JP2021001383A - Precursor supply container - Google Patents

Abstract

To provide a method that reduces the pressure loss to accurately measure the pressure inside a precursor supply container in a period during which vapor of the precursor is supplied and that allows the detachment or replacement of a pressure sensor even when the precursor remains in the container.SOLUTION: A precursor container 105 comprises: a storage unit 10 for storing a precursor; a carrier gas introduction line 11; a first carrier gas introduction valve 21; an inlet side joint 12; a precursor lead-out line 13; a first precursor lead-out valve 31; and an outlet side joint 14. A container pressure measuring unit 41 is provided at least one of between the first precursor lead-out valve 31 and the outlet side joint 14 and between the first carrier gas introduction valve 21 and the inlet side joint 12, and the container pressure measuring unit is detachably attached to a precursor supply device at the inlet side joint 12 and at the outlet side joint 14.SELECTED DRAWING: Figure 5

Description

The present invention relates to a container for storing a precursor having a low vapor pressure, and in particular, the internal pressure of the container can be accurately measured while supplying the vapor of the precursor, and the precursor remains in the container. Also related to the container where the pressure sensor can be removed and replaced.

With the progress of the semiconductor industry, it is required to utilize new semiconductor materials that will meet strict thin film requirements. These materials (also called precursors) are used in a wide range of applications for thin film deposition and shape processing in semiconductor products.
For example, the precursor material may include a barrier layer, a high dielectric constant / low dielectric constant insulating film, a metal electrode film, an interconnect layer, a ferroelectric layer, a silicon nitride layer, or a component for a silicon oxide layer. In addition, constituents that act as dopants for compound semiconductors and etching materials can be mentioned. Exemplary precursor materials include aluminum, barium, bismuth, chromium, cobalt, copper, gold, hafnium, indium, yttrium, iron, lantern, lead, magnesium, molybdenum, nickel, niobium, platinum, ruthenium, silver, strontium. , Tantalum, titanium, tungsten, yttrium and zirconium inorganic compounds and organic metal compounds.
Many of these precursors are liquid or solid at room temperature. The precursor is stored in a container and supplied to the semiconductor manufacturing apparatus by a feeder attached to the container. When the precursor is a liquid, it is supplied to the semiconductor manufacturing apparatus in a gaseous state by heating the container to vaporize it or bubbling with a carrier gas to bring vapor into the carrier gas. .. When the precursor is a solid, it is sublimated or heated to liquefy it, and then supplied to the semiconductor manufacturing apparatus in a gaseous state by the same supply method as the liquid material.
Various configurations have been proposed as the precursor container. For example, Patent Document 1 and Patent Document 2 disclose a container including a carrier gas introduction valve, a dipping tube, and a precursor lead-out valve.
By the way, in order to form a uniform film, it is necessary to supply the vapor of the precursor to the semiconductor manufacturing apparatus at a constant concentration and a constant flow rate. Since the concentration and flow rate of steam depend on the pressure inside the vessel where the precursor vaporizes (or sublimates), the pressure must be controlled to remain constant.
However, when the valve is blocked or the filter is clogged due to the condensation of precursors or the generation of particles, the pressure inside the container rises. When the precursor vapor is supplied accompanied by the carrier gas, the concentration of the precursor vapor decreases as the pressure (total pressure) in the container increases when the temperature is constant. Since the partial pressure of the precursor at a constant temperature is constant, the partial pressure of the carrier gas increases as the total pressure increases, so that the concentration of the vapor of the precursor decreases.
On the other hand, when the remaining amount of the precursor decreases or the heat input to the container is insufficient with respect to the heat of vaporization of the precursor, the pressure inside the container decreases. When the pressure decreases, the differential pressure in the precursor supply line decreases, and the flow rate also decreases.
Therefore, the precursor supply device controls to supply the vapor of the precursor at a constant concentration based on the information such as the temperature and pressure in the container.
Here, the pressure sensor that detects the pressure inside the container is usually attached to the supply device side. This is because if it is attached to the supply device side, the pressure sensor portion can be purged by using the purge gas supply mechanism and the decompression mechanism provided in the supply device, and the pressure sensor can be removed or replaced after the purge. ..

