JP2003270118A - Method and device for manufacturing compressed gas containing fine particulates - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To easily and stably provide a fine particulate containing compressed gas under the condition where fine particulates are contained in high-pressure gas comprising a main component of optional gas, and to produce fine- particulate-containing compressed gas of main component gas having combustibil ity, explosibility and corrosivity, without any trouble. <P>SOLUTION: The fine particulate containing gas generated by a dry particle generating method in a fine particulate containing gas supplying part 10 is vacuum-sucked into a container 31 brought into a vacuum condition preliminarily by vacuum evacuating using a pump 39P, via vacuum suction part 20, and sealing gas supplied from a sealing gas supplying part 40 is thereafter pressurization sealed into the container. <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for producing a compressed gas containing fine particles, and more specifically, to fine particles or ultrafine particles having an arbitrary particle size at an arbitrary concentration in an arbitrary type and an arbitrary pressure. The present invention relates to a method and an apparatus for producing a dispersed gas containing fine particles.

[0002]

2. Description of the Related Art Various particle measuring instruments such as light scattering type are used for measuring and controlling fine particles in gases such as environmental air and industrial gases used in various industries, and for collecting fine particles. Various particle collectors such as filters and scrubbers are used. It is necessary for these manufacturers and users to confirm and manage the particle measuring ability and particle collecting ability of each device to meet the purpose. For example, in the case of a particle counter, it is necessary to calibrate the particle size measurement before use. For the performance confirmation or adjustment work, a gas containing fine particles whose particle size and concentration are controlled is used as a standard gas and a calibration gas.

In order to calibrate the particle size of a light scattering type particle measuring instrument for gas, polystyrene latex (PSL), which is a monodisperse particle, is suspended and dispersed in ultrapure water, and this is dispersed in nitrogen at atmospheric pressure or higher. A mist containing PSL is produced by spraying with gas, and the mist is dried by passing through a drying tube such as silica gel to produce nitrogen gas containing PSL.

Also, in the examination of the particle collection efficiency of a filter used for removing particles in a gas, dioctyl phthalate (DOP) and triphenyl phosphate (TPP) produced by the same principle as described above are generally used. )
A gas containing polydisperse particles such as Also,
According to the above-mentioned principle, by using an aqueous solution of any compound, for example, nitrogen gas containing fine particles such as sodium chloride can be generated. Such a method is called a wet particle generation method, and a solution method in which fine particles are synthetically produced in a solvent is also classified as the wet particle generation method.

On the other hand, in order to more accurately evaluate the performance of the particle measuring instrument and the particle collecting instrument, it is desirable to use a calibration gas close to the actual measurement object and measurement particles. For example, industrial gas for the semiconductor industry has a moisture content that is dried to a ppb level, and fine particles that are expected to be present in the gas include chromium, manganese, which is a component of a stainless steel material often used in a gas supply system, Since they are fine metal particles such as iron and nickel, it is desired to use industrial gas having a water concentration of ppb level with these fine metal particles dispersed therein as a calibration gas. Therefore, the above-mentioned wet particle generation method cannot be applied to such applications, and the dry particle generation method is suitable.

As a dry particle generation method for generating metal fine particles, a laser evaporation method, a sputtering method, a gas evaporation method, a gas phase reaction method and the like are known. The laser evaporation method is a method of evaporating a solid metal sample using a pulse laser, and can be used for any compound as long as it is a molded solid sample. The sputtering method is a method in which a high-speed ion beam of xenon (Xe) or the like is made to collide with the surface of a solid sample, and fine particles are continuously emitted by this ion bombardment. In the gas evaporation method, the raw material is put in a crucible or the like in a chamber filled with an inert gas, and the raw material is heated by a heating means such as resistance heating or arc heating to generate steam, which is then rapidly cooled. It is a method of condensing to obtain fine particles. The gas phase reaction method is a method of synthesizing fine particles by a chemical reaction of a metal compound vapor in a gas phase, and an electric furnace, a chemical flame, plasma,
A laser is used.

