JP2007239008A - Material feeding device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a bubbler provided with a monitoring apparatus where the stability in the amount of the objective material to be fed by bubbling can be monitored. <P>SOLUTION: A mass flow rate controlling means 13 and a first stop valve 18 are connected in order from the upstream side between the introduction port of a bubbler and a carrier gas source, further, a second stop valve 19 and a sonic nozzle 1 are connected in order from the upstream side between the leading-out port of the bubbler and a consumption apparatus, further, the inflow side of the first stop valve 18 and the outflow side of the second stop valve 19 are connected by a third stop valve 20, and the pressure on the inflow side of the sonic nozzle 1 is monitored, thus the content of the objective material is detected. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention provides a material supply device using a bubbler that causes a carrier gas to act on a liquid contained in a container or a solid to vaporize the liquid or sublimate the solid, and more specifically, supplies a predetermined amount of a target material. Alternatively, the present invention relates to a technique for monitoring whether or not a predetermined amount is supplied.

  For example, in the semiconductor industry, for the purpose of supplying a certain amount of semiconductor target material and MO target material to the reaction chamber, as shown in Patent Document 1, the semiconductor target material and MO target material are kept in a container maintained at a constant temperature. The mixed gas having a concentration equal to the partial pressure of the semiconductor target material and the MO target material is generated by allowing the carrier gas to act.

The concentration of this mixed gas is generally (Equation 1)
Pz / Pt = Qz / (Qz + Qc)
Where Pz is the target material vapor pressure, Pt is the total pressure in the container, Qz is the flow rate of the target material, Qc is the flow rate of the carrier gas, and Pz is the temperature of the target material held in the bubbler (T ) Represents the vapor pressure depending on each.
Can be expressed as

  Thus, since the partial pressure Pz of the target material depends on the target material temperature, sufficient consideration must be given to the temperature distribution in the bubbler and the temperature change due to the heat of vaporization. In other words, in order to realize a stable supply of the target material, in addition to examining the heat transfer and heat capacity of the bubbler, physical and chemical knowledge of the target target material is also required.

  Usually, it is assumed that the partial pressure Pz is maintained at a constant value. However, when the target material is solid, a predetermined concentration (vapor pressure) cannot be obtained due to the difference in surface area exposed to the carrier gas. The supply amount changes with time, and in the case of a liquid, the temperature decreases due to the heat of vaporization at the gas-liquid interface in the bubbler, and the supply amount also changes with time.

  For this reason, when using bubblers, we rely on operational know-how based on experience, or measure the amount of adhesion using a dummy wafer, etc. .

Of course, it is conceivable to connect a concentration monitoring device to the downstream side of the bubbler, but it is not only expensive but is not perfect in terms of performance, and various correction operations are required.
JP-A-6-32695

  The present invention has been made in view of such problems, and the object thereof is to monitor the stability of the amount of a target material to be supplied by a bubbler with a relatively simple configuration by using a sonic nozzle. Another object is to provide a material supply apparatus including a monitoring mechanism that can be used, and a material supply apparatus including a mechanism that controls the amount of a predetermined target material to a constant amount based on a monitoring value.

  In order to achieve such a problem, the invention of claim 1 is characterized in that a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device. The mass flow rate control means and the first on-off valve are connected in order from the upstream side between the inlet and the carrier gas source, and the outlet and the consumption device are connected to each other. A second on-off valve and a sonic nozzle are connected in order from the upstream side, and an inflow side of the first on-off valve and an outflow side of the second on-off valve are connected by a third on-off valve, When the first and second on-off valves are closed and the third on-off valve is opened, the mass flow rate control means supplies a carrier gas having a predetermined flow rate at which the sonic nozzle is choked to the sonic nozzle. Then the first and second on-off valves are opened, and the third Closing the on-off valve, supplying the carrier gas to the container at the predetermined flow rate, discharging the carrier gas containing the target material from the outlet, and monitoring the pressure on the inflow side of the sonic nozzle; A monitoring device for detecting the content of