Special Table 2002-524654 International Publication WO2017 / 187866

In recent years, precursors having a low vapor pressure have tended to be used, and the pressure inside the container of the precursor tends to decrease accordingly.
In the conventional method of arranging the pressure sensor on the precursor supply device side, the distance from the container to the pressure sensor is long, and a plurality of valves are also arranged between them. In addition, a filter is often arranged on the outlet side of the container. When the pressure in the system is low, the flow velocity of the flowing gas (carrier gas or precursor vapor) increases, so that the influence of conductance in the gas flow path becomes large and the pressure loss increases. For this reason, it has been found that the low vapor pressure precursor, which has come to be used in recent years, causes a pressure loss between the container and the pressure sensor, which causes a problem that the pressure inside the container cannot be measured accurately. ..
However, it is also difficult to attach the pressure sensor directly to the container. Precursors in containers often react with air and moisture to cause alteration, corrosion, heat generation, ignition, etc. However, when the pressure gauge is attached to the container side, the connection part for connecting the pressure gauge to the container cannot be purged, and the pressure gauge cannot be removed or replaced when the precursor remains in the container. Because.

Therefore, the pressure loss can be reduced, the pressure inside the container can be accurately measured during the period when the precursor vapor is supplied, and the pressure sensor can be used even when the precursor remains in the container. A method that can be removed or replaced is desired.

The precursor container according to the present invention for solving the above problems is
A storage unit that stores the precursor and
A carrier gas introduction line that introduces carrier gas into the storage unit,
The first carrier gas introduction valve arranged on the carrier gas introduction line and
An inlet side joint arranged on the primary side of the first carrier gas introduction valve on the carrier gas introduction line,
A precursor derivation line that derives the vapor of the precursor from the reservoir,
The first precursor lead-out valve arranged on the precursor lead-out line and
It has an outlet side joint arranged on the secondary side of the first precursor lead-out valve on the precursor lead-out line.
A container pressure measuring unit is provided between the first precursor lead-out valve and the outlet side joint, and at least one of the first carrier gas introduction valve and the inlet side joint.
The precursor container is detachably attached to the precursor supply device at the inlet side joint and the outlet side joint.

The vessel pressure measuring unit is arranged for the purpose of measuring the pressure at the point where the precursor vaporizes or sublimates (that is, the storage unit). In the configuration of the present invention, the pressure measuring unit is arranged not on the precursor supply device side but on the precursor container side. That is, it is arranged at a position closer to the storage portion than when it is arranged on the supply device side. With this arrangement, the pressure loss between the storage unit and the pressure measuring unit is reduced, and the pressure in the storage unit can be measured more accurately than when the pressure is arranged on the supply device side.

Further, in the present invention, a valve (first precursor lead-out valve or first carrier gas introduction valve) is arranged between the container pressure measuring unit and the precursor container, so that the precursor remains in the precursor container. The container pressure measuring unit can be purged in this state. This is because the precursor supply device side is usually provided with a line for introducing the inert gas and removing the gas by depressurizing.

The precursor container of the above invention may have a sluice valve between the container pressure measuring unit and the precursor lead-out line or the carrier gas introduction line.

The precursor container of the above invention may have a bypass line connecting the line from the first carrier gas introduction valve to the inlet side joint and the line from the first precursor lead-out valve to the outlet side joint. Good. A separation valve is arranged in the bypass line.

By providing a bypass line and arranging the container pressure measuring unit in the vicinity of the bypass line, it is possible to more efficiently purge the container pressure measuring unit.