Among these dry particle generation methods, the laser evaporation method and the sputtering method are not practical due to the large size of the apparatus, whereas the in-gas evaporation method allows the apparatus to be downsized and is of a distribution type. It has an advantage that fine particles can be continuously generated. For example, sodium chloride, lead nitrate,
Fine particles can be produced by placing a raw material such as silver or gold on a ceramic boat, heating the raw material in an electric furnace to evaporate it while flowing an inert gas, and cooling / condensing the raw material.

As one of the vaporization methods in the gas, an inert gas is heated from the outside while the inert gas whose pressure and flow rate are controlled to be constant is circulated inside the metal tube. A method of generating fine particles having a particle size of several tens of nanometer level has been developed. By such a method (hereinafter referred to as a metal tube heating method), it becomes possible to easily produce a gas containing fine particles having a stable fine particle concentration and a fine particle diameter under dry conditions. Moreover, when evaluating a particle measuring device and a particle collector for industrial gas for the semiconductor industry, by using a stainless material for the metal tube and using dry gas to generate fine particles, It is possible to perform evaluation using stainless steel components such as chromium, manganese, iron and chromium as standard particles.

[0009]

On the other hand, in the field of industrial gas, which is often supplied at high pressure, the particle collection efficiency is ascertained by measuring the particle concentration under high pressure close to the actual supply conditions and by filtering. Is desired. However, none of the above-mentioned particle generation methods has been reported to produce a high-pressure particulate-containing gas.
For example, in the wet particle generation method, spraying may be performed under the condition that the secondary side also has a high pressure, but the entire system must be capable of high pressure. Similarly, dry particle generation methods also typically assume use in vacuum or near atmospheric pressure. For example, in the metal tube heating method, the pressure difference between the inside and outside of the system is 0.5.
It is difficult to generate the fine particle-containing gas at a high pressure of 0.5 MPa or higher, because the hollow metal tube may burst at a pressure of more than 0.5 MPa.

Further, since various industrial gases are used in the industrial world, it is desired to generate and evaluate a fine particle-containing gas for each gas. However, in the wet particle generation method, hydrolyzable silanes such as monosilane, gases such as arsine, and tungsten hexafluoride cannot be used. On the other hand, in dry particle generation methods such as laser evaporation method and evaporation method in gas, it is possible to use flammable, explosive, and corrosive gases such as monosilane, arsine, hydrogen, oxygen, hydrogen chloride, and chlorine. could not.

Therefore, the present invention can easily and stably obtain a fine particle-containing compressed gas in which fine particles are contained in a high-pressure gas containing any gas as a main component, and it is flammable, explosive, and corrosive. An object of the present invention is to provide a method and an apparatus for producing a fine particle-containing compressed gas, which is capable of producing a fine particle-containing compressed gas containing a gas containing as a main component without any problem.

[0012]

In order to achieve the above object, a method for producing a compressed gas containing fine particles according to the present invention is such that a gas containing fine particles is sucked into a container which has been previously evacuated and then sealed in the container. The feature is that the gas for use is sealed under pressure. Furthermore, when the fine particle-containing gas is vacuum sucked into the container, the suction flow rate of the gas is adjusted to a constant flow rate, and the fine particles in the fine particle-containing gas are generated by a dry particle generation method. It has a feature.

In addition, vacuum suction of the fine particle-containing gas into the container and pressurization and sealing of the sealing gas into the container are performed in separate gas lines, and the compressed gas containing the fine particles is diluted. The gas is mixed to adjust the concentration of fine particles in the gas, and the diluent gas is used as a main component of the fine particle-containing compressed gas. Furthermore, the pressure of the gas containing fine particles is 0.2 MPa (gauge pressure, the same applies hereinafter).
It is characterized in that the pressure is not more than 15 MPa, especially in the range of 0.3 to 1.0 MPa.