  The invention of claim 2 uses a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device. The mass flow control means and the first on-off valve are connected in order from the upstream side between the inlet and the carrier gas source, and the second in turn from the upstream side between the outlet and the consumer device. The on-off valve and the sonic nozzle are connected, and the inflow side of the first on-off valve and the outflow side of the second on-off valve are connected by a third on-off valve. A dilution gas source is connected via the flow rate control means, the first and second on-off valves are closed, and the third on-off valve is opened from the carrier gas and the dilution gas source. The carrier gas and the diluting gas so that the sonic nozzle is choked. The diluting gas is caused to flow into the sonic nozzle at a predetermined flow rate, then the first and second on-off valves are opened, and the third on-off valve is closed to supply the carrier gas at the predetermined flow rate. A monitoring device is provided that detects the content of the target material by supplying the container to discharge the carrier gas containing the target material from the outlet and monitoring the pressure on the inflow side of the sonic nozzle.

  The invention of claim 3 uses a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device. The mass flow control means and the first on-off valve are connected in order from the upstream side between the inlet and the carrier gas source, and the second in turn from the upstream side between the outlet and the consumer device. An on-off valve and a sonic nozzle, and an inflow side of the first on-off valve and an outflow side of the second on-off valve are connected by a third on-off valve. The sonic velocity is measured with a mass flow rate measuring means and a dilution gas source connected from the side through a pressure regulating valve, the first and second on-off valves are closed, and the third on-off valve is opened. The pressure regulating valve controls the pressure on the inflow side of the sonic nozzle so that the nozzle is choked. In addition, the carrier gas is allowed to flow into the sonic nozzle at a predetermined flow rate, the first and second on-off valves are then opened, and the third on-off valve is closed to attain the carrier gas at the predetermined flow rate. Is supplied to the container, the carrier gas containing the target material is discharged from the outlet, and the monitoring device detects the content of the target material by monitoring the flow rate of the mass flow rate measuring means.

  The invention of claim 4 uses a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device. The mass flow control means and the first on-off valve are connected in order from the upstream side between the inlet and the carrier gas source, and the second in turn from the upstream side between the outlet and the consumer device. The on-off valve of the first on-off valve and the outflow side of the second on-off valve are connected by a third on-off valve to the upstream side of the sonic nozzle. The sonic velocity is measured with a mass flow rate measuring means and a dilution gas source connected from the side through a pressure regulating valve, the first and second on-off valves are closed, and the third on-off valve is opened. The pressure regulating valve controls the pressure on the inflow side of the sonic nozzle so that the nozzle is choked. In addition, the carrier gas is allowed to flow into the sonic nozzle at a predetermined flow rate, then the first and second on-off valves are opened, and the third on-off valve is closed to dilute the mass flow rate measuring means. The carrier gas flow rate is controlled by the mass flow rate control means so that the sum of the working gas flow rate and the carrier gas flow rate becomes a predetermined flow rate to obtain a desired content of the target material.

  The invention of claim 5 uses a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device. Mass flow measuring means, a pressure regulating valve, and a first on-off valve are connected in order from the upstream side between the inlet and the carrier gas source, and the upstream side between the outlet and the consumer device. The second on-off valve and the sonic nozzle are connected in order, and the inflow side of the first on-off valve and the outflow side of the second on-off valve are connected by a third on-off valve, With the second on-off valve closed and the third on-off valve open, the carrier gas is caused to flow into the sonic nozzle from the pressure adjusting valve at a predetermined pressure at which the sonic nozzle is choked, Next, the first and second on-off valves are opened, and the third on-off valve is closed. A monitoring device for detecting the content of the target material by supplying a carrier gas to the container at a predetermined pressure, discharging the carrier gas containing the target material from the outlet, and monitoring the flow rate of the mass flow rate measuring means Is provided.

