JP2020143315A - Solid material container - Google Patents

Abstract

To provide means for cooling a solid material container in an arbitrary shape without making large-sized an apparatus where the solid material container is arranged speedily in an easy manner with simple constitution.SOLUTION: A solid material container 1 is for use to vaporize and supply a solid material 2 housed therein, and has a cooling gas introduction line 10 for introducing the cooling gas into the solid material container 1 and a cooling gas delivery line 11 for delivering the cooling gas from the solid material container 1, and the cooling gas introduction line 10 has one or two or more cooling gas jet holes 21 for jetting the cooling gas into the solid material container.SELECTED DRAWING: Figure 1

Description

The present invention relates to a solid material container for supplying vapor of a semiconductor manufacturing material, for example, a solid material for thin film manufacturing.

With the progress of the semiconductor industry, it is required to utilize new semiconductor materials that will meet strict thin film requirements. These materials are used in a wide range of applications for thin film deposition and shape processing in semiconductor products.
For example, the solid 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, examples of this solid precursor include components that act as dopants for compound semiconductors and etching materials. Exemplary precursor materials include aluminum, barium, bismuth, chromium, cobalt, copper, gold, hafnium, indium, iridium, iron, lantern, lead, magnesium, molybdenum, nickel, niobium, platinum, ruthenium, silver and strontium. , Tantalum, titanium, tungsten, ruthenium and zirconium inorganic compounds and organic metal compounds.

Some of this new material is in solid form at standard temperature and pressure and cannot be supplied directly to the semiconductor deposition chamber for the manufacturing process.
Since these materials generally have a very high melting point and low vapor pressure, they must be heated, vaporized and sublimated inside the solid material container prior to feeding into the film formation chamber.

In order to supply a sufficient amount of steam for use in the semiconductor manufacturing process, it is required that there is sufficient heat input from the solid material container to the solid material during heating.
Since the heat of vaporization is taken away when the solid material is vaporized, the temperature of the surface of the solid material drops when the supply of the solid material vapor is started. Then, since the vapor pressure of the solid material decreases in the portion where the temperature has decreased, the amount of vapor derived from the solid material container decreases with the lapse of the supply time. Such fluctuations in the amount of steam derived are not preferable because they hinder uniform film formation in the semiconductor manufacturing process.
For this reason, solid material containers are generally designed to be heavy. This is because by increasing the weight, the amount of heat possessed by the solid material container itself increases, and it becomes possible to quickly supply the amount of heat to the surface of the solid material whose temperature has decreased due to vaporization.

By the way, the solid material container is arranged close to the semiconductor manufacturing apparatus in order to supply the vapor of the solid material to the semiconductor manufacturing apparatus. When the solid material inside the solid material container is consumed here, it is replaced with another solid material container filled with the solid material.
In order to replace the solid material container, it is necessary to cool the solid material container to around room temperature from the viewpoint of safety. Also, considering the progress of the semiconductor process, it is necessary to cool as quickly as possible.

Methods for cooling a solid material container are disclosed in, for example, Patent Document 1 and Patent Document 2.
Patent Document 1 discloses an apparatus for heating a solid material by introducing a heat medium (for example, heat medium oil) into a space provided outside a container in which the solid material is stored. When cooling the solid material container in this device, a cooling medium (for example, cooling water) is introduced in the space where the heat medium is introduced.
Patent Document 2 discloses an apparatus in which a water-cooled casing is arranged so as to cover the bottom surface, side surfaces, and the top surface of a container in which a solid material is stored, and the solid material container is cooled by introducing cooling water into the water-cooled casing. To do.

Special Table 2010-533790 Japanese Unexamined Patent Publication No. 2014-114491

The apparatus described in Patent Document 1 has a problem that the solid material becomes large in size because it is necessary to further arrange a space for introducing a refrigerant or a heat medium on the outside of the solid material container. The solid material itself has a large weight, but by arranging a space for introducing a refrigerant or a heat medium, the weight becomes even larger, which makes it difficult to replace or transport the container. Further, since the structure of the solid material container becomes complicated, the maintenance process becomes complicated and the manufacturing of the solid material container becomes difficult.
Furthermore, since it is necessary to alternately introduce the heat medium and the refrigerant into the same space, the heat medium remaining in the space may be mixed with the refrigerant to contaminate the refrigerant, or the refrigerant may be introduced into the heated space. There is a risk that the refrigerant will be heated rapidly and a large amount of refrigerant vapor will be generated.

