JP5264122B2 - Heat treatment apparatus and liquefied gas supply apparatus using the same - Google Patents

Abstract

The invention a heat treatment apparatus and a liquefying gas supply apparatus using the same. The invention solves the problem that single energy source generates a plurality of cold sources and thermal sources and provides the compact and high performance heat treatment apparatus and the liquefying gas supply apparatus by using the same. The heat treatment apparatus of the invention is characterized in that the apparatus generates a plurality of cooling mediums with different temperatures by using a refrigerating device (71) system, carries out the cooling treatment for heating treatment ata plurality heating treatment parts such as a liquefaction mechanism (3a), a storage mechanism (3b) and a vaporization mechanism (3c) and simultaneously controls at least one cooling medium temperature so as to make the medium as a reference cold source for the heat treatment of the heating treatment parts such as the liquefaction mechanism (3a), the storage mechanism (3b) and the vaporization mechanism (3c).

Description

TECHNICAL FIELD The present invention relates to a heat treatment apparatus and a liquefied gas supply apparatus using the same, and in particular, a low vapor pressure special material gas for semiconductors represented by HF, CLF ₃ , BCL ₃ , SiH ₂ CL ₂ , WF _{6 and the} like. The present invention relates to a heat treatment apparatus used for liquefaction treatment or vaporization treatment of liquefied gas such as various process gases and a liquefied gas supply device for supplying liquefied gas treated using the heat treatment apparatus.

A liquefied gas with a low vapor pressure typified by HF, CLF ₃ , BCL ₃ , SiH ₂ CL ₂ , WF ₆ or the like is often used as a special material gas or various process gases used in semiconductor manufacturing processes or various processes. It has been. Such a low vapor pressure liquefied gas is normally filled in a high pressure gas container (hereinafter referred to as “container”) in a liquid state and delivered to a semiconductor manufacturing factory or various processes that consume the liquefied gas. At this time, in a semiconductor manufacturing process apparatus and various process apparatuses (hereinafter referred to as “process apparatus”) which are liquefied gas consumption facilities, these liquefied gases are received in a gas state instead of a liquid state and used in a gas state. At this time, the container filled with the liquefied gas is accommodated in a gas supply facility called a cylinder cabinet, and is vaporized in the container to be in a gaseous state and sent out to a pipe connected to the process apparatus.

  In such a manufacturing process, when liquefied gas is supplied from a gas supply facility to a process device through a supply flow path, in the middle, cooling treatment or a combination of this and heat treatment is performed from the viewpoint of operability and safety. It may be necessary to perform the heat treatment. Conventionally, in such a heat treatment apparatus, it has been common to separately prepare cooling and heating by separately using a cooling processing means and a heating processing means.

  Specifically, as the heat treatment means, for example, a heating device used in a liquefied gas supply device as shown in FIG. That is, the heat treatment means is used to prevent re-liquefaction of the material gas in the liquefied material gas supply piping system, and the liquefied material gas supplied into the liquefied material gas supply piping 205 passes through the pipe through its own line. Since it is heated above the vaporization point, reliquefaction is prevented. Here, 201 is a mass flow controller. A temperature sensor 202 detects the temperature of the liquefied material gas. 203 is a temperature control circuit, 204 is a heater for heating the material gas supply system piping, and 205 is a liquefied material gas supply piping. 206 is a process chamber, and 207 is a liquefied material gas storage cylinder. (For example, refer to Patent Document 1).

  Further, as the cooling processing means, for example, a heat treatment apparatus (low temperature liquefied gas cooling apparatus) for producing cold using a refrigerator as shown in FIG. That is, the storage container 102 that stores the low-temperature liquefied gas, the condensing tank 104 disposed above the storage container 102, the transfer pipes 122 and 124 that communicate the condensing tank 104 and the storage container 102, and the condensing tank 104 The cooling device provided with the refrigerator 106 for condensing gas. A recondenser 138 of the refrigerator 106 is disposed in the condensing tank 104, and the evaporated gas in the storage container 102 flows into the condensing tank 104 through the transfer pipe 122, and the liquefied gas condensed in the condensing tank 104 overflows. It flows down into the storage container 102 through the transfer pipe 124. (For example, refer to Patent Document 2).

Japanese Patent Laid-Open No. 10-12556 JP-A-11-1931979

However, in the heat treatment apparatus as described above or a liquefied gas supply apparatus using the same, the following problems may occur.
(1) In a manufacturing process facility in which a semiconductor factory or a process apparatus using a low vapor pressure liquefied gas is installed, a plurality of cooling processing means and heat processing means are often used, and a place for installing a plurality of heat treatment apparatuses. The area occupied by the facility for securing This is a very large obstacle to the installation and delivery of other equipment in the above-mentioned factories that require special equipment such as a clean room. In addition, the cost load increases.
(2) When a plurality of cooling processing means are used, a plurality of refrigerant tanks are required separately, and energy loss due to cold heat leakage from the refrigerant tank is also large.
(3) The number of parts is large, and therefore the reliability may be inferior, and the number of maintenance points increases, leading to an increase in management items and maintenance man-hours.

  An object of the present invention is to provide a heat treatment apparatus that is high in energy efficiency, compact, and functionally, and a liquefied gas supply apparatus using the same, by producing a plurality of colds and heats with a single power source. . In particular, a heat treatment apparatus that can be used for heat treatment of liquefied gas such as special material gas for semiconductors with low vapor pressure and various process gases, and that can perform a plurality of liquefaction treatments and vaporization treatments in one apparatus, and a treatment using the same. It is providing the liquefied gas supply apparatus which supplies liquefied gas.

  As a result of intensive studies to solve the above problems, the present inventors have found that the above object can be achieved by the heat treatment apparatus shown below and a liquefied gas supply apparatus using the heat treatment apparatus, and have completed the present invention. It was.

  The present invention is a heat treatment apparatus, generating a plurality of refrigerants at different temperatures using a single refrigerator, performing cooling treatment or heating treatment of a plurality of heat treatment units using the refrigerant, It is characterized in that at least one of the refrigerants is temperature-controlled and used as a reference cold heat for the heat treatment of the heat treatment part.

  As described above, in a manufacturing process having a liquefied gas supply device or a liquefied gas consumption facility, the heat treatment device plays an important role, and thus requires a plurality of stable cooling supply with high energy efficiency and compactness. There is also a need for a functionally superior heat treatment apparatus. In response to such a demand, the present invention generates a plurality of refrigerants having different temperatures using a single system refrigerator, and performs cooling treatment or heating treatment of a plurality of heat treatment units using the refrigerant. It is possible to systematically control and manage from the production to the final heat treatment, and it is possible to provide a compact and functionally excellent heat treatment apparatus capable of highly efficient temperature control with high energy efficiency. In particular, by performing temperature control with high accuracy on at least one refrigerant to obtain reference cold heat, a refrigerant controlled with the same accuracy is supplied to each heat treatment unit, and a refrigerant having a desired temperature is supplied. It is possible to perform temperature control in which a plurality of heat treatment units are associated with each other, and control in conjunction with sample conditions and environmental conditions is also possible. Further, it is possible to recover energy according to each refrigerant used in circulation. The “refrigerant” here refers to a heat medium that can be used not only as a cold heat source but also as a heat source, and will be described in detail later.

  The present invention is the above heat treatment apparatus, wherein the refrigerant tank for generating and storing the refrigerant is composed of a plurality of refrigerant tanks having multiple structures, and the first refrigerant at the lowest temperature is stored in the innermost first refrigerant tank. The second refrigerant tank stores the second refrigerant, the third refrigerant tank stores the third refrigerant, the nth refrigerant tank in the nth refrigerant tank, and the refrigerant from the refrigerant tank to the heat treatment section. Is provided.