The apparatus for producing compressed gas containing fine particles according to the present invention contains a container for storing the compressed gas containing fine particles, a vacuum pump for evacuating the inside of the container, and fine particles contained in the compressed gas containing fine particles. A fine particle-containing gas supply unit for generating the fine particle-containing gas, a vacuum suction unit for sucking the fine particle-containing gas generated in the fine particle-containing gas supply unit into the container, and an encapsulation that is pressurized and sealed in the container. It is characterized in that it is provided with an encapsulating gas supply section for supplying a working gas and a fine particle-containing compressed gas supply line for supplying the fine particle-containing compressed gas in the container to the destination.

Further, all the parts in contact with the fine particle-containing gas and the fine particle-containing compressed gas are made of metal, and the fine particle-containing compressed gas supplied to the fine particle-containing compressed gas supply line is diluted. A dilution gas introduction line for introducing and mixing the dilution gas is provided, and the vacuum suction unit discharges the fine particle-containing gas generated in the fine particle-containing gas supply unit toward the outside air. A diameter pipe and a suction pipe composed of a small diameter pipe coaxially inserted in the large diameter pipe, wherein the suction pipe adjusts the suction flow rate of the particulate-containing gas. And a vacuum gauge for measuring the degree of vacuum in the container and a pressure gauge for measuring the pressure.

[0016]

1 is a system diagram showing an embodiment of a device for producing compressed gas containing fine particles for carrying out the method for producing compressed gas containing fine particles according to the present invention. This apparatus comprises a fine particle-containing gas supply unit 10 for generating a fine particle-containing gas, a vacuum suction unit 20 for vacuum-suctioning the fine particle-containing gas generated by the gas supply unit 10, and a container 31 for storing a fine particle-containing compressed gas. And a filling gas supply unit 40 for supplying the filling gas to the container unit 30, and a diluting gas for introducing and mixing the diluting gas into the particulate-containing compressed gas taken out from the container unit 30. And a supply unit 50.

The fine particle-containing gas supply unit 10 supplies the fine particle-containing gas generated by the fine particle generation source 11 to a fine particle-containing gas supply line 12 having a valve 12V.
As the fine particle generation source 11, a gas containing fine particles generated by the various particle generation methods described above can be used according to the purpose of use of the compressed gas containing fine particles, and the conventional wet particle generation method and dry particle generation method can be used. Although any of these methods may be used, it is preferable to use a dry particle generation method such as a laser evaporation method, a sputtering method, an in-gas evaporation method, or a gas phase reaction method, which can avoid the influence of moisture, and particularly, the type of gas. The metal tube heating method, which allows a wide selection of metal types, is most suitable. By producing fine particles by these methods, 10
It is possible to easily obtain a fine particle-containing gas in the range of Pa to 0.5 MPa, particularly 0.2 MPa or less.

The size and shape of the fine particles contained in the fine particle-containing gas can be set according to the purpose of use of the fine particle-containing compressed gas, and are not particularly limited, and their composition is also particularly limited. Not something. For example,
In the metal tube heating method, the particle size and concentration of the fine particles can be adjusted by variously setting the heat input from a welding machine or the like for heating the metal tube and the flow rate and pressure of the gas flowing in the tube. Further, the fine particles produced by this method will depend on the material of the metal tube.
When 316L stainless steel is used, the fine particles produced are chromium, manganese, which is a component of SUS316L,
It is composed mainly of iron, nickel and the like.

The vacuum suction section 20 includes a large-diameter pipe 21 connected to the fine particle-containing gas supply line 12, a small-diameter pipe coaxially inserted into the large-diameter pipe 21, and a suction pipe 22. The flow rate controller 23 is provided, and the space between the inner surface of the large diameter tube 21 and the outer surface of the suction tube 22 is open to the outside air. Then, the amount of the fine particle-containing gas sucked from the suction pipe 22 is set to be smaller than the amount of the fine particle-containing gas supplied to the large-diameter pipe 21, and a part of the fine particle-containing gas is sucked from the suction pipe 22 without involving the outside air. I am able to inhale. Therefore, in the vacuum suction unit 20, a part of the fine particle-containing gas discharged from the large-diameter pipe 21 toward the outside air is sucked into the suction pipe 22, and the remaining fine-particle-containing gas is discharged from the opening of the large-diameter pipe 21 to the system. It will be exhausted to the outside.

