JP5242140B2 - Solid raw material supply method and apparatus - Google Patents

Description

  The present invention relates to a solid raw material supply method and apparatus, and more specifically, supplies a solid powder raw material having a vapor pressure at a temperature of normal temperature or higher to a supply destination such as a reaction chamber at a constant concentration accompanied with a gaseous carrier gas at normal temperature. The present invention relates to a solid raw material supply method and apparatus.

  In a semiconductor manufacturing factory or the like, supplying a solid raw material quantitatively and constantly to a reaction chamber or the like is one of important elemental technologies. This elemental technology is also an extremely important elemental technology for the standard gas generation method for the analysis of trace hazardous substances. In these fields, solid substances with vapor pressure can be fixed at room temperature or by heating. Various devices have been devised to supply at a concentration.

  For example, in a semiconductor manufacturing apparatus, specifically an apparatus that uses an organic metal as a raw material and forms an oxide thin film, a solid raw material is used to stably supply a solid organic metal to a CVD chamber with good reproducibility. A method of adsorbing to a porous adsorbent granule, placing the adsorbent granule after adsorbing the raw material in a high temperature atmosphere, and allowing a carrier gas to pass through the granule (see, for example, Patent Document 1). The solid organic metal supported on the surface of a large number of through holes penetrating from one end surface of the organic metal support supporting the solid organic metal to the other end surface is supported in an atmosphere at a temperature at which the solid organic metal sublimates. A method of supplying a raw material gas obtained by mixing a solid organic metal into a carrier gas by passing the carrier gas through each through hole (for example, see Patent Document 2) has been proposed.

  On the other hand, as a means for supplying a solid organic metal to the CVD chamber stably and with good reproducibility without using an adsorbent or a carrier, the solid organic metal mixed with an inert filler is placed in the container at room temperature. In a method of supplying a solid organic metal, which is filled and passed through a carrier gas into the container to obtain a carrier gas mixed with an organic metal, the shape of the container is a column-shaped straight pipe, and the container is formed at either the upper or lower end of the container. There has also been proposed a solid organic metal supply device in which a carrier gas introduction port is provided and a carrier gas outlet port in which an organic metal is mixed at the other end is provided (for example, see Patent Document 3).

As a standard gas generation means for analyzing trace hazardous substances, a standard substance is introduced into a small container equipped with capillaries as a method of generating a solid substance at a constant concentration at room temperature, and the small container is placed in a thermostatic chamber. The diluting gas that is disposed and heated through the heat exchange circuit in the thermostatic chamber is guided to the periphery of the small container, thereby evaporating the sample substance in the small container and containing it at a predetermined low concentration A method has been proposed (see, for example, Patent Document 4). In this method, when the sample substance is a solid substance at room temperature, it is dissolved in a solvent and introduced into the small container, and then the solvent is removed by heating and a thin film of the sample substance is formed on the inner wall of the small container. After this, the thin film sample material is evaporated.
JP-A-9-40489 JP 2003-273093 A Japanese Patent Application Laid-Open No. 6-151311 JP 2002-273202 A

  In the methods described in Patent Documents 1 and 2, when the solid raw material is adsorbed on the porous adsorbent granules or supported on the support, both methods dissolve the solid raw material in the solvent. Thereafter, a method of mixing with the adsorbent granules and the carrier to volatilize and remove only the solvent is employed. However, in these methods, when the volatilization and removal of the solvent is insufficient, it is possible to send the unnecessary solvent to the reaction chamber at the same time as the solid raw material, which may cause deterioration of the product quality. Is porous, there is a high possibility that a trace amount of solvent remains. Furthermore, it is difficult to apply to a hardly soluble solid, and the method of Patent Document 2 has a problem that it is necessary to mold the carrier into a complicated shape, which makes it difficult to process.

  In addition, the method described in Patent Document 3 simply mixes the powdered solid raw material and the filler, so that the uniformity of the mixture is improved and the contact area between the solid and the carrier gas is highly accurate. Therefore, there is a problem that the supply amount of the solid raw material cannot be made constant with high accuracy.

  Further, in the method described in Patent Document 4, since the solid raw material is dissolved in a solvent, it is difficult to apply the solvent to the problem of residual solvent and a hardly soluble solid, and since the solid raw material is used as a thin film, Another problem is that it is not suitable for stable supply.

  Therefore, the present invention provides a solid raw material supply method and apparatus capable of supplying a solid substance having a vapor pressure by heating at room temperature or with high accuracy and for a long period of time using an apparatus having a very simple structure. It is aimed.