In the apparatus described in Patent Document 2, it is necessary to form a water channel for circulating cooling water in the water-cooled casing, which complicates the apparatus. Further, it is necessary to further arrange the water-cooled casing on the outside of the solid material container, which causes a problem that the apparatus becomes large in size.

As described above, since the solid material container is heavy and has a large amount of heat, it takes time to cool it. In the device for cooling the solid material container from the outside as described in Patent Document 1 or Patent Document 2, the device for arranging the solid material container becomes large. Further, when the solid material container is removed and replaced with another solid material container, a step of taking out from the cooling device on the outside thereof is required, which complicates the replacement work. Further, since the cooling device provided on the outside of the solid material container needs to be arranged tightly on the outer periphery of the solid material to enhance heat conduction, it is manufactured according to the shape of the solid material container and is a solid having a different shape. Material containers cannot be attached.

Based on the above background, it is desired to develop a means for cooling a solid material container of an arbitrary shape quickly by a simple method and configuration without increasing the size of the device for arranging the solid material container.

The solid material container according to the present invention is
A solid material container for vaporizing and supplying the solid material stored inside.
A cooling gas introduction line that introduces cooling gas into the solid material container,
It has a cooling gas lead-out line for leading out the cooling gas from the solid material container, and has.
The cooling gas introduction line has one or more cooling gas ejection holes for ejecting the cooling gas into the solid material container.

The solid material container is connected by piping to equipment that uses the solid material (for example, a semiconductor manufacturing apparatus). When the solid material is supplied, the solid material container is heated by the heating means. The heating temperature is arbitrarily set according to the process of using the solid material, the physical properties of the solid material, and the like, and is, for example, 50 ° C. or higher and 300 ° C. or lower.
The heat input from the heated solid material container raises the temperature of the solid material inside the solid material container, and the solid material is vaporized or sublimated and led out as steam to the outside of the solid material container.
Here, the heating means of the solid material container may be a constant temperature bath, an oil bath, a mantle heater, a tape heater, a jacket heater, or a block heater.

After using the solid material, if the derivation of the vapor of the solid material is stopped and the solid material container is to be replaced, it is necessary to lower the temperature of the solid material container. The container temperature at the time of replacement is arbitrarily set depending on the safety viewpoint, the material of the container, and the like, and is, for example, a temperature of 15 ° C. or higher and 50 ° C. or lower.

In the solid material container (1 shown in FIG. 1) according to the present invention, cooling gas is introduced from the cooling gas introduction line 10 to cool the solid material container 1 from the inside, thereby rapidly cooling the container. Is possible. The cooling gas may be a gas having a temperature lower than the heating temperature of the solid material container 1, and may be, for example, a gas having a temperature of −50 ° C. or higher and 50 ° C. or lower. The cooling gas may be inert to the solid material, and the gas type may be, for example, nitrogen, argon, helium, hydrogen or dry air. The cooling gas may be pre-cooled. The cooling means is not particularly limited, and may be, for example, heat exchange with a refrigerant using a heat exchanger or cooling by a Peltier element. The refrigerant is not particularly limited and may be liquid nitrogen, water, oil, or fluoroline.
The arrows in the figure are arrows indicating the gas flow direction.

The introduction pressure of the cooling gas is not particularly limited, and can be, for example, 0.01 MPaA or more and 2 MPaA or less. The introduction pressure of the cooling gas can be determined according to the design of the solid material container 1, the physical properties of the solid material filled therein, and the like, and can be increased with the lapse of the introduction time of the cooling gas.