In the precursor container of the above invention, the second carrier gas introduction valve is arranged between the first carrier gas introduction valve and the inlet side joint.
A second precursor lead-out valve is arranged between the first precursor lead-out valve and the outlet side joint.
The container pressure measuring unit is arranged between the first carrier gas introduction valve and the second carrier gas introduction valve, or between the first precursor outlet valve and the second precursor outlet valve. It may be configured.

In the precursor container of the above invention, when the container pressure measuring unit is arranged on the precursor lead-out line, the CV value of the first precursor lead-out valve may be 0.4 or more.

In the precursor container of the above invention, when the container pressure measuring unit is arranged in the carrier gas introduction line, the CV value of the first carrier gas introduction valve may be 0.4 or more.

The larger the CV value of the valve arranged between the container pressure measuring unit and the storage unit, the smaller the pressure loss, and the more accurately the pressure in the storage unit can be detected.

The precursor lead-out line between the storage unit of the precursor container of the above invention and the container pressure measuring unit may have a configuration without a filter.

Not only does the filter itself cause pressure loss, but it can also cause even greater pressure loss due to clogging due to the adhesion of precursor condensates and particles to the filter. The pressure loss can be reduced by not arranging the filter between the storage unit and the container pressure measuring unit.

The supply system according to the present invention has a temperature control unit that controls a heating mechanism for heating the precursor so that the pressure in the container pressure measurement unit falls within a predetermined range.

The heating mechanism may control the temperature of the container heating unit that heats the precursor container and / or the gas heating unit that heats the carrier gas.

As described above, the pressure in the container pressure measuring unit can accurately measure the pressure inside the precursor container. Therefore, by controlling the heating of the precursor so as to maintain this pressure within a certain range, the precursor having a constant concentration can be measured. Can be supplied.

In the precursor supply device, the device-side pressure measuring unit may be arranged on the secondary side of the connection portion with the outlet-side joint. In this case, the supply system may have a differential pressure detecting unit that detects the difference between the pressure in the device-side pressure measuring unit and the pressure in the container pressure measuring unit.

In the precursor supply device, a filter may be arranged between the connection unit and the pressure measurement unit on the device side. In this case, the supply system may have a monitoring unit that monitors clogging of the filter based on the differential pressure detected by the differential pressure detecting unit.

It is a figure which shows the structural example of the precursor container of Embodiment 1. FIG. It is a figure which shows the structural example of the precursor container of Embodiment 2. It is a figure which shows the structural example of the precursor container of Embodiment 3. It is a figure which shows the structural example of the precursor container of Embodiment 4. It is a figure which shows the structural example of the precursor container of Embodiment 5. It is a figure which shows the configuration example of the supply system of Embodiment 6. It is a figure which shows the configuration example of the supply system of Embodiment 7. It is a figure which shows the configuration example of the supply system of Embodiment 8.

Hereinafter, preferred embodiments of the present invention will be described with reference to the drawings.
(Embodiment 1)
The precursor container 101 according to the present invention shown in FIG. 1 is arranged on a storage unit 10 for storing a precursor, a carrier gas introduction line 11 for introducing a carrier gas into the storage unit 10, and a carrier gas introduction line 11. The first carrier gas introduction valve 21, the inlet side joint 12 arranged on the primary side of the first carrier gas introduction valve 21 on the carrier gas introduction line 11, and the precursor that derives the precursor steam from the storage unit 10. The body lead-out line 13, the first precursor lead-out valve 31 arranged on the precursor lead-out line 13, and the outlet side arranged on the secondary side of the first precursor lead-out valve 31 on the precursor lead-out line 13. It has a joint 14.

The precursor stored in the precursor container 101 is not particularly limited as long as it is a material used for manufacturing a semiconductor product, and may be a liquid or a solid at room temperature (20 ° C.). Each of these precursors has a unique vapor pressure and is either accompanied by a carrier gas or supplied to a semiconductor device (not shown) as its own vapor without a carrier gas.