To achieve the above object, the solid raw material supply method of the present invention is a solid raw material supply method in which a solid raw material is heated to evaporate, and the evaporated raw material gas is supplied with a carrier gas. The inner surface is the same as the outer surface shape of the solid raw material, in which the cross-sectional area is a constant cross-sectional area, the upper surface is a horizontal plane, there is no gap between the particles, and the molded solid raw material is formed into a uniform and dense structure. The top of the solid material is fixed from the upper opening edge of the evaporation container by filling the inside of the evaporation container having an open shape and urging the tray on which the solid material is placed by the urging means. The evaporation container is sealed in a mixing container that mixes the raw material gas evaporated from the solid raw material with the carrier gas, and the atmospheric temperature in the mixing container is maintained at a preset temperature. Pressure in the mixing vessel And flow rate introduced preset carrier gas was adjusted to a pressure and flow rate, supplying a carrier gas to the evaporated raw material gas was entrained by mixing the carrier gas from the upper surface to the supply destination derived from the mixing vessel It is characterized by doing.

Furthermore, the method of the solid material supply present invention, prior Symbol solid material is xenon difluoride, xenon tetrafluoride is characterized in that it is any one of xenon hexafluoride.

Further, the solid raw material supply apparatus of the present invention is a solid raw material supply apparatus that heats and evaporates the solid raw material and supplies the evaporated raw material gas with the carrier gas. The evaporation container is filled with a solid material molded into a uniform and dense structure with no gaps between the particles, the mixing container in which the evaporation container is sealed, and the carrier gas is introduced into the mixing container Carrier gas introduction path, pressure adjusting means and flow rate adjusting means provided in the carrier gas introduction path, temperature adjusting means for adjusting the atmospheric temperature in the mixing container, and the evaporation container in the mixing container An entrained gas deriving path for deriving an entrained gas obtained by mixing the source gas evaporated from the solid source and the carrier gas from the mixing container and supplying the entrained gas to the supply destination. , The inner surface shape is formed the same as the outer surface shape of the molded solid material, and a pan for placing a solid material after the molding, the upper surface of the solid material to urge the pan upward And an urging means for holding the evaporation container at a certain distance from the upper opening edge of the evaporation container .

Furthermore, the solid material supply device of the present invention, prior Symbol solid material is xenon difluoride, xenon tetrafluoride is characterized in that it is any one of xenon hexafluoride.

  According to the present invention, the solid raw material has a shape with a constant cross-sectional area and a top surface that is a horizontal plane, no gaps between particles, and is formed into a uniform and dense structure. By uniformly evaporating from the upper surface and entraining it with the carrier gas whose pressure and flow rate are adjusted, it can be supplied to the supply destination at a stable concentration. In particular, since the cross section of the solid raw material has a constant cross-sectional area, the amount of evaporation from the top surface can be kept constant even if the amount decreases with evaporation.

  In addition, by keeping the distance from the upper opening edge of the evaporation container to the upper surface of the solid raw material constant, the contact state between the upper surface of the solid raw material and the gas in the mixing container can be kept constant, and the evaporation amount of the solid raw material Can be more reliably maintained constant. Furthermore, since no solvent is used, the entrained gas is not contaminated by the solvent, and it can be applied to a hardly soluble solid material.

  FIG. 1 is a system diagram showing an embodiment of the solid material supply apparatus of the present invention, and FIG. 2 is a perspective view showing an embodiment of the evaporation container. The solid raw material supply apparatus includes an evaporation container 12 filled with a solid raw material 11, a mixing container 13 that houses the evaporation container 12, a carrier gas introduction path 14 that introduces a carrier gas into the mixing container 13, and a mixing container. 13 is provided with an entrained gas deriving path 15 for deriving from the mixing container 13 an entrained gas in which the carrier gas and the source gas evaporated from the solid material are mixed.

  The solid material 11 has a vapor pressure at room temperature or under heating, and is intended for a solid material for semiconductor production such as xenon fluoride such as xenon difluoride, xenon tetrafluoride, xenon hexafluoride, for example. be able to. In order to obtain a uniform and constant evaporation amount, the solid raw material 11 is formed into a uniform and dense structure by using a molding machine so that the powder has a cross-sectional area with a constant cross-sectional area and a top surface with a horizontal plane, no gaps between particles. Used in the state of the molded product. The cross-sectional shape is arbitrary, but usually circular or square is preferable, and even when the volume (height) is reduced by evaporation by setting the upper surface to be the evaporation surface as a horizontal plane and the cross-section as a constant cross-sectional area, A uniform and constant evaporation amount can be obtained. The height of the molded product can be appropriately set in consideration of the evaporation amount and the supply time. Although the pressure applied at the time of molding varies depending on the properties of the solid raw material 11, it is usually preferably set to 10 MPa or more in order to obtain a uniform and dense state with no gaps.