At this time, the fine particle-containing gas may be taken into the container while the source of the fine particle-containing gas is directly connected to the container by the pipe. By opening to the inside, the generation and supply of the fine particle-containing gas in the fine particle-containing gas supply unit 10 can be performed in a stable state, and the suction pipe 22 is provided.
Since it is possible to easily adjust the suction amount of the fine particle-containing gas from the chamber by the flow rate controller 23 to obtain the constant velocity suction, the suction pipe 2
It is possible to keep the particle concentration of the particle-containing gas supplied from No. 2 through the gas suction line 24 to the container section 30 constant. Further, since the fine particle-containing gas can be taken into the container in a stable state, it is possible to downsize the container 31, stabilize the enclosed pressure, facilitate delicate adjustment of the enclosed pressure, etc., and maintain a stable state. Thus, it becomes possible to obtain a high-quality fine particle-containing gas.

The container portion 30 uses a flow-type container having a gas inlet and a gas outlet in opposite directions as the container 31,
On the gas inlet side 31i, a gas introduction line 32 having a valve 32V, the gas suction line 24 connected to the vacuum suction unit 20 via a valve 24V, and the filling gas supply unit 40.
Gas supply line 41 for sealing, which is connected to the valve via a valve 41V, a filter 42 and a pressure regulator 43, and a gas inlet side 31i and a gas outlet side 31o which bypass the container 31 and are connected via a pair of bypass valves 33V. A bypass line 33 is provided, and on the gas outlet side 31o, a gas outlet line 34 having a valve 34V, an exhaust line 35 having a valve 35V, a usage destination of the compressed gas containing fine particles, for example, a device for performing performance evaluation ( (Not shown) is provided with a fine particle-containing compressed gas supply line 36 for supplying the fine particle-containing compressed gas through a valve 36V.

Further, the pressure gauge 3 is installed in the gas outlet line 34.
7a and a vacuum gauge 37b are provided via a switching valve 37V, and the exhaust line 35 is provided with a pressure release line 38 having a valve 38V and a vacuum exhaust line 39 having a valve 39V and a vacuum pump 39P. There is.

The container 31 to be used can be selected according to the type of the compressed gas containing fine particles to be produced and the set pressure, but the maximum filling pressure generally used is 15 MPa.
Made of metal that withstands pressure of about (gauge pressure), eg SUS
A stainless steel container such as 316L is most suitable, and the valve attached to the container must have the same pressure resistance as the container.

Further, in order to suppress the adsorption of fine particles as much as possible, it is preferable to use a container or a valve in which all the parts in contact with the compressed gas containing fine particles or the gas containing fine particles are made of metal. For example, if resin parts are used in the parts that come in contact with the compressed gas containing fine particles,
Fine particles are likely to be adsorbed to the portion, the amount of fine particles floating in the gas is reduced, and stability may be impaired.
Further, as the structure of the container 31, it is preferable to use a flow-through type container as shown in the drawing in which the gas inlet and the gas outlet are provided in opposite directions. It is also possible to use a container provided in the direction. Furthermore, by reliably controlling the pressure inside the container with the pressure gauge 37a and the vacuum gauge 37b, it is possible to improve the reproducibility and stability of the compressed gas containing fine particles to be produced.

Container 3 for vacuum suction of gas containing fine particles
The degree of vacuum in 1 is arbitrary and can be set according to the conditions such as the concentration of fine particles in the fine particle-containing gas to be sucked in, the amount of enclosed gas for enclosing, the purpose of use of the compressed gas containing fine particles to be produced, etc. In addition, the suction efficiency of fine particles can be increased by increasing the degree of vacuum in the container. Further, by adjusting the suction flow rate of the fine particle-containing gas according to the generation rate and production amount of the fine particle-containing gas, the generated fine particles can be more effectively taken into the container. In addition, the Differential Mobility Anal is attached to the vacuum suction unit 20 and the like.
By providing a classifier such as yzer (DMA) to classify the fine particles, only fine particles having a particle diameter within a certain range can be sucked into the container 31.