  In a heat treatment apparatus used for a liquefied gas supply device, a liquefied gas consumption facility, etc., it is preferable to supply a plurality of refrigerants having different temperatures as described above. Is required. In order to meet such demands and to improve the energy efficiency obtained by downsizing, the present invention constitutes a refrigerant tank having a plurality of refrigerant tanks with multiple structures, and supplies a plurality of refrigerants in order from the inside to the low temperature. Storable. Thus, unlike the conventional method in which a heat insulating layer is provided around each tank and individual temperature control is required, heat insulation between the tanks can be easily performed, energy loss is small, and at least 1 If the temperature of one refrigerant tank is controlled, the temperature of the adjacent refrigerant tank can be controlled within a predetermined accuracy range, so that the heat treatment apparatus can be made more compact. Note that the “multiple structure” here is not limited to the case where a plurality of refrigerant tanks are arranged concentrically, and any two of the refrigerant tanks are partly planar or three-dimensional. It means that it is an adjacent overlapping arrangement.

  The present invention is the above-described heat treatment apparatus, having at least two heat treatment sections functioning as a liquefaction means, a storage means, and a vaporization means, and having a function capable of switching these independently and alternately. 1 refrigerant is used as cold heat of the heat treatment section for liquefying means, the second refrigerant is used as cold heat of the heat treatment section for storage means, and the third refrigerant is used as heat of the heat treatment section for vaporization means. To do.

  In semiconductor manufacturing processes and various processes, liquefied gas is often used, and liquid phase and gas phase cooling and heating processes, liquid to gas phase shift processes, gas to liquid phase shift processes, and The stored liquid phase or gas phase temperature maintenance process is performed, and a plurality of refrigerants having different temperatures are required. In the present invention, a plurality of refrigerants having different temperatures are used as the cooling heat of the heat treatment section for the liquefying means, the cooling heat of the heat treatment section for the storage means, and the heat heat of the heat treatment section for the vaporization means in order according to the processing conditions. Accordingly, it is possible to provide a heat treatment apparatus capable of performing a plurality of liquefaction processes and vaporization processes with one apparatus.

  The present invention is the above-described heat treatment apparatus, and in the switching from the function as the liquefaction means and the storage means to the function as the vaporization means or vice versa, any one of the functions can be secured after switching. In this case, the supply paths of the first to third refrigerants are switched in advance or the control temperatures of the respective functions are switched.

  As described above, in the heat treatment apparatus, the functions as the liquefaction means and the storage means and the function as the secondary vaporization means are functions for independently processing the liquefied gas, and the control temperature is as described above. Plays an important role. However, when these functions are alternately switched, it is relatively easy to quickly switch the processing function of the liquefied gas, while ensuring the speed of switching the temperature in each means in which the gas phase and the liquid phase coexist. Difficult to do. The present invention switches the operating temperature of each means in advance to the control temperature of each function when any function of each means constituting the heat treatment section can be secured when switching such functions. In order to ensure each function quickly, it is possible to stably supply the liquefied gas.

  This invention is the said heat processing apparatus, Comprising: The heat in the thermal radiation part of the said refrigerator is used as a heat for temperature adjustment of the said refrigerant | coolant by which temperature control is carried out.

  The refrigerator used for producing the refrigerant is provided with a compression section and a heat radiation section that are responsible for repeated compression and expansion of the heat medium for the refrigerator. On the other hand, in producing a plurality of refrigerants, heat for adjusting the temperature of the refrigerant is required. The present invention is not intended to naturally dissipate the heat from the heat radiating part, but is intended to be used as the temperature of the refrigerant whose temperature is controlled. By effectively using the energy of the entire heat treatment apparatus including the refrigerator, It is possible to provide a compact and functionally excellent heat treatment apparatus that can perform temperature control with high energy efficiency and high accuracy without requiring addition of a special function.

  The present invention is the heat treatment apparatus as described above, wherein the vaporizing means has a space through which the third refrigerant can flow so as to come into contact with an outer periphery and a bottom of a container that stores an object to be vaporized, and a bottom surface of the container A nozzle for injecting the third refrigerant at right angles to the bottom of the space.

  In order to stably supply liquefied gas or the like by the vaporizing means, it is important to maintain the temperature of the liquid phase by the heat of vaporization after the start of supply, as well as the temperature conditions at the start of supply. At this time, particularly in a liquid phase liquefied gas filled in a pressure vessel or a corresponding vessel, in the conventional heating method using the jacket type, the temperature decreases due to transpiration from the liquid phase surface at the center of the vessel. It was difficult to replenish the gas, and it was difficult to supply a stable liquefied gas. The present invention has a space through which the third refrigerant can flow so as to be in contact with the outer periphery and the bottom of the container, thereby ensuring the supply of warm heat from the periphery of the container and injecting at a right angle to the bottom surface of the container. By injecting the third refrigerant from a nozzle having a mouth, an upward flow is generated in the central portion of the liquid phase to form a convection in the liquid phase, thereby ensuring uniformity of the liquid phase temperature. . As a result, the liquefied gas can be uniformly vaporized from the liquid phase inside the container, and a stable liquefied gas can be supplied.

  The present invention is a liquefied gas supply device for supplying a liquefied gas to a gas consuming facility separated from the gas supplied from a container filled with liquefied gas, wherein the liquefied gas in the gas state supplied by the pipe is supplied. In the heat treatment apparatus according to any one of the above, the gas is subjected to liquefaction treatment and vaporization treatment, or liquefaction treatment, storage treatment, and vaporization treatment.

  The liquefied gas supply device plays an important role in, for example, a semiconductor manufacturing process, and is supplied to a gas consuming facility separated from the gas supplied from a container filled with the liquefied gas (hereinafter referred to as “filled container”). Even when supplying liquefied gas, stable supply of liquefied gas is required. In particular, in the case of a liquefied gas having a low vapor pressure, problems such as reliquefaction in the air supply flow path and a decrease in supply amount due to pressure loss cannot be adequately addressed by conventional liquefied gas supply devices. The present invention is characterized by performing liquefaction treatment and vaporization treatment, or liquefaction treatment, storage treatment, and vaporization treatment using the above-described heat treatment apparatus, whereby a low vapor pressure liquefied gas is obtained. Even in this case, liquefaction in the air supply piping (primary piping and secondary piping) can be prevented and the air supply pressure from the filling container to the process equipment can be secured to stably supply the desired flow rate. It has become possible to provide a liquefied gas supply device capable of performing the above. In other words, the liquefied gas vaporized and sent in the filling container is not sent as it is to the process equipment which is the gas consuming equipment, but after being forced to liquefy in the immediate vicinity of the process equipment or in the process equipment, By evaporating and supplying the air to the process device, it was possible to prevent reliquefaction in the air supply pipe and to secure the air supply pressure.

The present invention is the above liquefied gas supply apparatus, which has at least two heat treatment apparatuses, and uses a plurality of refrigerants having different temperatures produced in the heat treatment apparatus,
In the first heat treatment apparatus, the gaseous liquefied gas is liquefied with the coldest refrigerant, or further the liquid liquefied gas is stored with the second coldest refrigerant,
In another heat treatment apparatus, the storage-treated liquefied gas is vaporized by a refrigerant having a temperature higher than those of these refrigerants,
The liquefaction / storage process and the vaporization process can be switched, and simultaneously with the switching, the refrigerant flow path for automatically switching between the refrigerant supplied to the first heat treatment apparatus and the refrigerant supplied to the other heat treatment apparatus It has a switching system.

  As described above, the liquefied gas supply apparatus used in various manufacturing processes requires heat treatment under a plurality of temperature conditions, requires a high energy efficiency and a plurality of stable cooling supply, and is compact and functionally excellent. Heat treatment apparatus is required. In addition, the liquid phase and gas phase cooling treatment mode and heat treatment mode, or the liquid-to-gas phase-shifting process, the gas-to-liquid phase-shifting process, and the stored liquid-phase and gas-phase temperature maintenance In some cases, the heat treatment mode is switched, and the cooling processing temperature and the heating processing temperature are switched as the processing is performed. The present invention produces a plurality of refrigerants having different temperatures, and arbitrarily switches the refrigerant supply flow path to the plurality of heat treatment units according to the processing conditions, thereby switching the heat treatment mode with one apparatus. It has become possible to provide a liquefied gas supply device capable of switching the cooling treatment temperature and the heating treatment temperature to stably supply the liquefied gas.