The flow rate for introducing the cooling gas can be arbitrarily determined, but a flow rate in which the space inside the solid material container 1 that is not filled with the solid material is replaced at least once per minute is preferable. If the flow rate is too small, the time required for cooling the container becomes long, and the efficiency decreases. On the other hand, if the flow rate is too large, the solid material is wound up inside the solid material container, which causes a problem in the piping and equipment in the subsequent stage. Considering the above, the flow rate of the cooling gas per minute is one or more times the volume of the portion of the internal space of the solid material container that is not filled with the solid material in the state before the start of use of the solid material container. The amount can be doubled or less. Considering the phenomenon that the solid material is rolled up by the gas flow of the cooling gas, it is preferably 1 time or more and 10 times or less, and more preferably 1 time or more and 5 times or less.

The introduced cooling gas is used for cooling the solid material container 1. The cooling gas whose temperature has risen due to heat exchange between the solid material container 1 and the solid material 2 inside the solid material container 1 is led out from the cooling gas lead-out line 11 to the outside of the solid material container 1.
The vapor of the solid material is accompanied by the cooling gas to be derived. The cooling gas lead-out line 11 may be heated by a heating means (not shown) in order to prevent the accompanying steam from condensing in the pipe. Examples of the heating means include, but are not limited to, a piping block heater, a jacket heater, a line heater, and the like.

The solid material container 1 is provided in advance with a carrier gas introduction line for introducing a carrier gas for accommodating the solid material and a solid material derivation line for deriving the vapor of the solid material accompanied by the carrier gas. It is common. In this case, the carrier gas introduction line or the solid material lead-out line can also serve as the cooling gas introduction line 10 or the cooling gas lead-out line 11.
For example, when the cooling gas lead-out line 11 also serves as a solid material lead-out line, the cooling gas lead-out line 11 may be branched and a sluice valve may be provided as shown in FIG.

The position of the opening of the cooling gas introduction line 10 is such that it is inserted inside the powdery or granular solid material (shown by A in FIG. 1) as the inside of the solid material 2 filled in the solid material container 1. It may be arranged in.
Further, as in the arrangement in FIG. 1, the opening may be arranged in the space (shown by B in FIG. 1) inside the solid material container 1 in which the solid material 2 is not arranged.

The cooling gas introduction line 10 is provided with one or more cooling gas ejection holes 21 for ejecting the cooling gas into the solid material container.
2 to 6 are enlarged views of the tip portion of the cooling gas lead-out line 10.
When there is one cooling gas ejection hole 21, the cooling gas ejection hole 21a can be opened at the tip of the columnar cooling gas introduction line 10 (the portion corresponding to the bottom of the column) as shown in FIG. As shown in FIG. 3, a cooling gas ejection hole 21b may be opened on the side surface of the columnar cooling gas introduction line 10.
When two or more cooling gas ejection holes 21 are provided, a plurality of cooling gas ejection holes 21c may be provided on the side surface of the cooling gas introduction line 10 as shown in FIG. 4, and the cooling gas may be ejected in a shower shape. ..

When there is one cooling gas ejection hole 21, the ejection area from which the cooling gas is ejected can be increased, so that the flow velocity of the cooling gas can be reduced, and the scattering of the solid material due to the spraying of the cooling gas can be suppressed. ..
When the number of the cooling gas ejection holes 21 is two or more, it is possible to disperse the ejection direction of the cooling gas. Therefore, it is possible to prevent the solid material from being unevenly distributed by blowing gas onto the solid material from a specific direction. It will be possible.

By introducing the cooling gas into the solid material container 1 in this way, the solid material container 1 can be cooled from the inside of the solid material container 1, so that the container can be cooled in a shorter time. be able to.

The cooling gas ejection hole 21 of the solid material container 1 according to the present invention is arranged above the surface of the solid material 2 housed inside the solid material container 1, and the cooling gas is a solid material in the cooling gas ejection hole 21. It may be formed so as to be ejected in the horizontal direction or in the upward direction above the horizontal direction in the space inside the container 1 in which the solid material 2 is not stored.
The cooling gas introduction line 10 of the solid material container 1 according to the present invention is arranged so as to be vertically inserted into the inside of the solid material container 1 from the upper part of the solid material container 1, and two or more cooling gas ejection holes 21. However, it may be arranged in the vertical direction on the side surface of the cooling gas introduction line.

