JP2005079528A - High precision high pressure annealer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To solve problems of: the wear of a sealing means due to the complicated shape and structure of a reaction vessel; a requirement for a certain degree of skill in manufacturing, handling, and maintaining a device; difficulty in installing a heating means to the vicinity of the reaction vessel; poor efficiency in annealing operation; unnecessarily uniform temperature distribution inside the vessel performing the operation all the time; the indefinite dimension of steam supplied to a work and the indefinite finishing accuracy of the work; and poor operation efficiency. <P>SOLUTION: A high precision high pressure annealer has: a pressure vessel; a reaction vessel that is arranged in the vessel to define an annealing chamber for performing annealing to a work and comprise a tube and an end cap that are sealed and connected with each other by a sealing means; a heating means; a quartz glass sheet; a temperature control sensor; a deionized water supplying means for supplying deionized water into the reaction vessel; a part that is located inside the reaction vessel to hold the deionized water from the deionized water supplying means; and a pressure control means controlling the pressure inside the reaction vessel. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention generally relates to a high-pressure annealing apparatus for generating an oxide film or the like on a glass substrate for liquid crystal, a silicon wafer or the like, or for performing a desired heat treatment, and more particularly to an oxide film or the like on a glass substrate for liquid crystal or a silicon wafer. Therefore, high-precision annealing work can be achieved by supplying a proper amount of fluid such as pure water into the annealing chamber to prevent emptying and forming a uniform temperature distribution in the processing chamber. The present invention relates to a high-precision high-pressure annealing apparatus.

  When annealing a liquid crystal glass substrate or silicon wafer, etc., a method of heating the surface of the liquid crystal glass substrate or silicon wafer to a temperature of 600 ° C. or higher to oxidize the surface and forming an oxide film thereon Is known. However, in such a method, soda glass having a softening point of about 500 to 600 ° C. cannot withstand high temperatures, and the glass surface may melt. Therefore, it is required to use quartz glass having a softening point of about 1400 to 1700 ° C. instead of soda glass. However, quartz glass is generally expensive and not economical. Therefore, a laser annealing method that can instantaneously oxidize only the glass surface has been proposed. According to this method, even when soda glass is used, its surface does not melt, and it is not always necessary to use expensive quartz glass. However, with this laser annealing method, it is difficult to form a highly accurate oxide film, and it is not expected to form a highly accurate oxide film on glass. For this reason, recently, a high-pressure annealing water vapor treatment method in which an oxide film is formed using water vapor has been widely adopted.

FIG. 8 shows an apparatus 1 (for example, see Patent Document 1) that embodies the high-pressure annealing water vapor treatment method. In general, the high-pressure annealing apparatus 1 supplies high-temperature steam heated by the heating means 3 and 4 in the end cap 2 into the reaction vessel 6 in a high-pressure state via the flow path 5. The glass substrate for liquid crystal, that is, the workpiece 7 disposed in the reaction vessel 6 is subjected to high-pressure annealing steam treatment. At this time, in order to prevent the reaction vessel 6 from being destroyed by the high-temperature and high-pressure gas from the inside of the reaction vessel, the entire reaction vessel 6 is accommodated in a large pressure vessel 8, and the pressure vessel 8 and the reaction vessel 6 is pressurized to balance the pressure inside and outside the reaction vessel 6. Further, in order to speed up the treatment reaction and to form a high quality oxide film, a first additional heater 9 is provided between the pressure vessel 8 and the reaction vessel 6, and a second additional heater is provided above the reaction vessel 6. The additional heater 10 is provided to promote the reaction of water vapor in the reaction vessel 6. In this annealing apparatus 1, pure water for generating water vapor is accommodated in an internal container 11 formed at the lower end portion of the flow path 5 below the center portion of the end cap 2. In addition, in order to prevent the emptying state of the internal container 11 due to the lack of pure water in the internal container 11, valve means 12 that operates properly even under high pressure (for example, see Patent Document 2). An appropriate amount of pure water is fed from time to time from a pure water storage tank 13 installed outside the system (see, for example, Patent Document 3) to prevent emptying (see, for example, Patent Document 4).
Japanese Patent Application No. 2003-101651 Japanese Patent Application No. 2003-101627 Japanese Patent Application No. 2003-101610 Japanese Patent Application No. 2003-101548

  However, in the apparatus of the present invention, the shape and structure of the inner container are somewhat complicated, and the sealing means of the reaction container is expected to be worn out. In addition, a certain level of skill in manufacturing, handling and maintenance of the apparatus is expected. Was requested. Furthermore, it may be somewhat difficult to attach the heating means to the periphery of the inner container, and attention is required for its arrangement and attachment. In addition, since the heating means used is a normal electric heater, the efficiency of the annealing operation is not so excellent, and furthermore, the temperature distribution in the container for performing the annealing operation is not always uniform. It was not a thing. Further, since there is no means for always providing the vapor supplied to the workpiece in a fine ideal state, the finishing accuracy of the workpiece may not be constant, and the work efficiency is not necessarily ideal. Therefore, the problem to be solved by the present invention is to simplify the structure of the high-pressure annealing apparatus, and further to provide an apparatus with higher annealing work efficiency in the present invention. An object of the present invention is to provide an apparatus capable of performing an annealing operation with higher accuracy by making the temperature distribution in the container performing the annealing operation more uniform.

  The high-accuracy high-pressure annealing apparatus of the present invention defines a pressure vessel and an annealing chamber disposed in the pressure vessel for annealing a workpiece and sealed and connected to each other by a sealing means. A reaction vessel composed of a cylindrical body and an end cap, heating means for heating the inside of the reaction vessel, a quartz glass plate provided in the reaction vessel above the heating means, and a quartz glass plate A temperature control sensor arranged between the workpiece and the workpiece, a pure water supply means for supplying pure water into the reaction vessel, and a section for holding pure water from the pure water supply means in the reaction vessel And pressure control means for controlling the pressure in the reaction vessel.