On the other hand, even if an attempt is made to store the fine particle-containing gas in the container while circulating the fine particle-containing gas in the container at atmospheric pressure or higher, the fine particles are not sufficiently diffused in the container. Compared with Since the generation pressure of the particulate-containing gas in the generation source is limited as described above, it is not possible to obtain the desired high pressure state by directly filling the particulate-containing gas generated here into the container.

The encapsulating gas supply unit 40 generally encloses the encapsulating gas filled in a high-pressure gas container (gas cylinder) 44 with the pressure regulator 43 depressurized to a preset pressure. From gas supply line 41 to container 3
It is formed to supply 0. As the filling gas, one kind of gas (pure gas) or a plurality of kinds of mixed gas can be used depending on the purpose of use of the compressed gas containing fine particles. When a mixed gas is used, it may be prepared in a mixed state, or each gas may be sequentially introduced into a container to be in a mixed state.

The pressure-filling of the filling gas is usually carried out by depressurizing the gas filled in the cylinder with a pressure regulator, but if it is desired to pressurize and fill at a higher pressure, the filling gas is compressed by a compressor. It is also possible to pressurize and then pressurize and seal in a container. That is, the filling pressure is usually 15 MPa or less, which is a range lower than the general filling pressure of various gases in the cylinder, and when the filling pressure is increased, the fine particle concentration is relatively diluted. Therefore, considering practicality, the range of 0.3 to 1.0 MPa is suitable.

The operation of pressurizing and enclosing the encapsulating gas can be carried out continuously from vacuum suction of the fine particle-containing gas into the container. After the vacuum suction, the gas is temporarily stored and then, for example, before use or before shipment. You may make it connect a container to the gas line for injection of another type | system | group, and pressurize and inject the gas for injection.

The dilution gas supply section 50 is used when it is necessary to dilute the fine particle concentration of the fine particle-containing compressed gas when evaluating the performance of equipment such as a particle measuring instrument and a particle collector. The diluent gas filled in the high-pressure gas container (gas cylinder) 51 is passed through the diluent gas introduction line 55 having the pressure regulator 52, the flow rate regulator 53, the filter 54, and the valve 55V, and the fine particle-containing compressed gas supply line 3
6 is formed so as to be introduced. Therefore, by setting the introduction amount of the diluting gas with respect to the amount of the fine particle-containing compressed gas supplied to the fine particle-containing compressed gas supply line 36 in advance, the fine particle-containing compressed gas supplied to the destination is adjusted to a desired fine particle concentration. can do. It is possible to use the same gas as the filling gas for the dilution gas,
Different kinds of gases may be used, and various mixed gases may be used.

When the pressure of the compressed gas containing fine particles supplied to the equipment is higher than the pressure in the high pressure gas container 51,
A compressor may be installed instead of the pressure regulator 52. The fine particle-containing compressed gas adjusted to the preset fine particle concentration in this manner is supplied from the fine particle-containing compressed gas supply line 36 through the flow rate adjuster 56 to the place of use, for example, a device for performance evaluation.

Further, by providing a filter 54 for removing fine particles in the dilution gas introducing line 55, it is possible to prevent extra fine particles from being mixed from the dilution gas introducing line 55 to the fine particle-containing compressed gas supply line 36. You can Further, it is desirable that the pipes and valves, the pressure controller, the flow controller, and the like in the dilution gas introduction line 55 are all made of metal at the parts in contact with the gas.

As the filling gas and the diluting gas,
Any gas may be used in combination as long as the fine particles and the gas used for producing the fine particles, the filling gas and the diluting gas do not react with each other. When the filling gas and the diluting gas are different gas species, the diluting gas can be made the main component of the compressed gas containing fine particles by increasing the diluting gas amount relative to the filling gas amount. it can.