The storage unit 10 is not particularly limited as long as it can store the precursor, and may be made of a metal such as stainless steel, iron, or aluminum, or may be made of a non-metal such as glass. ..
The shape of the storage portion 10 is not particularly limited, and may be, for example, a hollow cylindrical shape, or a cylindrical shape having a tray structure or a protrusion structure inside.

The carrier gas introduction line 11 may be a line for introducing the carrier gas into the storage unit 10, and is provided with a first carrier gas introduction valve 21 for stopping or starting the flow of the carrier gas to the storage unit 10. Has been done. As the carrier gas, a gas that is inert to the precursor stored in the storage unit 10 is usually selected, and examples thereof include nitrogen, argon, helium, hydrogen, and a mixed gas thereof.
The carrier gas introduction line 11 may be inserted into the storage unit 10, and the end portion on the inner side of the storage unit may be opened to the upper part of the storage unit. Further, as shown in FIG. 1, the carrier gas introduction line may be extended to near the bottom surface of the storage portion, and the end portion may be opened to the lower part of the storage portion.
It is also possible not to use carrier gas.

An inlet side joint 12 is arranged on the primary side of the first carrier gas introduction valve 21. The inlet side joint 12 is a portion that connects the precursor container 101 and the precursor supply device.

The precursor derivation line 13 is a line extending from the storage unit 10. From the precursor derivation line 13, the vapor of the precursor vaporized or sublimated in the precursor container 101 is derived. When a carrier gas is used, the vapor of the precursor accompanying the carrier gas is derived.
A first precursor lead-out valve 31 for stopping or starting the flow of precursor vapor from the storage unit 10 to the precursor supply device is arranged in the precursor lead-out line 13.
An outlet side joint 14 is arranged on the secondary side of the first precursor lead-out valve 31. The outlet side joint 14 is a portion that connects the precursor container 101 and the precursor supply device.

When supplying the vapor of the precursor, the pressure measured by the vessel pressure measuring unit 41 is controlled to be within a certain range. The container pressure measuring unit 41 is not particularly limited as long as it can measure the pressure, and may be a diaphragm type pressure gauge.
The container pressure measuring unit 41 is arranged between the first precursor lead-out valve 31 and the outlet side joint 14. If necessary, a pressure measuring unit may be further arranged between the first carrier gas introduction valve 21 and the inlet side joint 12.
The configuration shown by 42 in FIG. 1 is a joint for making the container pressure measuring unit 41 removable.

An example of the procedure for using the precursor container 101 is as follows.
The precursor container 101 is attached to the precursor supply device after being filled with the precursor offsite. At this time, the first carrier gas introduction valve 21 and the precursor lead-out valve 31 are closed, and the inlet side joint 12 and the outlet side joint 14 are attached to the precursor supply device. After installation, the primary side of the first carrier gas introduction valve 21 and the secondary side of the precursor lead-out valve 31 are purged, and then the precursor is opened by opening the first carrier gas introduction valve 21 and the precursor lead-out valve 31. The supply of steam is started.
When the remaining amount of the precursor in the precursor container 101 decreases, the first carrier gas introduction valve 21 and the precursor lead-out valve 31 are closed, and the primary side of the first carrier gas introduction valve 21 and the precursor lead-out valve are closed. The secondary side of 31 is purged. After that, the inlet side joint 12 and the outlet side joint 14 are removed, and the precursor container 101 is removed from the precursor supply device.
In the precursor container 101 of the present invention, the container pressure measuring unit 41 is arranged between the first precursor outlet valve 31 and the outlet side joint 14. Therefore, by closing the first precursor lead-out valve 31, the container pressure measuring unit 41 and the precursor of the storage unit 10 are separated from each other. Therefore, the container pressure measuring unit 41 can be purged with the precursor remaining in the storage unit 10 both when the precursor container 101 is attached and when the precursor container 101 is removed.