  The invention of claim 6 uses a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device. Mass flow measuring means, a pressure regulating valve, and a first on-off valve are connected in order from the upstream side between the inlet and the carrier gas source, and the upstream side between the outlet and the consumer device. The second on-off valve and the sonic nozzle are connected in order, and the inflow side of the first on-off valve and the outflow side of the second on-off valve are connected by a third on-off valve, A gas source for dilution is connected to the inflow side via a mass flow control means, the first and second on-off valves are closed, and the sonic nozzle is choked with the third on-off valve opened. Pressure of the dilution gas on the inflow side of the sonic nozzle by the pressure regulating valve so as to be in a state The carrier gas is allowed to flow into the sonic nozzle at a predetermined pressure, then the first and second on-off valves are opened, and the third on-off valve is closed to carry the carrier at the predetermined flow rate. The mass flow rate control means for supplying the gas to the container and discharging the carrier gas containing the target material from the outlet, so that the sum of the flow rate of the carrier gas and the dilution gas flow rate by the mass flow rate measurement means becomes a predetermined flow rate. The desired content of the target material is obtained by controlling the flow rate of the gas for dilution in step (b).

  According to a seventh aspect of the present invention, a plurality of sonic nozzles are selectably connected via the flow path switching means, and the characteristics of the plurality of sonic nozzles are different.

According to the invention of claim 1, since the sonic nozzle is connected to the outlet of the bubbler, it is contained in the carrier gas with a simple configuration of detecting the pressure (back pressure) on the inflow side of the sonic nozzle. The amount and stability of the target material can be monitored. Further, since the supply is made to the consumer device via the sonic nozzle, the supply amount due to the pressure fluctuation on the consumer device side can be eliminated.
Moreover, since it has a flow path which bypasses a bubbler and supplies carrier gas to a sonic nozzle, the flow volume of carrier gas itself can also be monitored.

  According to the invention of claim 2, by using the dilution gas, in addition to the effect of the invention of claim 1, the dilution rate can be easily changed over a wide range.

  According to the invention of claim 3, in addition to the effect of the invention of claim 2, in order to keep the inflow pressure to the sonic nozzle constant at the desired pressure, the internal pressure of the bubbler is kept constant at the desired pressure. The absolute amount of the target material can be kept constant.

  According to the invention of claim 4, in addition to the effect of the invention of claim 3, the carrier gas flow rate is adjusted even when the state of the bubbler such as a change in surface area of the target material or a temperature drop due to heat of vaporization changes, By keeping the sum of the dilution gas flow rate and the carrier gas flow rate constant, the supply amount of the target material can be kept constant.

  According to the invention of claim 5, the amount of the target material contained in the carrier gas can be determined by monitoring the flow rate of the carrier gas. Further, when the sonic nozzle is contaminated by the flow path for bypassing the bubbler and supplying the carrier gas to the sonic nozzle, the state change of the sonic nozzle due to the influence of the deposits or the like can be monitored. Further, since the supply is made to the consumer device via the sonic nozzle, the influence on the supply amount due to the pressure fluctuation on the consumer device side can be eliminated.

  According to the invention of claim 6, in addition to the effect of the invention of claim 5, the dilution gas flow rate is adjusted even when the state of the bubbler such as a change in the surface area of the target material or a temperature drop due to heat of vaporization changes. By keeping the sum of the dilution gas flow rate and the carrier gas flow rate constant, the supply amount of the target material can be kept constant.

  According to the seventh aspect of the present invention, the pressure and flow rate of the carrier gas and dilution gas can be changed over a wide range without removing the sonic nozzle from the flow path.

First, the sonic nozzle that is a constituent of the present invention will be described.
The sonic nozzle 1 has a throat portion 1a that is narrowed as shown in FIG. 1, and has a large pressure difference between the upstream side and the downstream side across the throat portion 1a, that is, the upstream / downstream pressure ratio (downstream / downstream / If it is set so that (upstream) is equal to or less than a certain value (critical pressure ratio), this is a nozzle in which the flow velocity of the gas passing through the throat portion 1a becomes equal to the sound velocity.
With this function, once the flow velocity of the throat portion 1a becomes the sonic velocity, the flow velocity of the throat portion 1a does not depend on the downstream state of the nozzle 1, and if it is below the critical pressure ratio, it depends on the state of the downstream flow. Therefore, a constant flow rate of fluid can always be supplied downstream.

