentration of film-forming material S in the mixed gas (mixed gas concentration): 5% by volume

[0235] Pressure in the container: The pressure regulating device 8 is automatically controlled based on the concentration measurement value of the mixed gas measuring device 9 through the mixed gas concentration regulating device 17.

[0236] The results are shown in Fig. 9 and Fig.10 .exist Fig. 9 In the figure, the X-axis represents the supply time (min), and the Y-axis represents the concentration of the mixed gas, i.e., N2H4 gas (volume %). Fig.10 In the graph, the X-axis represents the supply time (min), and the Y-axis represents the pressure in the container (kPa).

[0237] like Fig. 9 As shown, by providing the first buffer tank 10 and automatically adjusting the pressure in the raw material container 2 by the mixed gas concentration adjusting device 17, the mixed gas can be stably supplied at a concentration of 5 volume %.

[0238] In addition, if Fig.10 As shown, it was confirmed that the pressure in the raw material container 2 was gradually reduced by the pressure regulating device 8 in order to maintain the set value of 5 volume % in the mixed gas concentration regulating device 17 .

[0239] (Example 3)

[0240] use Figure 4 The mixed gas supply device 41 shown was used as the mixed gas supply device, and a mixed gas supply test was conducted. The test conditions were as follows.

[0241] Carrier gas: Nitrogen (N2)

[0242] Carrier gas flow rate: 3000sccm

[0243] Film-forming material S: Hydrazine (N2H4)

[0244] Concentration of film-forming material S in the mixed gas (mixed gas concentration): 5% by volume

[0245] ·Pressure in the container: The pressure regulating device 8 is automatically controlled by the mixed gas concentration regulating device 17 based on the calculated value of the mixed gas concentration calculating device 18 .

[0246] The results are shown in Fig.11 .exist Fig.11 In the figure, the X-axis represents the supply time (min), the first Y-axis represents the concentration of the mixed gas, namely N2H4 gas (volume %), and the second Y-axis represents the pressure in the container (kPa).

[0247] like Fig.11As shown, by providing the first buffer tank 10 and automatically adjusting the pressure in the raw material container 2 by the mixed gas concentration adjusting device 17, the mixed gas can be stably supplied at a concentration of 5 volume %.

[0248] In addition, if Fig.11 As shown, it was confirmed that the pressure in the raw material container 2 was gradually reduced by the pressure regulating device 8 in order to maintain the set value of 5 volume % in the mixed gas concentration regulating device 17 .

[0249] (Example 4)

[0250] use Figure 6 The mixed gas supply device 61 shown was used as a mixed gas supply device, and the flow rate stability when the supply process and the stop process were repeated was evaluated under the assumption of an ALD process. The test conditions are as follows.

[0251] Carrier gas: Nitrogen (N2)

[0252] Carrier gas flow rate: 3000sccm

[0253] Film-forming material S: Hydrazine (N2H4)

[0254] Mixed gas flow rate: 3.00 (slm)

[0255] ·Pressure in container: 70kPa

[0256] Supply time: supply for 30 seconds and stop for 30 seconds

[0257] Number of repetitions: 10

[0258] The results are shown in Fig.12 .exist Fig.12 In the graph, the X-axis represents the supply time (min), the first Y-axis represents the pressure in the container (kPa), and the second Y-axis represents the mixed gas flow rate (slm).

[0259] like Fig.12 As shown, by providing the first buffer tank 10 and monitoring the pressure in the first buffer tank by the supply control device 19 and controlling the supply of the carrier gas and the opening and closing of the valve, the mixed gas can be stably supplied at a set flow rate.

[0260] In addition, if Fig.12 As shown, it was confirmed that the pressure in the raw material container 2 was stabilized by suppressing the pressure fluctuation caused by the installation of the first buffer tank 10 .

[0261] (Comparative Example 2)

[0262] Use from Figure 6The mixed gas supply device 61 shown in the figure was a mixed gas supply device in which the first buffer tank 10 was omitted, and the flow rate stability when the supply process and the stop process were repeated was evaluated assuming an ALD process. The test conditions are as follows.

[0263] Carrier gas: Nitrogen (N2)

[0264] Carrier gas flow rate: 3000sccm

[0265] Film-forming material S: Hydrazine (N2H4)

[0266] Mixed gas flow rate: 3.00 (slm)

[0267] ·Pressure in container: 70kPa

[0268] Supply time: supply for 30 seconds and stop for 30 seconds

[0269] Number of repetitions: 10

[0270] The results are shown in Fig.13 .exist Fig.13 In the graph, the X-axis represents the supply time (min), the first Y-axis represents the pressure in the container (kPa), and the second Y-axis represents the mixed gas flow rate (slm).

[0271] like Fig.13 As shown, when the first buffer tank 10 is not provided, even if the flow rate of the mixed gas is controlled by the supply control device 19, the mixed gas cannot be stably supplied at the set flow rate.

[0272] In addition, if Fig.13 As shown, since the first buffer tank 10 is not provided, the rapid pressure fluctuation in the raw material container 2 cannot be suppressed.