The precursor container 101 according to the present invention can be applied to a precursor having any vapor pressure, but the vapor pressure is particularly low (not particularly limited, for example, the vapor pressure at 100 ° C. is 50 torr or less). Has a significant effect on the supply of precursors.
The precursor of a liquid having a low vapor is not particularly limited, and examples thereof include tetrakis (ethylmethylamino) hafnium and tetrakis (ethylmethylamino) zirconium.
The precursor of a solid having a low vapor pressure is not particularly limited, and examples thereof include molybdenum chloride, tungsten chloride, and aluminum chloride.

The concentration and flow rate of the precursor vapor derived from the precursor vessel 101 varies depending on the pressure of the reservoir 10 in which the precursor vaporizes or sublimates. Therefore, in order to supply the precursor vapor having a constant concentration and flow rate, it is necessary to maintain the pressure of the storage unit 10 at a constant level.
When a precursor having a low vapor pressure is supplied as steam having a concentration equal to or higher than a predetermined concentration, the pressure in the storage unit 10 becomes low. Then, the flow velocity of the precursor vapor increases, and it becomes easily affected by the pressure loss in the above-mentioned distribution path.
In the precursor container 101 of the present invention, since the container pressure measuring unit 41 is arranged near the valve (first carrier gas introduction valve 21 or first precursor lead-out valve 31), from the storage unit 10 to the pressure measuring unit 41. The distance between the two is close, the influence of pressure loss is reduced, and more accurate pressure measurement becomes possible.
The distance from the storage unit 10 to the pressure measurement unit 41 can be determined according to the pipe diameter, valve specifications, vapor pressure of the precursor, and the like. For example, the distance from the top of the space accommodating the precursor of the storage unit 10 to the pressure measuring unit 41 can be 30% or less of the height of the space accommodating the precursor, and must be 15% or less. Is preferable. The distance to the pressure measuring unit is preferably shortened as the pipe diameter becomes smaller and the vapor pressure of the precursor becomes lower.

The first precursor lead-out valve 31 located between the container pressure measuring unit 41 and the storage unit 10 is preferably a valve having as little pressure loss as possible. Therefore, the CV value of the first precursor lead-out valve 31 is preferably large, for example, 0.4 or more.
Similarly, from the viewpoint of pressure loss, the pipe diameter of the precursor lead-out line 13 is preferably large, for example, 1/4 inch, but more preferably 1/2 inch.

(Embodiment 2)
FIG. 2 shows the precursor container 102 according to the second embodiment. In the precursor container 102 of FIG. 2, the container pressure measuring unit 41 is arranged on the carrier gas introduction line 11 between the first carrier gas introduction valve 21 and the inlet side joint 12.
Similar to the case of the precursor container 101 shown in FIG. 1, even when the precursor remains in the storage unit 10, by closing the first carrier gas introduction valve 21, the container pressure measuring unit 41 It is possible to purge. Further, since the container pressure measuring unit 41 is arranged in the vicinity of the storage unit 10, it is possible to measure the pressure of the storage unit 10 more accurately.

The first carrier gas introduction valve 21 located between the container pressure measuring unit 41 and the storage unit 10 is preferably a valve having as little pressure loss as possible. Therefore, the CV value of the first carrier gas introduction valve 21 is preferably large, for example, 0.4 or more.
Similarly, from the viewpoint of pressure loss, the diameter of the carrier gas introduction line 11 is preferably large, for example, 1/4 inch, but more preferably 1/2 inch.

(Embodiment 3)
As the third embodiment, a sluice valve 51 can be provided between the container pressure measuring unit 41 and the precursor lead-out line 13 or the carrier gas introduction line 12. FIG. 3 shows a state in which a sluice valve 51 is provided between the container pressure measuring unit 41 and the carrier gas introduction line 12 in these embodiments.