  The evaporation container 12 has an inner surface shape identical to the shape of the outer surface of the molded product of the solid raw material 11, and is an open top cylinder. For example, if the molded product is cylindrical, the evaporation container 12 has a diameter of the molded product. A cylinder with a corresponding inner diameter is used. The height of the evaporation container is set to a height at which the upper surface of the molded product does not protrude upward from the upper opening edge when the molded product of the solid raw material 11 is filled. It is preferable to set the height to be several times higher than the height. In addition, the bottom part of the evaporation container 12 may be opened and may be closed with a bottom plate.

  Also, at the lower part of the evaporation container 12 shown in the present embodiment, a tray 16 on which a molded product of the solid raw material 11 is placed, and a biasing means 17 such as a coil spring that biases the tray 16 upward are provided. ing. The tray 16 is a thin plate having a shape on which a molded product of the solid raw material 11 can be placed and can move in the evaporation container 12 in the container axial direction. The biasing means 17 has a length of the evaporation container. When the solid raw material 11 is placed on the receiving tray 16 with a height of less than 12, it elastically shrinks with the load of the solid raw material 11 and the receiving tray 16 and elastically stretches when the solid raw material 11 evaporates and the load decreases. A material having elasticity that holds the upper surface evaporation surface of the solid raw material 11 at a certain distance from the upper opening edge of the evaporation container 12 is used.

  The mixing container 13 has an internal shape capable of accommodating the evaporation container 12, and is formed of a container main body 18 formed of a bottomed cylindrical body having an opening at the top, and a lid body 19 that seals the opening, The evaporation container 12 is taken in and out by removing the lid 19. The shape of the mixing container 13 is not particularly limited, but a cylindrical shape and a rectangular tube shape are preferable in consideration of manufacturability. The volume of the mixing vessel 13 can be arbitrarily set according to conditions such as the evaporation amount of the solid raw material 11 and the flow rate of the carrier gas. However, if the volume is too small, the gas flow in the mixing vessel 13 is likely to be disturbed. If the evaporation container 12 and the mixing container 13 are both cylindrical, the diameter of the mixing container 13 is about 2 to 4 times the height of the evaporation container 12 and the height is high. About 3 to 5 times is appropriate.

  The carrier gas introduction path 14 and the accompanying gas lead-out path 15 are connected to the upper part of the side wall of the container body 18. The carrier gas introduction path 14 and the accompanying gas lead-out path 15 are arranged so that the axes of the paths 14 and 15 are aligned with each other at positions facing the container body 18 in order to make the gas flow in the container body 18 smooth. It is preferable to provide the carrier gas introduced from the carrier gas introduction path 14 at a position where the carrier gas does not directly hit the evaporation container 12.

  Further, the container body 18 of the mixing container 13 is embedded in the heat transfer means 20 formed of an aluminum block or the like including the connection part of the carrier gas introduction path 14 and the accompanying gas outlet path 15. The heat transfer means 20 is for efficiently and uniformly heating the entire container body 18. Inside the heat transfer means 20, there are a heating means 21 such as a sheathed heater and a temperature measurement means 22 such as a thermocouple. Is provided. The heat transfer means 20 only needs to be able to heat and keep the mixing container 13 at a predetermined temperature, and a hot water bath or an oil bath can be used. The heat transfer means 20 is formed of a solid such as metal. If it is, it is preferable to form it so as to be in close contact with the outer surface of the mixing container 13 as much as possible.

  The heating means 21 and the temperature measuring means 22 are connected to a temperature adjusting means 23 such as an electronic temperature controller provided outside the heat transfer means 20. The temperature adjusting means 23 is a temperature measured by the temperature measuring means 22. The heating means 21 is controlled according to the difference between the preset temperature set in advance and the temperature measured by the temperature measuring means 22 according to the signal. For example, when the measured temperature is higher than the set temperature using a relay or the like In the mixing container 13 via the heat transfer means 20, the power supply of the heating means 21 is turned off, and when the measured temperature is lower than the set temperature, the power supply of the heating means 21 is turned on. Can be controlled from room temperature to a temperature of about 100 ° C.