By utilizing this principle, a highly accurate mass flow meter having no moving parts can be configured.
Theoretically, the mass flow rate of the gas flowing through the sonic nozzle 1 is determined by the sound velocity and density of the gas throat portion 1a, and the cross-sectional area of the throat portion 1a, but in reality, the boundary generated in the throat portion 1a. The effective cross-sectional area is reduced by the layer, and further, the flow in the main flow portion is accelerated, so that the flow velocity distribution is distorted.
For this reason, since the actual mass flow rate is smaller than the theoretically required mass flow rate, it is necessary to multiply the correction coefficient (outflow coefficient of the sonic nozzle), and the correction count indicates the state of the flow at the throat portion 1a. Since this is a function of the Reynolds number, the relationship between the outflow coefficient and the Reynolds number is obtained through experiments.
In other words, if the outflow coefficient of the sonic nozzle is obtained by calibration, the mass flow rate can be obtained with high accuracy with a simple configuration by measuring the pressure and temperature upstream of the sonic nozzle.

That is, the mass flow rate conversion formula at the sonic nozzle 1 is
(Equation 2)
Q = Cd × A × Pt × √ (k × Mw / (R × Tc))
Where Cd is the outflow coefficient, A is the cross-sectional area of the throat part 1a, k is a numerical value obtained from the specific heat ratio, Mw is the molar mass, R is the gas universal constant, Pt is the pressure of the throat part 1a, and Tc is the temperature of the throat part 1a. Respectively.
It becomes.

  FIG. 2 shows an embodiment of the present invention. As is well known, a bubbler 10 includes a tank 12 containing a target material 11 and a flow rate control means 13, which in this embodiment is a mass flow rate control device (MFC). ) By a jet pipe 14 for jetting the carrier gas whose flow rate is controlled to the bottom of the liquid surface of the target material, and a discharge pipe 16 that communicates with the space 15 of the tank 12 and extracts the carrier gas containing the target material 11. It is comprised, and the shunt pipe 17 is connected as needed. In the figure, reference numerals 18 to 20 denote stop valves, and reference numeral 21 denotes a temperature detecting means.

A monitoring device 30 characterized by the present invention is connected to the discharge pipe 16 via a stop valve 19.
The monitoring device 30 includes a tube body 31 that accommodates the sonic nozzle 1, a pressure detection unit 32 connected to the upstream side of the sonic nozzle 1, and a temperature detection unit 33 that detects a gas temperature upstream of the tube body 31. The downstream side (right side in the figure) of the sonic nozzle 1 is connected to the consumer device.

When the carrier gas is directly introduced so that the stop valves 18 and 19 are closed and the stop valve 20 is opened and the throat portion 1a of the sonic nozzle 1 is in the choked state, the mass flow rate Qc of the introduced carrier gas and The pressure Pt of the throat portion 1a is
(Equation 3)
Qc = B × Pt × √Mwc
(However, Qc represents the mass flow rate of the carrier gas, and Mwc represents the molar mass of the introduced carrier gas. The temperature conditions are constant.)
Shows the correlation.

Next, the stop valves 18 and 19 are opened, and the stop valve 20 is closed and the flow rate for maintaining the relationship of the above formula 3, that is, the carrier gas having the same mass flow rate as that passed through the sonic nozzle 1 in the above-described process. Is introduced into the bubbler 10, the mass flow rate Qz of the gas of the target material itself depending on the vapor pressure of the target material, as expressed by the general formula (Expression 1) indicating the target material supply amount of the bubbler 10, is as described above. In addition to the mass flow rate Qc of the carrier gas, it flows through the sonic nozzle 1,
(Equation 4)
Qc + Qz = B1 × Px × √ ((Qc × Mwc + Qz × Mwz) / (Qc + Qz))
(However, Qz represents the target material gas flow rate, Mwz represents the molar mass of the target material, and Px represents the pressure in the throat part. Note that the temperature condition is the same as Equation 3.)
It becomes.
It should be noted that when the target material gas flow rate is smaller than the carrier gas flow rate, B1 and B are almost the same.