  According to the present invention, the structure of the high-pressure annealing apparatus has a very simple shape and configuration, and the sealing means of the reaction vessel can be actively cooled, so that it does not require skill in operation, and the apparatus can be manufactured, handled, and It is intended to provide equipment that makes maintenance easier and further increases the efficiency of annealing work. In addition, by making the temperature distribution in the container that performs annealing work more uniform, extremely high accuracy is achieved. It has become possible to provide an apparatus capable of performing an appropriate annealing operation.

  In the present invention, the annealing apparatus having a complicated shape and structure so far is changed to an annealing apparatus having a simple shape and structure, and the sealing means of the reaction vessel is actively cooled to manufacture, handle and maintain it. Opaque quartz glass plate to make it easy and easy to perform each operation and operation, to improve the efficiency of annealing work, and to make the temperature distribution in the container that performs annealing work uniform. It was assumed that far infrared heat rays were used. Specific examples will be described below.

  FIG. 1 discloses a high-precision high-pressure annealing apparatus 15 that supplies pure water from outside into a predetermined portion of a pressure vessel and then performs a predetermined annealing water vapor treatment while heating and pressurizing the inside of the pressure vessel. This high-precision high-pressure annealing apparatus 15 generally has a sturdy pressure vessel 16 made of, for example, steel. The pressure vessel is composed of an upper vessel 17 and a lower vessel 18, and the upper vessel 17 and the lower vessel 18 are tightly coupled to each other through a sealing means 19 such as an O-ring. The pressure vessel 16 is desirably cooled around the periphery by means (not shown) such as a cooling jacket.

  Inside the pressure vessel 16, a reaction vessel 20 made of, for example, a stainless steel material is fixed at a predetermined position by a known means. The reaction vessel 20 is composed of a bottomed cylindrical body 21 disposed downward and an end cap 22 having a generally upper bay shape that closes the lower end portion of the cylindrical body. The lower end of 21 and the outer peripheral edge of the end cap 22 are hermetically sealed by a sealing means 23 such as a 0 ring. The reaction vessel 20 has an annealing chamber 24 formed therein.

  A predetermined number of workpieces, that is, workpieces 25 to be annealed are arranged in the annealing chamber 24 by known means. In the annealing chamber 24, a temperature control sensor 26 for measuring the temperature in the annealing chamber and controlling the chamber temperature is disposed below the work 25. The temperature control sensor 26 performs on / off adjustment or PID (proportional integral derivative) control of heating means 28 and 34, which will be described later, as necessary. Further, a quartz glass plate, preferably an opaque quartz glass plate 27, is disposed below the temperature control sensor 26, and the heat rays radiated from the main heating means 28 disposed below the opaque quartz glass plate 27 are converted into far-infrared rays. It has been converted to heat rays. Thus, the temperature distribution in the annealing chamber 24 is made uniform. Further, a dispersion made of another quartz glass plate having substantially the same dimensions as the quartz glass plate 27, a stainless steel material or other materials (for example, ceramics) is preferably disposed between the workpiece 25 and the temperature control sensor 26. The plates 27A are arranged approximately 20 mm to 50 mm apart. The glass plate 27 and the dispersion plate 27 </ b> A have a diameter slightly smaller than the diameter of the cylindrical body 21. In the illustrated example, both the glass plate 27 and the dispersion plate 27A are shown as solid flat plates. However, for example, a round hole with a diameter of 30 mm is provided in the center of the glass plate 27 with a radius R, and the radius is the same. It is also possible to arrange circular holes with a radius of 15 mm on the concentric circle of the radius (R / 2) of the R dispersion plate 27A with a 90 ° interval.

  At this time, attention should be paid to the quartz glass plate 27 so as to form an annular gap of about 1 cm to 5 cm, for example, between the inner wall surface of the cylinder 21 and the outer peripheral edges of the quartz glass plate 27 and the dispersion plate 27A. And defining the dimensions of the dispersion plate 27A, providing the total area of the holes of the glass plate and the total area of the holes of the dispersion plate equal to each other, and the positions of the holes of the glass plate and the holes of the dispersion plate It is desirable to arrange them so that they do not match each other. This is because the vapor can be appropriately dispersed. This is because if the distance between the inner wall surface of the cylindrical body 21 and the quartz glass plate 27 is too narrow, it becomes difficult to attach the quartz glass plate or the like, and if it is too wide, the dispersion efficiency decreases. This is because the speed of the vapor passing through the upper and lower holes is different, so that pressure fluctuations may occur and the vapor grains grow, and if the positions of the holes are aligned, the dispersion efficiency is lowered. Of course, it is possible to further increase the number of dispersion plates, and as the number increases, the dispersion efficiency increases accordingly. However, it is possible to dispense with a dispersion plate. Furthermore, it is possible to provide a desired hole only in the quartz glass plate 27 or only in the dispersion plate 27a. A reservoir 29 for containing pure water is formed on the central upper surface of the end cap 22 having the upper bay shape. Further, an annular groove portion 30 opened in the annealing chamber 24 is formed at a joint portion between the outer peripheral edge of the end cap 22 sealed and joined by the sealing means 23 and the lower end portion of the bottomed cylindrical body 21. Is formed.