  The carrier gas introduction path 14 supplies an inert gas such as nitrogen or argon or hydrogen as a carrier gas from a gas supply source 24, and includes a pressure adjusting means 25 for adjusting the pressure of the carrier gas, and a flow rate. Is provided with a flow rate adjusting means 26 and an introduction valve 27. The accompanying gas lead-out path 15 is connected to a supply destination (not shown) via a lead-out valve 28.

  As the gas supply source 24, a cylinder filled with a carrier gas may be used, or a gas used in the facility in the site may be drawn in and used. A general pressure regulator corresponding to the pressure on the primary side and the secondary side can be used for the pressure adjusting means 25, and the flow rate adjusting means 26 can be used according to the pressure, the flow rate adjustment range, and the flow rate adjustment accuracy. A commonly used mass flow controller can be used. For the introduction valves 27 and 28, ball valves, diaphragm valves, or the like can be used.

  For each member including the evaporation container 12 and the mixing container 13, a material that does not have reactivity with the solid raw material 11, the evaporated raw material gas, and the carrier gas may be selected according to the type of the solid raw material 11. It can be formed of stainless steel or aluminum alloy.

  In order to supply a solid raw material gas having a constant concentration to a use facility at a constant flow rate using the solid raw material supply apparatus thus formed, first, the solid raw material 11 is formed into a shape corresponding to the evaporation container 12. This molding can be performed using a mold having a predetermined shape and a press machine, and a predetermined pressure, preferably 10 MPa or more, is applied by the press machine in a state where a predetermined amount of the powder of the solid raw material 11 is put into the mold. A molded product having a predetermined shape can be produced by compression molding with the above. As described above, the molded product has a uniform and dense structure with a constant cross-sectional area, a horizontal surface at the top, no gaps between particles. The outer surface shape of the molded product is equal to the inner surface shape of the evaporation container 12, and the height of the molded product may be in a range that can be accommodated in the evaporation container 12, and when the urging means is provided, When the molded product is placed on the receiving pan 16, the upper surface of the molded product is set to a height that does not exceed the opening edge of the evaporation container 12.

  After filling the molded solid material 11 into the evaporation container 12, the evaporation container 12 is installed at a predetermined position in the mixing container 13 from which the lid 19 is removed, and the mixing container 13 is sealed by attaching the lid 19. Thus, the evaporation container 12 filled with the solid raw material 11 is sealed in the mixing container 13. Next, the temperature adjustment means 23 is set to a temperature corresponding to the vapor pressure, supply concentration, etc. of the solid raw material 11 to adjust the ambient temperature in the mixing container 13 to a predetermined constant temperature.

  In addition, the introduction valve 27 of the carrier gas introduction path 14 and the outlet valve 28 of the accompanying gas lead-out path 15 are opened to introduce the carrier gas into the mixing container 13 from the carrier gas introduction path 14, and the solid raw material in the mixing container 13. The entrained gas in which the source gas evaporated from 11 and the carrier gas are mixed is led out to the accompanying gas deriving path 15 and discharged from a purge path (not shown). Then, the pressure adjusting unit 25 and the flow rate adjusting unit 26 adjust the pressure and flow rate of the carrier gas to preset pressures and flow rates, and when the source concentration of the accompanying gas led out to the accompanying gas lead-out path 15 becomes stable. Supply of the accompanying gas from the accompanying gas outlet path 15 to the supply destination is started.

  The solid raw material 11 in the evaporation vessel 12 gradually decreases with the passage of time, but the evaporation surface is only the upper surface of the molded product, the upper surface is a horizontal surface without unevenness, and the cross section is formed into a constant cross-sectional area. Since the evaporation container 12 is filled, the solid raw material 11 evaporates only from the evaporation surface on the upper surface and evaporates uniformly from the entire upper surface. Therefore, even if the amount of the solid raw material 11 is reduced, the area of the evaporation surface on the upper surface does not change and there is no gap between the particles, and the uniform solid structure is formed. It is possible to obtain a certain amount of evaporation. Thereby, the source gas concentration in the accompanying gas can be maintained at a constant concentration over a long period of time.