  As described above, according to the heat treatment apparatus according to the present invention or the liquefied gas supply apparatus using the same, the heat treatment apparatus can be used for heat treatment of liquefied gas such as low vapor pressure semiconductor special material gas and various process gases. It has become possible to perform a stable supply of liquefied gas by performing liquefaction treatment and vaporization treatment.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. Here, a plurality of refrigerants having different temperatures are generated using a single-system refrigerator, and a cooling process or a heating process is performed on the plurality of heat treatment units using the refrigerant, and at least one of the refrigerants is controlled in temperature. The heat treatment apparatus used as the reference cold heat for the heat treatment of the heat treatment section is fundamental.

<Example of basic configuration of heat treatment apparatus according to the present invention>
FIG. 1 is a schematic view showing a basic configuration example of a heat treatment apparatus (hereinafter referred to as “the present apparatus”) according to the present invention. Here, a case where three heat treatments of liquefaction, storage, and vaporization are performed using refrigerants having three different temperatures as exemplified in Table 1 will be described.

  This apparatus 3 includes one refrigerator 71 for producing cold heat serving as a cold heat source, a flow path 72 for transferring a heat medium for the refrigerator, three refrigerant tanks (first refrigerant tank 7a, second refrigerant tank 7b, third A "refrigerant generating unit 7" comprising a refrigerant tank 73 having a refrigerant tank 7c), a liquefying means 3a for liquefying a part of the object to be heat treated (liquefied gas, etc.), a storage means 3b for storing the same, and a vaporizing process It is composed of a “heat treatment unit (liquefied gas supply facility) 3u” composed of the vaporizing means 3c.

  In the refrigerant generating unit 7, the cold heat (refrigerating medium for the refrigerator) produced by the refrigerator 71 is supplied to the first refrigerant tank 7 a of the refrigerant tank 73 via the flow path 72. The refrigerant in the first refrigerant tank 7a is cooled, the refrigerant in the second refrigerant tank 7b is cooled through the partition wall Wa along with the cooling, and the refrigerant in the second refrigerant tank 7c is further cooled through the partition wall Wb for a predetermined time. Later, a refrigerant having a predetermined temperature is stored in each refrigerant tank. The stored refrigerant in each of the refrigerant tanks is supplied to the heat treatment unit 3u by the first, second, and third circulation pumps Pa, Pb, and Pc, and the liquefaction means heat treatment section 3a, the storage means heat treatment section 3b, and the vaporization section, respectively. A circulation system returning from the means heat treatment section 3c back to each refrigerant tank is formed, and is responsible for cooling processing and heat treatment of each heat treatment section. Hereinafter, the refrigerant generation unit 7 and the heat treatment unit 3u will be described in detail.

[Refrigerant generation unit 7]
As illustrated in FIG. 2, the refrigerant generating unit 7 used in the present apparatus preferably constitutes an integrated unit in which the refrigerator 71 is one system and three refrigerant tanks for producing refrigerant have a triple structure. In addition, it is preferable to control the temperature of at least one of the refrigerant tanks and use it as the reference cold heat for the heat treatment of this apparatus. While clarifying the control criteria for the heat treatment of the entire apparatus using one system of cold heat, the required heat supply of each heat treatment unit can be adjusted by adjusting the structure of each refrigerant tank and the refrigerant supply amount. It becomes possible to control to. At this time, when the temperature difference between the second refrigerant in the second refrigerant tank 7b and the third refrigerant in the third refrigerant tank 7c is large, as shown in FIG. 2, the second refrigerant tank 7b and the third refrigerant tank 7c It is preferable that the partition wall Wb has a double structure and an air layer is provided inside. As a result, it is possible to suppress the loss of cooling and reduce the burden for temperature control. Such a refrigerant generation unit 7 has the following characteristics.

  (I) The refrigerator 71 is one system, and a plurality of refrigerants are produced. That is, as before, three systems are not required to produce three refrigerants, and the cold heat (refrigerant heat medium) produced by the refrigerator 71 is exclusively supplied to the first refrigerant tank via the flow path 72. In order to cool the 1st refrigerant in 7a, it is arranged so that it may be immersed in the 1st refrigerant, and 2nd refrigerant tank 7b and 3rd refrigerant tank 7c are the cold heat transmitted from partition tank Wa and Wb from refrigerant tank 1 It is characterized by using. Here, the refrigerator 71 is not particularly limited, and a vapor compression refrigerator as illustrated in FIG. 2 can be used. The compressor 71a, the condenser 71b, the liquid receiver 71c, the expansion valve 71d, and the evaporator 71e are highly versatile refrigerators that use ammonia, hydrocarbons, carbon dioxide, or the like as a heat medium. In addition, an absorption refrigerator using water or ammonia as a heat medium or an adsorption refrigerator using zeolite or silica gel as an adsorption medium can be used.

  (Ii) A refrigerant tank 73 that generates and stores refrigerant is composed of a plurality of refrigerant tanks 7a, 7b, 7c,..., And stores the lowest temperature first refrigerant in the innermost first refrigerant tank 7a. The second refrigerant tank 7b and the third refrigerant tank 7c store the second refrigerant in the second refrigerant tank 7b and the nth refrigerant tank 7n in the nth refrigerant tank 7n, and each refrigerant is supplied to the heat treatment unit 3u. The refrigerant is supplied from the tank (in FIG. 2, the case where n is 3 is illustrated, and the same shall apply hereinafter). Unlike the conventional method in which a heat insulating layer is provided around each refrigerant tank to individually control the temperature, heat insulation between the refrigerant tanks can be easily performed, and energy loss from the entire refrigerant tank 73 is reduced. If the temperature of at least one refrigerant tank is small, the temperature of the refrigerant tank adjacent to the refrigerant tank can be controlled within a predetermined accuracy range.

  (Iii) The partition wall Wa between the first refrigerant tank 7a and the second refrigerant tank 7b is made of metal (for example, aluminum or stainless steel) and has a structure in which cold heat is easily transmitted from the first refrigerant tank 7a to the second refrigerant tank 7b. The partition wall Wb between the refrigerant tank and the third refrigerant tank is characterized by a double metal wall surface having an air layer in the middle in order to suppress the transmission of cold heat. In addition, the periphery of the third refrigerant tank 7c is covered with a heat insulating material or has a double wall structure to suppress heat transfer from the outside air by making the inside an air layer or a vacuum, etc., and prevent condensation due to moisture of the outside air. A structure is preferable.

  (Iv) In FIG. 2, in the refrigerant generating unit 7, a cooling flow path 72 from the refrigerator 71 is introduced into the first refrigerant tank 7 a to cool the refrigerant in the tank below a predetermined temperature, and the second The case where the refrigerant | coolant stored by each tank is each controlled by predetermined | prescribed temperature by the heaters Hb and Hc and the refrigerant | coolant temperature control parts 74b and 74c provided in the refrigerant | coolant tank 7b and the 3rd refrigerant | coolant tank 7c is shown. At this time, it is preferable to provide stirrers Ma, Mb, and Mc in each refrigerant so that the thermal diffusion of the refrigerant increases. However, two refrigerant tanks controlled to a predetermined temperature are not necessarily required. If the structure of the refrigerant tank 73, the usage conditions of the refrigerant, and the like are set, the heat balance in each refrigerant tank will be determined. The temperature of each refrigerant tank can be controlled by controlling the temperature with reference to the refrigerant in any refrigerant tank (reference refrigerant). That is, heaters Hc and Hc and temperature sensors Sb and Sc for measuring the temperature of the refrigerant are immersed in the second refrigerant in the second refrigerant tank 7b and the third refrigerant in the third refrigerant tank 7c, respectively. 7b, the partition wall Wa from the first refrigerant tank 7a, and the third refrigerant tank 7c from the state of being supercooled by the cold heat transmitted from the second refrigerant tank 7b to the partition wall Wb, It is characterized in that feedback control is performed so that each becomes a predetermined temperature by appropriately supplying heat with Hc. In addition, about the 1st refrigerant | coolant tank 7a which does not require the precision of refrigerant | coolant temperature so much, a heater is not integrated but only the flow path 72 of the 1st cold heat from the refrigerator 71 is integrated, and even if there is no temperature sensor, it is functional. There is no particular problem.

  (Iv) In the refrigerant generation unit 7 obtained by such a structure, the temperature distribution of each refrigerant tank is as shown in FIG.