  Further, a pipe 31 having an opening for supplying pure water from the outside to the reservoir 29 of the end cap 22 is hermetically disposed in the annealing chamber 24. The pipe 31 communicates with an external fluid source 33 through valve means 32 as necessary. Here, the valve means 32 may be anything that can be freely opened and closed even in a high pressure state. For example, the valve means 32 described in Patent Document 2 is desirable, but not limited thereto. The external fluid source 33 is substantially the same as the pure water storage tank 13 shown in FIG. 8, and the configuration thereof is described in detail in Patent Document 3 as described above. Since a similar external fluid source is used in the embodiment of FIG. 5, the outline of the configuration will be described in some detail in FIG. However, in this embodiment, the means for supplying pure water to the pipe 31 is not limited to an external fluid source having a complicated configuration as shown in the figure, and is merely a container for supplying pure water. Also good. This is because the valve means 32 is opened only when pure water is supplied to the reservoir 29 at the start of work.

  A sub-heating means 34 is arranged in the pressure space between the reaction vessel 20 and the pressure vessel 16 so as to surround the reaction vessel 20. This sub-heating means assists the processing temperature in the annealing chamber 24 provided by the main heating means 28 to maintain a constant value during the annealing process. Further, the end cap 22 has a conduit 35 extending downward from the upper edge portion of the groove portion 30 hermetically formed at the joint portion between the lower end portion of the bottomed cylindrical body 21 and the outer peripheral edge of the end cap 22. A pressure sensor 36 is attached to the conduit 35 and extends to the outside of the pressure vessel 16. Further, a water level detection sensor (not shown) can be disposed in the groove 30 so that the sensor can close the valve means in synchronization with the valve means 32. It should be noted that internal pressure means, pressure reduction means, work holding means, auxiliary heating means, and other various pressure sensor means and temperature sensors that are usually provided in known annealing apparatuses are also provided in the present invention. Are not directly related and are not shown for clarity. The same applies to the following embodiments.

  The operation of the device 15 shown in FIG. 1 will be described. First, the work 25 is disposed inside the annealing chamber 24 of the apparatus 15. The valve means 32 is opened and pure water is supplied from the opening of the pipe 31 into the reservoir 29. The amount of pure water supplied at this time is set to be approximately equal to the amount to be consumed in one annealing process in order to eliminate waste. Therefore, the size of the reservoir 29 only needs to be large enough to accommodate pure water consumed in one annealing process. Thereafter, the heating means 28 and 34 are activated in a sealed state to heat the annealing chamber. As the temperature in the annealing chamber rises, pure water starts to vaporize in the annealing chamber 24. The temperature in the annealing chamber is finally raised to a predetermined value (for example, 300 ° C.) optimum for the annealing operation. On the other hand, the indoor pressure is sequentially increased with the evaporation of pure water, and finally rises to a predetermined value (for example, 1.31 MPa in absolute pressure) optimum for the annealing process. Therefore, the saturated steam temperature at a pressure of 1.31 MPa is about 192 ° C., and the saturated steam pressure at 300 ° C. is 8.59 MPa. For this reason, the pure water at room temperature is sequentially heated in the reaction vessel 20, but the vaporized vapor before being pressurized to a pressure of 1.31 MPa is below the cylinder 21 that has not yet reached the saturated water vapor temperature. It adheres to the portion and the end cap 22 and condenses to become condensed water and accumulates in the groove 30. Of course, when pure water is supplied to the reservoir 29, it is also possible to supply a predetermined amount to the groove 30 at the same time.

  The moisture in the groove 30 is in contact with the lower end portion of the cylinder 21 and the outer peripheral portion of the end cap 22 and these portions are cooled by cooling means (not shown), so that the temperature rises. Inferior to other parts. For this reason, the moisture in the groove 30 is not vaporized even during the annealing operation, and is kept at about 192 ° C. or lower. The moisture in the groove portion 30 thus provides a function of cooling the sealing means 23 that seals and joins the lower end portion of the cylindrical body 21 and the outer peripheral portion of the end cap 22. The sealing means 23 usually causes damage at about 200 ° C., but as long as the sealing means 23 is maintained at about 192 ° C., the sealing means 23 always functions normally. On the other hand, when the pure water stored in the reservoir 29 is heated to 300 ° C. by the main heating means 28, the pure water evaporates and becomes superheated steam, fills the inside of the annealing treatment chamber and fills the treatment chamber to 1.31 MPa. Pressurize. In this manner, the desired annealing process can be achieved by appropriately superheated vaporization to form a desired oxide film. Some steam that has just been boiled has dimensions similar to water droplets. Therefore, in the present invention, in order to prevent the water vapor having a size close to that of the water droplets from directly acting on the work piece to prevent inappropriate annealing treatment, the water vapor generating source is provided near the reservoir. A quartz glass plate 27 is disposed, and a dispersion plate 27A is further disposed thereon. These glass plates and dispersion plates convert water vapor of this size into the desired small size of vapor while dispersing it to the periphery to achieve a uniform temperature distribution, so that all the water vapor becomes the water vapor with the most favorable size for annealing treatment. This guarantees that it will rise into the annealing chamber.

  From this, it can be seen that the quartz glass plate 27 provides a function of dispersing water vapor in addition to forming far-infrared heat rays. It is also effective to provide the above-described holes in the quartz glass plate 27 and the dispersion plate 27A. This is because a water vapor labyrinth is positively formed and the same effect can be obtained. As described above, the temperature in the annealing chamber 24 is maintained at a predetermined value by the temperature control sensor 26, and the pressure is maintained by the pressure sensor 36 in the conduit 35 by on-off control or PID control. When the pressure exceeds a predetermined value, the sensor 36 adjusts by releasing the relief valve 37. Since the amount of pure water supplied to the reservoir 29 is sufficient to be consumed in a single annealing process, the reservoir 29 is not sprinkled, and excess pure water is also generated. It does not occur. In addition, since the sealing means 19 of the pressure vessel 16 is cooled to a predetermined value or less by the cooling medium of the pressure vessel 16, it is not necessary to consider means for cooling the sealing means 19 in particular.