When the ejection direction of the cooling gas is the direction of the solid material 2, the solid material inside the solid material container 1 is blown up by the ejection of the cooling gas, and the equipment such as the valve and the pressure gauge connected to the solid material container is blocked. There is a child that leaks or a large amount of powdery substance flows into the subsequent pipe and blocks the pipe.
The cooling gas ejection hole 21 of the solid material container 1 according to the present invention is opened in a space (the space shown by B in FIG. 1) in which the solid material 2 is not stored, and the cooling gas ejection direction is horizontal or horizontal. It is arranged so as to be upward from the direction.

For example, in FIG. 3, a cooling gas ejection hole 21b is arranged above the solid material 2 on the side surface of the cooling gas introduction line 10 inserted in the direction perpendicular to the solid material container 1, and the cooling gas ejection hole 21b is arranged above the solid material 2. The gas derived from 21b is ejected horizontally with respect to the solid material container 1.
For example, in FIG. 4, a plurality of cooling gas ejection holes 21c are arranged in the vertical direction on the side surface of the cooling gas introduction line 10 inserted in the direction perpendicular to the solid material container 1, and are derived from the cooling gas ejection holes 21c. The gas is ejected horizontally with respect to the solid material container 1. The cooling gas ejection holes 21c may be arranged in one row vertically in the vertical direction, or may be arranged in a plurality of rows as shown in FIG.
With this structure, it is possible to suppress the phenomenon that the flow of the cooling gas directly blows onto the solid material 2 and the solid material soars.

The cooling gas introduction line 10 of the solid material container 1 according to the present invention is vertically inserted into the inside of the solid material container 1 from the upper part of the solid material container 1, and then L-shaped at the end on the solid material container 1 side. It can also be characterized in that the cooling gas ejection hole 21 is opened in the solid material container 1 in the horizontal direction by being curved in a shape.

For example, in FIG. 5, the cooling gas introduction line 10 inserted in the direction perpendicular to the solid material is curved at L at the end on the solid material container 1 side, and the cooling gas ejection hole 21d is directed in the horizontal direction. Since it is open, the cooling gas ejection hole ejects in the horizontal direction.
As another example, in FIG. 6, the cooling gas introduction line 10 inserted in the direction perpendicular to the solid material is curved at L at the end on the solid material container 1 side, and the cooling gas ejection hole 21d is inclined. It opens at an angle, and the cooling gas is ejected upward from the horizontal direction.
As yet another example, in FIG. 7, the cooling gas introduction line 10 inserted in the direction perpendicular to the solid material is curved in a U shape at the end on the solid material container 1 side, and the cooling gas ejection hole 21e is formed. It opens upward.
By curving the cooling gas introduction line 10 inside the solid material container 1 in this way, the ejection direction of the cooling gas is adjusted and the cooling gas is prevented from directly spraying on the solid material, thereby suppressing the soaring of the solid material. It becomes possible to do.

In the solid material container 1 according to the present invention, the cold trap 30 for cooling the cooling gas and the cooling gas derived from the cold trap 30 are reintroduced into the solid material container 1 at the subsequent stage of the cooling gas outlet pipe 11. It may further have a cooling gas return line 31.
After cooling the solid material container 1, the cooling gas is led out from the cooling gas lead-out line 11. Here, the derived cooling gas is accompanied by vaporized vapor of the solid material. The vapor of a solid material may condense and precipitate due to a decrease in temperature, which may cause clogging of pipes and generation of particles. Therefore, a cold trap 30 is provided, and the cold trap 30 is taken out from the solid material container and then cooled. As a result, the solid material contained in the cooling gas is condensed and remains in the cold trap. By reducing the content of the solid material contained in the cooling gas in this way, it is possible to suppress the phenomenon that the solid material is deposited in the piping at the subsequent stage of the solid material container 1 and is thereby blocked.
The cooling gas that has been cooled and the solid material has been reduced may be introduced again as the cooling gas into the solid material container. With such a configuration, the cooling gas can be reused and the cold heat of the cold trap can be used for cooling the solid material container, so that energy-efficient cooling can be performed. ..