The sluice valve 51 is mainly used when replacing the pressure measuring unit 41. For example, in the embodiment shown in FIG. 3, (1) the sluice valve 51 is opened and the first carrier gas introduction valve 21 is closed even when the precursor container 103 is still attached to the supply device. By (2) purging the upstream side of the first carrier gas introduction valve 21 and (3) closing the sluice valve 51, the container pressure measuring unit 41 can be safely removed. Since the sluice valve 51 is closed when the container pressure measuring unit 41 is removed, the upstream side of the sluice valve 51 (that is, between the supply device side and the carrier gas introduction line 11) is exposed to the atmosphere and contaminated. Can be prevented.

(Embodiment 4)
The precursor container 104 of the fourth embodiment shown in FIG. 4 is between the first carrier gas introduction valve 21 and the inlet side joint 12 of the carrier gas introduction line 11 and the first precursor out of the precursor lead-out line 13. It has a bypass line 61 connecting the valve 31 and the outlet side joint 14.

When there is no bypass line 61, it is necessary to purge the carrier gas introduction line 11 and the precursor lead-out line 13 separately. In the fourth embodiment, since the carrier gas introduction line 11 and the precursor lead-out line 13 are connected by having the bypass line 61, the purge gas is circulated from the carrier gas introduction line 11 to the precursor lead-out line 13. It becomes possible to purge, and the purging efficiency increases. Since the container pressure measuring unit 41 is arranged on the bypass line 61 or in the vicinity of the bypass line 61, it becomes easier to purge.

A separation valve 62 is arranged on the bypass line 61. The separation valve may be a valve capable of separating the upstream side and the downstream side of the bypass line 61 (that is, the side close to the carrier gas introduction line 11 and the side close to the precursor lead-out line 13), for example, the bypass line 61. It may be a two-way valve arranged near the center, but it may be a three-way valve arranged so as to cut off the bypass line 61 at the branch portion with the carrier gas introduction line 11, as shown in FIG. As shown, it may be a three-way valve arranged so as to block the bypass line 61 at the branch portion with the precursor lead-out line 13.

When purging the bypass line 61, the first carrier gas introduction valve 21 and the first precursor lead-out valve 31 are closed, and the separation valve 62 is opened. When supplying the steam of the precursor stored in the precursor container 104, the separation valve 62 is closed and the first carrier gas introduction valve 21 and the first precursor lead-out valve 31 are opened. As a result, the carrier gas is introduced into the precursor container 104 from the carrier gas introduction line 11 and is led out from the precursor out-out line 13 with the precursor vapor vaporized in the precursor container 104.

Although not shown in FIG. 4, a sluice valve may be arranged between the container pressure measuring unit 41 and the precursor lead-out line 13 as in the third embodiment. The container pressure measuring unit 41 may be arranged on the precursor lead-out line 13 as shown in FIG. 4, but may also be arranged on the carrier gas introduction line 11.

(Embodiment 5)
The precursor container 105 of the fifth embodiment shown in FIG. 5 has a second carrier gas introduction valve 22 between the first carrier gas introduction valve 21 and the inlet side joint 12, and the first precursor lead-out valve 31 and the outlet. It has a second precursor lead-out valve 32 between it and the side joint 14. The container pressure measuring unit 41 may be arranged between the first carrier gas introduction valve 21 and the second carrier gas introduction valve 22, but as shown in FIG. 5, the first precursor lead-out valve 31 and the second It may be arranged between the precursor lead-out valve 32 and the precursor valve 32.
The second carrier gas introduction valve 22 and the second precursor lead-out valve 32 are provided so that the container pressure measuring unit 41 is not exposed to the surrounding environment (atmosphere) when the precursor container 105 is removed from the precursor supply device. .. This is because the valve is arranged at a position farther from the storage unit 10 than the container pressure measuring unit 41, and the precursor container 105 can be removed from the supply device with the valve closed.