  After the annealing process is completed, the heating unit and the pressurizing unit are turned off, and the workpiece that has completed the annealing operation is taken out. Further, condensed water remaining in the groove 30 is taken out. In this annealing process, far-infrared heat rays are used as a heat source, and since the vapor is further dispersed by the dispersion plate, the temperature distribution in the annealing chamber 24 is made uniform, and an extremely accurate annealing operation is achieved. Is done. Furthermore, since the reaction vessel 20 has a very simple structure with only the reservoir 29, the device 15 can be easily manufactured, and the operation does not require high technology.

  FIG. 2 shows another embodiment obtained by improving the apparatus shown in FIG. 1, and the overall configuration is similar to that of FIG. However, the embodiment shown in FIG. 2 differs from the embodiment shown in FIG. 1 in that the reservoir provided in the end cap in FIG. 1 is omitted, and instead, a groove is formed larger, and the reservoir is opened to the reservoir. The opening of the pipe is oriented to the groove. The other points are substantially the same as in the apparatus of FIG. Therefore, in the following, the same reference numerals as in FIG. 1 are given to members similar to those in FIG. 1, and only differences from the apparatus in FIG. 1 will be described.

    In the high-precision high-pressure annealing apparatus 15a shown in FIG. 2, the end cap 22a has an upper bay shape, and the opening of the pipe 31a communicating with the external fluid source 33a is directed to the groove 30a. Pure water required for the annealing process is directly supplied to the groove 30a from the outside. By the operation of the heating means 28a and 34a, the pure water in the upper part of the pure water located in the groove 30a becomes water vapor, and the excellent annealing effect similar to that in the case of FIG. 1 can be provided. On the other hand, the pure water in the lower part of the pure water accumulated in the groove 30a is in contact with the lower end portion of the cylindrical body 21a cooled by a cooling means (not shown) and the outer peripheral portion of the end cap 22a. The temperature rise is inferior to the upper part. For this reason, the moisture in the lower part of the groove 30a is not vaporized even during the annealing operation, and is kept at about 192 ° C. or lower. Thus, the moisture in the lower portion of the groove 30a has a function of cooling the sealing means 23a that seals and joins the lower end portion of the cylindrical body 21a and the outer peripheral portion of the end cap 22a, as in the embodiment of FIG. provide. Other configurations and operations are the same as those of the embodiment shown in FIG.

  After the annealing process is completed, the heating unit and the pressurizing unit are turned off, and the workpiece that has completed the annealing operation is taken out. Further, condensed water remaining in the groove 30a is taken out. In this annealing process, far-infrared heat rays are used as a heat source, and since the vapor is appropriately dispersed, the temperature distribution in the annealing chamber 24a is made uniform, and an extremely accurate annealing operation is achieved. The Furthermore, since the reaction vessel 20a has a very simple structure, the apparatus 15a can be easily manufactured, and therefore, the operation does not require high technology.

  The high-precision high-pressure annealing apparatus shown in FIG. 3 is substantially the same as the apparatus shown in FIG. 2, but the attachment position of the main heating means is different in FIG. That is, in FIG. 2, the main heating means 28a is disposed inside the annealing chamber 24a above the end cap 22a, but in the embodiment of FIG. 3, it is disposed outside the annealing chamber. In general, when the heating means is operated, it is known that metal ions are scattered from the heating means to the surroundings with heating. For this reason, when the workpiece does not like such scattered metal ions, it is necessary to separate the heating means from the annealing chamber for processing the workpiece, as in the embodiment shown in FIG. In the following, members similar to those in FIG. 1 are denoted by “b” to the numbers of those members, and only differences from the embodiment shown in FIG. 2 are described.

  In the high-accuracy high-pressure annealing apparatus 15b shown in FIG. 3, the main heating means 28b is arranged outside the annealing chamber 24b. In such a case, preferably, the bottomed cylinder 21b and the end cap 22b constituting the annealing chamber 24b, and the dispersion plate disposed between the workpiece and the temperature control sensor all generate scattered metal ions. For example, it is desirable to form with quartz glass. Furthermore, in the embodiment of FIG. 3, it is desirable that the pipe 31b, the valve means 32b, the conduit 35b, the pressure sensor 36b, the valve means 37b in the conduit 35b, the external fluid source 33b, etc. are all covered with a quartz member. This is to prevent scattered metal ions generated from these members from adhering to the workpiece. The operation of the apparatus shown in FIG. 3 and the treatment method after completion of the annealing process are substantially the same as those described in FIG. Also in this annealing process, far-infrared heat rays are used as a heat source, and since the vapor is appropriately dispersed, the temperature distribution in the annealing chamber 24b is made uniform, and an extremely accurate annealing operation is achieved. The Furthermore, since the reaction vessel 20b has a very simple structure, the apparatus 15b can be easily manufactured, and therefore, the operation does not require high technology.

  FIG. 4 discloses another specific example of a high-precision high-pressure annealing apparatus. In the apparatus shown in FIG. 4, the main heating means is disposed outside the annealing chamber. In this respect, as in the apparatus of FIG. 3, it is optimal for the work where it is desired to prevent metal ions from adhering to the workpiece. However, the form in which pure water for forming an oxide film is sent to the annealing chamber is different. That is, in this embodiment, the pure water sent to the annealing chamber is not a liquid as in the embodiments of FIGS. As a result, the pressure in the annealing chamber can be quickly adjusted, thereby making it possible to further reduce the occurrence of defective products. Other points are the same as those of the above-described embodiment. Therefore, only differences from the above-described embodiment will be described below.