The cold trap is cooled by a cooling medium such as liquid nitrogen or dry ice. When a cooling gas accompanied by vapor of a solid material is introduced there, the solid material in a gaseous state condenses and becomes a liquid or solid state and remains in a cold trap, and the cooling gas is cold in a state where the temperature is lowered. Derived from the trap.
The cooling gas derived from the cold trap is used as it is or by adding a new cooling gas and used again as the cooling gas.

It is a figure which shows the structural example of a solid material container. It is an enlarged view of the example of the structure of the cooling gas introduction line of a solid material container. It is an enlarged view of the example of the structure of the cooling gas introduction line of a solid material container. It is an enlarged view of the example of the structure of the cooling gas introduction line of a solid material container. It is an enlarged view of the example of the structure of the cooling gas introduction line of a solid material container. It is an enlarged view of the example of the structure of the cooling gas introduction line of a solid material container. It is a figure which shows the structural example of a solid material container. It is a figure which shows the structural example of a solid material container.

(Example)
The solid material container 1 shown in FIG. 1 to which the cooling gas introduction line 10 having the shape shown in FIG. 2, FIG. 4 or FIG. 6 was attached was manufactured, and the cooling state after heating was confirmed.
The solid material container 1 was a stainless steel solid material container (container weight 20 kg) having an internal volume of 18 L and a wall thickness of 0.28 cm. As a solid material, 10 kg of alumina was introduced therein and heated in a constant temperature bath so that the temperature of the outer wall surface of the container became 250 ° C. or 150 ° C. After the temperature of the outer wall surface of the container reached 250 ° C. or 150 ° C., the container was kept for 5 hours. After that, the heating by the constant temperature bath was stopped, and the cooling gas was introduced from the cooling gas introduction line 10. The cooling gas was nitrogen gas having a temperature of 20 ° C. and a flow rate of 15 SLM. Since the volume of the portion of the internal space of the solid material container that is not filled with the solid material in the state before the start of use is 8 L, the flow rate of the cooling gas per minute is 1.9 times the volume.

(Example 1)
In the cooling gas introduction line 10 having the cooling gas ejection hole 21b having the shape shown in FIG. 3, the pipe diameter was 1/2 inch and the opening area was 0.71 cm ² . The opening was arranged 5 mm above the tip of the pipe.

(Example 2)
In the cooling gas introduction line 10 having the cooling gas ejection holes 21c having the shape shown in FIG. 4, the diameter of each cooling gas ejection hole 21c was 1 mm, and the number of the cooling gas ejection holes 21 was 32. Eight cooling gas ejection holes 21 of 32 were arranged in the vertical direction at 5 mm intervals, and four rows in which the eight cooling gas ejection holes 21 were arranged vertically were arranged on the side wall surface of the cooling gas introduction line. ..

(Example 3)
In the cooling gas introduction line 10 having the cooling gas ejection hole 21e having the shape shown in FIG. 6, the cooling gas introduction line 10 is inserted into the solid material container 1 and then 70% of the total height of the solid material container 1 from the bottom. At the height position of, it was curved in an L shape. Since the initial filling height of the solid material is 50% of the height of the entire solid material container 1 from the bottom, the L-shaped curved portion is located higher than the filling height of the solid material. .. The tip of the curved pipe was cut at an oblique direction of 45 ° C., and the cut end was used as a cooling gas ejection hole 21e.

In Examples 1, 2 and 3, when the heating temperature of the solid material container is 250 ° C., the time required from the start of introduction of the cooling gas to the temperature of the outer wall surface of the solid material container 1 reaching 50 ° C. is measured. As a result, the required time was 800 minutes in each case.
In the case of the shape shown in FIG. 6 (Example 3), Table 1 shows a graph showing the transition of the temperature of the outer wall surface of the container. When the cooling gas shown by the dotted line in Table 1 is not introduced, it takes a long time (1800 minutes or more) to cool the container outer wall temperature to 50 ° C. or less, but when the cooling gas shown by the solid line is introduced, cooling is performed. The time has been greatly reduced. From this, it can be said that the container cooling effect by introducing the cooling gas was sufficiently obtained.
The temperature of the outer wall surface of the container was measured by using a thermocouple on the surface of the central side surface of the cylindrical solid material container 1.