Further, by arranging these valves, it is possible to purge the line with the storage unit 10 independently of the line on the precursor supply device side.
For example, when the pressure measuring unit 41 is arranged between the first precursor outlet valve 31 and the second precursor outlet valve 32, the first precursor outlet valve 31 is installed after the container pressure measuring unit 41 is attached. With the valve closed, the purge gas can be introduced from the second precursor lead-out valve 32 and the purge gas can be evacuated. Moisture or the like may be adsorbed on the pressure measuring unit 41, which may cause impurities to be generated when the vapor of the precursor is supplied. However, if the container pressure measuring unit 41 is attached in advance and then purged in this way, the precursor container 105 can be kept sufficiently clean before being attached to the precursor supply device.

Similarly, when the container pressure measuring unit 41 is provided between the first carrier gas introduction valve 21 and the second carrier gas introduction valve 22, the first carrier gas introduction valve 21 is closed and the second carrier is closed. Purging can be performed using the gas introduction valve 22.
Further, when the bypass line 61 is provided, the vicinity of the bypass line 61 surrounded by the first carrier gas introduction valve 21, the first precursor lead-out valve 31, the second precursor lead-out valve 32, and the second carrier gas introduction valve 22. Can be purged.

When trying to measure the pressure of the storage unit 10, it is possible to measure more accurately when there is less material that causes a pressure loss between the storage unit 10 and the container pressure measuring unit 41. Therefore, the larger the CV value of the valves arranged between them (the first precursor lead-out valve 31 or the first carrier gas introduction valve 21), the smaller the pressure loss and is suitable. The CV value is more preferably 0.4 or more.
Further, if the filter is arranged during this period, a pressure loss may occur, and the pressure loss may be further increased due to the condensation of the precursor or the adhesion of particles during the supply. Therefore, it is more preferable not to arrange a filter between the storage unit 10 and the container pressure measuring unit 41.

(Embodiment 6)
The sixth embodiment shown in FIG. 6 is a supply system in which the heating mechanism 70 is introduced into the precursor container 105 of the fifth embodiment. A heating mechanism 71 that determines the desired internal pressure of the container according to the conditions for using the precursor and heats the precursor so that the pressure detected by the container pressure measuring unit 41 becomes the desired internal pressure of the container. Control. Here, the heating mechanism is not particularly limited as long as it can heat the precursor stored in the storage unit 10, and for example, as shown in FIG. 6, a heater that heats the precursor container 105 from the outside is used. There may be. An internal heater that heats the precursor from the inside of the storage unit 10, a constant temperature bath that stores the entire precursor container 105, and a carrier gas introduced into the storage unit 10 are added in place of or in addition to the heater. A heater or the like for heating can also be used.

(Embodiment 7)
In the supply system according to the seventh embodiment shown in FIG. 7, the precursor container 105 shown in the fifth embodiment is connected to the precursor supply device 80, and the connection portion with the outlet side joint 14 (the joint shown by 81 in FIG. 7). The device-side pressure measuring unit 82 is arranged on the secondary side of (there is). The differential pressure detecting unit 84 detects the differential pressure between the pressure detected by the device-side pressure measuring unit 82 and the pressure detected by the container pressure measuring unit 41.
When a blockage occurs between the container pressure measuring unit 41 and the device-side pressure measuring unit 82, the differential pressure increases. Possible causes of blockage include condensation, alteration, and particle generation of precursors inside the valve or piping, which may lead to unstable supply of precursors and maintenance or replacement of these components. May be needed. Therefore, when the differential pressure increases more than a predetermined value, an alarm may be set to be issued.

(Embodiment 8)
The supply system according to the eighth embodiment shown in FIG. 8 has a configuration in which the filter 90 is arranged in the supply system of the seventh embodiment. The filter 90 is on the side of the precursor supply device 80 for the purpose of preventing a phenomenon in which particles or the like caused by the precursor are led out to the piping on the precursor supply device 80 side to cause a problem such as valve outflow. Often placed in. When the filter 90 is clogged, the vapor of the precursor normally derived in the precursor container 105 cannot reach the precursor supply device 80 in a stable manner. Therefore, the differential pressure detecting unit 84 detects the differential pressure between the container pressure measuring unit 41 and the device-side pressure measuring unit 82, and when the differential pressure increases to a predetermined value or more, the filter 90 is clogged. A monitoring unit 85 that monitors clogging by determining that it has occurred is arranged. The predetermined differential pressure for determining that the filter 90 is clogged can be arbitrarily determined according to the specifications of the filter and the properties of the solid material. In addition to determining the presence or absence of clogging based on whether or not the above-mentioned arbitrary differential pressure has been reached, the monitoring unit 85 can also be provided with a function of issuing an alarm when clogging occurs.