  Since the first refrigerant in the innermost first refrigerant tank 7a is cooled by the cold heat flow path 72 from the refrigerator 71 as described above, the temperature is the lowest among the three refrigerants, for example, −10 The refrigerator 71 operates so as to be about -5 ° C. At this time, since the temperature of the first refrigerant is not controlled unlike the second refrigerant and the third refrigerant, the temperature of the first refrigerant is somewhat affected by fluctuations in the operating conditions (such as the ambient temperature of the refrigerator) of the refrigerator 71. It varies with the width.

  The second refrigerant tank 7b is not cooled by the refrigerator 71 like the first refrigerant tank 7a, but is cooled by the cold heat transmitted from the partition wall Wa of the first refrigerant tank 7a in contact with the second refrigerant. At this time, if it is left as it is, it will be affected by the fluctuation of the temperature of the first refrigerant as it is, but the heater Hb is built in the second refrigerant tank 7b, and the temperature of the second refrigerant is always changed by the heating operation by this heater Hb. Unlike the first refrigerant tank 7a, the temperature is controlled to be around 0 ° C., and the temperature is constant. Here, instead of the heating operation by the heater Hb, the heat in the heat radiating part of the refrigerator 71 (specifically, the condenser 71b corresponds) is used as the temperature for adjusting the temperature of the third refrigerant whose temperature is controlled. Is possible. Since this apparatus constitutes a heat treatment apparatus integrated with the refrigerator 71, the energy use of the entire heat treatment apparatus including the refrigerator 71 is effectively utilized without requiring the addition of the heater Hb function. Highly accurate temperature control is possible. Further, the energy efficiency can be further improved by replacing the heating operation with the heater Hc described later.

  Similarly to the second refrigerant tank 7b, the third refrigerant tank 7c is not cooled by the refrigerator 71, but is cooled by the cold heat transmitted from the partition wall Wb of the second refrigerant tank 7b in contact with the third refrigerant. At this time, the third refrigerant tank 7c fluctuates due to thermal disturbance from the outside air and other factors only by the transmitted cold heat, but the heater Hc is incorporated in the third refrigerant tank 7c as well as the second refrigerant tank 7b. Thus, the temperature of the third refrigerant is controlled to be always about 15 ° C. ± 1 ° C., for example, by the heating operation by the heater Hc. At this time, instead of the heating operation by the heater Hc as described above, it is possible to use the heat in the heat radiating portion (specifically, the condenser 71b) of the refrigerator 71.

  (V) Although FIG. 2 illustrates the case where the three refrigerant tanks are formed as an integral type having a triple structure arranged concentrically, the present apparatus is not limited to such a structure. It is sufficient that any two of the refrigerant tanks have an overlapping arrangement in which a part of them is brought into planar or three-dimensional contact. Specifically, as illustrated in FIGS. 4A to 4D, a structure in which the first refrigerant tank 7 a, the second refrigerant tank 7 b, and the third refrigerant tank 7 c are adjacent to each other in a planar shape or one refrigerant tank. As shown in FIGS. 4E to 4H, the first refrigerant tank 7a, the second refrigerant tank 7b, and the third refrigerant tank 7c are sequentially adjacent to each other as illustrated in FIGS. It is possible to apply a structure, a structure in which one refrigerant tank is adjacent to two refrigerant tanks, or a combination thereof.

[About heat treatment unit 3u]
The heat treatment unit 3u used in the present apparatus has a function of liquefying the supplied gaseous liquefied gas and temporarily storing the liquefied gas in a liquid state (hereinafter sometimes referred to as “liquefied storage mode”), and the liquefied gas once stored. It has a function of vaporizing gas again and supplying it in a gaseous state (hereinafter sometimes referred to as “revaporization mode”). At this time, in the configuration illustrated in FIG. 1, the liquefying means 3a, the storage means 3b, and the vaporizing means 3c are connected via the communication part 3d, and liquefied by the action of a liquid feed pump or the like incorporated in the communication part 3d. An object to be processed such as a gas can be sequentially processed successively.

  Here, as illustrated in FIG. 5, the liquefying means 3a is disposed at the upper part of the storage means 3b as a precooler for liquefying the liquefied gas, and is incorporated in the liquefied gas introduction pipe 3e to the heat treatment unit 3u. ing. The first refrigerant supplied from the first refrigerant tank 7a by the first refrigerant circulation pump Pa and introduced from the refrigerant introduction part 3aa at the lower part of the liquefaction means 3a cools the liquefied gas introduction pipe 3e in the liquefaction means 3a, The refrigerant is discharged from the upper refrigerant outlet 3ab and returned to the first refrigerant tank 7a, so that a new first refrigerant is always circulated. The gaseous liquefied gas introduced into the liquefied gas introducing pipe 3e is rapidly cooled by the liquefying means 3a, and is condensed while condensing, and is stored in the storage means installed below the liquefying means 3a. It acts to be stored as a liquid in 3b. Further, heat insulation covers 3be and 3ae are provided on the outer surface of the storage means 3b, the refrigerant introduction pipe 3aa and the refrigerant outlet pipe 3ab to reduce the loss of cold heat and prevent condensation.

  Further, as shown in FIG. 5, the storage means 3b has a cooling jacket 3bb assembled so as to surround a container 3ba for storing the liquefied gas introduced from the liquefied gas introduction pipe 3e, and a refrigerant is provided below the cooling jacket 3bb. A refrigerant outlet 3bd is provided in the inlet 3bc and the upper part, and the refrigerant flows through the space 3be in the cooling jacket 3bb and circulates the second refrigerant between the second refrigerant tank 7b by the second refrigerant circulation pump Pb. It has a structure that can be done. The outer surface of the cooling jacket 3bb, the refrigerant introduction pipe 3bc, and the refrigerant outlet pipe 3bd use heat-insulated coated pipes to prevent the loss of cold and prevent condensation on the outer surface of the cooling jacket 3bb and the refrigerant circulation pipe surface. It is supposed to be.

  The vaporization means 3c is basically between a container 3ca (not shown) for storing liquefied gas and a third refrigerant tank 7c (not shown) around it, like the storage means 3b shown in FIG. And a liquefied gas lead-out pipe for supplying a vaporized liquefied gas, having a structure comprising a cooling jacket 3cb (not shown) capable of circulating and supplying the third refrigerant by a third refrigerant circulation pump Pc (not shown). 3f.

  In addition to such a structure, various structures can be applied. For example, as shown in FIG. 6 (A), there is a method in which a liquid liquefied gas filled in the container 3ca is vaporized by introducing a liquid-phase carrier gas and bubbling, and a carrier gas introducing portion 3cc is provided, The carrier gas introduction pipe 3cd is inserted to the vicinity of the lowest layer of the liquid phase liquefied gas. Even when it is difficult to secure a sufficient supply amount due to the low vapor pressure, the air supply capability can be improved by accompanying the carrier gas with the supply capability. In addition, when supply of a low concentration liquefied gas is required, or when a plurality of gases are mixed and used, the use conditions are determined by supplying the liquefied gas with an inert gas or other gas as a carrier. The liquefied gas corresponding to can be supplied.

At this time, in order to control the amount of the liquefied gas accompanying the carrier gas (this is usually referred to as “pickup rate”), the flow rate of the carrier gas can be controlled. That is, when the liquid phase temperature is controlled to be substantially constant, the mass flow controller 3mf is provided in the carrier gas flow path, and this is controlled to increase the flow rate of the carrier gas, thereby increasing the pickup rate. be able to. If it is sufficient to entrain the liquefied gas with the carrier gas, the carrier gas is added to the carrier gas from the primary vaporization means 1b or the method of passing the carrier gas through the surface layer of the liquid phase without bubbling. It is also possible to use a dilution method. As the carrier gas, it is required to use a gas that does not hinder the gas consumption process. Usually, an inert gas such as He, Ar, or N ₂ is often used. However, when SiHCl ₃ is used as the liquefied gas as in the epitaxial wafer processing process, it is preferable to use H ₂ .