For example, in the above various fine particle generating methods,
When producing a compressed gas containing fine particles whose main components are monosilane, arsine, oxygen, hydrogen, hydrogen chloride, chlorine, etc., which are difficult to use because they may react with pipes, burn, or explode. By using a safe inert gas such as argon or nitrogen as the gas for the generation of fine particles or as the filling gas, and using these gases as the final diluting gas, compression containing fine particles containing these gases as the main component Gas can be produced more safely.

[0035]

EXAMPLES Example 1 An experiment was conducted to confirm the performance of the apparatus for producing compressed gas containing fine particles, using the apparatus having the configuration shown in the system diagram of FIG. In addition, all the pipes, valves, and gas contacting parts of the equipment including the container 31 are made of metal. Further, the metal tube heating method was adopted as the particle generation source 11 in the particle-containing gas supply unit 10. Specifically, while flowing argon gas in a metal tube made of SUS316L, the metal tube is externally heated by a welding machine to generate fumes in the metal tube, and the fumes are entrained in the argon gas to generate fine particles. The contained argon gas was generated and supplied to the vacuum suction unit 20 from the fine particle-containing gas supply line 12. The fine particles generated at this time are chromium, manganese, which is a component of SUS316L,
Main components are iron and nickel.

Further, in the vacuum suction unit 20, the large diameter pipe 21
The amount of the fine particle-containing gas sucked from the suction pipe 22 is set to be smaller than the amount of the fine particle-containing gas supplied to, and the flow rate regulator 23 is set to suck the fine particle-containing gas at a constant velocity. From the filling gas supply unit 40, the argon gas filled in the high-pressure gas container 44 at about 15 MPa was decompressed by the pressure regulator 43 and supplied. Similarly, from the diluting gas supply unit 50, about 15M is stored in the high pressure gas container 51.
The pressure and flow rate of the argon gas filled with Pa were adjusted by the pressure adjuster 52 and the flow rate adjuster 53, and were introduced into the fine particle-containing compressed gas supply line 36.

First, as a comparative control, a gas containing fine particles was circulated in a container to produce a compressed gas containing fine particles (flow collection). That is, the valves 12V, 24V, 32V, 34
V, 35V, 39V are opened (other valves are closed), and while the inside of the container 31 is exhausted by the vacuum pump 39P via the gas outlet line 34 and the exhaust line 35, the particulate-containing gas supply unit 10
The fine particle-containing gas generated in Step 2 was circulated into the container 31 via the fine particle-containing gas supply line 12, the gas suction line 24, and the gas introduction line 32. At this time, the gas circulation pressure in the container 31 was set to about atmospheric pressure.

On the other hand, when the compressed gas containing fine particles is produced by applying the method of the present invention (suction collection), first, the valve 34 is used.
V, 35V, 39V are opened (other valves are closed), the inside of the container 31 is evacuated to -95 kPa by the vacuum pump 39P, and after confirming the degree of vacuum in the container 31 with the vacuum gauge 37b,
The valves 34V, 35V and 39V were closed and closed to vacuum.

Next, open the valves 12V, 24V and 32V,
The fine particle-containing gas generated at the fine particle-containing gas supply unit 10 at a rate of 3.6 liters per minute is used as the flow rate controller 23 of the vacuum suction unit 20.
While controlling so that the suction flow rate is constant at 1.0 liter per minute, vacuum suction is performed in the container 31, and the fine particle-containing gas is introduced into the container until the pressure in the container becomes −15 kPa, and then the valve is closed. 12V, 24V and 32V were closed and sealed. After that, the valves 41V, 33V, 33V, 34V are opened, and the filling gas from the filling gas supply unit 40 is introduced into the container 31 from the opposite direction through the filling gas supply line 41, the bypass line 33, and the gas outlet line 34. Then, the pressure in the container 31 is increased to 0.5 MPa, and this pressure is confirmed by the pressure gauge 37a, and then the valves 41V, 33V, 33
V and 34 V were closed and sealed.