  The high-accuracy high-pressure annealing apparatus 40 includes a pressure vessel 41 that is formed of a strong upper vessel and a lower vessel made of, for example, steel, and is sealed by a sealing means such as a 0 ring. The pressure vessel 41 is desirably cooled by a means such as a cooling jacket. Inside the pressure vessel 41, a reaction vessel 42 made of, for example, quartz glass material is accommodated and fixed at a predetermined position. The reaction vessel 42 has a bottomed cylindrical body 43 disposed downward, an end cap 44 having a generally upper bay shape closing the lower end portion of the cylindrical body, and a lower end portion and an end of the cylindrical body 43. And a sealing means 45 such as an O-ring that hermetically seals the outer peripheral edge of the cap 44. The reaction vessel 42 has an annealing chamber 46 formed therein.

  In the annealing chamber 46, a predetermined number of workpieces to be annealed, that is, workpieces 47, are arranged by known means. In the annealing chamber 46, a dispersion plate 49A, preferably made of a quartz glass plate, is disposed below the workpiece 47. Further, below the dispersion plate 49A, the temperature in the annealing chamber is measured and A temperature control sensor 48 for controlling the room temperature is arranged. The purpose and effect of the dispersion plate and the relationship with the quartz glass plate 49 are as described in detail with reference to FIG. However, this dispersion plate can also be deleted. Further, a quartz glass plate, preferably an opaque quartz glass plate 49 is disposed below the temperature control sensor 48. Below the opaque quartz glass plate 49 is disposed a pure water supply pipe 50 formed by winding a transparent or opaque quartz glass tube in a ring shape. A main heating means 51 is disposed below the end cap 44. The opaque quartz glass plate 49 converts the heat rays radiated from the main heating means 51 into far-infrared heat rays, thereby achieving a uniform temperature distribution in the annealing chamber 46. An annular groove 52 that opens into the annealing chamber 46 is formed at the joint between the outer peripheral edge of the end cap 44 that is sealed and joined by the sealing means 45 and the lower end of the bottomed cylinder 43. Has been.

  Furthermore, an opening 60 that opens into the annealing chamber 46 is formed at one end of the pure water supply pipe 50 that is arranged in the annealing chamber 46 and is wound in a ring shape. On the other hand, the other end 61 of the supply pipe 50 extends from the annealing chamber 46 through the end cap 44 and then the pressure vessel 41 to the outside of the apparatus. A valve means 53 and then a pressurizing means 54 such as a pump are connected to the other end extended to the outside of the apparatus. A sub-heating means 55 is disposed between the reaction vessel 42 and the pressure vessel 41 so as to surround the reaction vessel 42. This sub-heating means assists the processing temperature inside the annealing chamber 46 provided by the main heating means 51 to maintain a constant value during the annealing process. Further, in the periphery of the end cap 44 made of a quartz glass member and slightly above the groove 52, there is provided a conduit means 56 penetrating through the pressure vessel 41 from there. This conduit means 56 is equipped with a pressure sensor 57 and a relief valve 58. It should be noted that internal pressure means, pressure reduction means, work holding means, auxiliary heating means, and other various pressure sensor means and temperature sensors that are usually provided in known annealing apparatuses are also provided in the present invention. Are not directly related and are not shown for clarity.

  The operation of the high-precision high-pressure annealing apparatus 40 shown in FIG. 4 will be described. A work 47 is disposed inside the annealing chamber 46 of the apparatus 40. The valve means 53 is opened and pure water is supplied from the opening 60 of the pure water supply pipe 50 into the groove 52 through the pressurizing means 54. At this time, the amount of pure water supplied to the groove portion may be an amount that can effectively cool the sealing means 45 below the groove portion 52. This is because there is not much use as pure water that is vaporized to form an oxide film in the annealing treatment. Thereafter, the heating means 51 and 55 are activated, and the annealing chamber 46 is heated in the same manner as described in FIG. For this reason, as the temperature in the annealing chamber rises, the pure water in the groove 52 starts to vaporize first. Therefore, the pressure in the processing chamber starts to rise. However, the steam that has contacted the cylindrical body 43 or the like that has not reached the predetermined temperature condenses and returns to the groove portion 52 as condensed water. The moisture in the groove 52 is in contact with the lower end portion of the cylinder 43 and the outer peripheral portion of the end cap 44, and these portions are cooled by a cooling means (not shown). Inferior to other parts. For this reason, even during the annealing operation, the moisture in at least the lower part of the groove 52 is not vaporized, and is kept at about 192 ° C. or lower as described with reference to FIG. The moisture in the groove portion 52 thus provides a function of cooling the sealing means 45 that seals and joins the lower end portion of the cylindrical body 43 and the outer peripheral portion of the end cap 44.

  When the internal pressure of the processing chamber increases, the valve means 53 is opened and pure water is supplied into the processing chamber 46 by the pressurizing means 54. At this time, the supply pipe 50 is sufficiently heated, and the pure water supplied from the other end 61 is further heated in the processing chamber. For this reason, the pure water supplied through the valve means 53 becomes steam and is discharged from the opening 60 of the supply pipe 50. This steam is further heated in the processing chamber, becomes superheated steam, reaches the workpiece 47, and achieves a predetermined annealing operation. When the pressure inside the processing chamber 46 exceeds a predetermined value, the pressure sensor 57 is actuated to close the valve means 53 to stop the supply of pure water and open the relief valve 58 to release steam from the processing chamber. 46 Reduce the pressure inside. When the pressure decreases below a predetermined value, the relief valve 58 is closed and the valve means 53 is opened to allow the introduction of steam.

  After the annealing process is completed, the heating unit and the pressurizing unit are turned off, and the workpiece that has completed the annealing operation is taken out. Further, condensed water remaining in the groove 52 is taken out. In this annealing process, far-infrared heat rays are used as a heat source, and since the vapor is further dispersed by the dispersion plate, the temperature distribution in the annealing chamber 46 is made uniform, and an extremely accurate annealing operation is achieved. Is done. Furthermore, since the end cap 44 of the reaction vessel 42 has a very simple structure such as an upper bay shape, the device 40 is easy to manufacture, and therefore, the operation does not require advanced techniques. As the valve means 53 and the relief valve 58, for example, those previously disclosed in the above-mentioned Patent Document 3 by the same applicant as the present applicant can be used, but the invention is not limited thereto.