  Further, as shown in FIG. 6B, the nozzle 3cf for injecting the third refrigerant at right angles to the bottom surface of the container 3ca may be arranged on the bottom side of the space 3ce in the cooling jacket 3cb. By having the space 3ce through which the third refrigerant can flow so as to be in contact with the outer periphery and the bottom of the cooling jacket 3cb, the third refrigerant is supplied in the direction perpendicular to the bottom surface of the container 3ca while supplying warm heat from the periphery of the container 3ca. By injecting the liquefied gas, heat conduction from the third refrigerant to the container 3ca or the liquefied gas stored in the container 3ca is promoted, and the thermal change can be promptly compensated for the temperature change factor of the liquefied gas. Gas can be supplied. Further, as shown in FIG. 6B, by incorporating an immersion heater Hn in the refrigerant introduction system and heating the supplied third refrigerant, the liquid phase liquefied gas is changed according to the supply amount of the liquefied gas, that is, the vaporization amount. Since the heat of vaporization that is taken away can be quickly compensated, liquefied gas can be supplied at a more stable pressure.

<Another configuration example of the heat treatment apparatus according to the present invention>
Next, another configuration example of the heat treatment apparatus according to the present invention will be described with reference to FIG. The basic components are the same as those illustrated in FIG. 1 above, but have at least two heat treatment units 3u that function as the liquefying means 3a, the storage means 3b, and the vaporizing means 3c illustrated in FIG. The refrigerant circulation switching system is constituted by the refrigerant generation unit 7, the three circulation pumps Pa, Pb, Pc, and the four flow path switching valves V1 to V4 so that they can be switched independently and alternately. Is configured. FIG. 7 shows a case where the heat treatment unit 3uA shown on the left side of the drawing is in the “liquefaction storage mode” and the heat treatment unit 3uB shown on the right side of the drawing is in the “revaporization mode” (STEP 1). Each mode is switched (STEP 2), and this is periodically repeated (STEP 3,...), Whereby the supplied liquefied gas can be re-vaporized and continuously supplied.

[Refrigerant circulation switching system]
Specifically, in each STEP, the refrigerant to be used is switched by the flow path switching valves V1 to V4. The operation modes of the heat treatment units 3uA and 3uB, the heat treatment targets, and the refrigerant to be used are as shown in Table 2.

  The flow path switching valve V1 sends out the second refrigerant pressure-fed by the second refrigerant circulation pump Pb to one of the two heat treatment units 3uA or 3uB that is a cooling target (FIG. 7 shows the heat treatment unit 3uA side). At the same time, it has a function of sending the third refrigerant pumped by the refrigerant circulation pump Pc to the heat treatment unit 3uB opposite to this. The flow path switching valve V2 has a function of switching the flow path so that the second and third refrigerants returned from the heat treatment unit 3uA and the heat treatment unit 3uB are returned to the second refrigerant tank 7b and the third refrigerant tank 7c, respectively. The flow path switching valve V3 and the flow path switching valve V4 control which of the two liquefaction means 3aA and 3aB the first refrigerant flows through. In FIG. 7, in the liquefaction means 3aA constituting the heat treatment unit 3uA, It shows that the first refrigerant is circulated and supplied to the liquefying means 3aB constituting the heat treatment unit 3uB.

  These four flow path switching valves V1 to V4 operate to switch the flow paths at the same time when the operation mode of the two heat treatment units 3uA and 3uB is switched from the “liquefaction storage mode” to the “revaporization mode”. To do. In FIG. 7, an example is shown in which a 2-position four-way switching valve is configured as the flow path switching valves V1 to V4, but the same function may be realized by a combination of three-way flow switching valves. However, it goes without saying that it may be realized by a combination of switching valves having an opening / closing function.

[About heat treatment units 3uA and 3uB]
In this apparatus, in FIG. 7, the heat treatment units 3uA and 3uB have functions corresponding to the “liquefaction storage mode” and the “revaporization mode”, respectively. In STEP 1 shown in Table 2, the gaseous liquefied gas is introduced into the heat treatment unit 3uA via the open switching valve 33a and the liquefied gas introduction pipe 3eA, liquefied by the liquefying means 3aA, and stored by the storage means 3bA. At the same time, the re-vaporized liquefied gas is supplied through the liquefied gas outlet pipe 3fB and the open switching valve 33d. In STEP 2, the liquefied gas introduced into the heat treatment unit 3uB via the open switching valve 33b and the liquefied gas introduction pipe 3eB is re-vaporized through the liquefied gas outlet pipe 3fA and the open switching valve 33c. Served through.

  That is, when the heat treatment unit 3uA is in the “liquefaction storage mode”, the switching valve 33a is in the open state, the switching valve 33c is in the closed state, and in the heat treatment unit 3uB in the “revaporization mode”, the switching valve 33b is closed. State, the switching valve 33d is in the open state. Conversely, when the heat treatment unit 3uB is in the “liquefaction storage mode”, the switching valve 33b is opened, the switching valve 33d is closed, and the heat treatment unit 3uA in the “revaporization mode” is closed. State, the switching valve 33c is opened. In FIG. 7, the “open state” of the switching valves 33 a to 33 d is indicated by the valve part white, and the “closed state” is indicated by the valve part black.

  The two heat treatment units 3uA and 3uB can supply liquefied gas continuously by switching control so that the two actions of “liquefaction storage mode” and “revaporization mode” are alternately performed. . The switching is performed when the remaining amount of the liquid in the heat treatment unit 3uB in the “revaporization mode” is equal to or lower than a preset level. The remaining amount is normally detected by measuring the weight. For this purpose, the two tanks are installed on the load cell 32.

  The operation of the heat treatment unit 3uA in the “liquefaction storage mode” will be described in a little more detail. The first refrigerant (for example, −10 to −5 ° C.) is circulated and supplied to the liquefying means 3aA, and the liquefied gas in the gas state sent through the open switching valve 33a is cooled by the liquefying means 3a. The liquid phase liquefied gas is gradually stored in the storage means 3bA. Further, since the storage means 3bA is cooled by the second refrigerant (for example, 0 ° C.) circulating around, the internal pressure can be suppressed sufficiently low, so that the liquefaction can be continuously performed and the liquefied gas is stored. be able to. During this time, since the switching valve 33c is closed, the liquefied gas is not supplied from the heat treatment unit 3uA, and only the liquefied gas supplied is liquefied and stored. The switching valve 33a of the heat treatment unit 3uA is automatically closed when the amount stored in this way reaches a preset predetermined amount, and at the same time, the set temperature of the temperature control is the set value for liquefaction so far. Automatically switches to the re-vaporization mode setting. At the same time, the pump Pb that sent the second refrigerant to the heat treatment unit 3uA and the pump Pa that sent the first refrigerant to the liquefying means 3aA are stopped. The pump Pb is restarted when the temperature of the liquefied gas stored in the heat treatment unit 3uA becomes equal to or higher than the newly set temperature, and is turned on / off so that the temperature of the liquid in standby maintains the temperature of the “revaporization mode”. Operate. Before switching from “liquefaction storage mode” to “revaporization mode”, the mode change is made by shifting the liquid temperature on the “liquefaction storage mode” side in standby to the temperature setting of “revaporization mode” in advance. It is possible to avoid an insufficient pressure state.

  On the other hand, in the heat treatment unit 3uB in the “revaporization mode”, since the switching valve 33b is closed, the liquefied gas is not supplied. Further, since the first refrigerant does not flow into the liquefying means 3aB by the flow path switching valves V3, V4, the condensing function is also stopped. Further, since the switching valve 33d is opened, the gas phase portion existing above the liquid phase liquefied gas stored in the vaporizing means 3cB can be discharged. When the liquefied gas is consumed in the equipment or the like connected to the liquefied gas outlet pipe 3fB, it moves in the direction in which the pressure of the gas phase portion decreases through the liquefied gas outlet pipe 3fB, and accordingly, the vaporizing means 3cB The liquid phase liquefied gas quickly vaporizes to compensate for the pressure drop. Since the third refrigerant (for example, 15 ° C.) is supplied to the vaporizing unit 3cB, the liquefied gas in the vaporizing unit 3cB is maintained at 15 ° C., and thus is stabilized at a pressure corresponding to the saturated vapor pressure at 15 ° C. Liquefied gas in a gaseous state is supplied. When the amount of gas in the vaporization means 3cB becomes a predetermined amount or less, the supply is switched from the heat treatment unit 3uA that has previously stored the liquefied gas in the liquefied storage mode. At that time, the flow path switching valves V1 to V4 and the switching valves 33a and 33b are switched simultaneously, the pumps Pa and Pb are turned on, the switching valve 33c is opened, and the switching valve 33d is opened.