Further, since the pressure loss due to the piping from the bubbler 10 to the sonic nozzle 1 is very small with respect to the pressure Pt of the throat portion 1a, the pressure Px of the throat portion 1a and the internal pressure (total pressure) of the bubbler 10 can be regarded as the same.
(Equation 5)
Pz / Px = Qz / (Qz + Qc)

Using the B obtained in Equation 3, the pressure Px of the throat portion 1a and the mass flow rate Qz of the target material from the relationship with Equations 4 and 5 are as follows:
Px
Qz
Can be obtained as

  Therefore, it is possible to easily determine the stability of the mass flow rate Qz of the target material 11 and whether the target material has a predetermined flow rate simply by monitoring the pressure Px of the throat portion 1a.

  Further, only the carrier gas is periodically introduced directly from the flow rate control means 13 via the branch pipe 17 into the sonic nozzle 1 of the monitoring device 30, and the flow rate control means 13 of the flow rate control means 13 is based on a highly accurate measurement value by the sonic speed nozzle 1. Changes over time can be examined.

  FIG. 3 shows a second embodiment of the present invention. In this embodiment, not only the carrier gas source but also the second mass flow rate control means 13 ′ is connected to the inflow side of the sonic nozzle 1. And an additional gas source for dilution is connected.

  In this embodiment, the stop valves 18 and 19 are closed, and the stop valve 20 is opened so that the carrier gas and the dilution gas flow into the sonic nozzle 1 at a predetermined flow rate so that the sonic nozzle 1 is in a choked state. The stop valves 18 and 19 are opened, the stop valve 20 is closed, the carrier gas is supplied to the container 12 at a predetermined flow rate, and the carrier gas containing the target material is discharged from the 16 outlets. By monitoring the pressure on the inflow side of the nozzle 1 by the pressure detecting means 32, the content of the target material can be detected.

  According to this embodiment, since dilution can be performed with the dilution gas, the dilution rate can be changed in a wide range.

FIG. 4 shows a third embodiment of the present invention. In this embodiment, a carrier gas is supplied via a flow rate adjusting valve 35 instead of the expensive flow rate control means 13. It is.
That is, the mass flow rate of the flow rate adjustment valve 35 is controlled by a signal from the pressure detection means 32 that detects the pressure on the inflow side of the sonic nozzle 1. In the figure, reference numeral 34 denotes a driving means for controlling the flow rate adjusting valve 35, and reference numeral 36 denotes a mass flow rate measuring device (MFM).

  When the mass flow rate is adjusted by the flow rate adjustment valve 35 so that the pressures Pt and Px of the throat portion 1a are equal (Equation 3 and Equation 4), the mass flow rate Qc of the carrier gas itself in Equation 4 contains the target material. Decreases by the amount of gas mass flow added. By monitoring the reduced mass flow ΔQ by the mass flow measurement device 36, it becomes possible to determine whether the mass flow stability of the target material itself and the content of the target material are maintained at the target value. .

That is, if the flow rate of the carrier gas flowing into the sonic nozzle 1 is Qc1,
(Equation 6)
Qc1 + Qz = B * Pt * √ ((Qc1 * Mwc + Qz * Mwz) / (Qc1 + Qz))
(Equation 7)
Pz / Pt = Qz / (Qz + Qc1)
Therefore, B and Pt in Equation 6 are known values obtained in Equation 3, and according to the relationship with Equation 7,
Qc1
Qz
Respectively.

  In the first embodiment shown in FIG. 2 and FIG. 3, when the mass flow rate of the target material is arbitrarily changed, the pressure (back pressure) on the inflow side of the sonic nozzle 1 is changed. Further, in the second embodiment shown in FIG. 4, this can be dealt with by adjusting the flow rate of the carrier gas by the flow rate adjusting valve 35, but it can be changed by the pressure on the secondary side of the sonic nozzle 1, that is, the consumer device side. The flow range is controlled.

  That is, if the secondary side of the sonic nozzle 1 is in a vacuum condition, the sonic nozzle 1 can be easily maintained in the choked state even if the total pressure of the bubbler 10 is low, but the secondary side of the sonic nozzle 1 is at atmospheric pressure or the like. When the pressure is higher than the vacuum, in order to choke the sonic nozzle 1, it is necessary to increase the pressure of the bubbler 10 to about twice or more of the atmospheric pressure. Lower pressure is limited.