Container 3 in the above-mentioned flow collection and suction collection
The state of the fine particles in 1 was determined by introducing the gas in both containers into a particle measuring instrument and measuring the relationship between the particle diameter and the number of particles (fine particles). The result is shown in Figure 2.
Shown in. From this result, it was confirmed that the suction collection was extremely effective as compared with the distribution collection. Although the production of the compressed gas containing fine particles by suction collection was repeated, it is possible to produce the compressed gas containing fine particles with good reproducibility by confirming the degree of vacuum and the enclosed pressure with the vacuum gauge 37b and the pressure gauge 37a, respectively. found.

Example 2 A compressed gas containing fine particles was manufactured by performing the same suction and collection operation as in Example 1 except that the valve seat was made of synthetic resin, and the valve seat was made of synthetic resin or metal. A comparison was made with the case. The results are shown in Fig. 3. From this result, it is found that it is desirable to form all the portions where the fine particle-containing gas and the fine particle-containing compressed gas come into contact with metal.

Example 3 As shown in the system diagram of FIG. 4, a classifier 25 was installed on the downstream side of the flow rate adjuster 23 to collect fine particles of 40 nm, 51 nm, 6
The compressed gas containing fine particles was manufactured by performing the same suction and collection operation as in Example 1 except that the particle size was 9 nm, and the relationship between the supply time of the compressed gas containing fine particles and the number of particles was measured for each particle size. Results are shown in FIG. From these results, it was found that 30
It can be seen that the supply is extremely stable for the minutes. In the following illustration of the apparatus for producing compressed gas containing fine particles, the same components as those in the apparatus for producing compressed gas containing fine particles shown in FIG. 1 are designated by the same reference numerals, and detailed description thereof will be omitted.

Embodiment 4 As shown in the system diagram of FIG. 6, a particle collector 71 and a particle measuring device 72 are connected to the downstream side of the flow rate controller 56 to collect the particle collector (filter) 71. The efficiency performance was evaluated.
That is, the valves 72V and 73V are opened and the valves 74V and 75V are opened.
When the compressed gas containing fine particles is passed through the particle collector 71 (at the time of collection), the valves 72V and 73V are closed and the valve 74 is closed.
V and 75V were opened, and the state of the fine particles in the gas when the particle collector 71 was not passed (at the time of bypass) was measured by the particle measuring device (condensation nucleus particle measuring device) 72.

A classifier 76 is provided in front of the particle measuring instrument.
However, vacuum pumps 77 are provided in the subsequent stages, respectively, to guide the amount of gas required for measurement to the particle measuring instrument 72, and the surplus gas is discharged from the exhaust valve 78V to the exhaust line.
The measurement results at the time of collection and bypass are shown in FIG. From this result, it was found that the collection efficiency of the metal fine particles in the particle collector 71 was 97%.

Example 5 As shown in the system diagram of FIG. 8, a container 31a having a common gas inlet / outlet was used and suction collection was carried out in the same manner as in Example 1 to produce a compressed gas containing fine particles. When the relationship between the particle size and the number of particles in the obtained fine particle-containing compressed gas was measured, the same results as in Example 1 were obtained.

[0046]

As described above, according to the present invention,
It is possible to easily and stably obtain a fine particle-containing compressed gas that has a pressure equivalent to that of a gas used in an actual industrial gas line and that contains an arbitrary gas as a main component. Therefore, it is possible to evaluate the particle measuring device and the particle collecting device, for example, calibrate and inspect the particle measuring device and inspect the particle collecting efficiency of the filter under conditions close to actual operating conditions.

[Brief description of drawings]

FIG. 1 is a system diagram showing an example of an embodiment of a device for producing compressed gas containing fine particles of the present invention.

FIG. 2 is a diagram showing the relationship between the particle size and the number of particles in the flow collection and suction collection of Example 1.

FIG. 3 is a diagram showing the relationship between the particle size and the number of particles when the material of the valve seat is synthetic resin and metal in Example 2.