  Further, the two heat treatment units 3uA and 3uB each have a temperature control function using the refrigerant circulation switching system so as to be lowered in temperature and maintained at a constant temperature. That is, means for measuring the liquefaction temperature in the liquefaction means 3a, means for measuring the storage temperature in the storage means 3b, means for measuring the liquefied gas temperature of the liquid phase in the vaporization means 3c, and liquefaction temperature, storage temperature, liquid phase It has a means for controlling the liquefied gas temperature (not shown), and the temperature is controlled so as to lower the temperature to a temperature sufficient to liquefy the supplied liquefied gas and to re-vaporize and supply the gas. The That is, the temperature control of the heat treatment unit 3uA in the “liquefaction storage mode” is feedback controlled so that the wall surface temperature of the bottom surface of the container 3ba becomes a preset temperature, while the temperature control of the heat treatment unit 3uB in the “revaporization mode” Is constantly monitored by the pressure sensor 34B incorporated in the liquefied gas lead-out pipe 3fB of the vaporizing means 3c, and the liquid temperature obtained by calculating from the “saturated vapor pressure vs temperature” characteristic curve specific to the liquefied gas from the pressure value. It is preferable to employ a feedback control method so that the temperature is set in advance.

  In the above description, the case where the two heat treatment units 3uA and 3uB as shown in FIG. 7 have a switching function between the “liquefaction storage mode” and the “revaporization mode” has been described. However, this apparatus is not limited to this. Instead of this, it is also possible to switch one storage tank 31 between the “reliquefaction storage mode” and the “revaporization mode” batchwise.

<Configuration example of liquefied gas supply device according to the present invention>
FIG. 8 is a schematic diagram showing a basic configuration example of a liquefied gas supply apparatus (hereinafter referred to as “the present supply apparatus”) according to the present invention using the heat treatment apparatus. Primary liquefaction installed in a room dedicated to liquefied gas (hereinafter referred to as “liquefied gas supply chamber 10”) that is separate from the room (hereinafter referred to as “clean room 30”) where the process apparatus 5 that is a liquefied gas consumption facility is placed. A gas supply facility 1, a secondary liquefied gas supply facility 3 (equivalent to the heat treatment device 3) installed in the immediate vicinity of the process device, a primary piping facility 2 for connecting both, and a secondary liquefied gas supply facility 3 and a process device 5 is constituted by a secondary piping facility 4 to which 5 is connected. In FIG. 8, the process apparatus 5 is placed on the clean room floor 30a of the clean room 30, and the secondary liquefied gas supply equipment 3 is placed on the plenum floor 30b. In the primary liquefied gas supply facility 1, the liquefied gas filled in the filling container 1a is vaporized by the primary vaporization means 1b. The liquefied gas in a gaseous state is sent to the secondary liquefied gas supply facility 3 by the primary piping facility 2 having the primary piping 2a. The sent liquefied gas is liquefied again by the reliquefaction means 3a in the secondary liquefied gas supply facility 3, and stored in a liquid state by the storage means 3b. The stored liquefied gas is vaporized by the secondary vaporization means 3c. The liquefied gas in a gaseous state is supplied to the process device 5 by the secondary piping equipment 4 having the secondary piping 4a. Note that the exhaust gas from the process device 5 including the introduced liquefied gas is discharged through the exhaust gas treatment device 6.

  Installation and removal work of the filling container 1a delivered from the liquefied gas manufacturer is performed only in the liquefied gas supply chamber 10, and therefore, in the clean room 30 where the process equipment 5 where general workers are working is placed, the atmosphere of the piping The dangerous work of opening is not necessary. Therefore, it is possible to completely separate and centrally supply all the liquefied gas including the low vapor pressure liquefied gas from the clean room 30, which has been impossible in the past, so that safety can be dramatically increased and work efficiency can be improved. it can. Hereinafter, each component will be described.

[Primary liquefied gas supply equipment 1]
Specifically, as illustrated in FIG. 9, the primary liquefied gas supply facility 1 stores a filling container 1a filled with a liquefied gas in a liquid state in a casing 1z. The casing 1z As the vaporizing means 1b, together with the cooling unit 1c for lowering the temperature of the liquefied gas in the filling container 1a to a preset temperature, the heat of vaporization lost when the liquefied gas is vaporized and supplied is replenished when necessary. A temperature control system (not shown) that operates so that the temperature of the liquefied gas does not drop too much below the set temperature is provided by disposing the heating unit 1d. As the cooling unit 1c, it is sufficient that the lower part or the side surface of the filling container 1a can be cooled to about 10 ° C. from the ambient temperature (usually 10 to 30 ° C.). For example, the refrigerant from the refrigerant unit 1e is cooled as shown in FIG. The method used as a source can be applied. As the heating unit 1d, a method of using, for example, heated air or a lamp as a heat source in the lower part or side surface of the filling container 1a can be applied.

  Here, a means (not shown) for measuring the liquid phase liquefied gas temperature To in the filling container 1a and a means (not shown) for controlling the liquid phase liquefied gas temperature To in the filling container 1a are required. The However, since the pressure container for conveyance as the filling container 1a is a pressure container that passes between the liquefied gas manufacturer and the liquefied gas supply device, a temperature sensor is directly incorporated in the container in order to measure the temperature of the liquefied gas. Is difficult. At this time, the liquid phase temperature of the liquefied gas inside the filling container 1a is constantly monitored by a pressure sensor (not shown) provided on the outlet pipe and the pressure of the vaporized liquefied gas is determined from the pressure value. It can be obtained by calculation from the “saturated vapor pressure vs. temperature” characteristic curve, and it is preferable to apply this method from the viewpoint of speed of measurement and accuracy. In this supply apparatus, it is preferable to employ a method of feedback control to a constant temperature so that the liquid phase temperature thus obtained becomes a preset temperature.

  Note that the detection of the remaining amount of liquefied gas inside the filling container 1a is usually performed by weight measurement. For this reason, the filling container 1a is placed on the load cell 1f, and the remaining amount is reduced. At that time, the filling container 1a is replaced.

[Primary air supply piping system 2]
The primary pipe 2a, which is the primary piping system 2 between the primary liquefied gas supply facility 1 and the secondary liquefied gas supply facility 3, has a special diameter except that it has a pipe diameter corresponding to the supply amount of the liquefied gas. This is not a specification, but may be a pipe that is usually used in general semiconductor liquefied gas supply pipes, etc., and a heat retaining device or a heating device required for the purpose of preventing reliquefaction in the primary pipe 2a as in the prior art. Etc. are absolutely unnecessary. However, as described above, the liquefied gas having a low vapor pressure includes many corrosive and toxic gases, and a stainless steel pipe (SUS) or the like which is usually subjected to inner surface processing or inner surface processing is used. In the primary air supply piping system 2, the distribution of the environmental temperature Ta of the system is measured, and the lower limit value of the fluctuation range of the environmental temperature Ta of the primary air supply piping system 2 is predicted from the data, and the primary liquefaction is made. It is desirable to set the control temperature of the liquid phase liquefied gas temperature To of the gas supply facility 1 to a value lower than the lower limit value.

[Secondary liquefied gas supply equipment 3]
The secondary liquefied gas supply facility 3 has a function of re-liquefying the gaseous liquefied gas sent from the secondary liquefied gas supplying facility 3 and the primary piping facility 2 and temporarily storing the liquefied gas in a liquid state. A function of vaporizing the stored liquefied gas again and supplying it to the process apparatus in a gaseous state is required. In this supply apparatus, such a function can be ensured by using the heat treatment apparatus 3 described above.

  At this time, the liquefied gas sent from the filling container 1a was controlled so as to be constantly vaporized at a temperature lower than the pipe ambient temperature Ta, for example, 10 ° C. so as not to be reliquefied in the primary pipe 2a. Since the air is fed, the liquid is continuously liquefied in the liquefying means 3a by cooling to, for example, −5 ° C. or lower in the liquefying means 3a.