Similarly, Table 2 shows a graph showing the transition of the container outer wall surface temperature when the heating temperature of the solid material container is 150 ° C. in Example 3.
When the cooling gas shown by the dotted line in Table 2 is not introduced, it takes a long time (900 minutes or more) to cool the container outer wall surface temperature to 50 ° C., but when the cooling gas shown by the solid line is introduced, it takes a long time. The cooling time was significantly reduced (about 480 minutes). From this, it can be said that the container cooling effect by introducing the cooling gas was sufficiently obtained.

Next, as shown in FIG. 6, a case where the cooling gas introduction line 11 is curved in an L shape so that the cooling gas blowing direction is the horizontal direction (Example 3) and a case where the cooling gas introduction line 11 is not curved (implementation). In Example 1), it was confirmed whether or not the solid material was soared inside the solid material container 1. Although the height of the cooling gas ejection hole 21 was the same in Example 1 and Example 3, the cooling gas ejection direction was horizontal in Example 3, whereas in Example 1, the cooling gas ejection direction was horizontal. Is downward and vertical.
The type and flow rate of the cooling gas during cooling were the same as described above, and the presence or absence of soaring of the solid material was confirmed by the presence or absence of particles detected by the particle counter provided in the cooling gas lead-out line 11.
In Example 1, the amount of detected particles having a diameter of 0.1 μm or more was 1000 particles per 1 cf. On the other hand, in the case of Example 3, the amount of detected particles having a diameter of 0.1 μm or more was 10 or less per 1 cf. From this, it is more likely that the cooling gas is ejected horizontally or upward than the horizontal direction with respect to the solid material container 1 than when the cooling gas is ejected in the direction of directly hitting the surface of the solid material. It was confirmed that it was possible to suppress the accompanying particles to the subsequent stage.

1. 1. Solid material container 2. Solid material 10. Cooling gas introduction line 11. Cooling gas lead-out line 21. Cooling gas vent

When the ejection direction of the cooling gas is the direction of the solid material 2, the solid material inside the solid material container 1 is blown up by the ejection of the cooling gas, and the equipment such as the valve and the pressure gauge connected to the solid material container is blocked. , or to leak, there likely to create a large amount of powdery material or to block the piping flows into the downstream pipe.
The cooling gas ejection hole 21 of the solid material container 1 according to the present invention is opened in a space (the space shown by B in FIG. 1) in which the solid material 2 is not stored, and the cooling gas ejection direction is horizontal or horizontal. It is arranged so as to be upward from the direction.

(Example)
The solid material container 1 shown in FIG. 1 equipped with the cooling gas introduction line 10 having the shape shown in FIG. 3 , FIG. 4 or FIG. 6 was manufactured, and the cooling state after heating was confirmed.
The solid material container 1 was a stainless steel solid material container (container weight 20 kg) having an internal volume of 18 L and a wall thickness of 0.28 cm. As a solid material, 10 kg of alumina was introduced therein and heated in a constant temperature bath so that the temperature of the outer wall surface of the container became 250 ° C. or 150 ° C. After the temperature of the outer wall surface of the container reached 250 ° C. or 150 ° C., the container was kept for 5 hours. After that, the heating by the constant temperature bath was stopped, and the cooling gas was introduced from the cooling gas introduction line 10. The cooling gas was nitrogen gas having a temperature of 20 ° C. and a flow rate of 15 SLM. Since the volume of the portion of the internal space of the solid material container that is not filled with the solid material in the state before the start of use is 8 L, the flow rate of the cooling gas per minute is 1.9 times the volume.