  Further, the molded product of the solid raw material 11 is placed on the biasing means 17 via the receiving pan 16, and the upper surface of the molded product is held at a certain distance from the upper opening edge of the evaporation container 12 by the biasing force of the biasing means 17. As a result, even if the amount of the solid raw material 11 in the evaporation container 12 decreases due to evaporation and the height of the molded product decreases, the urging means 17 moves the molded product upward as the weight decreases. Therefore, it always comes into contact with the atmospheric gas in the mixing container 13 under a certain condition, and the evaporation amount of the solid raw material 11 can be kept more accurately and constant.

  Further, the molded product of the solid raw material 11 is formed in a state of being in close contact with the heating means 21 through the receiving tray 16, the evaporation container 12, the mixing container 13, and the heat transfer means 20, so that the temperature control by the temperature adjusting means 23 is efficient. Since the solid raw material 11 can be maintained at a constant temperature, the evaporation amount of the solid raw material 11 can be further stabilized.

  The structure and shape of each member can be set as appropriate according to the type and supply amount of the solid raw material. For example, the evaporation container can be formed integrally with the bottom member of the mixing container. Can be part of the mold.

  Further, as shown in the present embodiment, the solid raw material supply apparatus of the present invention includes a mixing container 13 provided with a carrier gas introduction path 14, an accompanying gas outlet path 15, and temperature adjusting means 23, and a solid molded into a predetermined state. Since it can be comprised with the evaporation container 12 with which the raw material 11 is filled, it can form in a small size with a very simple structure, and can aim at reduction of an apparatus cost and a maintenance cost. In addition, a molding machine for molding a solid raw material powder into a predetermined shape can be composed of a simple-shaped mold and a general press machine, so there is no need to use special equipment and the molding cost can be kept low. .

An experiment for supplying xenon difluoride (XeF ₂ ), which is a solid material for manufacturing a semiconductor thin film, was performed using the solid material supply apparatus shown in FIG. The evaporation container is a bottomed cylindrical body having an inner diameter of 20 mm and a height of 35 mm, and a tray having an outer diameter equal to the inner diameter of the evaporation container and a coil spring as an urging means for urging the tray upward are disposed at the bottom. did. Xenon difluoride was formed into a cylindrical shape at a pressure of 10 MPa using a press machine by putting 5 g of the powder into a mold having a circular cross section. The molded product has a constant cross-sectional area with a circular cross section, a horizontal evaporation surface on the upper surface, no gap between particles, and a uniform and dense structure, and its outer diameter is 20 mm, the same as the inner diameter of the evaporation container, The height was 15 mm. In addition, the elasticity of the coil spring is set so as to balance the weight of the molded xenon difluoride, and even when the xenon difluoride is reduced by evaporation after the molded product immediately after molding is placed, The evaporation surface was kept at a substantially constant distance of about 10 mm from the upper opening edge of the evaporation container.

  The mixing container is a cylindrical body with a lid having an inner diameter of 60 mm and a height of 140 mm, and the carrier gas introduction path and the accompanying gas lead-out path are arranged in a straight line on the upper part. At the center of the bottom plate of the mixing container, an evaporation container filled with the molded product placed on a tray was placed, and the mixing container was sealed with a lid. The atmosphere temperature in the mixing vessel is set to 60 ° C., the pressure is adjusted to atmospheric pressure, and nitrogen gas whose flow rate is adjusted to 500 ml / min is introduced into the mixing vessel from the carrier gas introduction route, and from the accompanying gas lead-out route. The concentration of xenon difluoride in the derived entrained gas was measured by FTIR. The change with time of the xenon difluoride concentration is shown in FIG. As can be seen from FIG. 3, there is almost no change in the xenon difluoride concentration, and it can be seen that xenon difluoride can be supplied stably and with good reproducibility at a substantially constant concentration over a long period of time.

  The same operation as in Example 1 was performed except that the tray and the coil spring in the evaporation container were omitted, and the xenon difluoride concentration in the accompanying gas derived from the accompanying gas deriving path was measured by FTIR. A cradle was inserted into the evaporation container so that the evaporation surface when the molded product immediately after molding was filled in the evaporation container was positioned 10 mm from the upper opening edge of the evaporation container. FIG. 4 shows the change over time in the concentration of xenon difluoride in the accompanying gas derived from the accompanying gas deriving path as the same relative concentration as in Example 1. As is clear from FIG. 4, the xenon difluoride concentration slightly decreases with the passage of time, but the decrease rate after 11 hours remains at about 2%, which is a substantially constant concentration over a long period of time. It can be seen that xenon difluoride can be supplied.