  On the other hand, in the vaporization means 3c in the “revaporization mode”, the secondary pipe 4a connected to the process device 5 and the gas phase portion existing above the liquid liquefied gas stored in the vaporization means 3c are in an open state. Are connected, and liquefied gas can flow out. When the liquefied gas is consumed in the process apparatus 5, the pressure in the vapor phase portion of the vaporizing means 3c moves in a direction that decreases, and accordingly, the liquid liquefied gas in the vaporizing means 3c compensates for the pressure drop. Vaporize quickly. Since the third refrigerant (for example, 15 ° C.) is supplied around the vaporizing means 3c, the liquefied gas in the vaporizing means 3c is kept at 15 ° C. As a result, the process apparatus 5 has a saturated vapor pressure at, for example, 15 ° C. A gas phase liquefied gas stabilized at a corresponding pressure is supplied. At this time, since the secondary pipe 4a connecting the secondary liquefied gas supply facility 3 and the process device 5 is normally laid in a clean room, the pipe ambient temperature Tb is 20 to 23 ° C., and the secondary pipe 4a is connected to the secondary pipe 4a. The flowing liquefied gas saturated at 15 ° C. is exclusively in the direction of taking heat from the surroundings of the pipe and is not re-liquefied in the secondary pipe 4a.

[Secondary air supply piping system 4]
This is the secondary piping 4a which is the secondary piping system 4 between the secondary liquefied gas supply equipment 3 and the process device 5 which is a gas consuming equipment. Similar to the primary pipe 2a, it is not a special specification except that it has a pipe diameter corresponding to the supply amount, and may be a pipe that is usually used in a general semiconductor liquefied gas supply pipe, or as in the prior art. Therefore, there is no need for heat insulation or a heating device required for the purpose of preventing reliquefaction in the piping. Like the primary air supply piping system 2, the secondary piping 4 a is preferably made of SUS material or the like, and measures the environmental temperature Tb of the secondary air supply piping system 4 to perform temperature management.

[Operation method in this device]
In this apparatus, it is preferable to operate according to the following processes, making use of the above functions.
(1) Step of primary vaporization of liquefied gas filled in the filling container 1a (2) Step of primary gas supply of the vaporized liquefied gas via the primary pipe 2a (3) Gasified liquefaction Step of liquefying the gas again (4) Step of storing the liquefied liquefied gas in the liquid phase (5) Step of secondary vaporizing the liquefied gas in the liquid state (6) Secondary piping of the vaporized liquefied gas Step (7) for supplying secondary air to the process device 5 through 4a Step for replenishing the liquefied gas in the liquid state used in Step (5) using the liquefied gas stored in Step (4)

  That is, in the case of a liquefied gas having a low vapor pressure, the liquefied gas that has been vaporized and sent is forcibly liquefied once near the process device 5 and then vaporized again and sent to the process device 5. Even so, liquefaction in the air supply piping (primary piping 2a and secondary piping 4a) is prevented and the air supply pressure from the filling container 1a to the process device 5 is secured to stably supply a desired flow rate. can do.

<Temperature control in this supply device>
In this supply apparatus, as shown in FIG. 10, in the primary liquefied gas supply facility 1, the liquid phase liquefied gas temperature (primary liquid phase temperature) To in the filling container 1 a is set to the environmental temperature of the primary piping facility 2. In the secondary liquefied gas supply facility 3, the liquefying temperature Tc or the storage temperature Ts is equal to or lower than the liquefied gas temperature To of the liquid phase, and the liquefied gas temperature of the liquid phase (secondary liquid phase temperature). Tg is controlled to be equal to or lower than the minimum temperature of the environmental temperature Tb. Hereinafter, the preset primary liquid phase temperature is “Tset1,” the liquefaction temperature (the wall surface temperature of the bottom surface of the storage tank 31a in the “reliquefaction storage mode”) is “Tset2,” and the secondary vaporization temperature (“revaporization”). The liquid phase temperature in the storage tank 31b in the “mode” is set to “Tset3”.

  In the conventional supply method, along with the problem of reliquefaction in the liquefied gas supply pipe, in the case of liquefied gas having a low vapor pressure, the supply pressure, that is, the differential pressure from the primary liquefied gas supply facility 1 to the process device 5 is obtained. There is a problem that ΔP cannot be secured sufficiently, and therefore a sufficient flow rate cannot be secured, and remote piping supply of low vapor pressure liquefied gas is difficult. On the other hand, this supply apparatus is provided with a kind of liquefied gas relay section called secondary liquefied gas supply equipment 3 in the middle of the air supply pipe, so that the primary liquefied gas supply equipment 1 and the secondary liquefied gas supply equipment 3 The mechanism which can set the pressure of the liquefied gas which flows through the primary piping 2a in between separately from the pressure which the process apparatus 5 requires is enabled. As a result, the temperature of the saturated vapor of the liquefied gas flowing through the primary pipe 2a is lowered to a point where re-liquefaction does not occur in the pipe, thereby solving the problem of pipe liquefaction in the long-distance pipe and the pressure caused by the long-distance pipe as well. It solves the two problems of shortage at the same time.

  Specifically, the liquid phase temperature setting (Tset1) of the primary liquefied gas supply facility 1 is set to the environmental temperature Ta of the primary pipe 2a from the primary liquefied gas supply facility 1 to the secondary liquefied gas supply facility 3. When the temperature is, for example, 10 ° C. so as to be always lower than the temperature of the portion (for example, 15 to 30 ° C.), reliquefaction in the primary pipe 2a can be prevented. Also, under this condition, if the set temperature (Tset2) of the storage tank 31a to be reliquefied in the secondary liquefied gas supply facility 3 is set to, for example, 0 ° C. and controlled to about ± 2 ° C., the air supply pressure of about 20 to 30 kPa is set. Can be obtained, and the excellent function of the supply device can be utilized. On the other hand, the liquid phase temperature (Tset3) of the storage tank 31b to be revaporized is higher than the temperature Tset2 set at the time of reliquefaction, and the secondary piping from the secondary liquefied gas supply equipment 3 to the process device 5 is used. And by setting the temperature to, for example, 15 ° C. so as to be always lower than the temperature of any part of the environmental temperature Tb (for example, 20 to 25 ° C.) of the air supply pipe 2a in the process apparatus 5, For example, a supply pressure of about 30 to 100 kPa required by the process apparatus 5 can be secured.

  That is, as shown in FIG. 10, in this temperature control system, the primary liquidus temperature To is 5 ° C. at least 3 ° C. higher than the ambient temperature (environment temperature Ta of the primary piping equipment 2), and the control margin is 5 Vaporize while keeping the temperature as low as ℃. As a result, the heat flow on the pipe wall surface in the primary pipe 1a is maintained in the direction of being taken into the vaporized liquefied gas inside the pipe from the surrounding environment outside the pipe. That is, at the time of vaporization, the liquefied gas that was saturated vapor at the vaporization temperature always receives heat from the outside of the piping during the course of flowing through the piping, and overheating that is unlikely to cause re-liquefaction in the piping from the saturated steam reliably. Since the steam region is shifted, the liquefied gas is not liquefied again in the conventional relay pipe.

  Further, when the primary liquefied gas supply facility 1 is placed in a room 10 different from the clean room 30 in which the process device 5 is placed, the primary pipe 1a only passes through the manufacturing process building. Assuming, for example, 15 ° C. as the lowest ambient temperature of the pipe 1a, it is sufficient. In that case, if the liquid phase temperature in the filling container 1a of the primary liquefied gas supply equipment 1 is controlled at a temperature setting and control accuracy of about 10 ° C. ± 2 ° C. sufficiently lower than 15 ° C., the above-mentioned purpose is Can be achieved.