  In this embodiment, the reaction vessel 42 is made of a quartz glass material to prevent unnecessary metal ions from adhering to the workpiece. Accordingly, the pure water supply pipe 50 as well as the conduit means 56 and the dispersion plate 49A need to be made of quartz glass, and the valve means 53, the relief valve 58, the pressurizing means 54, and the pressure sensor 57 are made of quartz. Must be covered with glass. Further, in this embodiment, the pure water supply pipe 50 is made of opaque quartz glass and is densely arranged concentrically, so that the opaque quartz glass plate 49 becomes unnecessary. When the pure water supply pipe is made of transparent quartz glass or opaque quartz glass, when it is roughly arranged concentrically, the provision of the opaque quartz glass plate 49 generates far infrared heat rays. This is preferable. Also in this annealing process, far-infrared heat rays are used as a heat source, and since the vapor is appropriately dispersed, the temperature distribution in the annealing chamber 46 is made uniform, and an extremely accurate annealing operation is achieved. The Furthermore, since the reaction vessel 42 has a very simple structure, the apparatus 40 can be easily manufactured, and the operation does not require high technology.

  FIG. 5 discloses another specific example of a high-precision high-pressure annealing apparatus. The apparatus of FIG. 5 is substantially an improvement of the apparatus shown in FIG. 4, and the overall configuration and function are the same as those of the apparatus shown in FIG. Accordingly, with respect to FIG. 5, only the pure water supply method, which is different from the apparatus of FIG. 4, will be described. For easy understanding, in FIG. 5, the same members as those in the apparatus shown in FIG.

  In the high-accuracy high-pressure annealing apparatus 40c shown in FIG. 5, pure water having an opening 60c in the annealing chamber 46c and concentrically arranged in an annular shape to supply pure water into the annealing chamber 46c. The other end 61c of the supply pipe 50c extends from the annealing chamber 46c through the end cap 44c. Further, a pure water piping device 65 is arranged on a part of the outside of the sub-heating means 55c arranged between the reaction vessel 42c and the pressure vessel 41c. The piping device 65 includes an upper pipe 66 that communicates with the upper part of the annealing chamber 46 c of the reaction vessel 42 c, and a lower pipe 68 that communicates with the other end 61 c of the pure water supply pipe 50 c via a valve 67. The upper pipe 66 is connected to the upper pipe 66 and the lower pipe 68 is connected to the lower pipe 68. The pure water delivery pipe 70 is connected to the upper pipe 66. Further, a liquid level sensor 71 is preferably attached to the adjustment pipe 69. Further, the pure water delivery pipe 70 is connected to a pure water delivery tank device 75. The pure water delivery tank device 75 is preferably a tank device as described in detail in the above-mentioned Patent Document 3, for example. However, it is not limited to this. It should be noted that internal pressure means, pressure reduction means, work holding means, auxiliary heating means, and other various pressure sensor means and temperature sensors that are usually provided in known annealing apparatuses are also provided in the present invention. Are not directly related and are not shown for clarity.

  This pure water delivery tank device 75 generally has a tank main body 76 in a sealed state, a main supply line 77 for supplying pure water into the tank main body 76, and the atmospheric pressure in the tank main body 76. A vent line 79 having an on-off valve 78 for adjustment and a high-pressure inert gas (for example, nitrogen gas) is forcibly supplied into the tank body 76 to bring the tank body 76 into a high-pressure state, and pure water in the tank body is supplied. And an inert gas supply line 81 for forcibly feeding into the pure water flow path 80. The main supply line 77 and the pure water flow path 80 are provided with on-off valves 77a and 80a, respectively. The tank main body 76 is provided with an upper limit alarm sensor 82, an upper limit detection sensor 83, a backflow leakage detection sensor 84, a lower limit detection sensor 85, and a lower limit alarm sensor 86 for detecting the level of pure water in the tank main body. ing.

  In the operation of the apparatus 40c shown in FIG. 5, normally, the pressure in the annealing chamber can be maintained at a predetermined pressure as long as an appropriate amount of steam is provided from the opening 60c of the pure water supply pipe 50c. A part of the vapor in the annealing chamber is recovered to the adjustment pipe 69 through the upper pipe 66, and further, the other end portion 61c of the pure water supply pipe is passed through the lower pipe 68 by the water head force of the condensed water accumulated there. Then, it is sent back to the opening 60c. However, if the steam leaks from the processing chamber or condenses in the annealing chamber and accumulates in the groove 52c, pure water corresponding to the shortage is sent from the pure water sending tank device 75. The condensed water accumulated in the groove 52c provides a function of cooling the sealing means. Here, each sensor of the tank device 75 senses the state of pure water contained in the tank body 76, and the upper limit alarm sensor 82 is an alarm sensor for limiting the supply amount from the main supply line 77. is there. The upper limit detection sensor 83 detects an appropriate upper limit position in the tank body. The leak sensor 84 detects the backflow when the pure water flows back from the annealing chamber. The lower limit detection sensor 85 detects that the amount of pure water in the tank body 76 has reached the lower limit position. The lower limit alarm sensor 86 senses that pure water supply has become impossible. The detailed function of this tank is described in Patent Document 3.