[0273] Description of Reference Numerals

[0274] 1, 21, 31, 41, 51, 61 mixed gas supply device

[0275] 2.2A, 2B Raw material container

[0276] 3. 3A, 3B Container heater (first heater)

[0277] 4. Container heater temperature adjustment device (first heater adjustment device)

[0278] 5 Carrier gas flow control device

[0279] 6 Pipe heater (second heater)

[0280] 7 Pipe heater temperature control device (second heater control device)

[0281] 8 Pressure regulating device

[0282] 9 Mixed gas metering device

[0283] 9A Mixed Gas Concentration Analysis Device

[0284] 9B Mixed Gas Flow Meter

[0285] 10First buffer tank (buffer tank)

[0286] 11First Pressure Gauge

[0287] 12 Second pressure gauge (pressure gauge)

[0288] 13 Detector

[0289] 14 Second buffer tank

[0290] 15Mixed gas flow control device

[0291] 16 Vacuum pump

[0292] 17Mixed gas concentration regulating device

[0293] 18Mixed gas concentration calculation device

[0294] 19 Supply control device

[0295] L1, L1A, L1B Carrier gas introduction path

[0296] L2, L2A, L2B mixed gas outlet path

[0297] L3, L3A, L3B bypass path

[0298] L4A, L4B exhaust path

Claims

1. A mixed gas supply device for supplying a mixed gas containing at least one film-forming material by adjusting the concentration of the film-forming material in the mixed gas, the mixed gas supply device comprising: A raw material container, used for containing the film-forming material; A first heater, used for heating the raw material container; A carrier gas introduction path, used to introduce carrier gas into the raw material container; A mixed gas outlet path, used for outlet the mixed gas from the raw material container; A second heater, used for heating the mixed gas outlet path; A pressure regulating device, located on the mixed gas outlet path and used to regulate the pressure of the raw material container; A mixed gas metering device, located on the primary side or the secondary side of the pressure regulating device on the mixed gas outlet path, and used to measure the concentration or flow rate of the mixed gas; and One or more buffer tanks are located on the mixed gas outlet path.

2. The mixed gas supply device according to claim 1, wherein: The buffer tank includes a first buffer tank located at the secondary side of the mixed gas metering device.

3. The mixed gas supply device according to claim 2, further comprising: A mixed gas concentration adjusting device is used to adjust the concentration of the film-forming material in the mixed gas to a set value, The mixed gas concentration adjusting device has the following functions: calculating the difference between the measured value of the concentration of the mixed gas obtained by the mixed gas metering device and the set value set in the mixed gas concentration adjusting device, and updating the pressure setting value of the pressure adjusting device based on the difference so that the measured value becomes the set value.

4. The mixed gas supply device according to claim 2, further comprising: A mixed gas concentration adjusting device, used for adjusting the concentration of the film-forming material in the mixed gas to a set value; a carrier gas flow control device, located on the carrier gas introduction path; and a mixed gas concentration calculation device for calculating the concentration of the film-forming material in the mixed gas based on the set value of the flow rate of the carrier gas set in the carrier gas flow control device and the measured value of the flow rate of the mixed gas measured by the mixed gas metering device, The mixed gas concentration adjusting device has the following functions: calculating the difference between the calculated value of the concentration of the mixed gas obtained by the mixed gas concentration calculation device and the set value set in the mixed gas concentration adjusting device, and updating the pressure setting value of the pressure adjusting device based on the difference so that the calculated value becomes the set value.

5. The mixed gas supply device according to claim 3 or 4, wherein: The buffer tank includes a second buffer tank located between the pressure regulating device and the mixed gas metering device.

6. The mixed gas supply device according to claim 1, further comprising: a first heater adjustment device, used to adjust the output of the first heater; A mixed gas concentration adjusting device, used for adjusting the concentration of the film-forming material in the mixed gas to a set value; a carrier gas flow control device, located on the carrier gas introduction path; and a mixed gas concentration calculation device for calculating the concentration of the film-forming material in the mixed gas based on the set value of the flow rate of the carrier gas set in the carrier gas flow control device and the measured value of the flow rate of the mixed gas measured by the mixed gas metering device, The mixed gas concentration adjusting device has the following functions: calculating the difference between the measured value of the concentration of the mixed gas obtained by the mixed gas metering device or the calculated value of the concentration of the mixed gas obtained by the mixed gas concentration calculation device and the set value set in the mixed gas concentration adjusting device, and updating the set value of the output of the first heater adjusting device based on the difference so that the measured value or the calculated value becomes the set value.

7. The mixed gas supply device according to any one of claims 2 to 4, further comprising: A carrier gas flow control device, located on the carrier gas introduction path; a pressure gauge for measuring the pressure in the first buffer tank; and A supply control device is used to control the carrier gas flow control device and one or more opening and closing valves located on the mixed gas outlet path, The supply control device controls the carrier gas flow control device based on the measurement value of the pressure gauge, and controls the opening degree of each of the one or more opening and closing valves. 8 . The mixed gas supply device according to claim 2 , further comprising: a mixed gas flow rate control device located on the secondary side of the first buffer tank on the mixed gas outlet path. 9 . The mixed gas supply device according to claim 7 , further comprising: a mixed gas flow rate control device located on the secondary side of the first buffer tank on the mixed gas outlet path.

10. The mixed gas supply device according to claim 1, wherein: The film-forming material is one or more compounds selected from metal-containing compounds, nitrogen-containing compounds, carbon-containing compounds and oxygen-containing compounds.

11. The mixed gas supply device according to claim 10, wherein: The nitrogen-containing compound is a hydrazine compound. 12 . The mixed gas supply device according to claim 1 , further comprising: a bypass path branched from the carrier gas introduction path and bypassing the raw material container to merge with the mixed gas outlet path. 13 . The mixed gas supply device according to claim 1 , further comprising: one or more exhaust paths branching from the mixed gas outlet path and exhausting the mixed gas in the mixed gas outlet path.

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