Moreover, in this supply apparatus, it is preferable to perform the following operations (1-1) to (1-3) when starting the supply of the liquefied gas.
(1-1) The filled container is cooled by cold before the liquefied gas is supplied, and the liquefied gas temperature in the liquid phase is lower than the normal control temperature and lower than the minimum temperature of the primary piping system and the environment. (1-2) Start feeding the liquefied gas from the filled container (1-3) Heating the liquefied gas in the liquid phase, which has been further reduced in temperature by feeding, with normal heat, In other words, the temperature of the filling vessel is first cooled by cooling before the liquefied gas is supplied, and the liquefied gas temperature in the liquid phase is lower than the normal control temperature and lower than the minimum temperature of the primary piping system. In addition, even if the minimum temperature of the primary piping system is lower than the environmental temperature, the liquefaction of the air supply piping is surely prevented even if the temperature is lower than the environmental temperature. It is possible to secure air pressure.

<Another configuration example of the liquefied gas supply apparatus according to the present invention>
In the above description, the case where one secondary liquefied gas supply facility is connected to one primary liquefied gas supply facility has been described. However, the present invention provides a plurality of primary liquefied gas supply facilities. The secondary liquefied gas supply equipment can be connected to the primary piping equipment by branch piping, and the liquefied gas from the primary liquefied gas supply equipment is supplied to several of the secondary liquefied gas supply equipment at the same time. It is possible to configure a liquefied gas supply device (hereinafter referred to as “the present supply device 2”).

  As illustrated in FIG. 11, the supply device 2 is an embodiment in which three secondary liquefied gas supply facilities 3 x, 3 y, and 3 z are connected to one primary liquefied gas supply facility 1. It is. At this time, the secondary liquefied gas supply facilities 3x, 3y, and 3z may be in the same clean room zone having the same air-conditioning temperature, or the air-conditioning is distributed to a plurality of clean room zones 30x, 30y, and 30z. It may be installed.

  As described above, also in the present supply device 2, the setting of the air supply pressure in the secondary liquefied gas supply facilities 3x, 3y, 3z can be set regardless of the air supply pressure from the primary liquefied gas supply facility 1. it can. That is, in the supply device 2, the primary liquefied gas supply facility 1, the primary piping 2a, the secondary liquefied gas supply facilities 3x, 3y, and 3z and the secondary piping facilities 4x, 4y, and 4z have high independence. From the above, the primary piping facility 2 is constituted by a branch piping, and the primary liquefied gas is connected by connecting a plurality of secondary liquefied gas supply facilities 3x, 3y, 3z to one primary liquefied gas supply facility 1. The secondary liquefied gas supply facilities 3x, 3y, and 3z can be operated under different conditions for the liquefied gas from the supply facility 1. That is, for example, liquefied gas controlled to different secondary air supply pressures can be supplied to the plurality of process devices 5x, 5y, and 5z. Further, the secondary air supply flow rate can be set to different conditions for the process devices 5x, 5y, and 5z, respectively.

  In the above, a heat treatment apparatus such as a semiconductor special liquefied gas used in a semiconductor or FPD manufacturing process and a liquefied gas supply apparatus using the same have been described, but the present invention is not limited to such a liquefied gas for electronics, and various processes It can be applied to a heat treatment process for liquefied gas or various liquids. Further, when a plurality of temperature conditions are required, it is useful as an apparatus that supplies only a refrigerant having a corresponding temperature, and is particularly useful for a manufacturing process that requires heat treatment under a plurality of temperature conditions. For example, a processing means used for switching between cooling and heating in a process such as gas adsorption processing and purification processing is applicable.

Schematic showing a basic configuration example of a heat treatment device (this device) according to the present invention Explanatory drawing which illustrates the refrigerant generation unit in this device Explanatory drawing which illustrates temperature distribution of each refrigerant tank which constitutes a refrigerant generation unit in this device. Explanatory drawing which illustrates the structure of the refrigerant tank which comprises the refrigerant generation unit in this apparatus. Explanatory drawing which shows the structure of the liquefaction means which comprises the heat processing unit in this apparatus Explanatory drawing which shows the other structure of the liquefying means which comprises the heat processing unit in this apparatus. Explanatory drawing showing another configuration example of this device Explanatory drawing which shows the basic structural example of the liquefied gas supply apparatus (this supply apparatus) which concerns on this invention Explanatory drawing which shows the primary liquefied gas supply equipment which comprises this supply apparatus Explanatory drawing showing temperature control in this supply device Explanatory drawing which shows the other structural example of this supply apparatus Schematic illustrating a gas supply device according to the prior art Schematic illustrating the cooling processing means according to the prior art

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Primary liquefied gas supply equipment 1a Filling container 1b Primary vaporization means 2 Primary piping equipment 2a Primary piping 3 Thermal treatment apparatus (secondary liquefied gas supply equipment)
3a Liquefaction means 3b Storage means 3c Secondary vaporization means 3d Communication part 3u Heat treatment unit (liquefied gas supply equipment)
4 Secondary piping equipment 4a Secondary piping 5 Process device 6 Exhaust gas treatment device 7 Refrigerant generation unit 7a First refrigerant tank 7b Second refrigerant tank 7c Third refrigerant tank 10 Liquefied gas supply chamber 30 Clean room 30a Clean room floor 30b Plenum floor 71 Refrigeration Machine 72 Flow path 73 Refrigerant tanks Wa, Wb Partition Pa First circulation pump Pb Second circulation pump Pc Third circulation pump

Claims (7)

Generating a plurality of refrigerants having different temperatures using a single refrigerator, performing cooling treatment or heating treatment of the plurality of heat treatment units using the refrigerant, controlling the temperature of at least one of the refrigerants, Used as the reference cold energy for heat treatment in the heat treatment section ,
The refrigerant tank for generating and storing the refrigerant is composed of a plurality of refrigerant tanks having a multi-layer structure, storing the lowest temperature first refrigerant in the innermost first refrigerant tank, and surrounding the second in order of decreasing temperature. A heat treatment apparatus , wherein the second refrigerant is stored in the refrigerant tank, the third refrigerant is stored in the third refrigerant tank, and the nth refrigerant is stored in the nth refrigerant tank, and the refrigerant is supplied from the refrigerant tank to the heat treatment section. . It has at least two heat treatment parts that function as liquefaction means, storage means, and vaporization means, and has a function that can be switched independently and alternately, and the first refrigerant is used as cold heat for the heat treatment part for liquefaction means using, the with the second refrigerant used as a cold heat of the thermal processing unit for storage means, a heat treatment apparatus according to claim 1, wherein the use of the third refrigerant as a heat of the thermal processing for vaporizing means. In switching from the function as the liquefying means and the storage means to the function as the vaporizing means or vice versa, when any one of the functions can be secured after switching, the first to third are previously set. 3. The heat treatment apparatus according to claim 1, wherein switching of the refrigerant supply path or switching to the control temperature of each function is performed. The heat treatment apparatus according to any one of claims 1 to 3 , wherein the heat in the heat radiating part of the refrigerator is used as heat for temperature adjustment of the refrigerant whose temperature is controlled. The vaporizing means has a space through which the third refrigerant can flow so as to come into contact with the outer periphery and the bottom of the container that stores the object to be vaporized, and the third perpendicular to the bottom surface of the container on the bottom side of the space. The heat treatment apparatus according to claim 1 , further comprising a nozzle for injecting a refrigerant. A liquefied gas supply device for supplying a liquefied gas to a gas consuming facility that is supplied with a pipe from a container filled with liquefied gas and separated from the container,
The liquefied gas in a gas state fed through the pipe is liquefied and vaporized, or liquefied and stored, and vaporized using the heat treatment apparatus according to any one of claims 1 to 5. A liquefied gas supply device. Having at least two of the heat treatment apparatuses, using a plurality of refrigerants of different temperatures produced in the heat treatment apparatus,
In the first heat treatment apparatus, the gaseous liquefied gas is liquefied with the coldest refrigerant, or further the liquid liquefied gas is stored with the second coldest refrigerant,
In another heat treatment apparatus, the storage-treated liquefied gas is vaporized by a refrigerant having a temperature higher than those of these refrigerants,
The liquefaction / storage process and the vaporization process can be switched, and simultaneously with the switching, the refrigerant flow path for automatically switching between the refrigerant supplied to the first heat treatment apparatus and the refrigerant supplied to the other heat treatment apparatus The liquefied gas supply device according to claim 6 , further comprising a switching system.

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