  In such a case, it is conceivable to change the supply amount of the target material by increasing the temperature of the bubbler 10 to adjust the vapor pressure P of the target material, but until the bubbler 10 is stabilized at the target temperature. Since it takes a long time, new problems such as the necessity of interrupting the supply of the target material to the consumer device occur.

  FIG. 5 shows a fourth embodiment of the present invention for solving such inconvenience. In this embodiment, a dilution gas introduction for injecting a dilution gas into the outlet 16 of the bubbler 10 is shown. One end of the line 40 is connected, and the other end of the dilution gas introduction line 40 is connected to the dilution gas source via the mass flow rate measuring device 41 and the flow rate adjusting valve 42 as in the third embodiment. The flow rate adjustment valve 42 is controlled by a signal from the pressure detection means 32 that detects the pressure on the inflow side of the sonic nozzle 1. In the figure, reference numeral 43 indicates a driving means for controlling the flow rate adjusting valve 42.

  According to this, the pressure on the primary side (bubbler internal pressure) of the sonic nozzle 1 is controlled by the flow control device 13, and the flow rate of the dilution gas is monitored by the pressure detection means 32, so that Stability can be confirmed.

That is, when the stop valves 18 and 19 are closed, the stop valve 20 is opened and the carrier gas is introduced, and the dilution gas introduction line 40 is introduced into the sonic nozzle 1 via the flow rate adjustment valve 42,
(Equation 8)
Qd + Qc = B × Pt × √ ((Qd × Mwd + Qc × Mwc) / (Qd + Qc))
(However, Qd and Mwd represent the mass flow rate and molar mass of the dilution gas introduced from the dilution gas introduction line, respectively)
It becomes.

Next, when the stop valves 18 and 19 are opened, and the stop valve 20 is closed to maintain the relationship of the above formula 8, the carrier gas is introduced into the bubbler 10.
(Equation 9)
Qd 1 + Qc + Qz = B × Pt × √ ((Qd 1 × Mwd + Qc × Mwc + Qz × Mwz) / (Qd 1 + Qc + Qz))
(However, Qd1 is the flow rate of the dilution gas introduced from the dilution gas introduction line after the bubbler 10 functions)
Can be expressed.

  Since the mass flow rate of the target material depends on the flow rate of the carrier gas based on the relationship of Equation 1, it is only necessary to change the carrier gas flow rate to obtain an arbitrary flow rate.

  In the fourth embodiment described above, the mass flow rate of the dilution gas is controlled. In the fifth embodiment shown in FIG. 6, the flow rate of the carrier gas is controlled by the pressure on the inflow side of the sonic nozzle 1. Control and adjust the dilution gas flow rate to keep the sum of the dilution gas flow rate and the carrier gas flow rate constant even when the state of the bubbler changes, such as a change in surface area of the target material or a temperature drop due to heat of vaporization. By keeping it, the supply amount of the target material can be kept constant.

  That is, dilution gas is supplied to the inflow side of the sonic nozzle 1 via the mass flow rate control means 13 ′, and the pressure controlled by the pressure on the inflow side of the mass flow rate measurement means 41 ′ and the sonic nozzle 1 is applied to the bubbler. An adjustment valve 42 'is connected, and the pressure on the inflow side of the sonic nozzle 1 is controlled by the pressure adjustment valve 42' so that the sonic nozzle 1 is choked.

  In this embodiment, the stop valves 18 and 19 are closed, and the stop valve 20 is opened to allow the carrier gas to flow into the sonic nozzle 1 at a predetermined pressure, and then the stop valves 18 and 19 are opened. The valve 20 is closed and the carrier gas is supplied to the bubbler at a predetermined flow rate, and the carrier gas containing the target material is discharged from the outlet 16.

  The dilution gas flow rate may be controlled by the mass flow rate control means 13 'so that the sum of the carrier gas flow rate and the dilution gas flow rate by the mass flow rate measurement means 41' becomes a predetermined flow rate.

It is obvious that the dilution gas may be the same as the carrier gas or may be a different type of gas.
On the other hand, when the dilution gas and the carrier gas are the same type of gas, the total (Qc + Qd1) of the carrier gas mass flow rate Qc and the dilution gas mass flow rate Qd1 from the dilution gas introduction line 40 is constant. Thus, by controlling the flow rate control device 13, the amount Qz of the target material contained in the mixed gas of the dilution gas and the carrier gas can be maintained constant.