101. Precursor container 10. Reservoir 11. Carrier gas introduction line 12. Entrance side joint 13. Precursor derivation line 14. Outlet side fitting
21. First carrier gas introduction valve 22. Second carrier gas introduction valve 31. First precursor lead-out valve 32. Second precursor lead-out valve 41. Container pressure measuring unit 51. Gate valve 61. Bypass line 62. Separation valve 70. Heating mechanism 71. Temperature control unit 82. Device side pressure measuring unit

Claims (11)

A storage unit that stores the precursor and
A carrier gas introduction line that introduces carrier gas into the storage unit,
The first carrier gas introduction valve arranged on the carrier gas introduction line and
An inlet side joint arranged on the primary side of the first carrier gas introduction valve on the carrier gas introduction line,
A precursor derivation line that derives the vapor of the precursor from the reservoir,
The first precursor lead-out valve arranged on the precursor lead-out line and
It has an outlet side joint arranged on the secondary side of the first precursor lead-out valve on the precursor lead-out line.
A container pressure measuring unit is provided between the first precursor lead-out valve and the outlet side joint, and at least one of the first carrier gas introduction valve and the inlet side joint.
A precursor container that is detachably attached to a precursor supply device at the inlet side joint and the outlet side joint. The precursor container according to claim 1, further comprising a sluice valve between the container pressure measuring unit and the precursor lead-out line or the carrier gas introduction line. A bypass line connecting the line from the first carrier gas introduction valve to the inlet side joint and the line from the first precursor lead-out valve to the outlet side joint.
The precursor container according to claim 1 or 2, further comprising a separation valve arranged on the bypass line. A second carrier gas introduction valve is arranged between the first carrier gas introduction valve and the inlet side joint.
A second precursor lead-out valve is arranged between the first precursor lead-out valve and the outlet side joint.
The container pressure measuring unit is arranged between the first carrier gas introduction valve and the second carrier gas introduction valve, or between the first precursor lead-out valve and the second precursor lead-out valve. , The precursor container according to any one of claims 1 to 3. The invention according to any one of claims 1 to 4, wherein the CV value of the first precursor lead-out valve is 0.4 or more when the container pressure measuring unit is arranged in the precursor lead-out line. Precursor container. The method according to any one of claims 1 to 4, wherein the CV value of the first carrier gas introduction valve is 0.4 or more when the container pressure measuring unit is arranged in the carrier gas introduction line. Precursor container. The precursor container according to any one of claims 1 to 6, wherein the precursor lead-out line from the storage unit to the container pressure measuring unit does not have a filter. A supply system having a temperature control unit that controls a heating mechanism that heats the precursor so that the pressure in the container pressure measuring unit falls within a predetermined range. The supply system according to claim 8, wherein the heating mechanism controls the temperature of the container heating unit that heats the precursor container and / or the gas heating unit that heats the carrier gas. In the precursor supply device, a device-side pressure measuring unit is arranged on the secondary side of the connection portion with the outlet-side joint.
The supply system according to claim 8 or 9, further comprising a differential pressure detecting unit that detects a difference between the pressure in the device-side pressure measuring unit and the pressure in the container pressure measuring unit. In the precursor supply device, a filter is arranged between the connection unit and the pressure measurement unit on the device side.
The supply system according to claim 10, further comprising a monitoring unit that monitors clogging of the filter based on the differential pressure detected by the differential pressure detecting unit.

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