FIG. 4 is a system diagram of an apparatus for producing a compressed gas containing fine particles used in Example 3.

5 is a diagram showing a relationship between a supply time of a compressed gas containing fine particles and the number of particles in Example 3. FIG.

FIG. 6 is a system diagram of a device for producing compressed gas containing fine particles used in Example 4.

FIG. 7 is a diagram showing the relationship between the particle size and the number of particles during collection and bypass in Example 4.

FIG. 8 is a system diagram of a device for producing compressed gas containing fine particles used in Example 5.

[Explanation of symbols]

10 ... Fine particle-containing gas supply unit, 11 ... Fine particle generation source, 1
2 ... fine particle-containing gas supply line, 20 ... vacuum suction section, 2
1 ... Large diameter tube, 22 ... Suction tube, 23 ... Flow rate regulator, 24 ...
Gas suction line, 25 ... classifier, 30 ... container part, 31,
31a ... Vessel, 32 ... Gas introduction line, 33 ... Bypass line, 34 ... Gas derivation line, 35 ... Exhaust line, 3
6 ... Fine-particle-containing compressed gas supply line, 37a ... Pressure gauge,
37b ... Vacuum gauge, 38 ... Pressure release line, 39P ... Vacuum pump, 40 ... Filling gas supply section, 41 ... Filling gas supply line, 42 ... Filter, 43 ... Pressure regulator, 44 ... High pressure gas container, 50 ... Diluting gas supply unit, 51 ... High-pressure gas container, 52 ... Pressure regulator, 53 ... Flow rate regulator, 54 ... Filter, 55 ... Diluting gas introduction line, 56 ... Flow rate regulator, 71 ... Particle collector, 72 ... Particle counter

   ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Yu Kimura             1-16-7 Nishi-Shimbashi, Minato-ku, Tokyo Japan Oxygen Stock             Inside the company F term (reference) 2G052 AA00 AA39 AD22 AD24 AD44                       CA03 CA04 CA05 CA12 CA38                       DA27 EA03 FD00 FD01 GA09                       HA18 HC25 HC28

Claims (7)

[Claims] 1. A method for producing a compressed gas containing fine particles, which comprises vacuum-evacuating a fine particle-containing gas into a container that has been evacuated in advance, and then pressurizing and enclosing the filling gas in the container. 2. The method for producing a compressed gas containing fine particles according to claim 1, wherein the suction flow rate of the gas containing the fine particles is adjusted to a constant flow rate when the gas is sucked into the container under vacuum. 3. The pressure of the gas containing fine particles is 0.2 MP.
The method for producing a compressed gas containing fine particles according to claim 1, wherein the pressure is a (gauge pressure) or less. 4. The pressure of the filling gas pressurized by the filling gas is 1
The method for producing a compressed gas containing fine particles according to claim 1, wherein the pressure is 5 MPa (gauge pressure) or less. 5. A container for storing compressed gas containing fine particles,
A vacuum pump for evacuating the inside of the container, a fine particle-containing gas supply unit for producing a fine particle-containing gas containing fine particles contained in the fine particle-containing compressed gas, and a fine particle-containing gas produced by the fine particle-containing gas supply unit. A vacuum suction unit for sucking into the container, a filling gas supply unit that supplies a filling gas that is pressurized and sealed in the container, and a fine particle-containing unit that supplies the fine particle-containing compressed gas in the container to the destination. An apparatus for producing a compressed gas containing fine particles, comprising: a compressed gas supply line. 6. The apparatus for producing a fine particle-containing compressed gas according to claim 5, wherein all the portions in contact with the fine particle-containing gas and the fine particle-containing compressed gas are formed of a metal. 7. The vacuum suction unit is composed of a large-diameter pipe that discharges the fine-particle-containing gas generated in the fine-particle-containing gas supply unit toward the outside air, and a small-diameter pipe that is coaxially inserted into the large-diameter pipe. It has a suction pipe, and it is characterized by the above-mentioned.
An apparatus for producing a compressed gas containing fine particles as described.