  Furthermore, in the above-described embodiment, a single sonic nozzle is used. For example, when the embodiment shown in FIG. 2 is taken as an example, the throat portion is connected via the switching valve 50 as shown in FIG. Are connected to the target material outlet from the bubbler 10 via the switching valve 50, and the outlets of the monitoring devices 30, 30 'are connected. Is a flow path configuration communicating with the consumer device.

According to this embodiment, by selecting an appropriate one of the two sonic nozzles having different characteristics by the switching operation of the switching valve 50,
1) If the gas type of the carrier gas or dilution gas is changed, if there is a single sonic nozzle, the flow rate and pressure conditions are determined by the conditions of the sonic nozzle, but multiple sonic nozzles must be selected and switched. The pressure on the inflow side (primary side) of the sonic nozzle can be set to a predetermined pressure at a predetermined flow rate.
2) Also, even if the gas type is the same, if you want to change the relationship between flow rate and pressure, you can change the pressure and flow rate without switching the sonic nozzle from the flow path by switching to a sonic nozzle with different characteristics.
Such effects can be obtained.

  In other embodiments shown in FIGS. 3 to 6, a plurality of monitoring devices can be selectively connected via a switching valve so that a target material can be supplied to a consumer device via a sonic nozzle having different characteristics. It is a matter that can be easily implemented by those skilled in the art.

It is sectional drawing which shows an example of a sonic nozzle. It is a block diagram which shows the 1st Example of this invention. It is a block diagram which shows the 2nd Example of this invention. It is a block diagram which shows the 3rd Example of this invention. It is a block diagram which shows the 4th Example of this invention. It is a block diagram which shows the 5th Example of this invention. It is a block diagram which shows the 6th Example of this invention.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1, 1 'Sonic nozzle 1a Throat part 10 Bubbler 18-20 Stop valve 30, 30' Monitoring apparatus 35, 42 Flow control valve

Claims (7)