  Since the pure water piping device 65 is directly connected to the pure water delivery tank device 75, the supply of pure water to the annealing chamber does not stop. That is, the liquid level sensor 71 is installed in the adjustment pipe 69, and if the liquid level in the adjustment pipe 69 reaches a shortage position, the valve 80a of the pure water piping device is released to replenish pure water into the adjustment pipe. Because. When the pressure sensor 57c provided in the conduit means 56c senses that the pressure in the annealing chamber 46c has risen to a predetermined value or more, the valve 67 is closed and the relief valve 58c is opened. On the other hand, when the pressure sensor 57c senses that the pressure in the processing chamber has dropped below a predetermined value, the relief valve 58c is closed and the valve 67 is opened. Other operations of the apparatus shown in FIG. 5 are the same as those already described with reference to FIGS. Further, similarly to the embodiment shown in FIG. 4, the reaction vessel 42c is made of a quartz glass material to prevent unnecessary metal ions from adhering to the workpiece. Therefore, the pure water supply pipe 50c as well as the conduit means 56c and the dispersion plate need to be made of quartz glass, and the valve means, relief valve, pressure sensor, etc. need to be covered with quartz glass. is there. Furthermore, in this embodiment, the pure water supply pipe 50c is made of opaque quartz glass and is densely arranged concentrically, so that the opaque quartz glass plate 49 becomes unnecessary. When the pure water supply pipe is made of transparent quartz glass or opaque quartz glass, when it is roughly arranged concentrically, the provision of the opaque quartz glass plate 49 generates far infrared heat rays. This is preferable. Also in this annealing process, far-infrared heat rays are used as a heat source, and since the vapor is appropriately dispersed, the temperature distribution in the annealing chamber 46c is made uniform, and an extremely accurate annealing operation is achieved. The Furthermore, since the reaction vessel 42c has a very simple structure, it is easy to manufacture the apparatus 40c, and therefore, the operation does not require high technology.

  6 and 7 show still another embodiment. These embodiments are specifically described as modifications of the embodiment shown in FIG. 3, but are substantially embodiments in which the main heating means is disposed outside the annealing chamber. 5 is a modification of all the embodiments shown in FIG. In the embodiment shown in FIGS. 3 to 5, as described above, when the main heating means is heated, metal ions are generated from the heating means and the scattered metal ions are prevented from adhering to the workpiece. The means is arranged outside the annealing chamber, thereby eliminating the concern that scattered metal ions adhere to the workpiece. However, nothing has been done to deal with metal ions that may be generated from a temperature control sensor that measures the internal temperature of the annealing chamber. 6 and 7 disclose means for that purpose.

  6 will be described as a modification of the embodiment of FIG. Therefore, in FIG. 6, only points different from the embodiment of FIG. 3 will be described with reference to the reference numerals used for the embodiment of FIG. In FIG. 6, in the annealing chamber 24c, three opaque quartz plates 27c are disposed below the workpiece 25c, and one plate member 90 is disposed above the workpiece 25c. This quartz plate serves to prevent heat radiation from the work 25c to the periphery of the groove portion 30c having a relatively low temperature due to the generation of steam, but in particular, there are holes in the lower two of the three quartz plates. Appropriate distribution of the vapor formed and rising through the annealing chamber is intended. Further, the upper plate member 90 provides a function of appropriately reflecting the raised vapor downward, and serves to block the influence of heat above the plate member 90. If a plurality of plate members 90 are used, a better temperature distribution can be obtained. . It is preferable to use a quartz plate or a ceramic member that does not generate metal ions.

  However, for example, a cylindrical hollow portion 91 extending downward is preferably formed integrally with the end cap at the center of the end cap 22c. A test tube-shaped bottomed cylindrical body 92 preferably made of quartz glass is inserted into the hollow portion 91, and a lower portion where the opening of the bottomed cylindrical body 92 is provided is a lower end portion of the hollow portion 91. The bottomed cylindrical body 92 is disposed so as to open to the lower portion of the end cap 22c. At this time, the bottomed cylindrical body 92 is disposed so that the bottomed portion is located below the workpiece 25c and above the quartz plate 27c. In addition, a temperature control sensor 26c similar to that described above is inserted into and fixed to the bottomed portion of the bottomed cylindrical body 92.

  By adopting such a configuration, the temperature control sensor 26c can accurately measure the temperature in the annealing chamber 24c without causing any metal ions to scatter into the annealing chamber 24c. Other structural functions and operations of this embodiment are substantially similar to those described with respect to FIG.

  A high-precision high-pressure annealing apparatus 15d shown in FIG. 7 describes a further improvement of FIG. 6 discloses a configuration in which a hollow portion extending downward is formed in the center portion of the end cap, and a bottomed cylindrical body for inserting a temperature control sensor is inserted into the hollow portion to couple them together. An embodiment in which the structure of the apparatus of FIG. 6 is simplified by forming a temperature control sensor cylinder extending upward from the end cap itself is disclosed. Therefore, in the following description, only points different from the embodiment of FIG. 6 will be described, particularly by attaching d to the reference numerals used for the embodiment of FIGS. That is, in FIG. 7, the temperature control sensor cylinder 93 is preferably formed integrally with the end cap upward from the central portion of the end cap 22d. The temperature control sensor cylinder 93 has a bottomed cylindrical shape, and is arranged so that the bottomed portion is located below the workpiece 25d and above the quartz plate 27d. Further, a temperature control sensor 26d similar to that described above is inserted into the bottomed portion of the temperature control sensor cylinder 93 and fixed thereto.

  By adopting such a configuration, the temperature control sensor 26d can measure the temperature in the annealing chamber 24d without scattering any metal ions into the annealing chamber 24d. Compared to the configuration, the configuration is simple.

  It will be apparent to those skilled in the art that the embodiments shown in FIGS. 6 and 7 can be applied to the embodiment shown in FIGS. 4 and 5 in addition to the embodiment shown in FIG. .