(Comparative Example 1)
The same operation as in Example 1 was performed except that the evaporation vessel was not used, the xenon difluoride powder was not molded, and the powdered xenon difluoride was charged into the mixing vessel, and the accompanying gas was derived. The xenon difluoride concentration in the entrained gas derived from the route was measured by FTIR. The result is shown in FIG. 5 as the same relative concentration as in Example 1. As can be seen from FIG. 5, the xenon difluoride concentration decreased with the passage of time and decreased by about 10% after the passage of 11 hours.

(Comparative Example 2)
A stainless steel column-type container (inner diameter: 30 mm, length: 200 mm) with a valve at both ends is filled with 5 g of xenon difluoride and 5 g of a stainless steel packing material, placed in a constant temperature bath at 60 ° C., and nitrogen gas is supplied from one valve. The gas was vented at a flow rate of 500 ml / min at atmospheric pressure, and the xenon difluoride concentration in the gas derived from the other valve was measured by FTIR. The result is shown in FIG. As can be seen from FIG. 6, the xenon difluoride concentration decreased with time and decreased by about 6% after 11 hours.

It is a systematic diagram which shows one example of a solid raw material supply apparatus of this invention. It is a perspective view of an evaporation container. It is a figure which shows the time-dependent change of the xenon difluoride density | concentration in Example 1. FIG. It is a figure which shows the time-dependent change of the xenon difluoride density | concentration in Example 2. FIG. It is a figure which shows the time-dependent change of the xenon difluoride density | concentration in the comparative example 1. It is a figure which shows the time-dependent change of the xenon difluoride density | concentration in the comparative example 2.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 11 ... Solid raw material, 12 ... Evaporation container, 13 ... Mixing container, 14 ... Carrier gas introduction path | route, 15 ... Entrainment gas derivation | leading-out path | route, 16 ... Receptacle, 17 ... Energizing means, 18 ... Container main body, 19 ... Cover body, 20 ... Heat transfer means, 21 ... Heating means, 22 ... Temperature measuring means, 23 ... Temperature adjusting means, 24 ... Gas supply source, 25 ... Pressure adjusting means, 26 ... Flow rate adjusting means, 27 ... Inlet valve, 28 ... Derived valve

Claims (4)

In the solid raw material supply method for heating and evaporating the solid raw material and supplying the evaporated raw material gas with the carrier gas,
The solid raw material powder is shaped into a uniform and dense structure with a constant cross-sectional area and a horizontal top surface with no gaps between the particles,
The molded solid material is filled in an evaporation vessel having the same inner surface shape as the outer surface shape of the solid material, and the upper part is open, and a tray on which the solid material is placed is attached upward by a biasing means. Holding the upper surface of the solid raw material at a constant distance from the upper opening edge of the evaporation vessel,
The evaporation container is sealed in a mixing container that mixes the raw material gas evaporated from the solid raw material with the carrier gas,
In a state where the atmospheric temperature in the mixing container is maintained at a preset temperature, a carrier gas adjusted to a preset pressure and flow rate is introduced into the mixing container,
A solid raw material supply method, wherein the raw material gas evaporated from the upper surface is mixed with a carrier gas to be accompanied by the accompanying gas being led out from the mixing container and supplied to a supply destination. The solid material supply method according to claim 1, wherein the solid material is any one of xenon difluoride, xenon tetrafluoride, and xenon hexafluoride. In the solid raw material supply apparatus that heats and evaporates the solid raw material and supplies the evaporated raw material gas with the carrier gas,
An evaporation container filled with a solid raw material formed into a uniform and dense structure with a constant cross-sectional area and a shape in which the upper surface is a horizontal plane, no gap between particles,
A mixing container in which the evaporation container is enclosed;
A carrier gas introduction path for introducing the carrier gas into the mixing container;
Pressure adjusting means and flow rate adjusting means provided in the carrier gas introduction path;
Temperature adjusting means for adjusting the atmospheric temperature in the mixing container;
An entrained gas deriving path for deriving an entrained gas in which the source gas evaporated from the solid material in the evaporating container and the carrier gas are mixed in the mixing container and supplying the mixed gas to a supply destination;
The evaporating container has an opening at the top, an inner side surface shape that is the same as the outer side surface shape of the molded solid raw material, and a tray on which the solid raw material after molding is placed, and the upper side of the tray And a biasing means for biasing the upper surface of the solid material at a fixed distance from the upper opening edge of the evaporation container . 4. The solid raw material supply apparatus according to claim 3, wherein the solid raw material is any one of xenon difluoride, xenon tetrafluoride, and xenon hexafluoride.

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