Using a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device, the inlet and the carrier gas source The mass flow control means and the first on-off valve are connected in order from the upstream side between the second on-off valve and the sonic nozzle in order from the upstream side between the outlet and the consumer device. And connecting the inflow side of the first on-off valve and the outflow side of the second on-off valve with a third on-off valve,
When the first and second on-off valves are closed and the third on-off valve is opened, the mass flow rate control means supplies a carrier gas having a predetermined flow rate at which the sonic nozzle is choked to the sonic nozzle. Then, the first and second on-off valves are opened, the third on-off valve is closed, and the carrier gas is supplied to the container at the predetermined flow rate. A material supply apparatus comprising a monitoring device that detects the content of the target material by monitoring the pressure on the inflow side of the sonic nozzle by discharging from the outlet. Using a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device, the inlet and the carrier gas source The mass flow control means and the first on-off valve are connected in order from the upstream side between the second on-off valve and the sonic nozzle in order from the upstream side between the outlet and the consumer device. And the inflow side of the first on-off valve and the outflow side of the second on-off valve are connected by a third on-off valve, and the inflow side of the sonic nozzle is diluted via mass flow control means. Connect the gas source,
With the first and second on-off valves closed and the third on-off valve opened, the sonic nozzle is choked by the carrier gas and the dilution gas from the dilution gas source. The carrier gas and the diluting gas are respectively flowed into the sonic nozzle at a predetermined flow rate, then the first and second on-off valves are opened, and the third on-off valve is closed to at the predetermined flow rate. A monitoring device that detects the content of the target material by supplying the carrier gas to the container, discharging the carrier gas containing the target material from the outlet, and monitoring the pressure on the inflow side of the sonic nozzle. Equipped material supply device. Using a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device, the inlet and the carrier gas source The mass flow control means and the first on-off valve are connected in order from the upstream side between the second on-off valve and the sonic nozzle in order from the upstream side between the outlet and the consumer device. And an inflow side of the first on-off valve and an outflow side of the second on-off valve are connected by a third on-off valve, and the mass flow rate measuring means from the upstream side to the inflow side of the sonic nozzle Connect the dilution gas source through the pressure regulating valve,
The pressure regulating valve controls the pressure on the inflow side of the sonic nozzle so that the sonic nozzle is choked with the first and second on-off valves closed and the third on-off valve opened. In addition, the carrier gas is allowed to flow into the sonic nozzle at a predetermined flow rate, the first and second on-off valves are then opened, and the third on-off valve is closed to attain the carrier gas at the predetermined flow rate. Is supplied to the container, the carrier gas containing the target material is discharged from the outlet, and the material supply provided with a monitoring device for detecting the content of the target material by monitoring the flow rate of the mass flow rate measuring means apparatus. Using a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device, the inlet and the carrier gas source The mass flow control means and the first on-off valve are connected in order from the upstream side between the second on-off valve and the sonic nozzle in order from the upstream side between the outlet and the consumer device. And an inflow side of the first on-off valve and an outflow side of the second on-off valve are connected by a third on-off valve, and the mass flow rate measuring means from the upstream side to the inflow side of the sonic nozzle Connect the dilution gas source through the pressure regulating valve,
The pressure regulating valve controls the pressure on the inflow side of the sonic nozzle so that the sonic nozzle is choked with the first and second on-off valves closed and the third on-off valve opened. In addition, the carrier gas is allowed to flow into the sonic nozzle at a predetermined flow rate, then the first and second on-off valves are opened, and the third on-off valve is closed to dilute the mass flow rate measuring means. A material supply apparatus for obtaining a desired content of the target material by controlling the carrier gas flow rate by the mass flow rate control means so that the sum of the gas flow rate and the carrier gas flow rate becomes a predetermined flow rate. Using a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device, the inlet and the carrier gas source The mass flow rate measuring means, the pressure regulating valve, and the first on-off valve are connected in order from the upstream side between them, and the second on-off in turn from the upstream side between the outlet and the consumer device A valve and a sonic nozzle, and further, an inflow side of the first on-off valve and an outflow side of the second on-off valve are connected by a third on-off valve,
When the first and second on-off valves are closed and the third on-off valve is opened, the carrier gas is supplied from the pressure adjusting valve to the carrier gas at a predetermined pressure at which the sonic nozzle is choked. Then, the first and second on-off valves are opened, the third on-off valve is closed, and the carrier gas is supplied to the container at the predetermined pressure, and the carrier gas containing the target material is supplied. A material supply device provided with a monitoring device that detects the content of the target material by discharging from the outlet and monitoring the flow rate of the mass flow rate measuring means. Using a bubbler comprising a container capable of storing a target material, an inlet connected to a carrier gas source, and an outlet for supplying a gas containing the target material to a consumer device, the inlet and the carrier gas source The mass flow rate measuring means, the pressure regulating valve, and the first on-off valve are connected in order from the upstream side between them, and the second on-off in turn from the upstream side between the outlet and the consumer device The valve and the sonic nozzle are connected, and the inflow side of the first on-off valve and the outflow side of the second on-off valve are connected by a third on-off valve, and mass flow control is performed on the inflow side of the sonic nozzle. Connecting a dilution gas source via means,
When the first and second on-off valves are closed and the third on-off valve is opened, the pressure adjusting valve causes the dilution gas to flow into the sonic nozzle so that the sonic nozzle is in a choke state. Side pressure is controlled, the carrier gas is allowed to flow into the sonic nozzle at a predetermined pressure, the first and second on-off valves are then opened, and the third on-off valve is closed to provide the predetermined The carrier gas is supplied to the container at a flow rate, the carrier gas containing the target material is discharged from the outlet, and the mass so that the sum of the carrier gas flow rate and the dilution gas flow rate by the mass flow rate measuring means becomes a predetermined flow rate. A material supply device that obtains a desired content of the target material by controlling the flow rate of the dilution gas with a flow rate control means.   7. The material supply apparatus according to claim 1, wherein a plurality of the sonic nozzles are selectably connected via a flow path switching unit, and the characteristics of the sonic nozzles are different from each other. Feeding device.

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