Then, when the upper direction than the blowing direction horizontal direction of the cooling gas to cooling gas inlet line 1 0 is bent in an L shape as shown in FIG. 6 (Example 3), the cooling gas inlet line 1 0 In the case where the gas was not curved ( Comparative Example 1), it was confirmed whether or not the solid material was soared inside the solid material container 1. In Comparative Example 1 and Example 3, the height of the cooling gas ejection hole 21 was the same, but in the case of Example 3, the cooling gas ejection direction was higher than the horizontal direction. In the case of Comparative Example 1, the direction is downward and vertical.
The type and flow rate of the cooling gas during cooling were the same as described above, and the presence or absence of soaring of the solid material was confirmed by the presence or absence of particles detected by the particle counter provided in the cooling gas lead-out line 11.
In Comparative Example 1, the amount of detected particles having a diameter of 0.1 μm or more was 1000 particles per 1 cf. On the other hand, in the case of Example 3, the amount of detected particles having a diameter of 0.1 μm or more was 10 or less per 1 cf. From this, it is more likely that the cooling gas is ejected horizontally or upward than the horizontal direction with respect to the solid material container 1 than when the cooling gas is ejected in the direction of directly hitting the surface of the solid material. It was confirmed that it was possible to suppress the accompanying particles to the subsequent stage.

In the solid material container 1 according to the present invention, the cold trap 30 for cooling the cooling gas and the cooling gas derived from the cold trap 30 are reintroduced into the solid material container 1 after the cooling gas lead-out line 11. It may further have a cooling gas return line 31.
The cooling gas is led out from the cooling gas lead-out line 11 after cooling the solid material container 1. Here, the derived cooling gas is accompanied by vaporized vapor of the solid material. The vapor of a solid material may condense and precipitate due to a decrease in temperature, which may cause clogging of pipes and generation of particles. Therefore, a cold trap 30 is provided, and the cold trap 30 is taken out from the solid material container and then cooled. As a result, the solid material contained in the cooling gas is condensed and remains in the cold trap. By reducing the content of the solid material contained in the cooling gas in this way, it is possible to suppress the phenomenon that the solid material is deposited in the piping at the subsequent stage of the solid material container 1 and is thereby blocked.
The cooling gas that has been cooled and the solid material has been reduced may be introduced again as the cooling gas into the solid material container. With such a configuration, the cooling gas can be reused and the cold heat of the cold trap can be used for cooling the solid material container, so that energy-efficient cooling can be performed. ..

Claims (9)

A solid material container for vaporizing and supplying the solid material stored inside.
A cooling gas introduction line that introduces cooling gas into the solid material container,
It has a cooling gas lead-out line for leading out the cooling gas from the solid material container, and has.
The cooling gas introduction line is a solid material container having one or more cooling gas ejection holes for ejecting the cooling gas into the solid material container. The cooling gas vent is arranged above the surface of the solid material housed inside the solid material container.
The cooling gas ejection hole is formed so that the cooling gas is ejected horizontally or above the horizontal direction into a space inside the solid material container in which the solid material is not stored. The solid material container according to claim 1. The cooling gas introduction line is arranged so as to be vertically inserted into the inside of the solid material container from the upper part of the solid material container.
The solid material container according to claim 1 or 2, wherein two or more of the cooling gas ejection holes are arranged in the vertical direction on the side surface of the cooling gas introduction line. The cooling gas introduction line is vertically inserted into the inside of the solid material container from the upper part of the solid material container, and then curved in an L shape at the end on the solid material container side to form the cooling gas. The solid material container according to claim 1 or 2, wherein the ejection hole is opened so as to face the solid material container in the horizontal direction. The flow rate of the cooling gas per minute when ejected from the cooling gas ejection hole is not filled with the solid material in the internal space of the solid material container in the state before the start of use of the solid material container. The solid material container according to any one of claims 1 to 4, further comprising a cooling gas flow rate adjusting mechanism for adjusting the flow rate of the cooling gas so as to be 1 times or more and 30 times or less the volume of the portion. The solid material container according to any one of claims 1 to 5, wherein the temperature of the cooling gas is −50 ° C. or higher and 50 ° C. or lower. The method according to any one of claims 1 to 6, further comprising a gas cooling mechanism for cooling the temperature of the cooling gas introduced into the solid material container to a temperature of −50 ° C. or higher and 50 ° C. or lower. Solid material container. The solid material container according to any one of claims 1 to 7, wherein the cooling gas is at least one gas selected from the group consisting of nitrogen gas, helium gas, argon gas, and hydrogen gas. .. Claim 1 further includes a cold trap for cooling the cooling gas and a cooling gas return line for reintroducing the cooling gas derived from the cold trap into the solid material container after the cooling gas outlet pipe. The solid material container according to any one of claims 8.

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