  The high-accuracy high-pressure annealing apparatus of the present invention can achieve a high-precision high-pressure annealing operation with an apparatus having a very simple structure, so that the yield of the operation is increased and a uniform and high-quality annealing operation is extremely achieved. It becomes possible to carry out at a low price. Therefore, it can be optimally used for the manufacture of many liquid crystal color filters, the formation of liquid crystal TFT substrates, the firing of plasma display materials and their annealing operations, the drying of organic electric luminescent substrates, and other similar operations.

It is the figure which showed the 1st Example of this invention. It is the figure which showed the 2nd Example of this invention. It is the figure which showed the 3rd Example of this invention. It is the figure which showed the 4th Example of this invention. It is the figure which showed the 5th Example of this invention. It is the figure which showed the 6th Example of this invention. It is the figure which showed the 7th Example of this invention. It is the figure which showed one example of the prior art example regarding this invention.

Explanation of symbols

15, 15a, 15b, 15c, 15d High-precision high-pressure annealing apparatus 16, 16a, pressure vessel 17 upper vessel 18 lower vessel 20 reaction vessel 21, 21a, 21b bottomed cylindrical body 22, 22a, 22b, 22c, 22d end cap 23 , 23a Sealing means 24, 24a, 24b, 24c, 24d Annealing chamber 25, 25a, 25b, 25c, 25d Work piece 26, 26a, 26c, 26d Temperature control sensor 27, 27c, 27d Opaque quartz glass plate 27A Dispersion plate 28 28a, 28b Main heating means 29 Reservoirs 30, 30a, 30c Grooves 31, 31a, 31b Pipes 32, 32a, 32b Valve means 33, 33a, 33b External fluid sources 34, 34a Sub-heating means 35, 35a, 35b Conduit 36 36a, 36b Pressure sensors 37, 37a, 37b Relief valve 4 0, 40c High-precision high-pressure annealing apparatus 41, 41c Pressure vessel 42, 42c Reaction vessel 43 Bottomed cylinders 44, 44c End cap 45 Sealing means 46, 46c Annealing chamber 47 Work 48 Temperature control sensor 49 Opaque quartz glass plate 49A Dispersion plate 50, 50c Pure water supply pipe 51 Main heating means 52, 52c Groove 53 Valve means 54 Pressurization means 55, 55c Sub heating means 56, 56c Conduit means 57, 57c Pressure sensors 58, 58c Relief valves 60, 60c Opening 61, 61c Other end 65 Pipe for pure water 66 Upper pipe 67 Valve 68 Lower pipe 69 Adjustment pipe 70 Pure water delivery pipe 71 Liquid level sensor 75 Pure water delivery tank apparatus 76 Tank main body 77 Main supply line 77a On-off valve 78 On-off valve 79 Ventilation line 80 Pure water flow path 80a On-off valve 81 Inert gas supply line 82 Limit alarm sensor 83 upper limit detection sensor 84 leak detection sensor 85 lower limit detection sensor 86 limit alarm sensor 90 plate member 91 hollow portion 92 bottomed tubular body 93 temperature control sensor accommodating cylinder

Claims (13)

High-precision high-pressure annealing equipment,
A pressure vessel;
The cylinder is disposed in the pressure vessel, defines an annealing chamber for annealing the workpiece therein, and includes a cylindrical body and an end cap that are sealed and connected to each other by sealing means. A reaction vessel;
Heating means for heating the inside of the reaction vessel;
A quartz glass plate above the heating means and provided in the reaction vessel;
A temperature control sensor disposed between the quartz glass plate and the workpiece;
Pure water supply means for supplying pure water into the reaction vessel;
A portion in the reaction vessel that holds pure water from the pure water supply means;
Pressure control means for controlling the pressure in the reaction vessel;
A high-accuracy high-pressure annealing apparatus characterized by comprising:   The cylindrical body has a bottomed cylindrical shape, the end cap has an upper bay shape, the sealing means sealingly connects the lower end of the cylindrical body and the outer peripheral edge of the end cap, and the cylindrical body The high-precision and high-pressure annealing according to claim 1, wherein a groove is formed in the reaction vessel around a sealing means for sealingly connecting the lower end portion and the outer peripheral edge of the end cap. apparatus.   3. The high accuracy according to claim 1, wherein at least one dispersion plate is disposed between the workpiece and the end cap in the reaction vessel, and a temperature control sensor is provided immediately above or immediately below the dispersion plate. High pressure annealing equipment.   The high-accuracy high-pressure annealing apparatus according to claim 1 or 2, wherein at least one dispersion plate is disposed on the upper part of the work in the reaction vessel.   The high-precision high-pressure annealing apparatus according to any one of claims 1 to 4, wherein the pure water supply means supplies liquid pure water.   The high-precision high-pressure annealing apparatus according to any one of claims 1 to 4, wherein the pure water supply means supplies gaseous pure water.   6. The high-accuracy high-pressure annealing apparatus according to claim 5, wherein the portion for holding pure water is provided at the top of the end cap having an upper bay shape.   6. The high-accuracy high-pressure annealing apparatus according to claim 5, wherein a portion for holding pure water is provided on an outer peripheral edge of an end cap having an upper bay shape.   7. The high-accuracy high-pressure annealing apparatus according to claim 6, wherein the portion for holding pure water is provided on the outer peripheral edge of the end cap having an upper bay shape.   The high-precision high-pressure annealing apparatus according to any one of claims 1 to 5, and 7 to 9, wherein the heating means is provided in the annealing chamber.   The high-precision high-pressure annealing apparatus according to any one of claims 1 to 6, and 8 to 9, wherein the heating means is provided outside the annealing treatment chamber.   The high-precision high-pressure annealing apparatus according to claim 1, wherein the quartz glass plate is an opaque quartz glass plate.   The high-precision high-pressure annealing apparatus according to any one of claims 11 and 12, wherein the temperature control sensor is accommodated in a cylinder extending from the end cap.

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